New method for purifying silymarin

A technology for silymarin and silymarin, which is applied in the field of macroporous resin purification technology, can solve problems such as affecting product yield and quality, and achieve the effect of overcoming relatively low extraction rates

Active Publication Date: 2012-10-17
DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The oil-removed cake is first degreased and dewaxed with petroleum ether, then percolated or extracted with ethyl acetate or alcohol as a solvent, and then the solvent is recovered to obtain crude silymarin for sale, and few manufacturers continue to purify it; However, ethyl acetate is hydrolyzed to produce acetic acid during recycling, which affects the yield and quality of the product.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: A method for obtaining high-purity silymarin by using biological wall breaking and microwave pretreatment to obtain oil, and then undergoing microwave countercurrent and macroporous resin purification technology, the steps are as follows:

[0019] (1) Biological wall breaking: soak 1000g dried milk thistle seeds, add appropriate amount of cellulase and hemicellulase solution, keep warm for 60 minutes, and remove the cellulose, hemicellulose and pectin sheets wrapped in the shell of the seed coat Break the protein film, free the broken fat cells, and improve the oil extraction rate;

[0020] (2) Microwave pretreatment: crush milk thistle seeds through a 30-mesh sieve, add 4-6 times petroleum ether (boiling range 60-90°C) solution, and perform microwave pretreatment. The microwave power is 300 W and the frequency is 1000 MHz. The time was 300s, the extraction temperature was 60°C, petroleum ether was recovered, and 195.3g of milk thistle oil and 793g of deoi...

Embodiment example 2

[0027] Example 2: A method for obtaining high-purity silymarin by using biological wall breaking and microwave pretreatment to obtain oil, and then undergoing microwave countercurrent and macroporous resin purification technology. The steps are as follows:

[0028] (1) Biological wall breaking: soak 1000g of dry milk thistle seeds, add appropriate amount of cellulase and hemicellulase solution, keep warm for 60 minutes, and remove the cellulose, hemicellulose, and pectin sheets wrapped in the shell of the seed coat Break the protein film, free the wrapped oil cells, and improve the oil extraction rate;

[0029] (2) Microwave pretreatment: crush milk thistle seeds through a 40-mesh sieve, add 1-6 times petroleum ether (boiling range 60-90°C) solution, and perform microwave pretreatment. The microwave power is 400W, the frequency is 6000MHz, and the extraction time 400s, the extraction temperature was 60°C, petroleum ether was recovered, and 195g of milk thistle seed oil and 797...

Embodiment example 3

[0036] Example 3: A method of obtaining high-purity silymarin by using biological wall breaking and microwave pretreatment to obtain oil, and then using microwave countercurrent and macroporous resin purification technology. The steps are as follows:

[0037] (1) Biological wall breaking: soak 1000g of dry milk thistle seeds, add appropriate amount of cellulase and hemicellulase solution, keep warm for 60 minutes, and remove the cellulose, hemicellulose, and pectin sheets wrapped in the shell of the seed coat Break the protein film, free the wrapped oil cells, and improve the oil extraction rate;

[0038] (2) Microwave pretreatment: crush milk thistle seeds through a 50-mesh sieve, add 4-6 times petroleum ether (boiling range 60-90°C) solution, and perform microwave pretreatment. The microwave power is 500W, the frequency is 7000MHz, and the extraction time 400s, the extraction temperature was 60°C, petroleum ether was recovered, and 197g of milk thistle seed oil and 795g of ...

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Abstract

The invention belongs to the field of natural organic chemistry, and relates to a method for preparing high purity silymarin by the following steps: adopting biological wall breaking and microwave pretreatment to obtain oil, carrying out microwave countercurrent extraction and macroporous resin purification to obtain the high purity silymarin. The method has the following advantages that: 1, a step-by-step method is adopted to carry out degreasing, seeds are pretreated, microwave countercurrent extraction is performed, and isoelectric point precipitation is performed to remove proteins, such that complete dissolution of effective components of the silymarin is prompted; 2, with the microwave extraction, the extraction time is reduced to 60-80 minutes so as to improve extraction speed and increase effective component content, and reduce herb consumption and energy consumption; 3, the macroporous resin adsorption technology is adopted so as to reduce the amount of the solvent, and the macroporous resin can be conveniently and rapidly regenerated, such that the cost is substantially reduced; and 4, two products of silybum marianum oil and silymarin can be obtained. With the method, the biological wall breaking treatment is performed on the silybum marianum seeds at the early stage so as to shorten the microwave pretreatment time, such that the seed oil can be extracted in just a few minutes; with the two-step microwave extraction, the extraction time is shortened; and the disadvantages of long conventional extraction time, low extract purity and single extract are overcome.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry, and relates to a method for obtaining high-purity silymarin through biological wall breaking and microwave pretreatment to obtain oil, and then microwave countercurrent extraction and macroporous resin purification technology. Background technique: [0002] Milk thistle seed kernel contains 25.05% crude fat, and its fatty acids are mainly unsaturated oleic acid (47.46%) and linoleic acid (31.79%). The protein content of the defatted powder is 19.58%, which is higher than that of general cereals. Among them, albumin has the most content, accounting for 62.60% of the total protein. Milk thistle protein is mainly of medium and low molecular weight, and because it is rich in acidic amino acids, the isoelectric point of white matter is mainly distributed in the neutral to acidic range. [0003] Silymarin is a plant extract extracted from the seed coat of the medicinal plant Silybum marianum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D407/04C11B1/04C11B1/10
Inventor 姚德坤姚德利张亚红万莉
Owner DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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