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ARS Home » Southeast Area » Oxford, Mississippi » Natural Products Utilization Research » Research » Publications at this Location » Publication #326593

Research Project: Discovery and Development of Natural Products for Pharmaceutical and Agrochemical Applications II

Location: Natural Products Utilization Research

Title: Concurrent and supercritical fluid chromatographic analysis of Terpene Lactones and ginkolic acids in Ginko biloba

item WANG, MEI - University Of Mississippi
item CARRELL, EMILY - University Of Mississippi
item CHITTIBOYINA, AMAR - University Of Mississippi
item AVULA, BHARATHI - University Of Mississippi
item WANG, YAN-HONG - University Of Mississippi
item ZHAO, JIANPING - University Of Mississippi
item PARCHER, JON - University Of Mississippi
item KHAN, IKHLAS - University Of Mississippi

Submitted to: Analytical and Bioanalytical Chemistry
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 4/4/2016
Publication Date: 4/29/2016
Publication URL:
Citation: Wang, M., Carrell, E., Chittiboyina, A.G., Avula, B., Wang, Y., Zhao, J., Parcher, J.F., Khan, I.A. 2016. Concurrent and supercritical fluid chromatographic analysis of Terpene Lactones and ginkolic acids in Ginko biloba. Analytical and Bioanalytical Chemistry. 408(17):4649-4660. doi: 10.1007/s00216-016-9544-6.

Interpretive Summary: This manuscript describes a novel analytical method for the analysis of two classes of compounds are found in Ginkgo biloba extracts, a popular supplement for age-associated impairments. The safety and efficacy of dietary supplements containing ginkgo materials are directly dependent upon the analytical techniques used for the analysis of medicinally important components such as the terpene lactones and ginkgolic acids. This new supercritical fluid chromatographic technique is unique and allows the resolution and quantification of all the ginkgolic acids and terpene lactones concurrently, for the first time.

Technical 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 ion, 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, SIM 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, SIM 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 ng/mL 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 87-109%. 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 minutes.