The authors describe a zinc-based metal-organic framework/polyethersulfone nanocomposite (TMU-4/PES) coating deposited on a stainless steel wire via a single-phase inversion method. The nanocomposite represents a novel fiber coating for headspace solid-phase microextraction of organophosphorous pesticides (OPPs) from environmental water and soil samples. The synergistic effects of the high surface area and unique porous structure of TMU-4 as well as the rich π electron stacking and mechanical attributes of the PES polymer result in a high affinity of the composite for OPPs. Following thermal desorption, the OPPS were quantified by gas chromatography with a nitrogen-phosphorus detector. The preparation of the coating is simple, and the coated fiber is highly stable and reusable in that it can be used in about 100 consecutive extractions/desorption cycles. A central composite design was used for assessing the effect of the experimental parameters on the extraction process. Under optimized conditions, the limits of detection are in the 5–8 ng mL−1 range for the OPPs diazinon, fenitrothion, malathion and chlorpyrifos. The average repeatability and fiber-to-fiber reproducibility are 6.5% and 8.7%, respectively. The method was applied to the trace determination of OPPs in (spiked) water and soil samples where it gave good recovery (88–108%) and satisfactory reproduc- ibility (5.9–10.1%).
