Method for preparing crocetin from jasmine

A technology of crocetin and gardenia, which is applied in the field of biological enzymolysis and multiple resin columns to prepare crocetin, can solve the problems of non-specificity, achieve mild reaction, easy control of conditions, and product purity high effect

Inactive Publication Date: 2011-02-16
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Existing techniques for extracting saffron from gardenia include: Chinese patent (application number 94111504) "a method for extracting crocin f

Method used

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  • Method for preparing crocetin from jasmine

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Effect test

Embodiment 1

[0023] Pulverize the gardenia, take 1kg and mix it with ph4 hydrochloric acid aqueous solution, add 3g β-glucanosidase and mix well for enzymolysis at 40°C for 3 days, then put the enzymolysis raw materials into the extraction container, add 8kgph11 sodium hydroxide aqueous solution, stir and extract 2 hours, extract 3 times, add 500ml of D382 anion resin to neutralize the extraction solution with hydrochloric acid, and then add 500ml of D382 anion resin for adsorption, the resin column sugar reaction is negative, and then use 450ml of 10.1% sodium hydroxide solution to elute the active ingredients, and add 300ml of 001×7 cationic resin to the eluent Column desalination, add 100ml of AB-8 macroporous resin to the lowering solution for adsorption, elute with 500ml of 80% ethanol solution, recover ethanol under reduced pressure, place crystals, filter out the crystals, dissolve in anhydrous ethanol for recrystallization, and dry to obtain saffron Acid product (yield 83%), content...

Embodiment 2

[0025] Pulverize the gardenia, take 1kg and mix it with ph6 sulfuric acid aqueous solution, add 2g β-glucanase and 6g amylase and mix for 4 days at 30°C for enzymolysis, and then put the enzymolysis raw materials into the extraction container, add 13kgph9 sodium hydroxide The aqueous solution was stirred and extracted for 5 hours, extracted twice, the extract was adjusted to neutrality with hydrochloric acid, and 500ml of D392 anion resin was added for adsorption, the resin was washed with water and the column sugar reaction was negative, and then 300ml of 1% sodium hydroxide solution was used to elute the active ingredients, and 300ml of 001×7 was added to the eluent. The cation resin column was desalted, and 100ml of ADS-4 macroporous resin was added to the beating solution for adsorption, eluted with 800ml of 60% ethanol solution, the ethanol was recovered under reduced pressure, crystallized, and the crystallized product was filtered out, dissolved in anhydrous ethanol under...

Embodiment 3

[0027] Grind the gardenia to 1kg, mix it with a pH5 citric acid aqueous solution, add 1g β-glucanase and 7g cellulase and mix for 5 days at 30°C for enzymatic hydrolysis, then put the enzymolysis raw materials into the extraction container, add 13kgph11 The aqueous sodium hydroxide solution was stirred and extracted for 5 hours, extracted twice, the extract was adjusted to neutrality with hydrochloric acid, and 500ml of D280 anion resin was added for adsorption, the resin was washed with water and the sugar reaction was negative, and then 350ml of 0.4% sodium hydroxide solution was used to elute the active ingredients. Add 300ml of 001×7 cation resin column for desalination, add 100ml of LSA-7 macroporous resin to the beating solution for adsorption, elute with 600ml of 70% ethanol solution, recover the eluate under reduced pressure, stand for crystallization, filter out the crystals, dry Ethanol refluxed, dissolved and recrystallized, and dried to obtain a safranic acid produc...

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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: [0001] The invention relates to a method for preparing saffronic acid from gardenia, in particular to a method for preparing saffronic acid by combining biological enzymolysis and multiple resin columns. Background technique: [0002] Saffron acid is also called saffron acid, crocetin, trans-crocetin α-Crocetin. [0003] Molecular formula: C 20 H 24 O 4 ; [0004] Molecular weight: 328.39 [0005] Molecular structural formula: [0006] [0007] Physical and chemical properties: brick red orthorhombic crystal (acetic anhydride) melting point 285 ℃. Soluble in pyridine and very dilute sodium hydroxide solution, very slightly soluble in water and common organic solvents except pyridine and similar organic bases. [0008] Saffron acid has hypolipidemic and choleretic effects. [0009] At present, the extraction process of saffron acid is mainly extracted from saffron or gardenia. Due to the high price of saffron, the preparation from gardenia is the m...

Claims

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Application Information

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IPC IPC(8): C07C57/13C12P7/44C07C51/47
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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