固相萃取-高效液相色谱串联质谱法同时检测饮用水中的六种农药

Simultaneous determination of 6 pesticides in drinking water by high performance liquid chromatography-tandem mass spectrometry with solid phase extraction

目的建立同时测定生活饮用水中灭草松、2，4-滴、呋喃丹、甲萘威、莠去津和五氯酚6种农药的液相色谱一串联质谱方法，为《生活饮用水标准检验方法》（GB／T5750-2006）的修订提供参考，并对江苏境内12个集中式供水出厂水中上述6种农药含量进行评估。方法用盐酸调节水样至pH≤2，取10ml水样经反相固相萃取小柱富集，丙酮洗脱，氮吹仪浓缩，溶剂转换后，以甲醇和（或）水为流动相，经C，。液相色谱柱分离，用液相色谱-串联质谱仪外标法测定，并对方法的检测限、准确度和精密度进行评价。检测了江苏境内12个集中式供水出厂水中上述6种农药含量。结果采用本检测方法，6种农药最低检测质量浓度在0．02～0．41μg/L之间，回收率在75％--115％之间，RSD在2％--10％之间。江苏境内12个集中式供水出厂水中上述6种农药含量均小于最低检测浓度。结论建立的方法可同时检测6种农药，检测效率高，废液排放少，能更好地满足饮用水卫生监测的需要。

Objective To develop an analytical method for simultaneous determination of 6 pesticides, namely bentazone, 2, 4-diehlorophenoxyacetic acid, carbofuran, carbaryl, atrazine and pentachlorophenol, in drinking water by high performance liquid chromatography-tandem mass spectrometry, and thereby to provide a reference to revise the Health Standards for Drinking Water （GB/T 5750-2006 ）. Meanwhile,to evaluate the content of the above 6 pesticides in the drinking water samples supplied by 12 centralized water plants in Jiangsu province. Methods The l0 ml water sample was acidized by hydrochloric acid to pH ≤ 2, and then concentrated by solid phase extraction cartridge and eluted with acetone. The solvent was changed into methanol after drying by nitrogen blow. The target compounds were separated by Cls column using methanol/water as mobile phase, and detected by mass spectrometry with multi-reaction-monitoring（MRM） mode. The repeatability and sensitivity of the assay were evaluated. The drinking water samples from the 12 water plants were then detected. Results In this experimental method, the minimum detectable concentration were around 0.02 -0. 41 μg/L, with the recovery rate at 75% - 115% ,and the RSD between 2% and 10%. Under the experimental condition, there were no pesticides detected in the drinking water samples from the 12 centralized water plants. Conclusion The method is efficient and environment-friendly, with little discharge of effluent, which could meet the requirement of the drinking water monitor.