工作场所空气中8种N-亚硝胺化合物测定的GC-MS/MS法
Determination of 8 N-nitrosamines in the workplace air by GC-MS/MS method
目的:建立工作场所空气中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-亚硝基正丙胺、N-亚硝基吗啉、N-亚硝基二苯胺和N-亚硝基吡咯烷8种N-亚硝胺化合物的气相色谱-串联质谱(GC-MS/MS)检测方法。方法:于2023年1至8月,以ThermoSorb/N柱采集工作场所中空气中8种N-亚硝胺,用4 ml甲醇-二氯甲烷(体积比1∶1)溶液解吸,VF-624 ms毛细管色谱柱分离,多反应监测模式检测,外标法定量,并对方法的检出限和精密度等指标进行分析。结果:8种N-亚硝胺测定方法的线性范围为1.0~20.0 μg/L,相关系数0.999 3~0.999 9,方法检出限0.051~0.132 μg/L,最低定量浓度0.030~0.078 μg/m 3(以空气体积22.5 L,解吸液体积4.0 ml计),批内精密度2.05%~6.89%,批间精密度2.41%~8.26%,解吸效率67.20%~102.60%;样品在4 ℃条件下至少可保存7 d。 结论:GC-MS/MS测定工作场所空气中8种N-亚硝胺方法的灵敏度高、精密度好,可准确测定工作场所空气中8种N-亚硝胺含量。
更多Objective: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) .Methods: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.Results: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 ℃. Conclusion: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.
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