色谱

色谱 ›› 2013, Vol. 31 ›› Issue (1): 71-78.DOI: 10.3724/SP.J.1123.2012.07033

• 技术与应用 • 上一篇    下一篇

超快速液相色谱-串联质谱法快速筛查蔬菜中176种农药的残留量

郑姝宁1, 李凌云1, 林桓1, 赵文1, 张延国1, 姚周麟2, 刘肃1*   

  1. 1. 中国农业科学院蔬菜花卉研究所, 农业部蔬菜品质监督检验测试中心, 北京 100081; 2. 浙江省柑橘研究所, 浙江 台州 318020
  • 收稿日期:2012-07-18 修回日期:2012-09-08 出版日期:2013-01-28 发布日期:2013-01-21
  • 通讯作者:
  • 基金资助:

    中央级公益性科研院所基本科研业务费专项(2012ZL023);农业部园艺作物生物学与种质创制重点实验室项目.

Rapid screening of 176 pesticide residues in vegetables by ultra fast liquid chromatography-tandem mass spectrometry

ZHENG Shuning1, LI Lingyun1, LIN Huan1, ZHAO Wen1, ZHANG Yanguo1, YAO Zhoulin2, LIU Su1*   

  1. 1. Institute of Vegetables and Flowers, Chinese Academy of Agricultural Sciences, Supervision and Testing Center for Vegetable Quality, Ministry of Agriculture, Beijing 100081, China; 2. Zhejiang Citrus Research Institute, Taizhou 318020, China
  • Received:2012-07-18 Revised:2012-09-08 Online:2013-01-28 Published:2013-01-21

PDF

441

被引次数

20

摘要： 采用超快速液相色谱-串联质谱(UFLC-MS/MS)技术建立了蔬菜中176种农药残留快速筛查的分析方法。蔬菜样品采用乙腈提取,盐析后无需净化。采用多反应监测-信息关联采集-增强子离子扫描(MRM-IDA-EPI)的复合扫描模式,利用基于EPI谱图和色谱峰峰面积的谱库检索技术,完成了蔬菜中176种农药残留的定性定量分析。所有农药在各自的线性范围内线性关系良好(r＞0.99),除了丁硫克百威和灭蝇胺在3个添加水平下的平均回收率分别为46.8%和53.1%,其余174种农药的平均回收率范围为72.4%～126.4%,相对标准偏差范围为1.0%～18.7%,方法的检出限和定量限范围分别为0.005～2.0 μg/kg和0.1～10 μg/kg。该方法具有快速、灵敏度高、准确度高等优点,适合于蔬菜样品中农药多残留的快速筛查分析。

关键词: 超快速液相色谱-串联质谱, 农药残留, 谱库检索, 筛查, 蔬菜

Abstract:  A multiresidue analytical method for rapid screening of 176 pesticide residues in vegetables was developed by using ultra fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS). The vegetable samples were extracted by acetonitrile. It is not necessary for the extract to make a further purification after salting out. Multiple reaction monitoring with information-dependent acquisition of enhanced product ion (MRM-IDA-EPI) was used for the analysis. Based on EPI spectra and chromatographic peak area, identification and quantification of the 176 pesticide residues in vegetables were carried out by using library search technique. All the pesticides had the good linearity within their respective linear ranges (r＞0.99). The average recoveries of the 174 pesticides except for carbosulfan and cyromazine were in the range of 72.4% to 126.4% with the relative standard deviations (RSDs) from 1.0% to 18.7%. The limits of detection and quantification of the method were 0.005-2.0 μg/kg and 0.1-10 μg/kg, respectively. The results demonstrated that the method has distinct advantages of rapid speed, high sensitivity and good accuracy. Therefore, this method is suitable for the rapid screening of pesticide residues in vegetables.

Key words: library search, pesticide residues, screening, vegetables, ultra fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS)