Method for preparing periplogenin through enzymatic hydrolysis

A technology of salivarius and aglycone, which is applied in the field of enzymatic hydrolysis to prepare salivarius aglycone, can solve the problems of polluted environment, environmental pollution, large sample loss, etc., and achieves the effects of high extraction efficiency, less impurity dissolution, and easy handling.

Inactive Publication Date: 2012-02-15
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method produces a large amount of acid water during acid hydrolysis, which pollutes the environment. The sample loss in the column chromatography process is relatively large, and it also produces a large amount of silica gel and alumina waste, causing environmental pollution.

Method used

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  • Method for preparing periplogenin through enzymatic hydrolysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Grind the medicinal material of Persica cypress, take 1000g, add 8L90% methanol solution for ultrasonic extraction for 60min, filter the liquid and add 3L90% methanol for ultrasonic extraction for 30min, combine the extracts to recover methanol, add 500ml distilled water to azeotrope for 1 hour, add appropriate amount of diatomaceous earth Heat centrifugation, collect the centrifugate, adjust the pH to 4.5 with citric acid, heat to 50°C, add 1 g of helicase and incubate the enzymolysis for 32 hours, concentrate the enzymolysis solution under reduced pressure, and centrifuge to obtain 12 g of crude product. Mix chloroform, methanol, and water in a ratio of 4:3:3, take the upper phase and inject it into the chromatographic column as the stationary phase, turn on the high-speed countercurrent chromatograph, adjust the speed to 800r / min, inject the mobile phase, and after equilibrium, adjust the flow rate to 2ml / min, The crude product was dissolved in chloroform, injected, a...

Embodiment 2

[0029] Grind the medicinal material of Persica cypress, take 1000g, add 5L80% methanol solution for ultrasonic extraction for 40min, extract 3 times, combine the extracts to recover methanol, add 600ml distilled water to azeotrope for 1 hour, add appropriate amount of diatomaceous earth and centrifuge while it is hot, collect the centrifugate, hydrochloric acid Adjust the pH to 5, heat to 55° C., add 5 g of cellulase and incubate for 18 hours for enzymolysis, concentrate the enzymolysis solution under reduced pressure, and centrifuge to obtain 10 g of crude product. Mix chloroform, methanol, and water in a ratio of 4:3:3, take the upper phase and inject it into the chromatographic column as the stationary phase, turn on the high-speed countercurrent chromatograph, adjust the speed to 900r / min, inject the mobile phase, and after balancing, adjust the flow rate to 3ml / min. The crude product was dissolved in the mobile phase, injected, and the fractions were collected regularly by...

Embodiment 3

[0031] Grind the medicinal materials of Xiangjiapi, take 1000g, add 6L85% methanol solution for ultrasonic extraction for 60min, extract twice, combine the extracts to recover methanol, add 500ml distilled water to azeotrope for 1 hour, add appropriate amount of diatomaceous earth and centrifuge while it is hot, collect the centrifugate, lemon Adjust the pH to 5 with acid, heat to 50°C, add 3g of amygdalin and incubate it for 26 hours, then concentrate the enzymatic solution under reduced pressure, and centrifuge to obtain 12g of crude product. Mix chloroform, methanol, and water in a ratio of 4:3:3, take the upper phase and inject it into the chromatographic column as the stationary phase, turn on the high-speed countercurrent chromatograph, adjust the rotation speed to 1200r / min, inject the mobile phase, and after balancing, adjust the flow rate to 4ml / min. The crude product was dissolved in the mobile phase, injected, and the fractions were collected regularly by the detecto...

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Abstract

The invention relates to a method for preparing periplogenin through enzymatic hydrolysis. The method is characterized in that the method comprises the following steps: 1, taking a medicinal material Cortex Periplocae, crushing, adding 3-8 times of a 80-90% methanol solution, carrying out ultrasonic extraction, recovering methanol through concentrating an extract, adding a proper amount of water to the concentrated extract, carrying out azeotrope, and centrifuging while hot to obtain a centrifugate; 2, adjusting the pH value of the centrifugate to 4.5-5.5, adding a biological enzyme, carrying out insulation enzymatic hydrolysis for 18-32h, carrying out reduced pressure concentration on an enzymatic hydrolysate, and centrifuging to obtain a crude product; and 3, processing the crude product through a high speed counter current chromatograph, collecting a fraction, and drying the fraction to obtain periplogenin. The method of the invention, which has the advantages of low pollution and high yield, is suitable for the industrialization preparation.

Description

technical field [0001] The invention relates to a method for preparing barley aglycone, in particular to a method for preparing barley aglycon by enzymatic hydrolysis. Background technique [0002] Cortex Periplocae (Cortex Periplocae) is a plant of Asclepiadaceae (Asclepiadaceae) Periploca sepium The dry root bark of Bunge has the effect of dispelling wind-dampness and strengthening bones and muscles. It is a commonly used traditional Chinese medicine in clinical practice. [0003] Barley aglycone is (3beta,5beta)-3,5,14-trihydroxycard-20(22)-enolide, molecular formula C 23 h 34 o 5 , molecular weight 390.5131, molecular structure: [0004] [0005] Glycerin aglycone is a cardiac aglycone, which not only has a cardiotonic effect, but also has pharmacological effects such as anti-inflammatory and anti-tumor. Gu Wei et al. published "Study on the Effects of Salix Aglycone on Mast Cell Degranulation and Histamine Release" and Han Yubo et al. published "Study on the An...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P33/20
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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