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Method for extracting protopine from decumbent corydalis tuber

A technology for proto-opioid and extracting solution, which is applied in the field of extracting alkaloid pro-opiate, which can solve the problems of low solubility, inability to extract pro-opiate, unfavorable separation of pro-opiate, etc., and achieve improved purity, fewer steps, and low cost Effect

Inactive Publication Date: 2007-05-23
SHANGHAI INST OF PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the hydrochloride of tetrahydropalmatine, an alkaloid in summer, has very little solubility in water, it is not conducive to the separation of the original opioid; extracted from medicinal

Method used

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  • Method for extracting protopine from decumbent corydalis tuber

Examples

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Embodiment 1

[0037] Weigh 8 kg of clean Xiawu, put it in a 100L extraction kettle, add 40L of 85% ethanol, heat to 80°C for 2 hours, filter the extract through gauze, leave the filter residue in the extraction kettle, and add 40L of 85% Ethanol, continued heat extraction for 2 hours, and combined the two filtrates; recovered (that is, concentrated) the ethanol therein to obtain 10 L of residual liquid. Add 10L of 5% hydrochloric acid to the above residual liquid until the pH is 2, and let it stand for 10 hours; filter off the insoluble matter of hydrochloric acid, and neutralize the filtrate with 15% aqueous sodium hydroxide solution to pH = 12 to obtain alkaloid precipitation a; alkaloid precipitation a was dissolved in 5L of 5% hydrochloric acid, and 500ml of 85% ethanol was added at the same time to make the solution pH 3, and the newly generated precipitate was filtered off; the filtrate was neutralized with 15% aqueous sodium hydroxide solution, pH = 12, to obtain the alkaloid precipit...

Embodiment 2

[0039] Weigh 10kg of clean Xiawu, put it in a 100L extraction kettle, add 50L 95% ethanol, heat to 80°C for 2 hours, filter out through gauze, leave the filter residue in the extraction kettle, add 50L 95% ethanol, continue Heat extraction, combine the two filtrates; recover ethanol to obtain 11L of residual liquid, add 10L of 10% hydrochloric acid to the above residual liquid until the pH is 1.5, and let it stand for 12 hours; Neutralize pH = 11 to obtain alkaloid precipitate a; dissolve alkaloid precipitate a in 5L of 10% hydrochloric acid, add 500ml of 95% ethanol at the same time, make the solution pH 1, filter out the newly produced precipitate; filtrate is oxidized with 10% hydroxide Neutralize with aqueous sodium solution, pH = 10, to obtain alkaloid precipitate b, wash the precipitate b with distilled water to pH = 8, and dry to obtain a white solid; the solid is crystallized and recrystallized by chloroform and methanol (volume ratio: 1:1), 24.11 g of pro-opioid with ...

Embodiment 3

[0041]Weigh 1 kg of clean summer powder and place it in a 10L round-bottomed flask, add 6L of 90% ethanol, heat to 85°C, reflux for 2 hours, pour out the supernatant, leave the dregs in the round-bottomed flask, add 6L of 90% ethanol again % ethanol, continue heat extraction for 2 hours, combine the above solutions twice and concentrate; recover the ethanol to obtain 1L of residual liquid, add 3% hydrochloric acid to the above residual liquid to pH = 1, and let it stand for 20 hours; filter out insoluble matter, and use 30 % sodium hydroxide aqueous solution to neutralize pH = 11 to obtain alkaloid precipitation a; dissolve alkaloid precipitation a with 0.5 L of 10% hydrochloric acid, and add 80 ml of 95% ethanol at the same time to make the solution pH 1, and filter off the new precipitate; The filtrate was neutralized with 20% aqueous sodium hydroxide solution, pH = 9, to obtain an alkaloid precipitate b, which was washed with distilled water to pH = 8, and dried to obtain a ...

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Abstract

The process of extracting protopine from decumbent corydalis tuber includes the following steps: 1. hot extracting decumbent corydalis tuber with 85-100 % concentration alcohol and concentrating to obtain extract liquid; 2. recovering alcohol, adding 0.5-15 % concentration hydrochloric acid solution to the extract liquid and setting; 3. filtering out the hydrochloric acid insoluble matter and neutralizing the filtrate with 1-30 % concentration strong alkali solution to obtain alkaloid precipitate; 4. adding 0.5-15 % concentration hydrochloric acid solution and 85-100 % concentration alcohol to the alkaloid precipitate, filtering out the insoluble matter, neutralizing the filtrate with 1-30 % concentration strong alkali solution to obtain purified alkaloid precipitate, washing and drying to obtain solid matter; and 5. crystallizing the solid matter to obtain protopine. The said process can obtain protopine over 0.24 % weight of the decumbent corydalis tuber material and purity over 99.5 %.

Description

technical field [0001] The invention relates to a method for extracting the alkaloid protopine (Protopine) from the summer root. Background technique [0002] In summer, the dry tubers of Poppyaceae, Corydalis, and Corydalis decumbens (Thunb) Pers. (Corydalis amabilis Migo)] are used to treat rheumatoid arthritis, lumbar muscle strain, and hemiplegia caused by cerebrovascular accidents , has the effect of antispasmodic and pain relieving, promoting blood circulation and removing blood stasis and lowering blood pressure and promoting qi. Researchers found that summer contains more than 30 kinds of alkaloids such as summer analkaloid, corydalis metidine, piculicine, tetrahydropalmatine and protopine. Among them, Protopine has cholinesterase inhibitory effect and non-selective ion channel blocking effect, which can be used to treat Alzheimer's disease and is a potential drug candidate for Alzheimer's disease. If the compound is extracted from natural products, it is a simple,...

Claims

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Application Information

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IPC IPC(8): C07D491/153C07D317/00C07D225/00
Inventor 杨义芳杜立春
Owner SHANGHAI INST OF PHARMA IND
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