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

doi:10.13305/j.cnki.jts.2019.01.012

茶叶科学 ›› 2019, Vol. 39 ›› Issue (1): 105-113.doi: 10.13305/j.cnki.jts.2019.01.012

• • 上一篇

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^1,2,3, 周利^1,3,*, 罗逢健^1,3, 杨洁^1,2,3, 王新茹^1,3, 孙荷芝^1,3, 杨梅^1,3, 陈宗懋^1,3,*

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

收稿日期:2018-08-13 修回日期:2018-10-08 出版日期:2019-02-15 发布日期:2019-07-17
通讯作者: *
作者简介: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。
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^1,2,3, ZHOU Li^1,3,*, LUO Fengjian^1,3, YANG Jie^1,2,3, WANG Xinru^1,3, SUN Hezhi^1,3, YANG Mei^1,3, CHEN Zongmao^1,3,*

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:2018-08-13 Revised:2018-10-08 Online:2019-02-15 Published:2019-07-17

摘要/Abstract

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。

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

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.

Key words: pesticide additives, pesticide formulations, tea, alkylphenol ethoxylates, ultra high performance liquid chromatography-tandem mass spectrometry

中图分类号:

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.

LIN Qin, ZHOU Li, LUO Fengjian, YANG Jie, WANG Xinru, SUN Hezhi, YANG Mei, CHEN Zongmao. Determination of Alkylphenol Ethoxylates in Agrochemicals for Tea Garden by UPLC-MS/MS[J]. Journal of Tea Science, 2019, 39(1): 105-113. doi: 10.13305/j.cnki.jts.2019.01.012.

参考文献

[1] Zhou L, Luo F J, Zhang X Z, et al.Dissipation, transfer and safety evaluation of emamectin benzoate in tea[J]. Food Chemistry, 2016, 202: 199-204.
[2] 霍鹏. 茶叶中重金属污染物残留及消减研究[J]. 福建茶叶, 2016, 38(6): 253-254.
[3] Wang X, Zhou L, Luo F J, et al.9,10-Anthraquinone deposit in tea plantation might be one of the reasons for contamination in tea[J]. Food Chemistry, 2018: 254-259.
[4] 卜元卿, 王昝畅, 智勇,等. 368种农药制剂中助剂使用状况调查研究[C]//2014中国环境科学学会学术年会. 2014.
[5] Bennie D T.Review of the environmental occurrence of alkylphenols and alkylphenol ethoxylates[J]. Water Quality Research Journal of Canada, 1999, 34(1): 79-122.
[6] 佚名. 农业部农药检定所《关于征求〈农药助剂禁限用名单〉(征求意见稿)意见的通知》[J]. 中国食品, 2015(15):135-135.
[7] Koh Y K, Chiu T Y, Boobis A R, et al.A sensitive and robust method for the determination of alkylphenol polyethoxylates and their carboxylic acids and their transformation in a trickling filter wastewater treatment plant[J]. Chemosphere, 2008, 73(4): 551-556.
[8] 王艳平. 高风险农药助剂在土壤的残留特征及环境行为初探[D]. 北京: 中国农业科学院研究生院, 2011: 1-70.
[9] Jiang Z J, Cao X L, Li H, et al.Fast determination of alkylphenol ethoxylates in leafy vegetables using a modified QuEChERS and ultra-high performance supercritical fluid chromatography-tandem mass spectrometry[J]. Journal of Chromatography A, 2017, 1525: 161-177.
[10] Lu Y Y.A simplified method for simultaneous quantitation of alkylphenols and alkylphenol ethoxylates in meat and fish using high-performance liquid chromatography with fluorescence detection[J]. International Journal of Environmental Analytical Chemistry, 2006, 86(10):713-722.
[11] Ferrara F, Ademollo N, Orrù M A, et al.Alkylphenols in adipose tissues of Italian population[J]. Chemosphere, 2011, 82(7): 1044-1049.
[12] Chen M J, Zhu P F, Xu B, et al.Determination of nine environmental phenols in urine by ultra-high-performance liquid chromatography-tandem mass spectrometry.[J]. Journal of Analytical Toxicology, 2012, 36(9): 608-615.
[13] Ademollo N, Ferrara F, Delise M, et al.Nonylphenol and octylphenol in human breast milk[J]. Environment International, 2008, 34(7): 984-987.
[14] 郭文建, 王超, 吕怡兵,等. 固相萃取-液相色谱/荧光检测法同时测定水中8种烷基酚和烷基酚聚氧乙烯醚[J]. 环境化学, 2018(3): 497-504.
[15] 高俊伟, 叶平, 谢坚,等. 高效液相色谱-质谱法测定车用清洗剂中烷基酚聚氧乙烯醚[J]. 化学试剂, 2018(1): 57-59.
[16] 江泽军, 曹晓林, 李辉, 等. 液体农药制剂中烷基酚及其聚氧乙烯醚类助剂的高效液相色谱分析[J]. 农药学学报, 2017, 19(2): 245-253.
[17] Chen J, Mullin C A.Determination of nonylphenol ethoxylate and octylphenol ethoxylate surfactants in beehive samples by high performance liquid chromatography coupled to mass spectrometry[J]. Food Chemistry, 2014, 158(158): 473-479.
[18] 张鹏, 赵楠楠, 苏杭, 等. 高效液相色谱-串联质谱法检测三苯乙烯基苯酚聚氧乙烯醚[J]. 色谱, 2017, 35(7): 730-734.

