Tripterygium wilfordii medicinal material and method for determining wilforlidea in tripterygium wilfordii polyglycosides tablet

A technology of triptolide A and its determination method, which is applied in the direction of measuring devices, material separation, and analysis materials, etc., to achieve the effects of reduced separation cost, good reproducibility, and good separation effect

Active Publication Date: 2020-01-14
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, liquid-liquid partition chromatography is mostly used for the separation and purification of one or more substances, but there is no relevant report on the study of using it as a sample pretreatment technology to enrich relatively small target components in complex samples

Method used

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  • Tripterygium wilfordii medicinal material and method for determining wilforlidea in tripterygium wilfordii polyglycosides tablet
  • Tripterygium wilfordii medicinal material and method for determining wilforlidea in tripterygium wilfordii polyglycosides tablet
  • Tripterygium wilfordii medicinal material and method for determining wilforlidea in tripterygium wilfordii polyglycosides tablet

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Experimental program
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Effect test

Embodiment 1

[0034] 1. Instruments and reagents

[0035] 1.1 Instrument: Shanghai Wufeng LC100 liquid chromatograph; TBE-200V high-speed countercurrent distribution chromatography;

[0036] 1.2 Reagents and reagents: standard triptolide A (source: Chengdu Master Biotechnology Co., Ltd.) phosphoric acid is analytically pure; acetonitrile is chromatographically pure; n-hexane is analytical grade; ethyl acetate is analytical grade; ethanol is analytical grade Grade; water is double-distilled water; chromatographic column is phenomenonex SYNERGI (250×4.6mm 4u); see Table 5 and Table 7 below for the source and origin of samples.

[0037] 2. Methods and results:

[0038] 2.1 Preparation of the reference substance solution of triptolide A: accurately weigh an appropriate amount of the reference substance of triptolide A, dissolve it with ethanol and dilute it into a reference solution containing 0.1 mg / mL of triptolide A;

[0039] 2.2 Preparation of the test solution:

[0040] ① Preparation of...

Embodiment 2

[0065] Preparation of triptolide A reference substance solution: accurately weigh an appropriate amount of triptolide A reference substance, dissolve it with ethanol and dilute it into a reference substance solution containing 0.1 mg / mL of triptolide A;

[0066] The preparation of need testing solution: 1. the preparation of solvent system: n-hexane, ethyl acetate, ethanol, aqueous solution are mixed by volume ratio 7:3:7:3, shake vigorously 5min then, be placed in separating funnel, static After layering, the upper phase solution was used as the stationary phase, and the lower phase solution was used as the mobile phase, and ultrasonic degassed for 15 minutes;

[0067] ② Rough extraction of samples: Take 20 tripterygium glycosides tablets and grind them finely (sample 3), accurately weigh 1.5g, add 50mL ethyl acetate, ultrasonicate for 30min, wash with 90mL ethyl acetate for 3 times, combine the filtrate and The washing solution was evaporated to dryness, and the residue was ...

Embodiment 3

[0075] Three kinds of Tripterygium wilfordii medicinal materials from different origins were taken to determine the content of triptolide A. The sample numbers and origins are shown in Table 6. Sample 7 was taken as an example:

[0076] Preparation of triptolide A reference substance solution: accurately weigh an appropriate amount of triptolide A reference substance, dissolve it with ethanol and dilute it into a reference substance solution containing 0.1 mg / mL of triptolide A;

[0077] The preparation of need testing solution: 1. the preparation of solvent system: normal hexane, ethyl acetate, ethanol, aqueous solution are mixed by volume ratio 3:2:3:2, shake vigorously then 5min, be placed in separating funnel, static After layering, the upper phase solution was used as the stationary phase, and the lower phase solution was used as the mobile phase, and ultrasonic degassed for 15 minutes;

[0078] ②Coarse extraction of samples: crush the medicinal material of Tripterygium w...

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Abstract

The invention provides a tripterygium wilfordii medicinal material and a method for determining wilforlidea in a tripterygium wilfordii polyglycosides tablet. The method comprises the following stepsof taking an ethanol solution of 0.1 mg.mL<-1> of wilforlidea as a reference substance solution; acquiring a corresponding volume ratio range by establishing and optimizing normal hexane, ethyl acetate, ethanol and water of a solvent system so that a distribution coefficient K of the wilforlidea in the solvent system is 0.5-2; optimizing and controlling a rotating speed of a liquid-liquid distribution chromatographic separation column and a flowing speed of a mobile phase, and detecting the tripterygium wilfordii medicinal material and the method for determining the wilforlidea in the tripterygium wilfordii polyglycosides tablet by combining high performance liquid chromatography. The method is simple in operation process, high in specificity and good in reproducibility, separation cost isgreatly reduced, a wilforlidea chromatographic separation degree is high, a product recovery rate is high too, a sample dosage is small, stability is good, precision is high, qualitative and quantitative accuracy is high too, and quality of the tripterygium wilfordii medicinal material and the tripterygium wilfordii polyglycosides tablet can be effectively evaluated.

Description

technical field [0001] The invention relates to a method for determining triptolide A in tripterygium wilfordii medicinal material and its preparation tripterygium polyglycoside tablets, belonging to the technical field of quality control of Chinese medicinal materials and medicines. Background technique [0002] Tripterygium wilfordii (Tripterygiμm wilfordii Hook.f.) is a perennial vine of the genus Tripterygium in the family Celastraceae, and the medicinal part is the whole root or the xylem of the peeled root. Modern pharmacological and clinical studies have found that Tripterygium wilfordii has various biological activities such as anti-inflammatory immune regulation, anti-tumor and anti-fertility, anti-oxidation, anti-HIV virus and therapeutic effect on Alzheimer's disease. Tripterygium wilfordii polyglycoside is a mixture of effective parts extracted and refined from its roots, and it is the first anti-inflammatory and immune-regulating traditional Chinese medicine ext...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N30/14G01N30/74G01N30/54
CPCG01N30/02G01N30/06G01N30/08G01N30/14G01N30/74G01N30/54G01N2030/027G01N2030/062G01N2030/146
Inventor 童胜强赵姗姗
Owner ZHEJIANG UNIV OF TECH
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