Determination of load in blood and urine by SPME/GC

Lead is the most frequently quantitated toxic metal in biological matrixes. In this paper, a method is described for lead determination in whole blood and urine using solid-phase microextraction (SPME) gas chromatography, Lead ion is first derivatized with sodium tetraethylborate to form tetraethyllead, which is then extracted from the headspace over the sample by SPME. The analytical procedure was optimized for coating selection, pH, extraction time, and effect of salt. The relative standard deviation was less then 10% for both urine and blood samples. The limit of detection was 3 and 4 ppb; the limit of quantification is 5 and 10 ppb for urine and blood samples, respectively, Good linearity was found for both urine and blood samples when PDMS coating was used. The standard addition method was used for quantitation. Certified urine and blood samples were analyzed, and good accuracy was obtained.