Determination of Fenpyroximate from Four Types of Honey by Liquid Chromatography/Tandem Mass Spectrometry

Abstract

Fenpyroximate is an acaricide used to control phytophagous mites in beekeeping farms, and is used to regulate residual amounts in honey in European Union countries. An effective and accurate sample preparation method was established for a liquid chromatograph‐mass spectrometer/mass spectrometer (LC–MS/MS) analysis of four types of honey (acacia honey, wild honey, manuka, and chestnut honey). Experiments were carried out to determine the optimal values of parameters such as sample pH, type of solid‐phase cartridge, type and volume of extraction solvent, loading sample volume, type and volume of eluent for effective sample extraction, purification, and concentration. Chromatographic separation was performed using a C18 (3.0 mm i.d. × 50 mm length, 2.7 μm particle size) column under isocratic conditions of water and acetonitrile (30:70). The optimized parameters for the extraction of fenpyroximate are as follows: sample pH, 7; type of sorbent solid phase, aminopropyl; volume of extraction solvent, 20 mL; volume of loading sample, 2 mL; eluent, dichloromethane/n‐hexane (65/35%, v/v); eluent volume, 6 mL. The limits of detection and quantitation for spiked honey samples were 1.56 and 5.00 μg/kg, respectively. Linear correlation coefficient (r) obtained from a concentration range 5.00–50.0 μg/kg was 0.9914–0.9977, while the accuracy and precision were 87.99–119.06% and 0.68–14.71% (RSD), respectively. Residue monitoring of fenpyroximate was also performed on 30 commercially available honeys using established methods.