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茶叶科学 ›› 2018, Vol. 38 ›› Issue (4): 416-424.doi: 10.13305/j.cnki.jts.2018.04.010

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茶叶中邻苯二甲酰亚胺残留气相色谱-串联质谱测定

高贯威1, 陈红平1, 柴云峰1, 金莉莉1,2, 刘新1, 鲁成银1,*   

  1. 1.中国农业科学院茶叶研究所 农业部茶叶产品质量安全风险评估实验室 农业部茶叶质量安全控制重点实验室,浙江 杭州310008;
    2.中国农业科学院研究生院,北京 100081
  • 收稿日期:2018-02-07 修回日期:2018-03-07 出版日期:2018-08-15 发布日期:2019-10-15
  • 通讯作者: *lchy@mail.tricaas.com
  • 作者简介:高贯威,男,山东菏泽人,科研助理,主要从事茶叶质量安全检测与研究。
  • 基金资助:
    中国农业科学院创新团队茶叶质量与风险评估团队项目(CAAS-ASTIP-2014-TRICAAS-06); 浙江省公益应用项目(2017C32059); 现代农业产业技术体系建设专项基金资助项目(nycytx-26)

Determination of Phthalimide Residue in Tea Using Gas Chromatography-tandem Mass

GAO Guanwei1, CHEN Hongping1, CHAI Yunfeng1, JIN Lili1,2, LIU Xin1, LU Chengyin1,*   

  1. 1. Tea Research Institute, Chinese Academy of Agricultural Sciences, Tea Quality and Supervision Testing Center, Key Laboratory of Tea Quality and Safety Control, Ministry of Agriculture R. P. China, Hangzhou 310008, China;
    2. Graduate School of Chinese Academy of Agricultural Sciences, Beijing 100081, China
  • Received:2018-02-07 Revised:2018-03-07 Online:2018-08-15 Published:2019-10-15

摘要: 邻苯二甲酰亚胺(PI)和灭菌丹总量作为灭菌丹残留限量标准,造成茶叶中灭菌丹检测的假阳性误判,成为阻碍我国茶叶出口主要因素之一。本文优化了QuEChERS前处理条件,建立了气相色谱串联质谱法检测茶叶中PI残留的方法。样品经乙腈提取,多壁碳纳米管、十八烷基硅烷和苯磺基强阳离子交换剂组成的混合分散吸附剂净化。在10、20、50、100βμg∙kg-1添加水平下,回收率为73%~104%,相对标准偏差低于20%。方法定量限为10.0βμg∙kg-1。该方法简便、可靠、准确,灵敏度高,适用于茶叶中PI残留检测。

关键词: 茶, 邻苯二甲酰亚胺, QuEChERS, 气相色谱-串联质谱

Abstract: As folpet residues, phthalimide (PI) and folpet were responsible for a high risk of false positive detection of folpet in tea, which became a major factor restricting the export of Chinese tea. A modified QuEChERS method for the determination of PI residue in tea using gas chromatography-tandem mass was developed and validated. The target analyte was extracted using acetonitrile and the crude extracts were purified using multiwalled carbon nanotubes, octadecyl silica and strong cation exchanger. At the spiked levels of 10, 20, 50 and 100βμg∙kg-1, the average recoveries were from 73% to 104%, and the relative standard deviations were below 20%. The limit of quantification of PI in tea was 10.0βμg∙kg-1. The method was simple, reliable, accurate, sensitive and appropriate for the determination of PI residue in tea.

Key words: tea, phthalimide, QuEChERS, gas chromatography-tandem mass

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