CN100341422C - Method for descreasing colchicin content of fresh day lily - Google Patents
Method for descreasing colchicin content of fresh day lily Download PDFInfo
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- CN100341422C CN100341422C CNB2003101104832A CN200310110483A CN100341422C CN 100341422 C CN100341422 C CN 100341422C CN B2003101104832 A CNB2003101104832 A CN B2003101104832A CN 200310110483 A CN200310110483 A CN 200310110483A CN 100341422 C CN100341422 C CN 100341422C
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- IAKHMKGGTNLKSZ-INIZCTEOSA-N (S)-colchicine Chemical compound C1([C@@H](NC(C)=O)CC2)=CC(=O)C(OC)=CC=C1C1=C2C=C(OC)C(OC)=C1OC IAKHMKGGTNLKSZ-INIZCTEOSA-N 0.000 title claims abstract description 121
- 238000000034 method Methods 0.000 title claims abstract description 32
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- 239000011780 sodium chloride Substances 0.000 claims abstract description 42
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 29
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- 241000234435 Lilium Species 0.000 description 3
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- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
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Abstract
The present invention relates to a method for decreasing colchicine content in fresh day lilies, which comprises: fresh day lilies are soaked in a NaCl solution of a certain concentration under a cold condition for some time so as to effectively and rapidly reduce colchicine content in fresh day lilies to avoid food poisoning caused thereby and protect people body health. In addition, the present invention has the advantages of simple process, common material, low cost, easy manufacture, application to mass commercial process and practical performance, no influence on the original taste and nutrients of day lilies and value of popularization.
Description
Technical field:
The present invention relates to the essential a kind of vegetables processing and treating method of human daily life, be specifically related to a kind of method that reduces Colchicine Content in the cadmium yellow cauliflower.
Background technology:
Day lily is the dish of one aromatic flavour on people's dining table, especially the fresh day lily in summer is more good to eat, but owing to contain a certain amount of colchicin in the cadmium yellow cauliflower, if processing is dealt with improperly, can cause food poisoning after edible, symptoms such as headache, nausea,vomiting,diarrhea occur.This is owing to after colchicin enters the human intestines and stomach in the cadmium yellow cauliflower, through slowly absorbing, become a kind of noxious material that is oxidation two colchicins in vivo.The edible fresh day lily surpasses 100g/ time (the colchicum alkali number reaches 0.1-0.2mg) can cause poisoning.In order to make edible that fresh day lily can be relieved safely, just need carry out certain processing to fresh day lily product and reduce Colchicine Content.
Summary of the invention:
Technical problem to be solved by this invention is: solve existing cadmium yellow cauliflower and do not reduce the processing of Colchicine Content, can cause food poisoning after edible, endanger the healthy problem of people; And provide a kind of method that reduces Colchicine Content in the cadmium yellow cauliflower; effectively reduce Colchicine Content in the cadmium yellow cauliflower; cause food poisoning after avoiding people edible, protect people healthy; make the cadmium yellow cauliflower become the relieved vegetable food of people's safety; and the cadmium yellow cauliflower after handling by the inventive method still keeps the commercial value of bright fragrance U.S., is suitable for suitability for industrialized production and practical application.
The technical solution used in the present invention is: the method for Colchicine Content is in this reduction cadmium yellow cauliflower: adopt certain density NaCl solution fresh day lily to be carried out the immersion treatment of a period of time under cryogenic conditions.
In the technique scheme, described NaCl solution concentration can be 8-15%, i.e. NaCl:8-15%, water: 85-92%.
In the technique scheme, described cryogenic conditions can be :-4 ℃-+4 ℃
In the technique scheme, described soak time can be 0.1-2 hour.
In the technique scheme, the cadmium yellow cauliflower can be extractd the anthocaulus and the gynoecium part of cadmium yellow cauliflower before immersion.
