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Merck
  • 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
摘要

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.

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Supelco
N-甲基-N-(三甲基硅烷基)三氟乙酰胺, synthesis grade
Supelco
N-甲基-N-(三甲基硅烷基)三氟乙酰胺, for GC derivatization, LiChropur, ≥98.5%
Supelco
N-甲基-N-(三甲基硅烷基)三氟乙酰胺, BioReagent, for silylations, LiChropur
Supelco
MSTFA 试剂, ampule of 10 × 1.2 mL, analytical standard, Cerilliant®
Supelco
含有1%三甲基氯硅烷的N-甲基-N-(三甲基甲硅烷基)三氟乙酰胺, for GC derivatization, LiChropur