液液萃取-气相色谱法测定尿中四氯乙烷2种异构体  

Determination of two isomers of tetrachloroethane in urine by liquid-liquid extraction-gas chromatography

作　　者：吴凡 何嘉恒[1] 袁静 蒙瑞波[1] 谢威民 吴邦华[1] 戎伟丰[1] WU Fan;HE Jiaheng;YUAN Jing;MENG Ruibo;XIE Weimin;WU Banghua;RONG Weifeng(Guangdong Province Hospital for Occupational Disease Prevention and Treatment,Guangzhou,Guangdong 510300,China;不详)

机构地区：[1]广东省职业病防治院,广东广州510300 [2]广东药科大学公共卫生学院,广东广州510315 [3]广州医科大学公共卫生学院,广东广州510182

出　　处：《中国职业医学》2024年第1期85-89,共5页China Occupational Medicine

基　　金：广东省自然科学基金(2020A1515010893)。

摘　　要：目的建立人尿中1,1,1,2-四氯乙烷(TeCA)和1,1,2,2-TeCA的液液萃取-气相色谱法方法。方法取5.0 mL尿样加入2.0 g无水硫酸钠,再加入5.0 mL乙酸乙酯振荡混匀;取萃取液1.0 mL经100%二甲基聚硅氧烷毛细管气相色谱柱分离,火焰离子化检测器检测,外标法定量。结果尿中1,1,1,2-TeCA和1,1,2,2-TeCA在质量浓度为0.250~50.750 mg/L时线性关系良好,相关系数均>0.9999。尿中1,1,1,2-TeCA检出限为0.020 mg/L,定量下限为0.060 mg/L;平均加标回收率为88.02%~101.32%;批内、批间相对标准偏差(RSD)分别为0.11%~0.47%和0.39%~1.09%。尿中1,1,2,2-TeCA检出限为0.050 mg/L,定量下限为0.150 mg/L;平均加标回收率为93.42%~101.32%;批内、批间RSD分别为0.28%~1.04%和0.50%~1.03%。1,1,1,2-TeCA和1,1,2,2-TeCA均无法在常温下保存;4℃下1,1,2,2-TeCA可保存至少3 d;-20℃下,1,1,1,2-TeCA仅能保存1 d,1,1,2,2-TeCA可保存至少5 d。结论本方法灵敏度高、特异性好、样品前处理简单,结果更为直观可靠,可用于职业人群尿中1,1,1,2-TeCA和1,1,2,2-TeCA的检测。Objective To establish a method for the determination of 1,1,1,2-tetrachloroethane(TeCA)and 1,1,2,2-TeCA in human urine using liquid-liquid extraction-gas chromatography.Methods The 5.0 mL urine sample was mixed with 2.0 g anhydrous sodium sulfate and 5.0 mL ethyl acetate,then vortexed mixing.The 1.0 mL extraction was separated by 100%dimethylpolysiloxane capillary gas chromatography column,detected by flame ionization detector,and quantified by an external standard method.Results The linear ranges of 1,1,1,2-TeCA and 1,1,2,2-TeCA were 0.250-50.750 mg/L,with both correlation coefficients of>0.9999.The detection limit of 1,1,1,2-TeCA in urine was 0.020 mg/L,and the lower limit of quantification was 0.060 mg/L.The average recovery was 88.02%-101.32%,and the within-run and between-run relative standard deviations(RSDs)were 0.11%-0.47%and 0.39%-1.09%,respectively.The detection limit of 1,1,2,2-TeCA in urine was 0.050 mg/L,and the lower limit of quantification was 0.150 mg/L.The average recovery was 93.42%-101.32%,and the within-run and betweenrun RSDs were 0.28%-1.04%and 0.50%-1.03%,respectively.Both the 1,1,1,2-TeCA and 1,1,2,2-TeCA cannot be stored at room temperature.The 1,1,2,2-TeCA can be stored at 4℃for at least three days.At-20℃,the 1,1,1,2-TeCA can only be stored for one day,while 1,1,2,2-TeCA can be stored for at least five days.Conclusion This method has high sensitivity,good specificity,simple sample pretreatment,and more intuitive and reliable results.It can be used to determine the level of 1,1,1,2-TeCA and 1,1,2,2-TeCA in urine of occupational population.

关 键 词：四氯乙烷 1 1 1 2-四氯乙烷 1 1 2 2-四氯乙烷 乙酸乙酯 气相色谱法 液液萃取 

分 类 号：R134.4[医药卫生—劳动卫生]