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  • Enhancement of chemical derivatization of steroids by gas chromatography/mass spectrometry (GC/MS).

Enhancement of chemical derivatization of steroids by gas chromatography/mass spectrometry (GC/MS).

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2009-08-21)
John A Bowden, Dominic M Colosi, Diana C Mora-Montero, Timothy J Garrett, Richard A Yost
ABSTRACT

Steroid derivatization was investigated by varying the experimental parameters (reagent, reaction time, and reaction temperature) to determine the optimal conditions for individual steroids, and for larger subsets. Three methods of derivatization enhancement were also investigated: the use of sonication, the use of a microwave heating, and the addition of solvents to the reaction mixture. On a comprehensive level, derivatization using N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA) was most efficient, while the application of solvent addition and microwave heating, in several cases, provided a clear enhancement. In addition, generalized rules for steroid derivatization are described.

MATERIALS
Product Number
Brand
Product Description

Supelco
MSTFA Reagent, ampule of 10 × 1.2 mL, analytical standard, Cerilliant®
Supelco
N-Methyl-N-(trimethylsilyl)trifluoroacetamide with 1% trimethylchlorosilane, for GC derivatization, LiChropur
Supelco
N-Methyl-N-(trimethylsilyl)trifluoroacetamide, for GC derivatization, LiChropur, ≥98.5%
Supelco
N-Methyl-N-(trimethylsilyl)trifluoroacetamide, synthesis grade
Supelco
N-Methyl-N-(trimethylsilyl)trifluoroacetamide, BioReagent, for silylations, LiChropur