全血中四氯乙烯测定的自动顶空气相色谱-质谱法
Determination of Perchloroethylene in blood by headspace gas chromatography-mass spectrometry
冯洁 1刘武宾 1李燕 1丁春光1
作者信息
- 1. 国家卫生健康委职业安全卫生研究中心(国家卫生健康委煤炭工业职业医学研究中心),北京 102308
- 折叠
摘要
目的 建立顶空气相色谱-质谱法测定职业人群全血中四氯乙烯的分析方法.方法 于2021年10至12月,采3 ml血样于10 ml顶空瓶中,经60℃加热平衡30 min后,顶空气中的四氯乙烯经VF-WAX ms毛细管色谱柱分离,外标法定量.结果 血中四氯乙烯在5.09～200.17 μg/L内线性关系良好(r=0.999 3),方法检出限为0.21 μg/L,定量限为0.70 µg/L,不同浓度的样品加标回收率为95.3％～103.8％,批内相对标准偏差(RSD)为3.2％～4.6％,批间RSD为4.0％～6.1％.样品4 ℃可保存3 d,于-20℃可保存7 d.结论 本法简单实用,重现性好,灵敏度高,可应用于全血中PCE的生物检测.
Abstract
Objective To establish a method for determination of Perchloroethylene(PCE)in blood by headspace gas chromatography-mass spectrometry(HS/GC-MS).Methods From Dctober to December 2021,A total of 3 mL blood samples were taken into a 10 mL headspace bottle,after heated at 60 ℃ for 30 mins,PCE in the top air was separated by VF-WAXms capillary column and detected by GC-MS.The retention time and external standard method were used for qualitative and quantitative analysis of PCE in samples,respectively.Results There was good linear relationship in the range of 5.09-200.17 μg/L.The linear correlation coefficient was 0.9993.The detection limit was 0.21 μg/L and the lower limit of quantitation was 0.70μg/L.The recovery rates of samples with different concentrations were 95.3％-103.8％.The intra-batch relative standard deviations(RSD)were 3.2％-4.6％,and inter-batch RSD was 4.0％-6.1％.The samples can be stored at 4 ℃ for three days and at-20 ℃ for seven days.Conclusion This method is proved to be simple,practical and highly sensitive,which is suitable for the determination of PCE in blood.
关键词
四氯乙烯/血样/气相色谱-质谱法/顶空分析法Key words
Perchloroethylene(PCE)/Blood sample/Gas chromatography-mass spectrometry/Headspace analysis引用本文复制引用
出版年
2024
NETL
NSTL
维普
万方数据