The present invention is soluble in ethanol according to colchicin, water, alkaline solution, and the principle of some organic matter solvents, by repeatedly experiment, soak the cadmium yellow cauliflower as normal temperature NaCl solution, low temperature NaCl solution soaks the cadmium yellow cauliflower, NaOH solution soaks the cadmium yellow cauliflower, finite concentration alcohol immersion cadmium yellow cauliflower, the cadmium yellow that is soaked in water cauliflower ... Deng, after the immersion, it is detected, experimental results show that, under cryogenic conditions fresh day lily is carried out a period of time immersion treatment with certain density NaCl solution, its effect that reduces Colchicine Content in the cadmium yellow cauliflower is better than additive method.As normal temperature NaCl solution-treated, in the percentage maximum of colchicin decline in 1 hour, but the cadmium yellow cauliflower is wilted, destroyed the commodity of cadmium yellow cauliflower; Though it is basic identical with low temperature NaCl solution-treated effect with the percentage that colchicin after the NaOH solution-treated descends, but angle from actual production, the production cost of NaOH solution will be higher than low temperature NaCl solution, and low temperature NaCl solution can not pollute the cadmium yellow cauliflower; Use water treatment, the amplitude that colchicin reduces percentage is too little, and institute's time-consuming is oversize, is unfavorable for production application, and certain density ethanol is volatile, the cost height, and the percentage amplitude that colchicin descends is also on the low side ...Therefore, technology of the present invention is simple, draws materials easily; with low cost; easy to operate, effect is remarkable, is suitable for suitability for industrialized production and practical application; should vigorously promote the use; adopt the inventive method can reduce the content of colchicin in the cadmium yellow cauliflower effectively fast, avoid the edible poisoning of people, the protection people are healthy; and the cadmium yellow cauliflower after handling still keeps the characteristic of bright fragrance U.S., for human daily life provides a kind of safety relieved cadmium yellow flower vegetables and goods thereof.
The specific embodiment:
Embodiment: get concentration and be 10% NaCl solution, under 0 ℃ of condition, to cadmium yellow cauliflower immersion treatment after 1 hour, with untreated sample relatively, Colchicine Content descends 57.51%.The cadmium yellow cauliflower also can be extractd the anthocaulus and the gynoecium part of cadmium yellow cauliflower before immersion treatment.
Analysis and experiment that the present invention " reduces colchicin content method in the cadmium yellow cauliflower ":
One, the quantitatively method principle analysis of employing of colchicin
Thin-layer chromatography is to scheme to be distributed in holder on the support plate as fixing phase, is the phase that flows with suitable solvent, to biased sample separate, evaluation and quantitative a kind of chromatography technology.This is the especially effectively chromatography method of a kind of quick fractionation of fatty, steroids, amino acid, nucleotides, alkaloid and multiple material thereof, grows up so far from the fifties, still is widely adopted.
Thin-layer chromatography is holder evenly to be coated support plate (glass plate commonly used, also available woven dacron etc.) go up and form thin layer, launches by the paper chromatography operation then.Thin-layer chromatography can be divided into thin layer adsorption chromatography (adsorbent), thin layer Partition Chromatography (cellulose), thin layer ion-exchange chromatography (ion-exchanger), shallow layer gel chromatography (molecular sieve gel) etc. according to as the fixing holder difference of phase.Using more in the general experiment is to be the fixing thin layer adsorbent chromatography of phase with adsorbent.
Absorption is a critical nature on surface.Any two phases can form the surface, and absorption is exactly the material of one of them phase or is dissolved in wherein solute in this lip-deep intensive phenomenon.On the surface between solid and the gas, between solid and the liquid, between adsorptive liquid and the gas, adsorption phenomena can take place.
Why material molecule can stop at the surface of solids, and this is because the suffered attraction of the molecule (ion or atom) of the surface of solids and solid interior molecule is unequal.In solid interior, interactional power is symmetrical between the molecule, cancels out each other in its field of force.And the suffered active force of the molecule that is in the surface of solids is asymmetric, the active force that inside one side is subjected to the solid interior molecule is big, and surperficial suffered active force is little, thereby gas or solute molecule be subjected to the influence of this remaining force when running into the surface of solids at the volley, will be attracted and stop.Adsorption process is reversible, and absorbate can desorb under certain condition.In the unit interval, be adsorbed on the molecule on a certain surface area of adsorbent and leave in the same unit interval between this surperficial molecule and can set up dynamic equilibrium, be called adsorption equilibrium.The adsorption chromatography process is exactly constantly to produce balance and homeostasis process uneven, adsorption and desorption.
Make supporting agent with silica gel and aluminium oxide, what its cardinal principle was an absorption affinity with distribution coefficient is different, and mixture is separated.When solvent when adsorbent moves, move together with each component in the sample, continuous adsorption and desorption and distributional effects repeatedly take place simultaneously.Because the different solubility of each component in solvent, and adsorbent is to the difference of their adsorption capacity, mixture is separated into a series of spots the most at last, launch together on the thin layer thin plate as compound as standard, then can identify the component of each spot, also can further adopt simultaneously some method in addition quantitative according to the Rf value of these known compounds.
