Method for preparing and separating enkaurane-16-alkene-19-acid from wedelia trilobata

A technology of Wedaria trilobata and kaurine, which is applied in the field of extracting active ingredients from medicinal plants, can solve the problems of inability to meet market demands, long production process cycle, unfavorable large-scale production, etc., and achieves easy control of operating parameters and effective ingredients. Highly enriched, impurity reduction effect

Inactive Publication Date: 2014-11-05
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the products obtained by conventional extraction methods have low purity, low yield, troublesome operation, long production process cycle, and poor repeatability, which is not conducive to large-scale production and cannot meet market demand.

Method used

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  • Method for preparing and separating enkaurane-16-alkene-19-acid from wedelia trilobata

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dry Wedelia trilobata, pulverize, pass through a 30-mesh sieve, weigh 200 g of Wedelia trilobata powder and put it into the extraction kettle of a supercritical extractor (supercritical extractor: ISCO, USA, Model 260D, Syringe pump), entraining 60wt% ethanol was selected as the agent, the amount of entrainer added was 1200ml, and the flow rate of entrainer was 12ml / min; the extraction pressure was controlled at 25 MPa, the extraction temperature was 60°C, and the CO 2 The flow rate is 40L / h, and the extraction time is 3h; then concentrate under reduced pressure to remove ethanol to obtain about 40g of total extract, dissolve the total extract in 100ml of water, extract three times with 100ml of ethyl acetate, combine organic phases, and concentrate under reduced pressure to remove acetic acid Ethyl ester obtains about 20g of medicinal extract, 100g D101 type macroporous adsorption resin on the medicinal extract, elutes with 10L 60wt% ethanol aqueous solution, collects e...

Embodiment 2

[0020] Dry, grind, and pass through a 30-mesh sieve, weigh 250 g of Wedelia trilobata powder and put it into the extraction kettle of a supercritical extractor (supercritical extractor: ISCO, USA, Model 260D, Syringe pump), entraining The solvent used was 80 wt% ethanol, the amount of entrainer added was 1000ml, and the flow rate of entrainer was 10ml / min; the extraction pressure was controlled at 22 MPa, the extraction temperature was 50°C, and the CO 2 The flow rate is 35L / h, and the extraction time is 2.5h; then concentrate under reduced pressure to remove ethanol to obtain about 45g of total extract, dissolve the total extract in 150ml of water, extract three times with 150ml of ethyl acetate, combine the organic phase, and concentrate and remove the organic phase under reduced pressure Ethyl acetate obtains about 25g of medicinal extract, 200g D101 type macroporous adsorption resin on the medicinal extract, elutes with 10L 55wt% ethanol aqueous solution, collects eluent, c...

Embodiment 3

[0022] Dry, grind, and pass through a 30-mesh sieve, weigh 300 g of Wedelia trilobata powder and put it into the extraction kettle of a supercritical extractor (supercritical extractor: ISCO, USA, Model 260D, Syringe pump), entraining The solvent used was 95 wt% ethanol, the amount of entrainer added was 1200ml, and the flow rate of entrainer was 10ml / min; the extraction pressure was controlled at 20 MPa, the extraction temperature was 40°C, and the CO 2 The flow rate is 30L / h, and the extraction time is 2h; then concentrate under reduced pressure to remove ethanol to obtain about 50g of total extract, dissolve the total extract in 200ml of water, extract three times with 200ml of ethyl acetate, combine organic phases, and concentrate under reduced pressure to remove acetic acid Ethyl ester obtains about 30g of medicinal extract, 300g D101 type macroporous adsorption resin on the medicinal extract, elutes with 10L 50wt% ethanol aqueous solution, collects eluate, concentrates un...

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Abstract

The invention relates to the technical field of extracting of plant active ingredients and discloses a method for preparing and separating enkaurane-16-alkene-19-acid from wedelia trilobata. The method comprises the following steps of: drying, crushing and sieving the wedelia trilobata; putting the wedelia trilobata powder to an extraction kettle of a supercritical extractor for extracting, wherein an entrainer is alcohol, the extracting pressure is 20MPa-25MPa, the extracting temperature is 40 DEG C to 60 DEG C, the CO2 flow rate is 30L / h to 40L / h, and the extracting time is two hours to three hours; concentrating the extract under reduced pressure to obtain total extract, dissolving the total extract in water, extracting the solution for three times by using ethyl acetate and concentrating the organic phase under reduced pressure to remove ethyl acetate to obtain the extract; loading the extract to D101 macroreticular resin, eluting using alcohol aqueous solution, collecting the eluate, and concentrating under reduced pressure to obtain a crude crystal; and re-crystallizing the crude crystal by petroleum ether to obtain the product. The method disclosed by the invention is high in extracting speed, high in efficiency, less in energy consumption, and high in yield and purity of the obtained product.

Description

technical field [0001] The invention relates to the technical field of extraction of active ingredients of medicinal plants, in particular to a method for separating and preparing ent-kaurane-16-en-19-acid from Wedelia trilobata. Background technique [0002] Enantiokaurane-16-ene-19-acid (ent-KA) was first isolated from the traditional Mexican anti-fertility herbal medicine Montanoa tomentosa (Zoapatle), see literature: Journal of ethnopharmacology (1986), 18(1) , 89-94. It has been reported in the literature that the compound ent-KA has strong toxicity to human nasopharyngeal carcinoma cells (KB) and gastric cancer cells (BGC-823), see literature: (1) Phytotherapy Research (2002), 16, 387–388 and (2) Heilongjiang Medicine (2006), 19, 26-27. The compound and its derivatives have great antitumor research value and application prospect. It has been disclosed in the literature that this substance can also be isolated from some other plants, but the content is very small. T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C61/35C07C51/47C07C51/42
CPCY02P20/54
Inventor 高坤陈佳陈艳君
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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