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CN100537741C - Decolorized Yeast Cell Wall Components - Google Patents

Decolorized Yeast Cell Wall Components Download PDF

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Publication number
CN100537741C
CN100537741C CN 03824455 CN03824455A CN100537741C CN 100537741 C CN100537741 C CN 100537741C CN 03824455 CN03824455 CN 03824455 CN 03824455 A CN03824455 A CN 03824455A CN 100537741 C CN100537741 C CN 100537741C
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China
Prior art keywords
cell wall
film
yeast cell
yeast
wall fraction
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CN 03824455
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Chinese (zh)
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CN1688688A (en
Inventor
江口敬宏
中村智彦
五味俊一
松本理加
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MC Food Specialties Inc
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Kirin Brewery Co Ltd
Asahi Kasei Chemicals Corp
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Abstract

用脱色剂将经酶处理的酵母中除去可溶性细胞内成分得到的细胞残渣,或者进一步将该细胞残渣用酸性水溶液处理、除去可溶解于酸性水溶液的成分得到的细胞残渣进行脱色处理,从而获得不影响脱色处理前的酵母细胞壁组分所具有的优异的性质,还可以在该物性中新加入优异的性质的脱色酵母细胞壁组分。本发明的脱色酵母细胞壁组分呈白色,且可以一直保持脱色前的酵母细胞壁组分所具有的、作为包被剂使用时的优点,并且可以新附加使酵母细胞壁组分的机械特性提高、酵母臭等降低等的优异的性质。

Figure 03824455

Using a decolorizing agent to decolorize the cell residue obtained by removing soluble intracellular components from the enzyme-treated yeast, or further treating the cell residue with an acidic aqueous solution to remove components soluble in the acidic aqueous solution. In order to affect the excellent properties of the yeast cell wall fraction before the decolorization treatment, a decolorized yeast cell wall fraction with excellent properties may be newly added to the physical properties. The decolorized yeast cell wall component of the present invention is white, and can always maintain the advantages of the yeast cell wall component before decolorization when used as a coating agent, and can be newly added to improve the mechanical properties of the yeast cell wall component. Excellent properties such as reduction of odor, etc.

Figure 03824455

Description

Decolorized yeast cell wall fraction
Technical field
The present invention relates to through decoloration and deodorization and have decolorized yeast cell wall fraction, its preparation method and this decolorized yeast cell wall fraction of improved characteristics purposes as coating agent.
Background technology
For a long time, about the utilization of yeast cell wall fraction, people attempt developing thin-film material from yeast always.For example disclose in the Japanese Patent Publication 56-19971 communique by taking off and removed the yeast cell film component in the nucleic acid yeast, obtaining with water dissolvable protein is the edibility protein film of main component; A kind of preparation method of film is disclosed in the Japanese kokai publication sho 53-45385 communique: with microorganism cellss such as yeast with hot alkali treatment after, add acid, the enforcement isoelectric precipitation is handled, to generate sedimentary pH regulator is 6-8, plastic binder in the gel formation microorganism cells of gained is with the resulting composition film forming.
In addition, disclosing a kind of in Japan's No. 3349677 communique of special permission (TOHKEMY 2000-44878 communique) is the coating agent of main component with the yeast cell wall fraction, and wherein said yeast cells wall contains the cell residue of removing composition in the soluble cell from the yeast of handling through enzyme; The coating agent that uses this coating agent and added softening agent is also disclosed, as the service condition of coating agent or film-coat.As the characteristic of this coating agent excellence, it has following function: even 100% water dispersion medium also can wrap quilt, though can not produce adhesion in the toughness processing, bag can not adhered between the particle of back, and the may command dissolution time; In addition, the film that is formed by this coating agent shows to have the extremely low characteristic of oxygen permeability coefficient under drying conditions.
But, as mentioned above, though the coating agent of putting down in writing in No. 3349677 communique of Japan's special permission has utmost point excellent thin film characteristics, but when using the film-coat of putting down in writing in this patent gazette, be tawny-brown, therefore compare the face shaping variation of encrusting substance, compressing tablet with interior bag thing, might be mistaken as rotten (for example think by mistake and go mouldy) and might therefore delay real the going bad of discovery the painted deterioration etc. that takes for.
In addition, in the coating agent of this special permission communique record, contain more protein (weight ratio is 21%), lipid (weight ratio is 8.0%) in the yeast cell wall fraction itself, so might be in preservation produce painted because of the oxidation of lipid etc.
And, how many yeast cell wall fractions itself has some from zymic smell (following composition yeast is smelly), therefore with aroma component as object wrap by the time, keep the target aroma component, the reason that the yeast that self is had owing to yeast cell wall fraction is smelly has and makes the danger that required aroma component is covered or suffer a loss on the other hand, it is low-level to need addition with this component be controlled at, and the result also has the problem that can't give full play to its effect.
In addition,, be wanting in snappiness (plasticity-) as the mechanical characteristics of film itself, more crisp, when making up with interior bag thing sometimes, because of the variation of environment such as extraneous humidity, the crackly tendency of film can appear.
On the other hand, known and when utilizing yeast cell wall fraction, need decolour yeast cell wall fraction. re-use after the deodorization.Disclose in the Japanese kokai publication hei 4-248968 communique yeast extract residue alkali and acid treatment, used ozone decolorization then, simultaneously the method for before and after this ozonize, handling with ethanol; Disclose in the flat 6-504191 communique of Japanese Unexamined Patent Application Publication Yeast debris handled with alkali, hydrogen peroxide etc. after, method and handled thing that the acidifying Yeast debris is handled; The method of the insolubles of yeast autolysis being carried out alkaline purification is disclosed in Japan's No. 3407125 communique of special permission (Japanese kokai publication hei 9-103266 communique) under suspending with ethanol.
But in these previous methods, it is rotten that the processing of carrying out for decoloration and deodorization makes that object being treated takes place, and loses its characteristic, and original cellular form and structure are destroyed, and the problem of forfeiture film-forming properties, film slaking therefore occurs; If under maintenance film-forming properties, film slaking state, directly decolour, the problem that can't decolour to the color of object level is then arranged, on utilizing, it has various restrictions.
Promptly, decoloration and deodorization about extraction residue of yeast extract etc., people are attempting always, method in the decolouring of carrying out in the past, Japanese kokai publication hei 4-248968 communique (decoloration and deodorization method of the extraction residue of yeast extract) for example, Japanese kokai publication hei 6-70751 communique (Yeast debris product), can see in the flat 6-504191 communique of Japanese Unexamined Patent Application Publication (processing of Yeast debris and products therefrom) as a result etc.: carrying out heat treated (also comprising refluxes boil etc.) under the high alkalinity condition and under the peracidity condition, carrying out heat treated (also comprising refluxes boil etc.), remove soluble components etc., handle with chemical reagent such as hydrogen peroxide then, or make ozone etc. and its reaction, perhaps make SYNTHETIC OPTICAL WHITNER and its reactions such as hypochlorous acid.Handle if these methods are directly used in the decolouring of yeast cell wall fraction, then in the gained decolorized yeast cell wall fraction, then exist the problem that the character of the excellence of described yeast cell wall fraction suffers damage.
On the other hand, in the medicine, seldom effective component is directly used with the form of compound, but,, cooperated medicinal additive to make preparation and use for making the effective component stripping at purpose.All medicinal additives are arranged, enumerate an example here.
For example, as medicinal aqueous wrapped dose of Eudragit that uses (acrylic resin) if LS30-D55 as the non-natural product, resistance to air loss low increase package amount is arranged then the problems such as slaking variation of film.Therefore, people wait in expectation water-based, resistance to air loss height, have evaporable effects such as preventing aroma component or smell, have enough slakings, from the coating agent of natural product.In addition, the yeast cell wall fraction of No. 3349677 communiques records of Japan special permission is water-based, from natural product, the resistance to air loss height, have film-forming properties, the film slaking is good, but owing to have from zymic color, smell, wishes to have a kind of yeast cell wall fraction of colourless, odorless.And HPC that uses in the tackiness agent or HPMC if its addition increases, the problem that the saccharoid disintegration postpones then occurs.If the yeast cell wall fraction drying then shows firm bounding force, but then show slaking faster in water, hence one can see that, and this is to have fusible disintegrating agent, but because it is tawny-brown, so the saccharoid that produces is tawny-brown, people wish it is colourless.
As capsular capsule material, known have gelatin, water-soluble polymer (hydroxymethyl ethyl Mierocrystalline cellulose), general Shandong indigo plant, a polyvinyl alcohol (PVA) etc., but they all because be difficult to carry out stripping control, to the resistance to air loss of oxygen low and have that medicament is rotten, the problem of the security (BSE and synthetic compound) of raw material etc.
As the method that addresses these problems, people attempt utilizing yeast cell wall fraction as capsule capsule material, have the document of this record to have: TOHKEMY 2002-38133 communique, TOHKEMY 2003-70428 communique.Therefore but in these methods, yeast cell wall fraction is tawny-brown, and the capsule color of making is tawny-brown, and protein in the yeast cell wall fraction, lipid are many, therefore has the problem of the painted grade of yeast cell wall fraction itself.
Problem of the present invention is to provide: through decoloration and deodorization, make from the color of yeast cell wall fraction and smell etc. to be removed, and have excellent film-forming properties, the resistance to air loss etc. that further preferably has an excellence that keeps or improve film slaking and formed film is maintained or purposes in coating agent of decolorized yeast cell wall fraction, its preparation method and this decolorized yeast cell wall fraction of the rerum natura that improves, also provides with the bag object being treated of this coating agent processing etc.
Contain the yeast cell wall fraction (Yeast Cell Wall:YCW) of from the yeast that enzyme is handled, removing the cell residue of composition in the soluble cell, perhaps contain further this cell residue is handled with acidic aqueous solution, the yeast cell wall fraction of acid treatment yeast cell wall fraction (Acid-treated Yeast Cell Wall:AYC) etc. of removing the cell residue that is dissolvable in water the acidic aqueous solution composition is (following as not specially provided for, with above-mentioned yeast cell wall fraction: YCW and acid treatment yeast cell wall fraction: the two is generically and collectively referred to as yeast cell wall fraction AYC), its film-forming properties excellence, and have excellent resistance to air loss etc. by the film that these components form, they are the materials with excellent rerum natura.But because painted and distinctive smell etc. is arranged from zymic brown-xanchromatic, in the time of in being applied to medicine or food etc., these are painted, smell etc. may become obstruction.
The inventor has carried out deep research for solving above-mentioned problem, found that: by to from the yeast that enzyme is handled, removing the cell residue that composition obtains in the soluble cell, perhaps further this cell residue is handled with acidic aqueous solution, remove the such method that yeast cell wall fraction is decoloured and handles of cell residue that the acidic aqueous solution composition obtains that is dissolvable in water, can can't harm the excellent rerum naturas such as resistance to air loss of the film of film-forming properties that yeast cell wall fraction has and formation, acquisition has been removed from the color of yeast cell wall fraction and smell, liquid YI (yellowness index) low (13 or following), have film-forming properties, further preferably have the decolorized yeast cell wall fraction of film slaking; And handle by this, can obtain when using this decolorized yeast cell wall fraction, can prevent the rotten decolorized yeast cell wall fraction that waits of coated thing, thereby finish the present invention as coating agent.
Decolorized yeast cell wall fraction of the present invention can be used as excellent coating agent, for example in field of pharmaceutical preparations, in preparation, contain volatility or sublimate, and as " generation whisker " when occurring, component of the present invention also can be used as a kind of additive that prevents to volatilize or distil and the character that plays a role.Whisker described here is meant the volatilization sublimate volatilization in the solid preparation, separates out the phenomenon of needle-like crystal on the solid preparation top layer, because this phenomenon takes place, can propose the flowability reduction of solid preparation or be mistaken as problems such as mouldy.
Summary of the invention
The present invention includes: decolorized yeast cell wall fraction (claim 1) is characterized in that: decolorized yeast cell wall fraction with the liquid YI (yellowness index) of the method for reflection that is undertaken by Japanese electric look (strain) SE-2000 (light source C, visual angle 2 degree) mensuration be 13 or below; Decolorized yeast cell wall fraction (claim 2) according to claim 1, it is characterized in that: using oven dry coater (baker applicator) that the slurries of 5% (weight ratio) decolorized yeast cell wall fraction are gone up curtain coating at oriented polypropylene films セ ネ シ POP (ダ イ セ Le chemical industry (strain), the thick 0.02mm of film), drying is 45 minutes in 60 ℃ baking oven, when making cast film (the thick about 0.015mm of film), it is 250ml/m at the oxygen transmission rate of 60%RH humidity that decolorized yeast cell wall fraction has this continuous film of character that can form continuous film 2DMPa or its are following; Decolorized yeast cell wall fraction (claim 3) described in the claim 1 or 2, it is characterized in that: at the bulge of the slurries of 5% (weight ratio) decolorized yeast cell wall fraction being used the 60mm diameter, following dry 2 hours at 60 ℃, when making cast film (the thick about 0.1mm of film), the disintegration time of this film in pure water is in 60 minutes; The decolorized yeast cell wall fraction (claim 4) of claim 1-3 in each, it is characterized in that: this decolorized yeast cell wall fraction is to removing the cell residue that composition obtains in the soluble cell from the yeast that enzyme is handled, and perhaps further cell residue that the composition that is dissolvable in water acidic aqueous solution obtains is handled, removed to this cell residue with acidic aqueous solution and decolours and handle and preparation.
