WO2019004555A1 - FUNCTIONAL CRYSTALLINE SWEETENER - Google Patents

Abstract

The present invention relates to a functional saccharide having specific crystallinity, a method for producing the same, and a functional sweetener comprising the crystalline saccharide.

Description

 【Specification】

 Title of the Invention

Crystalline type ^' functional sweetener [Technical field]

 The present invention relates to a functional saccharide having a specific crystallinity, a process for producing the same, and a functional sweetener containing the crystalline saccharide.

BACKGROUND ART [0002]

 Sugar and starch sugar are the biggest markets around 65 trillion worldwide, but as consumers' needs for health-oriented functionalities and premium products around the world become stronger, it is becoming more common for sugar alcohols, fructose Oligosaccharides such as oligosaccharides, and functional sugars such as crystalline fructose. Functional sweeteners, such as sucralose and asparagus, are growing.

 Sweeteners, which collectively refers to seasonings and food additives that make them feel sweet. Among many sweeteners, sugar, glucose, and fructose are most widely distributed as natural components in foods, and are also widely used in the manufacture of processed foods. However, as a negative aspect of 'sugar' causing laxity, obesity, and diabetes, a functional alternative sweetener that can be used in place of sugar has attracted attention.

In recent years, there has been known as one of the saccharides which can be substituted for sugars or fructose as a functional sweetener, as a sugar. Allo Ross can be produced by chemical or biological methods, but it requires a process of purification and concentration because of the low content of aldehyde in the product. But in the case of concentrated syrup ^. Due to the limitations of its application, high but demand for crystalline powder, Los alreul is difficult to purify low crystalline ^grain.

In addition, even in the case of producing allelose by a biological method using an allelosyltransferase or a strain producing the enzyme, it is necessary to increase the purity of D-allose due to low conversion and then crystallize it. There is still a problem to be solved in the purification process and the yield of crystallization yield of the purification yield. DETAILED DESCRIPTION OF THE INVENTION

 [Technical Problem]

 It is an object of the present invention to provide a process for producing a specific crystalline alum and also for producing the crystalline alum with high yield and high purity. It is also an object of the present invention to provide a sweetener containing crystalline allylose, various foods and beverages to which the sweetener is applied, and the like.

[Technical Solution]

 The present invention provides a method for producing a specific crystalline allylose, producing the crystalline allyl at a high yield and a high purity, and to provide various uses of the specific crystalline allylus.

 The Alloy crystals according to an embodiment of the present invention are characterized by X-ray spectroscopy

15.24, 18.78, and 30.84 at diffraction angle (2 &thetas;) soil 0.2. ^In one embodiment of the present invention, the X-ray spectroscopic spectra show diffraction angles (2 &thetas;) of 15.24, 18.78, 30.84 and 31.87 at diffraction angles (2 &thetas; 0.2) of 15.24, 18.78, 30.84 and 28.37 in X- Master

Ray spectroscopic spectrum having a peak at 0.2 or a diffraction angle (2 &thetas;) of 0.2 at 15.24, 18.78, 30.84 and 47.06. The diffraction angles having peaks in the X-ray spectroscopic spectrum of the above-mentioned all-round crystals are shown by selecting X-ray diffraction analysis results of the peak (Relative Intensity%) main peak and shape-specific peak.

Alloy crystals according to an embodiment of the present invention may have a Tm temperature of 125.8 ^° C soil 5 ^° C or a melting enthalpy (ΔH) of 200-220 J / g according to DSC analysis, and the Tm is 125.8 ^° C soil 3 ^° C.

 (Long diameter / short diameter) of the long diameter (length C micrometer) to the short diameter of the all-round crystal according to an embodiment of the present invention may be 1.0 to 8.0. The allyl crystal according to an embodiment of the present invention may be an aluminum oxide having at least one characteristic selected from the group consisting of the above-mentioned (1) to (5)

 (1) having a powder X-ray spectroscopy spectrum with a peak at diffraction angle (2Θ) soil 0.2 of 15.24, 18.78, and 30.84 on a powder X-ray spectroscopy spectrum,

(2) having a Tm temperature of 125.8 ^° C and 5 ^° C according to differential scanning calorimetry (DSC) (3) having a melting enthalpy (? H) of 200 to 220 J / g according to differential scanning calorimetry,

 (4) having an average long diameter of 350 or more, preferably 350 to 2,000 / m, and

 (5) The ratio of the length (micrometer) of the long diameter to the short diameter of the aluminum crystal (= long diameter / short diameter) is in the range of 1.0 to 8.0.

 A further example of the present invention relates to a sweetener composition comprising an allyl crystal having at least one characteristic selected from the group consisting of the above-mentioned (1) to (5). Yet another example of the present invention includes foods, beverages, feeds, medicines or cosmetics containing the above-mentioned allolin crystals.

Than ^i, it is intended to describe the invention in more detail.

