Determination of 14 benzodiazepines and hydroxy metabolites, zaleplon and zolpidem as tert-butyldimethylsilyl derivatives compared with other common silylating reagents in whole blood by gas chromatography-mass spectrometry. Export

@article{citeulike:159084, abstract = {The most common commercially available silylating reagents, N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA), N,O-bis-(trimethylsilyl)trifluoroacetamide+1\% trimethylchlorosilane (BSTFA+1\% TMCS) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA) were evaluated to achieve optimal derivatization conditions for analyzing various benzodiazepines based on gas chromatography-electron impact ionization-mass spectrometry (GC-EI-MS). Sensitivity, repeatability, retention times and stability of the derivatives, as well as specificity of mass fragmentation, were studied in detail. Also other parameters affecting the derivatization chemistry of benzodiazepines are discussed. tert-Butyldimethylsilyl (TBDMS) derivatives proved to be more stable, reproducible and sensitive than corresponding trimethylsilyl (TMS) derivatives for the GC-EI-MS analysis of benzodiazepines. Based on the TBDMS derivatives, a rapid, reliable, sensitive and quantitative GC-MS method was developed for the determination of 14 benzodiazepines and two hydroxy metabolites, as well as two non-benzodiazepine hypnotic agents, zolpidem and zaleplon, using 50 microl of whole blood. The method was completely validated in terms of accuracy, intra- and interday precision, limit of detection (LOD), limit of quantitation (LOQ), linearity, selectivity and extraction efficiency; these were all within the required limits, except for the accuracy of nitrazepam at a medium concentration level.}, address = {National Public Health Institute, Drug Research Unit, Mannerheimintie 166, 00300 Helsinki, Finland. teemu.gunnar@ktl.fi}, author = {Gunnar, T. and Ariniemi, K. and Lillsunde, P.}, citeulike-article-id = {159084}, citeulike-linkout-0 = {http://dx.doi.org/10.1016/j.jchromb.2004.12.032}, citeulike-linkout-1 = {http://view.ncbi.nlm.nih.gov/pubmed/15734157}, citeulike-linkout-2 = {http://www.hubmed.org/display.cgi?uids=15734157}, day = {25}, doi = {10.1016/j.jchromb.2004.12.032}, issn = {1570-0232}, journal = {J Chromatogr B Analyt Technol Biomed Life Sci}, keywords = {benzodiazepines, chromatography, drugs, spectrometry}, month = {April}, number = {2}, pages = {175--189}, posted-at = {2005-04-12 13:20:29}, priority = {2}, title = {Determination of 14 benzodiazepines and hydroxy metabolites, zaleplon and zolpidem as tert-butyldimethylsilyl derivatives compared with other common silylating reagents in whole blood by gas chromatography-mass spectrometry.}, url = {http://dx.doi.org/10.1016/j.jchromb.2004.12.032}, volume = {818}, year = {2005} }

TY - JOUR ID - citeulike:159084 L3 - citeulike-article-id:159084 N2 - The most common commercially available silylating reagents, N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA), N,O-bis-(trimethylsilyl)trifluoroacetamide+1% trimethylchlorosilane (BSTFA+1% TMCS) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA) were evaluated to achieve optimal derivatization conditions for analyzing various benzodiazepines based on gas chromatography-electron impact ionization-mass spectrometry (GC-EI-MS). Sensitivity, repeatability, retention times and stability of the derivatives, as well as specificity of mass fragmentation, were studied in detail. Also other parameters affecting the derivatization chemistry of benzodiazepines are discussed. tert-Butyldimethylsilyl (TBDMS) derivatives proved to be more stable, reproducible and sensitive than corresponding trimethylsilyl (TMS) derivatives for the GC-EI-MS analysis of benzodiazepines. Based on the TBDMS derivatives, a rapid, reliable, sensitive and quantitative GC-MS method was developed for the determination of 14 benzodiazepines and two hydroxy metabolites, as well as two non-benzodiazepine hypnotic agents, zolpidem and zaleplon, using 50 microl of whole blood. The method was completely validated in terms of accuracy, intra- and interday precision, limit of detection (LOD), limit of quantitation (LOQ), linearity, selectivity and extraction efficiency; these were all within the required limits, except for the accuracy of nitrazepam at a medium concentration level. IS - 2 JF - J Chromatogr B Analyt Technol Biomed Life Sci SN - 1570-0232 AD - National Public Health Institute, Drug Research Unit, Mannerheimintie 166, 00300 Helsinki, Finland. teemu.gunnar@ktl.fi EP - 189 TI - Determination of 14 benzodiazepines and hydroxy metabolites, zaleplon and zolpidem as tert-butyldimethylsilyl derivatives compared with other common silylating reagents in whole blood by gas chromatography-mass spectrometry. VL - 818 SP - 175 KW - benzodiazepines KW - chromatography KW - drugs KW - spectrometry AU - Gunnar, T AU - Ariniemi, K AU - Lillsunde, P PY - 2005/04/25/ UR - http://dx.doi.org/10.1016/j.jchromb.2004.12.032 ER -