高效液相色谱-串联质谱联用法测定饮用水和水源水中莠去津、呋喃丹和甲基对硫磷

Determination of three pesticides in drinking water by high performance liquid chromatography-tandem mass spectrometry

目的:建立液相色谱-串联质谱法测定饮用水和水源水中莠去津、呋喃丹和甲基对硫磷等3种农药的方法,以完善现有国标《生活饮用水卫生标准检测方法》有关内容。方法:采用直接进样方式,用高效液相色谱-串联质谱(HPLC/MS/MS)测定饮用水和水源水中的3种农药。水样经0.22μm微孔滤膜过滤,采用HPLC/MS/MS电喷雾电离(ESI),多反应监测(MRM)模式检测,外标法定量。结果:方法的线性范围为0.5μg/L～50.0μg/L,线性相关系数在0.9991-0.9998之间,检出限在0.03μg/L～0.05μg/L之间;两个水平的平均加标回收率范围在92.0%～98.0%之间;相对标准偏差(RSD)均小于8.83%。结论:该方法用于测定饮用水和水源水中3种农药具有操作简单、干扰少、快速、准确可靠等特点,符合国家卫生标准方法建立的相关要求。

Objective ： A high performance liquid chromatography - tandem mass spectrometric method was estab- lished for determination of three pesticides in drinking water and source water to perfect the current ＂Standard test method for drinking water sanitation＂. The three pesticides were atrazine, carbofuran and methyl parathion. Meth- ods ： The three pesticides in water were cleaned by 0.22 μm millipore filter, then detected by high performance liq- uid chromatography - tandem mass spectrometry. Identification was achieved by electrospray ionization （ESI） in multiple reaction monitoring mode. Quantification was performed by external standard calibration. Results： The cal- ibration curves of three pesticides showed good linearity in the range of 0.5 μg/L - 50.0 μg/L with correlation coef- ficient in the range of 0. 9991 -0. 9998. The detection limit of the method was from 0.03 μg/L to 0.05 μg/L. The recoveries of two spiking levels ranged from 92.0% to 98.0% , and RSDs of the three pesticides were all less than 8.83%. Conclusion： The method for determination of three pesticides in drinking water and source water by HPLC - MS/MS had the advantages of simple operation, less interference, rapidity and accuracy, which could meet the re- quirements of national health standard method for the determination of pesticides in drinking water and source water.