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茶叶科学 ›› 2020, Vol. 40 ›› Issue (3): 397-406.doi: 10.13305/j.cnki.jts.2020.03.010

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固相萃取和分散固相净化-串联质谱测定茶鲜叶和干茶中的农药残留

杨洁1,2, 周利1,*, 余焕1,2, 孙荷芝1, 王新茹1, 张新忠1, 杨梅1, 陈宗懋1, 罗逢健1,*   

  1. 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
  • 收稿日期:2019-09-27 修回日期:2020-01-04 出版日期:2020-06-15 发布日期:2020-06-09
  • 通讯作者: *lizhou@tricaas.com,lfj@tricaas.com
  • 作者简介:杨洁,女,硕士研究生,主要从事茶园有害生物综合治理研究。
  • 基金资助:
    国家重点研发计划子课题(2016YFD0200207-2)、浙江省自然科学基金(LY18C16005)

Determination of Pesticide Residue in Fresh Tea Leaves and Dry Tea by Solid Extraction and Dispersive Solid Extraction Cleanup Coupled with Tandem Mass Spectrum

YANG Jie1,2, ZHOU Li1,*, YU Huan1,2, SUN Hezhi1, WANG Xinru1, ZHANG Xinzhong1, YANG Mei1, CHEN Zongmao1, LUO Fengjian1,*   

  1. 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
  • Received:2019-09-27 Revised:2020-01-04 Online:2020-06-15 Published:2020-06-09

摘要: 建立了茶鲜叶和干茶中9种农药的残留分析方法。样品中的残留农药经乙腈提取,Florisil/GCB固相萃取柱和PSA/GCB分散固相联合净化,超高效液相色谱串联质谱(UPLC-MS/MS)和气相色谱质谱联用(GC-MS)测定。在0.005~1.000 mg·kg-1的添加水平下,目标农药在鲜叶和干茶中的平均回收率在70.3%~103.9%,相对标准偏差(RSD)<20.0%。在0.005~2.000 mg·kg-1浓度范围,目标农药在鲜叶和干茶基质中的线性关系良好,r>0.995 4。定量限(LOQ)为0.005 mg·kg-1。实际样品检测结果表明,该方法灵敏度高,重现性好,能够满足农药多残留检测的要求。

关键词: 农药多残留, 超高效液相色谱串联质谱, 气相色谱质谱联用, 茶, 固相萃取, 分散固相净化

Abstract: A method for the determination of 9 pesticide residues in fresh and dry tea was established. Residual pesticides in samples were extracted by acetonitrile, purified by Florisil/GCB solid phase extraction column, followed by absorbent of PSA and GCB as dispersed solid phase, and determined by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and gas chromatography-mass spectrometry (GC-MS). In the spiked range of 0.005-1.000 mg·kg-1, the average recoveries of target pesticides in fresh leaves and dried tea were 70.3%-103.9%, and the relative standard deviations (RSD) were less than 20%. In the range of 0.005-2.000 mg·kg-1, the linear relationship of target pesticides in fresh leaves and dry tea matrix was good, with r>0.995 4. The limit of quantity (LOQ) was 0.005 mg·kg-1. The test results of actual samples showed that the method was highly sensitive and reproducible, and can meet the requirements of multi-residue detection.

Key words: multi-residue of pesticides, UPLC-MS/MS, GC-MS, tea, solid phase extraction, dispersive solid-phase extraction

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