色谱

色谱 ›› 2019, Vol. 37 ›› Issue (1): 8-14.DOI: 10.3724/SP.J.1123.2018.09007

• 特别策划：南京海关动植物与食品检测中心专栏 • 上一篇    下一篇

高效液相色谱-串联质谱法测定蜂蜜中9种农药残留

朱之烔1, 柳菡1, 宁倩倩1, 张健1, 沈伟健1, 陈惠兰1, 沈崇钰1, 谢文2   

  1. 1. 南京海关动植物与食品检测中心, 江苏 南京 210019;
    2. 杭州海关, 浙江 杭州 310016
  • 收稿日期:2018-09-04 出版日期:2019-01-08 发布日期:2014-11-29
  • 通讯作者: 柳菡E-mail:29186059@qq.com.
  • 基金资助:

    政府间国际科技创新合作重点专项（2017YFE0110800）.

Determination of nine pesticide residues in honey using high performance liquid chromatography-tandem mass spectrometry

ZHU Zhitong1, LIU Han1, NING Qianqian1, ZHANG Jian1, SHEN Weijian1, CHEN Huilan1, SHEN Chongyu1, XIE Wen2   

  1. 1. Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210019, China;
    2. Hangzhou Customs, Hangzhou 310016, China
  • Received:2018-09-04 Online:2019-01-08 Published:2014-11-29
  • Supported by:

    Key Projects of International Scientific and Technological Innovation Cooperation Between Governments(No. 2017YFE0110800).

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摘要：

建立了同时测定蜂蜜中9种苯并咪唑类和新烟碱类农药的全自动固相萃取-高效液相色谱-串联质谱检测方法。蜂蜜样品用磷酸盐缓冲液（pH=7.8）溶解，超声提取，经亲水亲脂平衡（hydrophilic-lipophilic balance，HLB）固相萃取小柱净化，氮吹浓缩，定容，过滤膜后进行高效液相色谱-串联质谱分析，采用多反应监测（MRM）模式测定，以内标法定量。结果表明，在0.002~0.05 mg/L范围内9种农药呈现出较好的线性关系（相关系数r2 ≥ 0.99），检出限和定量限分别为0.1~1.0 μg/kg和0.3~2.0 μg/kg。对阴性蜂蜜，在5.0、10.0、20.0 μg/kg 3个水平下分别进行加标回收试验，测出9种农药的平均回收率在78.2%~101.2%之间，相对标准偏差为1.3%~14.3%（n=6）。该方法可适用于大批量蜂蜜样品的快速准确测定。

关键词: 苯并咪唑类农药, 蜂蜜, 高效液相色谱-串联质谱法, 新烟碱类农药

Abstract:

A method is proposed for the simultaneous determination of nine benzimidazole and neonicotinoid pesticides present in honey by employing automatic solid-phase extraction with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A honey sample was dissolved in a phosphate buffer (pH=7.8) followed by ultrasonic extraction. The extracts were then purified through solid-phase extraction (SPE) with hydrophilic-lipophilic balance (HLB) cartridges. Finally, nitrogen was blown on the obtained mixture, and the mixture was subsequently filtered for conducting HPLC-MS/MS analysis. Nine compounds were detected under the multiple reaction monitoring (MRM) mode, and the corresponding quantification was performed by employing the method of internal standards. The nine detected pesticides demonstrated good linearity in the range of 0.002-0.05 mg/L, with the correlation coefficient values (r2) being higher than 0.99. The limits of detection (LODs) (S/N=3) and limits of quantification (LOQs) (S/N=10) were found to be in the ranges of 0.1-1.0 μg/kg and 0.3-2.0 μg/kg, respectively. Furthermore, the results indicated that the recoveries of the nine detected pesticides range from 78.2%-101.2% at three spiked levels of 5.0, 10.0, and 20.0 μg/kg with a relative standard deviation (RSD) range of 1.3%-14.3% (n=6). Hence, the proposed method is rapid and can be employed for accurate determination of pesticide residues in large quantities of honey samples.

Key words: benzimidazole pesticides, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), honey, neonicotinoid pesticides

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