Silybin purification method

A technology of silibinin and a purification method, which is applied in the field of chemical purification to achieve significant economic benefits, low production costs, and simple equipment

Inactive Publication Date: 2017-08-29
JIANGSU TIANSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the current production capacity and extraction status, the domestic market demand cannot be met. In the international market, silibinin is favored by the international pharmaceutical industry for its "natural plant source, green, environmental protection, no residue and no pollution."

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take 500g of milk thistle seed coat, crush it, add 1L of 80% ethanol according to the ratio of material to liquid 1:2, and perform ultrasonic extraction for 2 hours at a temperature of 40 °C; then transfer the material liquid into a Soxhlet extractor, Add 2.5L of 80% ethanol solution, the ratio of milk thistle seed coat to ethanol solution is: 1kg:5L, and extract at 60°C for 4h, the obtained extract is at 50°C temperature Rotary evaporation in a water bath for 2h, then put it to room temperature, filter, dissolve in methanol with a concentration of 80%, and the ratio of the wet weight of the filter cake to the methanol solution is: 1kg: 2L, and then placed at 5 °C for crystallization 48h, filtered again, the filter cake was washed with cold water at 5°C, and then vacuum-dried at 50°C for 8 hours. After UV detection, silibinin with a purity of 97.9% was obtained.

Embodiment 2

[0015] Take 800g milk thistle seed coat, crush it, add 1.6L of 80% ethanol according to the material-to-liquid ratio of 1:2, and perform ultrasonic extraction for 2 hours at a temperature of 40 °C; then transfer the material to a Soxhlet extractor , add 4.8L of 80% ethanol solution, the ratio of milk thistle seed coat to ethanol solution is: 1kg: 6L, and extract at 60°C for 4h, the obtained extract is at 50°C temperature Under the condition of water bath rotary evaporation for 3h, then put it to room temperature, filter, dissolve in methanol with a concentration of 80%, and the ratio of the wet weight of the filter cake to the methanol solution is: 1kg: 3L, and then placed under the temperature condition of 8 ℃ Crystallize for 60 hours, filter again, wash the filter cake with cold water, then vacuum dry for 8 hours at a temperature of 50°C, and obtain silibinin with a purity of 97.5% by UV detection.

Embodiment 3

[0017] Take 1000g milk thistle seed coat, pulverize it, add 2 L of 80% ethanol according to the ratio of material to liquid 1:2, and perform ultrasonic extraction for 2 hours at a temperature of 40 °C; then transfer the material liquid into a Soxhlet extractor, Add 7L of 80% ethanol solution, the ratio of milk thistle seed coat to ethanol solution is: 1kg: 7L, and extract at 60°C for 4h, and the obtained extract is at 50°C. Water bath rotary evaporation for 4h, then put it to room temperature, filtered, dissolved in methanol with a concentration of 80%, and the ratio of the wet weight of the filter cake to the methanol solution was 1kg:4L, and then placed at 10 °C for crystallization for 72h , filtered again, the filter cake was washed with cold water, and then vacuum-dried at 50°C for 8 hours. After UV detection, silibinin with a purity of 98.1% was obtained.

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PUM

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Abstract

The invention discloses a silybin purification method. The silybin purification method comprises the following steps: taking silybum marianum seed skins, crushing the material, adding ethanol according to the solid-liquid ratio of 1 kg: 2L, and performing ultrasonic extraction for 2 h at the temperature of 40 DEG C; then transferring the material liquid into a soxhlet extractor, adding an ethyl alcohol solution of 5-7 BV, performing extraction for 4 h at the temperature of 60 DEG C, performing water-bath rotary evaporation on an extract at the temperature of 50 DEG C for 2-4 hours, then placing the material under room temperature, filtering the material, and dissolving the material by 2-4 BV methanol, placing the material at the temperature of 5-10 DEG C for crystallization for 48-72 h, refiltering the material, performing cold water washing on a filter cake, and then performing vacuum drying at the temperature of 50 DEG C for 8 hours to obtain silybin with purity being greater than or equal to 97%. The method has the advantages of simple required equipment, clear process, easy realization, and low production cost, and the prepared silybin has the advantages of good quality, high purity, and obvious economic benefit.

Description

technical field [0001] The invention relates to a purification method, in particular to a purification method of silibinin, and belongs to the technical field of chemical purification. Background technique [0002] Milk thistle, also known as milk thistle and milk pheasant, is a plant of the genus Asteraceae, native to southern Europe and North Africa. As a folk medicine, milk thistle has been used for thousands of years in Europe and Africa, mainly for the treatment of liver diseases. Silybinin is a flavonoid present in the fruit of silymarin, among which the main active substance silibinin is a natural flavonoid lignan compound, which is clinically used for the treatment of hepatitis, cholecystitis and other diseases. Bing not only has the effect of protecting liver and gallbladder, but also has obvious anti-lipid peroxidation, anti-radiation, scavenging free radicals and anti-stomach ulcer. [0003] The production of silibinin in my country is basically the direct proce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 季浩闫成亮阚建伟窦长清孔繁博
Owner JIANGSU TIANSHENG PHARMA
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