 The Alloy crystal crystallized in an example of the present invention may have one or more properties selected from the group consisting of the following (1) to (5):

 (1) with a powder X-ray spectroscopy spectrum having peaks at diffraction angles (2Θ) ± 0.2 at 15.24, 18.78, and 30.84 on a powder X-ray spectroscopy spectrum,

(2) having a Ttn temperature of 125.8 ^° C soil 5 ^° C according to differential scanning calorimetry (DSC)

 (3) having a melting enthalpy (? H) of 200 to 220 J / g according to differential scanning calorimetry,

 (4) those having an average long diameter of 350 to 2000 or more, and

(= Long diameter / short diameter) of the length (micrometer) of the long diameter to the short diameter of the alumina crystal (5) is in the range of 1.0 to 8.0, and the alumite crystal according to the present invention is obtained by various crystallization methods It can be, but may be a characteristic measured by the ^{"manufacturing} hanalreul loss determined by the nyaeng gakbeop. The powder X-ray spectral analysis of the Alloys crystals according to the present invention may have a powder X-ray spectroscopy spectrum having peaks at diffraction angles (2Θ) soil 0.2 of 15.24, 18.78, and 30.84. Preferably, the crystals have a diffraction angle (2Θ) of 0.25 at 15.24, 18.78, 30.84 and 31.87 at a diffraction angle (2Θ) of 0.2 at 15.24, 18.78, 30.84 and 28.37, or diffraction angles of 15.24, 18.78, 30.84 and 47.06 Ray diffraction spectrum with a peak at each (2Θ) soil 0.2. More specifically, the X-ray spectroscopic spectra were recorded at 15.24, 18.78, 30.84, 27.37, 47.06 and 31.87 And may have a peak at a diffraction angle (2Θ) of 0.2.

 The diffraction peak value at the above-mentioned diffraction angle (2 &thetas;) may indicate a slight measurement error due to the measuring instrument or measurement condition or the like. Specifically, the measurement error may be in the range of soil 0.2, preferably soil 0.1, and more preferably soil 0.06.

The Alloy crystal according to the present invention can be analyzed by thermal analysis, specifically, differential scanning calorimetry (DSC). According to the DSC analysis, the melting temperature (Tm) of the Alloy crystal according to the present invention may have a temperature of 125.8 ^° C soil 5 ^° C, preferably 3.0 ^° C soil, more preferably 1.0 ^° C soil. The melting temperature of the alumina crystal may be 200 to 220 J / g, for example, 212.7 J / g, as measured by DSC analysis. Differential Scanning Calorimetry (DSC) is a measure of the energy provided to keep the temperature increase of the Alloy powder sample at 2: 5 depending on the silver gradient. In the DSC analysis of crystals, it can be predicted that the higher the heat capacity, the easier the dissolution is, and the higher the heat capacity and the narrower the width of the endothermic peak, the more uniform and harder the crystal is formed.

 The Alloy crystal according to the present invention may have an average short diameter of crystals of 50 or more to 1,000, preferably 50 or more to 500 / zm, and an average long diameter of 350 or more, preferably 350 to 2, 000, and more preferably 400 micrometers or more to 2,000.

 The length (micrometer) ratio (= long diameter / short diameter) of the long diameter to the short diameter of the allodynic crystal according to the present invention is preferably 1.0 to 8.0, 1.0 to 6.9,

1.0 to 6.0, 1.0 to 5.5, 1.0 to 5.0, 1.1 to 8.0, 1.1 to 6.9,

1.1 to 6.0, 1.1 to 5.5, 1.1 to 5.0, 1.3 to 8.0, 1.3 to 6.9, 1.3 to 6.0, 1.3 to 5.5, 1.3 to 5.0, 1.5 to 8.0, 1.1 to 6.9, 1.5 to 6.0, 1.5 to 5.5, 5.0, 2.0 to 8.0, 2.0 to 6.9,

2.0 to 6.0, 2.0 to 5.5, and 2.0 to 5.0.

 According to the result of the powder XRD pattern analysis on the Alloy crystal according to the present invention, the Allox crystal according to the present invention is a pure crystal grain and has a rectangular hexahedron or a structure close thereto. The closer the crystal structure of the present invention is to a cubic system, the more preferable is the uniformity and firmness of crystals.

Further, the more uniform the crystals produced in the crystallization process of the Alloys, the higher the crystal strength and the smaller the particle breakage, The flowability can be improved. On the other hand, when the uniformity is low, it is undifferentiated due to breakage of the crystal grains in the drying and transferring stages, and may melt relatively easily, adversely affecting the quality of the product.

 In the present invention, " purity of crystal " means the purity of the crystals of alum. The physical properties including the purity of the crystals of the present invention can be obtained by methods such as X-ray powder diffraction analysis, differential scanning calorimetry (DSC) analysis, infrared spectroscopy (FTIR) analysis, HPLC analysis, LC / MS analysis , And the purity can be specifically analyzed by HPLC chromatography.