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

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 15

Metrics

本文评价

推荐阅读 10

[1]	陈宇宏, 高颖, 韩震, 尹军峰. 不同种质茶叶籽皂素含量及组成分析[J]. 茶叶科学, 2022, 42(5): 705-716.
[2]	李峥, 刘锭, 霍增辉, 陈富桥. 中国与RCEP成员国茶叶贸易竞争性与互补性分析[J]. 茶叶科学, 2022, 42(5): 740-752.
[3]	李自强, 杨梅, 张新忠, 罗逢健, 周利, 楼正云, 孙荷芝, 王新茹, 陈宗懋. 超高效液相色谱-串联质谱法检测绿茶中16种农药残留[J]. 茶叶科学, 2022, 42(4): 537-548.
[4]	方梦瑞, 吕军, 阮建云, 边磊, 武传宇, 姚青. 基于改进YOLOv4-tiny的茶叶嫩芽检测模型[J]. 茶叶科学, 2022, 42(4): 549-560.
[5]	刘奇, 欧阳建, 刘昌伟, 陈宏宇, 李娟, 熊立瑰, 刘仲华, 黄建安. 茶叶品质评价技术研究进展[J]. 茶叶科学, 2022, 42(3): 316-330.
[6]	向晶, 梁月荣, 赵东, 王开荣, 陆建良, 袁名安, 郑新强. 不同品种、地区茶叶籽仁含油量及茶叶籽油中脂肪酸组分和含量差异性分析[J]. 茶叶科学, 2022, 42(2): 233-248.
[7]	胡高华, 曹建荣, 杨蕾文宣, 王晨, 周苏娟, 刘新, 鲁成银, 陈红平, 马桂岑. 基于壳聚糖/氧化石墨烯/硅藻土固相萃取-液相色谱串联质谱测定茶叶中多种农药残留[J]. 茶叶科学, 2022, 42(2): 249-262.
[8]	疏再发, 郑生宏, 邵静娜, 周慧娟, 吉庆勇, 刘瑜, 何卫中, 王丽鸳. 不同茶树品种（系）对减半施肥的响应研究[J]. 茶叶科学, 2022, 42(2): 277-289.
[9]	吴芹瑶, 杨江帆, 林程, 管曦. 中国茶叶生产布局变迁研究[J]. 茶叶科学, 2022, 42(2): 290-300.
[10]	何文丽, 潘杉, 管曦. 可追溯茶叶产品的认知、信任与购买意愿研究[J]. 茶叶科学, 2022, 42(1): 140-150.
[11]	王春晓, 高峰, 陈富桥, 曾亮. “一带一路”倡议对中国茶叶出口的影响——基于渐进双重差分模型的实证分析[J]. 茶叶科学, 2021, 41(6): 865-875.
[12]	刘诗羽, 李道和. 中国对美国市场茶叶出口贸易波动成因分析——基于修正的CMS模型[J]. 茶叶科学, 2021, 41(6): 876-888.
[13]	许丽佳, 刘琦, 代建武, 陈小虎. 茶叶嫩梢采摘末端执行器的设计研究[J]. 茶叶科学, 2021, 41(5): 705-716.
[14]	马佳丽, 王晨, 陈红平, 柴云峰, 诸力, 刘新. 注射器内分散固相萃取-超高效液相色谱-串联质谱法快速测定茶叶中24种农药残留[J]. 茶叶科学, 2021, 41(5): 717-730.
[15]	陈冬梅, 韩文炎, 周贤锋, 吴开华, 张竞成. 基于自适应增强的BP模型的浙江省茶叶产量预测[J]. 茶叶科学, 2021, 41(4): 564-576.