Extraction method of crocin I

An extraction method, crocin technology, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve problems such as difficulty in obtaining high-purity crystals and large degree of mixing

Active Publication Date: 2015-12-09
HENAN ZHONGDA HENGYUAN BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the strong hydrophilicity of crocin I, it is more difficult to obtain high-purity crystals than other ingredients. The relevant materials and literatures known at present and the purity of products known in the market are mostly around 50%. The mixing degree of glycoside components is relatively large, and the color value is basically below 600

Method used

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  • Extraction method of crocin I
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  • Extraction method of crocin I

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1 Extraction of Crocetin I

[0048] The dried gardenia fruit is pulverized to 10-20 mesh by a rotary blade pulverizer, 100 kg of the pulverized raw material is taken, 60% ethanol solution is added, and extracted three times at 30°C. After the extracts were combined, they were concentrated under vacuum and reduced pressure until the ethanol content of the feed liquid was less than 2%, and cooled to obtain 27Kg of the feed liquid.

[0049] Add 4.5 times deionized water to dilute the feed solution and filter, and the obtained filtrate is adsorbed by the macroporous adsorption resin HPD100, and the resin bed is washed with 5 times the volume of the resin. The analysis was carried out with 75% ethanol, and the obtained analysis solution was concentrated under reduced pressure to an ethanol content of less than 2% to obtain 5 kg of concentrated solution.

[0050] The obtained analytical material concentrate is diluted 2 times with 30% ethanol, and then subjected to medium p...

Embodiment 2

[0052] Example 2 Extraction of Crocetin I

[0053] The dried gardenia fruit is pulverized to 10-20 mesh by a rotary vane pulverizer, 100 kg of the pulverized raw material is taken, 70% ethanol solution is added, and extracted three times at 25°C. After the extracts are combined, they are concentrated under vacuum and reduced pressure until the ethanol content of the feed liquid is less than 2%, and cooled to obtain 28Kg of the feed liquid.

[0054] Add 4.5 times deionized water to dilute the feed solution and filter, and the obtained filtrate is adsorbed by the macroporous adsorption resin HPD300, and the resin bed is washed with 5 times the volume of the resin. The analysis was carried out with 75% ethanol, and the obtained analysis solution was concentrated under reduced pressure to an ethanol content of less than 2% to obtain 4.8 kg of concentrated solution.

[0055] The obtained analytical material concentrate was diluted 2 times with 45% ethanol, and then subjected to medium-pr...

Embodiment 3

[0057] Example 3 Extraction of Crocetin I

[0058] The dried gardenia fruit is crushed to 10-20 mesh by a rotary vane crusher, 100 kg of the crushed raw material is taken, 65% ethanol solution is added, and extracted three times at 20°C. After the extracts are combined, they are concentrated under vacuum and reduced pressure until the ethanol content of the feed liquid is less than 2%, and then cooled to obtain 35Kg of the feed liquid.

[0059] Add 4.5 times deionized water to dilute the feed solution and filter, and the obtained filtrate is adsorbed by the macroporous adsorption resin HPD300, and the resin bed is washed with 5 times the volume of the resin. The analysis was carried out with 75% ethanol, and the obtained analysis solution was concentrated under reduced pressure to an ethanol content of less than 2% to obtain 5.6 kg of concentrated solution.

[0060] The obtained analytical material concentrate was diluted 2 times with 40% ethanol, and then subjected to medium-pressu...

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Abstract

The invention relates to the technical fields of separation and purification of medicines and especially relates to an extraction method of crocin I. The extraction method includes following steps: 1) performing alcohol-extraction to medicinal parts of a plant containing the crocin I to obtain an extract liquid; 2) performing adsorption and separation to the extract liquid to prepare a first intermediate; 3) purifying the first intermediate by a medium-pressure chromatographic system to obtain a second intermediate, wherein a chromatographic agent in the medium-pressure chromatographic system is a polystyrene-type high-molecular macroporous polymer material and a mobile phase is an ethanol aqueous solution; and 4) crystallizing the second intermediate to obtain the crocin I. The extraction method is used for preparing a crocin I crystal being high in purity and color value, of which the purity can reach more than 95% and the color value can reach more than 950.

Description

Technical field [0001] The present invention relates to the technical field of drug separation and purification, in particular to a method for extracting crocin I. Background technique [0002] Crocusin is the main medicinal component of the traditional Chinese medicine crocus saffron. It is a sugar ester formed by the combination of crocetic acid and different sugar groups, mainly including crocin I and crocin II. The content of crocin I and crocin II in saffron from different producing areas is between 4.6%-11.0% and 1.1%-4.5%, respectively. Crocetin compounds have a wide range of pharmacological activities, such as hypolipidemic effect, antioxidant activity, myocardial damage repair, etc., and have good application prospects. Saffron is a very expensive spice, and its price in the international market is about 2,000 to 4,000 US dollars / kg, which is known as "plant gold". At present, about 70% of the saffron in the international market is produced in Iran, and other European ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/06C07H1/08
Inventor 文雁君李林正李宏龙章文晋李轩
Owner HENAN ZHONGDA HENGYUAN BIOTECH CO LTD
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