 The purity of the crystals of the present invention may be 70% by weight or more, preferably 80% by weight or more, more preferably 90% by weight or more, further preferably 95% by weight or more and most preferably 98% by weight or more. Purity within this range is desirable for quality assurance.

The Alloy crystal of the present invention has better flowability than the powder of the powder of the non-powder type, is not stable in caking, is stable in storage, and has characteristics of easy circulation and handling. In addition, since the aldolose powder has a calorie lower than that of sugar and has characteristics similar to sweet sugar, it is easy to produce a sweet sweetener, solid sweet syrup sweet chocolate, chewing gum, instant juice, instant soup, granule, . In addition, the alreul Los crystal powder is contained in the various compositions, such as sikeumryopum symbol water, feed and feed _i cosmetics, and pharmaceuticals can be used, methods of incorporating the saccharide is exemplified by the process until the ssepum is complete Known methods such as stirring, mixing, dissolving, melting, immersion, penetration, spraying, coating, coating, spraying, injection, crystallization and solidification can be appropriately selected. , And a specific example of the present invention can provide a sweetener composition comprising the aldolose crystal powder. The sweetener composition may contain a lotus crystal powder having various contents, and may further include at least one selected from the group consisting of high sweetness sweeteners, monosaccharides except for allyose, disaccharides, sugar alcohols, dietary fibers and oligosaccharides have.

For example, the monosaccharides and disaccharides may be selected from the group consisting of aloses; Deoxiribosu, Erythrose, Galactose, Idose, Mannose, Ribose, Solbos, Tagatos, Eritrose, Fructos Gentiobios, Gentio Biodoros, Isomaltos, Isomar Roth, Koji Bios, , Melanoblast, melibios, melibius, nigerros, raffinose, mannose, mannoseose, mannose, crossroads, Ruti North, Ruti pressing can be at least one member selected from the group consisting of loss, stachyose, trehalose, trehalose, Tre halreul Ross, two Lanos, a xylene agarobiose, ^fructose, glucose, and alreul loss. ^'

 Wherein the sugar alcohol is selected from the group consisting of xylitol, maltitol, erythritol, mannitol, lactitol, inosine and sorbic acid. Or more. The dietary fiber may be a water-soluble dietary fiber, and the water-soluble dietary fiber may be at least one selected from the group consisting of polytextrose, indigestible maltodextrin and pectin. The oligosaccharides include fructooligosaccharides, isomaltooligosaccharides, maltooligosaccharides And galacto-oligosaccharides.

 Wherein the high-sweetening sweetener is one selected from the group consisting of aspartame, acesulfame potassium, sodium cyclamate, saccharin sodium, sucralose, stevia sweetener (steviol glycoside, enzyme-treated stevia), dicin, tau martin, Ribavirin, rebaudioside, and monelin. ≪ / RTI >

The method for producing an allrozole crystal according to the present invention can be carried out by various methods, and preferably by the grating method. For example, the method for preparing the above-mentioned all-round crystals comprises the step of mixing at least 90wt% of rosin with 60-85 bricks of Alloy solution at 20-40 ^° C or 30-40 ^° C, Stirring the solution at a temperature of 35 ^DEG C slowly to produce crystal nuclei, and cooling the solution to a temperature of i (rc) to grow crystals, for example, an Alloy solution at 35 to 10 It is preferable to keep the cooling rate at 0.01 to 20 ^° C / min, and if the cooling rate is low, the productivity of the co-crystal may be low due to the long formation time of the co-crystal When the angular velocity is high, crystals having a small particle size are formed and it may be difficult to recover the crystals. The method for producing the above-mentioned alumina crystals comprises 90% by weight or more of alumina, 60 to 85 Bricks and The method may include the steps of forming a crystal nucleus in an Alloy solution having an electrical conductivity of 1, 000 LiS / cm or less, and cooling the temperature of the solution to grow crystals. Specifically, Slowly stirring an allylose solution containing 80 to 83 Bricks of allylose in an amount of at least 90% by weight at 35 ^° C to produce crystal nuclei, and growing crystals by agitating the solution to KC . The method may further include one or more times of increasing the temperature of the solution to a range of 20 to 40 ^° C, preferably 30 to 35 ^° C, to redissolve the microcrystals produced during cooling. The method for producing the allylose crystal may further include a step of adding the seed. The seedling addition step and the redissolution step may be optionally included in the method for producing the allolose crystal, or may include both of the above two steps.

