A simple and highly selective molecularly imprinted solid-phase extraction (MISPE) combined with ultrasound-assisted dispersive liquid-liquid microextraction (DLLME) was developed for the determination of four Sudan dye (I, II, III, and IV) residues in sausage products. The novel molecularly imprinted microspheres (MIMs) synthesized by aqueous suspension polymerization using phenylamine-naphthol as the dummy template show high affinity to the four Sudan dyes and were applied as selective sorbents of MISPE-DLLME to overcome the drawbacks of template leakage in quantitative analysis. Good linearity was obtained in a range of 0.005-2.0 μg g(-1) and the average recoveries of the four Sudan dyes at three spiked levels ranged from 86.3 to 107.5%. The MISPE-DLLME-HPLC protocol significantly improved the purification and enrichment of the analytes and eliminated the template leakage of the conventional MISPE on quantitative analysis.
A simple and miniaturized pretreatment procedure combining matrix solid-phase dispersion (MSPD) with ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) technique was proposed in first time for simultaneous determination of three pyrethroids (fenpropathrin, cyhalothrin and fenvalerate) in soils. The solid samples were directly extracted using MSPD procedure, and the eluent of MSPD was used as the dispersive solvent of the followed DLLME procedure for further purification and enrichment of the analytes before GC-ECD analysis. Good linear relationships were obtained for all the analytes in a range of 5.0-500.0 ng/g with LOQs (S/N=10) ranged from 1.51 to 3.77 ng/g. Average recoveries at three spiked levels were in a range of 83.6-98.5% with RSD≤7.3%. The present method combined the advantages of MSPD and DLLME, and was successfully applied for the determination of three pyrethroids in soil samples.
A new magnetic dummy molecularly imprinted dispersive solid-phase extraction (MAG-MIM-dSPE) coupled with gas chromatography-FID was developed for selective determination of phthalates in plastic bottled beverages. The new magnetic dummy molecularly imprinted microspheres (MAG-MIM) using diisononyl phthalate as a template mimic were synthesized by coprecipitation coupled with aqueous suspension polymerization and were successfully applied as the adsorbents for MAG-MIM-dSPE to extract and isolate five phthalates from plastic bottled beverages. Validation experiments showed that the MAG-MIM-dSPE method had good linearity at 0.0040-0.40 μg/mL (0.9991-0.9998), good precision (3.1-6.9%), and high recovery (89.5-101.3%), and limits of detection were obtained in a range of 0.53-1.2 μg/L. The presented MAG-MIM-dSPE method combines the quick separation of magnetic particles, special selectivity of MIM, and high extraction efficiency of dSPE, which could potentially be applied to selective screening of phthalates in beverage products.
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