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目的建立生活饮用水中三氯生(triclosan,TCS)和三氯卡班(triclocarban,TCC)残留的固相萃取-超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。方法水样经0.45μm滤膜过滤后,采用Oasis HLB固相萃取柱进行富集净化,以ACQUITY UPLC BEH C18色谱柱(2.1 mm×50 mm,1.7μm)分离,甲醇-0.1%甲酸溶液为流动相进行梯度洗脱,质谱采用电喷雾负离子电离、多反应监测模式检测。结果三氯卡班、三氯生的线性范围分别为0.01~10.0μg/L、0.1~100μg/L,所得回归方程线性均较好(r≥0.999 8);方法检出限分别为0.07、0.02 ng/L,定量下限分别为0.23、0.07 ng/L,平均回收率分别在61.6%~101.8%和78.6%~97.8%之间,RSD分别在2.4%~4.7%和2.2%~4.1%之间。结论该方法灵敏度和准确度均较高,精密度较好,适用于生活饮用水中三氯生和三氯卡班残留的测定。
Objective To establish a method for the determination of triclosan (TCS) and triclocarban (TCC) residues in drinking water by solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods The water samples were filtered through a 0.45 μm membrane filter and cleaned up using an Oasis HLB solid phase extraction column and separated on an ACQUITY UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm). The methanol-0.1% formic acid solution was flowed Phase gradient elution, electrospray ionization mass spectrometry, multi-reaction monitoring mode detection. Results The linear ranges of triclocarban and triclosan were 0.01 ~ 10.0μg / L and 0.1 ~ 100μg / L, respectively. The linear regression equations were good (r≥0.9998). The detection limits were 0.07,0.02 ng / L, the lower limit of quantification was 0.23 and 0.07 ng / L respectively, the average recoveries were between 61.6% and 101.8% and 78.6% to 97.8%, respectively, with RSDs between 2.4% and 4.7% and between 2.2% and 4.1% . Conclusion The method has higher sensitivity and accuracy and better precision, and is suitable for the determination of triclosan and triclocarban residues in drinking water.