固相萃取-超高效液相色谱-串联质谱法测定人指甲中的三氯生和三氯卡班

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 ACQUITY^TM UPLC HSS T3色谱柱(100 mm×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0.5~500.0 μg/kg和0.1~100.0 μg/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0.2 μg/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

Determination of triclosan and triclocarban in human nails by solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry

An analytical method was developed to simultaneously detect triclosan (TCS) and triclocarban (TCC) in human nails using solid phase extraction (SPE) with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Nail clippings were digested by sodium hydroxide, and then concentrated and purified with C18 cartridges. Chromatographic separation was performed on a Waters ACQUITY^TM UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm) with gradient elution using methanol and water at a flow rate of 0.3 mL/min. The target compounds were determined by triple quadrupole mass spectrometer operated in the negative ion mode and quantified by isotopic-dilution technique. The satisfactory linearities (r²=0.999) was obtained over the ranges of 0.5-500.0 μg/kg for TCS and 0.1-100.0 μg/kg for TCC, with the limits of quantification (LOQs) of 2.0 μg/kg for TCS and 0.2 μg/kg for TCC. The average recoveries of the two target compounds (spiked at three concentration levels) ranged from 95.9% to 110.2%, with the relative standard deviations (RSDs) between 0.6% and 9.7% (n=6). This method can be applied in rapid detection of target contaminants in nails due to its high sensitivity, high recovery and good reproducibility. Sixty collected human nail samples were analyzed by means of the developed method. TCS and TCC were detected in all samples with content ranges of