In the present work, we developed a simple and rapid sample preparation method for the determination of neonicotinoid pesticides in honey based on the matrix-induced sugaring-out. Since there is a high concentration of sugars in the honey matrix, the honey samples were mixed directly with acetonitrile (ACN)-water mixture to trigger the phase separation. Analytes were extracted into the upper ACN phase without additional phase separation agents and injected into the HPLC system for the analysis. Parameters of this matrix-induced sugaring-out method were systematically investigated. The optimal protocol involves 2 g honey mixed with 4 mL ACN-water mixture (v/v, 60:40). In addition, this simple sample preparation method was compared with two other ACN-water-based homogenous liquid-liquid extraction methods, including salting-out assisted liquid-liquid extraction and subzero-temperature assisted liquid-liquid extraction. The present method was fully validated, the obtained limits of detection (LODs) and limits of quantification (LOQs) were from 21 to 27 and 70 to 90 μg/kg, respectively. Average recoveries at three spiked levels were in the range of 91.49% to 97.73%. Precision expressed as relative standard deviations (RSDs) in the inter-day and intra-day analysis were all lower than 5%. Finally, the developed method was applied for the analysis of eight honey samples, results showed that none of the target neonicotinoid residues were detected.
A simple, rapid, and effective sample preparation method was developed for the recovery of 5-hydroxymethylfurfural from honey samples with negligible co-extracted sugars.
In the present work, a novel sample preparation method, micro salting-out assisted matrix solid-phase dispersion (μ-SOA-MSPD), was developed for the determination of bisphenol A (BPA) and bisphenol B (BPB) contaminants in bee pollen. The proposed method was designed to combine two classical sample preparation methodologies, matrix solid-phase dispersion (MSPD) and homogenous liquid-liquid extraction (HLLE), to simplify and speed-up the preparation process. Parameters of μ-SOA-MSPD were systematically investigated, and results indicated the significant effect of salt and ACN-H2O extractant on the signal response of analytes. In addition, excellent clean-up ability in removing matrix components was observed when primary secondary amine (PSA) sorbent was introduced into the blending operation. The developed method was fully validated, and the limits of detection for BPA and BPB were 20 μg/kg and 30 μg/kg, respectively. Average recoveries and precisions were ranged from 83.03% to 94.64% and 1.76% to 5.45%, respectively. This is the first report on the analysis of bisphenol contaminants in bee pollen sample, and also on the combination of MSPD and HLLE. The present method might provide a new strategy for simple and fast sample preparation of solid and semi-solid samples.
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