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Zhang L, Thevis M, Piper T, et al. Carbon isotope ratio analysis of steroids by high-temperature liquid chromatography-isotope ratio mass spectrometry. Anal Chem. 2014;86(5):2297-302doi: 10.1021/ac403353x.
Zhang, L., Thevis, M., Piper, T., Jochmann, M. A., Wolbert, J. B., Kujawinski, D. M., Wiese, S., Teutenberg, T., & Schmidt, T. C. (2014). Carbon isotope ratio analysis of steroids by high-temperature liquid chromatography-isotope ratio mass spectrometry. Analytical chemistry, 86(5), 2297-302. https://doi.org/10.1021/ac403353x
Zhang, Lijun, et al. "Carbon isotope ratio analysis of steroids by high-temperature liquid chromatography-isotope ratio mass spectrometry." Analytical chemistry vol. 86,5 (2014): 2297-302. doi: https://doi.org/10.1021/ac403353x
Zhang L, Thevis M, Piper T, Jochmann MA, Wolbert JB, Kujawinski DM, Wiese S, Teutenberg T, Schmidt TC. Carbon isotope ratio analysis of steroids by high-temperature liquid chromatography-isotope ratio mass spectrometry. Anal Chem. 2014 Mar 04;86(5):2297-302. doi: 10.1021/ac403353x. Epub 2014 Feb 12. PMID: 24491121.
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Anal Chem. 2014 Mar 04;86(5):2297-302. doi: 10.1021/ac403353x. Epub 2014 Feb 12.

Carbon isotope ratio analysis of steroids by high-temperature liquid chromatography-isotope ratio mass spectrometry.

Analytical chemistry

Lijun Zhang, Mario Thevis, Thomas Piper, Maik A Jochmann, J Benjamin Wolbert, Dorothea M Kujawinski, Steffen Wiese, Thorsten Teutenberg, Torsten C Schmidt

Affiliations

  1. Instrumental Analytical Chemistry, University Duisburg-Essen , Universitätsstr. 5, 45141 Essen, Germany.

PMID: 24491121 DOI: 10.1021/ac403353x

Abstract

Generally, compound-specific isotope analysis of steroids is carried out by gas chromatography combined with isotope ratio mass spectrometry. Thus, a derivatization of the steroids prior to the measurement is compulsory, and a correction of the isotopic data is often necessary. To overcome this limitation, we present a new approach of high-temperature liquid chromatography coupled with photodiode array detection and isotope ratio mass spectrometry (HT-LC/PDA/IRMS) for the carbon isotope ratio analysis of unconjugated steroids. A steroid mixture containing 19-norandrosterone, testosterone, epitestosterone, androsterone, and 5β-pregnane-3α,17α,20α-triol was fully separated on a C4 column under high-temperature elution with water as the sole eluent. The accuracy for isotope analysis (±0.5 ‰) was around 20 μg g(-1) for testosterone, epitestosterone (79 ng steroid absolute on column), and 30 μg g(-1) for 19-norandrosterone, androsterone, and 5β-pregnane-3α,17α,20α-triol (119 ng steroid absolute on column). The applicability of the method was tested by measuring a pharmaceutical gel containing testosterone. With this work, the scope of LC/IRMS applications has been extended to nonpolar compounds.

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