Tags

Type your tag names separated by a space and hit enter

Simultaneous screening analysis of multiple beta-blockers in urine by gas chromatography-mass spectrometry in selected ion monitoring mode.
Anal Chim Acta. 2007 Oct 10; 601(2):230-3.AC

Abstract

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%.

Links

Publisher Full Text

Authors+Show Affiliations

Paik MJ
Metabolomic Analysis Laboratory, Institute for Neuroregeneration and Stem Cell Research, School of Medicine, Ajou University, Wonchon-dong, Yeongtong-gu, Suwon 443-721, South Korea.
Lee J
No affiliation info available
Kim KR
No affiliation info available

MeSH

Adrenergic beta-AntagonistsGas Chromatography-Mass SpectrometryHumansReference StandardsReproducibility of ResultsSensitivity and Specificity

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't
Validation Study

Language

eng

PubMed ID

17920396

Citation

Paik, Man-Jeong, et al. "Simultaneous Screening Analysis of Multiple Beta-blockers in Urine By Gas Chromatography-mass Spectrometry in Selected Ion Monitoring Mode." Analytica Chimica Acta, vol. 601, no. 2, 2007, pp. 230-3.
Paik MJ, Lee J, Kim KR. Simultaneous screening analysis of multiple beta-blockers in urine by gas chromatography-mass spectrometry in selected ion monitoring mode. Anal Chim Acta. 2007;601(2):230-3.
Paik, M. J., Lee, J., & Kim, K. R. (2007). Simultaneous screening analysis of multiple beta-blockers in urine by gas chromatography-mass spectrometry in selected ion monitoring mode. Analytica Chimica Acta, 601(2), 230-3.
Paik MJ, Lee J, Kim KR. Simultaneous Screening Analysis of Multiple Beta-blockers in Urine By Gas Chromatography-mass Spectrometry in Selected Ion Monitoring Mode. Anal Chim Acta. 2007 Oct 10;601(2):230-3. PubMed PMID: 17920396.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous screening analysis of multiple beta-blockers in urine by gas chromatography-mass spectrometry in selected ion monitoring mode. AU - Paik,Man-Jeong, AU - Lee,Jinwoo, AU - Kim,Kyoung-Rae, Y1 - 2007/08/28/ PY - 2007/07/16/received PY - 2007/07/25/revised PY - 2007/08/22/accepted PY - 2007/10/9/pubmed PY - 2007/11/14/medline PY - 2007/10/9/entrez SP - 230 EP - 3 JF - Analytica chimica acta JO - Anal Chim Acta VL - 601 IS - 2 N2 - 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%. SN - 1873-4324 UR - https://www.unboundmedicine.com/medline/citation/17920396/Simultaneous_screening_analysis_of_multiple_beta_blockers_in_urine_by_gas_chromatography_mass_spectrometry_in_selected_ion_monitoring_mode_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0003-2670(07)01440-7 DB - PRIME DP - Unbound Medicine ER -