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

- GC-MS/MS applied to the analysis of tributyltin and pentachlorophenol in seawater.
- MeOH/MeOTMS mixture allowed gas chromatographic separation of underivatized tributyltin and pentachlorophenol.
- Method performance in compliance with the strict EU requirements.

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−1 for TBT and 0.2 μg L−1 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−1 for TBT and 0.050 μg L−1 for PCP.

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