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Method for detecting 4-nitro-2, 3, 5-trimethylpyridine-N-oxide by UPLC-MS/MS

A collidine and oxide technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of small molecular weight, many heteroatoms, and low boiling point, and achieve good linearity, high sensitivity, and good selectivity.

Inactive Publication Date: 2020-04-28
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, small molecular weight and many heteroatoms of 4-nitro-2,3,5-trimethylpyridine-N-oxide, it is difficult to use the commonly used detection methods GC-FID, HPLC-UV, GC- Low concentration limit of 4-nitro-2,3,5-trimethylpyridine-N-oxide in MS detection sample
[0006] At present, there is a lack of an ultra-high performance liquid chromatography-tandem mass spectrometry method with high detection sensitivity, simplicity, rapidity, and ease of operation to effectively detect the residual 4-nitro-2,3, 5-Collidine-N-oxide

Method used

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  • Method for detecting 4-nitro-2, 3, 5-trimethylpyridine-N-oxide by UPLC-MS/MS
  • Method for detecting 4-nitro-2, 3, 5-trimethylpyridine-N-oxide by UPLC-MS/MS
  • Method for detecting 4-nitro-2, 3, 5-trimethylpyridine-N-oxide by UPLC-MS/MS

Examples

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Embodiment 1

[0047] The invention provides a method for detecting 4-nitro-2,3,5-collidine-N-oxide by UPLC-MS / MS, comprising the following steps:

[0048] Step (1), take the sample to be tested and place it in a volumetric flask, add acetonitrile-water (3-8): 6 to make up to 20-50ml, vortex and mix for 2-10min, ultrasonically extract for 2-10min, filter through 0.22μm Membrane, sample injection to detect 4-nitro-2,3,5-collidine-N-oxide in the sample;

[0049] Step (2), detection conditions: using ultra-high performance liquid chromatography-tandem mass spectrometry UPLC-MS / MS as a detection instrument for 4-nitro-2,3,5-trimethylpyridine-N-oxide detection.

[0050] In step (1), take 0.02 g of the sample to be tested, accurate to 0.01 mg, put it in an empty volumetric flask, add acetonitrile-water 4:6 to make the volume to 20 ml, vortex and mix for 10 min, ultrasonically extract for 5 min, pass through 0.22 μm filter membrane.

[0051] In step (2), the data acquisition method of the ultra-...

Embodiment 2

[0075] The difference between Example 2 and Example 1 is: in step (1), add acetonitrile-water 7:6 to make it constant to 25ml, vortex for 10min, ultrasonically extract for 6min, pass through a 0.22μm filter membrane, and inject the sample into the sample 4-nitro-2,3,5-collidine-N-oxide for detection; take 0.025g of the sample to be tested, accurate to 0.01mg, put it in an empty volumetric flask, add acetonitrile-water 7:6 Dilute to 25ml, vortex mix for 10min, and ultrasonically extract for 6min.

Embodiment 3

[0077] The difference between Example 3 and Example 1 is that in step (1), add acetonitrile-water 7:6 to make it constant to 50ml, vortex for 10 minutes, ultrasonically extract for 8 minutes, pass through a 0.22 μm filter membrane, and inject the sample into the sample 4-nitro-2,3,5-collidine-N-oxide for detection; take 0.05g of the sample to be tested, accurate to 0.01mg, put it in an empty volumetric flask, add acetonitrile-water 7:6 Dilute to 50ml, vortex mix for 10min, and ultrasonically extract for 8min.

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Abstract

The invention relates to a method for detecting 4-nitro-2, 3, 5-trimethylpyridine-N-oxide by UPLC-MS / MS. The method comprises the following steps: (1) putting a to-be-detected sample into a volumetricflask, adding acetonitrile-water (3-8): 6, fixing a volume to 20-50ml, carrying out vortex mixing for 2-10min, carrying out ultrasonic extraction for 2-10min, passing through a 0.22 mum filter membrane, and introducing a sample to detect the 4-nitro-2, 3, 5-trimethylpyridine-N-oxide in the sample; and (2) determining detecting conditions: detecting the 4-nitro-2, 3, 5-trimethylpyridine-N-oxide byadopting an ultra-high performance liquid chromatography-tandem mass spectrometer UPLC-MS / MS as a detection instrument. In the step (1), 0.01-0.05g of the product to be detected is taken. The UPLC-MS / MS is used so that qualitative and quantitative detection can be simply, quickly and efficiently performed on the 4-nitro-2, 3, 5-trimethylpyridine-N-oxide in pharmaceutical raw materials, agricultural chemicals and foods.

Description

technical field [0001] The invention relates to a detection method for 4-nitro-2,3,5-trimethylpyridine-N-oxide, in particular to a method for detecting 4-nitro-2,3,5-trimethylpyridine by UPLC-MS / MS based pyridine-N-oxide method. Background technique [0002] With the development of society and the progress of science and technology. Human beings pay more and more attention to health, and medicine plays 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 potentially harmful substances with low limit requirements in pharmaceutical reagents is a challenge that the pharmaceutical industry is currently facing. Applying advanced modern instrumental 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 means of modern detection, instrume...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 刘长生肖石基
Owner 江苏乾元生物科技有限公司
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