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气相色谱-串联质谱法测定工作场所空气中8种N-亚硝胺

[Determination of 8 N-nitrosamines in the workplace air by GC-MS/MS method].

作者信息

Meng X J, Liu X D, Zhang X M, Hu Y, Guo Q F

机构信息

Central Laboratory, the Beijing Prevention and Treatment Hospital of Occupational Disease for Chemical Industry, Beijing 100093, China.

出版信息

Zhonghua Lao Dong Wei Sheng Zhi Ye Bing Za Zhi. 2024 Aug 20;42(8):616-620. doi: 10.3760/cma.j.cn121094-20230922-00065.

DOI:10.3760/cma.j.cn121094-20230922-00065
PMID:39223051
Abstract

To establish a method for the determination of eight N-nitrosamines (N-nitrosodimethylamine, N-nitrosodimethylamine, N-nitrosomethylmethylamine, N-nitrosodibutylamine, N-nitrosopropylamine, N-nitrosomorpholine, N-nitrosodianiline and N-nitrosopiperidine) in the air of workplace by gas chromatography-tandem mass spectrometry (GC-MS/MS) . From January to August 2023, eight N-nitrosamines in the air of workplace were collected by ThermoSorb/N column, eluted with 4 ml methanol-dichloromethane (1∶1 volume ratio), separated by VF-624 ms capillary column, detected by multiple reaction monitoring mode and quantified by external standard method. The detection limit and precision of the method were also analyzed. The linear range of the method for the determination of eight N-nitrosamines was 1.0-20.0 μg/L, the correlation coefficient was 0.9993-0.9999, the detection limit was 0.051-0.132 μg/L, and the minimum quantitative concentration was 0.030-0.078 μg/m(3) (calculated by collecting 22.5 L of air sample and eluting with 4.0 ml stripping liquid). The within-run precisions were 2.05%-6.89% and the between-run precisions were 2.41%-8.26%. The desorption rates were 67.20%-102.60%. The sample can be kept at least 7 days at 4 ℃. GC-MS/MS method for the determination of eight N-nitrosamines in workplace air has high sensitivity and good precision, and can accurately determine the content of eight N-nitrosamines in workplace air.

摘要

建立气相色谱-串联质谱法(GC-MS/MS)测定工作场所空气中8种N-亚硝胺(N-亚硝基二甲胺、N-亚硝基二乙胺、N-亚硝基甲基乙胺、N-亚硝基二丁胺、N-亚硝基丙胺、N-亚硝基吗啉、N-亚硝基二苯胺和N-亚硝基哌啶)的方法。2023年1月至8月,采用ThermoSorb/N柱采集工作场所空气中的8种N-亚硝胺,用4 ml甲醇-二氯甲烷(体积比1∶1)洗脱,经VF-624 ms毛细管柱分离,采用多反应监测模式检测,外标法定量。并对该方法的检出限和精密度进行了分析。该方法测定8种N-亚硝胺的线性范围为1.020.0 μg/L,相关系数为0.999 30.999 9,检出限为0.0510.132 μg/L,最低定量浓度为0.0300.078 μg/m³(以采集22.5 L空气样品并以4.0 ml解吸液洗脱计算)。批内精密度为2.05%6.89%,批间精密度为2.41%8.26%。解吸率为67.20%~102.60%。样品在4℃下至少可保存7天。GC-MS/MS法测定工作场所空气中8种N-亚硝胺具有灵敏度高、精密度好的特点,能够准确测定工作场所空气中8种N-亚硝胺的含量。

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