Determination of dichlorobenzidine-hemoglobin adducts by GC/MS-NCI.
European Meeting on Mass Spectrometry in Occupational Health. Erlangen (DEU), 1995/06/21.
A method based on gas chromatography mass spectrometry-negative ion chemical ionization detection (GC/MS-NCl) was developed for the determination of 3,3'-dichlorobenzidine (DCB) - hemoglobin adducts.
Adducts were released from hemoglobin by mild alkaline hydrolysis and determined by GC/MS-NCl after extraction and derivatization with heptafluorobutyric anhydride (HFBA). 2,2'-DCB was used as internal standard and the recovery of the diarylamine derivatives in the overall procedure was 65-88%. The limit of detection attained was below 0.1 ng/g hemoglobin for DCB as well as for the metabolite N-acetyl-3,3'-dichlorobenzidine (acDCB).
The method was shown to be linear up to 150 ng/g hemoglobin.
In the NCl mass spectra of the HFB derivatives the dominant ion is (M-HF) - Due to the presence of two chlorines in the diarylamines, the characteristic ratio of 1.5 for m/z 624 to 626 (for diHFB-DCB and diHFB-2,2'-DCB) and m/z 470 to 472 (for HFB-acDCB) can be observed and used for identification.
The method was applied to the determination of DCB-hemoglobin adducts formed in young female Wistar rats after treatment for 4 weeks with 0.006%, 0.0012% or 0.00024% DCB via the drinking water.
Two adducts were detectable by GC/MS-NCl after alkaline hydrolysis of hemoglobin samples, extraction and derivatization. (...)
Mots-clés Pascal : Exposition professionnelle, Médecine travail, Homme, Surveillance biologique, Marqueur biologique, Adduit moléculaire, Hémoglobine, Chromatographie phase gazeuse, Spectrométrie masse, Ion négatif, Ionisation chimique, Sang, Liquide biologique, Rat, Rodentia, Mammalia, Vertebrata, Animal, Benzidine(dichloro)
Mots-clés Pascal anglais : Occupational exposure, Occupational medicine, Human, Biological monitoring, Biological marker, Molecular adduct, Hemoglobin, Gas chromatography, Mass spectrometry, Negative ion, Chemical ionization, Blood, Biological fluid, Rat, Rodentia, Mammalia, Vertebrata, Animal
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Inist-CNRS - Institut de l'Information Scientifique et Technique
Cote : 97-0251934
Code Inist : 002B03L06. Création : 11/06/1997.