Evaluation of extraction conditions and use of HPLC-MS for the simultaneous determination of acrylamide and its primary metabolite, n-acetyl-S-(2-carbamoylethyl)cysteine, in human urine.
B'Hymer C; Cheever KL
J Liq Chromatogr Relat Technol 2007 May; 30(9-10):1303-1316
Extraction conditions were evaluated for the simultaneous determination of acrylamide and its primary metabolite, N-Acetyl-S-(2-carbamoylethyl)cysteine (NACEC), in human urine. Acrylamide is an animal carcinogen and a human neurotoxicant; and it is widely used within industry. The toxicity of acrylamide makes it a health concern, and the use of its metabolite, NACEC, as a biomarker of exposure would be of value in the prevention of occupational diseases. Sample preparation studies evaluating several different types of solid-phase extraction (SPE) cartridges and different buffered or acidic matrices of standing urine samples were conducted. Measurement of acrylamide and NACEC was by reversed-phase high performance liquid chromatography (HPLC) with a mobile phase gradient. Detection for quantification was by single ion monitoring using electrospray mass spectrometry (MS). A basic method validation, using the final optimized SPE conditions, was conducted. Recovery studies of fortified urine samples at various concentration levels demonstrated good accuracy and precision; recovery varied between 97 and 108% for acrylamide and with relative standard deviations (RSD) of 7.6% or less. Recovery for the NACEC metabolite varied between 97 and 102% with RSD of 10% or less. The limit of detection (LOD) for the optimized procedure was found to range from 0.02 to 0.03 mg/mL for acrylamide and 0.1 to 0.2 mg/mL for NACEC in urine, using two chromatographic columns of different production lots.
Acrylamides; Urinalysis; Analytical-chemistry; Analytical-processes; Analytical-methods; Biomarkers
C. B'Hymer, U.S. Department of Health and Human Services, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, Taft Laboratory, 4676 Columbia Parkway, Cincinnati, Ohio 45226, USA
Healthcare and Social Assistance; Services
Journal of Liquid Chromatography & Related Technologies