Enhancement of chemical derivatization of steroids by gas chromatography/mass spectrometry (GC/MS).
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.
Bowden
John A
JA
Department of Chemistry, University of Florida, PO Box 117200, Gainesville, FL 32611, United States.
Colosi
Dominic M
DM
Mora-Montero
Diana C
DC
Garrett
Timothy J
TJ
Yost
Richard A
RA
D000081:Acetamides; D005463:Fluoroacetates; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D008872:Microwaves; D015203:Reproducibility of Results; D012997:Solvents / Q000737:chemistry; D013010:Sonication; D013256:Steroids / Q000737:chemistry*; D013696:Temperature; D013997:Time Factors; D014269:Trifluoroacetic Acid / Q000737:chemistry; D014297:Trimethylsilyl Compounds / Q000737:chemistry
D000081:Acetamides; D005463:Fluoroacetates; D012997:Solvents; D013256:Steroids; D014297:Trimethylsilyl Compounds; C086665:N-methyl-N-(trimethylsilyl)trifluoroacetamide; D014269:Trifluoroacetic Acid