The present invention also comprises: preparation method's (claim 5) of the decolorized yeast cell wall fraction of claim 1-4 in each, it is characterized in that:, perhaps further residue that the composition that is dissolvable in water acidic aqueous solution obtains is handled, removed to this cell residue with the discoloring agent processing of decolouring with acidic aqueous solution from the yeast that enzyme is handled, removing the cell residue that composition obtains in the soluble cell; Preparation method's (claim 6) of the decolorized yeast cell wall fraction of claim 5 is characterized in that: the decolouring processing of being undertaken by discoloring agent is to handle by the decolouring that hydrogen peroxide and ozone carry out.
The present invention also comprises: coating agent (claim 7) is characterized in that: described coating agent is a main component with the decolorized yeast cell wall fraction of claim 1-4 in each; Bag object being treated, described bag object being treated are to use with the decolorized yeast cell wall fraction of claim 7 and implement processed the obtaining of bag as the coating agent of main component; The bag object being treated of claim 8 is characterized in that: the bag object being treated is particulate, particle or tablet; Claim 8 or 9 bag object being treated is characterized in that: the bag object being treated is pharmaceutical preparation or food.
The accompanying drawing summary
Fig. 1 is in the expression embodiments of the invention, carries out the photo of film forming test-results with decolorized yeast cell wall fraction.A represents the moulding shape test-results (film forming) of comparative example goods 4, and B represents the film forming test-results (film forming) of embodiment goods 1.
Fig. 2 is expression present embodiment goods 1,3 and the different scanning electronic microscope of cell walls form retentivity of comparative example product 1,3: the photo of SEM.
The preferred plan that carries out an invention
The present invention includes decolorized yeast cell wall fraction, described decolorized yeast cell wall fraction is through decoloration and deodorization, the YI of liquid (yellowness index) low (13 or following), has film-forming properties, further preferably in the film slaking, film forming resistance to air loss and other rerum natura aspect, has excellent character, preparation by the following method: will contain the yeast cell wall fraction of from the yeast that enzyme is handled, removing the cell residue that composition obtains in the soluble cell, perhaps contain further this cell residue is handled with acidic aqueous solution, remove the yeast cell wall fraction of the cell residue that the composition that is dissolvable in water acidic aqueous solution obtains, decolour with discoloring agent and handle and prepare.Decolorized yeast cell wall fraction of the present invention has excellent especially character when using as coating agent.
[character of decolorized yeast cell wall fraction]
Decolorized yeast cell wall fraction of the present invention has following character.
(yellow chromaticity YI: yellowness index)
The bleaching level of decolorized yeast cell wall fraction of the present invention is determined with the YI value.Among the present invention, the YI value defines with " method for reflection that is undertaken by the electric look of Japan (strain) SE-2000 (light source C, visual angle 2 degree) is measured the YI (yellowness index) of liquid ".
That is, yeast cell wall fraction presents from zymic tawny-brown, and therefore as JIS K7103 defined, decolouring I represents with positive quantity for by the colourless or white degree that departs to yellow.YI is low more, then whiteness high more (yellow chromaticity is low more).For example in the solid ingredient of decolorized yeast cell wall fraction was 5% liquid (5g), YI was shown as the material of negative value, shows its decolouring degree height, and yellow chromaticity is low, therefore YI is defined as 0.Among the present invention,, be that 5% liquid tone is measured, represent with the mean value of measuring three times to solid ingredient with the reflection measurement of the beam splitting type color difference meter SE-2000 of Japanese electric look industry (strain), by light source C, visual angle 2 degree.The liquid YI of decolorized yeast cell wall fraction of the present invention be 13 or below.Below preferred 6 or 6, more preferably 1 or below.Liquid YI is yellow than 13 high decolorized yeast cell wall fractions, when being applied to preparation, produces aberration with medicine and other excipient, thereby not preferred.
When comparing, also can make tablet state (weight that package amount is converted into tablet is 10% tablet) and filminess (the about 0.1mm of thickness), compare by tablet YI, film YI respectively with the yellow chromaticity of existing coating agent.
Therefore, even also can estimate, define to the bleaching level of tablet and film itself by these tablets YI, film YI.
(cell walls form retentivity)
By using scanning electronic microscope (SEM) that decolorized yeast cell wall fraction is observed, the prototype that whether roughly kept yeast cell in 10-100 the yeast cell wall fraction (7 one-tenth or more than) is judged.By this method, the component that has kept prototype is defined as has cell walls form retentivity.
Use particles distribution instrument (for example: the laser particle size distribution instrument LA-920 of HORIBA system), measure size-grade distribution according to ordinary method.Relative reflectance adopts χ 2Value is 0.3 or following value, for preventing particle aggregation, measures under ultrasonic irradiation, by whether measuring size-grade distribution mould footpath to small direction displacement, judges the destruction situation of cell walls shape.
Preferably in various processed goods (film) shown below, has desirable character.The measuring method of various rerum naturas, be defined as follows described.
(film-forming properties)
(oxygen transmission rate that ダ イ セ Le chemical industry (strain), the thick 0.02mm of film, products catalogue provide is 304ml/m at oriented polypropylene films セ ネ シ POP with the slurries of the yeast cell wall fraction of 5% (weight ratio) to use oven dry coater (baker applicator) (ヨ シ ミ Star smart machine (strain)) 2DMPa) upper reaches is delayed, 60 ℃ oven dryings 45 minutes, and preparation film (the thick about 0.015mm of film).
Use the OX-TRAN100 of MOCON (modern Controls company), at 20 ℃ of temperature, humidity 60%RH, test area 5cm 2, oxygen concn 100% condition under carry out the oxygen transmission rate test of above-mentioned cast film.Here, oxygen transmission rate represents that film thickness determined under the situation of (the about 0.015mm of thickness, the about 0.035mm of film integral thickness) oxygen permeability under flat thin film area, unit time, the unit pressure.The oxygen transmission rate of the film that the curtain coating decolorized yeast cell wall fraction obtains on the oriented polypropylene films is less than 250ml/m 2During dMPa (60%RH), can form continuous thin film, be defined as and have film-forming properties.
As long as it is goods of the present invention satisfy aforesaid liquid YI and the important document relevant with film-forming properties at least, further preferred satisfied with each character headed by the slaking of film.
(film decomposability)
Preferred decolorized yeast cell wall fraction of the present invention also preferably has excellent film slaking.The film slaking of decolorized yeast cell wall fraction of the present invention is determined by the following method: " the slurries of 5% (weight ratio) decolorized yeast cell wall fraction with the bulge of 60mm diameter, 60 ℃ dry 2 hours down; when making cast film (the thick about 0.1mm of film), the disintegration time of this film in pure water ".
Promptly, the meaning that " has film slaking (water dispersible) " be meant " the slurries of 5% (weight ratio) decolorized yeast cell wall fraction with the bulge of 60mm diameter, 60 ℃ dry 2 hours down; (film is thick: about 0.1mm), be 4cm to the area of this film for the cast film of preparation 2Decolorized yeast cell wall fraction adopt the used device of the slaking test method in the 14 revision Pharmacopeia of Japan, put down in writing, use under the situation of 37 ℃ of pure water, film was scattered in the water in 60 minutes, not residual on the 2.0mm sieve aperture in the Glass tubing film was arranged ".Decolorized yeast cell wall fraction of the present invention disintegration in 60 minutes has shown good film slaking (water dispersible).Decolorized yeast cell wall fraction of the present invention has the good film slaking, therefore, during used as coating agent, can carry out the stripping of medicament effectively in preparations such as medicament.
(film forming)
Film forming of the present invention be meant slurries with the decolorized yeast cell wall fraction of 7-10g5 ± 1% in the bulge of 70-100mm diameter, 120 ℃ dry 30 minutes down, make cast film (film is thick: 100 μ m or its are following), (the be full of cracks number on the thin film planar is few for 3 of described cast film formation or 3 following continuous film sheets, the successive area is bigger as a result, because of be full of cracks continuous film face disconnected from each other is 3 or following); On the contrary, the non-formability of film is meant that under the same conditions film becomes 4 or above enclosed planar (the be full of cracks number on the thin film planar is many, and the successive area is smaller as a result, because of be full of cracks continuous film face disconnected from each other is more than 4 or 4).
Decolorized yeast cell component of the present invention has excellent film forming.Therefore, when using, continuous thin film can be made definite shape, suppress the stripping of effective constituent effectively and cover smell as the coating agent of preparation.
(film mechanical characteristics)
Add be converted into dry thing weight be 10% glycerine as softening agent, (film is thick: 50-100 μ m) for the casting film of preparation decolorized yeast cell wall fraction.Use above-mentioned film to carry out tension test, measure tensile strength (MPa) and elongation at break (%), further measure intensity (N), the amount of being pressed into (mm) of puncturing.The mensuration of tensile strength is as follows: prepare test film according to JIS Z1702, according to JIS K7161, K7162, accurate universal material testing instrument 2005 types that adopt (strain) イ Application テ ス コ company to make, draw speed with 500mm/ minute is tested, measure tensile strength, elongation, with this as tensile strength, elongation.Puncturing intensity tests with the film shape of thickness 50-100 μ m, accurate universal material testing instrument 2005 types that use (strain) イ Application テ ス コ company to make, trial speed with 200mm/ minute, by end shape is that 1/4 inch the mallet of smashing is tested, (the unit: N) and smash the amount of the being pressed into (unit: mm) as puncturing intensity (unit: N) of mallet of the load in the time of will puncturing film respectively.Tension test is n=5, punctures test and measures intensity, the amount of being pressed into of puncturing respectively with n=3, adopts mean value.
For example: when in the past yeast cell wall fraction and decolorized yeast cell wall fraction, adding 10% softening agent respectively, each mechanical characteristics of the latter is corresponding with the former to be compared, and can expect that 1-20 times of this load (N) raising, the amount of being pressed into (mm) improve 1-20 times, puncture 1-20 times of intensity (N) raising.In addition, can also expect that 1-20 times of tensile strength (MPa) raising, elongation improve 1-20 doubly.
(resistance to air loss)
Decolorized yeast cell wall fraction of the present invention has excellent resistance to air loss.The resistance to air loss of decolorized yeast cell wall fraction of the present invention is determined with " slurry of the decolorized yeast cell wall fraction of 5% (weight ratio) being gone up curtain coating at oriented polypropylene films セ ネ シ POP (ダ イ セ Le chemical industry (strain), the thick 0.02mm of film) using oven dry coater (baker applicator); 60 ℃ oven dryings 45 minutes; during preparation cast film (the thick about 0.015mm of film), the oxygen transmission rate under 60%RH humidity ".
Promptly, among the present invention, about resistance to air loss, be that (oxygen transmission rate that ダ イ セ Le chemical industry (strain), the thick 0.02mm of film, products catalogue provide is 304ml/m at oriented polypropylene films セ ネ シ POP at the slurry that uses oven dry coater (baker applicator) with 5% (weight ratio) decolorized yeast cell wall fraction 2DMPa) go up curtain coating, 60 ℃ oven dryings 45 minutes, during preparation cast film (the thick about 0.015mm of film), the oxygen transmission rate that is formed under the 60%RH humidity was shown as 250ml/m 2DMPa or its following continuous film.Here, if when not forming continuous film, then preparation etc. is wrapped by the time because shortcoming ductility, the bag at tablet mint-mark position or edge by deficiency, is produced be full of cracks sometimes, can not form the effect of content being protected as coating agent.
(tint permanence of film)
The tint permanence that preferred decolouring yeast parietal cell component of the present invention is not seen film.With the slurry of 5% (weight ratio) decolorized yeast cell wall fraction 60 ℃ of dryings 2 hours, (film is thick: about 0.10mm) to make film, with the YI of this film during as initial YI, with the YI of above-mentioned film after keeping 1 month under 40 ℃, 75R.H.% as current YI.Deduct initial YI by current YI, the YI of increase be 5 or more than, then film is colored as dark brown, with it as having tint permanence.YI surpasses at 5 o'clock, because of the painted preparation that makes to the yeast cells wall of bag quilts such as tablet painted, thereby not preferred.
[removing composition in the soluble cell and the preparation of the cell residue (yeast cell wall fraction) that obtains] by yeast
The present invention includes decolorized yeast cell wall fraction, described decolorized yeast cell wall fraction is a yeast cell wall fraction of removing the cell residue that composition obtains in the soluble cell to containing from the yeast that enzyme is handled, perhaps contains yeast cell wall fraction that the cell residue that the composition that is dissolvable in water acidic aqueous solution obtains was handled, removed to this cell residue further with acidic aqueous solution and decolours and handle and preparation.The present invention particularly is made up of following decolorized yeast cell wall fraction: to by using ethyl acetate, toluene, hexane, acetone, ether, sherwood oil, various alcohol (methyl alcohol, ethanol, propyl alcohol or Virahol etc.) etc. organic solvent or their mixture or the pH water and their mixture (for example pH is water and the alcoholic acid mixture of 2-12) that are 2-12 composition in the soluble cell is carried out carrying out washing treatment, from the yeast that enzyme is handled, remove the yeast cell wall fraction of the cell residue composition that composition obtains in the soluble cell, or by this cell residue is handled with acidic aqueous solution, remove the processing of decolouring of yeast cell wall fraction that cell residue that the composition that is dissolvable in water acidic aqueous solution obtains forms, do not damage decolouring and handle the excellent properties that preceding yeast cell wall fraction is had, can also aspect its rerum natura, add excellent character.In the above-mentioned organic solvent, preferred hexane, acetone, various alcohol (methyl alcohol, ethanol, propyl alcohol etc.), the further preferred ethanol that uses.The cell residue of removing composition gained in the soluble cell from yeast that uses among the present invention is prepared as follows.
