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Preparation method of polygonum multiflorum cis and trans-stilbene glycoside reference substances

A technology of stilbene glycosides and Polygonum multiflorum, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of long cycle and cumbersome operation, and achieve the effect of appropriate peak time

Active Publication Date: 2015-11-18
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, experts and scholars at home and abroad have paid much attention to the research on THSG in Polygonum multiflorum. There are many reports on related extraction and separation methods, but the refining methods are mostly limited to macroporous adsorption resin methods, polyamide adsorption methods, etc., which are cumbersome to operate and take a long time.

Method used

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  • Preparation method of polygonum multiflorum cis and trans-stilbene glycoside reference substances
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  • Preparation method of polygonum multiflorum cis and trans-stilbene glycoside reference substances

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Embodiment 1

[0027] Embodiment 1: the investigation of liquid phase condition

[0028] In high-performance liquid chromatography analysis, the number of theoretical plates, resolution, and tailing factor are important indicators of separation and detection effects, which are reflected in the relative positions and peak shapes of chromatographic peaks in the chromatogram. From the visual analysis of the chromatogram, the separation of narrow peaks and large distances between different peaks is satisfactory.

[0029] In the present invention, the degree of separation is used as an investigation index, and the types of polar and non-polar solvents used in chromatographic analysis and the ratio of solvents are tested and screened. The specific process is as follows:

[0030] Methanol-water, methanol-acetonitrile-water, and acetonitrile-water were prepared into a series of mobile phase solutions according to different volume ratios.

[0031] The preparation of test sample and reference substa...

Embodiment 2

[0037] Example 2: Preparation of cis- and trans-stilbene glycoside reference substances in Polygonum multiflorum

[0038] (1) Preparation of crude extract of stilbene glycosides from Polygonum multiflorum

[0039]500g of Radix Polygoni Multiflori, powdered, ultrasonically extracted twice with 70% ethanol for 0.5h each time, filtered, combined filtrates, concentrated under reduced pressure until no alcohol smell. The concentrated solution was extracted 3 times with an equal volume of petroleum ether. After extraction, the aqueous phase was adjusted to pH 10 with ammonia water, extracted 3 times with an equal volume of ethyl acetate, and the ethyl acetate phase was concentrated under reduced pressure to obtain 3 g of the extract, which was stored in a refrigerator for later use. .

[0040] (2) Semi-preparative HPLC separation and purification

[0041] Dissolve the extract of step (1) with methanol, and then filter it with a microporous membrane (0.45 μm) to obtain a sample sol...

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Abstract

The present invention discloses a preparation method of polygonum multiflorum cis and trans-stilbene glycoside reference substances. The method comprises the steps of: (1) drying and crushing a polygonum multiflorum medicinal material, adding an ethanol solution for extraction, filtering the extract, and concentrating the filtrate to a state without alcohol taste, so as to obtain a concentrated solution; (2) adding petroleum ether to the concentrated solution for extraction, adjusting the pH value of a water phase after extraction to 9-11, adding ethyl acetate for extraction, concentrating the ethyl acetate phase to obtain an extract; (3) separating and purifying the extract by a semi-preparative high performance liquid chromatography, wherein the chromatographic conditions are as below: a chromatographic column of Shim-pack PREP-ODS column, a mobile phase of acetonitrile-water, volume ratio of 25:75, and detection wavelength of 320 nm; collecting chromatographic peaks, detecting purity and merging the same fractions, so as to isolate cis-stilbene and trans-stilbene glycoside reference substances. The high purity trans-stilbene glycoside monomer and cis-stilbene glycoside monomer prepared by the invention provide pure substances for physiological activity tests.

Description

technical field [0001] The invention relates to a preparation method of cis- and trans-stilbene glycoside reference substances in Radix Polygoni Multiflori. Background technique [0002] Polygonum multiflorum is the dry tuber root of Polygonum multiflorum Thunb. of the Polygonaceae plant, detoxifying, eliminating carbuncle, cutting off malaria, moistening intestines and defecating. For sore carbuncle, scrofula, rubella pruritus, chronic malaria, physical weakness, dryness of the intestine and constipation. Stilbene glycoside (2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside) is one of the main active substances in Radix Polygoni Multiflori, and its content is stipulated in Chinese Pharmacopoeia Wu Wu should not be less than 1%, making Shou Wu should not be less than 0.7%. There are cis-trans isomers of stilbene glycosides, and the trans-stilbene glycosides (as shown in structural formula B) in Polygonum multiflorum under light conditions are partially converted into cis str...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/08
Inventor 王岱杰王晓耿岩玲段文娟赵恒强于金倩闫慧娇
Owner SHANDONG ANALYSIS & TEST CENT
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