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Preparation method of sesamin

A technology of sesamin and sesame seeds, applied in directions such as organic chemistry, can solve problems such as low yield and low content, and achieve the effects of good effect, convenient reuse, and solvent cost saving

Inactive Publication Date: 2012-05-02
苏州北商智业管理咨询有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Another example is patent 200710043757.9 (application number) "a kind of method that extracts and prepares sesamin with HZ816 modified resin", this technique discloses the method for extracting sesamin from sesame oil, but content is lower, and yield is low

Method used

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  • Preparation method of sesamin

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Take 1kg of sesame seeds (0.4% of sesamin content), pulverize, add 5L of 60% ethanol, first reflux extraction for 3 hours, then use 5L of 60% ethanol to extract the medicinal residues for 2 hours, combine the extracts, recover the ethanol by distillation under reduced pressure, and concentrate to obtain Paste, apply 5L X-5 macroporous resin, use 5L ethyl acetate methanol 10:1 mixed solution to elute low polarity impurities, then use 1:0.5 ethyl acetate-methanol to elute impurities until TLC detects that sesamin flows out , and eluted with ethyl acetate-methanol 1:8 (v / v) until there is no sesamin fraction. Collect this fraction, recover the reagent to 1 / 10 of its volume and let it crystallize, and filter out 5.2 g of crude crystals. The crude crystals were saturated and dissolved in an anhydrous ethanol water bath, left to crystallize, grown for 2 hours, repeated 3 times, filtered out and dried at low temperature to obtain 3.5 g of the product with a content of 97.3%. ...

Embodiment 2

[0028] Take 1kg of sesame seeds (0.4% of sesamin content), pulverize, add 6L of 70% ethanol, first reflux extraction for 3 hours, then extract the dregs with 6L of 70% ethanol for 2 hours, combine the extracts, recover the ethanol by distillation under reduced pressure, and concentrate to extract Paste, apply 5L H103 macroporous resin, use 5L ethyl acetate-methanol 10:2 mixed solution to elute low-polarity impurities, then use 1:2 ethyl acetate-methanol to elute impurities until TLC detects that sesamin flows out, change Elute with ethyl acetate-methanol 1:10 (v / v) until there is no sesamin fraction. Collect this fraction, recover the reagent to 1 / 8 of its volume and let it crystallize, and filter out 5.9 g of crude crystals. The crude crystals were saturated and dissolved by heating in an anhydrous ethanol water bath, left to crystallize, and grown for 3 hours. Repeated twice, the crystals were filtered out and dried at low temperature to obtain 3.2 g of the product with a co...

Embodiment 3

[0030] Take 1kg of sesame seeds (0.4% of sesamin content), pulverize, add 7L of 80% ethanol, first reflux extraction for 3 hours, then extract the dregs with 7L of 80% ethanol for 2 hours, combine the extracts, recover the ethanol by distillation under reduced pressure, and concentrate to obtain Paste, apply 5L HP20 macroporous resin, use 5L ethyl acetate-methanol 10:3 mixed solution to elute low-polarity impurities, and then use 1:1 ethyl acetate-methanol to elute impurities until TLC detects that sesamin flows out. Elute with ethyl acetate-methanol 1:9 (v / v) until there is no sesamin fraction. Collect this fraction, recover the reagent to 1 / 12 of its volume and let it crystallize, and filter out 6.3 g of crude crystals. The crude crystals were saturated and dissolved by heating in an anhydrous ethanol water bath, left to crystallize, and grown for 2 hours. Repeated 3 times, the crystals were filtered out and dried at low temperature to obtain 3.4 g of the product with a cont...

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Abstract

The invention relates to a preparation method of sesamin. With sesame as a raw material, the method comprises the steps of: adding ethanol for twice refluxing extraction, conducting pressure reduction and solvent recovery, carrying out mixing to obtain a sample which is then applied on macroporous resin for adsorption, performing gradient elution with a mixed solution of ethyl acetate and methanol, collecting sesamin fractions, recovering the reagent to a small volume, disposing the fractions for crystallization, then implementing refluxing in absolute ethyl alcohol for saturated dissolution, and conducting crystallization so as to obtain a product. Adoption of the method provided in the invention for production has the advantages of low cost, high yield as well as high purity, and is in accord with the principles of circular economy and also characterized by low carbon and environmental protection.

Description

Technical field: [0001] The invention relates to a method for preparing sesamin, in particular to a method for preparing sesamin by adopting macroporous adsorption resin adsorption. Background technique: [0002] Sesamin [0003] English name: Sesamin [0004] Synonyms: sesamin, sesamin, sesame Ming, synergistic sensitivity. [0005] Molecular formula: C 20 h 18 o 6 [0006] Molecular weight: 354.36 [0007] Molecular Structure: [0008] [0009] 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. [0010] Sesamin has inhibitory effects on influenza virus, Sendai virus and Mycobacterium tuberculosis, and has the effects of lowering cholesterol, promoting fat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
Inventor 李法庆钱钰
Owner 苏州北商智业管理咨询有限公司
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