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, 1.7 μm), 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 0.5-100.0 μg/L and 1.0-100.0 μg/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 0.33 μg/L, and 0.5 and 1.0 μg/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 80.0 μg/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.
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，1.7 μm）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0.5~100.0 μg/L和1.0~100.0 μg/L，相关系数分别为0.999 7、0.999 1；方法检出限分别为0.17和0.33 μg/L，定量限分别为0.5和1.0 μg/L；在2.0、10.0、80.0 μg/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。.
Keywords: QuEChERS; Tandem mass spectrometry; Triclocarban; Triclosan; Ultra-performance liquid chromatography; Urine.