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Clinical Chemistry 42: 286-291, 1996;
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Clinical Chemistry, Vol 42, 286-291, Copyright © 1996 by American Association for Clinical Chemistry

Determination of blood lead by electron-capture negative chemical ionization gas chromatography-mass spectrometry

GS Baird, RL Fitzgerald, SK Aggarwal and DA Herold
Laboratory Service, VA Medical Center, San Diego CA 92161, USA.

An electron-capture negative chemical ionization (NCI) gas chromatography-mass spectrometry (GC-MS) method for determination of lead (Pb) in blood samples is described. Extraction of Pb from the sample does not involve hot digestion but is based on treatment at ambient temperature. The blood sample is supplemented with a known amount of internal standard (204Pb) for isotope dilution and is treated with concentrated nitric acid. After adjusting the pH to 7, the Pb is extracted into toluene as the pyrrolidine-dithiocarbamate chelate. Samples are then derivatized with 4- fluorophenylmagnesium bromide to form Pb(FC6H4)4. The use of NCI offers enhanced sensitivity (by 75-fold better than previously used electron ionization), gives good precision and accuracy, and has no observable memory effect. The isotope dilution GCoff methodology typically agreed within 2-3% of expected values for the College of American Pathologists blood Pb specimens and the National Institute of Standards and Technology Standard Reference Material 955a.




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Copyright © 1996 by the American Association for Clinical Chemistry.