(raw material yeast)
Yeast as coating agent raw material of the present invention, get final product so long as on taxonomy, belong to zymic, can use yeast arbitrarily, cereuisiae fermentum is for example arranged, wine yeast, bread yeast, Candida utilis etc., more particularly, can exemplify and belong to cereuisiae fermentum, yeast saccharomyces cerevisiae of the Saccharomycodes of bread yeast (Saccharomyces cerevisiae) or pasteurellaceae sugar yeast (Saccharomyces pastorianus), other also has Lu Shi yeast (Saccharomycesrouxii), saccharomyces carlsbergensis (Saccharomyces carlsbergensis), fission yeast (Saccharomyces pombe), produce methanol yeast-candidal Candida utilis (Candida utilis) in addition, candida tropicalis (Candida tropicalis), Candida lipolytica (Candida lipolytica), (Candida flaveri), Candida boidiniis (Candidaboidinii) etc. also have small rhodotorula (Rhodotrura minuta) etc.
(proterties of used yeast)
These yeast can be used alone or in combination.Yeast preferably uses fresh yeast, even when using the yeast of form beyond the fresh yeast such as dry yeast, for example can suspend in water etc., similarly handles with fresh yeast.And employed zymic shape, size are not particularly limited, and preferable shape approaches the spheric yeast as far as possible, and its big or small preferable range is 1-20 μ m.
(composition removes in the soluble cell)
There are compositions such as the cellular content be dissolvable in water water or polar solvent, for example protein, amino acid, sugar, nucleic acid, organic acid in the yeast, these cellular contents are soluble in water, and preferred the use removed the yeast cell wall fraction behind the composition in these soluble cells.If directly use under the state that composition exists in soluble cell, then film-forming properties reduces (film becomes fragile), is unfavorable.
In order from yeast, to remove composition in these soluble cells, obtain yeast cell wall fraction, need handle these cellular content dissolvings by enzyme, be rejected to the extracellular.Handle as enzyme, get final product so long as prepare the method for using when composition is as yeast extract in the yeast cell, can use enzyme facture arbitrarily, with the treatment process of additive such as alcohol and enzyme combination, the wherein said method of using when composition is as yeast extract in the yeast cell for preparing has: the so-called autolysis method that uses the enzyme in the yeast cell; Add the enzyme additive process of enzymes such as proteolytic enzyme, nuclease, beta-glucanase, esterase, lipase, Phosphoric acid esterase by the outside; And they are united method of use etc.This shows, can effectively utilize the yeast extract in the known yeast extract preparation to extract residue as yeast cell wall fraction of the present invention.
Handle in order to carry out enzyme fast, before enzyme is handled or in the enzyme processing, can carry out high-pressure homogenization and handle (preferably under 10-150MPa, being less than 6 times processing) or the ultrasonication (ultrasonic oscillator of use 20KHz, peak swing 50 μ m, output 2KW, output with 50-100%, shone 0.01-100 minute, preferably with the irradiation of the output more than 70% or 70% 0.01-45 minute), in order to improve decolorizing efficiency, preferably be used these two kinds of methods and handle.About the pre-treatment number of times, as long as the characteristic (YI: yellow chromaticity or yield etc.) of component is not had detrimentally affect, then be not particularly limited, preferably less than 10 times, further preferably be less than 6 times, especially preferably less than 2 times.Carry out 10 times or during above processing, then can observe film and shrink, the film-forming properties variation, thereby not preferred.
Yeast after the enzyme processing finishes is by being that water and their mixture (for example water of pH2-12 and alcoholic acid mixture) of 2-12 cleans (carrying out washing treatment) with the organic solvent of ethyl acetate, toluene, hexane, acetone, ether, sherwood oil, various alcohol (methyl alcohol, ethanol, propyl alcohol or Virahol etc.) etc. or their mixture or pH, for example remove the processing of composition in the soluble cell with implementing centrifugation etc. behind the enzyme treatment solution thin up, just can be used as this cell residue, obtain yeast cell wall fraction.After enzyme reaction, the homogenate by adopting above-mentioned record simultaneously, ultrasonication etc. disperse to handle, and help to remove intracellular unnecessary composition (coloring components lipid odour component protein etc.).
As mentioned above; need not to implement especially chemical treatment; the gained yeast cell wall fraction by physics and chemical aspect have patience epithelium form; contain dextran, mannosans, chitin layer in the wherein said epithelium, therefore can not damage the defencive function of internal bag material, and can fill the more material of volume; can be used as excellent coating agent uses; as required, also can cooperate the conciliation processing of zymic carrying out washing treatment, pH temperature, pressure etc., the preparation yeast cell wall fraction.
(the removing of composition of this aqueous solution handled and be dissolvable in water to acidic aqueous solution)
Then, preferably to carrying out the acidic aqueous solution processing by removing the above-mentioned yeast cell wall fraction that composition obtains in the soluble cell.Use 0.01-2N, preferably handle with the acid of organic acids such as for example hydrochloric acid of 0.1-0.5N, sulfuric acid, phosphoric acid, nitric acid etc. or acetate, citric acid, then this suspension is separated into cleer and peaceful yeast cell residue by centrifugal grade, prepares above-mentioned yeast cell wall fraction by collecting this yeast cell residue.In addition, during acid treatment, preferably be heated to about 60 ℃-80 ℃.Usually acid concentration or temperature of reaction are too high, film-forming properties variation then, thereby not preferred.
[decolouring of yeast cell wall fraction is handled]
(decolouring is handled)
To above-mentioned yeast cell wall fraction decolour (or bleaching) handle, the color of the distinctive tawny that yeast cell wall fraction is had before handling-brown system comes off, and becomes white.Handle as decolouring (or bleaching), can use hypochlorous acid is the oxidation system decolouring processing of SYNTHETIC OPTICAL WHITNER, hydrogen peroxide, ozone, dioxide peroxide, percarbonic acid, peracetic acid etc., and well-known decolouring (or bleaching) agent such as the reduction system decolouring processing of sulfurous acid reduction etc. are carried out.Can carry out separately by the processing that such decolouring (or bleaching) agent is carried out, also can suitably the several different methods combination be carried out.In this several different methods, consider preferred ozonize or hydrogen peroxide treatment from aspects such as the residual danger of agents useful for same, the complexity of removing residuals, smell are residual.These methods can be used alone or in combination.Number of times or order that these decolourings are handled are not particularly limited, handle as above-mentioned decolouring, when adopt respectively ozone and hydrogen peroxide the two when handling, at first handle with ozone, handle with hydrogen peroxide then, the YI of the product of gained or product processed goods like this: yellow chromaticity is good, film-forming properties when this decolorized yeast cell wall fraction is used as coating agent, also have aspect the film slaking desirable especially, so preferably carry out ozonize earlier, carry out hydrogen peroxide treatment then.In addition, two kinds of processing can be carried out under the alkali condition, can also be between two kinds of decolourings be handled, carry out all or part of alkaline purification separately, for example according to (1) ozonize, alkaline purification, hydrogen peroxide treatment, the hydrogen peroxide treatment under (2) ozonize, alkaline purification, the alkali condition, ozonize, alkaline purification, hydrogen peroxide treatment under (3) alkali condition, (4) hydrogen peroxide treatment under the ozonize under the alkali condition, alkaline purification, the alkali condition, order handle.When carrying out hydrogen peroxide treatment earlier, can be according to (5) hydrogen peroxide treatment, alkaline purification, ozonize, (6) ozonize under hydrogen peroxide treatment, alkaline purification, the alkali condition, (7) hydrogen peroxide treatment, alkaline purification, the ozonize under the alkali condition, the order of the ozonize under the hydrogen peroxide treatment under (8) alkali condition, alkaline purification, the alkali condition is handled.
Ozonize, for example when the 1000-100000ppm concentration of ozone mixed gas that produces with ozonizer is handled the slurry of the yeast cell wall fraction of 0.1-10% concentration, preferably with 1000-100000ppm, carry out contact reacts with the micro bubble form.More particularly, preferably with the amount of being blown into of 0.01-10g ozone/(g decolouring object hour), handle with 1-24 hour reaction times.The ozone concn maximum of this ozone reaction condition stipulates that with the ability of used ozone generating-device ozone purity improves, and then reaction efficiency more improves, therefore, do not stipulate maximum concentration originally, if but concentration is 0.1% or below it, then the YI height is unfavorable.Color reversion phenomenon russet can take place to become again in the decolorized yeast cell wall fraction that is obtained by ozonize, therefore preferably carry out alkaline purification (being adjusted to pH7-13) by the slurry of alkaline solutions such as sodium hydroxide after with decoloring reaction, and carry out centrifugation (4200rpm, 10 minutes), washing.In order to decompose residue ozone, preferred one side is carried out the affirmation of residue ozone with superoxide detection lug (for example Merckoquant Peroxide-Test etc.) etc., simultaneously regulates the addition of reductive agent.
It is 0.1-10% that hydrogen peroxide treatment preferably should be starched concentration adjustment, in temperature is 20-120 ℃, (pH is 7.0-13.0) reaction is 0.1-30 hour under the alkali condition, further preferably concentration of hydrogen peroxide is adjusted to 0.5-5%, in temperature is 40-80 ℃, and pH is reaction 1-20 hour under the condition of 8.5-11.5.Concentration be 0.1% or its when following, the YI height, not preferred.In order to remove residual hydrogen peroxide, preferably carry out suitable catalase (for example Na ガ セ ケ system テ Star Network ス (strain) makes レ オ ネ Star ト F プ ラ ス) and handle (treatment condition: pH3.0-8.5, temperature 10-50 ℃), and reducing pH (pH2 or following) as required, the inactivation that carries out this enzyme by thermal treatment is handled or the reduction of sulfurous acid etc. is handled again.The preferred one side of the detection of residual hydrogen dioxide waits the affirmation process by superoxide detection lug (for example Merckoquant Peroxide-Test etc.), simultaneously adds reductive agent, catalase at any time.
For the lipid of removing yeast cell wall fraction and the lipid peroxide that generates in decoloring reaction, preferred decolouring is handled the back and is washed by centrifugation.Further preferably wash by organic solvent (ethyl acetate, toluene, hexane, acetone, ether, sherwood oil, methyl alcohol, ethanol, propyl alcohol, Virahol etc.).By the washing of this organic solvent, also can reduce the reactive of yeast cell wall fraction itself and with the reactivity of coated medicine, thereby preferred.
With organic solvent (ethyl acetate, toluene, hexane, acetone, ether, sherwood oil, methyl alcohol, ethanol, propyl alcohol, Virahol etc.) water of the pulpous state yeast cell wall fraction of replacement water-dispersion, make with organic solvent or water-organic solvent blended solution, can make the slurry cohesion of yeast cell wall fraction thus, improve the solid ingredient concentration of this component, the vapour pressure of slurry is reduced, make the water constituent evaporation easily, like this, need not to be applied to directly necessary high temperature when carrying out drying (100 ℃ or more than) by the water-dispersion slurry, at short notice can be dry, can reduce being subjected to thermal process.
[utilization of decolorized yeast cell wall fraction]
(the use form of decolorized yeast cell wall fraction)
Decolorized yeast cell wall fraction of the present invention is generally the slurry form, also can use the exsiccant form.For example,, the water dispersion of decolorized yeast cell wall fraction is made powder, can obtain the powder or the dry thing of decolorized yeast cell wall fraction by drying meanss such as known spray-drying process or freeze-dryings.
(is the medicinal of main component or food additive with the decolorized yeast cell wall fraction)
Decolorized yeast cell wall fraction color of the present invention is pure white, and odorless shows firm binding property when dry, but therefore its disintegration in water can be used as medicinal or food additive widespread use.As application examples can enumerate wetting Agent for Printing Inks, granulation auxiliary agent, suspension agent, the raising flowability of coating agent, capsule capsule material, sorbent material, stablizer, ointment etc. additive, tackiness agent, by with the combination drying of crystalline cellulose saccharoid have simultaneously formability and slaking novel excipient, be used with other coating agent simultaneously.
Below describe in detail.
(decolorized yeast cell wall fraction is as the rerum natura of coating agent)
The coating agent that with decolorized yeast cell wall fraction of the present invention is main component is compared with traditional edibility coating agent, though have viscosity but work in-process is not clamminess, bag is not adhered between back particle and the particle, but also has as the excellent rerum natura that can control enteric solubility coating agent and the bitter taste sequestering agent of stripping time opening.In addition, the transmitance of gases such as the oxygen of film-coat, Water Vapour Permeability are extremely low, are excellent especially in existing edible film, preferably prevent that as whisker agent or odor masking agent from using.When air penetrability was high, problems such as rotten took place in the medicament of interior bag, thereby not preferred.
Do not postpone even disintegration can not take place for increase package amount, decolorized yeast cell wall fraction of the present invention, thus preferred.In the past bag by in, if wrap by the slaking variation thereby is unfavorable.
When decolorized yeast cell wall fraction of the present invention was used as coating agent, the concentration of preferred solid ingredient was 0.1-30%.Further preferred 1-10%.The concentration of solid ingredient be 30% or more than, coating buffer viscosity height then, spraying does not form very little droplet and causes taking place problem such as aggegation, thereby not preferred.
