Determination of hexahydrophthalic acid and methylhexahydrophthalic acid in plasma after derivatisation with pentafluorobenzyl bromide using gas chromatography and mass spectrometric detection.
A method for the simultaneous determination of hexahydrophthalic acid (HHP acid) and methylhexahydrophthalic acid (MHHP acid) in human plasma was developed. The procedure was a rapid, single step extractive derivatisation with pentafluorobenzyl bromide as the derivatisation agent. The formed pentafluorobenzyl esters were analysed by gas chromatography-mass spectrometry in negative ion chemical ionisation mode with ammonia as the moderating gas. Deuterium-labeled HHP acid and MHHP acid were used as internal standards. The detection limit was 0.4 ng/ml for HHP acid (m/z 153) and 0.3 ng/ml for MHHP acid (m/z 365). The within-day precision of the method was between 2 and 3% and the between-day precision was between 3 and 12%. The overall recovery was between 65 and 83%. A comparison between HHP acid determinations with a previous and this method showed that the methods gave similar results. The method was applicable for analysis of plasma from occupationally exposed workers.
Lindh
C H
CH
Department of Occupational and Environmental Medicine, University Hospital, Lund, Sweden.
Jönsson
B A
BA
D003509:Cyclohexanecarboxylic Acids / Q000097:blood*; D004853:Epoxy Resins / Q000378:metabolism; D005464:Fluorobenzenes; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D010795:Phthalic Acids / Q000097:blood*; D010796:Phthalic Anhydrides / Q000378:metabolism; D000644:Quaternary Ammonium Compounds; D005466:Fluorocarbons
D003509:Cyclohexanecarboxylic Acids; D004853:Epoxy Resins; D005464:Fluorobenzenes; D010795:Phthalic Acids; D010796:Phthalic Anhydrides; D000644:Quaternary Ammonium Compounds; C074866:hexahydrophthalic acid; C025063:pentafluorobenzyl bromide; D005466:Fluorocarbons; C051070:4-methylcyclohexyl-1,6-dicarboxylic acid anhydride; C005752:araldite; C106919:methylhexahydrophthalic acid; C009405:tetrabutylammonium