MICROWAVE ACCELERATED SAMPLE PREPARATION FOR SPECIATION ANALYSIS OF ORGANOTIN COMPOUNDS IN BIOMATERIALS

One- and two-step protocols for microwave-assisted preparation of biom aterials in a low-power focused microwave field were developed for spe ciation analysis of organotin. The two-step procedure teas based on th e alkaline hydrolysis of the biomaterial using 25% tetramethylammonium hydroxide, followed by the adjustment to pH 5, ethylation of ionic or ganotin compounds with sodium tetraethylborate (NaBEt4) and extraction into iso-octane. The one-step procedure involved the simultaneous dis solution of biomaterial in acetic acid, ethylation with NaBEt4 and ext raction with nonane. Both procedures gave good agreement with the cert ified values for TBT in the NIES11 reference fish tissue. The content of TPhT determined in the NIES11 sample was close to the indicated val ue using the one- and two-step procedures. The procedure bused on the simultaneous sample dissolution-derivatization-extraction was found to be he fastest ever reported but suffers from the elevated consumption of NaBEt4.