超高效液相色谱-串联质谱联法测定茶园用农药制剂中烷基酚聚氧乙烯醚含量

Determination of Alkylphenol Ethoxylates in Agrochemicals for Tea Garden by UPLC-MS/MS

建立了超高效液相色谱-串联质谱法测定茶园用农药制剂中烷基酚聚氧乙烯醚(APEOs)的检测方法。APEOs经Waters-BEH C_(18)色谱柱分离,电喷雾正离子源(ESI+)条件下多反应监测模式(MRM)测定,外标法定量。APEOs(n=3～20)在水剂、水乳剂、悬浮剂、乳油、颗粒剂和可湿性粉剂中的基质标准曲线在0.047～1503.6 mg·kg^(-1)范围内线性关系良好,相关系数(r)为0.996 1～0.999 9;在0.5～1 503.6 mg·kg^(-1)添加范围内,添加回收率为83.8%～120.4%,相对标准偏差(RSD)为0.6%～13.7%,LOQ为0.5～150.4 mg·kg^(-1)。测定的51种茶园农药制剂中,辛基酚聚氧乙烯醚(OPEOs)百分数含量均低于0.5%;壬基酚聚氧乙烯醚(NPEOs)质量分数为ND～32.1%,检出率90.2%,NPEOs在茶园用农药中应用普遍。

This study established an ultra high performance liquid chromatography-tandem mass spectrometry method for the determination of alkylphenol polyoxyethylene(APEOs)in pesticide formulations.APEOs were separated on a Waters-BEH C18 column,measured by a multi-reaction monitoring mode(MRM)with an electrospray positive ion source(ESI+),and quantified by an external standard method.The matrix standard curve of APEOs(n=3-20)in aqueous solutions,water emulsion,suspension concentrate,emulsif iable concentrate,granules and wettable powder had a good linearity in the range of 0.047-1 503.6μg·kg^-1 with the correlation coefficient(r)between 0.996 1 and 0.999 9.The recovery of APEOs spiked in the level of 0.5-1 503.6μg·kg^-1 ranged from 83.8%-120.4%with relative standard deviation(RSD)of 0.6%-13.7%,and the limits of quantity(LOQs)of 0.5~150.4μg·kg^-1.Among the 51 pesticide formulations used in tea gardens,the percentage of Octylphenol ethoxylates(OPEOs)was less than 0.5%.The mass fraction of nonylphenol ethoxylates(NPEOs)was ND-32.1%and the detection rate was 90.2%,indicating the wide use of NPEOs in pesticides in tea gardens.