Chinese Journal of Chromatography

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

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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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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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