地表水中致癌芳香胺的高效液相色谱-串联质谱直接测定方法

Direct determination of carcinogenic aromatic amines in surface water by UHPLC-MS /MS

建立了超高效液相色谱-串联质谱(UHPLC-MS/MS)快速直接测定地表水中致癌芳香胺物质的方法.样品采集后,用0.22μm的聚四氟乙烯(PTFE)滤膜过滤,用C18 RRHD色谱柱进行梯度洗脱分离,流动相为甲醇和水,采用电喷雾正离子模式,并采用多反应监测模式(MRM)测定,外标法定量.方法重点优化了色谱分离条件、质谱碎裂电压、碰撞能量,考察了流动相中甲酸铵或甲酸浓度对目标化合物响应的影响.23种组分不同浓度水平的加标回收率在70.3%—119.8%之间,相对标准偏差在2.1%—10.2%(n=7)之间,方法的定量限(LOQ)在0.01—2.0μg·L-1之间.方法具有操作方便、灵敏度较高、快速准确的优点,能为环境水体污染源监测、饮水安全提供技术保障.

A rapid method was developed for the quantitative determination of 23 carcinogenic aromatic amines in surface water by ultra high performance liquid chromatography tandem electrospray ionization mass spectrometry （UHPLC-MS/MS）. After water sample was collected, it was filtered with a 0.22 μm polytetrafluoroethylene （PTFE） membrane, and then the target compounds were separated on a C18 RRHD column, gradient eluted with methanol and water, and determined by positive electrospray ionization mass spectrometry with multiple reaction monitoring mode （MRM）. Quantitative analysis was performed with external standard calibration method in the study. UHPLC separation condition, concentration of ammonium formate and formic acid in mobile phase, fragmentor voltages, and collision energies were optimized. The relative standard deviation （RSD） of the developed method was in the range of 2.1%-10.2% （n = 7）. Standard added recoveries in sample matrix ranged from 70.3% to 119.8%. The limit of quantification （LOQ） was from 0.01 to 2.0μg·L^-1. The proposed method is easy to operate, highly sensitive, fast, and accurate.