Search

This study reports the development of magnetic solid-phase extraction combined with high-performance liquid chromatography for the determination of ten trace amounts of emerging contaminants (fluoroquinolone antibiotics, parabens, anticonvulsants and β-blockers) in water systems. Magnetic mesoporous carbon/β-cyclodextrin–chitosan (MMPC/Cyc-Chit) was used as an adsorbent in dispersive magnetic solid-phase extraction (DMSPE). The magnetic solid-phase extraction method was optimized using central composite design. Under the optimum conditions, the limits of detection (LODs) ranged from 0.1 to 0.7 ng L−1, 0.5 to 1.1 ng L−1 and 0.2 to 0.8 ng L−1 for anticonvulsants and β-blockers, fluoroquinolone and parabens, respectively. Relatively good dynamic linear ranges were obtained for all the investigated analytes. The repeatability (n = 7) and reproducibility (n = 5) were less than 5%, while the enrichment factors ranged between 90 and 150. The feasibility of the method in real samples was assessed by analysis of river water, tap water and wastewater samples. The recoveries for the investigated analytes in the real samples ranged from 93.5 to 98.8%, with %RSDs under 4%.

In this study, a simple, rapid and effective in-syringe micro-solid phase extraction (MSPE) method was developed for the separation and preconcetration of parabens (methyl, ethyl, propyl and butyl paraben) in environmental water samples. The parabens were determined and quantified using high performance liquid chromatography and a photo diode array detector (HPLC-PDA). Chitosan-coated activated carbon (CAC) was used as the sorbent in the in-syringe MSPE device. A response surface methodology based on central composite design was used for the optimization of factors (eluent solvent type, eluent volume, number of elution cycles, sample volume, sample pH) affecting the extraction efficiency of the preconcentration procedure. The adsorbent used displayed excellent absorption performance and the adsorption capacity ranged from 227–256 mg g−1. Under the optimal conditions the dynamic linear ranges for the parabens were between 0.04 and 380 µg L−1. The limits of detection and quantification ranged from 6–15 ng L−1 and 20–50 ng L−1, respectively. The intraday (repeatability) and interday (reproducibility) precisions expressed as relative standard deviations (%RSD) were below 5%. Furthermore, the in-syringe MSPE/HPLC procedure was validated using spiked wastewater and tap water samples and the recoveries ranged between from 96.7 to 107%. In conclusion, CAC based in-syringe MSPE method demonstrated great potential for preconcentration of parabens in complex environmental water.