Two, handle the method for cadmium yellow cauliflower
The NaCl solution of concentration: 8-15%
Temperature :-4 ℃-+4 ℃
Soak time: 0h-2.0h
Addition method: the anthocaulus and the gynoecium part of extracing the cadmium yellow cauliflower
Three, experiment:
1 materials and methods
1.1 material
The bud of day lily (Hemerocallis cibrina Baroni) liliaceous plant tawny daylily, elite agricultural product Co., Ltd provides by the Shaodong County.The kind that provides is bright soaring flower.
1.2 the processing of day lily
Take by weighing a cadmium yellow cauliflower, day lily is peeled off by petal, stamen, gynoecium, ovary classification, smash to pieces respectively.
Take by weighing the approaching cadmium yellow cauliflower of six parts of quality respectively as in the 80ml centrifuge tube with cover, use water, the water of an amount of 10%NaCl, 10% ethanol, pH12 (NaOH transfers pH) respectively, the 10%NaCl that at room temperature reaches 0 ℃ respectively soaks 0.5h, 0.1h, 1.5h, 2.0h, 2.5h, 3.0h.
1.3 the extraction of colchicin and preliminary purification
Cadmium yellow cauliflower after treatment shreds back stone roller alms bowl and smashs to pieces, presses the absolute ethyl alcohol amount lixiviate 15min of 0.5ml/g, and the centrifugal 15min of 4000rmp gets supernatant.Extract places 4 ℃ of placements, adds the centrifugal 8min of a little powder activated carbon 1000rmp and removes large biological molecule and pigment.The extract of preliminary purification places 4 ℃ of preservations.
1.4 colchicin thin-layer chromatography
Thin layer chromatography board is that GF254 adds 0.7% sodium carboxymethylcellulose water and is in harmonious proportion by a certain percentage, is layered on uniformly on the clean glass plate, forms thin plate, dries back 110 ℃ naturally and activates one hour, places drier standby
[4] [5] [6], the point sample amount is 5 μ l, and point sample is followed successively by colchicin standard specimen 10mg/L and 100mg/L in proper order, is each six different time treatment samples handling sample then, and solvent is a methyl alcohol: ammoniacal liquor (20: 1), development distance are 1cm-1.5cm.Thin layer chromatography board scans with high performance thin layer chromatography (Thin-layerchromatoyraphy) CAMAG-III.
1.5 the data of high performance thin layer chromatography are handled
The content of colchicin carries function software by CAMAG-III, according to the content and the proportional relation of crest area of standard specimen, calculates the content of the colchicin of each sample.
2 results
2.1 cadmium yellow cauliflower flower different parts Colchicine Content
The cadmium yellow cauliflower different parts Colchicine Content that calculates after the high performance thin layer chromatography scanning sees Table 1.
The result shows that the amount of contained colchicin is the highest in the ovary of unit mass, reaches 0.00516mg/g, is the twice of the contained colchicin of unit mass petal.But in the day lily of unit mass, the contained colchicin of ovary has only 0.00015mg/g, and petal is up to 0.00169mg/g.In the day lily of unit mass, the total amount only petalled 1/2 of the colchicin at stamen, gynoecium, three positions of ovary.See Fig. 1, Fig. 1 is a cadmium yellow cauliflower different parts Colchicine Content table.
* sample flower gross mass is 18.785g, and wherein the quality of petal is 14.630g, and petal is sampled as 3.680g in the experiment
Fig. 2 is a cadmium yellow cauliflower different parts Colchicine Content, the three-dimensional collection of illustrative plates of efficient thin layer scanning, and the right of figure is the crest figure of colchicin.
Fig.2?The?Different position colchicines contents?of?fresh?day?lily?Three-dimensional?atlas?that?thehigh-efficient thin layer?scans(Crest?picture?in?the?right)
2.2 chrysanthemum cauliflower Colchicine Content after the different disposal mode
2.2.1 after the following NaCl with 10% of normal temperature handled, the cadmium yellow cauliflower Colchicine Content that calculates after high performance thin layer chromatography scanning was seen Fig. 3, Fig. 3 is that NaCl (10%) handles back cadmium yellow cauliflower Colchicine Content table.
Colchicin in the cadmium yellow cauliflower after handling with the 10%NaCl of normal temperature descends apparent in view at 0.0h～1.0h, but 1.0h～2.5h during this period of time the colchicin slippage diminish.The decline percentage of overall colchicin is about 61%.10%NaCl with normal temperature handles for the colchicin effect that reduces in the cadmium yellow cauliflower obvious.Find in the processing procedure that with the 10%NaCl processing cadmium yellow cauliflower of normal temperature, the processing time occurs wilting greater than 1.0h cadmium yellow cauliflower, has reduced the commodity value of cadmium yellow cauliflower.
