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Content detection method of 14 non-volatile components in dragon tiger Rendan mini-pill vegetable drug

A technology of volatile components and detection methods, which is applied in the field of content determination of traditional Chinese medicine components, and can solve problems such as long detection time and complicated processing steps

Inactive Publication Date: 2015-09-23
SHANGHAI ZHONGHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the quality control methods of Longhu Rendan mainly include microscopic identification, thin layer identification, high performance liquid chromatography and gas chromatography. Zhang Yujie et al. used gas chromatography to determine the content of borneol and menthol in it. A single component in Longhu Rendan, the detection time is long, the pre-treatment steps of the sample detection are complicated, etc.
So far, there is no research report on the simultaneous detection of multiple components in Longhuren Dan, and there is no such compound (1) catechin, (2) epicatechin, (3) schaftoside, (4) ) Liquiritin, (5) Isoliquiritin, (6) Glycyrrhizin, (7) Glycyrrhizalcone, (8) Glycyrrhizic Acid, (9) Isoliquiritigenin, (10) Piperine, (11) Glycyrrhizin Simultaneous Determination Method of Corone A, (12) Coynelide, (13) Dehydrocoylidene, (14) Glycyrrhetinic Acid

Method used

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  • Content detection method of 14 non-volatile components in dragon tiger Rendan mini-pill vegetable drug
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  • Content detection method of 14 non-volatile components in dragon tiger Rendan mini-pill vegetable drug

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] 1. Instruments and reagents

[0052] Instrument: UFLC XR (Shimadzu Corporation, Japan) liquid phase-LCQ ion trap mass spectrometer (Thermo Fisher Scientific Corporation, Germany).

[0053] Test medicine: Longhu Rendan botanical medicine

[0054] Other reagents: acetonitrile, acetone, methanol, ethylene glycol, formic acid

[0055] 2. Method

[0056] (1) Preparation of the test solution: take Longhu Rendan herbal medicinal solvent to prepare a 0.3-2mg / ml test solution;

[0057] Preparation of the reference substance solution: Accurately weigh an appropriate amount of the reference substance, place it in a 10mL volumetric flask, dissolve it with a solvent and dilute to the mark. Shake well to obtain the stock solution of each reference substance, and store in a refrigerator at 4°C.

[0058] Precisely measure the appropriate amount of each stock solution, and dilute it with acetonitrile-water (30:70, v / v) to obtain a mixed standard solution of each reference substance. ...

Embodiment 2

[0080] 1. Instruments and reagents

[0081] Instrument: UFLC XR (Shimadzu Corporation, Japan) liquid phase-LCQ ion trap mass spectrometer (Thermo Fisher Scientific Corporation, Germany).

[0082] Test medicine: Longhu Rendan botanical medicine

[0083] Other reagents: acetonitrile, acetone, methanol, ethylene glycol, formic acid

[0084] 2. Method

[0085] (1) Preparation of the test solution: take Longhu Rendan herbal medicinal solvent to prepare a 0.3-2mg / ml test solution;

[0086] Preparation of the reference substance solution: Accurately weigh an appropriate amount of the reference substance, place it in a 10mL volumetric flask, dissolve it with a solvent and dilute to the mark. Shake well to obtain the stock solution of each reference substance, and store in a refrigerator at 4°C.

[0087] Precisely measure the appropriate amount of each stock solution, and dilute it with acetonitrile-water (30:70, v / v) to obtain a mixed standard solution of each reference substance....

Embodiment 3

[0110] 1. Instruments and reagents

[0111] Instrument: UFLC XR (Shimadzu Corporation, Japan) liquid phase-LCQ ion trap mass spectrometer (Thermo Fisher Scientific Corporation, Germany).

[0112] Test medicine: Longhu Rendan botanical medicine

[0113] Other reagents: acetonitrile, acetone, methanol, ethylene glycol, formic acid

[0114] 2. Method

[0115] (1) Preparation of the test solution: take Longhu Rendan herbal medicinal solvent to prepare a 0.3-2mg / ml test solution;

[0116] Preparation of reference substance solution: Accurately weigh an appropriate amount of reference substance, place it in a 10mL volumetric flask, add 30% acetonitrile solvent to dissolve and dilute to the mark. Shake well to obtain the stock solution of each reference substance, and store in a refrigerator at 4°C.

[0117] Precisely measure the appropriate amount of each stock solution, and dilute it with acetonitrile-water (30:70, v / v) to obtain a mixed standard solution of each reference subs...

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Abstract

The invention provides a method for detecting contents of 14 non-volatile components in a dragon tiger Rendan mini-pill vegetable drug by liquid chromatography-LCQ ion trap mass spectrometry. The method comprises the following steps: firstly preparing a test solution and a control solution, and respectively detecting according to the following method: introducing a sample to a Thermo BDS Hypersil C18 chromatographic column according to the sample size of 1-20 microliters, controlling column temperature to 20-40 DEG C, carrying out gradient elution with a mobile phase composed of a phase A and a phase B at the speed of 0.2-1.5 mL / min according to an established procedure, simultaneously detecting an eluant by the liquid chromatography-LCQ ion trap mass spectrometry to obtain ion chromatograms of a test sample medicine and a control medicine, and detecting each component and its content through comparison of the chromatograms. The phase A of the mobile phase is pure water containing 0.005-0.015% of formic acid (containing 0.2mM of ammonium formate), and the phase B is acetonitrile.

Description

technical field [0001] The invention relates to a content determination method and a quality control method of traditional Chinese medicine components, in particular to a content detection method and a quality control method of Longhu Rendan botanical medicine. Background technique [0002] Longhu Ren Dan (Z20025168) was created in 1909 by Mr. Huang Chujiu according to the ancient prescription "Zhuge Xingjun Powder". Its functions and indications are clearing away summer-heat and resuscitating, warding off filth and turbidity, dispelling wind and invigorating the stomach. In 1923, the "Dragon Tiger Brand" and "Rendan and Pattern" trademarks were applied to and approved by the government, and became the first standardized pharmaceutical registered trademarks in China, marking the beginning of the national pharmaceutical industry in Shanghai and even in China. Over the past century, the sales of Longhu Rendan products have lasted for a long time, and it has become an exclusiv...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 金家骅丁礼琴杜子荣马越鸣王天明
Owner SHANGHAI ZHONGHUA PHARMA
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