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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

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

Teemu Gunnar, Kari Ariniemi, Pirjo Lillsunde

J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Apr 25;818(2):175-89.

PMID: 15734157

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.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP87020426	N,O-Bis(tert-butyldimethylsilyl)trifluoroacetamide		87020-42-6	Price

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