2.2.2 after transferring pH12 to handle with NaOH under the normal temperature, the cadmium yellow cauliflower Colchicine Content that calculates after high performance thin layer chromatography scanning is seen Fig. 4, Fig. 4 handles cadmium yellow cauliflower Colchicine Content table afterwards for NaOH.
The variation of the decline percentage of the colchicin in the cadmium yellow cauliflower after transferring pH12 to handle with normal temperature NaOH is with the unanimity of handling with normal temperature 10%NaCl as a result.But the slippage of overall colchicin is more on the low side than normal temperature 10%NaCl processing.But normal temperature NaOH transfers pH12 processing day lily that its commodity value influence degree is lower than the processing with normal temperature NaCl, does not have significantly wilting of appearance behind the immersion 3.0h.See Fig. 5
Fig. 5 is cadmium yellow cauliflower Colchicine Content after NaOH transfers pH12 to handle, the three-dimensional collection of illustrative plates of efficient thin layer scanning, and the right of figure is the crest figure of colchicin.
Fig.5the colchicines content of fresh?day?lily?after?treated?by?NaOH(10％)，Three-dimensional?atlas?thatthe high-efficient?thin?layer?scans(Crest?picture?in?the?right)
2.2.3 after normal temperature was handled with 10% ethanol down, the cadmium yellow cauliflower Colchicine Content that calculates after high performance thin layer chromatography scanning was seen Fig. 6, Fig. 6 is that ethanol (10%) is handled back cadmium yellow cauliflower Colchicine Content table.
With 10% Ethanol Treatment cadmium yellow cauliflower, the percentage that Colchicine Content descends is irregular variation, and total decline percentage is lower than several processing modes in front, that is to say that the effect of handling back reduction colchicin is not too obvious.Do not occur wilting but in the processing procedure, do not destroy the commodity value of cadmium yellow cauliflower.
2.2.4 use H under the normal temperature
2After O handled, the cadmium yellow cauliflower Colchicine Content that calculates after high performance thin layer chromatography scanning was seen Fig. 7, and Fig. 7 is for using normal temperature H
2O handles back cadmium yellow cauliflower Colchicine Content table.
The percentage that descends with the cadmium yellow cauliflower Colchicine Content of water treatment is that effect is the poorest in all results, and the trend that increases one by one appears in the percentage that colchicin descends.The phenomenon of wilting does not appear in the cadmium yellow cauliflower in the processing procedure, but the processing time greater than 1.5h after the bud of cadmium yellow cauliflower can open the commodity value that has influenced the cadmium yellow cauliflower to a certain extent.
2.2.5 after handling with 10%NaCl under 0 ℃, the cadmium yellow cauliflower Colchicine Content that calculates after high performance thin layer chromatography scanning is seen Fig. 8, Fig. 8 is for handling back cadmium yellow cauliflower Colchicine Content table with NaCl (10%, 0 ℃).
Fig. 9 is cadmium yellow cauliflower Colchicine Content after 0 ℃ of 10%NaCl handles, the three-dimensional collection of illustrative plates of efficient thin layer scanning, and the right of figure is the crest figure of colchicin.
Fig.9?the?colchicines?content?of?fresh?day?lily?after?treated?by?NaCl(10％，0℃)Three-dimensional?atlas?that?the?high-efficient?thin?layer?scans(Crest?picture?in?theright)
After 0 ℃ 10%NaCl handled the cadmium yellow cauliflower, the percentage that Colchicine Content descends was identical with the results change trend that 10%NaCl under the normal temperature handles.Compare the percentage of colchicin decline on average about 52% with untreated sample.In processing procedure, the NaCl that the time ratio normal temperature of wilting appears in the cadmium yellow cauliflower handles and will prolong, and apparent in view wilting just occurs greater than 2.0h, and is less to the commodity value influence of cadmium yellow cauliflower less than the processing of 2.0h.
3 conclusions
3.1 cadmium yellow cauliflower different parts colchicin
In the cadmium yellow cauliflower, the different parts Colchicine Content of unit mass is followed successively by ovary, gynoecium, stamen, petal from high to low.And each several part Colchicine Content order is on the contrary in the unit mass cadmium yellow cauliflower.Colchicin is present in whole colored part in the cadmium yellow cauliflower, just the content of each part difference to some extent.Suggestion can be extractd the anthocaulus part that comprises ovary and gynoecium when eating the cadmium yellow cauliflower.Anthocaulus also can be extractd adding man-hour by factory, as a method that reduces colchicin, also can further process the extraction colchicin to the part of extracing simultaneously.
