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Method used for preparing high-purity gardenoside and crocin from gardenia jasminoides ellis

A technology of crocin and geniposide, which is applied in the fields of food and medicine, can solve the problems of being unsuitable for industrialized production, low possibility of industrialization, and long production cycle, so as to improve the comprehensive utilization rate, improve the first pass rate, and shorten the production cycle Effect

Inactive Publication Date: 2014-07-30
云南云药医药研究有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing crocin preparation methods mainly include solvent extraction method and macroporous adsorption resin method, such as Chinese patent (application number 201110417356.1) "a method for preparing crocetin and crocetin", which uses ethanol to prepare Gardenia jasminoides under ultrasonic conditions Fruit extract, concentrated to obtain extract, dissolved in water, added an equal volume of n-butanol for extraction 3 times, concentrated under reduced pressure of n-butanol layer to obtain extract, dissolved with 20-30 times of water, then added polyethylene glycol, followed by Use petroleum ether to extract small polar impurities, and ethyl acetate to obtain crocetin; the aqueous layer in the extract is precipitated with ethyl acetate-ethanol mixture, filtered, washed, dissolved in water, and the solution is passed through ethyl acetate- N-butanol is extracted multiple times to obtain saccharin. This process requires multiple extractions, the production cycle is long, the amount of solvent used is large, and n-butanol has great environmental pollution, high solubility in water, difficult to recycle and reuse, and poor economy
Chinese patent (Application No. 201110361410.5) "A method of producing saffron with a purity of more than 95% using gardenia as raw material", which is extracted by percolation with water at room temperature, and removed by microfiltration to remove impurities such as solid particles and pectin, as well as microorganisms such as bacteria , and then pressurized multi-section continuous adsorption by macroporous adsorption resin, and then refined by multi-section adsorption of C18 column. Although crocin with higher purity can be obtained, the process is cumbersome and the production cycle is long, so it is not suitable for industrialized production; another example is the Chinese patent (Application No. 201010130269.3) "A process for extracting α-crocin from gardenia", including degreasing, water extraction, polyamide resin tannin removal, macroporous adsorption resin adsorption, hot water and propylene glycol recrystallization, polyamide in the process Resin and tannin undergo dead adsorption, which cannot be recycled, and the cost is high; propylene glycol is flammable and highly toxic, and the possibility of industrialization is small

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] a. Take 100 kg of gardenia, crush it to coarse powder, add 15 times the mass percentage of 60% ethanol solution, extract 2 times under the condition of 40 ℃, each extraction time is 1.5 hours, combine the extracts and wait for the extracts Cool to room temperature, add 1 part by weight of activated carbon per 100 parts by volume of the extract, stir, centrifuge at 3000r / min for 5 minutes, and filter to obtain a clear extract, which is concentrated under reduced pressure to obtain an extract;

[0026] b. Dissolve the extract in water, adjust the pH to 8, adopt dynamic adsorption method, load the sample on the MCI GEL CHP20P chromatography column, the sample concentration of the sample is 20mg / ml, the flow rate is 200ml / min, the sample is finished Then, let it stand for 2 hours, first eluting with 4 times BV of water, then eluting with 7 times BV of 20% by mass concentration of ethanol solution to obtain the eluate containing geniposide, and then use 6 times of BV Ethanol so...

Embodiment 2

[0029] a. Take 150 kg of gardenia, crush it to coarse powder, add 7 times the mass percentage of 80% methanol solution, extract 3 times under the condition of 60 ℃, each extraction time is 1 hour, combine the extracts and wait for the extracts Cool to room temperature, add 3 parts by weight of diatomaceous earth per 100 parts by volume of the extract, stir, centrifuge at 2000r / min for 5 minutes, and filter to obtain a clear extract, which is concentrated under reduced pressure to obtain an extract;

[0030] b. Dissolve the extract in water, adjust the pH to 8.2, use dynamic adsorption method, load the sample on the MCI GEL CHP20Y chromatography column, the sample concentration of the sample is 15mg / ml, the flow rate is 50ml / min, the sample is finished Then, let it stand for 2 hours, first eluting with 4 times BV of water, and then eluting with 6 times BV of 15% by mass concentration of ethanol solution to obtain the eluate containing geniposide, and then use 5 times of BV Ethanol...

Embodiment 3

[0033] a. Take 150 kg of gardenia, crush it to coarse powder, add 20 times the weight of water, extract once at 70°C for 2 hours, combine the extracts, wait until the extracts are cooled to room temperature, according to 100 volumes Add 0.1 parts by weight of activated carbon to a portion of the extract, stir, centrifuge at 4000r / min for 5 minutes, and filter to obtain a clear extract, which is concentrated under reduced pressure to obtain an extract;

[0034] b. Dissolve the extract in water, adjust the pH to 8, adopt the dynamic adsorption method, and load the sample on the MCI GEL CHP20SS chromatography column. The sample concentration of the sample is 25mg / ml, the flow rate is 500ml / min, and the sample is completed Then, let it stand for 2 hours, eluted with 6 times BV of water, and then eluted with 5 times BV of 25% by mass concentration in ethanol to obtain the eluate containing geniposide, and then use 5 times of BV. Ethanol solution with 75% mass percentage concentration ...

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PUM

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Abstract

The invention relates to a method used for preparing high-purity gardenoside and crocin from gardenia jasminoides ellis, and belongs to the technical field of food and medicine. The method comprises following steps: a, gardenia jasminoides ellis is collected, and is extracted at a temperature of 40 to 70 DEG C, an obtained extracted solution is cooled to room temperature, active carbon or diatomite is added, and an obtained mixture is filtered and concentrated so as to obtain an extractum; b, the extractum is dissolved in water, pH value is adjusted to 7.8 to 9, an obtained solution is processes by using a MCI gel chromatographic column, is allowed to stand, and is subjected to elution with water, an obtained mixed material is subjected to elution with an ethanol solution with a mass percent concentration of 5 to 30% so as to obtain an eluent containing gardenoside, and an obtained product is subjected to elution with an ethanol solution with a mass percent concentration of 60 to 90% so as to obtain an eluent containing crocin; c, the eluent containing gardenoside is concentrated, is dissolved in ethyl acetate or absolute ethyl alcohol, and is subjected to crystallization so as to obtain high-purity gardenoside; the eluent containing crocin is concentrated and dried so as to obtain high-purity crocin. Beneficial effect of the method is that: purity of gardenoside and purity of crocin are both high.

Description

Technical field [0001] The invention belongs to the technical field of food and medicine, and specifically relates to a method for preparing high-purity geniposide and crocin from gardenia. Background technique [0002] Gardenia (Gardenia jasminoides Ellis), also known as yellow gardenia, mountain gardenia, and white toad, is the fruit of Rubiaceae gardenia, mainly distributed in Zhejiang, Jiangxi, Hunan, Fujian and other places. It has extensive resources and is issued by the Ministry of Health. The first batch of medicine and food resources. It has been recorded in "Compendium of Materia Medica" that gardenia enters the heart, liver, lungs, and stomach meridians, can clear away heat, purify fire, and cool blood. It has the effects of protecting liver, promoting choleretics, reducing blood pressure, sedation, hemostasis, and reducing swelling. It mainly contains Various active ingredients such as gardenia oil, geniposide, gardenia yellow pigment and chlorogenic acid. Geniposid...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08C07C57/13C07C51/42C09B61/00
Inventor 周志宏刘菲菲张宝洪王兵
Owner 云南云药医药研究有限公司
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