CN101974571A - Method for preparing crocetin from jasmine - Google Patents
Method for preparing crocetin from jasmine Download PDFInfo
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- CN101974571A CN101974571A CN2010102357138A CN201010235713A CN101974571A CN 101974571 A CN101974571 A CN 101974571A CN 2010102357138 A CN2010102357138 A CN 2010102357138A CN 201010235713 A CN201010235713 A CN 201010235713A CN 101974571 A CN101974571 A CN 101974571A
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Abstract
The invention relates to a method for preparing crocetin from jasmine, comprising the following steps: grinding the raw material jasmine, moistening the ground jasmine with acidulous water, adding bio-enzyme for enzymolysis at 30-40 DEG C for 3-5d, extracting the enzymolysis raw material with sodium hydroxide aqueous solution with pH value of 9-11, adjusting the pH value of the extract liquor to be neutral, adding anion exchange resins for adsorption, eluting the active ingredients with 0.1-1% of alkali liquor, adsorbing the eluent with macroporous resins after desalting the eluent with cation exchange resins, concentrating and crystallizing the eluent and recrystallizing ethanol. Used for producing crocetin, the method is low in cost and simple and easily operated in process. The method has high specificity.
Description
Technical field:
The present invention relates to a kind of method that from cape jasmine, prepares bayer acid, particularly relate to the method that a kind of biological enzymolysis and the coupling of various kinds of resin post prepare bayer acid.
Background technology:
Bayer acid is crocetin again, crocetin, crocetin α-Crocetin.
Molecular formula: C
20H
24O
4
Molecular weight: 328.39
Molecular structural formula:
Physico-chemical property: 285 ℃ of brick-red quadrature crystallization (aceticanhydride) fusing points.Be dissolved in pyridine and very rare sodium hydroxide solution, the atomic water-soluble and organic solvent commonly used except that pyridine and similar organic bases.
Bayer acid has reducing blood-fat, choleretic effect.
At present, the bayer acid extraction process is mainly extracted from Stigma Croci or cape jasmine, because the Stigma Croci price is higher, preparation is the bayer acid main source from cape jasmine.The existing technology of extracting bayer acid from cape jasmine has: Chinese patent (application number 94111504) " a kind of extracting method of crocin of anti-angiocardiopathy ", the method of this patent disclosure is that earlier preparation Stigma Croci glycosides adds the sour water bath water that boils again and separates and make bayer acid, does not possess specificity.
Summary of the invention:
The objective of the invention is for a kind of specificity technology for preparing bayer acid is provided, this method is simple to operate, can reduce production costs save energy.
Technical solution of the present invention is:
A kind of method that from cape jasmine, prepares bayer acid, it is characterized in that comprising following steps: mix wet with the sour water of ph4-6 to the cape jasmine raw material pulverizing, added the biological enzyme mixing 30-40 ℃ of enzymolysis 3-5 days, the enzymolysis raw material drops into extraction vessel again, the aqueous sodium hydroxide solution that adds 8-20 times of ph9-11 stirs and extracted 1-5 hour, extract 1-3 time, extracting solution is regulated the neutral resin anion(R.A) absorption that adds, wash sugared reaction negative, 6-9BV sodium hydroxide solution wash-out effective constituent, elutriant adds the cationic resin column desalination, and following fluid injection adds macroporous resin adsorption again, 5-8BV ethanolic soln wash-out, the reclaim under reduced pressure elutriant, place crystallization, leach crystallisate dehydrated alcohol backflow dissolving-recrystallization, be drying to obtain.
Described biological enzyme is one or more in beta-glucan glycosides enzyme, amylase and the Carboxymethylcellulose enzyme, and add-on is the 3-8 ‰ of raw material weight.
A kind of among the optional D382 of described resin anion(R.A), D392 or the D280, resin cation (R.C.) is 001 * 7, a kind of among the optional AB-8 of macroporous resin, ADS-4 or the LSA-7.
