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Construction method of specific chromatogram of volatile components in Zhengtian pill preparation and detection method of volatile components in Zhengtian pill preparation

A technology of volatile components and characteristic maps, which is applied in the field of detection of traditional Chinese medicine preparations, to achieve good separation, large number of peaks, and good map integrity

Active Publication Date: 2016-05-04
CHINA RESOURCES SANJIU MEDICAL & PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Therefore, in view of the fact that there is no more comprehensive quality control method in the prior art to reflect the quality status of the volatile drug components in Zhengtian pill preparations, a method for detecting various volatile drug ingredients in Zhengtian pills is constructed to It is of great significance to control the quality of Zhengtian pill preparations as a whole and effectively

Method used

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  • Construction method of specific chromatogram of volatile components in Zhengtian pill preparation and detection method of volatile components in Zhengtian pill preparation
  • Construction method of specific chromatogram of volatile components in Zhengtian pill preparation and detection method of volatile components in Zhengtian pill preparation
  • Construction method of specific chromatogram of volatile components in Zhengtian pill preparation and detection method of volatile components in Zhengtian pill preparation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] The construction method of the characteristic map of the volatile components in the Zhengtian pill preparation described in this embodiment comprises the following steps:

[0052] (1) Preparation of the test solution: Take 15g of Zhengtian pill preparation powder (passed through a No. 3 sieve), accurately weigh it, put it in a flask, add 240mL of distilled water and glass beads, connect the volatile oil extractor, add water from the upper end of the volatile oil extractor to Add 2 mL of ethyl acetate quantitatively from the upper end of the volatile oil extractor until water overflows into the flask, and keep it in a slightly boiling state for 2 hours; after cooling, collect the ethyl acetate layer and add ethyl acetate to make it to 2 mL, add anhydrous sulfuric acid Sodium, stand still, take the upper layer, filter;

[0053] (2) Preparation of the reference substance solution: take the ligustilide reference substance and accurately weigh it, add methanol to prepare a r...

Embodiment 2

[0074] The detection method of the volatile components in the Zhengtian pill preparation described in this embodiment comprises the following steps:

[0075] (1)供试品溶液制备:将16批正天丸制剂(批号:1503023H、1503024H、1503025H、1503026H、1503027H、1503028H、1503029H、1503030H、1503031H、1503032H、1503033H1503034H,1407025H,1408001H,1408003H,1408027H,华润 Provided by Sanjiu Pharmaceutical Co., Ltd.), each batch took 15g of Zhengtian pill preparation powder (passed through a No. 3 sieve), accurately weighed, put in a flask, added 240mL of distilled water and glass beads, connected to a volatile oil extractor, and extracted from the volatile oil Add water to the upper end of the extractor until water overflows into the flask, and quantitatively add 2 mL of ethyl acetate from the upper end of the volatile oil extractor, and keep it in a slightly boiling state for 2 hours; after cooling, collect the ethyl acetate layer and add ethyl acetate to dilute to 2 mL. Add anhydrous sodium sulfate, let stand, take the su...

experiment example 1

[0083] Experimental example 1 condition optimization

[0084] 1. Instruments and reagents

[0085] 1.1 Instrument

[0086] Shimadzu GC-2014 gas chromatograph (Shimadzu Corporation of Japan);

[0087] DFID detector (Shimadzu Corporation of Japan);

[0088] RTX-5 capillary column (30m×0.25mm×0.25μm, Restek),

[0089] 1.2 Reagent

[0090] Ethyl acetate (analytical pure), produced by Shanghai Aladdin Biochemical Technology Co., Ltd.; ligustilide reference substance (batch number: 111737-201305; ID number: LTVC-SY2T), purchased from China National Institutes for Food and Drug Control;

[0091] Methyl eugenol reference substance (batch number: 111642-200301), purchased from China Food and Drug Control Institute; ferulic acid reference substance (batch number: 110773-201313; ID number: 6WOF-B3AT), purchased from China Food and Drug Control hospital;

[0092] 16批正天丸制剂样品(批号:1503023H、1503024H、1503025H、1503026H、1503027H、1503028H、1503029H、1503030H、1503031H、1503032H、1503033H1503034H,...

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Abstract

The invention relates to a construction method of a specific chromatogram of volatile components in a Zhengtian pill preparation and a detection method of the volatile components in the Zhengtian pill preparation. According to the construction method and the detection method, a water steam distillation method is used for extracting the volatile components in the Zhengtian pill preparation, the gas chromatography is used for performing specific chromatogram analysis on the volatile components, the relative retention time ratio is used as an evaluation index, the specific chromatogram of the volatile components in the Zhengtian pill preparation is built, and detection is performed on the Zhengtian pill preparation. The construction method and the detection method are good in repeatability, the characteristic peak separation degree is high, and method references are provided for overall quality control over the Zhengtian pill preparation.

Description

technical field [0001] The invention relates to the field of detection of traditional Chinese medicine preparations, in particular to a method for constructing a characteristic map of volatile components in Zhengtian pill preparations and a method for detecting volatile components in Zhengtian pill preparations. Background technique [0002] Zhengtian Pills is recorded in the 2015 edition of the Chinese Pharmacopoeia. It is developed from the clinical experience of Chen Baotian, a famous old Chinese medicine doctor from the Department of Traditional Chinese Medicine of the Nanfang Hospital of the First Military Medical University. Composed of 15 herbs including Rehmannia, Angelica, Fangfeng, Notopterygium, Peach Kernel, Safflower, Asarum, Duhuo, Ephedra, Heishun Tablets, and Caulis Spatholobus. [0003] Regarding the detection of Zhengtian pill preparations, there are microscopic identification of safflower, Caulis Spatholobus, peach kernel, and Fangfeng; Among the 7 herbs ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 王勇张保献刘志刚朱琼李琼娅聂其霞代瑶霞马鹏岗
Owner CHINA RESOURCES SANJIU MEDICAL & PHARMA
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