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Separation and purification method of crocin I monomer and crocin II monomer

A crocin, separation and purification technology, applied in chemical instruments and methods, organic chemistry, esterification saccharides and other directions, can solve problems such as being unfavorable for high-efficiency chromatographic continuous production, achieve convenient product quality, increase production costs, and facilitate control effect

Active Publication Date: 2014-03-26
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This technology focuses on the research of product purity detection, and the gradient is not conducive to the continuous production of high-efficiency chromatography

Method used

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  • Separation and purification method of crocin I monomer and crocin II monomer
  • Separation and purification method of crocin I monomer and crocin II monomer
  • Separation and purification method of crocin I monomer and crocin II monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 1) extract

[0047] Crush 10 g of saffron medicinal material into a coarse powder of 1-4 mm, add 0.5 L of ethanol solution with a concentration of 90% by volume, extract 3 times, each time for 2 hours, combine and filter the extracts, a total of 1500 mL;

[0048] 2) concentrated

[0049] Concentrate the extract obtained in step 1) at 60°C until alcohol-free to obtain 200 mL of concentrated solution;

[0050] 3) filter

[0051] Filter the 200mL concentrated solution obtained in step 2) with a 0.45μm filter membrane to obtain 210mL of the filtrate;

[0052] 4) HPLC preparation

[0053] The filler is C 18 chromatographic column, the column specification is 50cm×8cm;

[0054] The composition of the mobile phase is: acetonitrile-0.35% phosphoric acid aqueous solution (V / V=25:75)

[0055] The detection wavelength is 440nm, and it operates at room temperature;

[0056] Take the filtrate obtained in step 3) and inject the sample, the injection volume is 70mL / needle, carr...

Embodiment 2

[0070] 1) extract

[0071] Crush 10 g of saffron medicinal material into a coarse powder of 1-4 mm, add 0.5 L of ethanol solution with a concentration of 95% by volume, extract 3 times, each time for 2 hours, combine and filter the extracts, a total of 1500 mL;

[0072] 2) concentrated

[0073] Concentrate the extract obtained in step 1) at 60°C until alcohol-free to obtain 200 mL of the concentrate;

[0074] 3) filter

[0075] Filter the 200mL concentrated solution obtained in step 2) with a 0.45μm filter membrane to obtain 210mL of the filtrate;

[0076] 4) HPLC preparation

[0077] The filler is C 18 chromatographic column, the column specification is 50cm×8cm;

[0078] The composition of the mobile phase is: acetonitrile-0.35% phosphoric acid aqueous solution (V / V=25:75)

[0079] The detection wavelength is 440nm, and it operates at room temperature;

[0080] Take the filtrate obtained in step 3) and inject the sample, the injection volume is 70mL / needle, carry out ...

Embodiment 3

[0094] 1) extract

[0095] Crush 100 g of the saffron medicinal material into a coarse powder of 1-4 mm, add 8 L of ethanol solution with a concentration of 95% by volume, extract 3 times, each time for 2 hours, combine and filter the extracts, a total of 24 L;

[0096] 2) concentrated

[0097] Concentrate the extract obtained in step 1) at 60°C until alcohol-free to obtain 1.7L of concentrated solution;

[0098] 3) filter

[0099] Filter the 1.7L concentrated solution obtained in step 2) with a 0.45μm filter membrane to obtain 1.8L of the filtrate;

[0100] 4) HPLC preparation

[0101] The filler is C 18 chromatographic column, the column specification is 50cm×8cm;

[0102] The composition of the mobile phase is: acetonitrile-0.35% phosphoric acid aqueous solution (V / V=25:75)

[0103] The detection wavelength is 440nm, and it operates at room temperature;

[0104] Take the filtrate obtained in step 3) and inject the sample, the injection volume is 70mL / needle, carry ou...

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Abstract

The invention relates to a method capable of synchronously separating and purifying a crocin I monomer and a crocin II monomer, and belongs to the technical field of separation and purification for active ingredients of Chinese traditional medicines. The method comprises the following steps: taking dried stigmas of Crocus sativus as raw materials, performing 90-95% ethanol extraction, concentration, filter, efficient preparative liquid chromatography separation, product recovery and sephadex gel column chromatography to obtain the crocin I monomer and the crocin II monomer. By virtue of the optimum technique and parameter conditions, the content of the crocin I monomer and the crocin II monomer in the product is up to 99% above respectively; the method is stable in the whole technical process, convenient to operate, high in separation efficiency and low in cost, and can separate out and prepare the crocin I monomer and the crocin II monomer with high purity and large scale.

Description

technical field [0001] The invention relates to a method for preparing and separating plant compound monomers, in particular to a method for separating and purifying monomers of crocin I and crocin II from saffron, and belongs to the technical field of separation and purification of active ingredients of traditional Chinese medicines. Background technique [0002] Saffron (Stigma Croci), also known as saffron, saffron, English name: Saffron, is the stigma of Crocus sativus L., a plant of the family Iridaceae, and its native place is from the Mediterranean coast to the foothills of the Himalayas. According to the "Compendium of Materia Medica", saffron can "promote blood circulation, control depression, and treat palpitations". Therefore, Chinese medicine is used to treat cardiovascular diseases. At present, the main producing areas of saffron are Iran, Greece, Spain and other countries, and only a small amount is cultivated in my country. Due to its extremely low yield and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/06C07H1/08
Inventor 陈军白兰辉夏柯郭建华刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH
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