The power of hyphenated chromatography—Time of flight mass spectrometry for unequivocal identification of spirostanes in bodybuilding dietary supplements

Publication date: Available online 1 February 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Bharathi Avula, Amar G. Chittiboyina, Ji-Yeong Bae, Saqlain Haider, Yan-Hong Wang, Mei Wang, Jianping Zhao, Patricia A. Deuster, Ikhlas A. KhanAbstractA previously unidentified purported botanical ingredient was found in dietary supplements marketed for anabolic benefits. In an attempt to assess the ‘naturalness’ of a group of steroid-like compounds called laxogenins, a UHPLC-QToF method was developed. Several dietary supplements claim to contain 5α-hydroxy laxogenin, which is a derivative of a naturally occurring spirostane-type steroid, laxogenin. Although laxogenin has been isolated from the rhizomes of Smilax sieboldii, 5α-hydroxy laxogenin has not been isolated or reported from any natural source. These derivatives of laxogenins have untested anabolic properties. Due to the low UV absorbance of the spirostanes, a mass spectrometric method in positive ion mode was developed for unambiguous identification of laxogenin and closely related compounds. To show the utility of developed method, twelve dietary supplements labeled to contain 5α-hydroxy laxogenin or laxogenin as 5α-hydroxy laxogenin were analyzed as a proof-of-concept. Five supplements did not contain any 5α-hydroxy laxogenin, whereas in the remaining seven samples, spirostane-type contaminants were identified along with the labeled 5α-hydroxy laxogeni...
Source: Journal of Pharmaceutical and Biomedical Analysis - Category: Drugs & Pharmacology Source Type: research

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