Matrix solid phase dispersion (MSPD) has proven to be an efficient sample preparation method for solid, semi-solid, and viscous samples. Applications of MSPD have covered biological, food, and environmental samples, including both organic and inorganic analytes. This review presents an update on the development of MSPD in the period 2015~June 2018. In the first part of this review, we focus on the latest development in MSPD sorbent, including molecularly imprinted polymers, and carbon-based nanomaterials etc. The second part presents the miniaturization of MSPD, discussing the progress in both micro-MSPD and mini-MSPD. The on-line/in-line techniques for improving the automation and sample throughput are also discussed. The final part summarizes the success in the modification of original MSPD procedures.

Ascorbic acid (AA) is one of the essential nutrients in bee pollen, however, it is unstable and likely to be oxidized. Generally, the oxidation form (dehydroascorbic acid (DHA)) is considered to have equivalent biological activity as the reduction form. Thus, determination of the total content of AA and DHA would be more accurate for the nutritional analysis of bee pollen. Here we present a simple, sensitive, and reliable method for the determination of AA, total ascorbic acids (TAA), and DHA in rape (Brassica campestris), lotus (Nelumbo nucifera), and camellia (Camellia japonica) bee pollen, which is based on ultrasonic extraction in metaphosphoric acid solution, and analysis using hydrophilic interaction liquid chromatography (HILIC)-ultraviolet detection. Analytical performance of the method was evaluated and validated, then the proposed method was successfully applied in twenty-one bee pollen samples. Results indicated that contents of AA were in the range of 17.54 to 94.01 µg/g, 66.01 to 111.66 µg/g, and 90.04 to 313.02 µg/g for rape, lotus, and camellia bee pollen, respectively. In addition, percentages of DHA in TAA showed good intra-species consistency, with values of 13.7%, 16.5%, and 7.6% in rape, lotus, and camellia bee pollen, respectively. This is the first report on the discriminative determination between AA and DHA in bee pollen matrices. The proposed method would be valuable for the nutritional analysis of bee pollen.

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.

5-Hydroxymethylfurfural (HMF) is an important index for evaluating the quality of honey. In the present study, the recovery of HMF via the salting-out-assisted liquid–liquid extraction (SALLE) was systematically investigated to develop a simple, rapid, and effective method for the determination of HMF in honey. Results indicated that at the concentration of 70 : 30 (acetonitrile : H₂O, v/v), sodium carbonate showed the best recovery of HMF from honey with the 0.5 g addition amount of salt. Compared with two other homogenous liquid–liquid extraction methods, i.e. subzero temperature-assisted liquid–liquid extraction and hydrophobic solvent-assisted liquid–liquid extraction, SALLE showed an advantage of higher recovery for HMF. In addition, fructose and glucose were analyzed to investigate the residue of sugars in the extractive. Results demonstrated that the SALLE method could dramatically reduce the residual contents of these two sugars. In addition, SALLE showed the advantages of less consumption of samples and extraction solvents. Finally, the developed method was fully validated and applied for real honey samples. The analysis results obtained using the present method were comparable to those obtained using the official method; this indicated that the proposed method could be used as an alternative method for the routine quality control of HMF in honey.