Method for detecting ethephon by applying ultra-high performance liquid chromatography-tandem mass spectrometry

An ultra-high performance liquid phase and tandem mass spectrometry technology, which is applied in the detection field of ethephon, can solve the problems of ineffective detection of ethephon concentration, low boiling point of ethephon, weak ultraviolet absorption, etc., so as to avoid matrix interference, high sensitivity, good linear effect

Inactive Publication Date: 2020-05-19
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, weak ultraviolet absorption and many heteroatoms of ethephon, the concentration of ethephon in the sample cannot be effectively detected by the commonly used detection methods GC-FID, HPLC-UV, and GC-MS
[0006] At present, there is a lack of a highly sensitive, simple, fast, and easy-to-operate ultra-high performance liquid chromatography-tandem mass spectrometry method to effectively detect ethephon

Method used

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  • Method for detecting ethephon by applying ultra-high performance liquid chromatography-tandem mass spectrometry
  • Method for detecting ethephon by applying ultra-high performance liquid chromatography-tandem mass spectrometry
  • Method for detecting ethephon by applying ultra-high performance liquid chromatography-tandem mass spectrometry

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Embodiment 1

[0045] The invention provides a method for detecting ethephon by using ultra-high performance liquid chromatography-tandem mass spectrometry, comprising the following steps:

[0046]Step (1), take the sample to be tested and put it in a volumetric flask, add formic acid-water (0.2~1):100 to make the volume to 20-50ml, vortex and mix for 2~10min, ultrasonically extract for 2~10min to make mother liquor 1, Then pipette 200 microliters of mother liquor 1, dilute it to 20~50ml with formic acid-water (0.2~1):100 to make mother liquor 2, then pipette 200 microliters of mother liquor 2, and dilute it with formic acid-water (0.2~1):100 Dilute to 20-50ml, inject sample to detect ethephon in the sample;

[0047] Step (2), detection conditions: use ultra-high performance liquid chromatography-tandem mass spectrometry UPLC-MS / MS as the detection instrument to detect ethephon.

[0048] In step (1), take 0.033g of the sample to be tested, accurate to 0.01mg, put it in an empty volumetric f...

Embodiment 2

[0072] The difference between Example 2 and Example 1 is that in step (1), add formic acid-water 0.3:100 to make the volume constant to 25ml, vortex for 10min, ultrasonically extract for 6min, pass through a 0.22μm filter membrane, and inject the sample into the sample Ethephon is tested; take 0.025g of the product to be tested, accurate to 0.01mg, put it in an empty volumetric flask, add formic acid-water 0.3:100 to make the volume to 20ml, vortex and mix for 10min, and ultrasonically extract for 6min to make mother liquor 1. Then pipette 200 microliters of mother liquor 1, dilute to 25ml with formic acid-water 0.3:100 to make mother liquor 2, then pipette 200 microliters of mother liquor 2, and dilute to 25ml with formic acid-water 0.3:100.

Embodiment 3

[0074] The difference between Example 3 and Example 1 is that in step (1), add formic acid-water 0.5:100 to make the volume 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 Ethephon is tested; take 0.065g of the product to be tested, accurate to 0.01mg, put it in an empty volumetric flask, add formic acid-water 0.5:100 to make the volume to 50ml, vortex and mix for 10min, and ultrasonically extract for 8min to make mother liquor 1. Then pipette 200 microliters of mother liquor 1 to make mother liquor 2, dilute to 25ml with formic acid-water 0.5:100, then pipette 200 microliters of mother liquor 2, and dilute to 25ml with formic acid-water 0.5:100.

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Abstract

The invention relates to a method for detecting ethephon by applying ultra-high performance liquid chromatography-tandem mass spectrometry. The method comprises the steps: putting a sample to be detected into a volumetric flask and adding formic acid-water (0.2-1): 1 wherein the volume is 100 to 20 to 50 ml; vortex mixing for 2-10 min, ultrasonically extracting for 2-10 minutes to prepare mother liquor 1; transferring 200 microliters of mother liquor 1, diluting the mother liquor 1 with formic acid-water (0.2-1): 100 to 20-50 ml to prepare mother liquor 2, transferring 200 microliters of mother liquor 2, diluting the mother liquor 2 with formic acid-water (0.2-1): 100 to 20-50 ml, introducing the sample, and detecting ethephon in the sample by adopting the ultra-high performance liquid chromatography-tandem mass spectrometer. The UPLC-MS / MS is used, the ethephon in green agricultural products, agricultural chemicals and foods can be qualitatively and quantitatively detected simply, quickly and efficiently, the detection sensitivity of ethephon can be effectively improved, matrix interference is effectively avoided, the detection limit of ethephon is reduced, good linearity is shownin the concentration range of 36.8 ng / mL-294.7 ng / mL and the linear correlation coefficient is 0.9998.

Description

technical field [0001] The invention relates to a detection method for ethephon, in particular to a method for detecting ethephon by using ultra-high performance liquid chromatography-tandem mass spectrometry. 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, instrumental analysis is wid...

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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