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Simultaneous screening analysis of multiple β-blockers in urine by gas chromatography–mass spectrometry in selected ion monitoring mode
A rapid screening procedure is described for the simultaneous determination of 13 β-blockers in urine at the range of 0.010–1.0 μg mL −1. The procedure involves N-ethoxycarbonyl (EOC) derivatization of β-blockers in urine sample, followed by extraction and further conversion to trimethylsilyl (TMS)...
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Published in: | Analytica chimica acta 2007-10, Vol.601 (2), p.230-233 |
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Main Authors: | , , |
Format: | Article |
Language: | English |
Subjects: | |
Citations: | Items that this one cites Items that cite this one |
Online Access: | Get full text |
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Summary: | A rapid screening procedure is described for the simultaneous determination of 13 β-blockers in urine at the range of 0.010–1.0
μg
mL
−1. The procedure involves
N-ethoxycarbonyl (EOC) derivatization of β-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 β-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
≥
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
μg
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%. |
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ISSN: | 0003-2670 1873-4324 |
DOI: | 10.1016/j.aca.2007.08.036 |