| Abstract: | A novel and robust phenyl-functionalized MSU-1 (Ph-MSU) coated fiber for solid-phase microextraction (SPME) coupled to high performance liquid chromatography (HPLC) was developed for the preconcentration and the determination of 2,4,4′-trichlorobiphenyl (PCB 28), 2,4′,5-trichlorobiphenyl (PCB 31), 2,2′,5,5′-tetrachlorobiphenyl (PCB 52), 2,2′,4,5,5′-pentachlorobiphenyl (PCB 101), 2,3′,4,4′,5-pentachlorobiphenyl (PCB 118), 2,2′,3,4,4′,5′-hexachlorobiphenyl (PCB 138), 2,2′,4,4′,5,5′-hexachlorobiphenyl (PCB 153), and 2,2′,3,4,4′,5,5′-heptachlorobiphenyl (PCB 180) in environmental water samples. Experimental conditions affecting SPME were examined in detail. The Ph-MSU coating provided large porosity and short-range mesostructures necessary for high extraction capacity and rapid mass transfer of PCBs. The Ph-MSU coated fiber exhibited selectivity for PCB 28, PCB 31, PCB 118, and PCB 138 in a limited extraction time. Good linearity for all PCBs was obtained with correlation coefficients from 0.9987 to 0.9994. The recoveries were within 94.3% to 103% for the spiked water with 300 ng · L?1 per PCB. The relative standard deviations (RSDs) ranged from 3.10% to 6.23% and the limits of detection (LODs) were between 8.73 ng · L?1 and 13.8 ng · L?1. The proposed method was applied for the determination of PCBs in real river water and rainwater samples. The median recoveries ranged from 85.6% to 118% with RSDs between 4.23% and 8.78%. The experimental results demonstrated that the Ph-MSU fiber coating could be reused for over 250 times without loss of the extraction efficiency. These results clearly indicate that the Ph-MSU coated fiber was rapid, sensitive, and suitable for the preconcentration and determination of trace PCBs in environmental water samples. |
