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Quantitative analysis method for dioscin in compounded traditional Chinese medicine preparation

A technology of dioscin and compound preparations, which is applied in the field of quantitative analysis of dioscin, can solve problems such as large fluctuations in the baseline of chromatographic peaks, interference of solvent peaks on target peaks, etc., and achieve improved quality control levels, simple and fast preparation methods, and high accuracy high effect

Inactive Publication Date: 2015-03-11
TIANJIN UNIV
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Problems solved by technology

Diosgenin belongs to steroidal saponins, and its UV absorption belongs to the terminal absorption. Due to the complexity of the traditional Chinese medicine compound preparation made of Chuanshanlong and Acanthopanax as medicinal materials, the baseline of the chromatographic peak fluctuates greatly under the condition of ultraviolet detection, and the solvent peak has great influence on the target peak. Large interference, using diode array detector (DAD) detection method can not make the target peak and impurity peak achieve baseline separation

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  • Quantitative analysis method for dioscin in compounded traditional Chinese medicine preparation
  • Quantitative analysis method for dioscin in compounded traditional Chinese medicine preparation
  • Quantitative analysis method for dioscin in compounded traditional Chinese medicine preparation

Examples

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Embodiment 1

[0025] A method for quantitative analysis of diosgenin in compound Chinese medicine capsules, comprising the steps of:

[0026] (1) Preparation of reference substance solution: Take an appropriate amount of diosgenin reference substance, weigh it accurately, add methanol to make a solution (1) containing 1.0mg per 1mL, and accurately draw 2.5mL from the reference substance solution (1) into a 10mL volumetric flask , add methanol to constant volume, and prepare a diosgenin reference solution (2) containing 250 μg per 1 mL;

[0027] (2) Preparation of the test solution: take the contents of the compound capsule of traditional Chinese medicine and grind it finely, pass through a No. 4 sieve, take about 0.4g, accurately weigh it as 0.3750g, put it in a stoppered Erlenmeyer flask, add 25mL of methanol precisely, and weigh it. For weight, ultrasonically treat for 50 minutes under the conditions of power 120W and frequency 40kHz, let cool to room temperature, weigh again, make up the...

Embodiment 2

[0030] A method for quantitative analysis of diosgenin in compound Chinese medicine tablets, comprising the steps of:

[0031] (1) prepare reference substance solution; Step is with embodiment 1 step (1);

[0032] (2) Preparation of the test solution: get the Chinese medicine compound tablet and grind it finely, pass through a No. 4 sieve, get about 0.4g, accurately weigh it as 0.3745g, put it in a stoppered Erlenmeyer flask, add methanol 25mL precisely, weigh it, Under the conditions of power 120W and frequency 40kHz, ultrasonically treat for 60min, let cool to room temperature, weigh again, make up the lost weight with methanol, shake well, filter, and take the filtrate to obtain the final product;

[0033] (3) content determination: get the reference substance solution that step (1) obtains and the need testing solution that step (2) obtains respectively in high performance liquid chromatography detection condition is: C 18 A chromatographic column with bonded silica gel a...

Embodiment 3

[0035] A method for quantitative analysis of diosgenin in traditional Chinese medicine compound granules, comprising the steps of:

[0036] (2) prepare reference substance solution; Step is with embodiment 1 step (1);

[0037] (2) Preparation of the test solution: get the Chinese medicine compound granule and grind it finely, pass through a No. 4 sieve, get about 0.4g, accurately weigh it as 0.3752g, put it in a stoppered conical flask, add methanol 25mL precisely, weigh it, and Under the conditions of power 120W and frequency 40kHz, ultrasonically treat for 55min, let cool to room temperature, weigh again, make up the lost weight with methanol, shake well, filter, and take the filtrate to obtain the final product;

[0038] (3) content determination: get the reference substance solution that step (1) obtains and the need testing solution that step (2) obtains respectively in high performance liquid chromatography detection condition is: C 18 Bonded silica gel is used as a chr...

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Abstract

The invention discloses a quantitative analysis method for dioscin in a compounded traditional Chinese medicine preparation. The quantitative analysis method comprises the following steps: (1) preparing a control solution; (2) preparing a test solution; and (3) testing the content, namely, respectively eluting the control solution prepared in the step (1) and the test solution prepared in the step (2) under the high performance liquid chromatography detection condition that a chromatographic column which adopts C18 bonded silica gel as a filling agent is used, and by using acetonitrile-water as mobile phase, performing high performance liquid chromatography detection by using an evaporative light-scattering detector as a detector so as to obtain high performance liquid chromatography spectrums of the control solution and the test solution, and measuring the content of dioscin in a test sample by using an external standard method. The quantitative analysis method is simple, convenient and rapid to operate, high in accuracy and good in repeatability, and the quality control level of a product can be increased.

Description

technical field [0001] The invention relates to a quantitative analysis method for diosgenin in a compound traditional Chinese medicine preparation. Background technique [0002] The main medicinal ingredients of the traditional Chinese medicine compound preparation made of Chuanshanlong and Acanthopanax as medicinal materials include diosgenin (diosgenin), trillium, methyldioscin, protodioscin, syringin (eleutheroside B), Eleutheroside E, isoferidin, quercetin, chlorogenic acid, syringetin, etc., the current "Chinese Pharmacopoeia" 2010 edition of the determination of the content of the medicinal materials in the Chinese Pharmacopoeia adopts high performance liquid chromatography with dioscin as the detection index at a wavelength of 203nm Determine its content below. Diosgenin belongs to steroidal saponins, and its UV absorption belongs to the terminal absorption. Due to the complexity of the traditional Chinese medicine compound preparation made of Chuanshanlong and Acan...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 蒋建兰孙秀婷
Owner TIANJIN UNIV