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Hydropyrolysis over a platinum catalyst as a preparative technique for the compound‐specific carbon isotope ratio measurement of C 27 steroids
Author(s) -
Meredith Will,
Gomes Rachel L.,
Cooper Mick,
Snape Colin E.,
Sephton Mark A.
Publication year - 2010
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.4314
Subject(s) - chemistry , catalysis , platinum , isotope , isotopes of carbon , carbon fibers , radiochemistry , organic chemistry , total organic carbon , nuclear physics , materials science , composite number , composite material , physics
Compound‐specific stable carbon isotope analysis by gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS) is an important method for the determination of the 13 C/ 12 C ratios of biomolecules such as steroids, for a wide range of applications. However, steroids in their natural form exhibit poor chromatographic resolution, while derivatisation adds carbon thereby corrupting the stable isotopic composition. Hydropyrolysis with a sulphided molybdenum catalyst has been shown to defunctionalise the steroids, while leaving their carbon skeleton intact, allowing for the accurate measurement of carbon isotope ratios. The presence of double bonds in unsaturated steroids such as cholesterol resulted in significant rearrangement of the products, but replacing the original catalyst system with one of platinum results in higher conversions and far greater selectivity. The improved chromatographic performance of the products should allow GC/C/IRMS to be applied to more structurally complex steroid hormones and their metabolites. Copyright © 2010 John Wiley & Sons, Ltd.