The Alloy solution for crystallization may be a high purity Alloy solution containing Alloy in an amount of 90 wt% or more, for example, 95 wt% or more. The viscosity of the composition may be from 2 cps to 200 cps at a temperature of 45 ^° C and the electrical conductivity is 1000 uS / cm or less, for example, 0.01 to 1000 uS / cm, preferably 30 LiS / cm or less, 1 to 30 uS / cm. The lower the electric conductivity of the composition for crystallization of the alumina is, the more preferable it is for crystallization. The Alloy solution for the crystallization may have a solids content of 60 or greater to 85 Bricks or less, such as greater than 60 Bricks to 80 Bricks, 65-85 Bricks, 65-80 Bricks, or 68-85 Bricks.

 In general, it is known that the greater the size of the alallose crystal is, the better the physical properties and the ease of use are. In order to produce such a large-sized crystal, both the seed crystal classified by the transfer process and the present crystallization process must be performed. The crystallization process according to the present invention can easily produce crystals of comparatively large size at a high yield even in a one-step process.

The crystallization process may be performed in the crystal growth process _. A process of dissolving the microcrystals can be performed by raising the temperature of the solution to 30 to 35 ^° C in order to redissolve the microcrystals produced during the agglomeration. In the crystallization process according to the present invention, the crystal growth process and the microcrystalline dissolution process can be repeated at least once or more.

 In the step of producing the crystal, seeds may be further added for the purpose of increasing the crystal generation rate and size.

In a specific example according to the present invention, the Alloy crystal comprises an Alloy sol based on solids content of 90% by weight or more and a total solids content of 60 to 85 Bricks at 20 to 40 ^° C, preferably 30 to 40 ^° C ^Deg.] C, for example, at 35 [ ^deg.] C to produce a small amount of crystal nuclei, followed by decreasing the temperature by rc to degrade at a temperature of 10 [ ^deg.] C. Microcrystals By remelting repeating at least once the step of increasing the temperature of the solution to 30 to 35? Dissolve the microcrystals to, it can ^'be prepared alreul LOS determined.

 In one embodiment of the present invention, a method for producing an aldolose crystal comprises the steps of: a second ion purification of an allyl fraction obtained in an SMB chromatographic separation step; a step of concentrating the ion-purified allyl fraction; To obtain an Alloy crystal, and may optionally further include a recovery process, a washing process and a drying process for the Alloy crystals.

 Specific examples of the preparation of the alumina crystals may include a first ion purification, an SMB chromatography separation, a secondary ion purification, a concentration and a crystallization process. Alternatively, The purification process, or both the activated carbon treatment process and the ion purification process can be performed.

The method of preparing an allrozole crystal according to the present invention can crystallize by controlling the temperature and concentration of an alcohol concentrate solution. Specifically, the supersaturated state required for crystallization can be obtained by lowering the temperature of the allolose solution or by adjusting the D- Alloy in solution. Can be maintained by varying the concentration of D-allose. In one embodiment of the present invention, the crystallization process is monitored by collecting a sample at a predetermined interval in the crystallization step and observing the concentration of the supernatant obtained by visual observation or microscopic observation or by centrifugation of the sample, Depending on the result, the temperature or the concentration of the D-allose can be controlled. In the case of crystallization by crystallization of an Alloy concentrate solution in order to produce an Alloy crystal, rapid cooling to a temperature range of 10 to 25 ^° C through a heat exchanger, followed by repeated heating and cooling, have.

The method for producing an allrox crystal according to the present invention is characterized by further comprising the steps of recovering the allyl crystals obtained in the crystallization step by various solid-liquid separation methods, for example, centrifugal separation, washing with deionized water, and drying . The drying step may be performed in a fluid bed dryer or a vacuum dryer _. But is not limited thereto. The allyl contained in the alumina crystals may be 94 wt% or more, 95 wt% or more, 96 wt% or more, 97 wt% or more, 98 wt% or more, or 99 wt% or more based on the total solid content of 100 wt% have. 【Effects of the Invention】

 The allrose crystal and the method for producing the same according to the present invention can produce allodyne crystals with high yield and high purity. The method for producing the allodolite crystals can be applied to various foods and beverages including the sweetener.

BRIEF DESCRIPTION OF THE DRAWINGS

 Figs. 1 to 3 are optical microscopic photographs of the alumina powder obtained in Examples 1 to 3 of the present invention at a magnification X100.

 4 to 6 are scanning electron microscope (SEM) photographs of the alumina powder obtained in Examples 1 to 3 of the present invention at a magnification X50.

