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茶叶科学 ›› 2019, Vol. 39 ›› Issue (5): 576-586.doi: 10.13305/j.cnki.jts.2019.05.009

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固相萃取-GC/LC-MS/MS测定茶叶中79种农药残留

曾艳1, 郎红1, 杨巧慧1, 2, 李霞雪1, 史朝婷1   

  1. 1. 雅安市农产品质量监测检验中心,四川 雅安 625000;
    2. 四川农业大学食品学院,四川 雅安 625000
  • 收稿日期:2019-03-01 修回日期:2019-04-24 出版日期:2019-10-15 发布日期:2019-10-15
  • 作者简介:曾艳,女,硕士研究生,高级农艺师,主要从事农产品及产地环境质量安全研究,Email: 276874503@qq.com
  • 基金资助:
    雅安市重点科技项目(2017yyjskf05)

Determination of 79 Pesticide Residues in Tea by Solid Phase Extraction with GC-MS/MS and LC-MS/MS

ZENG Yan1, LANG Hong1, YANG Qiaohui1, 2, LI Xiaxue1, SHI Chaoting1   

  1. 1. Ya'an Quality Inspection of Agricultural Products Monitoring Center, Ya'an 625000, China;
    2. College of Food Science, Sichuan Agricultural University, Ya'an 625000, China
  • Received:2019-03-01 Revised:2019-04-24 Online:2019-10-15 Published:2019-10-15

摘要: 建立了一套以一次固相萃取前处理方法,运用气相色谱-串联质谱(GC-MS/MS)和液相色谱-串联质谱(LC-MS/MS)两种检测技术,测定茶叶中79种农药残留的可靠、快速、高通量检测方法。该方法用20βmL乙腈一次均质提取,分取提取液10βmL,用乙腈+甲苯(3∶1)20βmL洗脱过Carbon/NH2小柱净化,用5βmL乙腈定容混匀,于GC-MS/MS和LC-MS/MS同时检测。结果表明,79种农药在0.01~0.40βmg·L-1范围内线性良好,相关系数(R2)在0.995以上;高、低、中3种水平加标回收率在67.3%~130.8%内;相对标准偏差(RSD)在15%内;98.7%的农药定量限(LOQ)≤0.01βmg·kg-1;使用多种类茶叶实际检测,结果均合格。因此,该方法能同时检测含有机磷、有机氯、拟除虫菊酯类、氨基甲酸酯类和有机杂环类5大类农药,更有利于大批量茶叶样品的多农残检测。

关键词: 茶叶, GC-MS/MS, LC-MS/MS, 农药残留

Abstract: In order to detect various pesticide residues in tea, a reliable, rapid and high throughput detection method was established: a solid phase extraction was developed for the determination of 79 pesticide residues in tea by gas chromatography-tandem mass spectrometry (GC-MS/MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). These samples were extracted by 20βmL acetonitrile. 10βmL extracts were cleaned by Carbon/NH2 column with 20βmL acetonitrile + toluene (3∶1) and then mixed with 5βmL acetonitrile, then these procdssed samples were detected by GC-MS/MS and LC-MS/MS, respectively. The results show that the concentrations of 79 pesticide residues had good linearity relationships in the range of 0.01-0.40βmg·L-1, with the correlation coefficients (R2) above 0.995, the recoveries of high, low and medium levels were ranged from 67.3%-130.8%, the relative standard deviations (RSDs) were less than 15%, the limits of quantification (LOQs) of 98.7 % pesticides were less than or equal to 0.01βmg·kg-1, multiple types of tea were detected, and the results were proved to be qualified. Consequently, the method can simultaneously detect 5 kinds of pesticides, including organophosphorus, organochlorine, pyrethroids, carbamates and organic heterocyclic pesticides, which would be useful to determine multi-pesticide residues in high numbers of tea samples.

Key words: tea, GC-MS/MS, LC-MS/MS, pesticide residues

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