顶空—气相色谱法与吹扫捕集—气相色谱质谱联用法测定水中3种五氯丙烷  

Determination of Three Pentachloropropanes in Drinking Water by Headspace-GC and Purge and Trap-GC-MS

作　　者：刘兰侠[1] 倪蓉[1] 钱杰峰[1] 杨凯[1] 陈翔[1] 路凌怡 LIU Lanxia;NI Rong;QIAN Jiefeng;YANG Kai;CHEN Xiang;LU Lingyi

机构地区：[1]上海市徐汇区疾病预防控制中心,上海市200237

出　　处：《环境卫生学杂志》2020年第3期311-316,共6页JOURNAL OF ENVIRONMENTAL HYGIENE

基　　金：中疾控生活饮用水标准方法研制(201831)。

摘　　要：目的建立生活饮用水中3种五氯丙烷的顶空—气相色谱法和吹扫捕集—气相色谱质谱联用法。方法顶空—气相色谱法采用高纯氮气为载气,70℃振荡平衡15 min,采用电子捕获检测器,外标法定量;吹扫捕集—气相色谱质谱联用法采用高纯氦气为载气,室温下吹扫,采用选择离子监测模式,内标法定量;并对两种方法的检出限、精密度以及准确度进行评价。结果顶空—气相色谱法和吹扫捕集—气相色谱质谱联用法均能完全分离3种五氯丙烷,两种方法都有良好的线性关系,相关系数均大于0.999。顶空—气相色谱法的检出限为(0.005~0.03)μg/L;回收率为86.4%~118%;精密度为1.9%~6.5%。吹扫捕集—气相色谱质谱联用法的检出限为(0.004~0.008)μg/L;回收率为80.5%~112%;精密度为0.9%~5.6%。结论两种方法均能较好的对饮用水中的五氯丙烷进行定性和定量分析,对实际样品的测定结果无显著性差异,适用于饮用水中五氯丙烷的分析测定.Objectives To develop the analysis method of 3 pentachloropropanes in drinking water by headspace(HS)-GC and purge and trap-GC-MS.Methods For HS-GC method,high purity nitrogen was used as carrier gas with oscillation at 70℃for 15 min,Electron capture detector was used,and external standard method was adopted for quantification;for purge and trap-GC-MS method,high purity helium was used as carrier gas,purge was conducted at room temperature,selected ion monitoring mode was used,and internal standard method was adopted for quantification;the detection limit,precision,and accuracy of two method were evaluated.Results Three pentachloropropanes could be completely isolated by HS-GC and purge and trap-GC-MS.Both method showed a good linear relationship,and the correlation coefficients were greater than 0.999.The detection limit,recovery,and precision of HS-GC method were(0.005-0.03)μg/L,86.4%-118%,1.9%-6.5%,respectively.The detection limit,recovery,and precision of purge and trap-GC-MS were(0.004-0.008)μg/L,80.5%-112%,0.9%-5.6%,respectively.Conclusions The two method both did well in the qualitative and quantitative analysis of pentachloropropanes in drinking water without significant difference among the determination result of actual samples,which could meet the analysis and determination of pentachloropropanes in drinking water.

关 键 词：五氯丙烷 顶空 吹扫捕集 气相色谱 气相色谱质谱联用 

分 类 号：R123[医药卫生—环境卫生学]