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Preparation method of 20-deoxyingenol

A technology of ingenol and euphorbia, which is applied in the field of preparation of ingenol diterpenoids, can solve the problems of poor repeatability, long time-consuming, large consumption of reagents, etc.

Inactive Publication Date: 2021-02-05
SHENYANG PHARMA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the preparation of 20-deoxyingenol is mainly through the traditional extraction and separation method, which has many defects, such as long time-consuming, large reagent consumption, poor repeatability, and the yield is only 1.6-4mg / kg (Phytochemistry, 1998, 47:1583-1600; J Nat Prod 2012, 75:1915-1921; Planta Med, 2018, 84:1334–1339; Phytochemistry, 2020, 172:112257)

Method used

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  • Preparation method of 20-deoxyingenol
  • Preparation method of 20-deoxyingenol
  • Preparation method of 20-deoxyingenol

Examples

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Embodiment 1

[0025] Take 1.0 kg of dry root tubers of Euphorbiaceae Euphorbi genus Gansui, reflux extraction with 2 L of 75% methanol water for 3 times, each time for 1.5 hours, and combine the extracts; filter the extracts, concentrate under reduced pressure to obtain 109 g of extract a Add 500mL of water to extract a, extract 5 times with ethyl acetate equal to the volume of water, combine the extract phases, concentrate under reduced pressure to obtain 14.2g of extract b; dissolve extract b with 160mL of anhydrous methanol and add 2.2g Potassium carbonate, stirred at room temperature for 8 hours, then added 1N hydrochloric acid at 0°C for neutralization and adjusted the pH to 6-7. Concentrate under reduced pressure, then add 200mL saturated saline to dilute, then add an equal volume of ethyl acetate to extract 3 times, concentrate under reduced pressure to obtain 10.0g extract c; dissolve extract c in 50mL methanol, add 100 mesh HP-20 resin 100g to mix the sample And packed into a colum...

Embodiment 2

[0028]Take 1 kg of dry root tubers of Euphorbiaceae Euphorbi genus Gansui, reflux extract with 2L of 75% ethanol water for 3 times, each time for 2 hours, and combine the extracts; filter the extracts, concentrate under reduced pressure to obtain 158 g of extract a; Add 500mL of water to the extract a to suspend, extract 5 times with ethyl acetate equal to the volume of water, combine the extract phases, and concentrate under reduced pressure to obtain 20.1g of extract b; dissolve extract b with 200mL of anhydrous methanol and add 5.0 g potassium carbonate, stirred at room temperature for 4 hours, then added 1N hydrochloric acid at 0°C for neutralization and adjusted the pH to 6-7. Then concentrate under reduced pressure and add 200mL saturated saline to dilute, then add an equal volume of dichloromethane to extract 5 times, concentrate under reduced pressure to obtain 15.6g of extract c; extract c is mixed with 200mL of 100 mesh HP-20 resin 100g and packed into a column, The ...

Embodiment 3

[0030] Take 1 kg of dry root tuber of Euphorbiaceae Euphorbi genus Gansui, reflux extraction with 75% ethanol water 2L for 5 times, each time for 1.5 hours, and combine the extracts; filter the extracts, concentrate under reduced pressure to obtain 149 g of extract a; Add 500mL of water to extract a to suspend, extract 5 times with ethyl acetate equal to the volume of water, combine the extract phases, concentrate under reduced pressure to obtain 19.0g of extract b; dissolve extract b with 200mL of anhydrous methanol and add 4.0 g barium hydroxide, stirred at room temperature for 6 hours, then added 1N hydrochloric acid at 0°C for neutralization and adjusted the pH to 6-7. After concentrating under reduced pressure, add 200 mL of saturated saline to dilute, then add an equal volume of ethyl acetate to extract 5 times, concentrate under reduced pressure to obtain 14.5 g of extract c; add 150 g of 100 mesh HP-20 resin to dissolve extract c in 50 mL of methanol The sample was pac...

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Abstract

The invention relates to the technical field of medicines for extracting and separating effective components in medicinal plants, in particular to a preparation method of ingenane diterpenoid compounds. The preparation method comprises the following steps of by taking dry tuberous roots of euphorbia kansui (Euphorbia kansui T.N.Liou ex T.P.Wang) as a raw material, extracting with an organic solvent, extracting, carrying out alkaline hydrolysis, carrying out macroporous resin column chromatography, and carrying out high performance liquid chromatography separation, thereby obtaining the product. According to the method, the separation efficiency and the yield can be greatly improved, the yield of the 20-deoxyingenol is over 100mg / kg, the yield is high, the repeatability is good, and the requirements of industrial production can be met after process amplification.

Description

technical field [0001] The invention relates to the technical field of medicine for extracting and separating active ingredients in medicinal plants, in particular to a preparation method of ingenane diterpenoids. Background technique [0002] Gansui (Euphorbia kansui T.N.Liou ex T.P.Wang) is the dry root tuber of Euphorbia genus (Euphorbia.) in the family Euphorbiaceae. Gansui is rich in resource reserves, widely distributed in Gansu, Shanxi, Shaanxi, Ningxia, Henan, Qinghai and other provinces. Gansui has the functions of purging water, dispelling swelling, reducing swelling and dissipating stagnation, etc. It is mainly used by folks to induce labor, edema and treat various difficult diseases. And its methanol extract showed obvious activity in the preliminary determination of HIV virus-related activity. Ingenane diterpene is a characteristic component of Gansui, which is composed of a 5-membered ring (A ring) and two 7-membered rings (B ring and C ring) system. The C-8 ...

Claims

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Application Information

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IPC IPC(8): C07C49/727C07C45/64C07C45/78C07C45/79
CPCC07C45/64C07C45/78C07C45/79C07C2603/86C07C49/727
Inventor 宋少江刘庆博李吉翀任会王茹祺
Owner SHENYANG PHARMA UNIVERSITY
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