 7 is an infrared spectroscopy (IR) spectrum of the aldol crystals obtained in Examples 1 to 3 of the present invention. DETAILED DESCRIPTION OF THE INVENTION

 The invention is illustrated in more detail by the following examples. However, the following embodiments are merely preferred embodiments of the present invention, and the present invention is not limited thereto. Example 1: Alloy crystal preparation

A high-purity allyl containing 94.6% by weight of allylose based on 100% by weight of solid content was concentrated to a concentration of 82.6 Bx (w / w%) to prepare a syrup for crystallization having an electrical conductivity of 8 uS / cm . The crystals were crystallized at a temperature of 35 ^° C at which the supersaturated state of the syrup was formed at a temperature of 1 ^° C. The crystals were gradually grown at 35 ^° C. and a small amount of crystals After the nucleus is formed, the crystal is grown by decreasing the temperature by 1 ^° C per hour. In order to redissolve the microcrystals produced during the crystal growth process in the crystal growth process, the solution is raised to 30-35 ^° C The crystallization was performed by repeating the above crystal growth process and the microcrystalline melting process at least once or more. The allyl crystals prepared in this manner were prepared by removing the mother liquor by centrifugal dehydration, The crystals were washed with cooling water, then dried and recovered. The obtained primary crystals were dissolved in water to prepare an 81.6 Brix Alloy lysine solution having an Alloy 99.5% solids content on the basis of a solid content of 100 wt%.

 Secondary crystallization was carried out using the prepared allyl lysate in substantially the same manner as the primary crystallization. The alallose crystals prepared here were removed by centrifugal dehydration to remove the mother liquor, and the final crystals obtained by the secondary crystallization were washed with 넁 water, dried and recovered.

 The purity of the above-prepared alumina crystal was determined by the following HPLC analysis.

 Analytical column: Biol ad Aminex HPX-87C column

 Mobile: Water

 Flow rate: 0.6 ml / min

Column temperature: 80 ^° C

 Detector: RI detector

 As a result of the above-mentioned HLPC analysis, the purity of the Alloy crystals prepared in Example 1 was as follows. 99.8% by weight, and the crystal yield was 62.5%. The crystal yield is calculated by dividing the weight of the raw material powder for crystallization by the percentage of the weight of the recovered crystalline powder to the weight of the solid content of the syrup. Example 2: Manufacture of alallose crystals

High-purity alum, containing 94.6% by weight of allylose based on 100% by weight of solid content, was concentrated to 82.6 Bx concentration to prepare a crystallization allyl for crystallization with an electrical conductivity of 16 uS / cm. When the crystals were cooled to a temperature of 35 ^° C at which the supersaturated state of the syrup was cooled to a temperature of rc to slowly crystallize the crystals, the resulting crystals were slowly stirred at 35 ^° C to obtain a small amount of crystals The temperature of the solution is raised to 30 to 35 ^° C in order to redissolve the microcrystals produced during the crystallization step in the crystal growth process. The crystallization was performed by repeating the above-mentioned crystal growth process and microcrystalline melting process at least once. The allyl crystals prepared in this case were removed by centrifugal dehydration to remove the mother liquor, and the crystals were washed with distilled water After that, it was dried and recovered.

The purity analysis of the above-prepared allylox crystal is performed as described above. The HPLC analysis was carried out in the same manner as in Example 1, By weight and the purity of the solution was 99.6% by weight), and the crystal yield was 52.8%. Example 3: Alloy crystal preparation

A high-purity allyl containing 91.5% by weight of allylose based on 100% by weight of solid content was concentrated to a concentration of 81.2 Bx to prepare a crystallized allyl syrup having an electrical conductivity of 21 uS / cm. Crystallization was carried out by gradually cooling the prepared allylose syrup for crystallization to a supersaturated state at a temperature of 35 ^° C to a temperature of C ^degrees . At this time, the aldolose seeds were added and slowly stirred at a temperature of 35 ^° C to produce a small amount of crystal nuclei, and the crystal was grown by decreasing the temperature by 1 ^° C per hour. In order to redissolve microcrystals produced during the crystallization step, the temperature of the solution is raised to 30 to 35 ^° C to dissolve the microcrystals. The crystallization process and the microcrystalline dissolution process are repeated at least once The crystallization was repeatedly performed. The columnar crystals prepared here were removed by centrifugal dehydration to remove the mother liquor, and the crystals were washed with cooling water, and then dried and recovered.

 The purity of the thus-prepared all-round crystals was analyzed by HPLC in the same manner as in Example 1, and the purity of the all-in-one crystals prepared in Example 3 was 99.6% by weight and the crystal yield was 34%.

 According to the production of the all-round crystals of Examples 1 to 3, as the crystallization raw material purity is lower, the components other than Alloch act as pure impurities that interfere with the crystal growth of the los, There was a difference in crystal yield depending on the purity. Specifically, in Example 1, the purity of the crystals obtained by the crystallization process of Alloy syrup twice and the yield of crystals of the crystals were higher than that of Example 2 in which the crystallization process was performed once. The purity of crystals and the yield of crystals were higher in Example 1 and Example 2 in which the purity of the crystallization stock solution was high than in Example 3 in which the crystallization stock solution having a relatively low purity was used. Example 4 Analysis of Alloy Crystal Characteristic

 4-1: Analysis of grain size distribution

Examples. The particle size distributions of the alallose crystals obtained from 1 and 3 were confirmed by using standard mesh of Mesh. Mesh si ze of the standard net was 20, 30, 40, 60, 80, 100mesh, and the size of the hole of the standard net, The distribution was measured.

