Method for measuring ethyl p-toluenesulfonate as genetic toxicity impurities in ibuprofen

A technology of ethyl toluenesulfonate and genotoxicity, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems such as the few methods of measuring ethyl toluenesulfonate, and achieve good specificity, short time consumption and low detection cost low effect

Inactive Publication Date: 2018-03-09
JIANGSU CHIA TAI FENGHAI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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But there is little relevant research about the assay metho

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  • Method for measuring ethyl p-toluenesulfonate as genetic toxicity impurities in ibuprofen
  • Method for measuring ethyl p-toluenesulfonate as genetic toxicity impurities in ibuprofen
  • Method for measuring ethyl p-toluenesulfonate as genetic toxicity impurities in ibuprofen

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Embodiment 1

[0060] The detection of genotoxic impurity ethyl p-toluenesulfonate in embodiment 1 ibuprofen

[0061] 1) Gas chromatography and mass spectrometry conditions:

[0062] Chromatographic column: TG-5MS (30m×0.32mm, 0.25μm);

[0063] Heating program: keep at 50°C for 2 minutes, rise to 200°C at 10°C / min, then rise to 300°C at 30°C / min and hold for 10 minutes;

[0064] Carrier gas: helium, constant flow mode;

[0065] Flow rate: 1.0mL / min;

[0066] Injection port: 280°C, splitless injection, splitless time 1min;

[0067] Injection volume: 1μl;

[0068] MS: EI source, selected ion scan mode, selected ions are m / z: 91, 92, 155;

[0069] Ion source temperature: 280°C;

[0070] Transmission line temperature: 280°C;

[0071] Solvent delay time: 5min;

[0072] 2) Solution preparation

[0073] Get 5g of ibuprofen, accurately weighed, put in a 10ml measuring bottle, add acetone to dissolve and dilute to the mark, shake well, as the test solution. Take an appropriate amount of eth...

Embodiment 2

[0076] The detection of genotoxic impurity ethyl p-toluenesulfonate in embodiment 2 ibuprofen

[0077] 1) Gas chromatography and mass spectrometry conditions:

[0078] Chromatographic column: TG-5MS (30m×0.32mm, 0.25μm);

[0079] Heating program: keep at 50°C for 2 minutes, rise to 200°C at 10°C / min, then rise to 300°C at 30°C / min and hold for 10 minutes;

[0080] Carrier gas: helium, constant flow mode;

[0081] Flow rate: 1.0mL / min;

[0082] Injection port: 280°C, splitless injection, splitless time 1min;

[0083] Injection volume: 1.0μl

[0084] MS: EI source, selected ion scan mode, selected ions are m / z: 91, 92, 155;

[0085] Ion source temperature: 280°C;

[0086] Transmission line temperature: 280°C;

[0087] Solvent delay time: 5min;

[0088] 2) Solution preparation

[0089] Get 2g of ibuprofen, accurately weighed, put in a 10ml measuring bottle, add n-hexane to dissolve and dilute to the mark, shake well, and use it as the test solution. Take an appropriate ...

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Abstract

The invention provides a method for detecting ethyl p-toluenesulfonate as genetic toxicity impurities in ibuprofen by gas chromatography-mass spectrometry. The method comprises the following main steps: taking 5% of phenyl-arylidene and 95% of dimethyl polysiloxane as a fixed-phase capillary column; preparing a reference substance linear solution and a sample solution; carrying out temperature programming; after samples are separated by a gas chromatograph, detecting the samples by a mass spectrometry detector, wherein a mass spectrum is an EI source; quantifying selected ions in a scanning mode, wherein the selected ions are m/z: 91, 92, 155; calculating an equation of linear regression by the concentration of a reference substance and the corresponding peak area; and calculating the content of the ethyl p-toluenesulfonate in the ibuprofen by the equation of linear regression. The method is simple, speedy and accurate, and is high in sensitivity; the detection method is scientific andobjective; and the method can be used for controlling the quality of an ibuprofen sample, and has practical value.

Description

technical field [0001] The invention relates to a method for measuring genotoxic impurity ethyl p-toluenesulfonate in ibuprofen by gas chromatography mass spectrometry. Background technique [0002] Ibuprofen is a non-steroidal anti-inflammatory drug, its chemical name: 2-methyl-4-(2-methylpropyl) phenylacetic acid, molecular formula: C 13 h 18 o 2 , the molecular weight is: 206.28, and the structural formula is: [0003] [0004] NSAIDs (Nonsteroidal Antiinflammatory Drugs, NSAIDs) are a class of anti-inflammatory drugs that do not contain a steroidal structure. Osteoarthritis , rheumatoid arthritis, various fever and relief of various pain symptoms. At present, NSAIDs are one of the most used drugs in the world, and about 30 million people in the world use them every day. As a non-steroidal anti-inflammatory drug, ibuprofen can stimulate the cellular immune function of the human body and experimental animals, increase the activity of natural killer cells, accelerat...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 朱琳包月红赵悦叶海英
Owner JIANGSU CHIA TAI FENGHAI PHARMA
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