SPECIATION OF IONIC ALKYLLEAD COMPOUNDS IN HUMAN URINE BY GAS-CHROMATOGRAPHY MASS-SPECTROMETRY AFTER BUTYLATION THROUGH A GRIGNARD REACTION

One analytical procedure for the determination of ionic alkyllead in h uman urine has been studied. The system consists of the extraction of Me3Pb+, Et3Pb+ and Pb2+ at pH 9.0 with diethyldithiocarbamate to an or ganic phase. Then, the ionic compounds are butylated with BuMgCl and t he final organic solution is analyzed by GC-MS-SIM. The elimination of both foam and gels in the extraction step and the general procedure f or the urine are discussed. The recovery of compounds ranges from 105. 1% for Me3Pb+ to 97.2% for Et3Pb+ using hexane as extracting agent and detection limits are 18.4 pg/ml of Me3Pb+ and 19.2 pg/ml of Et3Pb+ in urine. The speciation of ionic alkylleads in the urine of a petrol st ation worker showed a value of 27.9 pg/ml of Me3Pb+ in urine and Et3Pb + was below the detection limit. (C) 1998 Elsevier Science B.V. All ri ghts reserved.