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Method for detecting methyl methane sulfonate by gas chromatography and tandem mass spectrometry

A technology of methyl methanesulfonate and gas chromatography, which is applied in the field of detecting methyl methanesulfonate by gas chromatography-tandem mass spectrometry, can solve the problems of difficulty in meeting detection requirements, strong matrix interference, complicated processing, etc. The effect of lower detection limit and high sensitivity

Active Publication Date: 2015-02-18
JIANGSU SINOGRAPHY TESTING
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

This method has high accuracy and good reproducibility, and can effectively avoid the influence of volatile substances in the sample on the detection, but the pretreatment is more complicated and the detection limit is higher
Gas chromatography and gas chromatography-mass spectrometry, because of the simple operation and good reproducibility, but this method has strong matrix interference and high detection line, it is difficult to meet the detection requirements
[0006] At present, there is a lack of a method for detecting methyl methanesulfonate with high detection sensitivity and a simple and easy-to-operate gas chromatography-tandem mass spectrometry

Method used

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  • Method for detecting methyl methane sulfonate by gas chromatography and tandem mass spectrometry
  • Method for detecting methyl methane sulfonate by gas chromatography and tandem mass spectrometry
  • Method for detecting methyl methane sulfonate by gas chromatography and tandem mass spectrometry

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Embodiment 1

[0041] A kind of gas chromatography-tandem mass spectrometry method of the present invention detects methyl methanesulfonate, comprises the steps:

[0042] (1) Add acetonitrile to constant volume to 10ml, vortex and mix for 1min, ultrasonically extract for 10min, pass through a 0.22μm filter membrane, inject sample to determine methyl methanesulfonate in the sample;

[0043] (2) Detection conditions: Gas chromatography-tandem mass spectrometry GC-MS / MS was used as a detection instrument to determine methyl methanesulfonate.

[0044]In step (1), take 0.05 g of the sample to be tested, accurate to 0.1 mg, put it in an empty volumetric flask, add acetonitrile to dilute to 10 ml, vortex mix for 1 min, and ultrasonically extract for 10 min.

[0045] In step (2), the data acquisition method of the gas chromatography-tandem mass spectrometer is multiple reaction monitoring MRM, and the mass-to-charge ratio M / Z=79→65 is selected as the quantitative ion pair; M / Z=80→65, M / Z=79→48, M / ...

Embodiment 2

[0071] The difference between embodiment 2 and embodiment 1 is: in step (1), add acetonitrile to settle to 15ml, vortex mix 4min, ultrasonic extraction 13min, cross 0.22μm filter membrane, inject sample to methyl methanesulfonate in the sample Determination: Take 0.30 g of the product to be tested, accurate to 0.1 mg, put it in an empty volumetric flask, add acetonitrile to dilute to 15 ml, vortex mix for 4 min, and ultrasonically extract for 13 min.

Embodiment 3

[0073] The difference between embodiment 3 and embodiment 1 is: in step (1), add acetonitrile to settle to 25ml, vortex mix 5min, ultrasonic extraction 15min, cross 0.22μm filter membrane, inject sample to the methyl methanesulfonate in the sample Determination: Take 0.50 g of the product to be tested, accurate to 0.1 mg, put it in an empty volumetric flask, add acetonitrile to make up to 25 ml, vortex mix for 5 min, and ultrasonically extract for 15 min.

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Abstract

The invention discloses a method for detecting methyl methane sulfonate by gas chromatography and tandem mass spectrometry. The method is characterized by comprising the following steps: (1) placing a sample to be detected into a volumetric flask, adding acetonitrile to make up to the volume of 10 to 25 ml, carrying out vortex mixing for 1 to 5 min, carrying out ultrasonic extraction for 10 to 15 min, sieving the obtained product by a filter membrane with the specification of 0.22 [mu]m and carrying out sample injection to detect the methyl methane sulfonate in the sample; (2) under the detection conditions, using a gas chromatography and tandem mass spectrometry combined instrument GC-MS / MS as a detection instrument for detecting the methyl methane sulfonate. In the step (1), 0.05 to 0.50 g of the sample to be detected is taken, accuracy reaches 0.1 mg, the sample to be detected is placed in the volumetric flask, the acetonitrile is added to make up to the volume of 10 to 25 ml, vortex mixing is carried out for 1 to 5 min and ultrasonic extraction is carried out for 10 to 15 min. the method can simply, rapidly, conveniently and efficiently carry out qualitative and quantitative detection on MMS (methyl methane sulfonate) in medicine raw materials, chemical reagents and foods by using the GC-MS / MS.

Description

technical field [0001] The invention relates to a method for detecting methyl methanesulfonate MMS, in particular to a method for detecting methyl methanesulfonate by gas chromatography-tandem mass spectrometry. Background technique [0002] Since the beginning of the 21st century, with the advancement of science and technology and the rapid development of the economy, the life of human society has become more and more convenient; at the same time, people have encountered more and more challenges and hidden dangers in their lives. The fast pace of life makes people more vulnerable to serious diseases; medication is a fast and convenient treatment, and it is also the most common treatment at present. Therefore, the pharmaceutical industry is one of the most important areas of the entire society; however, due to technical capabilities and raw material quality, pharmaceutical reagents are likely to contain harmful substances, which is also a challenge for the pharmaceutical ind...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 徐锦忠袁博倪叶猛肖石基王祝超
Owner JIANGSU SINOGRAPHY TESTING
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