高效液相色谱-串联质谱法同时测定饮用水中的13种农药残留

Determination of thirteen pesticides in drinking water by HPLC- MS / MS

目的建立饮用水中的灭草松、甲基对硫磷、乐果、2,4-滴、多菌灵、呋喃丹、莠去津、敌敌畏、毒死蜱、丁草胺、甲草胺和乙草胺等13种农药残留的高效液相色谱-串联质谱(HPLC-MS/MS)同时测定方法。方法水样经0.22μm滤膜过滤后直接进样,采用液相色谱-串联质谱仪进行测定,色谱柱采用Accucore C18(100 mm×2.1 mm,2.6μm),以乙腈-水-甲酸为流动相,梯度洗脱。采用电喷雾电离(ESI),多反应监测(MRM)模式进行检测。结果本法测定的线性范围为0.50 ng/ml^100.00 ng/ml,线性相关系数(r)为0.998 8~1.000 0,检出限为0.001 ng/ml^0.250 ng/ml。在低、中、高3种添加浓度下,方法的平均回收率为81.0%~119.0%,相对标准偏差(RSD)为0.54%~11.00%。结论本法操作简单,准确、快速、灵敏,能满足日常大批量水样中多种农药残留的快速准确分析。

Objective To establish a method for the simultaneous determination of thirteen pesticides,including bentazone,parathion- methyl,dimethoate,2,4- D,carbendazim,carbofuran,atrazine,dichlorvos,chlorpyrifos,butachlor,alachlor and acetochlor in drinking water by high performance liquid chromatography- tandem mass spectrometry（ HPLC- MS / MS）. Methods Water samples were filtrated with a 0. 22 μm millipore filter,and then detected by HPLC- MS / MS. The analytes were separated on an Accucore C18column（ 100 mm × 2. 1 mm,2. 6 μm） using a programmed gradient elution with a mobile phase consisting of acetonitrile,water and formic acid. Identification was achieved by electrospray ionization（ ESI） in multiple reaction monitoring mode. Results The linearity ranged from 0. 50 ng / ml to 100. 00 ng / ml wutg this method,the correlation coefficients（ r） were from 0. 998 8 to 1. 000 0,and the detection limits were among 0. 001 ng / ml- 0. 250 ng / ml. The average recoveries were among 81. 0%- 119. 0%,and the relative standard deviation（ RSD） was among 0. 54%- 11. 00% under the high,the mid and the low addictive concentrations. Conclusion The method is simple,rapid and sensitive,so it is applicable for the simultaneous determination of multi- pesticides residues in drinking water.