Citation: ZHU Zhitong, LIU Han, NING Qianqian, ZHANG Jian, SHEN Weijian, CHEN Huilan, SHEN Chongyu, XIE Wen. Determination of nine pesticide residues in honey using high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2019, 37(1): 8-14. doi: 10.3724/SP.J.1123.2018.09007 shu

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

1.
Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210019, China;
2.
Hangzhou Customs, Hangzhou 310016, China

Received Date: 4 September 2018

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

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.
- high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS),
- benzimidazole pesticides,
- neonicotinoid pesticides,
- honey
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1.
沈阳化工大学材料科学与工程学院沈阳 110142