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Preparation method of unsaturated fatty acid in silybum marianum seed oil

A technology of unsaturated fatty acid and silymarin oil, applied in the field of medicine and chemical industry, can solve the problem of not much research and preparation of unsaturated fatty acid, and achieve the effects of low cost, good color and clear process

Inactive Publication Date: 2017-12-01
JIANGSU TIANSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are a large amount of milk thistle oil for sale on the market, but there are not many researches and preparations on its unsaturated fatty acid. In order to make milk thistle use to the greatest extent, the present invention provides a kind of synthesis of unsaturated fatty acid in milk thistle oil. Preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 10kg of milk thistle oil into the ethanol solution of NaOH, and the mass ratio of milk thistle oil, NaOH and ethanol solution is: 1:0.01:6, reflux at 75°C for 5h, recover ethanol, separate the liquid, take Supernatant (lower layer is glycerol); add 95% ethanol solution containing urea to the supernatant, the mass ratio of supernatant, urea, and ethanol solution is: 1:2:4, heat and stir at 70°C for 30 minutes , and then lower the temperature to 10±2°C at a rate of 0.5°C per minute, stir at this temperature for 4 hours, and carry out urea inclusion complexation to obtain a urea inclusion solution; then filter the urea inclusion solution under reduced pressure at 10±2°C, The ethanol solvent is recovered from the filtrate, and the result after recovering the ethanol solvent is dissolved in water at 50°C with 3 times the amount of the resultant, and then 10% hydrochloric acid is added to adjust the pH value to 4-5 (weak acidity, PH test paper detection), and then Then wa...

Embodiment 2

[0023] Add 10kg of milk thistle oil into the methanol solution of NaOH, and the mass ratio of milk thistle oil, NaOH and methanol solution is: 1:0.01:4, reflux at 70°C for 5h, recover methanol, separate the liquid, take Supernatant (lower layer is glycerol); add 95% ethanol solution containing urea to the supernatant, the mass ratio of supernatant, urea, and ethanol solution is: 1:1.5:4, heat and stir at 80°C for 30 minutes , and then lower the temperature to 10±2°C at a rate of 0.5°C per minute, stir at this temperature for 3 hours, and carry out urea inclusion complexation to obtain a urea inclusion solution; then filter the urea inclusion solution under reduced pressure at 8±2°C, The ethanol solvent is recovered from the filtrate, and the result after recovering the ethanol solvent is dissolved in water at 50°C with 4 times the amount of the resultant, and then 10% hydrochloric acid is added to adjust the pH value to 5-6 (weak acidity, PH test paper detection), and then The...

Embodiment 3

[0025] Add 10kg of milk thistle oil into the ethanol solution of NaOH, and the mass ratio of milk thistle oil, NaOH and ethanol solution is: 1:0.02:7, reflux at 80°C for 6h, recover ethanol, separate the liquid, take Supernatant (the lower layer is glycerin); add 95% ethanol solution containing urea to the supernatant, the mass ratio of supernatant, urea, and ethanol solution is: 1:2.5:4, heat and stir at 80°C for 40min , and then lower the temperature to 10±3°C at a rate of 0.5°C per minute, stir at this temperature for 6 hours, and carry out urea inclusion complexation to obtain a urea inclusion solution; then filter the urea inclusion solution under reduced pressure at 12±3°C, The ethanol solvent is recovered from the filtrate, and the result after recovering the ethanol solvent is dissolved in water at 50°C with 3 times the amount of the resultant, and then 10% hydrochloric acid is added to adjust the pH value to 5-6 (weak acidity, PH test paper detection), and then Then w...

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PUM

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Abstract

The invention discloses a preparation method of unsaturated fatty acid in silybum marianum seed oil. The method comprises the steps of (S1) adding the silybum marianum seed oil to a NaOH alcoholic solution, refluxing and taking supernatant liquid; (S2) adding an ethanol solution containing urea to the supernatant liquid, heating and stirring, cooling, stirring and carrying out urea esterification; (S3) carrying out vacuum suction filtration on the product obtained in the step (S2), adding water to dissolve the product obtained after recovering an ethanol solvent from filtrate, adding hydrochloric acid to adjust to achieve weak acidity, washing until neutral effect is achieved, and carrying out centrifugal drying to obtain the unsaturated fatty acid; (S4) adding filter cake obtained in the step (S3) to the ethanol solution and repeating the steps (S2) and (S3); and (S5) combining the products obtained in the step (S3) and (S4), adding the combined product to a NaOH water solution, heating and stirring, stopping reaction and adding hydrochloric acid to adjust to achieve acidity, standing and layering, taking the supernatant liquid and washing until neutral effect is achieved, carrying out centrifugal drying to obtain the unsaturated fatty acid. According to the method, the process is clear, the method is simple and the cost is low; the purified product is good in color and high in yield; and unsaturated fatty acid and fatty acid can be extracted to the maximal extent.

Description

technical field [0001] The invention relates to a preparation method of unsaturated fatty acid, in particular to a preparation method of unsaturated fatty acid in milk thistle oil, and belongs to the technical field of medicine and chemical industry. Background technique [0002] Milk thistle is a medicinal plant of Compositae, which is native to North Africa. It was introduced into my country in the 1970s and has been widely promoted and planted as a medicinal plant for protecting the liver. A large amount of literature research shows that milk thistle seeds contain a large amount of flavonoids, among which silymarin, the representative compound of flavonoids, has the functions of scavenging active oxygen, resisting lipid peroxidation, resisting liver toxin, promoting liver cell repair, Pharmacological activities such as anti-tumor and hypolipidemic have been widely known. [0003] Apart from flavonoids, milk thistle seeds contain a large amount of unsaturated fatty acids,...

Claims

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Application Information

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IPC IPC(8): C11C1/02C11C1/04C11C3/00C11C3/10C07C27/02C07C57/03C07C67/60C07C69/52C07C67/03
CPCC07C51/09C07C67/03C07C67/60C11C1/02C11C1/04C11C3/00C11C3/10C07C69/52C07C57/03
Inventor 季浩胡亚京阚建伟窦长清孔繁博徐娟
Owner JIANGSU TIANSHENG PHARMA
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