Preparation method of tubeimoside I

A technology of Tuibeimoside A and Tuibeimu, which is applied in the field of separation and preparation of active ingredients of traditional Chinese medicine

Inactive Publication Date: 2011-09-14
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are no patent reports and detailed studies on the preparation of tuimosi

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 5kg of decoction pieces of Tubeimu, crushed through a 20-mesh sieve, soaked in 15L of 50% ethanol for 5 hours, then added 50% ethanol to 30L, heated and refluxed for extraction, filtered, and the dregs were refluxed for 2 times, filtered, combined extracts, and decompressed Recover ethanol to 25L; pass the extract into a pretreated polyamide column (8L, 20-50 mesh), elute with 3BV water first, then elute with 80% ethanol, recover ethanol under reduced pressure, concentrate to a small volume to obtain a sample. Dry the sample with 200g of alumina, add it to a medium-pressure alumina column, and elute it with water until it is colorless, and then use the dichloromethane-methanol gradient elution, from high to low, in sequence according to 100:1, 50 : 1, 20: 1 and 5: 1, collected in sections, collected the active ingredient sections, concentrated to produce crystals, washed several times with acetone, and freeze-dried to obtain 35g of Tupimoside A, whose purity was 90.9% a...

Embodiment 2

[0018] Fritillaria decoction pieces 8kg, crushed through a 20-mesh sieve, soaked in 32L of 60% ethanol for 3 hours, then added 60% ethanol to 80L for percolation extraction, and the dregs were extracted by percolation once again, filtered, combined extracts, and recovered under reduced pressure Ethanol to 40L; the extract is passed into a pretreated Sephadex LH-20 chromatography column (15L, 20-50 mesh), first eluted with 3BV water, then eluted with 65% ethanol, and the ethanol is recovered under reduced pressure. Concentrate to a small volume to obtain a sample. Dry the sample with 300g of alumina, add it to a medium-pressure alumina column, and elute it with water until it is colorless, and then elute it with dichloromethane-methanol gradient, from high to low, according to 100:1, 50 : 1, 20: 1 and 5: 1, collected in sections, collected the active ingredient sections, concentrated to produce crystals, washed several times with acetone, and freeze-dried to obtain 58g of Tupim...

Embodiment 3

[0020] 5kg of fresh bulbs of S. fritillaria, crushed through a 20-mesh sieve, soaked in 13L of 60% methanol for 5 hours, added 60% methanol to 35L of ultrasonic extraction, 30min each time, filtered, and the dregs were ultrasonically extracted twice, filtered, and combined for extraction Liquid, recover methanol to 28L under reduced pressure; pass the extract into a pretreated polyamide column (8L, 20-50 mesh), elute with 3BV water first, then elute with 75% ethanol, recover ethanol under reduced pressure , concentrated to a small volume to obtain a sample. This sample was mixed with 200g Sephadex LH-20 Sephadex LH-20 and dried, added to a Sephadex LH-20 chromatographic column, first eluted with water, then eluted with 23% acetonitrile, collected the eluate, concentrated to produce crystals, Then washed several times with acetone, and freeze-dried to obtain 37 g of tulimoside A, the purity of which was 92.1% as detected by HPLC.

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Abstract

The invention provides a preparation method of tubeimoside I. The method comprises the following steps of: soaking tubeimu tuber bulbs into an appropriate quantity of organic solvent; extracting by heating, diacolation or by adopting an ultrasonic method; filtering to obtain a tubeimu tuber extracting solution; collecting eluent by adopting one or more processes of polyamide column chromatography, Sephadex LH-20 column chromatography, medium-pressure aluminum oxide column chromatography and the like; recovering a reagent from the eluent at reduced pressure; and cleaning acetone repeatedly to obtain tubeimoside I. The purity of the tubeimoside I prepared with the method is over 90 percent; the method is simple and practical and is suitable for large-scale production.

Description

Technical field: [0001] The invention belongs to the field of separation and preparation of active ingredients of traditional Chinese medicines. Specifically, the invention relates to a method for separating and preparing soil fritillary side A from soil fritillaria. Background technique: [0002] Tubeimoside A (Tubeimoside A) is a saponin extracted and isolated from the cucurbit plant Bolbostemma paniculatum, and is one of the main active ingredients of Bolbostemma paniculatum. Molecular formula: C 63 h 98 O 29 , molecular weight: 1319.43. Pharmacological tests have shown that it has various activities such as anti-tumor, anti-virus, and immunosuppression. The content of Tuimoside A in plants is relatively high. Wei Youliang et al. used HPLC method to measure the content of Tuimoside A in Tuibeimu from different origins. The mobile phase was 65% methanol, the flow rate was 1.0ml / min, and the detection wavelength was 214nm; The contents of Solimoside A in Soil Fritillar...

Claims

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Application Information

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IPC IPC(8): C07J63/00C07H15/256C07H1/08
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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