Zhang, Lijun, Thevis, Mario, Piper, Thomas ORCID: 0000-0002-7462-6693, Jochmann, Maik A., Wolbert, J. Benjamin, Kujawinski, Dorothea M., Wiese, Steffen, Teutenberg, Thorsten and Schmidt, Torsten C. (2014). Carbon Isotope Ratio Analysis of Steroids by High-Temperature Liquid Chromatography-Isotope Ratio Mass Spectrometry. Anal. Chem., 86 (5). S. 2297 - 2303. WASHINGTON: AMER CHEMICAL SOC. ISSN 1520-6882

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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 5 beta-pregnane-3 alpha,17 alpha,20 alpha-triol was fully separated on a C-4 column under high-temperature elution with water as the sole eluent. The accuracy for isotope analysis (+/- 0.5 parts per thousand) was around 20 mu g g(-1) for testosterone, epitestosterone (79 ng steroid absolute on column), and 30 mu g g(-1) for 19-norandrosterone, androsterone, and 5 beta-pregnane-3 alpha,17 alpha,20 alpha-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.

Item Type: Journal Article
Creators:
CreatorsEmailORCIDORCID Put Code
Zhang, LijunUNSPECIFIEDUNSPECIFIEDUNSPECIFIED
Thevis, MarioUNSPECIFIEDUNSPECIFIEDUNSPECIFIED
Piper, ThomasUNSPECIFIEDorcid.org/0000-0002-7462-6693UNSPECIFIED
Jochmann, Maik A.UNSPECIFIEDUNSPECIFIEDUNSPECIFIED
Wolbert, J. BenjaminUNSPECIFIEDUNSPECIFIEDUNSPECIFIED
Kujawinski, Dorothea M.UNSPECIFIEDUNSPECIFIEDUNSPECIFIED
Wiese, SteffenUNSPECIFIEDUNSPECIFIEDUNSPECIFIED
Teutenberg, ThorstenUNSPECIFIEDUNSPECIFIEDUNSPECIFIED
Schmidt, Torsten C.UNSPECIFIEDUNSPECIFIEDUNSPECIFIED
URN: urn:nbn:de:hbz:38-443552
DOI: 10.1021/ac403353x
Journal or Publication Title: Anal. Chem.
Volume: 86
Number: 5
Page Range: S. 2297 - 2303
Date: 2014
Publisher: AMER CHEMICAL SOC
Place of Publication: WASHINGTON
ISSN: 1520-6882
Language: English
Faculty: Unspecified
Divisions: Unspecified
Subjects: no entry
Uncontrolled Keywords:
KeywordsLanguage
DOPING CONTROL; WATER CHROMATOGRAPHY; STATIONARY PHASES; ORGANIC-COMPOUNDS; C-13/C-12 RATIOS; REVERSED-PHASE; TESTOSTERONE; CATTLE; DERIVATIZATION; INTERFACEMultiple languages
Chemistry, AnalyticalMultiple languages
URI: http://kups.ub.uni-koeln.de/id/eprint/44355

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