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.
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 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.
Dipartimento di Clinica Medica, Università di Parma, Italy.
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Andreoli
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Manini
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Mutti
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Bergamaschi
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Niessen
D000390:Air Ionization; D000399:Air Pressure; D000818:Animals; D002851:Chromatography, High Pressure Liquid; D006586:Hexanes / Q000378:metabolism*; D006588:Hexanones / Q000652:urine*; D006801:Humans; D006868:Hydrolysis; D008297:Male; D013058:Mass Spectrometry; D051381:Rats; D017207:Rats, Sprague-Dawley; D015203:Reproducibility of Results; D012997:Solvents
D006586:Hexanes; D006588:Hexanones; D012997:Solvents; C026385:n-hexane; C011269:2,5-hexanedione