Liquid-chromatogram and tandem-mass-spectrogram assay method for CEMA (Cyanoethyl Methacrylate) and HEMA (Hydroxyethyl Methacrylate) in urine

A measurement method, tandem mass spectrometry technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve good sensitivity and repeatability, reduce errors, and high sensitivity

Active Publication Date: 2013-05-22
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low content of CEMA and HEMA in the general population and the complex urine matrix, some established LC-MS / MS methods are limited in the detection of CEMA and HEMA in the urine of non-smokers

Method used

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  • Liquid-chromatogram and tandem-mass-spectrogram assay method for CEMA (Cyanoethyl Methacrylate) and HEMA (Hydroxyethyl Methacrylate) in urine
  • Liquid-chromatogram and tandem-mass-spectrogram assay method for CEMA (Cyanoethyl Methacrylate) and HEMA (Hydroxyethyl Methacrylate) in urine
  • Liquid-chromatogram and tandem-mass-spectrogram assay method for CEMA (Cyanoethyl Methacrylate) and HEMA (Hydroxyethyl Methacrylate) in urine

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0048] 1. Instruments and reagents: Agilent 1200 fast high-resolution liquid chromatography (Agilent, USA), equipped with G1367D autosampler, G1312B binary mixing pump and G1316B column thermostat; API 5500 triple quadrupole tandem mass spectrometer (Applied Biotechnology, USA) Systems Company), equipped with electrospray ion source and analyst 1.5 software data processing system.

[0049] N-acetyl-S-(2-cyanoethyl)-L-cysteine ​​(purity 98%), N-acetyl-S-(2-hydroxyethyl)-L-cysteine ​​( Purity 98%), N-acetyl-S-(2-cyanoethyl)-L-cysteine-D3 (chemical purity 98%, isotopic purity 99%), N-acetyl-S-(2 -Hydroxyethyl)-L-cysteine-D4 (chemical purity 98%, isotopic purity 99%) (Toronto Research Chemicals). Formic acid (chromatographically pure, Acros Organics). Methanol and acetonitrile (chromatographically pure, TEDIA company).

[0050] 2. Sample handling: Thaw urine at room temperature and mix well. Accurately pipette 1.0 mL of urine, add 10 μL of formic acid to acidify, and centrif...

example 2

[0052] Example 2: As described in Example 1, 37 urine samples were taken. The content of CEMA and HEMA in urine was measured as image 3 shown.

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Abstract

The invention relates to a liquid-chromatogram and tandem-mass-spectrogram assay method for CEMA (Cyanoethyl Methacrylate) and HEMA (Hydroxyethyl Methacrylate) in urine. The method is characterized by comprising the following steps of: (a) collecting the urine of a volunteer; (b) carrying out pretreatment on a sample; (c) preparing standard working liquid; and (d) carrying out liquid-chromatogram and tandem-mass-spectrogram assay. The method has the characteristics that the sample is directly introduced into a liquid chromatogram-electrospray ionization-tandem mass spectrometer for assaying after the sample is diluted, and the content of the CEMA and the HEMA in the urine can be quickly and accurately assayed. The method for assaying the content of the CEMA and the HEMA in the urine is bran-new, a deuterated standard is adopted as an interior-label quantitative analysis substance, and thus errors caused during the pretreatment of the sample can be reduced; and due to a tandem mass spectrogram method, the selectivity and the accuracy of the method are well improved. Through a chromatographic column and the selection and the optimization of elution conditions, the chromatographic separation process is well improved, and the time spent on chromatographic analysis is shortened.

Description

[0001] technical field : [0002] The invention belongs to the technical field of physical and chemical testing of urine samples, and mainly relates to the technical field of mercaptouric acid determination of urine samples. Methods for S-(2-cyanoethyl)-L-cysteine ​​(CEMA) and N-acetyl-S-(2-hydroxyethyl)-L-cysteine ​​(HEMA) content. Background technique: [0003] Acrylonitrile is an a,b-unsaturated nitrile compound containing active vinyl and nitrile groups. It can form a more active epoxy-type intermediate through metabolic activation, and further covalently bond with the nucleophilic center of the cell macromolecule in the body, thereby causing damage to the body. In vitro toxicology experiments and epidemiological investigation data show that acrylonitrile has certain carcinogenicity. In 1999, IARC classified it as a probable human carcinogen. Acrylonitrile exists in cigarette smoke (7.8-39.1 μg / cigarette), and the general population can be exposed to acrylonitrile ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/72
Inventor 侯宏卫张小涛田永峰刘彤陈欢韩书磊胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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