A new sulfobetaine polymer resin SPE method combined with HPLC-MS/MS for the determination of tetracycline (TC) antibiotics residues from honey samples is presented. The sulfobetaine resin was synthesized and was packed into a syringe-type tube, which served as the SPE cartridge for selective adsorption of TCs. TCs were quantitatively adsorbed on the sulfobetaine cartridge, when the loading solvent was 95% v/v acetonitrile solution, and TCs adsorbed were not eluted by aqueous acetonitrile washing solution. TFA aqueous solution was used for eluting the adsorbed TCs. The proposed SPE method has been applied to the determination of TCs in honey samples. The recoveries of TCs spiked in honey samples ranged from 70 to 80%. Reduction of the recoveries might be derived from low solubility of TCs in acetonitrile. Compared with other SPE resins, this resin was superior in terms of selectivity with simple pretreatment.
A simple HPLC method for the determination of adulteration in apple juice was developed. The method is based on the detection of D-malate, derived from racemic malic acid, which is added as an acidulant. A variable-wavelength optical rotation detector was used to determine the enantiomeric excess (ee). Using anion-exchange chromatography with a phosphate buffer eluent and UV (210 nm) detection, the limit of detection for L-malate was 2 microg. With an injection of 13.4 microg of malate, the standard deviation of the ee calibration curve was 2.5%. Several apple juice samples were analyzed according to the proposed procedure, and the results agreed with those obtained using enzymatic kits for food analysis.
A novel multi-functional adsorbent (RP-SAX adsorbent) bearing hydrophobic and anion exchange groups was synthesized for the simple and rapid determination of residual acephate (AP) in vegetables. Macroporous base resin was obtained by suspension copolymerization with glycidyl methacrylate, stearyl methacrylate and glycerin dimethacrylate, and then ethyldimethylamine was introduced at glycidyl groups on the base resin. The adsorbent was packed into a syringe-type tube and used for extraction of AP. AP in the vegetable extract was quantitatively entrapped on the adsorbent and was completely eluted with 3 mL of 30 mmol/L trisodium phosphate in 50 (v/v) methanol solution. The eluate was directly injected into an HPLC-UV detection system with a reverse-phased column. The recoveries of 5 mg/L AP spiked in vegetable extraction samples ranged from 77 to 100.
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