Described sodium hydroxide elute soln concentration is 0.1-1%.
Described ethanol eluate concentration is 60-80%.
Advantage of the present invention is:
1) the biological enzymolysis condition is easy to control, reaction temperature and, energy consumption is low.
2) ion exchange resin and macroporous resin coupling, purification effect is good, the product purity height.
3) whole technology is simple to operation, and the organic reagent consumption is few, is fit to preparation of industrialization.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment:
Embodiment:
Embodiment 1:
Cape jasmine is pulverized, getting 1kg mixes wet with the aqueous hydrochloric acid of ph4, added 40 ℃ of enzymolysis of 3g beta-glucan glycosides enzyme mixing 3 days, the enzymolysis raw material drops into extraction vessel again, the aqueous sodium hydroxide solution that adds 8kgph11 stirs and extracted 2 hours, extract 3 times, extracting solution hydrochloric acid is regulated the absorption of the neutral 500mlD382 of adding resin anion(R.A), washed resin post sugar reaction negative, use 450m10.1% sodium hydroxide solution wash-out effective constituent again, elutriant adds 300ml001 * 7 cationic resin column desalinations, and following fluid injection adds the 100mlAB-8 macroporous resin adsorption again, with 500ml80% ethanolic soln wash-out, decompression recycling ethanol, place crystallization, leach crystallisate, dehydrated alcohol backflow dissolving-recrystallization, dry bayer acid product (yield 83%), the content 98.2% (high performance liquid phase survey) of getting.
Embodiment 2:
Cape jasmine is pulverized, getting 1kg mixes wet with the aqueous sulfuric acid of ph6, added 2g beta-glucan glycosides enzyme and 30 ℃ of enzymolysis of 6g amylase mixing 4 days, the enzymolysis raw material drops into extraction vessel again, the aqueous sodium hydroxide solution that adds 13kgph9 stirs and extracted 5 hours, extract 2 times, extracting solution hydrochloric acid is regulated the absorption of the neutral 500ml of adding D392 resin anion(R.A), washed resin post sugar reaction negative, use 300ml1% sodium hydroxide solution wash-out effective constituent again, elutriant adds 300ml001 * 7 cationic resin column desalinations, and following fluid injection adds 100ml ADS-4 macroporous resin adsorption again, with 800ml60% ethanolic soln wash-out, decompression recycling ethanol, place crystallization, leach crystallisate, dehydrated alcohol backflow dissolving-recrystallization, dry bayer acid product (yield 80%), the content 98.5% (high performance liquid phase survey) of getting.
Embodiment 3:
Cape jasmine is crushed to, getting 1kg mixes wet with the aqueous citric acid solution of ph5, added 1g beta-glucan glycosides enzyme and 30 ℃ of enzymolysis of 7g cellulase mixing 5 days, the enzymolysis raw material drops into extraction vessel again, the aqueous sodium hydroxide solution that adds 13kgph11 stirs and extracted 5 hours, extract 2 times, extracting solution hydrochloric acid is regulated the absorption of the neutral 500ml of adding D280 resin anion(R.A), washed resin post sugar reaction negative, use 350ml0.4% sodium hydroxide solution wash-out effective constituent again, elutriant adds 300ml001 * 7 cationic resin column desalinations, and following fluid injection adds 100ml LSA-7 macroporous resin adsorption again, with 600ml70% ethanolic soln wash-out, the reclaim under reduced pressure elutriant, place crystallization, leach crystallisate, dehydrated alcohol backflow dissolving-recrystallization, dry bayer acid product (yield 78%), the content 99% (high performance liquid phase survey) of getting.