3.2 the comparison of different disposal mode
After normal temperature 10%NaCl and 0 ℃ of 10%NaCl handled the cadmium yellow cauliflower, the amount of colchicin wherein was the high variation that reduces again in low earlier back.The appearance of this situation may be that at first extraneous osmotic pressure is higher than cadmium yellow cauliflower cell, causes its cell dehydration, and intracellular liquid discharges to external environment, causes the petal of flower to tighten the tightr than in the past of parcel because of dehydration simultaneously.Because the osmotic pressure that closely causes 10%NaCl can not enter the interior and inner solution of petal of petal parcel changes, may cause that outside solution enters inside or can not diffuse out petal fast with the colchicin that the 10%NaCl that advances into wherein dissolves than the outer height of petal, and then cause elder generation's high situation in low back of Colchicine Content to occur.Concrete reason remains further to be studied.
After NaOH accent pH12 processing cadmium yellow cauliflower, it is the same that the appearance of the variation of the content of colchicin is handled the cadmium yellow cauliflower with normal temperature 10%NaCl, and its reason also may be identical.Variation for the day lily Colchicine Content after 10% the Ethanol Treatment is identical with the results change that 10%NaCl handles, and the reason of its appearance also may be identical.In addition might cause the concentration reduction relevant with ethanol is volatile.
After the cadmium yellow that the is soaked in water cauliflower, Colchicine Content is the variation that progressively reduces, and this may be owing to colchicin physical property soluble in water is relevant.Because the content of the colchicin in the external environment is low, causes the colchicin in the cadmium yellow cauliflower cell to spread to external environment.And the osmotic pressure of cell is higher than external environment, and the continuous imbibition of cell causes the bud of day lily open, makes more abundant that water contacts with day lily, is beneficial to colchicin and spreads to external environment.So the progressively phenomenon of reduction occurs.
Five kinds of processing modes, in general the treatment effect of 0 ℃ of 10%NaCl is better than other four kinds of modes.Normal temperature 10%NaCl handles, and in the percentage maximum that the 1.0h colchicin descends, day lily is wilted, and has destroyed the commodity value of cadmium yellow cauliflower.Basic identical with percentage and 0 ℃ of 10%NaCl treatment effect that NaOH transfers pH12 processing back colchicin to descend.From the angle of actual production, NaOH transfers the production cost of pH12 will be higher than 0 ℃ of 10%NaCl, and 0 ℃ of 10%NaCl can not pollute the cadmium yellow cauliflower.It is longer mainly to be with water treatment that colchicin reduces the too little and spent time of the amplitude of percentage, is unfavorable for production application.And 10% ethanol is not only volatile, the cost height, and the percentage amplitude that colchicin descends is also on the low side.
Claims (1)
1, a kind of method that reduces Colchicine Content in the cadmium yellow cauliflower, it is characterized in that adopting concentration is 10% NaCl solution, under 0 ℃ of condition, the cadmium yellow cauliflower is carried out 0.1～2 hour immersion treatment.
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| CNB2003101104832A CN100341422C (en) | 2003-11-03 | 2003-11-03 | Method for descreasing colchicin content of fresh day lily |
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| CNB2003101104832A CN100341422C (en) | 2003-11-03 | 2003-11-03 | Method for descreasing colchicin content of fresh day lily |
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| CN100341422C true CN100341422C (en) | 2007-10-10 |
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| CN103815212B (en) * | 2014-03-20 | 2015-09-02 | 齐鲁工业大学 | A kind of method reducing Colchicine Content in day lily |
| CN110419669A (en) * | 2019-08-10 | 2019-11-08 | 武汉轻工大学 | A kind of device and method that colchicin in hemerocallis is eliminated in scale |
| CN112823663A (en) * | 2019-11-21 | 2021-05-21 | 湖南有吉食品有限公司 | Daylily dish and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1188482A (en) * | 1995-06-27 | 1998-07-22 | 因迪纳有限公司 | Colchicine derivatives, use thereof and formulations containing them |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1188482A (en) * | 1995-06-27 | 1998-07-22 | 因迪纳有限公司 | Colchicine derivatives, use thereof and formulations containing them |
Non-Patent Citations (1)
| Title |
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| 秋水仙碱的研究进展 何红平，刘复初，中草药，第1998－10期 1998 * |
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