(wrapping the interior bag material of quilt by decolorized yeast cell wall fraction)
So long as the material that exists with solid under the normal temperature gets final product, can be any material by the interior bag material of coating agent bag quilt of the present invention, for example food, food material, enzyme, microorganism, medicine, seed, agricultural chemicals, fertilizer, spices, pigment etc.Above-mentioned food, the example of food material can specifically exemplify: starch food, tablet form food, western-style cake class (sugar, the maltose class, chocolate, chewing gum etc.), Japanese cake class (rice cake etc.), baking cake class (cake, biscuit, spiced salt biscuit), soft capsule preparation, fried pot foods (potato chips class such as potato, bag pot foods class), various dip soy sauce beans pickled egg yellow bean sauce sauce classes are made solid-state food of powder or food material, with various beverage (nectars, the nectar beverage, refreshment drink, sports beverages, tea, coffee, cocoa, the soup class, alcohol drink class etc.) make solid-state food of powder or food material, various extraction powder (fowl livestock products such as beef pork chicken, fishery products such as shrimp shellfish fish sea-tangle, the vegetables fruit tree kind, plant, yeast etc.), with lipid perfumery (vanilla, Citrus, pine fish etc.) make solid-state food of powder or food material, powder seasonings herbal medicine class (capsicum, pepper, Chinese pepper, shaddock, sweet basil etc.), powder-form drink food (soluble coffee, instant black tea, instant milk, instant soups Miso Soup etc.), various Dairy products (cheese etc.), various nutrition dietary supplement starting material classes (vitamins such as vitamin A B CDE of family, useful mushrooms such as bifidus bacillus milk-acid bacteria Butylic acid bacteria, chlorella, mineral substance such as Ca or Mg class, propolis etc.), seasonings, the sliced food class, accessories on the food (flavor) categories (fried broken bloomer loaf etc.), with beans processed food (bean curd, bean dregs etc.) make solid-state food or food material, with fresh product cooking processing (curry, the stew class) food is made solid-state food or the food material frozen product (vegetables that cut, the meat bag is by fried category), various processed foods.
When the bag material is own and the similar shape of saccharoid in interior bag material is particulate, particle or tablet even-granular thing and seed etc., can effectively utilize coating agent of the present invention.By bag material in described being wrapped quilt, can obtain bag object being treated of the present invention with coating agent of the present invention.On the other hand,, use coating agent film forming of the present invention, then can obtain the extremely low film-coat of the present invention of oxygen permeability coefficient or moisture permeable coefficient if the bag material does not wrap quilt.
(is softening agent that adds in the coating agent of main component and the additive that improves film-forming properties with the decolorized yeast cell wall fraction)
Even directly use decolorized yeast cell wall fraction of the present invention also to have excellent effect, but, preferably add softening agent.When being used for field of food, it is the lipid at center etc. that these softening agent can exemplify with glycerine, Sorbitol Powder, amino acids, organic acid, monoglyceride, Diglyceride, triglyceride, MCT (medium chain triacylglycerol).When being used for field of medicaments, can exemplify the softening agent of permissions such as triactin, triethyl citrate, acetylated monoglycerides as drug additive.In addition, except that softening agent or replace softening agent, can add following additive.
The example of additive has: thickening polyose (gum arabic; amylopectin; carrageenin etc.); polysaccharide degradation production (mannosans; curdlan; xylan; the resolvent of Mierocrystalline cellulose etc.); oligosaccharides (trehalose; sucrose; Palatinose; raffinose; oligosaccharides etc.); sugar alcohol (mannitol; Sorbitol Powder; maltose alcohol; hydroxyl isomaltulose; tetramethylolmethane; arabitol; Xylitol; sorbitol; melampyrum; ribitol etc.); foodstuff fibre class (pine fibre (insoluble dextrin) etc.); Stevia rebaudiana; cyclodextrin; jelling agent (agar; gelatin; zierane glue; curdlan etc.); arginine hydrochloride; ferrous sulfate; phosphoric acid salt (sodium phosphate; potassiumphosphate); starch hydrolysate; Octyl adipate; pure aluminium silicate; triethyl citrate; glycerol fatty acid ester; lipid (sesame oil; whiteruss; Semen Maydis oil; soybean oil; castor seeds oil; peanut oil; Oleum Gossypii semen soybean oil blend etc.); dimethyl polysiloxane two silicon mixtures; sucrose fatty ester; dipropylene glycol; propylene carbonate; Triglycerides,C8-10; triactin; plant sterol; adjacent benzene and formic acid dimethyl ester; diethyl phthalate; dioctyl phthalate (DOP); dibutyl phthalate; butyl phthaloyl butyl glycol ester; propylene glycol; polyoxyethylene (105) polyoxypropylene (5) glycol; poly-Sorbic Acid 80; polyvinyl alcohol; polyvinylpyrrolidone; polypropylene glycol 2000; polyoxyethylene glycol; isopropyl myristate; glyceryl monostearate; linolic acid isopropyl ester etc.
Above-mentioned listed softening agent and additive can both are one of any one or more, perhaps both each one or more, perhaps one or more combinations among both suitably join in the decolorized yeast cell wall fraction of the present invention and use.
(adding the resistance oxygen modifying agent in the decolorized yeast cell wall fraction coating agent to)
Compare with independent decolorized yeast cell wall fraction, add additive (resistance oxygen modifying agent), then hinder oxygen and be improved, thus preferred.The resistance oxygen modifying agent that is added for example has: monose (sucrose for example, glucose, seminose etc.) or oligosaccharides (maltose for example, trehalose, fructose, arabinose, the aspergillus niger oligose, lactose, D-glyconic acid-1,5-lactone etc.) short chain carbohydrate, the amino acids that water absorbability is low (for example arginine hydrochloride etc.), form the inorganic salts (ferrous sulfate for example of polyhydrate, SODIUM PHOSPHATE, MONOBASIC etc.), the glycitols that water absorbability is low (mannitol for example, hydroxyl isomaltulose, maltose alcohol etc.), vitamins (vitamins C etc.), existing coating agent (PVA (polyvinyl alcohol), Eudragit L30-D55, hydroxypropylcellulose (HPMC TC-5) etc.), thickening polyose (gum arabic etc.), gelifying agent (gelatin etc.).Be not particularly limited for described resistance oxygen modifying agent, when still in food or pharmaceutical preparation, using, preferably contain the material of edibility.In addition, also can add the particulate (preferred nano level dispersion thing) etc. of titanium oxide, zinc oxide, aluminum oxide, talcum powder, mica, montmorillonite, wilkinite etc. as inorganics.
These resistance oxygen modifying agents can use a kind of, also can be used two or more suitable properties-correcting agent simultaneously, further preferably use above-mentioned softening agent and the multiple additives such as additive that are used to improve film-forming properties (additive beyond resistance oxygen modifying agent+softening agent or the resistance oxygen modifying agent+resistance oxygen modifying agent or the additive beyond resistance oxygen modifying agent+softening agent+resistance oxygen modifying agent) simultaneously.
(using volatilization or distillation to prevent the manufacturing of the solid preparation of agent)
Use when preventing that as the volatilization of main component or distillation agent from making solid preparation with decolorized yeast cell wall fraction of the present invention, so long as the material of volatility or sublimability is prevented that by volatilization of the present invention or distillation agent from covering basically, forming obstruct with the outside gets final product, it is not particularly limited, can uses the preparation method of mixing, the covering common suitable solid preparations that in this field, uses such as (bag quilts).For example; when using volatilization of the present invention or distillation to prevent that agent from making solid preparation such as pharmaceutical preparation; cooperate volatilization of the present invention or distillation to prevent agent with volatility or sublimability effective constituent, various excipient, additive, lubricant etc.; it is granulated with wet method or dry granulation method or the granulations such as comminution granulation directly powder suppressed etc., can be shaped to the such solid preparation of particle or tablet.Coat volatilization of the present invention or distillation and prevent agent, when making it form preparation, can cooperate in effective constituent on the particle and tablet that excipient or other Synergist S-421 95 granulate, the method for coating bag that adopts usually by this area is prevented agent by whisker, makes preparation.
(rerum natura when being prevented that by volatilization of the present invention or distillation agent from forming preparation) by bag
Volatilization or distillation that use is made up of decolorized yeast cell wall fraction of the present invention prevent agent, and the method that is made into preparation by bag is effective especially for the generation that prevents whisker etc.
Use volatilization of the present invention or distillation to prevent that the bag of agent from being compared with edibility bag in the past, though toughness but work in-process are not clamminess, bag is not adhered between the particle by the back, even and the enteric solubility bag of interaction energy control stripping time opening by or the bitter taste sequestering agent use and also have excellent rerum natura.By the clothing layer (film) that coating agent of the present invention is made, the transmitance of gases such as oxygen, Water Vapour Permeability are extremely low, are excellent especially in existing edible film, in extensive fields such as food, medicine, feed, agricultural chemicals.
Whisker of the present invention prevents that agent from being coating agent itself, does not have special drug effect, and is therefore different with the situation of mixing effective components such as antacid, can required drug effect do not exerted an influence, without detriment to versatility.And, known bag in the past by in, if wrap by the slaking variation, but the present invention's product do not influence slaking, do not see because of causing the sex change of preparation aspect with reacting to each other of interior bag material yet.
(bag material in the solid preparation that prevents to volatilize or distil)
Among the present invention, as prevent to volatilize or distil for the volatility in the solid preparation of purpose or sublimate it is contemplated that contain in the solid preparation for pharmaceutical preparation, food, food material, foodstuff additive, agricultural chemicals or spices, have various materials of volatilization or sublimability at normal temperatures, can be listed below especially as the object material in the generation that prevents whisker etc.
Promptly; as the material that distillation takes place at normal temperatures; caffeine (1 hydrate) is for example arranged; Caffein anhydrous; caffeine citrate; caffeine classes such as caffeine sodio-benzoate; Whitfield's ointment; acetylsalicylic acid; acetoamidophenol; Ethoxybenzamide; chlorphenylamine maleate; the hibenzic acid tipedine; Noscapine (cough medicine), pentoxyverine citrate, potassium sulfoguaiacol; Chinese ephedra as extracts from crude drugs; cassia bark; earthworm; genseng; Radix Glycyrrhizae; the various extracts of cow-bezoar etc.; Chinese patent medicine extracts the GEGEN TANG in the preparation; Herba Sidae Rhombifoliae soup; XIAOQINGLONG TANG; various extracts such as bupleuri and Ramuli Cinnamomi Decoction, the 1-menthol; the d-menthol; peppermint alcohols such as dl-menthol, for example ethyl benzoate; phenol benzoate; propyl benzoate; phenylformic acid benzyl ester; methyl benzoate; benzoic acids such as Sodium Benzoate etc.
(preventing the bag quilt of agent) to solid preparation by the volatilization of using decolorized yeast cell wall fraction or distillation
Particularly with prevent whisker occur as purpose, use bag that the present invention's volatilization or distillation prevent agent by, can operate by the following method: use separately or be used above-mentioned in the bag material; suitable size particles such as preparation fine-grained particles or tablet are with aforementioned volatilization of the present invention or prevent that agent is suspended in the suspension bag of water or solvent gained by above-mentioned particle.
(operation of using decolorized yeast cell wall fraction to wrap quilt)
The bag that is undertaken by coating agent of the present invention can be wrapped quilt to the suspension in the mixed solution that is suspended in water or water and solvent.Specifically, for example by using De リ ァ コ--coaters such as ((strain) パ ウ レ Star Network systems), with the suspension of coating agent of the present invention spray to should carry out on the material of bag and wrap quilt, so long as known method for coating or known bag then can be used any means or device by device.
(using the decolorized yeast cell wall fraction bag) by the drying temperature of operation and package amount
Bag by the drying temperature in the operation, promptly with the suspension of coating agent of the present invention internally wrap material wrap by after drying temperature be not particularly limited, usually preferably under 60-90 ℃ temperature, carry out drying, can also set drying temperature according to the temperature stability of interior bag material.If at 90 ℃ or carry out drying more than it, then the film-forming properties variation is not preferred.Replenish dryly after being moved to end by bag, can improve the stability of film, can obtain to stablize the result of extraction of controlling packet object being treated.Package amount is preferably suitably set according to bag amount of substance, needed purposes etc. in used.
(can with the material of decolorized yeast cell wall fraction combination)
When decolorized yeast cell wall fraction of the present invention is applied to above-mentioned medicine that exemplifies or food uses, preferably use with following combinations of substances.Specifically have: stablizer (trehalose for example; mannitol; fumaric acid etc.); excipient (crystalline cellulose for example; W-Gum; yam starch; Starch rice; lactose; Icing Sugar etc.); tackiness agent (HPMC for example; polyvinyl alcohol; polyvinylpyrrolidone; amylopectin etc.); film-coat agent (hydroxypropylcellulose for example; HPMC; the phthalic acid HPMC; acetyl succsinic acid HPMC; carboxymethylethylcellulose; ethyl cellulose; the ethyl cellulose aqueous dispersions; amino alkyl methacrylate multipolymer E; Sipacril 2739OF L; Sipacril 2739OF S; Sipacril 2739OF LD; EudragitRS PO etc.); tensio-active agent (sucrose fatty ester for example; the polyoxyethylene polyoxypropylene glycol; polysorbate; Sodium Lauryl Sulphate BP/USP; sugar etc.); disintegrating agent (low-substituted hydroxypropyl cellulose for example; carboxymethylcellulose calcium; cross-linked carboxymethyl cellulose sodium; part alphalysed starch etc.); inorganics (talcum powder for example; Magnesium Stearate; light silicon anhydride; synthetic aluminium silicate; titanium oxide etc.); softening agent (Sudan Gum-arabic for example; amylopectin; carrageenin etc.); polysaccharide degradation production (mannosans for example; curdlan; xylan; the resolvent of Mierocrystalline cellulose etc.); oligosaccharides (sucrose for example; Palatinose; raffinose; oligosaccharides etc.); sugar alcohol (Sorbitol Powder for example; maltose alcohol; hydroxyl isomaltulose; tetramethylolmethane; arabitol; Xylitol; sorbitol; melampyrum; ribitol etc.); foodstuff fibre class (pine fibre (insoluble dextrin) etc.); Stevia rebaudiana; cyclodextrin; jelling agent (agar for example; gelatin; zierane glue; curdlan etc.); amino acids (for example arginine hydrochloride etc.); form the inorganic salts (for example ferrous sulfate etc.) of polyhydrate; phosphoric acid salt (sodium phosphate for example; hydrochloric acid potassium; SODIUM PHOSPHATE, MONOBASIC etc.); starch hydrolysate; Octyl adipate; pure aluminium silicate; triethyl citrate; glycerol fatty acid ester; lipid (sesame oil for example; whiteruss; Semen Maydis oil; soybean oil; castor seeds oil; peanut oil; Oleum Gossypii semen soybean oil blend etc.); dimethyl polysiloxane two silicon mixtures; dipropylene glycol; propylene carbonate; Triglycerides,C8-10; triactin; plant sterol; dimethyl phthalate; diethyl phthalate; dioctyl phthalate (DOP); dibutyl phthalate; butyl phthaloyl butyl glycol ester; propylene glycol; polyoxyethylene (105) polyoxypropylene (5) glycol; polysorbate 80; polypropylene glycol 2000; polyoxyethylene glycol; isopropyl myristate; glyceryl monostearate; linolic acid isopropyl ester etc.).More than be typical example, can with the 14th correct all combinations of substances of putting down in writing in the pharmaceuticals additive specification of Pharmacopeia of Japan and distribution in 1996 and use.
