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Determination of n ‐hexane metabolites by liquid chromatography/mass spectrometry 1. 2,5‐Hexanedione and other phase I metabolites in untreated and hydrolyzed urine samples by atmospheric pressure chemical ionization
Author(s) -
Andreoli Roberta,
Manini Paola,
Mutti Antonio,
Bergamaschi Enrico,
Niessen Wilfried M. A.
Publication year - 1998
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/(sici)1097-0231(19981015)12:19<1410::aid-rcm339>3.0.co;2-m
Subject(s) - chemistry , chromatography , atmospheric pressure chemical ionization , mass spectrometry , hexane , chemical ionization , repeatability , urine , selected ion monitoring , liquid chromatography–mass spectrometry , metabolite , analytical chemistry (journal) , high performance liquid chromatography , gas chromatography–mass spectrometry , ionization , ion , organic chemistry , biochemistry
The capabilities of atmospheric pressure chemical ionization liquid chromatography/mass spectrometry (APCI‐LC/MS) were investigated for the analysis of urinary 2,5‐hexanedione (2,5‐HD) and for the identification and characterization of other n ‐hexane Phase I metabolites in hydrolized urine samples. Chromatography was performed under reversed phase conditions at 0.75 mL min −1 flow rate. The ionization of 2,5‐HD and other n ‐hexane metabolites was obtained in positive ion mode. After optimization of several interface parameters, the linearity, sensitivity and precision of the method were determined operating in the selected ion monitoring mode. Detection limits were 0.02 and 0.05 mg L −1 in water and urine respectively, with linear calibration curves in the 0.05–10 mg L −1 concentration range. Repeatability and both intra‐day and inter‐day precision were determined at two concentration levels (0.5 and 5.0 mg L −1 ), and relative standard deviations were in the 1.3%–5.3% range. The method was applied to the quantitative analysis of 2,5‐HD in urine samples from an external Quality Assurance Programme for Organic Solvent Metabolites. Moreover, the metabolites 5‐hydroxy‐2‐hexanone, 2,5‐hexanediol and 4,5‐dihydroxy‐2‐hexanone were identified and confirmed in hydrolyzed urine of rats exposed to n ‐hexane. © 1998 John Wiley & Sons, Ltd.