Simultaneous determination of parabens, triclosan and triclocarban in water by liquid chromatography/electrospray ionisation tandem mass spectrometry
Simultaneous determination of parabens, triclosan and triclocarban in water by liquid chromatography/electrospray ionisation tandem mass spectrometry
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DOI：
10.1002/rcm.4069
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发表时间：
2009-06-01
影响因子：
2
通讯作者：
Cela, Rafael
中科院分区：
文献类型：
--
作者：
Gonzalez-Marino, Iria;Benito Quintana, Jose;Cela, Rafael
建立了液相色谱-电喷雾串联质谱法（LC/ESI-MS/MS）测定水中几种家用杀菌剂的方法。它允许同时测定三氯生（ITCS）、三氯卡班（TCC）和七种对羟基苯甲酸酯，包括丙基（i-PrP和n-PrP）和对羟基苯甲酸丁酯（i-BuP和n-BuP）的支链异构体和线性异构体的区别。在LC/MS/MS之前，分析物在Oasis HLB （60 mg）筒上以自然样品pH进行固相萃取（SPE）预浓缩，然后用4ml甲醇洗脱。这个简单的SPE程序提供了85%以上的萃取回收率，除了原始废水，其中TCC下降到65%。该方法的性能通过两台来自低/中和中高市场范围的三重四极杆LC/MS仪器进行测试：一台瓦里安1200L和一台API-4000。在0.08 ~ 0.44 ng/L的地表水中，后一种体系的定量下限（loq）是第一种体系的3 ~ 80倍。此外，对两种工具的基质效应的比较显示出非常不同的行为，特别是对羟基苯甲酸酯。对于这些化合物，在1200L仪器上观察到信号抑制，而在4000仪器上观察到信号增强。结果表明，在不同色谱/质谱系统之间的方法转换中，需要对矩阵效应进行重新评估。该方法在实际样品中的应用表明，对羟基苯甲酸甲酯（MeP）和n-PrP（原液中含量为1-6 μ g/L）普遍存在，i-BuP和n-BuP在相似水平下共存（原液中含量约为100-200 ng/L）。版权所有John Wiley & Sons， Ltd. 2009
A method for the determination of several household biocides in water by liquid chromatography/electrospray ionisation tandem mass spectrometry (LC/ESI-MS/MS) is presented. It permits the simultaneous determination of triclosan ITCS), triclocarban (TCC) and seven parabens, including the distinction between branched and linear isomers of propyl (i-PrP and n-PrP) and butyl parabens (i-BuP and n-BuP). Prior to LC/MS/MS, analytes are preconcentrated by solid-phase extraction (SPE) on Oasis HLB (60 mg) cartridges at natural sample pH and subsequently eluted with 4 mL of methanol. This simple SPE procedure provides extraction recoveries above 85% except for raw wastewater, where it falls to 65% for TCC. The performance of the method was tested with two triple-quadrupole LC/MS instruments from a low/mid and mid/high market range: a Varian 1200L and an API-4000. The latter system provided between 3 and 80 times lower limits of quantification (LOQs) than the first one, in the 0.08-0.44 ng/L range for surface water. Moreover, a comparison of matrix effects on both instruments showed a very different behaviour, particularly in the case of parabens. For these compounds signal suppression was observed in the 1200L instrument and signal enhancement with the 4000 instrument. As a result, different calibration approaches were chosen for them and this pointed to the need of matrix effect re-evaluation in method transfer between different LC/MS systems. The application of the method to real samples showed the ubiquity of methyl paraben (MeP) and n-PrP (at the 1-6 mu g/L in raw wastewater) and the coexistence of i-BuP and n-BuP at similar levels (ca. 100-200 ng/L in raw wastewater). Copyright (C) 2009 John Wiley & Sons, Ltd.