Preparation of enol-tert.∼Butyldimethylsilyl and mixed tert.∼Butyldimethylsilyl-trimethylsilyl ethers for gas chromatography-mass spectrometry of steroids and bile acids

Silyl Derivatization of Alkylphenols, Chlorophenols, and Bisphenol A for Simultaneous GC/MS Determination

“…So removal of unreacted excess derivatizing reagent is desired. It was reported that propanol can be used for the removal of unreacted excess silyl reagent in steroid and bile acid analysis . However, this technique cannot be applied to phenolic analytes because most phenolic silyl derivatives rapidly transform backward to phenolic compounds.…”

Silyl Derivatization of Alkylphenols, Chlorophenols, and Bisphenol A for Simultaneous GC/MS Determination

“…So removal of unreacted excess derivatizing reagent is desired. It was reported that propanol can be used for the removal of unreacted excess silyl reagent in steroid and bile acid analysis . However, this technique cannot be applied to phenolic analytes because most phenolic silyl derivatives rapidly transform backward to phenolic compounds.…”

Mass Spectrometric Fragmentation of Trimethylsilyl and Related Alkylsilyl Derivatives

“…The spectra of the 3-enol-TBDMS/TMS/methyl ester derivatives of cholic acids are characterized by a very abundant [M − 57] + ion with no other fragment above about 20% relative abundance (Andersson & Sjövall, 1984). Enolized hydroxy-3oxo-Δ 4 -steroids, however, give much more abundant fragment ions even though the molecular ion is usually the most abundant (Ballhorn et al, 1979;Steffenrud, 1996).…”

Silyl Derivatization of Alkylphenols, Chlorophenols, and Bisphenol A for Simultaneous GC/MS Determination

“…So removal of unreacted excess derivatizing reagent is desired. It was reported that propanol can be used for the removal of unreacted excess silyl reagent in steroid and bile acid analysis . However, this technique cannot be applied to phenolic analytes because most phenolic silyl derivatives rapidly transform backward to phenolic compounds.…”

Mass Spectrometric Fragmentation of Trimethylsilyl and Related Alkylsilyl Derivatives

“…The spectra of the 3-enol-TBDMS/TMS/methyl ester derivatives of cholic acids are characterized by a very abundant [M − 57] + ion with no other fragment above about 20% relative abundance (Andersson & Sjövall, 1984). Enolized hydroxy-3oxo-Δ 4 -steroids, however, give much more abundant fragment ions even though the molecular ion is usually the most abundant (Ballhorn et al, 1979;Steffenrud, 1996).…”

Silyl Derivatization of Alkylphenols, Chlorophenols, and Bisphenol A for Simultaneous GC/MS Determination

“…So removal of unreacted excess derivatizing reagent is desired. It was reported that propanol can be used for the removal of unreacted excess silyl reagent in steroid and bile acid analysis . However, this technique cannot be applied to phenolic analytes because most phenolic silyl derivatives rapidly transform backward to phenolic compounds.…”

Mass Spectrometric Fragmentation of Trimethylsilyl and Related Alkylsilyl Derivatives

“…The spectra of the 3-enol-TBDMS/TMS/methyl ester derivatives of cholic acids are characterized by a very abundant [M − 57] + ion with no other fragment above about 20% relative abundance (Andersson & Sjövall, 1984). Enolized hydroxy-3oxo-Δ 4 -steroids, however, give much more abundant fragment ions even though the molecular ion is usually the most abundant (Ballhorn et al, 1979;Steffenrud, 1996).…”