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Trace determination of organotin compounds in water, sediment and mussel samples by low‐pressure gas chromatography coupled to tandem mass spectrometry
Author(s) -
Vidal J. L. Martínez,
Vega A. Belmonte,
Arrebola F. J.,
GonzálezRodríguez M. J.,
Sánchez M. C. Morales,
Frenich A. Garrido
Publication year - 2003
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.1152
Subject(s) - chemistry , detection limit , chromatography , extraction (chemistry) , solid phase extraction , matrix (chemical analysis) , tributyltin , derivatization , mass spectrometry , gas chromatography , gas chromatography/tandem mass spectrometry , tandem mass spectrometry , environmental chemistry
A fast method for the determination of eight organotin compounds (OTs), monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), tetrabutyltin (TeBT), monophenyltin (MPhT), diphenyltin (DPhT), triphenyltin (TPhT) and tetraphenyltin (TePhT), in water, sediments and mussels, was developed using low‐pressure gas chromatography/tandem mass spectrometry (LPGC/MS/MS). The method is based on sodium diethyldithiocarbamate (DDTC) complexation of the ionic organotins, followed by extraction of the target matrices and derivatization by a Grignard reagent, as described in a previously published method for water samples (S. Tsunoi et al. , J. Chromatogr. A 2002; 962: 197). Solid‐phase extraction was selected as extraction method from water samples after comparison with liquid–liquid extraction, but extraction of the OTs from sediment and mussel samples was performed using toluene. Matrix‐matched calibration standards were used to minimize matrix effects. The analytical process was validated by the analysis of spiked blank samples. Performance characteristics such as linearity, detection limit (LOD), quantitation limit (LOQ), precision, and recovery were determined. Recoveries of OTs in spiked matrices ranged from 86–108% in water and from 78–110% in sediments and mussels, with precision values lower than 18%. Detection limits ranged from 0.1–9.6 ng L −1 in water, and 0.03–6.10 μg kg −1 in the other matrices. The present implementation of LPGC rather than conventional capillary GC permitted use of large‐volume injection and reduced analysis time by a factor of two. The proposed methodology was applied to the determination of OTs in real samples of water, marine sediments and mussels from the west coast of the Mediterranean Sea (Spain). Copyright © 2003 John Wiley & Sons, Ltd.