同位素稀释超高效液相色谱串联质谱测定尿液中苯系物和三氯乙烯代谢产物  

Determination of Metabolites of Benzene Compounds and Trichloroethylene in Urinary by Isotope Dilution-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：朱婧[1] 李妍[1] 雍莉[2] 郑波[1] 邹晓莉[1] 刘珍[3] 

机构地区：[1]四川大学华西公共卫生学院卫生检验教研室,成都610041 [2]四川省疾病预防控制中心,成都610041 [3]四川大学华西第二医院出生缺陷中心,成都610041

出　　处：《分析化学》2016年第1期81-87,共7页Chinese Journal of Analytical Chemistry

基　　金：国家重点基础研究发展计划(No.2010CB529502)资助~~

摘　　要：建立同位素内标稀释超高效液相色谱串联质谱（Ultra performance liquid chromatography-tandem mass sepctrometry,UPLC-MS/MS）同时测定尿中苯系物和三氯乙烯代谢产物的方法,并用于孕妇尿样的分析。尿样过经合同位素内标的醋酸铵缓冲液稀释10倍后,过滤,取滤液进样分析。采用C18色谱柱,梯度洗脱进行UPLC分离,电喷雾负离子扫描多反应监测（Multiple reaction monitoring,MRM）模式检测。方法检出限在0.0350-1.75μg/L之间,方法的日内和日间精密度分别为1.2%-9.1%和2.0%-9.7%;用所建立的方法测定了650个孕妇尿液样品,并统计分析了其地区差异加标回收率为85.0%-104%。所建立的方法快速灵敏,适合尿液样品的批量分析。A method for simultaneous determination of metabolites of benzene compounds and trichloroethylene in pregnant urine by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry was established.Urine samples were diluted 10 times with ammonium acetate buffer containing working mixed internal standard and the filtrate was injected into UPLC/MS/MS for analysis.UPLC-MS/MS was performed on Waters C18 column and the gradient elution was used for separation.The negative electrospray ionization（ESI） source under the multiple reaction monitoring（MRM） mode was used for quantitative analysis.The limits of detection（LOD） ranged from 0.0350 μg/L to 1.75 μg/L.The inter-day and intra-day precisions of method were 1.2%-9.1%and 2.0%-9.7%,respectively.The proposed method was applied on detecting 650 urine samples of pregnant women in different region and the results were analyzed by statistical method.The spiked recoveries were in the range of 85.0%-104%.The method was quick,sensitive and suitable for batch analysis of urine samples.

关 键 词：同位素稀释 超高效液相色谱串联质谱 苯系物 三氯乙烯 代谢物 尿液 

分 类 号：O657.63[理学—分析化学] R446.12[理学—化学]