In the purposes of the present invention's product as health care of food food, when in such use, using, can use with the combinations of substances put down in writing on the foodstuff additive table.
Be described more specifically situation of the present invention by the following examples, but the present invention is not subjected to the restriction of these embodiment.
[measuring method of rerum natura shown in the embodiment]
The measuring method of each rerum natura in present embodiment, the comparative example beyond the above-mentioned rerum natura is as follows.Decolorized yeast cell wall fraction weight shown in the embodiment all is the weight (dry weight) under the virtual condition.
Each character when using the present invention's product to make tablet is measured as follows.
(slaking of tablet)
Disintegration of tablet test method(s) according to putting down in writing in the 14 revision Pharmacopeia of Japan uses slaking test instrument NT-40HS (Fushan Mountain industry (strain)) to implement.Experimental liquid uses 37 ℃ of pure water, represents by the average disintegration time of 6 tablets of tablets.
(tablet hardness)
Use shuroin gel hardness instrument 6D type (Off ロ イ Application ト industry (strain)), obtain the average hardness of 10 tablets of tablets.
(smell sensory test)
Convert 20 tablets of tablets that carried out 10% bag quilt vial sealing of packing into the weight of tablet.At room temperature place a night, whether drug smell is arranged when evaluating Kaifeng by three reviewers then.Three reviewers all answer does not have drug smell, and then smell is covered well; Answer has drug smell, and then expression fails to cover smell.
(centrifugal WATER-WASHING METHOD)
Below, use separating centrifuge (Hitachi: himac CR7), under 4200rpm10 minute condition, reaction solution is carried out centrifugation, obtain deposited components.In this deposited components, add the water about 3 times of weight, make its redispersion, carry out centrifugation then, obtain deposited components, above operation is defined as centrifugal water cleans 1 time.To adding the water stage when carrying out centrifugal operation and repeat N time, be expressed as centrifugal water and clean N time, below this statement of unification employing from above-mentioned.The separating centrifuge that this statement is not only handled for above-mentioned intermittent type when using continuous discharge formula separating centrifuge also is.
Embodiment 1
Specially permit the method for No. 3349677 record according to Japan, (NOVO company makes with proteolytic enzyme, use neutral enzymatic, the alkalescence enzyme, at 45-60 ℃, pH7.5 reacted 15 hours down) the interior composition of dissolved cell, remove composition in the soluble cell by centrifugation (4200rpm 10 minutes), to gained yeast cell wall fraction (liquid YI:45), yeast cell wall fraction concentration with 5% concentration, under the hydrochloric acid acidic conditions of 0.5N, handled 10 minutes at 80 ℃, remove the solubility in acid cellular content by centrifugation, wash then, make the acid treatment yeast cell wall fraction.To this acid-treated yeast cell wall fraction (liquid YI:49), yeast cell wall fraction concentration with 5% concentration, with concentration be that 1.5% hydrogen peroxide, pH are 10,60 ℃ of temperature, reaction is 3 hours under the certain condition of pH, to the processing of decolouring of the acid treatment yeast cell wall fraction of 5% concentration, after reaction finishes, fully wash by centrifugation (4200rpm, 10 minutes).To wash thing reaction 15 hours under above-mentioned reaction conditions once more, wash by centrifugation (4200rpm, 10 minutes).
The liquid YI of this washing thing (embodiment product 1) is 12, has film-forming properties (11ml/m 2DMPa), has film slaking (28 minutes).
Embodiment 2
The centrifugation precipitation of embodiment 1 is scattered in 99.5% ethanol of 3 times of amounts, stirs after 30 minutes, remove the ethanol of supernatant part, fully wash by centrifugation again by centrifugation.The liquid YI of this washing thing (embodiment product 2) is 12, has film-forming properties (13ml/m 2DMPa), has film slaking (29 minutes).
Embodiment 3
In 5% concentration acid treatment yeast cell wall fraction described in the 600g embodiment 1 slurry, be blown into the ozone gas of 15 hours 10000ppm with 3g/ hour ratio, decolour.Only wash when placing then after the ozonize, the decolouring thing that bleaches because of processing is colored as sorrel once more, produce the color reversion phenomenon, therefore being adjusted to pH by sodium hydroxide is 11, make the color reversion substance dissolves, carry out centrifugation (4200rpm, 10 minutes) washing, again to the washing thing carry out 2 hours with the above-mentioned processing that is blown into ozone equally.With the residue ozone of this ozonize thing S-WAT reduction decomposition, being adjusted to pH with sodium hydroxide then is 11, carries out centrifugation (4200rpm, 10 minutes), fully washes once more, the material that produces color reversion is cleaned removed.The liquid YI of this washing thing (embodiment product 3) is 0, has film-forming properties (10ml/m 2DMPa), there is not film slaking (above 60 minutes).
Embodiment 4
Under the condition of pH1.2, making the 200g effective chlorine density is that 12% the clorox and the slurry of 5% concentration acid treatment yeast cell wall fraction described in the 600g embodiment 1 react.React after 2 hours, carry out centrifugation (4200rpm, 10 minutes) washing, the liquid YI of this washing thing (embodiment product 4) is 11, has film-forming properties (11ml/m 2DMPa), has film slaking (30 minutes).
Embodiment 5
Yeast cell wall fraction is adjusted into 10% slurry, by high-pressure homogenizer with 50MPa pressure treatment 12 times, yeast cell wall fraction is carried out fragmentation, broken thing was handled 10 minutes at 80 ℃ with the hydrochloric acid of 0.1N, wash by centrifugation (4200rpm, 10 minutes).The acid-treated yeast cell wall fraction that this washing obtains is made 5% slurry, add 1% chlorine bleach liquor (chlorine effective concentration is 12%), under the condition of (pH1-2) under the hydrochloric acid acidity, decolour.This decolouring thing (embodiment product 5) is for highly white.The liquid YI of these embodiment product 5 is 1, has film-forming properties (13ml/m 2DMPa), there is not film slaking (above 60 minutes).
Embodiment 6
Under the certain condition of 60 ℃ of hydrogen peroxide, pH10, temperature, the pH of 3% concentration to embodiment 1 in the slurry of 5% concentration yeast cell wall fraction react, after reaction finishes, wash fully by centrifugation (4200rpm, 10 minutes).With 4N hydrochloric acid this slurry is transferred to and to be pH7-7.5, add 0.05-0.1% catalase (Na ガ セ ケ system テ Star Network ス: レ オ ネ Star ト F プ ラ ス), stirred 30 minutes, remaining hydrogen peroxide decomposition is removed, implement 2 centrifugal washings then, obtain deposited components.With 4N hydrochloric acid this deposited components is transferred to and to be pH4, make the slurry of 1.5L3%, under the condition of 10 ℃ of fluid temperatures of 0.1MPa pressure, be blown into ozone, carry out 1 hour ozonize.Ozone gas, be by supplying with oxygen by oxygen cylinder, produce oxygen ozone mixed gas with commercially available discharge type ozonizer, use this gas, under the condition of 0.11MPa pressure, 2L/ minute flow, 4.5% (w/w) ozone concn, be blown into, make ozone gas form micro-bubble, carry out gas liquid reaction.By S-WAT the residue ozone of ozonize thing is carried out reduction decomposition, be adjusted to pH11 with sodium hydroxide then, carry out centrifugation (4200rpm, 10 minutes), fully wash again, obtain deposited components.This deposited components is scattered in 99.5% ethanol of equivalent, stirred 30 minutes, remove the ethanol of supernatant part then by centrifugation, fully wash by centrifugation again, obtain this embodiment product 6.The liquid YI of these embodiment product 6 is 0, has film-forming properties (16ml/m 2DMPa), there is not film slaking (above 60 minutes).
Embodiment 7
Under the certain condition of 3.0% concentration hydrogen peroxide, pH10,60 ℃ of temperature, pH.The acid-treated yeast cell wall fraction of 5% concentration to preparation similarly to Example 1 carries out 3 hours decolouring processing reaction, after reaction finishes, washes fully by centrifugation (4200rpm, 10 minutes).To wash thing reaction 15 hours under above-mentioned reaction conditions once more, wash by centrifugation (4200rpm, 10 minutes), with gained as embodiment product 7.
The liquid YI of these embodiment product is 1, has film-forming properties (10ml/m 2DMPa), has film slaking (28 minutes).
Embodiment 8
With 4N hydrochloric acid the slurry of 5% acid-treated yeast cell wall fraction described in the embodiment 1 is adjusted to pH4,, carries out 1 hour ozonize in the above-mentioned slurry of 1L, being blown into ozone under the condition of 10 ℃ of liquid temperature of 0.1MPa pressure.Ozone gas, be by supplying with oxygen by oxygen cylinder, produce oxygen ozone mixed gas with commercially available discharge type ozonizer, use this mixed gas, under the condition of the pressure of 0.11MPa, 2L/ minute flow, 4.5% (w/w) ozone concn, be blown into, make ozone gas form micro-bubble, carry out gas liquid reaction.After ozonize finishes, it is adjusted to pH11, with 2 centrifugal washings of condition enforcement of 4200rpm10 minute, the gained deposited components is adjusted to pH3.8 then with 25% sodium hydroxide solution, with this as embodiment product 8.The liquid YI of these embodiment product 8 is 9, has film-forming properties (10ml/m 2DMPa), do not have a film slaking (above 60 minutes).
Embodiment 9
The component of (alkaline purification after the ozonize) is handled in preparation similarly to Example 8, the dry substrate concentration with 2.5%, 2% concentration hydrogen peroxide, be adjusted to the slurry of pH10, reacted 5 hours at 60 ℃ with 25% sodium hydroxide.After reaction finishes,,, make dry thing weight concentration and be about 3% slurry then with the centrifugal sediment dilute with water with 4200rpm centrifugation 10 minutes.With 4N hydrochloric acid this slurry is adjusted to pH7-7.5, add 0.05-0.1% catalase (Na ガ セ ケ system テ Star Network ス: レ オ ネ Star ト F プ ラ ス), stirred 30 minutes, remaining hydrogen peroxide decomposition is removed, implement 2 centrifugal washings then, obtain deposited components.With this deposited components of obtaining with etc. the ethanol of weight be added in the deposited components, stir, disperse, after making the state of slurry, stir carry out after 30 minutes centrifugal, this washing with alcohol processing is carried out 3 times, implement 2 centrifugal washings then, the gained deposited components be adjusted to pH3.8, with this component as embodiment product 9.The liquid YI of these embodiment product 9 is 0, has film-forming properties (10ml/m 2DMPa), tool film slaking (7 minutes).
Embodiment 10
The component of preparation similarly to Example 8 being handled (alkaline purification after the ozonize) is with 2.5% dry substrate concentration, 2% concentration hydrogen peroxide, is adjusted to the slurry of pH10 with 25% sodium hydroxide, reacts 2 hours at 60 ℃.After reaction finishes,,, make dry thing weight concentration and be about 3% slurry then with the centrifugation dilute with water with 4200rpm centrifugation 10 minutes.With 4N hydrochloric acid this slurry is adjusted to pH7-7.5, add 0.05-0.1% catalase (Na ガ セ ケ system テ Star Network ス: レ オ ネ Star ト F プ ラ ス), stirred 30 minutes, remaining hydrogen peroxide decomposition is removed, implement 2 centrifugal washings then, obtain deposited components.With this deposited components of obtaining with etc. the ethanol of weight be added in the deposited components, stir, disperse, make the state of slurry after, stir and carry out 2 centrifugal washings after 30 minutes, the gained deposited components is adjusted to pH3.8, with this as embodiment product 10.The liquid YI of these embodiment product 10 is 0, has film-forming properties (10ml/m 2DMPa), has film slaking (14 minutes).
Embodiment 11
Specially permit the method for the 3349677th record according to Japan, the beer fresh yeast slurry centrifugation (4200rpm10 minute) to the bright bacterium state that obtains as brew-house's byproduct makes the gained yeast suspension, makes solid ingredient reach 10% weight.This yeast is handled with the homogenizer of 100MPa, then by composition in proteolytic enzyme (NOVO makes, and uses neutral enzymatic, alkaline enzyme, and reaction is 15 hours under 45-60 ℃, the pH7.5) dissolved cell.By this slurry being carried out centrifugation (4200rpm, 10 minutes), remove composition in the soluble cell, washing gained cell residue is made yeast cell wall fraction (YCW).With this YCW with the hydrogen peroxide of 5% dry weight concentration, 1% concentration, be adjusted to the slurry of pH10 with the sodium hydroxide of 25% concentration, with the gained slurry 60 ℃ of reactions 2.5 hours.After reaction finishes, adding the hydrogen peroxide that is equivalent to 1% amount once more, is 10 with pH regulator by 25% sodium hydroxide again, then 60 ℃ of reactions 2.5 hours.After reaction finishes,,, make dry thing weight concentration and be about 3% slurry then with the centrifugation dilute with water with 4200rpm centrifugation 10 minutes.With 4N hydrochloric acid this slurry is adjusted to pH7-7.5, adds 0.5% catalase (Na ガ セ ケ system テ Star Network ス: レ オ ネ Star ト F プ ラ ス), stirred 30 minutes, remaining hydrogen peroxide decomposition is removed, implement 2 centrifugal washings then.The gained deposited components is adjusted to pH3.8, with this component as embodiment product 11.The liquid YI of these embodiment product 11 is 13, has film-forming properties (10ml/m 2DMPa), has film slaking (14 minutes).