Embodiment 4:
Cape jasmine is crushed to, getting 5kg mixes wet with the aqueous hydrochloric acid of ph5, added 40 ℃ of enzymolysis of 5g beta-glucan glycosides enzyme mixing 5 days, the enzymolysis raw material drops into extraction vessel again, the aqueous sodium hydroxide solution that adds 50kgph11 stirs and extracted 1 hour, extract 3 times, extracting solution hydrochloric acid is regulated the absorption of the neutral 2.5LD382 of adding resin anion(R.A), washed resin post sugar reaction negative, use 1.8L0.2% sodium hydroxide solution wash-out effective constituent again, elutriant adds 1.5L001 * 7 cationic resin column desalinations, and following fluid injection adds the 500mlAB-8 macroporous resin adsorption again, with 3L70% ethanolic soln wash-out, the reclaim under reduced pressure elutriant, place crystallization, leach crystallisate, dehydrated alcohol backflow dissolving-recrystallization, dry bayer acid product (yield 75%), the content 98.2% (high performance liquid phase survey) of getting.
Embodiment 5:
Cape jasmine is crushed to, getting 10kg mixes wet with the aqueous sulfuric acid of ph5, added 20g beta-glucan glycosides enzyme and 30 ℃ of enzymolysis of 50g cellulase mixing 4 days, the enzymolysis raw material drops into extraction vessel again, the aqueous sodium hydroxide solution that adds 80kgph10 stirs and extracted 2 hours, extract 3 times, extracting solution hydrochloric acid is regulated the absorption of the neutral 5LD280 of adding resin anion(R.A), washed resin post sugar reaction negative, use 4.5L0.1% sodium hydroxide solution wash-out effective constituent again, elutriant adds 3L001 * 7 cationic resin column desalinations, and following fluid injection adds the 1L1AB-8 macroporous resin adsorption again, with 7L70% ethanolic soln wash-out, the reclaim under reduced pressure elutriant, place crystallization, leach crystallisate, dehydrated alcohol backflow dissolving-recrystallization, dry bayer acid product (yield 75%), the content 98% (high performance liquid phase survey) of getting.
Claims (5)
1. method that from cape jasmine, prepares bayer acid, it is characterized in that comprising following steps: mix wet with the sour water of ph4-6 to the cape jasmine raw material pulverizing, added the biological enzyme mixing 3040 ℃ of enzymolysis 3-5 days, the enzymolysis raw material drops into extraction vessel again, the aqueous sodium hydroxide solution that adds 8-20 times of ph9-11 stirs and extracted 1-5 hour, extract 1-3 time, extracting solution is regulated the neutral resin anion(R.A) absorption that adds, wash sugared reaction negative, 6-9BV sodium hydroxide solution wash-out effective constituent, elutriant adds the cationic resin column desalination, and following fluid injection adds macroporous resin adsorption again, 5-8BV ethanolic soln wash-out, the reclaim under reduced pressure elutriant, place crystallization, leach crystallisate dehydrated alcohol backflow dissolving-recrystallization, be drying to obtain.
2. the method for preparing bayer acid according to claim 1 from cape jasmine is characterized in that described biological enzyme is one or more in beta-glucan glycosides enzyme, amylase and the Carboxymethylcellulose enzyme, and add-on is the 3-8 ‰ of raw material weight.
3. the method for preparing bayer acid according to claim 1 from cape jasmine is characterized in that a kind of among the optional D382 of described resin anion(R.A), D392 or the D280, and resin cation (R.C.) is 001 * 7, a kind of among the optional AB-8 of macroporous resin, ADS-4 or the LSA-7.
4. the method for preparing bayer acid according to claim 1 from cape jasmine is characterized in that described sodium hydroxide elute soln concentration is 0.1-1%.
5. the method for preparing bayer acid according to claim 1 from cape jasmine is characterized in that described ethanol eluate concentration is 60-80%.
