title: Liquid chromatography/electrospray tandem mass spectrometry of terpenoid lactones in Ginkgo biloba.
abstract: Ginkgo biloba (ginkgo) is one of most frequently used botanical dietary supplements. The bioactive constituents include the terpenoid lactones consisting of bilobalide and the ginkgolides A, B, C and J. A new assay based on high-performance liquid chromatography/electrospray tandem mass spectrometry (LC/MS/MS) was developed for the measurement of the terpenoid lactones in ginkgo products such as leaf powder and extracts. Initially, the MS/MS fragmentation pathways of ginkgolides were investigated to identify abundant fragment ions that might be useful for the sensitive and selective detection of ginkgolides and bilobalide during LC/MS/MS. Then, sample preparation and clean-up procedures were streamlined to maximize throughput by taking advantage of the selectivity of LC/MS/MS detection. Analyte recoveries exceeded 90%, the intra-assay and inter-assay relative standard deviations were <5%, the relative error was <8% and the limits of detection and quantification were 3.6-120 and 11-350 fmol, depending on the analyte that was injected on to the LC column. Therefore, this LC/MS/MS assay facilitated the rapid quantitative analysis of ginkgolides A, B, C and J and bilobalide in ginkgo dietary supplements with excellent recovery, reproducibity, accuracy and sensitivity.
authors.affiliation: Department of Medicinal Chemistry and Pharmacognosy, UIC/NIH Center for Botanical Dietary Supplements Research, College of Pharmacy, University of Illinois at Chicago, 833 S. Wood Street, Chicago, Illinois 60612, USA.
authors.forename: Yongkai
authors.initials: Y
authors.lastname: Sun
authors.forename: Wenkui
authors.initials: W
authors.lastname: Li
authors.forename: John F
authors.initials: JF
authors.lastname: Fitzloff
authors.forename: Richard B
authors.initials: RB
authors.lastname: van Breemen
mesh_terms: D002853:Chromatography, Liquid; D019587:Dietary Supplements / Q000032:analysis*; D020441:Ginkgo biloba / Q000737:chemistry*; D007783:Lactones / Q000032:analysis* / Q000737:chemistry* / Q000302:isolation & purification; D010936:Plant Extracts / Q000032:analysis / Q000737:chemistry; D010946:Plants, Medicinal / Q000737:chemistry; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization; D013729:Terpenes / Q000032:analysis* / Q000737:chemistry* / Q000302:isolation & purification
chemical_list: D007783:Lactones; D010936:Plant Extracts; D013729:Terpenes