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建立了水中21种有机污染物的在线固相萃取-超高效液相色谱-质谱联用分析方法,包括微囊藻毒素-LR,微囊藻毒素-RR以及19种农药。方法均只需对样品进行简单过滤即可上机测定,进样量为5 m L。水样首先通过在线SPE柱净化(HLB柱),再经过BEH C18柱分离目标化合物,采用多反应监测模式测定。方法的线性相关系数R2>0.99,地表水和自来水样品的加标回收率为70.1%~118.2%,RSD在1.0%~19%之间,定量限(LOQ,S/N=10)范围1~100 ng/L,满足测定饮用水残留限量要求。
An online on-line SPE-UHPLC-MS method was developed for 21 organic pollutants in water, including microcystin-LR, microcystin-RR and 19 pesticides. The method is simple to filter the sample can be measured on the machine, the injection volume of 5 m L. Water samples were first purified on an on-line SPE column (HLB column) followed by a BEH C18 column to separate the target compounds using multiple reaction monitoring. The linear correlation coefficient R2> 0.99, the spiked recoveries of surface water samples and tap water samples were 70.1% ~ 118.2%, RSD ranged from 1.0% to 19%, and the limits of quantification (LOQ, S / N = 100 ng / L, to meet the determination of drinking water residue limit requirements.