Embodiment 12
Is 4 5% YCW slurry with 4N hydrochloric acid with pH regulator to 1L, is blown into ozone under the condition of 10 ℃ of liquid temperature of 0.1MPa pressure, carries out 1 hour ozonize.Ozone gas is by supplying with oxygen by oxygen cylinder, produce oxygen ozone mixed gas with commercially available discharge type ozonizer, use this gas, under the condition of the pressure of 0.11MPa, 2L/ minute flow, 4.5% (w/w) ozone concn, the YCW slurry is blown into, make ozone gas form micro-bubble, carry out gas liquid reaction.After ozonize finishes, the YCW slurry is adjusted to pH11, with 2 centrifugal washings of condition enforcement of 4200rpm10 minute, the gained deposited components is adjusted to pH3.8 then with 25% sodium hydroxide solution, with this component as embodiment product 12.The liquid YI of these embodiment product 12 is 6, has film-forming properties (10ml/m 2DMPa), do not have film slaking (above 60 minutes).
Embodiment 13
2.5% slurry to 1L embodiment product 12 under the condition of 10 ℃ of liquid temperature of 0.1MPa pressure is blown into ozone, carries out 0.5 hour ozonize.Ozone gas, be by supplying with oxygen by oxygen cylinder, produce oxygen ozone mixed gas with commercially available discharge type ozonizer, use this gas, under the condition of 0.11MPa pressure, 2L/ minute flow, 7.2% (w/w) ozone concn, the YCW slurry is blown into, make ozone gas form micro-bubble, carry out gas liquid reaction.After ozonize finishes, be adjusted to pH11, with 2 centrifugal washings of condition enforcement of 4200rpm10 minute, the gained deposited components be adjusted to pH3.8 then with 25% sodium hydroxide solution, with this as embodiment product 13.The liquid YI of these embodiment product 13 is 0, has film-forming properties (10ml/m 2DMPa), do not have film slaking (above 60 minutes).
Embodiment 14
Embodiment 13 finally is adjusted to deposited components before the pH3.8 and the ethanol of equivalent is added in the deposited components, dispersed with stirring is made the state of slurry, stirred then 30 minutes, centrifugal washing 2 times is adjusted to pH3.8 with the gained deposited components, with this component as embodiment product 14.The liquid YI of these embodiment product 14 is 0, has film-forming properties (10ml/m 2DMPa), do not have film slaking (above 60 minutes).
Embodiment 15
With embodiment product 12 with 2.5% dry substrate concentration, 1% concentration hydrogen peroxide, be adjusted to the slurry of pH10 with 25% concentration hydrogen sodium oxide, 60 ℃ of reactions 2 hours.After reaction finishes,,, make dry thing weight concentration and be about 3% slurry then with the centrifugal sediment dilute with water with 4200rpm centrifugation 10 minutes.With 4N hydrochloric acid this slurry is adjusted to pH7-7.5, add 0.05-0.1% catalase (Na ガ セ ケ system テ Star Network ス: レ オ ネ Star ト F プ ラ ス), stirred 30 minutes, remaining hydrogen peroxide decomposition is removed, implement 2 centrifugal washings then, obtain deposited components.The gained deposited components is adjusted to pH3.8, with this component as embodiment product 15.The liquid YI of these embodiment product 15 is 0, has film-forming properties (10ml/m 2DMPa), has film slaking (19 minutes).
Embodiment 16
With embodiment 15 finally be adjusted to deposited components before the pH3.8 and the ethanol of equivalent is added in the deposited components, dispersed with stirring is made the state of slurry, after stirring 30 minutes then, carry out centrifugal washing 2 times, the gained deposited components be adjusted to pH3.8, with this component as embodiment product 16.The liquid YI of these embodiment product 16 is 0, has film-forming properties (10ml/m 2DMPa), has film slaking (9 minutes).
Comparative example 1
10g exsiccant yeast extract residue is suspended in the NaOH solution of 500g 0.5N concentration.The hydrogen peroxide that mixes 100g 2% refluxes and boiled 120 minutes, washes by centrifugal then, with gained deposited components product 1 as a comparative example.The liquid YI of these comparative example product 1 is 7, does not have film-forming properties and (surpasses 250ml/m 2DMPa), and do not form continuous film, therefore can't measure the film slaking.
Comparative example 2
20g exsiccant yeast extract residue is suspended in the NaOH solution of 1000g 0.5N concentration, refluxes and boiled 120 minutes.Wash by centrifugation, the gained deposited components is suspended in 1000g 0.5N hydrochloric acid soln, reflux and boiled 120 minutes.Wash by centrifugation (3000rpm, 20 minutes) once more afterwards, with deposited components product 2 as a comparative example.The liquid YI of these comparative example product 2 is 30, does not have film-forming properties and (surpasses 250ml/m 2DMPa), and do not form continuous thin film, therefore can't measure the film slaking.
Comparative example 3
With 1000g 2% superoxol comparative example product 2 are refluxed and to boil, wash, with deposited components product 3 as a comparative example by centrifugation (3000rpm, 20 minutes).The liquid YI of these comparative example product 3 is 7, does not have film-forming properties and (surpasses 250ml/m 2DMPa), and do not form continuous thin film, therefore can't measure the film slaking.
Comparative example 4
20g exsiccant yeast extract residue is suspended in the NaOH solution of 1000g 0.5N concentration, refluxes and boiled 120 minutes.Wash by centrifugation, deposited components is suspended in the 1000g 0.5N hydrochloric acid soln, reflux and boiled 120 minutes.Wash by centrifugation (3000rpm, 20 minutes) once more afterwards, in this deposited components, be blown into the ozone of 1 hour 10000ppm, wash by centrifugation.Add 1000mL99.5% ethanol, remove ethanol, add entry, wash, with gained deposited components product 4 as a comparative example by centrifugation by centrifugation.The liquid YI of these comparative example product 4 is 1, does not have film-forming properties and (surpasses 250ml/m 2DMPa), and do not form continuous thin film, therefore can't measure the film slaking.
Comparative example 5
Make the cereuisiae fermentum self-dissolving, the extract part is removed in washing, and it is 5% (weight ratio) that the yeast cell wall fraction that obtains is made solid ingredient concentration, makes the aqueous dispersions of 1L, is adjusted to pH8.5 with sodium bicarbonate, stirs at normal temperatures 1 hour.This dispersion soln is carried out centrifugation with 4200rpm10 minute condition.Deposited components is suspended in 2.5% sodium hydroxide, is adjusted to pH12.5, remain on 65 ℃ by hot water bath then, add the hydrogen peroxide of 30% concentration, being adjusted to integral body is 1.5% concentration (concentration of hydrogen peroxide), reacts 15 hours.After the reaction, be adjusted to pH7.0 with the 12N concentrated hydrochloric acid, obtain deposited components by centrifugation (4200rpm10 minute) after, with its solid ingredient concentration adjustment to 5%, be adjusted to pH5, with this component product 5 as a comparative example by 4N hydrochloric acid.The liquid YI of these comparative example product 5 is 36, does not have film-forming properties and (surpasses 250ml/m 2DMPa), and do not form continuous thin film, therefore can't measure the film slaking.
Comparative example 6
Make the cereuisiae fermentum self-dissolving, the extract part is removed in extraction, carry out acid treatment according to the method for embodiment 1 record then, the acid-treated yeast cell wall fraction of gained is carried out the processing same with the decoloring method of comparative example 5, with the component of gained product 6 as a comparative example.The liquid YI of these comparative example product 6 is 31, does not have film-forming properties and (surpasses 250ml/m 2DMPa), and do not form continuous thin film, therefore can't measure the film slaking.
Comparative example 7
According to No. 3349677 disclosed preparation methods of communique of Japan special permission, the YCW slurry that the dry substrate concentration that makes YCW is 5%, concentration of hydrochloric acid is 0.3N keep 80 ℃ 10 minutes, centrifugal then washing 2 times.With the dilution of this deposited components is the slurry of 5% dry substrate concentration, is adjusted to pH7.5, and then centrifugal washing 2 times.The gained deposited components is adjusted to pH3.8, with this component product 7 as a comparative example.The liquid YI of these comparative example product 7 is 49, has film-forming properties (5ml/m 2DMPa), has film slaking (25 minutes).
Comparative example 8
The dry substrate concentration of preparation YCW is about 2%, naoh concentration is the slurry of 0.5N, refluxes and boils 120 minutes.Slurry after negate should finish, centrifugal washing 2 times is with obtained component product 8 as a comparative example.The liquid YI of these comparative example product 8 is 49, does not have film-forming properties and (surpasses 250ml/m 2DMPa), and do not form continuous thin film, therefore can't measure the film slaking.
Comparative example 9
The dry substrate concentration of preparation YCW is about 2.5%, naoh concentration is that 0.5N, concentration of hydrogen peroxide are 2% slurry, refluxes and boils 120 minutes.Slurry after negate should finish, centrifugal washing 2 times is with obtained component product 9 as a comparative example.
Comparative example 10
Dry substrate concentration in the 1000g comparative example product 8 is about 2.5% slurry and carries out ozonize at normal temperatures and pressures.Ozone to be blown into condition as follows: supply with oxygen by oxygen cylinder, with commercially available discharge type ozonizer generation oxygen ozone mixed gas.Use this gas, in the YCW slurry, be blown under the condition of 0.11MPa pressure, 1L/ minute flow, 10000ppm ozone concn, make ozone gas form micro-bubble, carry out gas liquid reaction.Slurry after negate should finish, centrifugal washing 2 times is with obtained component product 10 as a comparative example.The liquid YI of these comparative example product 10 is 25, does not have film-forming properties and (surpasses 250ml/m 2DMPa), and do not form continuous thin film, therefore can't measure the film slaking.
Comparative example 11
The ethanol of weight such as adding and comparative example product 10 disperses by stirring, makes the state of slurry, stirs centrifugal washing 2 times then 30 minutes.With gained deposited components product 11 as a comparative example.The liquid YI of these comparative example product 11 is 23, does not have film-forming properties and (surpasses 250ml/m 2DMPa), and do not form continuous thin film, therefore can't measure the film slaking.
Comparative example 12
Dilution comparative example product 8, preparation 1000g concentration of hydrochloric acid is the slurry of 0.5N, refluxes and boils 120 minutes.Slurry after negate should finish, centrifugal washing 2 times is made the 1000g slurry with the gained deposited components, carries out ozonize at normal temperatures and pressures.Ozone to be blown into condition as follows: supply with oxygen by oxygen cylinder, with commercially available discharge type ozonizer generation oxygen ozone mixed gas.Use this gas, in the YCW slurry, be blown under the condition of 0.11MPa pressure, 1L/ minute flow, 10000ppm ozone concn, make ozone gas form micro-bubble, carry out gas liquid reaction.Slurry after negate should finish, centrifugal washing 2 times.The ethanol of weight such as adding and gained deposited components disperses by stirring in deposited components, makes the state of slurry, stirs centrifugal washing 2 times then 30 minutes.With gained deposited components product 12 as a comparative example.The liquid YI of these comparative example product 12 is 26, does not have film-forming properties and (surpasses 250ml/m 2DMPa), and do not form continuous thin film, therefore can't measure the film slaking.
Embodiment 17
The solid ingredient and the softening agent of embodiment product 1 are scattered in the water, and the preparation coating buffer wherein makes 40% weight that reaches solid ingredient in the above-mentioned decolouring acid treatment yeast cell wall fraction as the ratio of the trehalose of softening agent.Embodiment product 1 account for 5.8% weight in the solid ingredient of each coating buffer.Then, with crystalline cellulose " ァ ゼ セ Le " PH-301 (Asahi Chemical Industry's (strain) manufacturing)/mannitol (east and change into industry (strain) make)/L-halfcystine (military field medicine (strain) manufacturings) according to 20/50/30 mass ratio mixing, as interior bag material, with L-HPC (Japanese Cao Da (strain) manufacturing) as slurry, use マ Le チ プ レ Star Network ス MP-01 (manufacturing of (strain) パ ウ レ Star Network company) to make particle, with the mixed of dried particle/Magnesium Stearate (peaceful industry (strain)) according to 100/0.5, use Rotarytabletpress (chrysanthemum water is made institute's (strain) and made) then, make diameter 8mm, quality 200mg, the tablet of tablet hardness 1N (plain sheet).Bag by the time, the coater FREUND MODEL-MINI that uses Off ロ イ Application ト industry to make, the plain sheet of the ready-made 400g that packs into, under the condition of container rotating speed 20rpm, 80 ℃ of gas temperatures, 35 ℃ of exhaust temperatures, gaseous tension 0.1MPa, one side was sprayed by solution above-mentioned bag with 2.5g/ minute, one side is wrapped quilt, and to make the epithelium amount be scaled tablet weight be 10%.Then, in one evening of drying treatment in 60 ℃ drying machine, obtain the peridium patch agent.With the peridium patch agent of embodiment product 1 as tablet (a).Do not see the adhesion between the tablet during bag is operated, the tablet surface top layer coats fully and equably.The YI of tablet is 25, and disintegration time is 460 seconds, and smell is covered well, and tablet hardness is 2.1N.
