Method for detecting malononitrile by applying ultra-high performance liquid chromatography-tandem mass spectrum

An ultra-high performance liquid phase and tandem mass spectrometry technology, which is applied in the detection field of malononitrile, can solve the problems of easily interfered detection of malononitrile, low molecular weight of malononitrile, low mass-to-charge ratio, etc., so as to avoid matrix interference, good Linear, high-sensitivity effects

Inactive Publication Date: 2019-02-05
江苏乾元生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Due to the low boiling point of malononitrile, the GC-MS method is usually considered for the detection of low concentration of malononitrile in the sample, but the molecular weight of malononitrile is low, especially the mass-to-charge ratio of its fragment ions is lower, so the GC-MS method is used Detection of malononitrile is susceptible to interference
[0006] At present, there is a lack of a highly sensitive, simple, rapid and easy-to-operate detection method to effectively detect residual malononitrile in drugs

Method used

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  • Method for detecting malononitrile by applying ultra-high performance liquid chromatography-tandem mass spectrum
  • Method for detecting malononitrile by applying ultra-high performance liquid chromatography-tandem mass spectrum
  • Method for detecting malononitrile by applying ultra-high performance liquid chromatography-tandem mass spectrum

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Embodiment 1

[0041] see figure 1 with figure 2 , A method for detecting malononitrile using ultra-high performance liquid chromatography-tandem mass spectrometry of the present invention includes the following steps:

[0042] (1) Take the sample to be tested and place it in a volumetric flask, add acetonitrile to the volume to 10-50ml, vortex for 5-10min, ultrasonically extract for 15-25min, pass through a 0.22μm filter membrane, and inject the malononitrile in the sample. Detection

[0043] (2) Detection conditions: UPLC-MS / MS was used as the detection instrument to detect malononitrile.

[0044] In step (1), take 0.067g of the test product, accurate to 0.1mg, place it in an empty volumetric flask, add nitrile to make the volume to 20ml, vortex and mix for 5min, ultrasonically extract for 15min, and pass through a 0.22μm filter membrane.

[0045] In step (2), the data acquisition method of the ultra-high performance liquid chromatography-tandem mass spectrometer is selective reaction detection S...

Embodiment 2

[0068] The difference between Example 2 and Example 1 is: in step (1), add acetonitrile to make the volume up to 25ml, vortex for 4min, ultrasonically extract for 10min, pass through a 0.22μm filter membrane, and then sample to detect malononitrile in the sample ; Take the test product 0.084g, accurate to 0.1mg, place it in an empty volumetric flask, add nitrile to make the volume to 25ml, vortex for 4min, and ultrasonically extract for 10min.

Embodiment 3

[0070] The difference between Example 2 and Example 1 is that in step (1), add acetonitrile to 50ml, vortex for 10min, ultrasonically extract for 5min, pass through a 0.22μm filter membrane, and then sample to detect malononitrile in the sample. ; Take the test product 0.17g, accurate to 0.1mg, place it in an empty volumetric flask, add nitrile to 50ml, vortex for 10min, and ultrasonically extract for 5min.

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Abstract

The invention relates to a method for detecting malononitrile by applying an ultra-high performance liquid chromatography-tandem mass spectrum. The method is characterized by comprising the followingsteps of (1) placing a to-be-detected sample in a volumetric flask, adding acetonitrile until a constant volume of 10-50 ml, performing vortex mixing for 5-10 min, performing ultrasonic extracting for15-25 min, performing filtering with a 0.22-micron filter membrane, performing sample injection to detect malononitrile in a sample; and (2) detection conditions: detecting malononitrile by taking the ultra-high performance liquid chromatography-tandem mass spectrum (UPLC-MS / MS) as a detection instrument. In the step (1), 0.05-0.5 g, which is accurate to 0.1 mg, of a to-be-detected product is weighed, and is placed in an empty volumetric flask, acetonitrile is added until a constant volume of 10-50 ml, vortex mixing is performed for 5-10 min, ultrasonic extracting is performed for 15-25 min and filtering is performed with the 0.22-micron filter membrane. According to the method for detecting malononitrile by applying the ultra-high performance liquid chromatography-tandem mass spectrum, by use of the UPLC-MS / MS, malononitrile in a crude drug, an agricultural chemical product and foods can be qualitatively and quantitatively detected simply, rapidly and efficiently.

Description

Technical field [0001] The invention relates to a method for detecting malononitrile, in particular to a method for detecting malononitrile by using ultra-high performance liquid chromatography-tandem mass spectrometry. Background technique [0002] With the development of society and technological progress. Human beings are paying more and more attention to health, and medicine has played a pivotal role in ensuring human health. Therefore, the pharmaceutical industry has become one of the most important areas of society. How to accurately and quickly detect potential hazardous substances with low limit requirements in pharmaceutical reagents is a challenge facing the pharmaceutical industry. The application of advanced modern instrument analysis technology to meet this challenge is of great significance for promoting the safety evaluation of drugs and improving the commercial value of drugs. [0003] As the main method of modern detection, instrumental analysis is widely used i...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N30/72G01N2030/146
Inventor 刘长生肖石基
Owner 江苏乾元生物科技有限公司
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