Simultaneous determination of N-hydroxymethyl-N-methylformamide, N-methylformamide and N-acetyl-S-(N-methylcarbamoyl)cystein in urine samples from workers exposed to N,N-dimethylformamide by liquid chromatography-tandem mass spectrometry
- Authors
- Sohn, JH; Han, MJ; Lee, MY; Kang, SK; Yang, JS
- Issue Date
- Feb-2005
- Publisher
- ELSEVIER SCIENCE BV
- Keywords
- N,N-dimethylformamide; N-hydroxymethyl-N-methylformamide; N-methylformamide; N-acetyl-S-(N-methylcarbamoyl)cystein; LC-MS/MS
- Citation
- JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS, v.37, no.1, pp.165 - 170
- Journal Title
- JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
- Volume
- 37
- Number
- 1
- Start Page
- 165
- End Page
- 170
- URI
- https://scholarworks.bwise.kr/gachon/handle/2020.sw.gachon/79285
- DOI
- 10.1016/j.jpba.2004.10.001
- ISSN
- 0731-7085
- Abstract
- N-Hydroxymethyl-N-methylformamide (HMMF) and N-methylformamide (NMF) in urine samples from workers exposed to N,N-dimethylformamide (DMF) cannot be distinguished by a gas chromatographic method because HMMF is converted to NMF at the injection port of gas chromatography (GC). Total NMF (HMMF + NMF) has been measured instead. Also, the determination of N-acetyl-S(N-methylcarbamoyl)cystein (AMCC), which is supposed to be related to the toxicity of DMF, needs multiple treatments to convert to a volatile compound before GC analysis. There is no previous report of a simultaneous determination of three major metabolites of DMF in urine. The aim of this study is to develop a simple and selective method for the determination of DMF metabolite in urine. By using a liquid chromatography-tandem mass spectrometry, we can directly distinguish these three major metabolites of DMF in a single run. The diluted urine samples were analyzed on Capcell Pak MF SG80 column with the mobile phase of methanol in 2 mM formic acid (10:90, v/v). The analytes were detected by an electrospray ionization tandem mass spectrometry in the multiple-reaction-monitoring mode. The standard curves were linear (r>0.999) over the concentration ranges of 0.004-8 mug/mL. The precision and accuracy of quality control samples for inter-batch (n = 6) analyses were in the range of 1.3-9.8% and 94.7-116.8, respectively. The sum of each HMMF and NMF concentration determined by LC-MS/MS method shows high correlation (r = 0.9927 with the slope of 1.0415, p < 0.0001) with NMF included HMMF concentration determined by GC method for 13 urine samples taken from workers exposed to DMF. The excretion ratio of HMMF:NMF:AMCC is approximately 4: 1: 1 in molar concentration. (C) 2004 Elsevier B.V. All rights reserved.
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