Supercritical fluid extraction of chlorpyrifos and 3,5,6-trichloro-2-pyridinol from garden compost

A method was developed for the simultaneous supercritical carbon dioxide extraction of chlorpyrifos and its primary degradate, 3,5,6-trichloro-2-pyridinol (TCP), from garden compost. In situ derivatization with N,O-bis(trimethylsilyl)trifluoracetamide was necessary for extraction of TCP. Recoveries for TCP and chlorpyrifos were quantitative for spiked compost samples. Sodium chloride was used as the packing material in extractions with in situ derivatization. Optimum results were obtained for air-dried samples containing 4-7% moisture. No sample cleanup was required prior to analysis by GC-flame ionization detection. The effects of compost moisture content and ageing were investigated for chlorpyrifos recovery. No significantly negative effect on recovery for up to 20% (w/w) moisture for chlorpyrifos was observed. Effects of ageing showed a decrease in extraction efficiency over time with 52% recovery after 10 days.