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

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5.09~200.17μg/L内线性关系良好(r=0.9993),方法检出限为0.21μg/L,定量限为0.70μg/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。

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 5.09-200.17μg/L.The linear correlation coefficient was 0.9993.The detection limit was 0.21μg/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.