Embodiment 18
Use embodiment product 7, prepare coating buffer similarly to Example 17, making trehalose is 40% weight of the solid ingredient of embodiment product 7.Use this coating buffer (solid ingredient concentration is 7.3% weight) to carry out operation similarly to Example 17, obtain peridium patch agent (b).Bag is by good.The YI of tablet is 11, and disintegration time is 442 seconds, and smell is covered well, and tablet hardness is 2.1N.
Embodiment 19
Use embodiment product 5, prepare coating buffer similarly to Example 17, making trehalose is 40% weight of the solid ingredient of embodiment product 5.Use this coating buffer (solid ingredient concentration is 4.9% weight) to carry out operation similarly to Example 17, obtain peridium patch agent (c).Bag is by good.The YI of tablet is 18, and disintegration time is 1800 seconds or more than it, smell is covered well, and tablet hardness is 2.1N.
Embodiment 20
Use embodiment product 9, prepare coating buffer similarly to Example 17, making mannitol is 40% weight of the solid ingredient of embodiment product 9.Use this coating buffer (solid ingredient concentration is 7.0% weight) to carry out operation similarly to Example 17, obtain peridium patch agent (A).Bag is by good.The YI of tablet is 7, and disintegration time is 347 seconds, and smell is covered well, and tablet hardness is 3.3N.
Embodiment 21
Use embodiment product 16, prepare coating buffer similarly to Example 17, making mannitol is 40% weight of the solid ingredient of embodiment product 16.Use this coating buffer (solid ingredient concentration is 8.0% weight) to carry out operation similarly to Example 17, obtain peridium patch agent (B).Bag is by good.The YI of tablet is 7, and disintegration time is 348 seconds, and smell is covered well, and tablet hardness is 3.3N.
Comparative example 13
Use comparative example product 7, prepare coating buffer similarly to Example 17, making trehalose is 40% weight of acid-treated yeast cell wall fraction solid ingredient.Use this coating buffer (solid ingredient concentration is 11.1% weight), carry out and above-mentioned same operation, obtain peridium patch agent (d).Bag is by good.The YI of tablet is 50, and disintegration time is 434 seconds, and smell is covered well, and tablet hardness is 2.3N.
Comparative example 14
The coating buffer of 5% weight HPMC (TC-5, SHIN-ETSU HANTOTAI's chemistry (strain) make) is carried out similarly to Example 17 operation, make peridium patch agent (e).With above-mentioned same, bag is by good.The YI of tablet is 12, and disintegration time is 450 seconds, fails to cover smell, and tablet hardness is 2.1N.
Comparative example 15
Use comparative example product 7, prepare coating buffer similarly to Example 17, making mannitol is 40% weight of acid-treated yeast cell wall fraction solid ingredient.Use this coating buffer (solid ingredient concentration is 11.1% weight), carry out operation similarly to Example 17, obtain peridium patch agent (C).Bag is by good.The YI of tablet is 55, and disintegration time is 429 seconds, and smell is covered well, and tablet hardness is 2.1N.
(resistance to air loss of single comparative example film-coat)
Comparative example 16
In humidity is under the condition of 60%RH, and the oxygen transmission rate of comparative example product 7 is 5ml/m 2DMPa.
Comparative example 17
In humidity is under the condition of 60%RH, and the oxygen transmission rate of HPMC:TC-5 (SHIN-ETSU HANTOTAI's chemistry (strain) manufacturing) is 172ml/m 2DMPa or more than it.
Comparative example 18
In humidity is under the condition of 60%RH, and the oxygen transmission rate of Eudragit L30-D55 (sale of (strain) akebi mouth chamber of commerce) (mixing of Eudragit/PEG2000/TWIN 80=100/10/3.9 weight ratio) is 49ml/m 2DMPa.
Embodiment 22
(resistance oxygen modifying agent)
Solid ingredient at embodiment product 7 is in the solution of 5% weight, whole solution is stirred and makes its dispersion with stirrer, obtains uniform solution, makes the 10-80 weight % of resistance oxygen modifying agent for solid ingredient in the decolouring acid treatment yeast cell wall fraction.
With the coating machine this coating buffer is gone up curtain coating at oriented polypropylene films セ ネ シ POP (ダ イ セ Le chemical industry (strain)),, obtain the cast film of the about 0.015mm of film thickness (the thick 0.035mm of whole film) 60 ℃ oven dryings 45 minutes.Testing apparatus uses the OX-TRAN100 of MOCON (manufacturing of modern Controls company), at 20 ℃ of temperature, humidity 60% or 85%, test area 5cm 2, oxygen concn 100% condition under measure, the gained result as oxygen transmission rate (ml/m 2DMPa) calculate, as shown in Table 1 and Table 2.By table 1 and table 2 as can be known: in decolouring acid treatment yeast cell wall fraction of the present invention, add resistance oxygen modifying agent, even then under high humidity, also show good resistance oxygen.
(table 1)
Sample (under 60% humidity) Oxygen transmission rate [mL/m 2·d·MPa]
Embodiment product 7 10
Embodiment product 7: mannitol=10:2 3
Embodiment product 7: mannitol=10:4 3
Embodiment product 7: mannitol=10:6 5
Embodiment product 7: mannitol=10:8 4
Embodiment product 7: trehalose=10:4 2
Embodiment product 7:PVA=10:2 8
Embodiment product 7:PVA=10:4 2
Embodiment product 7: white sugar=10:4 3
(table 2)
Sample (under 85% humidity) Oxygen transmission rate [mL/m 2·d·MPa]
Embodiment product 7 42
Embodiment product 7: mannitol=10:1 40
Embodiment product 7: mannitol=10:2 16
Embodiment product 7: mannitol=10:4 11
Embodiment product 7: mannitol=10:6 8
Embodiment product 7: mannitol=10:8 8
Embodiment product 7: trehalose=10:2 24
Embodiment product 7: trehalose=10:4 27
Embodiment product 7: trehalose=10; 5 37
Embodiment product 7:PVA=10:2 34
Embodiment product 7:PVA=10:4 21
Embodiment product 7: white sugar=10:4 33
Embodiment product 7: gum arabic=10:4 32
Embodiment product 7: gelatin=10:4 32
Embodiment 23
(the yeast cells wall shapes of embodiment product and existing similar product (comparative example))
Embodiment product 1,3 and comparative example product 1,3 have been taken scanning electronic microscope (SEM) photo (Fig. 2).As can be known: the cell walls shape of embodiment product (1,3) keeps (maintenance form) (Fig. 2 A, B) in fact fully, but the cell walls shape of comparative example product (1,3) then disappears (Fig. 2 C, D).
Embodiment 24
(the yeast cells wall shape of the present invention's product and existing similar product (relatively product) (estimating)) by the size-grade distribution variation
Make the laser particle size distribution instrument LA-920 of manufacturing by the hole field, making relative refractive index is 200A000I, and to embodiment product 1 and 3, and comparative example product 1, comparative example product 3, comparative example product 4 carry out particle size distribution respectively.
Embodiment product 1 and 3 mould footpath are all near 5.5-5.7 μ m, and in the comparative example product 1,3,4, particle diameter is reduced near the 3.2-3.7 μ m.In the comparative example product 3,4, the following particle diameter ratio of 3.9 μ m or its is respectively 39%, 52%, 54%, is at high proportion, and is respectively 16.7%, 5.8% in embodiment product 1 and 3, be comparative example product half or half below low ratio.Hence one can see that: in the comparative example product, the cell walls shape is damaged, and then can keep its shape in the embodiment product.
Embodiment 25 (film-forming properties)
Film forming to embodiment product and comparative example product is measured.Data are the result to each sample determination 2 times.
In embodiment product 1-16, the comparative example product 7, YCW shows the good film formability, all be complete film or the film that be full of cracks is partly arranged, but comparative example product 1-6 or 8-12 all is scrappy diaphragm, do not see film forming, can't carry out the mensuration of following physics value as film.
Embodiment 26 (mechanical characteristics of film)
Carry out the mechanical mensuration of film for the good sample of film forming.
Being produced as follows of the film of estimating: the dry thing slurries of 10% glycerine are added in preparation, convert with dry thing, the dry substrate concentration in the slurries is about 2% will be scaled the slurries that dry thing is equivalent to 1.0g and pour in 100mm * 100mm polystyrene system square ware.With dry about one day of this ware, the sample of making cast film is used for following film physical property measurement test.
The result is the mean value of each value, is illustrated in the table 3.
As shown in the following Table 3, with YCW, 7 comparisons of comparative example product among the embodiment 11, along with the processing of decolouring, film strength improves.Particularly in embodiment product 10 and the embodiment product 16, can see film strength and significantly improve, tensile strength is increased to nearly 5 times of YCW film, and with respect to comparative example product 7 films, intensity also is enhanced about more than once.In addition, the breakthrough intensity of expression film film thickness direction intensity also be 4.5 times of YCW, is 3 times of comparative example 7, the effect of visual intensity raising.And tool also can seen effect aspect the raising of the amount of being pressed into of the flexible elongation of representing film or breakthrough.
(table 3)
Film forming and film mechanical characteristics
Figure C03824455D00381
→: can't estimate
Embodiment 27
(preparing yeast cell wall fraction (YCW-2)) by dry yeast
Specially permit the method for the 3349677th record according to Japan, the dry cereuisiae fermentum of the dead bacterium state that obtains as the byproduct of brew-house is suspended, making solid ingredient is 10% weight.This yeast is handled with the homogenizer of 100MPa, then by composition in proteolytic enzyme (NOVO makes, and uses neutral enzymatic, alkaline enzyme, and reaction is 15 hours under 45-60 ℃, the pH7.5) dissolved cell.By this slurry being carried out centrifugation (4200rpm, 10 minutes), remove composition in the soluble cell, washing gained cell residue is made yeast cell wall fraction.The pH of this moment is about 7.0.
Following Yeast Cell Wall simplification, abbreviate this yeast cell wall fraction as YCW-2 (liquid YI:75).
(ozonize of YCW-2)
1L through using 5% slurries of 4N hydrochloric acid with the YCW-2 of pH regulator to 4, is blown into ozone under the condition of 0.1MPa10 ℃ of liquid temperature, carries out 1 hour ozonize.Ozone gas is by supplying with oxygen by oxygen cylinder, produce oxygen ozone mixed gas with commercially available discharge type ozonizer, use this mixed gas, under the condition of 0.11MPa pressure, 2L/ minute flow, 4.5% (w/w) ozone concn, the YCW slurry is blown into, make ozone gas form micro-bubble, carry out gas liquid reaction.After ozonize finishes, with 25% sodium hydroxide solution YCW is starched and to be adjusted to pH11, centrifugal washing 2 times under 4200rpm10 minute condition then obtains deposited components.
(hydrogen peroxide treatment of YCW-2 after ozonize)
This deposited components is adjusted to the slurry of pH10 with 2.5% dry substrate concentration, 1% concentration of hydrogen peroxide, 25% sodium hydroxide, 60 ℃ of reactions 2 hours.After reaction finishes,,, make dry thing weight concentration and be about 3% slurry then with the centrifugal sediment dilute with water with 4200rpm centrifugation 10 minutes.With 4N hydrochloric acid this slurry is adjusted to pH7-7.5, add 0.05-0.1% catalase (Na ガ セ ケ system テ Star Network ス: レ オ ネ Star ト F プ ラ ス), stirred 30 minutes, remaining hydrogen peroxide decomposition is removed, implement 2 centrifugal washings then, obtain deposited components.This deposited components is adjusted to pH3.8, with this component as embodiment product 27.
The liquid YI of these embodiment product 27 is 0, has film-forming properties (10ml/m 2DMPa), has film slaking (in 30 minutes).
Embodiment 28
(Ethanol Treatment)
The deposited components that finally is adjusted to before the pH3.8 of embodiment 27 is mixed with the part by weight of ethanol according to 1:1, and dispersed with stirring is made the state of slurry, stirred then 30 minutes, centrifugal again washing 2 times is adjusted to pH3.8 with the gained deposited components, with this component as embodiment product 28.The liquid YI of these embodiment product 28 is 0, has film-forming properties (10ml/m 2DMPa), do not have film slaking (in 30 minutes).
Embodiment 29
(preparing AYC-2) by dry yeast
According to the preparation method of No. 3349677 communiques of Japan special permission, make the dry substrate concentration of YCW-2 and be 5%, the YCW slurry of 0.3N concentration of hydrochloric acid, keep 80 ℃ 10 minutes, centrifugal then washing 2 times.With the dilution of this deposited components is the slurry of 5% dry substrate concentration, is adjusted to pH7.5, and then centrifugal washing 2 times.The gained deposited components is adjusted to pH3.8.
Below this component is called AYC-2.Liquid YI is 82.
(ozonize of AYC-2)
(alkaline purification after the ozonize) handled in the preparation that above-mentioned AYC-2 carries out similarly to Example 27, and centrifugal washing is 2 times under 4200rpm10 minute condition, obtains deposited components.(hydrogen peroxide treatment of AYC-2 after ozonize)
This deposited components is adjusted to the slurry of pH10 with 2.5% dry substrate concentration, 1% concentration of hydrogen peroxide, 25% sodium hydroxide, 60 ℃ of reactions 2 hours.After reaction finishes,,, make dry weight concentration and be about 3% slurry then with the centrifugal sediment dilute with water with 4200rpm centrifugation 10 minutes.With 4N hydrochloric acid this slurry is adjusted to pH7-7.5, add 0.05-0.1% catalase (Na ガ セ ケ system テ Star Network ス: レ オ ネ Star ト F プ ラ ス), stirred 30 minutes, remaining hydrogen peroxide decomposition is removed, implement 2 centrifugal washings then, obtain deposited components.This deposited components is adjusted to pH3.8, with this component as embodiment product 29.The liquid YI of these embodiment product 29 is 0, has film-forming properties (10ml/m 2DMPa), has film slaking (in 30 minutes).
