超高效液相色谱-串联质谱法快速测定地表水中联苯胺、苦味酸、甲萘威、阿特拉津和溴氰菊酯

Rapid determination of benzidine,picric acid,carbaryl,atrazine,and deltamethrin in surface water by ultra-performance liquid chromatography-tandem mass spectrometry

建立了一种经简单过滤即可直接进样的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法,可快速测定地表水中联苯胺、苦味酸、甲萘威、阿特拉津和溴氰菊酯5种有机物的残留。样品经0.2μm针式滤头过滤除去颗粒性杂质后,进行UPLC-MS/MS分析,采用UPLC HSS T3色谱柱,2 mmol/L乙酸铵甲醇溶液和2 mmol/L乙酸铵水溶液作为流动相进行梯度洗脱,电喷雾离子源电离,正、负离子切换多反应监测模式进行定性和定量分析。5种目标化合物分别在0.10~10.0μg/L或1.00~100μg/L范围内线性关系良好,相关系数为0.996~0.999,方法的检出限为0.01~0.22μg/L;高、中、低3个添加水平的回收率为81.4%~113%,相对标准偏差为0.84%~14.0%。利用该方法对杭州市部分河流和水库的地表水样品进行分析,其中阿特拉津和溴氰菊酯在部分水样中有阳性检出。结果表明,该方法简便快捷、灵敏准确,适用于地表水样品中联苯胺、苦味酸、甲萘威、阿特拉津和溴氰菊酯的快速测定。

A method requiring no pre-treatment steps other than filtration,using ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),has been developed and applied for the rapid determination of benzidine,picric acid,carbaryl,atrazine,and deltamethrin residues in surface water.Water samples were filtered with a 0.2-μm syringe filter for particle removal and injected directly into the UPLC instrument.The separation was performed on a Waters Acquity UPLC HSS T 3 column utilizing a gradient elution program of methanol(containing 2 mmol/L ammonium acetate)and water(containing 2 mmol/L ammonium acetate)as the mobile phases at a flow rate of 0.4 mL/min.The detection was accomplished by multiple-reaction monitoring scanning in positive/negative ion-switching electrospray ionization mode.Good linearity was observed in the range 0.10-10.0μg/L or 1.00-100μg/L for different targets with correlation coefficients of 0.996-0.999.The limits of detection(LODs)were 0.01-0.22μg/L.The recoveries ranged between 81.4%and 113%at three spiked levels with relative standard deviations(n=6)between 0.84%and 14.0%.The developed method was applied to the analysis of surface waters(river water and reservoir water)from Hangzhou;atrazine and deltamethrin were detected in part of the analyzed samples.This proposed method was characterized by high sensitivity and precision,extensive analytical range,and a high analytical rate,and showed suitability for the analysis of the five named pollutants in surface water.