Citation: LIANG Xiu-Mei, WANG Xiang-Yun, XUE Xiao-Feng, QI Pei-Pei, LIU Zhen-Zhen, LIU Zhi-Wei, ZHOU Li, WANG Xin-Quan, WANG Qiang. Determination of Imidacloprid and Its Three Metabolites in Honey and Bee Pollen by Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(4): 553-559. doi: 10.11895/j.issn.0253-3820.160833 shu

Determination of Imidacloprid and Its Three Metabolites in Honey and Bee Pollen by Liquid Chromatography-Tandem Mass Spectrometry

1.
State Key Lab Breeding Base for Zhejiang Sustainable Plant Pest Control, Ministry of Agriculture, Key Lab for Pesticide Residue Detection, Institute of Quality and Standard for Agro-products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China;
2.
College of Plant Protection, Nanjing Agricultural University, Nanjing 210095, China;
3.
College of Science, China Agricultural University, Beijing 100094, China;
4.
Institute of Apiculture Research, Chinese Academy of Agricultural Sciences, Beijing 100093, China

Received Date: 15 November 2016
Revised Date: 6 February 2017

A method was developed for the determination of imidacloprid and its metabolites imidacloprid olefin, imidacloprid urea and 6-chloronicotinic acid in honey and bee pollen by liquid chromatography tandem mass spectrometry (LC-MS/MS). On the basis of typical QuEChERS method, the pH and times of extraction solvent, sorbents were optimized to ensure the extraction efficiency and the purification of extraction. Finally, the method was developed as follows: matrix was extracted with 5% formic acid-acetonitrile twice, and the extraction was cleaned with enhanced matrix removal-lipid (EMR), detected with LC-MS/MS and quantified with external matrix standards. The results indicated that the average spiked recoveries of imidacloprid, imidacloprid olefin, imidacloprid urea and 6-chloronicotinic acid in honey and pollen samples were 86.0%-111.5% with relative standard deviations (RSDs) of 1.7%-9.6%, the LODs were 0.20, 3.50, 0.40 and 14.00 μg/kg, and the LOQs were 0.60, 11.64, 1.20 and 45.00 μg/kg. The method was rapid and simple with high sensitivity and good reproducibility, and suitable for the determination of imidacloprid and its three metabolites residues in honey and bee pollen.
- Liquid chromatography tandem mass spectrometry,
- Honey,
- Hollen,
- Imidacloprid,
- Imidacloprid olefin,
- Imidacloprid urea,
- 6-Chloronicotinic acid,
- Enhanced matrix removal-Lipid
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沈阳化工大学材料科学与工程学院沈阳 110142