Method for analyzing genotoxic impurities in pantoprazole sodium and starting raw materials of pantoprazole sodium

A technology for pantoprazole sodium and genotoxicity, applied in the directions of material separation, analysis materials, measuring devices, etc., can solve the problems of separation and determination methods that have no public reports, etc., achieve high accuracy, simple and convenient experimental operation method, strong specific effect

Active Publication Date: 2019-11-22
INST OF MATERIA MEDICA AN INST OF THE CHINESE ACAD OF MEDICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] At present, there is no public report about the separation and determination method for the s

Method used

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  • Method for analyzing genotoxic impurities in pantoprazole sodium and starting raw materials of pantoprazole sodium
  • Method for analyzing genotoxic impurities in pantoprazole sodium and starting raw materials of pantoprazole sodium
  • Method for analyzing genotoxic impurities in pantoprazole sodium and starting raw materials of pantoprazole sodium

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0059] Embodiment 1, the separation and determination method of potential genotoxic impurity in pantoprazole sodium

[0060] (1) Instruments and Conditions

[0061] Shimadzu LC-MS / MS8050 high performance liquid chromatography triple quadrupole mass spectrometer;

[0062] Column: Alltima C 18 Chromatography column (150mm×4.6mm, 5μm);

[0063] Mobile phase: 0.02mol / L ammonium acetate:acetonitrile (40:60);

[0064] Flow rate: 0.5ml / min;

[0065] Column temperature: 40℃;

[0066] Injection volume: 10 μL;

[0067] Solvent: acetonitrile-water (50:50).

[0068] Mass spectrometry conditions: Electrospray ionization (ESI), positive ion scanning mode;

[0069] The atomizing gas, drying gas and heating gas are nitrogen, and the collision gas is argon;

[0070] The atomizing gas flow rate is 3L / min;

[0071] The drying gas flow rate is 10.0L / min;

[0072] The heating gas flow rate is 10.0L / min;

[0073] The interface temperature is 300℃;

[0074] The temperature of the curved ...

Example Embodiment

[0090] Embodiment 2. Separation and determination method of potential genotoxic impurities in 5-difluoromethoxy-2-mercapto-1H-benzimidazole

[0091] (1) Instruments and Conditions

[0092] Shimadzu Agilent 6410B Triple Quadrupole LC-MS high performance liquid chromatography-triple quadrupole tandem mass spectrometer;

[0093] Column: Alltima C 18 Chromatography column (150mm×4.6mm, 5μm);

[0094] Mobile phase: 0.005Mol / L ammonium acetate aqueous solution (containing 0.1% formic acid): methanol (60:40)

[0095] Flow rate: 0.5ml / min;

[0096] Column temperature: 40℃;

[0097] Injection volume: 10 μL;

[0098] Solvent: methanol.

[0099] Mass spectrometry conditions: ion source is electrospray ion source, positive ion scanning mode;

[0100] Gas Temp: 300℃;

[0101] Gas Flow: 10L / min;

[0102] Nebulizer: 30psi;

[0103] Capillary: 5500V.

[0104] MRM detection mode, the parameters are as follows:

[0105]

[0106]

[0107] (2) Experimental steps

[0108] Sample (...

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Abstract

The invention belongs to the field of pharmaceutical analytical chemistry, and particularly relates to two methods for analyzing and measuring potential genotoxic impurities in pantoprazole sodium anda synthetic starting material 5-difluoromethoxy-2-mercapto-1H-benzimidazole thereof. According to the method, octadecylsilane chemically bonded silica is used as a stationary phase, and a mass spectrometry detector is used for analysis and determination; the mobile phase is an aqueous solution containing acetonitrile, methanol and organic ammonium salt; the structural types of the potential genotoxic impurities comprise halogenated methylpyridine compounds, azaaryl N-oxides, N-acylated aminobenzene compounds, aromatic amines compounds and nitrobenzene compounds. According to the method, the effective separation of potential genotoxic impurities in pantoprazole sodium and synthesis starting raw materials of pantoprazole sodium can be realized, the genotoxic impurities can be accurately andquantitatively determined; the method is high in sensitivity and specificity; the experimental operation is simple, convenient and rapid, and the method has important significance for quality controland medication safety of pantoprazole sodium.

Description

technical field [0001] The invention belongs to the field of pharmaceutical analytical chemistry, and specifically relates to two methods for analyzing and measuring potential genotoxic impurities, which are respectively used for pantoprazole sodium and its synthetic starting material 5-difluoromethoxy-2-mercapto-1H-benzene Analysis and limit determination of potential genotoxic impurities in imidazoles. Background technique [0002] Pantoprazole Sodium (Pantoprazole Sodium), the chemical name is 5-difluoromethoxy-2-[[(3,4-dimethoxy-2-pyridyl)-methyl]sulfinyl]-1H - Sodium benzimidazole monohydrate, the molecular formula is C 16 h 14 f 2 N 3 o 4 S·H 2 O, its structural formula is: [0003] [0004] Pantoprazole sodium is a proton pump inhibitor that can highly selectively act on DA-2 receptors, selectively act on gastric mucosal parietal cells, and inhibit H in the cell wall. + / K + -ATPase activity, making H in parietal cells + Can not be transported into the st...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/14G01N30/86
CPCG01N30/02G01N30/14G01N30/8679
Inventor 杨庆云吴松张金兰王琰王喆符洁马春华张文轩李天磊夏杰陈谕园
Owner INST OF MATERIA MEDICA AN INST OF THE CHINESE ACAD OF MEDICAL SCI
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