Process for preparing silymarin

A technology for silymarin and silymarin, which is applied in the field of preparation of silymarin, can solve the problems of sensitive ethyl acetate quality, time-consuming cold soaking method, low recovery rate and the like, and achieves the effects of simplifying the extraction and separation process, shortening the extraction time and increasing the content.

Inactive Publication Date: 2006-03-15
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the solubility of silymarin in ethanol is larger than that in ethyl acetate, the extraction speed of silymarin is faster and the extraction is more complete, but the extract has many impurities and must be re-extracted with ethyl acetate after drying to achieve high quality. Require; Ethyl acetate extracts technological process short, and investment is low, and energy consumption is low, but product quality, yield are very sensitive to the quality of ethyl acetate, and (Xu Yong, discussion of silymarin production technology, Chinese Wild Plant Resources, 1996(4): 34-35)
And, solvent extraction cold soaking method is time-consuming, and efficient is low; Thermal reflux method silibinin is thermally decomposed, and recovery rate is low (Chen Yuquan, basic research on comprehensive utilization of silymarin I active ingredient extraction process, 1997, 6 (4) 91- 93) Northwest Agricultural Journal)
In addition, the existence of oil is not conducive to the extraction of the product, and the oil removal by cold pressing is not complete, which directly affects the yield and quality of silymarin
And when the oil is removed by cold pressing, the local temperature is very high, which will also damage the activity of silymarin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) The milk thistle seed material 500g that pulverizes is packed into extractor, with the supercritical CO of purity 99% 2 , extracted at a pressure of 30Mpa and a temperature of 55°C for 3 hours to obtain 105g of milk thistle seed oil and 394g of deoiled milk thistle powder;

[0023] (2) 394 g of deoiled silymarin powder was extracted with 400 g of 95% ethanol (ultrasonic oscillation for 15 minutes) to obtain an extract containing silymarin, extracted 3 times, and combined the extracts;

[0024] (3) The extract containing silymarin is loaded into the extractor, and the supercritical CO with a purity of 99% is used to 2 , extracted at a pressure of 16 MPa and a temperature of 45° C. for 3 hours, and ethanol was extracted to obtain 26 g of product silymarin, whose silymarin content was 81% through analysis and testing.

Embodiment 2

[0026] (1) The milk thistle seed material 500g that pulverizes is packed into extractor, with the supercritical CO of purity 99% 2 , extracted for 4 hours at a pressure of 20Mpa and a temperature of 50°C to obtain 105g of milk thistle seed oil and 394g of deoiled milk thistle powder;

[0027] (2) 394 g of deoiled silymarin powder was extracted with 400 g of 95% ethanol (ultrasonic oscillation for 15 minutes) to obtain an extract containing silymarin, extracted 3 times, and combined the extracts;

[0028] (3) The extract containing silymarin is loaded into the extractor, and the supercritical CO with a purity of 99% is used to 2 , extracted at a pressure of 20 MPa and a temperature of 55° C. for 3 hours, and ethanol was extracted to obtain 24 g of product silymarin, whose silymarin content was 80% through analysis and testing.

Embodiment 3

[0030] (1) The milk thistle seed material 500g that pulverizes is packed into extractor, with the supercritical CO of purity 99% 2 , extracted at a pressure of 35Mpa and a temperature of 55°C for 2.5 hours to obtain 105g of milk thistle seed oil and 392g of deoiled milk thistle powder;

[0031] (2) 392 g of deoiled silymarin powder was extracted with 400 g of 95% ethanol (ultrasonic oscillation for 15 minutes) to obtain an extract containing silymarin, which was extracted 3 times, and the extracts were combined;

[0032] (3) The extract containing silymarin is loaded into the extractor, and the supercritical CO with a purity of 99% is used to 2 , extracted at a pressure of 12 MPa and a temperature of 40° C. for 4 hours, and ethanol was extracted to obtain 23 g of product silymarin, whose silymarin content was 81% through analysis and testing.

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Abstract

The preparation process of silybin with silybum mariamum as material includes supercritical CO2 extraction of silybum mariamum seed oil, organic solvent extraction of silybin and the separation of extractive liquid in supercritical CO2 environment to obtain high-activity silybin. The said process is superior to traditional process with local high temperature and incomplete deoiling to affect product quality and yield, and has simplified extraction and separation process, short extraction period, and high silybin content in product. The silybum mariamum seed oil product of the present invention is clear and transparent health food oil with excellent commercial foreground.

Description

Technical field: [0001] The invention belongs to a method for preparing silymarin from milk thistle seeds, in particular to a method for preparing highly active silymarin and milk thistle seed oil by using a supercritical carbon dioxide extraction method. Background technique: [0002] Silymarin is the total flavonoid extract from the seeds of Silybum marianum (L.) Gaertn, a plant of Compositae. After my country introduced milk thistle from Germany in 1972, it has been successfully promoted and planted in various places, and in-depth research has been carried out on its chemical composition, pharmacology, and clinical aspects. As an anti-liver injury drug, silymarin can stabilize cell membranes and improve liver function; it also has obvious anti-lipid peroxidation, anti-radiation, scavenging free radicals and anti-gastric ulcer effects. The drug has low toxicity, no teratogenic and mutagenic effects, and has shown gratifying effects in reducing blood fat, preventing and tr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/20
CPCY02P20/54
Inventor 侯相林王国富乔欣刚杜俊民杨晋安李燕生
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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