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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

  • 林琴 ,
  • 周利 ,
  • 罗逢健 ,
  • 杨洁 ,
  • 王新茹 ,
  • 孙荷芝 ,
  • 杨梅 ,
  • 陈宗懋
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  • 1. 中国农业科学院茶叶研究所农产品质量安全研究中心,浙江 杭州 310008;
    2. 中国农业科学院研究生院,北京 100081;
    3. 农业部茶叶质量安全控制重点实验室,浙江 杭州 310008
林琴,女,硕士研究生,主要从事茶叶中农药和污染物残留研究。E-mail: 13318703097@sina.cn。

收稿日期: 2018-08-13

  修回日期: 2018-10-08

  网络出版日期: 2019-07-17

基金资助

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)

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

  • LIN Qin ,
  • ZHOU Li ,
  • LUO Fengjian ,
  • YANG Jie ,
  • WANG Xinru ,
  • SUN Hezhi ,
  • YANG Mei ,
  • CHEN Zongmao
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  • 1. Research Center of Quality Safety for Agricultural Products, Tea Research Institute, Chinese Academy of Agricultural Sciences, Hangzhou 310008, China;
    2. Graduate School of Chinese Academy of Agricultural Sciences, Beijing 100081, China;
    3. Key Laboratory of Tea Quality and Safety Control, Ministry of Agriculture, Hangzhou 310008, China

Received date: 2018-08-13

  Revised date: 2018-10-08

  Online published: 2019-07-17

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 C18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0.047~1β503.6βmg·kg-1范围内线性关系良好,相关系数(r)为0.996β1~0.999β9;在0.5~1β503.6βmg·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0.5~150.4βmg·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。

本文引用格式

林琴 , 周利 , 罗逢健 , 杨洁 , 王新茹 , 孙荷芝 , 杨梅 , 陈宗懋 . 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[J]. 茶叶科学, 2019 , 39(1) : 105 -113 . DOI: 10.13305/j.cnki.jts.2019.01.012

Abstract

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, emulsifiable concentrate,granules and wettable powder had a good linearity in the range of 0.047-1β503.6βmg·kg-1with the correlation coefficient (r) between 0.996β1 and 0.999β9. The recovery of APEOs spiked in the level of 0.5-1β503.6βmg·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 0.5~150.4βmg·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.

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