title: Chemical fingerprint analysis and quantitative determination of steroidal compounds from Dioscorea villosa, Dioscorea species and dietary supplements using UHPLC-ELSD.
abstract: Ultra high-performance liquid chromatography (UHPLC) with evaporative light scattering detection was used for the quantification of steroidal saponins and diosgenin from the rhizomes or tubers of various Dioscorea species and dietary supplements that were purported to contain Dioscorea. The analysis was performed on an Acquity UPLC™ system with an UPLC™ BEH Shield RP18 column using a gradient elution with water and acetonitrile. Owing to their low UV absorption, the steroidal saponins were observed by evaporative light scattering detection. The 12 compounds could be separated within 15 min using the developed UHPLC method with detection limits of 5-12 µg/mL with 2 μL injection volume. The analytical method was validated for linearity, repeatability, accuracy, limits of detection and limits of quantification. The relative standard deviations for intra- and inter-day experiments were <3.1%, and the recovery efficiency was 97-101%. The total content of standard compounds was found to be in the ranges 0.01-14.5% and 0.9-28.6 mg daily intake for dry plant materials and solid commercial preparations, respectively. UHPLC-mass spectrometry with a quadrupole mass analyzer and ESI source was used only for confirmation of the identity of the various saponins. The developed method is simple, rapid and especially suitable for quality control analysis of commercial products.
authors.affiliation: National Center for Natural Products Research, Research Institute of Pharmaceutical Sciences, The University of Mississippi, University, MS, 38677, USA.
authors.forename: Bharathi
authors.initials: B
authors.lastname: Avula
authors.forename: Yan-Hong
authors.initials: YH
authors.lastname: Wang
authors.forename: Zulfiqar
authors.initials: Z
authors.lastname: Ali
authors.forename: Troy J
authors.initials: TJ
authors.lastname: Smillie
authors.forename: Ikhlas A
authors.initials: IA
authors.lastname: Khan
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D019587:Dietary Supplements / Q000032:analysis*; D027742:Dioscorea / Q000737:chemistry*; D004144:Diosgenin / Q000032:analysis* / Q000737:chemistry; D057230:Limit of Detection; D016014:Linear Models; D010936:Plant Extracts / Q000737:chemistry*; D015203:Reproducibility of Results; D012503:Saponins / Q000032:analysis* / Q000737:chemistry
chemical_list: D010936:Plant Extracts; D012503:Saponins; D004144:Diosgenin
keywords: Dioscorea spp; Dioscorea villosa L; UHPLC-ELSD; diosgenin; steroidal saponins
references.citation: J Mass Spectrom. 2006 Jan;41(1):1-22
references.pmid: 16402411
references.citation: Food Chem. 2008 Jun 1;108(3):1068-74
references.pmid: 26065772
references.citation: Magn Reson Chem. 2007 Nov;45(11):1001-5
references.pmid: 17887511
references.citation: J Pharm Biomed Anal. 2010 Nov 2;53(3):462-74
references.pmid: 20561762
references.citation: Carbohydr Res. 2013 Apr 5;370:86-91
references.pmid: 23454141
references.citation: Planta Med. 1997 Jun;63(3):258-62
references.pmid: 9225609
references.citation: Nat Prod Commun. 2013 Mar;8(3):323-6
references.pmid: 23678801
references.citation: J Asian Nat Prod Res. 2002 Sep;4(3):211-5
references.pmid: 12118511
references.citation: Steroids. 2004 Feb;69(2):111-9
references.pmid: 15013689
references.citation: Yao Xue Xue Bao. 2001 Jan;36(1):42-5
references.pmid: 12579859
references.citation: Am Fam Physician. 2006 Feb 1;73(3):457-64
references.pmid: 16477892
references.citation: Altern Ther Health Med. 1996 Mar;2(2):34-9
references.pmid: 8795885
references.citation: Chem Pharm Bull (Tokyo). 2007 Feb;55(2):308-16
references.pmid: 17268107
references.citation: Phytochem Anal. 2012 Sep-Oct;23(5):462-8
references.pmid: 22407490
references.citation: J Agric Food Chem. 2010 Aug 11;58(15):8806-13
references.pmid: 20681669
references.citation: Planta Med. 1996 Dec;62(6):573-5
references.pmid: 9000889
references.citation: Anal Chim Acta. 2007 Jan 16;582(1):61-8
references.pmid: 17386475