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Method for separating and determining carbocisteine and impurities thereof by liquid chromatography

A technology of carbocisteine ​​and high-performance liquid chromatography, which is applied in the field of drug analysis, can solve problems such as simultaneous separation and determination of carbocisteine, and achieve the effects of quality controllability, good repeatability, and high precision

Active Publication Date: 2021-05-11
广东逸舒制药股份有限公司 +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The applicant found that the above patent documents can only partially separate and measure carbocisteine ​​and its impurities, and cannot achieve simultaneous separation and determination of carbocisteine ​​and the seven impurities, and there is no report on carbocisteine ​​and the seven impurities. Simultaneous separation and determination method, the present invention starts from the deficiencies in the prior art, provides a kind of analysis method, can accurately, rapid separation and determination carbocisteine ​​and these seven impurities, and does not contain organic solvent in mobile phase, to the analytical instrument Lower requirements, and then control the quality of carbocisteine ​​in daily production, improve the efficacy of drugs, and reduce toxic and side effects

Method used

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  • Method for separating and determining carbocisteine and impurities thereof by liquid chromatography
  • Method for separating and determining carbocisteine and impurities thereof by liquid chromatography
  • Method for separating and determining carbocisteine and impurities thereof by liquid chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0049] Instrument: Agilent 1260 Infinity II;

[0050] Chromatographic column: ZORBAX SB-Aq chromatographic column (4.6mm×250mm, 5μm);

[0051] Mobile phase: 20mmol / L potassium dihydrogen phosphate-9.2mmol / L sodium octane sulfonate ion-pair buffer;

[0052] Column temperature: 25°C;

[0053] Flow rate: 1mL / min;

[0054] Detection wavelength: 215nm;

[0055] Preparation containing carbocisteine ​​and its impurity concentration: 2mg / mL;

[0056] Injection volume: 25μL;

[0057] Preparation of mobile phase: Take 2.72g of potassium dihydrogen phosphate and 2g of sodium octane sulfonate, add water to dissolve and dilute to 1000mL, adjust the pH value to 1.7 with phosphoric acid;

[0058] Preparation of positioning solution: Accurately weigh 5mg of impurity A, impurity B, impurity C, impurity D, impurity E, impurity F, and impurity G respectively, and place them in 50mL measuring bottles and add diluent (0.02mol / L dipotassium hydrogen phosphate Solution) was dissolved and dilut...

Embodiment 2

[0062] Instrument: Agilent 1260 Infinity;

[0063] Chromatographic column: Shim-pack GIST C18 chromatographic column (4.6mm×250mm, 5μm);

[0064] Mobile phase: 15mmol / L sodium dihydrogen phosphate-8.0mmol / L sodium octanesulfonate ion-pair buffer;

[0065] Column temperature: 23°C;

[0066] Flow rate: 0.8mL / min;

[0067] Detection wavelength: 215nm;

[0068] Preparation containing carbocisteine ​​and its impurity concentration: 1mg / mL;

[0069] Injection volume: 20μL;

[0070] Preparation of mobile phase: Take 1.8g of sodium dihydrogen phosphate and 1.73g of sodium octane sulfonate, add water to dissolve and dilute to 1000mL, adjust the pH value to 1.6 with phosphoric acid;

[0071] Solution preparation method and assay method are carried out according to embodiment 1, and the collection of illustrative plates of carbocisteine ​​tablet solution sees figure 2 . The chromatographic conditions of this embodiment can effectively distinguish the peaks of carbocisteine ​​and ...

Embodiment 3

[0073] Instrument: Agilent 1260 Infinity;

[0074] Chromatographic column: CAPCELL PAK C18 AQ chromatographic column (4.6mm×250mm, 5μm);

[0075] Mobile phase: 25mmol / L dipotassium hydrogen phosphate-12.5mmol / L sodium octanesulfonate ion-pair buffer;

[0076] Column temperature: 30°C;

[0077] Flow rate: 1.2mL / min;

[0078] Detection wavelength: 215nm;

[0079] Preparation containing carbocisteine ​​and its impurity concentration: 2.5mg / mL;

[0080] Injection volume: 30μL;

[0081] Preparation of mobile phase: Take 4.3g of dipotassium hydrogen phosphate and 2.70g of sodium octane sulfonate, add water to dissolve and dilute to 1000mL, adjust the pH value to 2.0 with phosphoric acid;

[0082] Solution preparation method and assay method are carried out according to embodiment 1, and the collection of illustrative plates of carbocisteine ​​tablet solution sees image 3 . The results showed that the qualitative detection and quantitative detection of impurities A~G could be...

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Abstract

The invention discloses a method for separating and determining carbocisteine and impurities thereof by high performance liquid chromatography. The determination method adopts a chromatographic column taking octadecylsilane chemically bonded silica as a filler, and the detection conditions are as follows: chromatographic conditions: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column, a mobile phase is a phosphate-ion pair buffer solution, the pH value of the mobile phase is 1.6-2.0, and the detection wavelength is 215 nm. The method disclosed by the invention is high in precision, good in repeatability and high in recovery rate, and can be widely applied to quality detection of carbocisteine raw material medicines from different sources and corresponding preparations thereof.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for separating and measuring carbocisteine ​​and its impurities by high performance liquid chromatography. Background technique [0002] Carbocysteine ​​(Carbocysteine) is a phlegm-reducing and cough-relieving medicine used to treat cough and expectoration caused by diseases such as chronic bronchitis and bronchial asthma. In addition, it can be used for non-suppurative otitis media in children to prevent deafness. Carbocysteine The chemical name of Stein is S-(carboxymethyl)cysteine ​​(S-Carboxymethyl-L-cysteine), and the molecular formula is C 5 h 9 NO 4 S. The molecular weight is 179.19, and the structural formula of carbocisteine ​​is: [0003] [0004] During the production and storage of carbocisteine, the purity of the drug may be affected due to incomplete removal of starting materials and intermediates and degradation impurities generated during storage. Thes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8809
Inventor 程志伟吴健辉孙金鑫顾云
Owner 广东逸舒制药股份有限公司
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