自动顶空-气相色谱法测定人尿中1,1,2,2-四氯乙烷  

Determination of 1,1,2,2-tetrachloroethene in human urine by automated headspacegas chromatography

作　　者：李思燕 钟苑琴 蔡小璇 周常侠 庄小舟 马争 叶立和 杨佩珊 熊劲光 陈满连 LI Siyan;ZHONG Yuanqin;CAI Xiaoxuan;ZHOU Changxia;ZHUANG Xiaozhou;MA Zheng;YE Lihe;YANG Peishan;XIONG Jinguang;CHEN Manlian(The Sixth People’s Hospital of Dongguan,Dongguan,Guangdong 523008,China)

机构地区：[1]东莞市第六人民医院,广东东莞523008

出　　处：《职业卫生与应急救援》2024年第4期528-532,共5页Occupational Health and Emergency Rescue

基　　金：东莞市社会发展科技项目(20231800902442);东莞市社会发展科技项目(20211800900962);东莞市职业卫生检测重点实验室。

摘　　要：目的建立人尿中1,1,2,2-四氯乙烷的自动顶空-气相色谱检测方法。方法准确移取5.00 mL待检尿样于20 mL顶空瓶中,加入2.0 g无水亚硫酸钠后立刻密封顶空瓶盖,置于自动顶空仪中80℃加热平衡50 min。在加热条件下,同时加入无水亚硫酸钠使得尿中1,1,2,2-四氯乙烷发生完全消去反应生成三氯乙烯,顶空瓶上方三氯乙烯蒸气经DB-624毛细管色谱柱分离,火焰离子化检测器检测,以三氯乙烯的峰面积对1,1,2,2-四氯乙烷的质量浓度绘制标准曲线进行定量。结果实验结果表明,尿中1,1,2,2-四氯乙烷在质量浓度为0.0083~32.000 mg/L范围内线性关系良好,相关系数>0.9994,方法检出限为2.5μg/L,定量下限为8.3μg/L。批内相对标准偏差为4.79%~5.28%,批间相对标准偏差为4.61%~6.44%。加标回收率为87.53%~101.17%。结论自动顶空-气相色谱法测定尿中1,1,2,2-四氯乙烷灵敏度高、线性关系好、干扰少、精密度好、样品前处理简单,可用于人尿中1,1,2,2-四氯乙烷质量浓度的测定。Objective To establish an automated headspace-gas chromatography method for the determination of 1,1,2,2-tetrachloroethene in human urine.Methods A urine sample of 5.00 mL was placed in a 20 mL headspace vial,and 2.0 g of anhydrous sodium sulfite was added before sealing the vial.The vial was placed in an automated headspace sampler and heated at 80℃for 50.00 min to equilibrate.Under these heating conditions,1,1,2,2-tetrachloroethene in human urine was completely reacted with anhydrous sodium sulfite to form trichloroethylene.The trichloroethylene vapor above the headspace vial was separated by a DB-624 capillary column and detected with a flame ionization detector.Quantification was achieved by plotting a standard curve with the peak area of trichloroethylene and the mass concentration of 1,1,2,2-tetrachloroethane.Results The results showed good linear ranges of 1,1,2,2-tetrachloroethene in urine between 0.0083 and 32.000 mg/L,and the correlation coefficient was higher than 0.9994.For this method,the limit of detection was 2.5μg/L,and the lower limit of quantification was 8.3μg/L;the intra-batch precision was 4.79%to 5.28%,and the interbatch precision was 4.61%to 6.44%;the average recovery rate was 87.53%to 101.17%.Conclusions The automated headspace gas chromatography method for determining 1,1,2,2-tetrachloroethene in human urine was characterized by high sensitivity,good linearity,minimal interference,high precision,and simple sample preparation.It is suitable for measuring the concentration of 1,1,2,2-tetrachloroethene in human urine.

关 键 词：1 1 2 2-四氯乙烷 三氯乙烯 消去反应 尿 自动顶空-气相色谱法 

分 类 号：R134.4[医药卫生—劳动卫生]