色谱

色谱

• 研究论文 • 上一篇    下一篇

基质固相分散-超高效液相色谱-串联质谱法检测蔬菜中残留的苯甲酰脲类和双酰肼类杀虫剂

韩笑1, 娄喜山2, 张莉3, 王国卿3, 马明1, 王明林1*   

  1. 1. 山东农业大学食品学院, 山东 泰安 271000; 2. 烟台杰科检测服务有限公司, 山东 莱阳 265231; 3. 山东省化工研究院, 山东 济南 250014
  • 收稿日期:2009-10-08 修回日期:2009-12-08 出版日期:2010-04-28 发布日期:1980-12-25
  • 通讯作者: 王明林

Determination of benzoylurea and bishydrazide pesticide residues in vegetables by ultra performance liquid chromatography-tandem mass spectrometry with matrix solid phase dispersion

HAN Xiao1, LOU Xishan2, ZHANG Li3, WANG Guoqing3, MA Ming1, WANG Minglin1*   

  1. 1. College of Food Science and Engineering, Shandong Agricultural University, Taian 271000, China; 2. Yantai Jieke Inspection Service Co., Ltd., Yantai 265231, China; 3. Shandong Institute of Chemical Industry, Jinan 250014, China
  • Received:2009-10-08 Revised:2009-12-08 Online:2010-04-28 Published:1980-12-25
  • Contact: WANG Minglin

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836

被引次数

80

摘要： 建立了基质固相分散技术结合超高效液相色谱-串联质谱(UPLC-MS/MS)测定蔬菜中苯甲酰脲类杀虫剂(除虫脲、灭幼脲、杀铃脲、氟苯脲、氟虫脲、氟啶脲、氟铃脲)和双酰肼类杀虫剂(甲氧虫酰肼、虫酰肼)的方法。蔬菜样品经中性氧化铝和石墨化炭黑研磨,乙酸乙酯淋洗,洗脱液浓缩定容后,经超高效液相色谱分离,分别在正、负离子多反应监测(MRM)模式下用电喷雾电离串联质谱测定,外标法定量。结果表明,9种杀虫剂在1～100 μg/L质量浓度范围内有良好的线性关系(R2≥0.99);在1、5、10、100 μg/kg 4个加标水平上的回收率为78.5%～112.8%;相对标准偏差为2.3%～10.2%,检出限为0.5～1.0 μg/kg。该方法操作简便快速,样品和溶剂用量少,检出限低,可满足蔬菜中苯甲酰脲类和双酰肼类杀虫剂同时检测的要求。

关键词: 苯甲酰脲类杀虫剂, 超高效液相色谱-串联质谱法, 基质固相分散, 蔬菜 , 双酰肼类杀虫剂

Abstract: A method for the determination of nine pesticides including benzoylureas (diflubenzuron, chlorobenzuron, triflumuron, teflubenzuron, flufenoxuron, chlorfluazuron, hexaflumuron) and bishydrazides (methoxyfenozide, tebufenozide) in vegetables was developed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with matrix solid phase dispersion. The sample was graphitized with neutral alumina as dispersant and carbon black as purifying, and eluted with ethyl acetate. The separation was achieved by UPLC, and then the identification and quantification were performed using MS/MS with multiple-reaction monitoring and electrospray ionization in positive or negative mode. The following results were obtained: The calibration curves showed good linearity in the ranges of 1~100 μg/L with R2≥0.99; The recoveries were 78.5%~112.8% at four spiked levels of 1, 5, 10, 100 μg/kg, and the relative standard deviations were 2.3%~10.2%; The limits of determination were 0.5~1.0 μg/kg. The method has the advantages of easy to operate, fast to perform, lower limits of quantification, consuming less sample and organic solvents. It can meet the demands of practical use for the rapid and simultaneous determination of benzoylureas and bishydrazides in vegetables.

Key words: benzoylurea pesticides, bishydrazides pesticides, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), vegetables , matrix solid-phase dispersion