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Preparation method of high pure crocin and geniposide

A technology of saffron and geniposide, which is applied in chemical instruments and methods, preparation of sugar derivatives, separation/purification of carboxylic acid compounds, etc., can solve the problems of difficult to meet international product requirements, difficult to realize industrial production, and product recovery rate Low-level problems, achieve automation and operability, realize industrial scale-up, and achieve high-purity effects

Inactive Publication Date: 2015-05-06
SUZHOU QIUSHI HERBAL HEALTH TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Through long-term research, the current process of purifying gardenia yellow with macroporous resin technology is relatively mature, but the color price of the product of this process is generally only below 400, and it is difficult to meet the international product requirements
It is reported in the literature that various methods and steps such as silica gel column chromatography and reversed-phase silica gel column high-pressure preparation are used to further separate and purify saffron monomer, but the process steps are complicated, the product recovery rate is low, and the cost is high, so it is difficult to realize industrial production

Method used

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  • Preparation method of high pure crocin and geniposide
  • Preparation method of high pure crocin and geniposide
  • Preparation method of high pure crocin and geniposide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1 macroporous resin static adsorption performance investigation

[0022] Weigh 1 kg of gardenia medicinal herb pieces, beat into a coarse powder and pass through a 60-mesh sieve, soak in 40% ethanol overnight, reflux and extract twice, filter for 2 hours each time, and concentrate the filtrate under reduced pressure at 65°C until it has no alcohol smell. Each 1mL of liquid medicine is equivalent to 0.5g of crude drug, stored in a refrigerator at 4°C, and the extract is ready for use.

[0023] Chromatographic conditions: Cosmosil AR-II C 18 Chromatographic column (250mm×4.6mm, 5μm); mobile phase: methanol (A)-1% acetic acid aqueous solution (B), 0-4min, 20%A; 4-40min, 20%A-90%A; flow rate 1. OmL / min; detection wavelength 238nm, 440nm; column temperature: room temperature; injection volume 20 μL.

[0024] Weigh each type of resin equivalent to 1.00g of dry weight, place them in ten 50mL Erlenmeyer flasks with stoppers, add 50mL of extract (0.3g crude drug / ml)...

Embodiment 2

[0033] The refining of embodiment 2 gardenia extract

[0034]Weigh 80kg gardenia medicinal material, soak it in 40% ethanol overnight, reflux extraction twice, each time for 2 hours, filter, combine the filtrate, rotary evaporate to no alcohol smell, adjust the medicinal solution so that each 1ml medicinal solution is equivalent to 0.5g crude drug, spare. Weigh 120kg (wet weight) of LX60 resin, put it into a stainless steel column (300×2300cm), the column volume is 150L, ​​load the sample, after absorbing for 1h, first remove impurities with 300L of water and 300L of 10% ethanol, wash with 360L of 30% ethanol Remove geniposide, then use 360L of 75% ethanol to elute saffron, and finally use 95% ethanol to regenerate the resin, the flow rate is 150-200L / h, respectively concentrate and evaporate the 30% and 75% ethanol to dryness, and then obtain geniposide Refined extract (gardeniposide content 83.38%) 2.76kg, yield 3.45%; gardenia yellow refined extract (color value 390, where...

Embodiment 3

[0036] Embodiment 3 middle pressure column prepares crocin

[0037] Take 1 g of the refined extract of Jasmina Jasminoides obtained in Example 2, dissolve it with 10 ml of 40% methanol, separate it with a medium-pressure column system, pack it into a column (150 × 25 mm i.d.) with C18 reversed-phase silica gel, load the sample liquid, and use 43 % Methanol 10L elution, flow rate 50mL / min, UV 328nm and 440nm detection, collect geniposide and chlorogenic acid fractions; then elute with methanol 2L, collect saffron fractions; Concentrate under pressure, dry, respectively get geniposide 0.24g, yield 2.4%; Chlorogenic acid component 1.65g, yield 16.5%; Crocin 8.02g, yield 80.2% (color value 756, wherein crocin content 61.78% %).

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Abstract

The invention discloses a preparation method of high pure crocin and geniposide. The preparation method comprises following main steps: selecting raw materials of gardenia ellis plants, extracting with water or an alcohol-water mixed solution, merging the extracting solutions, condensing, filtering, subjecting the obtained extracting solution to an adsorption treatment by macroporous resin, then performing gradient elution with a ethanol-water mixed solution, obtaining geniposide and gardenia yellow refined extracts; subjecting the geniposide refined extract to a recrystallization treatment with ethyl acetate so as to obtain the geniposide product; subjecting the gardenia yellow refined extract to go through column chromatography, which has been pressurized and stuffed with modified silica gel, to separate, and obtaining the high pure crocin product (color value larger than 600) and a chlorogenic acid component. The products have the advantages of high purity, simple technology, strong operability and convenience for automation, comprehensive utilization of the plant resources is achieved, the solvent is convenient to recycle and reuse, and the preparation method is easy to apply to the industrial amplification.

Description

technical field [0001] The invention relates to a preparation method of high-purity saffron and geniposide, which belongs to the field of medicine and health food. technical background [0002] Crocin is a kind of precious water-soluble carotene derivatives. It is the main active ingredient in the precious medicinal material saffron. It has various functions such as anti-oxidation and anti-tumor. It is also used in health food as a natural edible yellow pigment. In recent years, crocin components (called gardenia yellow) have also been found in gardenia, a commonly used traditional Chinese medicine in China, so the extraction of valuable crocin from gardenia has become a research hotspot. Gardenia mainly contains geniposide, crocin, chlorogenic acid and other components, among which geniposide is one of the effective components of gardenia for clearing heat and detoxifying, and can also be converted into food coloring gardenia by combining with certain amino acids Blue and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C57/13C07C51/42C07H17/04C07H1/08C09B61/00
Inventor 刘江云周胜冯建勇李贺然杨世林
Owner SUZHOU QIUSHI HERBAL HEALTH TECH CO LTD
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