色谱

色谱 ›› 2012, Vol. 30 ›› Issue (12): 1246-1252.DOI: 10.3724/SP.J.1123.2012.07014

• 研究论文 • 上一篇    下一篇

高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速检测6种农产品中96种农药的残留量

吴斌, 丁涛*, 柳菡, 陈惠兰, 赵增运, 张睿, 沈崇钰   

  1. 江苏出入境检验检疫局动植物与食品检测中心, 江苏 南京 210001
  • 收稿日期:2012-07-09 修回日期:2012-09-23 出版日期:2012-12-28 发布日期:2012-12-19
  • 通讯作者: 丁涛,硕士,高级工程师,研究方向为食品安全. Tel: (025)52345187, E-mail: dingt@jsciq.gov.cn.
  • 基金资助:

    国家质检总局项目(2011IK218和201010073-04).

Fast screening ninety-six pesticides in six kinds of agricultural products by high performance liquid chromatography-quadrupole/electrostatic field orbit trap high-resolution mass spectrometry

WU Bin, DING Tao*, LIU Han, CHEN Huilan, ZHAO Zengyun, ZHANG Rui, SHEN Chongyu   

  1. Animal, Plant and Food Inspection Center of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • Received:2012-07-09 Revised:2012-09-23 Online:2012-12-28 Published:2012-12-19

PDF

514

被引次数

40

摘要： 利用高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛选辣椒、青花菜、脱水土豆、大豆、绿茶和大蒜中96种农药残留。样品经含0.1%醋酸的乙腈提取,分散固相萃取脱水、除色、净化后,以C18色谱柱为分析柱,甲醇和5 mmol/L醋酸铵水溶液作为流动相进行梯度洗脱分离。采用正、负离子切换同时测定96种农药残留,大大提高了检测通量。通过优化分辨率,在全扫描模式下提取目标化合物的精确质量数,有效地去除了基质干扰;采用自动触发采集二级质谱图进一步提高了定性的准确性。在1～200 μg/L范围内,96种农药的线性相关系数均大于0.99。通过实际样品的添加回收试验,回收率范围为58%～105%,相对标准偏差为8.8%～18.3%。该方法的检测低限可以达到5 μg/kg,可以作为蔬菜中多种农药残留高通量筛选和确认检测方法。

关键词: 高分辨质谱, 高效液相色谱, 静电场轨道阱, 农产品, 农药残留

Abstract: A high-throughput method for the determination of 96 pesticides in six kinds of agricultural products by liquid chromatography-quadrupole/electrostatic field orbit trap high-resolution mass spectrometry was developed. After extraction with 0.1% acetic acid in acetonitrile solution and concentration, dispersive solid-phase extraction was further utilized to reduce the matrix interference. The chromatographic analysis was performed on a C18 column with methanol and 5 mmol/L ammonium acetate solution as the mobile phases with a gradient elution program. The 96 pesticide residues were analyzed in switching positive and negative modes at the same time. With the optimized mass resolution, accurate mass-to-charge ratio extraction of the target pesticide compounds in full scan mode could eliminate matrix interference effectively. Two-stage threshold-triggered full mass scan mode was utilized to further improve the accuracy of qualitative analysis. The linear ranges of all the 96 pesticides were from 1 μg/L to 200 μg/L with correlation coefficients greater than 0.99. By detecting spiked samples, the detection limits were 5 μg/kg for all the residues and the recoveries were in the range of 58%~105% with the relative standard deviations (RSDs) between 8.8% and 18.3%.

Key words: agricultural products, electrostatic field orbit trap, high-resolution mass spectrometry, pesticide residues, high performance liquid chromatography (HPLC)