 For each mesh, the standard mesh size is 850, 600, 425, 250, 180, and 150 ^ 1. Each sample was weighed at a weight of 100 g, placed in a standard mesh of mesh size, and vibrated for 3 minutes to pass through a standard mesh. The weight of the sample remaining in the sieve according to each mesh size is determined and the percentage value is shown in Table 1. In Table 1, the particle size distribution of each mesh shows the weight percentage of the particles.

[Table 1]

상기 표 1에 나타낸 바와 같이， 실시예 1의 알롤로스 결정은 입자 분포가 90.2 중량 %가 집중되어 매우 좁은 분포를 나타내며 , 실시예 3의 알를로스 결정은 40†에서 .가장 많은 분포를 보이기는 하지만, 80† , 60† , 40† ， 및 30†에서 고르게 분포하여 입자 분포가 넓게 퍼져 있는 것으로 확인하였다. 실시예 1과 같이 장직경 /단직경의 비율이 작고 견고한 결정 입자일 수록, 제품의 미분함량이 상대적으로 낮고, 균일한 입도 분포를 갖고 있음을 확인하였다. 또한 장직경 /단직경의 비율이 크고 낮은 균일도의 입자일수록, 건조 및 이송 과정에서 입자 깨짐에 의해 미분화되고, 입도가 불균일하게 되어 넓은 범위의 입도 분포를 갖게 될 수 있다. 4-2： 결정 형태 및 결정 입자 크기 분석

As shown in Table 1, the allylose crystals of Example 1 exhibit a very narrow distribution of 90.2% by weight of the particle distribution, while the allyl crystals of Example 3 have the largest distribution at 40 캜 , 80 †, 60 †, 40 †, and 30 †. It was confirmed that the fineness of the product was relatively low and the particle size distribution was uniform as the ratio of the long diameter to the short diameter was small and the crystal grains were solid as in Example 1. Further, particles having a large diameter / small diameter ratio and a low uniformity are undifferentiated due to particle breakage during drying and transportation, and the particle size becomes uneven, so that a wide range of particle size distribution can be obtained. 4-2: Crystalline morphology and crystal grain size analysis

 1 to 3 show photographs of the optical microscope photographs obtained by measuring the magnifications X100 of the all-round crystals obtained in Examples 1 to 3. Scanning electron micrograph (SEM) photographs of the aluminum crystals obtained in Examples 1 to 3, which were measured at a magnification X100, are shown in Figs. 4 to 6. Fig.

Further, with respect to nine samples of the allodyne crystals obtained in Examples 1 to 3 The long diameter (length) and the short diameter (width) were measured, and the particle diameter ratio (= long diameter / short diameter) was obtained. Specifically, for the five crystals, the ratio of the length () of the long diameter to the length of the short diameter (1) was shown.

 [Table 2]

도 4 내지 도 6에 나타낸 바와 같이, 본 발명에 따른 알를로스 결정은 장방형 육면체 또는 이에 근접한 결정구조를 가진다. 상기 표 2에 나타낸 결정의 단직경 길이 ( )을 1로 기준하여 나타낸 장직경의 길이 ) 비율은, 실시예 1의 경우 평균 1 .6 , 실시예 2의 결정은 평균 4.3 , 및 실시예 3의 결정은 평균 7.6으로서, 상대적으로 실시예 1의 결정이 실시예 2와 3의 결정보다 각각의 결정면이 균일하게 성장하여 정방형에 가까운 사방정계의 결정형태를 형성하고 있다. 또한, 결정면이 균일하게 성장할 수록 장직경 /단직경 비율이 감소하는 경향을 나타남을 확인할 수 있었다. 이는 결정화 원료의 알를로스 순도가 낮을수록, 알를로스 외 다른 성분들이 순수 알를로스의 결정 성장을 방해하는 불순물로써 작용하기 때문에 결정 모양에 영향을 미친 것으로 해석된다. 실시예 5 : 시차주사열량계법 (DSC)분석

As shown in Figs. 4 to 6, the Alloy crystal according to the present invention has a rectangular hexahedron or a crystal structure close thereto. The length of the long diameter indicated by the length () of the short axis of the crystals shown in Table 2 as 1), the average of 1.6 in Example 1, the average of 4.3 crystals of Example 2, The crystals have an average of 7.6, and the crystals of Example 1 are grown more uniformly than the crystals of Examples 2 and 3, forming an orthorhombic crystal form close to a square. Also, it was confirmed that as the crystal surface grows uniformly, the ratio of long diameter / short diameter tends to decrease. It is considered that, as the purity of the crystallization raw material is lower, the influence of the other components on the crystal shape is caused by the fact that other components act as impurities which interfere with the crystal growth of the pure aluminum. Example 5: Differential scanning calorimetry (DSC) analysis

 DSC analysis of the Alloy crystals obtained in Examples 1 to 3 was carried out, and specific DSC analysis conditions were as follows.

