Method for preparing sesamin from sesame

Inactive Publication Date: 2010-09-01
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Another example is patent 200710043757.9 (application number) "a kind of method that extracts and prepares sesamin with HZ816 mo

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Get 20kg of sesame seeds (0.4% of sesamin content), pulverize, add 80L 95% edible ethanol, reflux extraction for 2 hours, extract 3 times, combine extracts, recover ethanol by vacuum distillation, concentrate into extract, wash with 10% ammonia water, Centrifuge to obtain 1.2kg of extract, dissolve it in chloroform, filter, add 7kg of 80-100 mesh neutral alumina, stir and mix, and recover chloroform. Take 7L of D101 macroporous resin, pack it into a column, add a 200-mesh screen to the upper part, then mix the sesamin sample into it, first elute the fat-soluble impurities with 56L of 6# solvent oil, and then use ethyl acetate methanol 1:1 (v / v) The mixed solution elutes low-polarity impurities. TLC detects that sesamin flows out, and then elutes with ethyl acetate methanol 1:10 (v / v) until there is no sesamin fraction. Collect this fraction, recover the reagent to 1 / 6 of its volume and place it for crystallization, grow the crystal for 4 hours, and filter out 102 g of ...

Embodiment 2

[0034] Get 20kg of sesame seeds (0.4% of sesamin content), pulverize, add 120L 90% edible ethanol, reflux extraction for 2 hours, extract twice, combine extracts, recover ethanol by vacuum distillation, concentrate into extract, wash with 8% ammonia water, Centrifuge to obtain 1 kg of extract, then dissolve in chloroform, filter, add 6 kg of 80-100 mesh neutral alumina, stir and mix, and recover chloroform. Take 6L of macroporous resin, pack it into a column, add a 200-mesh screen to the upper part, then mix the sesamin sample into it, first elute fat-soluble impurities with 48L of 6# solvent oil, and then use ethyl acetate methanol 1:1 (v / v) The mixed solution elutes low-polarity impurities. TLC detection shows that sesamin flows out. Use ethyl acetate methanol 1:10 (v / v) for elution until there is no sesamin fraction. Collect this fraction, recover the reagent to 1 / 10 of its volume and place it for crystallization, grow the crystal for 6 hours, and filter out 96 g of crude c...

Embodiment 3

[0036] Get 20kg of sesame seeds (0.4% of sesamin content), pulverize, add 100L 85% edible ethanol, reflux extraction for 2 hours, extract 3 times, combine extracts, recover ethanol by vacuum distillation, concentrate into extract, wash with 10% ammonia water, Centrifuge to obtain 1.1 kg of extract, then dissolve in chloroform, filter, add 5 kg of 80-100 mesh neutral alumina, stir and mix, and recover chloroform. Take 7 liters of macroporous resin, pack it into a column, add a 200-mesh screen to the upper part, then mix the sesamin sample into it, first elute the fat-soluble impurities with 6# solvent oil 60L, and then use ethyl acetate methanol 1:1 (v / v ) mixed solution to elute low-polarity impurities, TLC detection, sesamin flow out, use ethyl acetate methanol 1:10 (v / v) to elute until there is no sesamin fraction. Collect this fraction, recover the reagent to 1 / 10 of its volume and place it for crystallization, grow the crystal for 6 hours, and filter out 102 g of the crude...

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PUM

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Abstract

The invention relates to a method for preparing sesamin. In the process, sesame is used as a raw material, refluxing extraction in edible ethanol is performed, a solvent is reclaimed under reduced pressure, ammonia water is used for washing, chloroform is added to dissolve the product obtained by washing, the chloroform solution is mixed with 80 to 100-mesh neutral aluminum oxide by stirring, the product obtained after mixing is dried, macroporous resin is added for absorption, No.6 solvent oil and mixed solution of ethyl acetate and methyl alcohol are used for gradient elution, a sesamin fraction is collected, a reagent is recovered till the volume is small, the remaining product is stood for crystallization, refluxing and saturated dissolution is performed in 95 percent ethanol and 70 percent ethanol respectively, and the sesamin product can be obtained by crystallization. The product produced by the method has the advantages of low cost, high yield, high purity and high raw material utilization rate.

Description

Technical field: [0001] The invention relates to a method for preparing sesamin from sesame, in particular to a method for preparing sesamin by using ethanol extraction, alumina and D101 macroporous adsorption resin for adsorption. Background technique: [0002] Sesamin is a diepoxylignan. [0003] Molecular formula: Molecular formula C 20 h 18 o 6 . Molecular weight: 354.36 [0004] Properties: Sesamin is a white needle-like crystal with a melting point of 120-121°C and an optical rotation [α]D20+64.5° (c=1.75, chloroform). Natural sesamin is dextrorotatory. Soluble in chloroform, benzene, acetic acid, acetone, methanol, ethanol, slightly soluble in ether, petroleum ether. Almost insoluble in water, alkaline solution, hydrochloric acid. [0005] Sesamin has inhibitory effects on influenza virus, Sendai virus and Mycobacterium tuberculosis, and has the effects of lowering cholesterol, promoting fat oxidation and utilization while inhibiting fat synthesis, antihyperte...

Claims

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Application Information

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IPC IPC(8): C07D493/04
Inventor 刘东锋张翼杨成东
Owner NANJING ZELANG MEDICAL TECH
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