期刊
CHROMATOGRAPHIA
卷 64, 期 11-12, 页码 673-679出版社
VIEWEG
DOI: 10.1365/s10337-006-0095-4
关键词
gas chromatography-mass spectrometry; ethoxycarbonylation/trimethylsilylation; beta-blockers; tert-butyldimethylsilylation
Fourteen beta-blockers in pre-dried free base forms were simultaneously converted into tert-butyldimethylsilyl (TBDMS) derivatives in one-step. As a different approach, beta-blockers were directly transformed into N-ethoxycarbonyl (EOC) derivatives in aqueous solution, followed by extraction and trimethylsilyl (TMS) derivatization. The retention index sets measured by DB-5 and DB-17 dual-column GC were characteristic for each beta-blocker as TBDMS- and EOC/TMS derivatives. Their characteristic fragmentation patterns obtained by GC-MS facilitated easier peak identification of each beta-blocker. The overall EOC/TMS method for assays of 14 beta-blockers in aqueous solution was linear with acceptable precision and accuracy.
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