title: Concurrent supercritical fluid chromatographic analysis of terpene lactones and ginkgolic acids in Ginkgo biloba extracts and dietary supplements.
abstract: Supercritical fluid chromatography was used to resolve and determine ginkgolic acids (GAs) and terpene lactones concurrently in ginkgo plant materials and commercial dietary supplements. Analysis of GAs (C13:0, C15:0, C15:1, and C17:1) was carried out by ESI (-) mass detection. The ESI (-) spectra of GAs simply displayed only the [M-H](-) pseudo-molecular ions, and selected ion monitoring (SIM) for those ions was used for the quantification. Analysis of terpene lactones (ginkgolides A, B, C, J and bilobalide) was complicated by in-source collision-induced dissociation (IS-CID) in the ESI source. Thus, MS analysis could be influenced by the fragmentation pattern produced by the IS-CID. However, it was established that the fragmentation pattern, measured by ion survival yield (ISY), was independent of analyte concentration or matrix at a fixed cone voltage in the ESI source. Therefore, MS with SIM mode was applicable for the analysis of these analytes. The reported method provided consistent and sensitive analysis for the analytes of interest. The LOQs and LODs were determined to be below 100 and 40 ng/mL for GAs and 1 μg/mL and 400 ng/mL for terpene lactones, respectively. Intra- and inter-day precisions were found to be satisfactory with RSDs being below 5.2 %. Analyte recoveries ranged from 87 to 109 %. The developed method was successfully applied to the analysis of 11 ginkgo plant samples and 8 dietary supplements with an analysis time of less than 12 min.
authors.affiliation: National Center for Natural Products Research, School of Pharmacy, University of Mississippi, University, MS, 38677, USA.
authors.forename: Mei
authors.initials: M
authors.lastname: Wang
authors.affiliation: National Center for Natural Products Research, School of Pharmacy, University of Mississippi, University, MS, 38677, USA.
authors.forename: Emily J
authors.initials: EJ
authors.lastname: Carrell
authors.affiliation: National Center for Natural Products Research, School of Pharmacy, University of Mississippi, University, MS, 38677, USA.
authors.forename: Amar G
authors.initials: AG
authors.lastname: Chittiboyina
authors.affiliation: National Center for Natural Products Research, School of Pharmacy, University of Mississippi, University, MS, 38677, USA.
authors.forename: Bharathi
authors.initials: B
authors.lastname: Avula
authors.affiliation: National Center for Natural Products Research, School of Pharmacy, University of Mississippi, University, MS, 38677, USA.
authors.forename: Yan-Hong
authors.initials: YH
authors.lastname: Wang
authors.affiliation: National Center for Natural Products Research, School of Pharmacy, University of Mississippi, University, MS, 38677, USA.
authors.forename: Jianping
authors.initials: J
authors.lastname: Zhao
authors.affiliation: National Center for Natural Products Research, School of Pharmacy, University of Mississippi, University, MS, 38677, USA.
authors.forename: Jon F
authors.initials: JF
authors.lastname: Parcher
authors.affiliation: National Center for Natural Products Research, School of Pharmacy, University of Mississippi, University, MS, 38677, USA. ikhan@olemiss.edu.|Division of Pharmacognosy, Department of BioMolecular Science, School of Pharmacy, University of Mississippi, University, MS, 38677, USA. ikhan@olemiss.edu.|Department of Pharmacognosy, College of Pharmacy, King Saud University, Riyadh, 11451, Saudi Arabia. ikhan@olemiss.edu.
authors.forename: Ikhlas A
authors.initials: IA
authors.lastname: Khan
mesh_terms: D002849:Chromatography, Gas; D002853:Chromatography, Liquid; D025924:Chromatography, Supercritical Fluid / Q000379:methods*; D019587:Dietary Supplements / Q000032:analysis*; D020441:Ginkgo biloba / Q000737:chemistry*; D007783:Lactones / Q000032:analysis*; D010936:Plant Extracts / Q000737:chemistry*; D012459:Salicylates / Q000032:analysis*; D013729:Terpenes / Q000032:analysis*
chemical_list: D007783:Lactones; D010936:Plant Extracts; D012459:Salicylates; D013729:Terpenes; C112485:ginkgolic acid
keywords: Dietary supplements; Ginkgo biloba; Ginkgolic acids; In-source collision-induced dissociation (IS-CID); Supercritical fluid chromatography/photo diode array-mass spectrometry (SFC/PDA-MS); Terpene lactones