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Simultaneous Analysis of the di(2-ethylhexyl)phthalate Metabolites 2-ethylhexanoic Acid, 2-ethyl-3-hydroxyhexanoic Acid and 2-ethyl-3-oxohexanoic Acid in Urine by Gas Chromatography-Mass Spectrometry

Simultaneous Analysis of the di(2-ethylhexyl)phthalate Metabolites 2-ethylhexanoic Acid, 2-ethyl-3-hydroxyhexanoic Acid and 2-ethyl-3-oxohexanoic Acid in Urine by Gas Chromatography-Mass Spectrometry

H G Wahl, Q Hong, D Stübe, M E Maier, H U Häring, H M Liebich

J Chromatogr B Biomed Sci Appl. 2001 Jul 15;758(2):213-9.

PMID: 11486831

Abstract:

A gas chromatographic-mass spectrometric method was developed for the quantitative analysis of the three Di(2-ethylhexyl)phthalate (DEHP) metabolites, 2-ethylhexanoic acid, 2-ethyl-3-hydroxyhexanoic acid and 2-ethyl-3-oxohexanoic acid in urine. After oximation with O-(2,3,4,5,6-pentafluorobenzyl)-hydroxylamine hydrochloride and sample clean-up with Chromosorb P filled glass tubes, all three organic acids were converted to their tert.-butyldimethylsilyl derivatives. Quantitation was done with trans-cinnamic acid as internal standard and GC-MS analysis in the selected ion monitoring mode (SIM). Calibration curves for all three acids in the range from 20 to 1,000 microg/l showed correlation coefficients from 0.9972 to 0.9986. The relative standard deviation (RSD) values determined in the observed concentration range were between 1.3 and 8.9% for all three acids. Here we report for the first time the identification of 2-ethyl-3-hydroxyhexanoic acid and 2-ethyl-3-oxohexanoic acid in human urine next to the known DEHP metabolite 2-ethylhexanoic acid. In 28 urine samples from healthy persons we found all three acids with mean concentrations of 56.1 +/- 13.5 microg/l for 2-ethylhexanoic acid, 104.8 +/- 80.6 microg/l for 2-ethyl-3-hydroxyhexanoic acid and 482.2 +/- 389.5 microg/l for 2-ethyl-3-oxohexanoic acid.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP57981029	O-(2,3,4,5,6-Pentafluorobenzyl)hydroxylamine hydrochloride		57981-02-9	Price

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