建立了人指甲中三氯生和三氯卡班的固相萃取结合超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法.指甲样品经氢氧化钠消化,C18柱富集净化后,通过Waters ACQUITYTM UPLC HSS T3色谱柱(100mm×2.1 mm,1.8 μm)分离,以甲醇和水为流动相进行梯度洗脱,采用三重四极杆串联质谱仪负离子模式进行检测,同位素内标法定量.三氯生和三氯卡班分别在0.5～500.0μg/kg和0.1～ 100.0μg/kg范围内线性关系良好,相关系数(r2)均为0.999,方法定量限分别为2.0 μg/kg和0.2μg/kg.3个水平的平均加标回收率为95.9％～110.2％,相对标准偏差为0.6％ ～ 9.7％(n=6).本方法具有良好的灵敏度、回收率和重复性,适合指甲中痕量目标污染物的测定.利用该方法分析了60份实际样品,目标物的检出率为100％,三氯生和三氯卡班的含量范围分别为＜LOQ ～760.7μg/kg和4.1～1 926.5 μg/kg.
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