Cloud point extraction (CPE) coupled with QuEChERS for extraction and clean up of neonicotinoid pesticide residues in honey

An effective modified pre-concentration technique, namely Cloud Point Extraction (CPE) coupled with QuEChERS (quick, easy, cheap, effective, rugged, and safe)), was developed to extract and clean up four neonicotinoid pesticide residues (nitenpyram, imidacloprid, thiamethoxam, and thiacloprid) from honey samples. Two cloud point processes were performed, whereby Triton™ X-114 was used to extract neonicotinoid residues into the surfactant-rich phase and the analytes were then transferred into an alkaline solution by ultrasonication prior to clean-up via QuEChERS method. Numerous variables affecting extraction performance were investigated, including surfactant type and concentration, salt type and content, back-extraction agent type and concentration, solvent type, QuEChERS salt quantity, and incubation temperature and time. Ultra-high-performance liquid chromatography-tandem mass spectrometry triple-quadrupole (UHPLC-MS/MS) (QQQ) was used for analysis. The limits of detection (LODs) and quantification limits (LOQs) were 0.13 to 0.18 μg kg−1 and 0.2 to 2.3 μg kg−1 respectively. The overall recoveries of all target compounds were between 85.3% to 104.5%, and excellent repeatability was achieved with relative standard deviations (RSD) ranging from 2.0% to 11.5%. The proposed extraction approach successfully detected trace amounts of neonicotinoids in honey samples obtained from local markets.