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Purification method of anisomelic acid

A technology of parsnip oxalic acid and its purification method, which is applied in the direction of organic chemistry, can solve the problems such as high-content parsnip oxalic acid patent report, and achieve the effect of high product yield and simple impurity removal process

Inactive Publication Date: 2013-12-18
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] At present, there is no patent report on the purification method of high-content parsnip oxalic acid in China

Method used

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  • Purification method of anisomelic acid

Examples

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Effect test

Embodiment 1

[0029] Grind parsnips (0.2% parsnip oxalic acid content) to 20 mesh, take 200g and add 1.6L 80% ethanol solution, add to flash extractor, extraction voltage is 150V, extraction time is 90s, perform flash extraction, and combine to obtain the extracted solution, add 32g of activated carbon for decolorization, the decolorization temperature is 60°C, keep warm for 1h, concentrate the decolorization solution, place the precipitate, and filter with suction to obtain the precipitate, add 4 times the amount (V / W) of ammonia solution at pH 9, stir to dissolve, add the supernatant Adjust the pH to 5 with hydrochloric acid to obtain a precipitate, then reflux with 95% ethanol to dissolve the precipitate, filter while it is hot, place the filtrate to crystallize, recrystallize once, filter and dry to obtain 190 mg of a colorless crystal product with a content of 91.4% of oxalic acid.

Embodiment 2

[0031] Grind parsnips (0.2% parsnip oxalic acid content) to 40 mesh, take 200g and add 1.6L 90% ethanol solution, add to flash extractor, extraction voltage is 150V, extraction time is 90s, perform flash extraction, add 32g of activated carbon Decolorization, the decolorization temperature is 60°C, keep warm for 0.5h, concentrate the decolorization solution, place the precipitate, filter with suction to obtain the precipitate, add 4 times the amount (V / W) of ammonia solution with pH 9, stir to dissolve, add hydrochloric acid to the supernatant to adjust the pH to 4. 5. After obtaining the precipitate, reflux with 100% ethanol to dissolve the precipitate, filter while it is hot, place the filtrate to crystallize, recrystallize twice, filter and dry to obtain 249mg of colorless crystal product, the content of Fangfeng oxalic acid is 94.3%.

Embodiment 3

[0033] Grind parsnips (0.2% parsnip oxalic acid content) to 20 mesh, take 500g and add 4L85% ethanol solution, add to flash extractor, extraction voltage is 150V, extraction time is 90s, perform flash extraction, add 64g of activated carbon for decolorization , the decolorization temperature is 50°C, keep warm for 1h, concentrate the decolorization solution, place the precipitate, and filter with suction to obtain the precipitate, add 4 times the amount (V / W) of ammonia solution at pH 8.5, stir to dissolve, add hydrochloric acid to the supernatant to adjust the pH to 5. 5. Obtain the precipitate, then reflux with 95% ethanol to dissolve the precipitate, filter while it is hot, place the filtrate to crystallize, recrystallize twice, filter and dry to obtain 785 mg of colorless crystal product, the content of Fangfeng oxalic acid is 93.2%.

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Abstract

The invention relates to a method for purifying anisomelic acid from pastinaca sativa. The method comprises the following steps: 1) carrying out flash extraction on pastinaca sativa with an alcoholic solution; 2) decolorizing the extracting solution with activated carbon while keeping the temperature, concentrating the decolorization solution, and standing to precipitate; 3) dissolving the precipitate in an alkali solution, and regulating the pH value of the supernate to 4.5-5.5 to obtain the precipitate; 4) dissolving the precipitate in a high alcohol solution under reflux, filtering while the solution is hot, and standing the filtrate to crystallize; 5) recrystallizing. The anisomelic acid produced by the method provided by the invention has the advantages of high product purity and high yield; and the technique is simple and easy to operate.

Description

technical field [0001] The invention relates to an extraction and purification process of parsnip oxalic acid, in particular to a process for extracting and purifying parsnip oxalic acid from parsnips. Background technique [0002] Anisomelic acid, the molecular formula is C20H26O4, the molecular weight is 330.42, and the structural formula is [0003] [0004] Parsnip oxalic acid is derived from the whole plant of Anisomeles indica (L.) O.Ktze., Labiatae. Parsnip oxalic acid has cytotoxic activity and has inhibitory effect on KB cell growth, with an IC50 of 6.7 μg / ml. [0005] Fangfengcao, also known as Luomayi, False Perilla, Mayiye, etc., is warm in nature and bitter, and enters the bladder, liver, and kidney channels. It has the effects of expelling wind, relieving exterior, detoxifying and dehumidifying, and strengthening muscles and bones. It can cure cold and fever, vomiting, abdominal pain, muscle and bone pain, sores, eczema, hemorrhoids and other diseases. Pa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/93
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH
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