Determination of organotin compounds in biological samples using accelerated solvent extraction, sodium tetraethylborate ethylation, and multicapillary gas chromatography-flame photometric detection.
A method has been developed for species-selective analysis of organotin compounds in solid, biological samples. The procedure is based on accelerated solvent extraction (ASE) of analytes and includes extraction of the tin species with a methanol-water (90% methanol) solution of acetic acid/sodium acetate containing tropolone (0.03% w/ v), their ethylation with NaBEt(4), and separation and detection by GC-FPD. The analytical procedure was optimized with an unspiked sample of harbor porpoise ( Phocoena phocoena) liver. Effects of ASE operational variables (extraction temperature and pressure, solvent composition, number of static extraction steps) are discussed. Method detection limits (MDL) were in the range 6-10 ng(Sn) g(-1) dry weight and 7-17 ng(Sn) g(-1) dry weight for butyl- and phenyltin compounds, respectively. Recoveries were comparable with or better than those obtained by use of other procedures reported in the literature. The analytical procedure was validated by analysis of NIES No. 11 (fish tissue) certified reference material.
Wasik
Andrzej
A
Department of Analytical Chemistry, Chemical Faculty, Gdańsk University of Technology, 11/12 G. Narutowicza St, 80-952, Gdańsk, Poland. wasia@chem.pg.gda.pl
Ciesielski
Tomasz
T
D000478:Alkylation; D000818:Animals; D001881:Borates / Q000737:chemistry*; D005591:Chemical Fractionation / Q000379:methods*; D002849:Chromatography, Gas / Q000295:instrumentation / Q000379:methods; D005399:Fishes; D008099:Liver / Q000737:chemistry; D009947:Organotin Compounds / Q000032:analysis*; D010783:Photometry / Q000379:methods; D019576:Porpoises; D011312:Pressure; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012997:Solvents / Q000737:chemistry; D013045:Species Specificity; D013696:Temperature; D013997:Time Factors
D001881:Borates; D009947:Organotin Compounds; D012997:Solvents; C080440:sodium tetraethylborate