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  • Determination of 5-hydroxy-N-methylpyrrolidone and 2-hydroxy-N-methylsuccinimide in human urine.

Determination of 5-hydroxy-N-methylpyrrolidone and 2-hydroxy-N-methylsuccinimide in human urine.

Journal of chromatography. B, Biomedical sciences and applications (1997-07-04)
B A Jönsson, B Akesson
ABSTRACT

A method for simultaneous determination of 5-hydroxy-N-methylpyrrolidone and 2-hydroxy-N-methylsuccinimide in urine is described. These compounds are metabolites of N-methyl-2-pyrrolidone, a powerful and widely used organic solvent. 5-Hydroxy-N-methylpyrrolidone and 2-hydroxy-N-methylsuccinimide were purified from urine by adsorption to a C8 solid-phase extraction column and then elution by ethyl acetate-methanol (80:20). After evaporation, the samples were derivatised at 100 degrees C for 1 h by bis(trimethylsilyl)trifluoroacetamide. Ethyl acetate was then added and the samples were analysed by gas chromatography-mass spectrometry in the electron impact mode. The extraction recovery for 5-hydroxy-N-methylpyrrolidone was about 80% while that for 2-hydroxy-N-methylsuccinimide was about 30%. The intra-day precision for 5-hydroxy-N-methylpyrrolidone was 2-4% and the between-day precision 4-21% (4 and 60 microg/ml). The intra-day precision for 2-hydroxy-N-methylsuccinimide was 4-8% and the between-day precision 6-7% (2 and 20 microg/ml). The detection limit was 0.2 microg/ml urine for both compounds. The method is applicable for analysis of urine samples from workers exposed to N-methyl-2-pyrrolidone.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
1-Methyl-2-pyrrolidinone, ReagentPlus®, 99%
Sigma-Aldrich
1-Methyl-2-pyrrolidinone, anhydrous, 99.5%
Supelco
1-Methyl-2-pyrrolidinone, analytical standard
Sigma-Aldrich
1-Methyl-2-pyrrolidinone, ACS reagent, ≥99.0%
Sigma-Aldrich
1-Methyl-2-pyrrolidinone, biotech. grade, ≥99.7%
Sigma-Aldrich
1-Methyl-2-pyrrolidinone, suitable for HPLC, ≥99%