Development of a solid-phase extraction method for the determination of polychlorinated biphenyls in water

Polychlorinated biphenyls (PCBs) in water were extracted with a rebuilt extraction unit using 47 mm C18 solid-phase extraction (SPE) disks. Three types of disks (SPEC, ENVI and Empore) were investigated for the extraction of seven PCBs from 1 l reagent water spiked at two concentration levels (20 and 1000 ng/l). The Empore disks produced the best analyte recoveries (91–107% with R.S.D. of 1–8%) at the low concentration level and displayed no leaking tendency. Empore disks were therefore considered superior to ENVI and SPEC disks for the conditions outlined in this work. The obtained extracts were dried and purified in an additional clean-up step using custom-made columns containing Florisil and Na2SO4. For water containing large amounts of organic matter, a pre-filtration was included. Final analysis was carried out on a dual-column GC–electron-capture detection system with on-column injection. The optimised extraction method, including clean-up, was less time-consuming and used less hazardous organic solvents than conventional liquid–liquid extraction (LLE) methods. Recoveries were 92–102% with R.S.D. of 3–8%.