Extraction studies on butyl‐ and octyltins were conducted with three poly(vinyl chloride) (PVC) product types: clear food container, rigid pipe and flexible membrane. Three solvents, tetrahydrofuran, xylene and methylene chloride were evaluated for extraction efficiency. Methylene chloride extracted more than 97% of the total extractable organotin in two extractions and resulted in the highest recoveries of analytes from all three PVC products. Method detection limits ranged from 0.3 to 0.9μgalkyltin/g PVC. The mean precision of the method is 6.8% relative standard deviation. Food industry PVC product samples contained between <0.8 and 8751μg/g octyltins and <0.3 and 4.7 μg/g butyltins. Butyltins (<0.9–5985 μg/g) were detected in potable water pipe samples. Pipe used in industrial applications contained both butyl‐ (13–1501μg/g) and octyltins (701–3033 μg/g).