血中四氯化碳的顶空气相色谱-质谱测定法  

Determination of carbon tetrachloride in blood by headspace gas chromatography-mass spectrometry

作　　者：蔡小璇[1] 戎伟丰[2] 彭建梅 唐斯[1] 叶立和 李思燕 钟苑琴[1] 张曼宇 马争[1] 陈惠鹏[1] CAI Xiao-xuan;RONG Wei-feng;PENG Jian-mei;TANG Si;YE Li-he;LI Si-yan;ZHONG Yuan-qin;ZHANG Man-yu;MA Zheng;CHEN Hui-peng(Occupational Health Testing Department of Dongguan Occupational Disease Control Center,Dongguan Key Laboratory of Occupational Health Testing,Dongguan Guangdong,523008,China;Guangdong Institute of Occupational Disease Control,Guangdong Key Laboratory of Occupational Disease Control,Guangzhou Guangdong,510300,China)

机构地区：[1]东莞市职业病防治中心职业卫生检测科东莞市职业卫生检测重点实验室,广东东莞523008 [2]广东省职业病防治院广东省职业病防治重点实验室,广东广州510300

出　　处：《职业与健康》2020年第12期1623-1627,共5页Occupation and Health

基　　金：广东省医学科研基金项目(A2020316);东莞市职业卫生检测重点实验室。

摘　　要：目的建立血中四氯化碳的顶空气相色谱-质谱测定法。方法血样经顶空前处理后,顶空气中的四氯化碳经DB-5MS弹性毛细管色谱柱分离,采用气相色谱-质谱联用仪检测。测定四氯化碳选择离子定量用117.0 m/z,确认用82.0、119.0 m/z。结果血中四氯化碳在3.19~191.40μg/L内线性关系良好,线性相关系数为0.999 9,检出限为0.24μg/L,定量下限为0.80μg/L,不同浓度的样品加标回收率为102.3%~106.6%,批内相对标准偏差(RSD)为3.3%~3.4%,批间RSD为4.0%~7.1%。样品在常温或4℃下可保存3天,在-8℃以下可保存7天。结论本法快速、简便,灵敏、准确、干扰少,可作为职业中毒患者血样中四氯化碳的检测方法。Objective To establish a headspace gas chromatography-mass spectrometry method for the determination of carbon tetrachloride in blood. Methods After headspace pretreatment of blood samples,carbon tetrachloride in the top air was separated by DB-5 MS elastic capillary column and detected by GC-MS. Carbon tetrachloride was determined by 117.0 m/z and confirmed by82.0 and 119.0 m/z in selective ion quantification. Results There was good linear relationship in the range of 3.19-191.40 μg/L.The linear correlation coefficient was 0.999 9.The detection limit was 0.24 μg/L and the lower limit of quantitation was 0.80 μg/L.The recovery rates of samples with different concentrations were 102.3%-106.6%. The intra-batch relative standard deviations(RSD)were 3.3%-3.4%,and inter-batch RSD was 4.0%-7.1%. The samples can be stored at room temperature or 4 ℃ for three days and lower than-8 ℃ for seven days. Conclusion This method is rapid,simple,sensitive,and accurate,and has less interference,which is suitable for the determination of carbon tetrachloride in occupational poisoning patients.

关 键 词：血样 四氯化碳 气相色谱-质谱法 顶空分析法 

分 类 号：R115[医药卫生—公共卫生与预防医学]