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Process for preparing periplocin

A technology of salicylic glycosides and cardiac glycosides, which is applied in the field of medicine, can solve the problems of toxicity, low solvent consumption, low yield and the like, and achieves the effects of less dosage, complete extraction of medicinal materials and high yield

Active Publication Date: 2005-03-16
TIANJIN TASLY PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Xiangjiapi is poisonous, and overdose can cause adverse reactions, and there are also fatal reports in clinical practice
2000 edition " People's Republic of China Pharmacopoeia " under the determination of the content of Cortex Persicae, adopting 4-methoxy salicylaldehyde is HPLC method to measure reference substance, but so far there is no 4-methoxy salicylaldehyde that has Reports on relevant pharmacological effects
[0006] Some of the preparation methods used so far for salivatoxin are to extract the raw material with 95% ethanol backflow, the extraction of medicinal materials is not complete, and there are many low-polarity impurities extracted, which is not conducive to the production of salivatoxin monomer. Separation; some have to undergo repeated silica gel column chromatography, which is solvent-intensive and time-consuming, with low yield and high cost

Method used

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  • Process for preparing periplocin
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  • Process for preparing periplocin

Examples

Experimental program
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Effect test

Embodiment 1

[0025] (1) Extraction of Chinese herbal medicine: 500g of Xiangjiapi, add 4000mL of 40% ethanol solution by volume, reflux extraction 3 times, each time for 2 hours, combine the extracts, concentrate under reduced pressure to about 500mL, add 500mL of water to dilute After filtration, the clarified Persica citrifolia aqueous solution was obtained;

[0026] (2) Adsorption and separation of macroporous resins: Adsorb the aqueous solution of Persica chinensis with pretreated AB-8 macroporous resin (manufactured by Nankai University Chemical Factory), elute with a gradient of 10% to 95% ethanol, and collect each eluted part, the solvent was evaporated to dryness under reduced pressure, the residue was dissolved in ethanol, and thin-layer chromatography was carried out respectively, and the lower layer of chloroform:methanol:water=65:30:10 was used as developing solvent, and 3,5-dinitrobenzoic acid reagent was used for color development , the results showed that there were purple-r...

Embodiment 2

[0066] (1) Extraction of the medicinal materials: 500g of Persica persicae, add 3000mL of 80% ethanol solution by volume, reflux extraction 3 times, each time for 2 hours, combine the extracts, concentrate under reduced pressure to about 500mL, add 800mL of water to dilute After filtration, the clarified Persica citrifolia aqueous solution was obtained;

[0067] (2) Adsorption and separation of macroporous resin: use the pretreated D 101 (produced by Tianjin Pesticide Factory) macroporous resin adsorption, gradient elution with 10% to 95% ethanol, collect the eluted parts, evaporate the solvent under reduced pressure, dissolve the residue with ethanol, and perform thin-layer chromatography respectively. Use the lower layer of chloroform:methanol:water=65:30:10 as developing solvent, and develop color with 3,5-dinitrobenzoic acid reagent. The results show that there are Merge the purple spots to obtain the cardiac glycoside site;

[0068] (3) High-performance liquid phase pre...

Embodiment 3

[0071] (1) Extraction of Chinese herbal medicine: 500g of Persica persicae plus 3500mL of 50% ethanol solution by volume, reflux extraction twice, each time for 3 hours, combine the extracts, concentrate under reduced pressure to about 400mL, add 1000mL of water to filter , to obtain a clarified aqueous solution of Cyanocarp bark;

[0072] (2) Adsorption and separation of macroporous resin: Adsorb the aqueous solution of Persica chinensis with pretreated Dm2 (produced by Tianjin Nankai University Chemical Factory) macroporous resin, elute with 10% to 95% ethanol gradient, and collect the eluted parts , the solvent was evaporated under reduced pressure, the residue was dissolved in ethanol, thin-layer chromatography was carried out respectively, and the lower layer of chloroform:methanol:water=65:30:10 was used as developing solvent, and 3,5-dinitrobenzoic acid reagent was used for color development. The results showed that there were purplish red spots in parts 3-5 (40%-60% et...

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Abstract

The invention provides a process for preparing periplocin which consists the steps of, (1) extracting medicinal material of Chinese silkvine bark, obtaining aqueous solution of Chinese silkvine bark, (2) carrying out macroporous resin absorption to the aqueous solution, eluting using 10-95% ethanol, collecting the elution position, concentrating and proceeding thin-layer chromatography, coloring with color-developing agent, collecting and merging positions with cardiac glycoside, (3) preparation and separation of liquid phase.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of cardiac glycoside for treating acute and chronic congestive heart failure. Background technique [0002] Xiangjiapi is the dry root bark of the Astragalus chinensis plant. In recent years, Xiangjiapi has been commonly used in the treatment of acute and chronic congestive heart failure (CHF). Xiangjia bark is poisonous, and overdose can cause adverse reactions, and there are also fatal reports in clinical practice. 2000 edition " People's Republic of China Pharmacopoeia " under the determination of the content of Cortex Persicae, adopting 4-methoxy salicylaldehyde is HPLC method to measure reference substance, but so far there is no 4-methoxy salicylaldehyde that has Reports on relevant pharmacological effects. Periplocin (periplocin), that is, periplocin G (see below for structural formula), is a cardiac glycoside component in Cortex Periplo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J19/00
Inventor 张伯礼刘虹高秀梅潘桂湘郭俊华朱晓薇
Owner TIANJIN TASLY PHARMA CO LTD
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