尿中三氯卡班和三氯生测定的QuEChERS-超高效液相色谱-串联质谱法

Determination of triclocarban and triclosan in urine by QuEChERS extraction and ultra-performance liquid chromatography-tandem mass spectrometry

目的建立QuEChERS净化后超高效液相色谱-三重四极杆质谱联用(UPLC-MS/MS)法测定尿液中三氯卡班(TCC)和三氯生(TCS)含量。方法于2022年5月,将尿液样品经乙腈提取,QuEChERS净化,Waters Acquity UPLC BEH C18柱(100 mm×2.1 mm,1.7μm)分离,以水-乙腈体系为流动相梯度洗脱,流速为0.3 ml/min,采用电喷雾负离子模式和多反应监测扫描方式检测,内标法定量分析,对建立的方法进行方法学验证。结果TCC和TCS的线性范围为分别为0.5~100.0μg/L和1.0~100.0μg/L,相关系数分别为0.9997、0.9991;方法检出限分别为0.17和0.33μg/L,定量限分别为0.5和1.0μg/L;在2.0、10.0、80.0μg/L 3个加标水平下,TCC和TCS的加标回收率分别为100.1%~102.8%和96.7%~108.6%,相对标准偏差分别为4.9%~6.7%和4.1%~8.3%。结论QuEChERS-UPLC-MS/MS法操作简便、快速、灵敏、重现性好,可用于职业人群TCC和TCS暴露水平的同时快速准确检测。

Objective To establish a method for the determination of triclocarban(TCC)and triclosan(TCS)in urine by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)after purification by QuEChERS.Methods In May 2022,urine samples were extracted by acetonitrile,purified by QuEChERS,separated by Waters Acquity UPLC BEH C18 column(100 mm×2.1 mm,1.7μm),and eluated with water-acetonitrile as mobile phase gradient at a flow rate of 0.3 ml/min.The detection was conducted in negative ion mode(ESI-)and multiple reaction monitoring(MRM)scanning,it was quantified with a internal standard method,and the methodology was verified.Results The linear ranges of TCC and TCS were 0.5-100.0μg/L and 1.0-100.0μg/L,and the correlation coefficients were 0.9997 and 0.9991,respectively.The limits of detection and quantitation of TCC and TCS were 0.17 and 0.33μg/L,and 0.5 and 1.0μg/L,respectively.The recoveries of TCC and TCS were 100.1%-102.8%and 96.7%-108.6%,and the relative standard deviations were 4.9%-6.7%and 4.1%-8.3%,respectively,at 2.0,10.0 and 80.0μg/L.Conclusion QuEChERS-UPLC-MS/MS method is simple,rapid,sensitive and reproducible,and can be used for rapid and accurate simultaneous detection of TCC and TCS exposure levels in occupational population.