Innovative analytical method for the determination of underivatized tributyltin and pentachlorophenol in seawater by gas chromatography-triple quadrupole mass spectrometry.

Tributyltin (TBT) and pentachlorophenol (PCP) are listed as priority substances that warrant monitoring in the European Water Framework Directive (WFD 2000/60/CE), since TBT and PCP were identified as environmental endocrine disruptors and exhibit considerable toxicity toward both aquatic organisms and mammals even at very low levels. This paper shows a novel approach to analyze underivatized tributyltin (TBT) and pentachlorophenol (PCP) in seawater based on capillary gas chromatography-triple quadrupole mass spectrometry. The optimized extraction method for TBT an PCP in water involved liquid-liquid microextraction with toluene. The reduced extract was added with a solvent mix, composed of methanol and trimethylsilyl derivatives of methanol (MeOTMS), that allowed good chromatographic resolution of underivatized TBT and PCP, interacting as a lubricant along the glass liner during the injection phase. The proposed method showed good linearity and repeatability (RSD%<20% at 0.05 ng L for TBT and 0.2 μg L for PCP). The overall recoveries were 74% and 106% for TBT and PCP, respectively. Very low quantification limits that met the strict statutory and regulatory demands were achieved: 0.002 ng L for TBT and 0.050 μg L for PCP.