Stir-bar supported micro-solid-phase extraction for the determination of polychlorinated biphenyl congeners in serum...

In present work, a new configuration of micro-solid phase extraction was introduced and termed as stir-bar supported micro-solid-phase extraction (SB-μ-SPE). A tiny stir-bar was packed inside the porous polypropylene membrane along with sorbent material and the edges of membrane sheet were heat sealed to secure the contents. The packing of stir-bar inside the μ-SPE device does not allow the device to stick with the wall or any corner of the sample vial during extraction, which is, however, a frequent observation in routine μ-SPE. Moreover, it enhances effective surface area of the sorbent exposed to sample solution through continuous agitation (motion and rotation). It also completely immerses the SB-μ-SPE device in the sample solution even for non-polar sorbents. Polychlorinated biphenyls (PCBs) were selected as model compounds and the method performance was evaluated in human serum samples. After extraction, samples were analyzed by gas chromatography mass spectrometry (GC-MS). The factors that affect extraction efficiency of SB-μ-SPE were optimized. Under optimum conditions, a good linearity (0.1-100ngmL(-1)) with coefficients of determinations ranging from 0.9868 to 0.9992 was obtained. Limits of detections were ranged between 0.003 and 0.047ngmL(-1). Acceptable values for inter-day (3.2-9.1%) and intra-day (3.1-7.2%) relative standard deviations were obtained. The optimized method was successfully applied to determine the concentration of PCB congeners in human serum samples.