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Method for determining dimethyl sulfate in medicine by derivatization gas chromatography-mass spectrometry

A technology of dimethyl sulfate and gas chromatography, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems affecting the specificity, accuracy, and long derivation reaction time of the detection, and achieve accurate and reliable detection results, specificity and Good sensitivity, simple and convenient operation

Inactive Publication Date: 2020-08-07
SHANGHAI SCIENPHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its derivatization reaction time is long (2 hours), and it is difficult to avoid the interference of other drug substrates in the process of detecting methylated aminopyrine, which affects the specificity and accuracy of detection.

Method used

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  • Method for determining dimethyl sulfate in medicine by derivatization gas chromatography-mass spectrometry
  • Method for determining dimethyl sulfate in medicine by derivatization gas chromatography-mass spectrometry
  • Method for determining dimethyl sulfate in medicine by derivatization gas chromatography-mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The mensuration of dimethyl sulfate content in embodiment 1, antiulcer medicine

[0044] 1. Chromatographic conditions

[0045] Instrument: Agilent 7890B Gas Chromatograph-5977B Mass Spectrometer-CTC Autosampler

[0046] Chromatographic column: VF-624ms (30m×0.25mm×1.4μm)

[0047] Inlet temperature: 200°C

[0048] Injection volume: 1ml

[0049] Split ratio: 50:1

[0050] Carrier gas: helium (constant flow 1.0mL / min)

[0051] Headspace conditions: equilibrium temperature 60°C, equilibrium time 30min

[0052] Column temperature: keep at 40°C for 2min, raise the temperature to 100°C at 10°C / min, then raise the temperature to 220°C at 30°C / min, and keep for 3min.

[0053] Detector: mass spectrometer detector, ion source temperature 230°C, quadrupole temperature 150°C

[0054] Selected ion monitoring mode (127, 142): m / z127 is used as an auxiliary qualitative ion, and m / z142 is used as a quantitative ion of dimethyl sulfate derivatized product methyl iodide.

[0055]...

Embodiment 2

[0062] Embodiment 2, the method verification of chromatographic method

[0063] 1. Exclusiveness

[0064] Precisely pipette 1ml of acetonitrile and 1ml of derivatization solution into a 20ml headspace bottle, seal it, shake well, and use it as a blank solution. Accurately weigh an appropriate amount of dimethyl sulfate, add acetonitrile to dilute to make a solution containing about 2 mg of dimethyl sulfate per 1 ml, as a stock solution; dilute the stock solution step by step with acetonitrile to obtain dimethyl sulfate with a concentration of 100 ng / mL Ester solution; pipette 1mL dimethyl sulfate solution and 1mL derivatization solution into a 20mL headspace bottle, seal and shake well to obtain a control solution with a concentration of 50ng / mL. Accurately weigh about 0.04g of the sample to be tested (ranitidine hydrochloride) into a 20mL headspace bottle, add 1mL of acetonitrile and 1mL of derivatization solution, seal, shake well, and obtain the test solution. Accuratel...

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Abstract

The invention discloses a method for determining dimethyl sulfate in a drug through derivatization gas chromatography-mass spectrometry. The method comprises the following steps of adding a derivatization solution into a drug sample, deriving dimethyl sulfate into methyl iodide, and detecting the content of methyl iodide through gas chromatography-mass spectrometry to obtain the content of dimethyl sulfate, wherein the derivatization solution is a saturated sodium iodide aqueous solution added with a trace amount of sodium thiosulfate. By adopting the method, the content of the genotoxic impurity dimethyl sulfate in the medicine can be accurately determined, and the method has the advantages of being convenient to operate, being capable of reducing the interference of a non-volatile medicine matrix and the like.

Description

technical field [0001] The invention belongs to the technical field of medical detection, and relates to a method for determining dimethyl sulfate in medicine by derivatization gas chromatography-mass spectrometry, in particular to a method for determining genotoxic impurity sulfuric acid in medicine by using online derivatization gas chromatography-mass spectrometry Method for dimethyl ester content. Background technique [0002] A genotoxic impurity is a DNA-reactive substance that can cause DNA damage that can cause mutations and potentially induce cancer. In order to ensure the drug safety of patients, it is necessary to pay attention to and control the genotoxic impurities in drugs. [0003] Dimethyl sulfate is a powerful methylating reagent, which is widely used in the chemical synthesis of drugs and their intermediates. When dimethyl sulfate is directly used in drug synthesis, there may exist Risk of residues in medicines. After dimethyl sulfate enters the human bo...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/30G01N30/16G01N30/72G01N30/02
CPCG01N30/02G01N30/06G01N30/16G01N30/30G01N30/72G01N2030/025G01N2030/047G01N2030/067
Inventor 刘娇谢军李惠姜春阳刘雪薇周小群
Owner SHANGHAI SCIENPHARM CO LTD
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