Quantitative determination of 5-hydroxy-N-methylpyrrolidone in urine for biological monitoring of N-methylpyrrolidone exposure.

Ligocka, D;Lison, Dominique;Haufroid, Vincent
(2002) Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences — Vol. 778, n° 1-2, p. 223-230 (2002)

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  • Ligocka, DUCLouvain
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  • Lison, Dominiqueorcid-logoUCLouvain
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Abstract
The aim of this work was to validate a sensitive method for quantitative analysis of 5-hydroxy-N-methylpyrrolidone (5-HNMP) in urine. This compound has been recommended as a marker for biological monitoring of N-methylpyrrolidone (NMP) exposure. Different solvents and alternative methods of extraction including liquid-liquid extraction (LLE) on Chem Elut and solid-phase extraction (SPE) on Oasis HLB columns were tested. The most efficient extraction of 5-HNMP in urine was LLE with Chem Elut columns and dichloromethane as a solvent (consistently 22% of recovery). The urinary extracts were derivatized by bis(trimethylsilyl)trifluoroacetamide and analysed by gas chromatography-mass spectrometry (GC-MS) with tetradeutered 5-HNMP as an internal standard. The detection limit of this method is 0.017 mg/l urine with an intraassay precision of 1.6-2.6%. The proposed method of extraction is simple and reproducible. Four different m/z signal ratios of TMS-5-HNMP and tetralabelled TMS-5-HNMP have been validated and could be indifferently used in case of unexpected impurities from urine matrix.
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Ligocka, D., Lison, D., & Haufroid, V. (2002). Quantitative determination of 5-hydroxy-N-methylpyrrolidone in urine for biological monitoring of N-methylpyrrolidone exposure. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 778(1-2), 223-230. https://doi.org/10.1016/S0378-4347(01)00441-8 (Original work published 2002)