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Simultaneous screening analysis of multiple beta-blockers in urine by gas chromatography-mass spectrometry in selected ion monitoring mode.

Paik MJ, Lee J, Kim KR

Metabolomic Analysis Laboratory, Institute for Neuroregeneration and Stem Cell Research, School of Medicine, Ajou University, Wonchon-dong, Yeongtong-gu, Suwon 443-721, South Korea.

A rapid screening procedure is described for the simultaneous determination of 13 beta-blockers in urine at the range of 0.010-1.0 microg mL(-1). The procedure involves N-ethoxycarbonyl (EOC) derivatization of beta-blockers in urine sample, followed by extraction and further conversion to trimethylsilyl (TMS) derivatives for the analysis by gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode (GC-SIM-MS). The characteristic fragment ions at m/z 260 and m/z 144, and [M-15]+ ions permitted sensitive and selective detection of most of the beta-blockers in the presence of co-extracted urinary amino alcohols at much higher levels. The whole procedure of EOC/TMS derivatization with subsequent GC-SIM-MS analysis was linear (r > or = 0.9988). The LODs were varied from 0.03 to 2.7 ng mL(-1). The ranges of precision (%relative standard deviation) and accuracy (%relative error) of the overall procedure at two different added amounts (0.02 and 0.5 microg mL(-1)) in urine matrix varied from 1.3 to 9.4 and from -9.6 to 9.7, respectively. The recoveries were measured to be ranged from 90.4 to 109.7%.

Published 8 October 2007 in Anal Chim Acta, 601(2): 230-3.
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