Equipment name: DSC [di f ferent ial scanner ng cal or imet ry] ": Perk in Elmer

Method: 30 to 250 ^° C, 10 t / min Souton, N2 gas purge

 (Reference method: see ASTM D 3418)

 The DSC analysis results of the above-mentioned all-round crystals are shown in Table 3 below.

[Table 3]

상기 DSC 분석 결과， 실시예 1의 결정에서 Tm값이 가장 높고, 열용량도 가장 높게 측정되었다. 결정의 DSC 분석에서 열용량이 높을수록 쉽게 녹기 어려우며, 열용량이 높고 흡열 피크의 폭이 좁올수록 결정이 균일하고 단단하게 형성되어 있음을 예측할 수 있다. 상기 실시예 1 내지 3의 열용량과 흡열 피크 엔탈피 값올 고려할 때, 샬시예 1의 결정이 상대적으로 더욱 균일하고 단단하게 형성되어 있음을 확인하였다. 실시예 6: 적외선흡수 (IR) 스펙트럼 분석

As a result of the DSC analysis, the Tm value was the highest and the heat capacity was the highest in the crystals of Example 1. In the DSC analysis of crystals, it can be predicted that the higher the heat capacity, the easier the dissolution is, and the higher the heat capacity and the narrower the width of the endothermic peak, the more homogeneous and harder the crystals are formed. When the heat capacity and the endothermic peak enthalpy values of Examples 1 to 3 were taken into consideration, it was confirmed that the crystals of Shirishi Example 1 were formed more uniformly and firmly. Example 6 Infrared Absorption (IR) Spectrum Analysis

 The infrared absorption (IR) spectral analysis of the crystals of Examples 1 to 3 was carried out in order to confirm the aldol crystals prepared above, and the measurement conditions were as follows.

Analytical Instruments: TENSOR II with Platinum ATR, manufacturer; Bruker (German) stem sword ^{': highly sensitive photovoltaic MCT detector with} liquid ni trogen cool ing.

 Number of scans: 64 scans at 20 kHz

Scan range: 800 - 4,000 ctrf ¹ and averaged at. 4 cm -1 resolution.

According to the results of infrared absorption (IR) spectral analysis, infrared spectroscopic analysis of the Alloy crystal according to the present invention showed that the functional groups -0H and C-0-C, CC, C-OH, And it was confirmed that the crystals of Examples 1 to 3 had the same structure as that of the Alloose molecule. The IR analysis spectrum is shown in Fig. Example 7: X-ray diffraction analysis (XRD ^' ) analysis

The aldolose obtained in Examples 1 to 3. To ^"the crystal higher the X- ray diffraction analysis was carried out for Example 1 X-ray of alrol Los crystals obtained in 1-3 diffraction analysis according to the specific assay conditions (Relative Intensity%) selected for the five peak shape and specific peak Are shown in Table 4

 Analytical instrument: D / MAX-2200 Ultima / PC

 Manufacture 1 ": Rigaku International Corporation (Japan)

 X-ray sauce system target: sealed tube Cu

 Tube voltage: 45 kV I tube current: 200 mA

Scan range: 5 to 80 ^° 2Θ

 Step size: 0.0Γ

Scan speed: 5 ^° / min

 [Table 4]

상기 표 4에 나타낸 바와 같이, 실시예 1에서 얻어진 알를로스 결정은, 분말 X—선 분광 스펙트럼 상에서 2Θ값이 15.24, 18.78 및 30.84; 15.24, 18.78, 30.84, 및 28.37； 또는 15.24, 18.78, 30.84 및 31.87;에서 특이적인 피크를 갖는 것임을 확인하였다.

As shown in Table 4 above, the Alloy crystals obtained in Example 1 had 2? Values of 15.24, 18.78, and 30.84 on a powder X-ray spectroscopic spectrum; 15.24, 18.78, 30.84, and 28.37; or 15.24, 18.78, 30.84, and 31.87;

On the X-ray spectroscopic spectrum, it is confirmed that the crystals of Examples 1 to 3 have the same range of Angle 2-Theta degree values, and thus have the same crystal lattice structure. However, since the crystals of Example 1 are somewhat different from the crystals of Examples 2 and 3 in appearance, the orientation of the crystal lattices There may be a difference, which can be deduced from the difference in Intensity values. Example 8: Measurement of Flowability of Alloy Crystal

 In order to analyze the flowability of the Alloy crystals, the angle of repose of the crystal powders of the yarn watches 1 and 3 was measured.

 Specifically, the crystal powders of Examples 1 and 3 were passed through a funnel fixed at a constant height of 20 cm on a perfectly flat reference plate to form a three-dimensional The angle of repose was measured at different points.

