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Method for determining content of related components of four bear gall powder in cooling-based phlegm eliminating injection

A measurement method and injection technology, applied in the field of chemistry, can solve the problems of low precision and poor reproducibility, and achieve the effects of high precision, stable results and remarkable curative effect

Active Publication Date: 2021-01-08
SHANGHAI KAIBAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Among them, the content of ursodeoxycholic acid and chenodeoxycholic acid in the current enterprise standard of the raw material bear bile powder extract is determined by a high-efficiency liquid phase evaporative light scattering detector, There are flat peaks in the original chromatogram, the reproducibility is poor, and the precision is low. Therefore, a method for determining the content of four bear bile powder-related components in Tanreqing injection is needed to improve the above problems.

Method used

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  • Method for determining content of related components of four bear gall powder in cooling-based phlegm eliminating injection
  • Method for determining content of related components of four bear gall powder in cooling-based phlegm eliminating injection
  • Method for determining content of related components of four bear gall powder in cooling-based phlegm eliminating injection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071]1. Select instrument: Waters Acquity high performance liquid chromatograph, Thermo Q-Exactive mass spectrometer;

[0072]2. Set chromatographic conditions: Chromatographic column: Pheomenex Luna C18 (5μm, 0.46 × 25cm); mobile phase: acetonitrile as mobile phase A, water as mobile phase B, gradient elution according to Table 2; column temperature: 30℃ ; Flow rate: 1.0ml / min; Injection volume: 1μl;

[0073]3. Set gradient elution conditions: 0~2min, volume percentage 10% mobile phase B, 2~3min, volume percentage 10-20% mobile phase B, 3~25min, volume percentage 20% – 40% mobile phase B, 25~55min, volume percentage concentration 40-42% mobile phase B;

[0074]4. Set mass spectrometry conditions: acquisition mode: negative mode; scanning range m / z: 70~1050. Ion source parameters: ion source temperature 325℃; capillary voltage 3500V; sheath gas is 40arb, auxiliary gas is 10arb; resolution is 70000;

[0075]5. According to the above method, search with precise molecular weight and compare the r...

Embodiment 2

[0091]Determination of 4 components in bear bile powder extract

[0092]1. Select instruments and reagents: Agilent 1260 high performance liquid chromatograph, ursodeoxycholic acid reference substance and chenodeoxycholic acid reference substance from China Pharmaceutical and Biological Products Inspection Institute, 3α-hydroxy-7-oxo-5β- Cholanic acid (TRC, 1-ALB-5-1), 7α-hydroxy-3-oxo-5 β-cholanoic acid (UHN, 4185-00-6), acetonitrile and methanol are chromatographically pure, bear bile powder Extracts and other reagents are of analytical grade;

[0093]2. Setting conditions: Chromatographic column: Pheomenex luna omega C18 (5μm, 0.46 × 25cm), mobile phase: acetonitrile as mobile phase A and 0.1% phosphoric acid as mobile phase B, column temperature: 30℃, flow rate: 1.0ml / min, injection volume: 10μl, with 203nm as the UV absorption detection wavelength;

[0094]3. Set gradient elution conditions: 0~10min, 90-45% volume percentage mobile phase B, 10~35min, volume percentage 45% mobile phase ...

Embodiment 3

[0104]Determination of 4 kinds of bear bile powder related components in Tanreqing injection, chromatographic conditions are the same as in Example 2

[0105]1. Take a blank sample (lack of bear bile powder) and a sample, prepare a blank sample solution and a test solution in parallel according to the preliminarily developed method, and analyze the samples. The result is that the test product chromatogram contains a reference substance with ursodeoxycholic acid. , 3α-hydroxy-7-oxo-5β-cholanic acid reference substance, chenodeoxycholic acid reference substance and 7α-hydroxy-3-oxo-5β-cholanic acid reference substance have the same retention time chromatographic peaks, and Without interference from other components, the blank sample (ursodeoxycholic acid powder) is in ursodeoxycholic acid reference substance, 3α-hydroxy-7-oxo-5β-cholanoic acid reference substance, chenodeoxycholic acid reference substance and 7α-hydroxy There is no chromatographic peak at the retention time of the refere...

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Abstract

The invention relates to the field of chemistry, in particular to a method for determining the content of related components of four bear gall powder in cooling-based phlegm eliminating injection. Themethod comprises the following steps: S1, preparing a reference solution; S2, preparing a test solution; S3, performing detecting by using a high performance liquid chromatograph-mass spectrometer; S4, carrying out qualitative detection; and S5, performing quantitative detection: according to the method, under the condition set by a high performance liquid chromatograph-mass spectrometer, respectively carrying out determination, repeating the process for 6 times, determining the peak area of the corresponding concentration, and carrying out linear regression to obtain a regression equation soas to obtain a correlation coefficient and a linear range and determine the contents of the four bear gall powder related components in the cooling-based phlegm eliminating injection. The method canbe used for qualitatively analyzing ursodeoxycholic acid, 3alpha- hydroxyl-7oxo-5beta-cholanic acid, chenodeoxycholic acid and 7alpha- hydroxyl-3-oxo-5beta-cholanic acid of the cooling-based phlegm eliminating injection and the bear gall powder extract, and is simple and convenient to operate, stable in result, good in reproducibility and high in precision.

Description

Technical field[0001]The invention belongs to the field of chemistry and relates to a method for determining the content of four kinds of bear bile powder related components in Tanreqing injection.Background technique[0002]Tanreqing injection is extracted and refined from five medicinal materials of scutellaria baicalensis, bear bile powder, goat horn, honeysuckle and forsythia. It has the effects of clearing heat, detoxifying, and reducing phlegm. It is used in the treatment of upper respiratory tract infections, acute bronchitis, pneumonia, Pulmonary tuberculosis complicated by pulmonary infection, advanced lung cancer complicated by pulmonary infection, severe asthma complicated by infection and other aspects have significant effects.[0003]Among the raw materials, bear gall powder extract, the current corporate standards of ursodeoxycholic acid and chenodeoxycholic acid are determined by using a high performance liquid evaporative light scattering detector. A flat peak appears in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/74
CPCG01N30/02G01N30/74Y02A50/30
Inventor 季申李雯婷苗水胡青毛秀红穆竟伟张小利李丽敏王少敏周恒兰岚张静娴
Owner SHANGHAI KAIBAO PHARMA
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