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 human urine has been studied. The system consists of the extraction of Me3Pb+, Et3Pb+ and Pb2+ at pH 9.0 with diethyldithiocarbamate to an organic phase. Then, the ionic compounds are butylated with BuMgCl and the final organic solution is analyzed by GC-MS-SIM. The elimination of both foam and gels in the extraction step and the general procedure for 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 station worker showed a value of 27.9 pg/ml of Me3Pb+ in urine and Et3Pb+ was below the detection limit.