Embodiment 30 (Ethanol Treatment)
With embodiment 29 finally be adjusted to deposited components before the pH3.8 and ethanol mixed according to weight ratio 1:1, dispersed with stirring is made the state of slurry, stirred then 30 minutes, centrifugal washing 2 times is adjusted to pH3.8 with the gained deposited components, with this component as embodiment product 30.The liquid YI of these embodiment product 30 is 0, has film-forming properties (10ml/m 2DMPa), has film slaking (in 30 minutes).
31 one-tenth mensuration that are grouped into (being generally 3 kinds of compositions) of embodiment
Below represent various present embodiment product and be carried out to branch comparative example (table 4) relatively with this comparative example product.As shown in table 4, the present embodiment product are compared with this comparative example product, and protein, lipid content have the tendency that reduces slightly.
(table 4)
3 kinds of one-tenth are grouped into
The sample title Ash content d.m.% Lipid d.m.% Crude protein d.m.%
Embodiment product 1 1.1 7.5 9.3
Embodiment product 2 1.0 1.9 10.9
Embodiment product 3 1.3 6.3 1.3
Embodiment product 4 2.1 15.5 9.3
Embodiment product 6 0.14 1.5 3.2
Embodiment product 7 1.29 15.6 5.2
Embodiment product 8 1.31 3.24 9.06
Embodiment product 9 1.11 2.63 1.62
Embodiment product 10 0.62 1.16 2.64
Described in the YCW (embodiment 11) 17.56 4.11 20.27
Embodiment product 11 3.03 10.56 11.64
Embodiment product 12 3.41 2.82 9.60
Embodiment product 13 2.95 1.90 7.89
Embodiment product 15 3.34 2.57 2.16
Embodiment product 16 3.31 1.39 2.00
Comparative example product 3 0.43 2.0 2.8
Comparative example product 4 0.05 0.0 2.9
Comparative example product 5 1.0 11.9 11.6
Comparative example product 6 1.0 8.9 15.8
Comparative example product 7 1.13 5.22 16.22
Comparative example product 9 34.89 5.53 2.16
Comparative example product 10 10.84 12.34 5.12
Comparative example product 11 1.06 6.74 2.14
Comparative example product 12 1.27 3.54 2.02
Comparative example product 13 0.14 5.31 3.26
YCW-2 (described in the embodiment 27) 4.81 1.78 41.75
Embodiment product 28 3.49 0.91 5.11
Embodiment product 30 0.45 1.05 5.27
AYC-2 (described in the embodiment 29) 0.81 2.87 33.31
The mensuration that embodiment 32 sugar are formed
The sugar that contains in the yeast cells wall (from yeast saccharomyces cerevisiae) is most of to be the dextran mannosans, contains the chitin of trace near the trace that sprouts (budding scar).For the sugar of measuring yeast cells wall is formed, to various present embodiment product or this comparative example product, the dextran mannosans is hydrolyzed to the glucose seminose of structure monose, measure its content.
Because structure monose is reducing sugar, therefore by method behind the post,, use high performance liquid chromatography (hereinafter referred to as HPLC) according to the order of following table 5, table 6, with n=1 each sample is measured.
(table 5)
The preparation method of testing liquid
1 The preparation of sample Make 3-6g slurry dry solidification become yeast cell wall fraction and pulverizing with boiling water
2 The preparation of sample Add 4ml 72% sulfuric acid, add 112ml water then
2 Hydrolysis 121 ℃ 1 hour
3 Neutralization Be adjusted to pH7-7.5 with 25% NaOH.
4 Filter No.5 filter paper → membrane filter (aperture: 0.45 μ m)
(table 6)
Condition determination: HPLC condition
Instrument kind condition etc. Instrument kind manufacturer
HPLC LC-10Advp Shimadzu Seisakusho Ltd.
Detector Spectrophotofluorometer Shimadzu Seisakusho Ltd.
Post Tsk gel SUGAR AXI φ 4.6 mm * 150mm East ソ-(strain)
Column temperature 60℃
Mobile phase 0.5mol/L borate buffer (pH8.7)
The mobile phase flow 0.4ml/ minute
Fluorescence exciting wavelength 320nm
The fluorometric assay wavelength 430nm
Behind the post Reaction reagent: 1m/v% L-arginine solution reaction solution flow: 0.7ml/ minute temperature of reaction: 150 ℃
As shown in table 7, the result of sugared compositional analysis shows: along with the raising of whiteness, the ratio of dextran improves, and content of mannan reduces, but in having the sample of film forming, and still remaining have a mannosans.Do not have on the other hand among the comparative example product 8-12 of film forming, do not detect the seminose that is equivalent to mannosans.
(table 7)
Sugar is formed guide look
The sample name Glucose % Seminose % Glucose %+ seminose % Glucose/seminose
YCW (described in the embodiment 11) 41.3% 25.6% 66.9% 1.61
Comparative example product 7 54.1% 20.7% 74.8% 2.61
Embodiment product 11 68.8% 1.6% 70.4% 43.00
Embodiment product 12 58.1% 20.6% 78.7% 2.82
Embodiment product 13 83.6% 6.4% 90.0% 13.06
Embodiment product 15 68.4% 5.6% 74.0% 12.21
Embodiment product 16 73.7% 5.1% 78.8% 14.45
Embodiment product 9 89.4% 2.0% 91.4% 44.70
YCW-2 (described in the embodiment 27) 24.7% 18.7% 43.4% 1.32
Embodiment product 28 73.3% 1.5% 74.8% 48.87
AYC-2 (described in the embodiment 29) 21.5% 36.7% 58.2% 0.59
Embodiment product 30 85.1% 1.3% 86.4% 65.46
Comparative example product 8 81.8% 0.0% 81.8%
Comparative example product 9 67.1% 0.0% 67.1%
Comparative example product 10 69.3% 0.0% 69.3%
Comparative example product 11 86.7% 0.0% 86.7%
Comparative example product 12 91.7% 0.0% 91.7%
Industrial applicability
Decolorized yeast cell wall fraction of the present invention makes the color decolouring of yellowish-brown-brown that yeast cell wall fraction in the past has, present white (for example liquid YI be 13 or it is following), and during as uses such as coating agents, though toughness but with by the bag thing adhere to, can not adhere between the particle after coated, oxygen permeability coefficient is extremely low, can control dissolution time, namely use organic solvent (methyl alcohol etc.) to process, film forming does not change etc. yet, and the shortcoming that yeast cell wall fraction has before the decolouring is improved decolorized yeast cell wall fraction all.
The present invention by take by the decolorized yeast cell wall fraction with above-mentioned character of manufacturing of the present invention as main component, further add and use plasticizer, oxygen barrier modifying agent etc., the excellent coating agent that can be used as in food, food material, pharmaceutical preparation, enzyme, microorganism, seed, agricultural chemicals, fertilizer, spices or the pigment etc. uses. Coating agent of the present invention is excellent to the effect of the volatilization that prevents insourcing ingredient or distillation, for example in field of pharmaceutical preparations, go wrong as " generation whisker " contain volatility or sublimate preparation prevent volatilize or the additive that distils and material with availability.

Claims (5)

1.脱色酵母细胞壁组分,其是通过下述方法制备的:用脱色剂将经酶处理从酵母中除去可溶性细胞内成分得到的细胞残渣,或者进一步将该细胞残渣用酸性水溶液处理、除去可溶解于酸性水溶液的成分得到的细胞残渣进行脱色处理,并用水或有机溶剂洗涤,所述的脱色处理指用0.01-10g臭氧/g脱色对象·小时的吹入量将臭氧吹入脱色对象,以1-24小时的反应时间进行处理,然后用过氧化氢处理,其中将该浆浓度调节为0.1-10%,在温度为20-120℃,碱条件下实施反应0.1-30小时;1. Decolorized yeast cell wall fraction, which is prepared by the following method: the cell residue obtained by removing soluble intracellular components from yeast by enzyme treatment with a decolorizing agent, or further treating the cell residue with an acidic aqueous solution to remove The cell residue obtained by dissolving the components in the acidic aqueous solution is subjected to decolorization treatment, and washed with water or an organic solvent. The decolorization treatment refers to blowing ozone into the decolorization object with the blowing amount of 0.01-10g ozone/g decolorization object·hour, to The reaction time is 1-24 hours for treatment, and then treated with hydrogen peroxide, wherein the slurry concentration is adjusted to 0.1-10%, and the reaction is carried out at a temperature of 20-120 ° C and alkaline conditions for 0.1-30 hours; 所制备的脱色酵母细胞壁组分通过日本电色株式会社的SE-2000在光源C、视角2度的条件下以反射方法测定的、前述步骤所获得的液体的黄度指数YI为13或以下;The prepared decolorized yeast cell wall component is measured by the SE-2000 of Nippon Denshoku Co., Ltd. under the condition of light source C and viewing angle of 2 degrees by reflection method, and the yellowness index YI of the liquid obtained in the previous steps is 13 or below; 其具有细胞壁保持性和形成连续薄膜的特性;且在使用烘干涂料器将重量百分比为5%的所述脱色酵母细胞壁组分的浆在膜厚0.02mm的、Daicel Chemical Industries的取向聚丙烯薄膜Senesi POP上流延,在60℃的烘箱内干燥45分钟,制备膜厚0.015mm流延薄膜时,所述脱色酵母细胞壁组分具有形成在60%RH湿度下的透氧率为250ml/m2·d·MPa或以下的连续薄膜的性质;It has the characteristics of cell wall retention and continuous film formation; and the slurry of the decolorized yeast cell wall component with a film thickness of 0.02mm, Daicel Chemical Industries' oriented polypropylene film is used to dry the coater Casting on Senesi POP, drying in an oven at 60°C for 45 minutes, when preparing a casting film with a film thickness of 0.015mm, the decolorized yeast cell wall component has an oxygen permeability of 250ml/m 2 formed at a humidity of 60%RH Properties of continuous thin films at or below d·MPa; 在将重量百分比为5%的脱色酵母细胞壁组分的浆于60mm直径的圆形容器内,60℃下干燥2小时制备膜厚0.1mm流延薄膜时,该由经脱色的酵母细胞壁形成的连续薄膜在纯水中的崩解时间为60分钟以内。When the slurry of decolorized yeast cell wall components with a weight percentage of 5% was placed in a circular container with a diameter of 60mm and dried at 60°C for 2 hours to prepare a cast film with a film thickness of 0.1mm, the continuous membrane formed by the decolorized yeast cell wall The disintegration time of the film in pure water is within 60 minutes. 2.权利要求1所述的脱色酵母细胞壁组分的制备方法,其特征在于所述的组分是由下述方法制备的:用脱色剂将从经酶处理过的酵母中除去可溶性细胞内成分得到的细胞残渣,或者进一步将该细胞残渣用酸性水溶液处理、除去可溶解于酸性水溶液的成分得到的残渣进行脱色处理,并用水或有机溶剂洗涤,所述的脱色处理指用0.01-10g臭氧/g脱色对象·小时的吹入量将臭氧吹入脱色对象,以1-24小时的反应时间进行处理,然后用过氧化氢处理,其中将该浆浓度调节为0.1-10%,在温度为20-120℃,碱条件下实施反应0.1-30小时。2. the preparation method of the described decolorizing yeast cell wall component of claim 1 is characterized in that described component is prepared by following method: will remove soluble intracellular component from the yeast that is through enzyme treatment with decolorizing agent The cell residue obtained, or the residue obtained by further treating the cell residue with an acidic aqueous solution to remove components soluble in the acidic aqueous solution, is subjected to decolorization treatment, and washed with water or an organic solvent. The decolorization treatment refers to the use of 0.01-10g ozone/ g decolorization object · blowing amount per hour Blow ozone into the decolorization object, treat with reaction time of 1-24 hours, and then treat with hydrogen peroxide, wherein the slurry concentration is adjusted to 0.1-10%, at a temperature of 20 -120°C, carry out the reaction under alkaline conditions for 0.1-30 hours. 3.根据权利要求2所述的脱色酵母细胞壁组分的制备方法,其特征在于:从经酶处理过的酵母中除去的可溶性细胞内成分是从经下述的酶处理的酵母中去除的,所述的酶指:在制备通常的酵母提取物中常用于提取酵母提取物的、选自蛋白酶、核酸酶、β-葡聚糖酶、酯酶、脂肪酶、磷酸酶的一种或多种酶。3. the preparation method of decolouring yeast cell wall fraction according to claim 2 is characterized in that: the soluble intracellular component that removes from the yeast of enzyme treatment is removed from the yeast through following enzyme treatment, The enzyme refers to: one or more of proteases, nucleases, β-glucanases, esterases, lipases, phosphatases commonly used for extracting yeast extracts in the preparation of common yeast extracts enzyme. 4.根据权利要求2中所述的脱色酵母细胞壁组分的制备方法,其特征在于:进一步将该细胞残渣用酸性水溶液处理是指:用盐酸、硫酸、磷酸、硝酸或者选自乙酸、柠檬酸的有机酸类进行处理。4. according to the preparation method of the decolorizing yeast cell wall component described in claim 2, it is characterized in that: further this cell residue is treated with acidic aqueous solution and refers to: with hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid or be selected from acetic acid, citric acid organic acids for processing. 5.包被剂,其特征在于:所述包被剂以如权利要求2所述制备的脱色酵母细胞壁组分为主要成分。5. The coating agent, characterized in that: the coating agent uses the decolorized yeast cell wall component prepared as claimed in claim 2 as the main component.
CN 03824455 2002-08-21 2003-08-21 Decolorized Yeast Cell Wall Components Expired - Fee Related CN100537741C (en)

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