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| CN2010102357138A CN101974571A (en) | 2010-07-26 | 2010-07-26 | Method for preparing crocetin from jasmine |
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| CN2010102357138A CN101974571A (en) | 2010-07-26 | 2010-07-26 | Method for preparing crocetin from jasmine |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073417A (en) * | 2013-03-04 | 2013-05-01 | 苏州衷中医药科技有限公司 | Preparation method for high-purity trans-crocetin |
| CN103183603A (en) * | 2011-12-30 | 2013-07-03 | 江苏天晟药业有限公司 | Crocetin organic amine salt and preparation method thereof |
| CN103539657A (en) * | 2013-10-24 | 2014-01-29 | 陕西源邦生物技术有限公司 | Method for preparing crocetin from cape jasmine |
| CN103641705A (en) * | 2013-12-02 | 2014-03-19 | 威海东宝制药有限公司 | Method for extracting crocetin from gardenia fruit |
| US20140141082A1 (en) * | 2012-11-16 | 2014-05-22 | Song Gao | Compositions Containing Enriched Natural Crocin and/or Crocetin, and Their Therapeutic or Nutraceutical Uses |
| CN104435237A (en) * | 2014-12-17 | 2015-03-25 | 鼎正动物药业（天津）有限公司 | Cape jasmine fruit oral solution and preparation method thereof |
| CN105063107A (en) * | 2015-08-31 | 2015-11-18 | 桂林茗兴生物科技有限公司 | Method for preparing crocetin through gardenias |
| CN109400660A (en) * | 2018-11-19 | 2019-03-01 | 江苏史蒂文生物科技有限公司 | The crocin standard items and preparation method thereof prepared from cape jasmine using new packing |
-
2010
- 2010-07-26 CN CN2010102357138A patent/CN101974571A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103183603A (en) * | 2011-12-30 | 2013-07-03 | 江苏天晟药业有限公司 | Crocetin organic amine salt and preparation method thereof |
| US9211298B2 (en) * | 2012-11-16 | 2015-12-15 | Song Gao | Compositions containing enriched natural crocin and/or crocetin, and their therapeutic or nutraceutical uses |
| US20140141082A1 (en) * | 2012-11-16 | 2014-05-22 | Song Gao | Compositions Containing Enriched Natural Crocin and/or Crocetin, and Their Therapeutic or Nutraceutical Uses |
| CN103073417A (en) * | 2013-03-04 | 2013-05-01 | 苏州衷中医药科技有限公司 | Preparation method for high-purity trans-crocetin |
| CN103073417B (en) * | 2013-03-04 | 2015-09-02 | 苏州衷中医药科技有限公司 | The preparation method of high-purity trans-crocetin |
| CN103539657B (en) * | 2013-10-24 | 2015-04-29 | 陕西源邦生物技术有限公司 | Method for preparing crocetin from cape jasmine |
| CN103539657A (en) * | 2013-10-24 | 2014-01-29 | 陕西源邦生物技术有限公司 | Method for preparing crocetin from cape jasmine |
| CN103641705A (en) * | 2013-12-02 | 2014-03-19 | 威海东宝制药有限公司 | Method for extracting crocetin from gardenia fruit |
| CN104435237A (en) * | 2014-12-17 | 2015-03-25 | 鼎正动物药业（天津）有限公司 | Cape jasmine fruit oral solution and preparation method thereof |
| CN105063107A (en) * | 2015-08-31 | 2015-11-18 | 桂林茗兴生物科技有限公司 | Method for preparing crocetin through gardenias |
| CN105063107B (en) * | 2015-08-31 | 2019-03-05 | 桂林三叶生物科技有限责任公司 | A method of preparing bayer acid from cape jasmine |
| CN109400660A (en) * | 2018-11-19 | 2019-03-01 | 江苏史蒂文生物科技有限公司 | The crocin standard items and preparation method thereof prepared from cape jasmine using new packing |
| CN109400660B (en) * | 2018-11-19 | 2021-11-09 | 江苏史蒂文生物科技有限公司 | Crocin standard prepared from fructus Gardeniae by using novel filler, and its preparation method |
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Application publication date: 20110216 |
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