Journal of Chromatography B 2004-04-05

Development of a gas chromatographic test for the quantification of the biomarker 3-bromopropionic acid in human urine.

C B'Hymer, K L Cheever

Index: J. Chromatogr. B. Analyt. Technol. Biomed. Life Sci. 802(2) , 361-6, (2004)

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Abstract

An accurate and precise method was developed for the detection and quantification of 3-bromopropionic acid (3-BPA), a metabolite and biomarker for exposure to 1-bromopropane (1-BP). 1-BP is used as an industrial solvent and exposure is a health concern for industrial workers due to its toxicity. It has been associated with neurological disorders in both animals and humans. Urine sample preparation for the determination of 3-BPA consisted of liquid-liquid extraction (LLE) with ethyl acetate and silylation with N-methyl-N-[tert-butyldimethylsilyl]trifluoroacetamide (MTBSTFA). Quantification was by means of a gas chromatograph (GC) equipped with a mass selective detector (MSD) using a dimethylpolysiloxane (HP-1) capillary column and 3-chloropropionic acid was used as an internal standard in the procedure. Demonstrated accuracy and precision during this method's validation was good; recovery varied between 93 and 98% with relative standard deviations (R.D.S.) of 5.7% or less. The limit of detection (LOD) for the procedure was approximately 0.01microg/ml 3-BPA in urine. These data and other factors of the development and validation of this test method will be discussed.