色谱

色谱 ›› 2014, Vol. 32 ›› Issue (3): 268-277.DOI: 10.3724/SP.J.1123.2013.11046

• 研究论文 • 上一篇    下一篇

气相色谱-四极杆飞行时间质谱准确鉴定常见水果蔬菜中的农药残留

李晓颍1,2, 张红医1, 常巧英2, 范春林2, 庞国芳2, 曹喆3, 王雯雯3   

  1. 1. 河北大学化学与环境科学学院, 河北 保定 071002;
    2. 中国检验检疫科学研究院, 北京 100123;
    3. 安捷伦科技有限公司, 北京 100102
  • 收稿日期:2013-11-26 修回日期:2014-01-03 出版日期:2014-03-08 发布日期:2014-03-04
  • 通讯作者: 范春林
  • 基金资助:

    “十二五”国家科技支撑计划项目（2012BAD29B01）.

Identification of pesticide residues in common fruits and vegetables by gas chromatography-quadrupole time-of-flight mass spectrometry

LI Xiaoying1,2, ZHANG Hongyi1, CHANG Qiaoying2, FAN Chunlin2, PANG Guofang2, CAO Zhe3, WANG Wenwen3   

  1. 1. College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China;
    2. Chinese Academy of Inspection and Quarantine, Beijing 100123, China;
    3. Agilent Technologies, Beijing 100102, China
  • Received:2013-11-26 Revised:2014-01-03 Online:2014-03-08 Published:2014-03-04

PDF

313

被引次数

28

摘要：

建立了一种新型农药多残留检测方法。采用气相色谱-四极杆飞行时间质谱（GC-QTOF MS）结合Carbon NH2柱固相萃取净化可对不同类别的152种农药残留进行准确的鉴定。一级（MS1）精确质量数据库评价3~5个特征离子，以3个及以上特征离子检出且离子丰度比（Q/qi）合适作为一级质谱定性依据。对部分特征离子数不足及特征离子检出情况不符合条件的农药进行二级（MS2）确证，应用二级谱图库检索及镜像结果对比分析实现疑似农药确证。本文对梨、甘蓝、番茄3种代表性果蔬在5.0和10.0 μg/kg 2个添加水平的152种农药进行测定，回收率在70%~120%范围的比例分别为甘蓝91.45 %、94.08%，番茄88.20%、88.80%，梨86.84%、92.10%。本方法为常见果蔬中农药残留的准确判断提供了可靠依据，扩大了分析范围。

关键词: 常见蔬菜, 常见水果, 农药残留, 气相色谱-四极杆飞行时间质谱

Abstract:

A new screening method was developed for the determination of 152 pesticide multi-residues in different chemical species with a Carbon NH2 column using solid-phase extraction (SPE) coupled with gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF MS). In the first stage (MS1) accurate mass database, up to three-five ions of the pesticides were monitored. The presence of at least three ions and the accomplishment of the intensity ratio (Q/qi) within the established tolerances were used as the confirmation of intensity criteria. The pesticides which have less characteristic ions or the peaks of the characteristic ions detected were up the tolerance were determined in the second stage (MS2) and the spectral difference was evaluated using MS2 library for the identified. Cabbage, tomato, pear were selected as typical fruits and vegetables to spike and detected all the 152 pesticides at two concentration levels of 5.0 and 10.0 μg/kg. The recoveries in the range of 70%-120% at two concentration levels were 91.45% and 94.08% for cabbage, 88.20% and 88.80% for tomato, 86.84% and 92.10% for pear respectively. Using the established 152 pesticide MS2 library some suspected pesticides were identified, and at the same time the analysis scope was expanded.

Key words: common fruits, common vegetables, gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF MS), pesticide residues

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