超高效液相色谱-三重四级杆串联质谱法快速测定水中苯胺和联苯胺

Rapid determination of aniline and benzidine in water by liqud chromatographytandem mass spectrometry

建立了直接进样-超高效液相色谱-三重四级杆串联质谱法(UPLC-MS/MS)快速测定水中苯胺和联苯胺的分析方法。样品经0.45μm聚醚砜(PES)滤膜过滤除去颗粒性杂质后,采用ACQUITY UPLC?BEH C8(1.7μm,2.1 mm×50 mm)为分离柱,甲醇-0.1%甲酸水溶液(v/v)为流动相进行梯度洗脱,电喷雾离子源(ESI)电离,多反应监测模式(MRM)进行定性和定量分析。经条件优化,苯胺和联苯胺可在3 min内分析完毕,检出限分别为0.1μg/L和0.03μg/L,且在0.2~20.0μg/L范围内线性关系良好(r>0.999)。对3组不同浓度(0.5μg/L,2.0μg/L,5.0μg/L)加标的实际水样平行测定6次,苯胺和联苯胺的相对标准偏差在1.0%~5.4%范围内,回收率为97.6%~113%。该方法简便快捷,灵敏度高,适用于实际水样的分析。

A new method was developed for the rapid determination of aniline and benzidine in water by direct injection-ul tra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The water samples were filtered through a 0.45μm polyether sulfone(PES)membrane,separated with a ACQUITY UPLC?BEH C8 column(1.7μm,2.1 mm×50 mm)using methanol-0.1%formic acid aqueous solution(v/v)as mobile phase in gradient elution mode,then detect ed with electrospray ionization mass spectrometry in multiple reaction monitoring(MRM)mode.In the optimized condi tion,aniline and benzidine can be analysed within 3 min,with detection limits of 0.1μg/L and 0.03μg/L and good linearity in the range of 0.2~20.0μg/L(r<0.999).The recoveries range from 97.6%to 113%with the relative standard deviations between 1.0%and 5.4%at three spiked levels(n=6).The established method showed the advantages of rapidity,sensitivity and accuracy,which is suitable for rapid determination of aniline and benzidine in water.