Determination of hexahydrophthalic and methylhexahydrophthalic acids in urine by gas chromatography-negative-ion chemical-ionisation mass spectrometry.
A method for determining hexahydrophthalic (HHP acid) and methylhexahydrophthalic acids (MHHP acid) from human urine was developed.
These acids are metabolites of the highly sensitising hexahydrophthalic anhydride and methylhexahydrophthalic anhydride.
The acids were purified from urine by liquid-solid extraction and derivatised with pentafluorobenzyl bromide to the corresponding esters.
These were analysed by GC-MS in the negative-ion chemical-ionisation mode with ammonia moderating gas.
Deuterium labelled HHP acid and MHHP acid were internal standards.
The precision for HHP acid was 3-6% in the range 70-620 ng mL-1 and that for MHHP acid was 2-8% in the range 60-680 ng mL-1.
Overall recovery of HHP acid from urine was 74-88% and that for MHHP acid 98-101%. Detection limits were 11 ng HHP acid mL-1 urine and 17 ng MHHP acid mL-1 urine.
There were no significant differences between determinations of HHP acid by a previous method and the present method.
Some instability of the acids in urine were found after extended storage at - 20 °C. The method was applicable for determination of HHP acid and MHHP acid from exposed workers.
Mots-clés Pascal : Anhydride organique, Durcisseur, Analyse quantitative, Surveillance biologique, Urine, Exposition professionnelle, Homme, Liquide biologique, Chromatographie phase gazeuse, Ion négatif, Ionisation chimique, Spectrométrie masse, Médecine travail, Isobenzofurane-1,3-dione(perhydro), Isobenzofurane-1,3-dione(méthyl perhydro)
Mots-clés Pascal anglais : Organic anhydride, Hardener, Quantitative analysis, Biological monitoring, Urine, Occupational exposure, Human, Biological fluid, Gas chromatography, Negative ion, Chemical ionization, Mass spectrometry, Occupational medicine
Notice produite par :
Inist-CNRS - Institut de l'Information Scientifique et Technique
Cote : 96-0328886
Code Inist : 002B03L06. Création : 10/04/1997.