Embodiment the angle of repose of the crystals obtained from Example 1 is ^{42 .6 °, 43 .3 °,} 42.2 °士0.2 ° and the mean value of the angle of repose of 42 .7土crystals obtained was 0.2 ^°, the third embodiment is 46.0 ^°, 45.3 ^° , 46 .2 ^°士0.2 ° and the average value was 45.8 ^° + 0 .2 ^°. The angle of repose is the shape created by the natural fall of the powder on the horizontal plane, which has a great influence on the flowability. Generally, if the angle of repose is small, it can be judged that the flowability of the powder is good. In the same manner as in the method of measuring the angle of repose of the above-mentioned alumina crystals, sugar (average particle size 420) and crystalline fructose

341), the mean value of the angle of repose of sugar was 41.2 ^° soil

And the average angle of repose with crystals was 41.8 ^° soil 0.2 ^° . When compared with the sugar, the fructose and the angle of repose, it was confirmed that the fructose of fructose has the same degree of powder flowability.

Claims

Claims:  Claim 11 Having an X-ray spectral spectrum having peaks at diffraction angles (2 &thetas;) at 0.2 ^DEG of 15.24, 18.78, and 30.84 in the X-ray spectral spectrum. [Claim 2] The method of claim 1 wherein the X- ray spectrum is X euseon diffraction angle (2Θ) of 15.24, ^18.78,, 30.84 and 28.37 in the spectrum土0. Having an X-ray spectral spectrum with a peak at 2 [ ^deg .].  [Claim 3] The method of claim 1, wherein the X-ray spectroscopy spectrum has an X-ray spectral spectrum having peaks at diffraction angles (2 &thetas;) at 0.2 ^DEG of 15.24, 18.78, 30.84 and 31.87 in X- decision.  [4] 2. The method of claim 1, wherein the X-ray spectral spectrum has an X-ray spectral spectrum with a peak at a diffraction angle (2 &thetas;) of 0.25 ^deg . At 15.24, 18.78, 30.84 and 47.06 in X- Ross decision.  [Claim 5] The method according to claim 1, wherein the X-ray spectral spectrum has an X-ray spectral spectrum having peaks at diffraction angles (2Θ) and 0.2 ^° of 15.24, 18.78, 30.84, 27.37, 47.06 and 31.87 in X-ray spectroscopy Ross decided to make a decision. [Claim 6] Alloy crystals having a Tm of 125.8 ^° C soil 5 ^° C or a melting enthalpy (ΔH) of 200-220 J / g according to differential scanning calorimetry (DSC) analysis.  [7] 5. The method according to claim 4, wherein said Tm is a temperature of 125.8 ^° C soil 3 ^° C.  8.  The average long length of crystals is 350 or more.  [Claim 9]  9. The Alloy crystal according to any one of claims 1 to 8, wherein the ratio (= long diameter / short diameter) of the long diameter length (micrometer) to the short diameter of the crystal is in the range of 1.0 to 8.0. Claim 10 9. The crystalline aldolose according to any one of claims 1 to 8, wherein the crystals have an average short diameter of 50 to 1,000.  Claim 11  At least one kind selected from the group consisting of the following (1) to (5):  (1) having an X-ray spectroscopic spectrum having peaks at diffraction angles (2 &thetas;) at 0.2 deg. At 15.24, 18.78, and 30.84 in the X-  (2) having a Tm temperature of 125.8 eV 51,  (3) having a melting enthalpy (? H) of 200 to 220 J / g, (4) having an average long diameter of 350 or more, and  (5) The ratio of the length (micrometer) of the long diameter to the short diameter of the crystal (= long diameter / short diameter) is in the range of 1.0 to 8.0.  Claim 12 12. The method according to claim 11, wherein the Tm is a temperature of 125.8 ^° C soil 3 ^° C.  [13]  12. The method according to claim 11, wherein the crystal purity of the crystals is at least 70% by weight.  [14]  14. The sweetener composition according to any one of claims 1 to 13, which comprises an allotrocerol crystal.  15.  15. The sweetener composition according to claim 14, wherein the sweetener composition further comprises at least one selected from the group consisting of high-sweetness sweeteners, monosaccharides except for allyose, disaccharides, sugar alcohols, dietary fibers and oligosaccharides.  16. The method of claim 16, Producing a crystal nucleus at a temperature of 20 to 40 [ ^deg.] C with an Alloy solution of 60 to 85 Bricks containing at least 90% by weight of Alloy, and And lowering the temperature of the solution to grow crystals.  17. 17. The method of claim 16, wherein the method further comprises increasing the temperature of the solution to a range of 20 ^° C to 40 ^° C to redissolve the microcrystals formed during cooling, Lt; / RTI >  Claim 18  17. The method of claim 16, wherein the method further comprises adding a seed.