RESUMO
Headspace solid-phase microextraction (HS-SPME) and gas chromatography with flame photometric detection (GC-FPD) have been investigated for determination of butyltin and octyltin stabilizers in poly(vinyl chloride) (PVC) products. The organotin stabilizers were first released from the plastic matrix by dissolving the PVC sample in tetrahydrofuran (THF). The stabilizers were then hydrolyzed to the chloride forms, by treatment with 6 mol L(-1) HCl, then derivatized with sodium tetraethylborate (NaBEt4) in 0.2 mol L(-1) sodium acetate buffer (pH 4.5) at 50 degrees C. HS-SPME was performed with a fused-silica fiber coated with a 100-microm film of polydimethylsiloxane (PDMS). The collected organotin compounds were then desorbed in the GC injector at 280 degrees C and analyzed by GC-FPD. Linearity (r > or =0.994) over a concentration of approximately two orders of magnitude was usually obtained. Limits of quantitation (LOQ) of the four organotin compounds studied, viz., monobutyltin (MBT), dibutyltin (DBT), monooctyltin (MOT), and dioctyltin (DOT), were in the range 0.3-1.0 ng Sn mL(-1). Recovery was >90% for butyltins and >80% for octyltins. The method was validated by analyzing two reference standard PVC sheets with known organotin content. The applicability of the method to analysis of organotin stabilizers in commercial PVC products was also demonstrated.
