摘要
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.
作者
林琴
周利
罗逢健
杨洁
王新茹
孙荷芝
杨梅
陈宗懋
LIN Qin;ZHOU Li;LUO Fengjian;YANG Jie;WANG Xinru;SUN Hezhi;YANG Mei;CHEN Zongmao(Research Center of Quality Safety for Agricultural Products,Tea Research Institute,Chinese Academy of Agricultural Sciences,Hangzhou 310008,China;Graduate School of Chinese Academy of Agricultural Sciences,Beijing 100081,China;Key Laboratory of Tea Quality and Safety Control,Ministry of Agriculture,Hangzhou 310008,China)
出处
《茶叶科学》
CAS
CSCD
北大核心
2019年第1期105-113,共9页
Journal of Tea Science
基金
科技部科技基础专项(2013FY110100)
浙江省自然科学基金(Y18C160027)
国家茶叶产业技术体系(CARS-23)
关键词
农药助剂
农药制剂
茶叶
烷基酚聚氧乙烯醚
超高效液相色谱-串联质谱
pesticide additives
pesticide formulations
tea
alkylphenol ethoxylates
ultra high performance liquid chromatography-tandem mass spectrometry