色谱

色谱 ›› 2013, Vol. 31 ›› Issue (9): 850-861.DOI: 10.3724/SP.J.1123.2013.01046

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时测定土壤中239种农药的残留量

朱永哲1, 冯雅男1, 金正汉2   

  1. 1. 青岛农业大学化学与药学院, 青岛 266109;
    2. 首尔大学农业与生命科学学院, 首尔 151742, 韩国
  • 收稿日期:2013-01-25 修回日期:2013-03-18 出版日期:2013-09-28 发布日期:2013-09-02
  • 通讯作者: 朱永哲
  • 基金资助:

    青岛市公共领域科技支撑计划项目(11-2-3-55-nsh);青岛农业大学高层次人才基金(630608).

Determination of 239 pesticide residues in soil by ultra performance liquid chromatography-tandem mass spectrometry

ZHU Yongzhe1, FENG Yanan1, KIM Jeonghan2   

  1. 1. College of Chemistry and Pharmacy, Qingdao Agricultural University, Qingdao 266109, China;
    2. Department of Agricultural Biotechnology, Seoul National University, Seoul 151742, Korea
  • Received:2013-01-25 Revised:2013-03-18 Online:2013-09-28 Published:2013-09-02

PDF

304

被引次数

23

摘要：

建立了超高效液相色谱-串联质谱法(UPLC-MS/MS),可于10 min内快速测定土壤中的239种农药残留。土壤样品经AOAC (Association of Official Analytical Chemists) QuEChERS方法处理,用乙腈萃取;无水硫酸镁、乙酸钠固液分离后,过0.2 μm滤膜;在UPLC-MS/MS正、负离子同步扫描多反应监测模式下进行分析。239种农药中,线性相关系数(r2)大于0.99的有236个,占总数的99%。在40 μg/kg添加水平下所有被检测农药的回收率均在50%~150%之间,且相对标准偏差(RSD)均小于20%;其中有209种农药的回收率达到70%~120%,有161种的RSD小于10%。方法的检出限(LOD)范围为0.69~29.04 μg/kg。土壤中多种农药残留的同时检测要求时间短、准确度和精密度高,本方法符合这些检测要求,适用于土壤中农药残留的检测。

关键词: QuEChERS, 超高效液相色谱-串联质谱法, 多残留, 农药, 土壤

Abstract:

A method for the determination of 239 pesticides in soil samples by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) is presented. The sample was prepared with AOAC (Association of Official Analytical Chemists) QuEChERS method for the extraction (acetonitrile, anhydrous MgSO4, CH3COONa). After filtered with a 0.2 μm membrane, the sample was separated and detected by UPLC-MS/MS performing on positive/negative electrospray ionization (ESI+/-) and the multiple reaction monitoring (MRM) mode. In this study, 236 of the 239 pesticides' correlation coefficients were above 0.99, which counted 99% of all the analytes. The limits of detection (LODs) ranged in 0.69-29.04 μg/kg (S/N=3). The recoveries of all the pesticides at 40 μg/kg spiked level were in the range of 50%-150%, and the relative standard deviations (RSDs) were below 20%. In addition, the recoveries of 209 pesticides were in the range of 70%-120%, and RSDs of 161 pesticides were less than 10%. The method is efficient, fast, simple, and accurate. The procedure is suitable for the determination of multi pesticide residues in soil.

Key words: multi-residues, pesticides, QuEChERS, soil, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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