高效液相色谱-电感耦合等离子体质谱法测定尿中的三甲基氯化锡和三乙基氯化锡  

Determination of trimethyltin chloride and triethyltin chloride in human urine by HPLC-ICP-MS

作　　者：董明[1] 马安平 罗晓婷[1] 张爱华[1] 阮小林[1] DONG Ming;MA An-ping;LUO Xiao-ting;ZHANG Ai-hua;RUAN Xiao-lin(Guangdong Province Hospital for Occupational Disease Prevention and Treatment,Guangzhou,Guangdong 510300,China)

机构地区：[1]广东省职业病防治院

出　　处：《中国卫生检验杂志》2018年第22期2693-2696,共4页Chinese Journal of Health Laboratory Technology

基　　金：广东省职业病防治重点实验室开放运行(2017B030-314152);广东省医学科研基金(A2017021)

摘　　要：目的 建立高效液相色谱-电感耦合等离子体质谱联用快速测定人尿中三甲基氯化锡和三乙基氯化锡的检测方法。方法 尿样用超纯水适当稀释后,采用Ruby@C4反相色谱柱对待测化合物进行分离,以4%乙酸水溶液和甲醇为流动相,2种有机锡化合物在7 min内得到了有效分离;利用电感耦合等离子体质谱检测,工作曲线法定量。结果 2种有机锡化合物分别在8. 60μg/L-451. 0μg/L、6. 35μg/L-472. 5μg/L时线性良好,相关系数〉 0. 998,以尿样稀释5倍计,方法检出限分别为8. 60μg/L和6. 35μg/L,批内精密度为1. 30%-6. 40%,批间精密度为1. 50%-6. 44%,加标回收率为87. 48%-96. 64%。结论 本方法操作简便,分离效果好,具有良好的灵敏度和精密度,适用于人尿中三甲基氯化锡和三乙基氯化锡的快速测定。Objective To establish the determination method of trimethyltin chloride and（TMT） and triethyltin chloride （TET） in urine by high performance liquid chromatography - inductively coupled plasma mass spectrometry （ HPLC - ICP - MS ）. Methods The urine was diluted by pure water properly, Ruby@ C4 colum was used to separate the target, and the mobile phases were 4% acetic solution and methanol, the two organotin compounds were separated in 7 min, and TMT and TET were determined by ICP - MS and quantified by working curve method. Results The method had good linearity in 8.60 μg/L - 451.0 μg/L and 6.35 μg/L -472.5 μg/L, and the correlation coefficients were greater than 0. 998, the quantitative limits were 8.60 μg/L and 6. 35 μg/L when the urine samples were diluted five times; the within - run precision was within 1.30% - 6.40% , the between - run precision was withihn 1.50% - 6.44%, and the recovery was within 87.48% - 96.64%. Condusion The method is simple and convenient with good accuracy and precision, which can be used for analyzing TMT and TET in urine rapidly.

关 键 词：人尿 三甲基氯化锡 三乙基氯化锡 高效液相色谱-电感耦合等离子体质谱联用法 

分 类 号：O657.63[理学—分析化学]