色谱

色谱 ›› 2015, Vol. 33 ›› Issue (10): 1080-1089.DOI: 10.3724/SP.J.1123.2015.05015

• 技术与应用 • 上一篇    下一篇

QuEChERS-液相色谱-质谱法快速筛查和确证大米中205种农药残留

陈溪1,2, 程磊2, 曲世超2, 黄大亮2, 刘佳成2, 崔晗2, 贾彦波3, 纪明山1   

  1. 1. 沈阳农业大学植物保护学院, 辽宁 沈阳 110866;
    2. 大连出入境检验检疫局检验检疫技术中心, 辽宁 庄河 116400;
    3. 上海爱博才思分析仪器贸易有限公司, 北京 100015
  • 收稿日期:2015-05-13 出版日期:2015-10-08 发布日期:2012-05-09
  • 通讯作者: 纪明山
  • 基金资助:

    国家质检总局科研项目(2010IK134).

Rapid screening and confirmation of 205 pesticide residues in rice by QuEChERS and liquid chromatography-mass spectrometry

CHEN Xi1,2, CHENG Lei2, QU Shichao2, HUANG Daliang2, LIU Jiacheng2, CUI Han2, JIA Yanbo3, JI Mingshan1   

  1. 1. Plant Protection College, Shenyang Agricultural University, Shenyang 110866, China;
    2. Inspection and Quarantine Technical Center of Dalian Entry-Exit Inspection and Quarantine Bureau, Zhuanghe 116400, China;
    3. Shanghai AB SCIEX Analytical Instrument Trading Co., Ltd., Beijing 100015, China
  • Received:2015-05-13 Online:2015-10-08 Published:2012-05-09

PDF

204

被引次数

25

摘要：

结合QuEChERS法与液相色谱-三重四极杆复合线性离子阱质谱(LC-Q-TRAP/MS)技术,建立了大米中205种农药残留的快速筛查确证方法。大米样品经乙腈提取,N-丙基乙二胺(PSA)、无水MgSO4和C18吸附剂净化后,采用多反应监测-信息关联采集-增强子离子(MRM-IDA-EPI)扫描方式及谱库检索技术,通过对化合物的保留时间、离子对以及高灵敏度的EPI谱库检索比对,完成了205种农药的筛查与确证,并采用外标法定量,实现了大米样品中205种农药的定性和定量分析。结果表明,所有农药的线性相关系数均大于0.995;方法的定量限在0.5~10.0 μg/kg之间。在10、50 μg/kg两个添加水平下,205种农药的平均回收率在62.4%~127.1%之间;相对标准偏差(RSD)在1.0%~20.0%之间。该方法能够对大米样品进行实际检测,且检测时间不超过20 min。该方法快速、准确、灵敏度高,适合于大米中农药残留的快速、全面筛查和确证分析。

关键词: QuEChERS法, 大米, 农药残留, 确证, 筛查, 液相色谱-三重四极杆复合线性离子阱质谱

Abstract:

A method for rapid screening and confirmation of 205 pesticide residues in rice was developed by combining QuEChERS and high performance liquid chromatography-triple quadrupole-linear ion trap mass spectrometry (LC-Q-TRAP/MS). The rice samples were extracted with acetonitrile, and then cleaned up with primary secondary amine (PSA), anhydrous magnesium sulfate (MgSO4) and C18 adsorbent. Finally, the samples were detected by LC-Q-TRAP/MS in multiple reaction monitoring with information-dependent acquisition of enhanced product ion (MRM-IDA-EPI) mode followed with database searching. A total of 205 pesticide residues were confirmed by retention times, ion pairs and the database searching using EPI library, and quantified by external standard method. All the pesticides showed good linearities with linear correlation coefficients all above 0.995. The limits of quantification (LOQs) for the 205 pesticides were 0.5-10.0 μg/kg. The average recoveries of the 205 pesticides ranged from 62.4% to 127.1% with the relative standard deviations (RSDs) of 1.0%-20.0% at spiked levels of 10 μg/kg and 50 μg/kg, and only 20 min were needed for the analysis of an actual rice sample. In brief, the method is fast, accurate and highly sensitive, and is suitable for the screening and confirmation of pesticide residues in rice.

Key words: confirmation, liquid chromatography-triple quadrupole-linear ion trap mass spectrometry (LC-Q-TRAP/MS), pesticide residues, QuEChERS, rice, screen

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