High-resolution gas chromatography/mass spectrometry method for characterization and quantitative analysis of ginkgolic acids in Ginkgo biloba plants, extracts, and dietary supplements.
A high-resolution gas chromatography/mass spectrometry (GC/MS) with selected ion monitor method focusing on the characterization and quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba L. plant materials, extracts, and commercial products was developed and validated. The method involved sample extraction with (1:1) methanol and 10% formic acid, liquid-liquid extraction with n-hexane, and derivatization with trimethylsulfonium hydroxide (TMSH). Separation of two saturated (C13:0 and C15:0) and six unsaturated ginkgolic acid methyl esters with different positional double bonds (C15:1 Δ8 and Δ10, C17:1 Δ8, Δ10, and Δ12, and C17:2) was achieved on a very polar (88% cyanopropyl) aryl-polysiloxane HP-88 capillary GC column. The double bond positions in the GAs were determined by ozonolysis. The developed GC/MS method was validated according to ICH guidelines, and the quantitation results were verified by comparison with a standard high-performance liquid chromatography method. Nineteen G. biloba authenticated and commercial plant samples and 21 dietary supplements purported to contain G. biloba leaf extracts were analyzed. Finally, the presence of the marker compounds, terpene trilactones and flavonol glycosides for Ginkgo biloba in the dietary supplements was determined by UHPLC/MS and used to confirm the presence of G. biloba leaf extracts in all of the botanical dietary supplements.
National Center for Natural Products Research, and ‡Division of Pharmacognosy, Department of BioMolecular Science, School of Pharmacy, University of Mississippi , University, Mississippi 38677, United States.
Mei
M
Wang
Jianping
J
Zhao
Bharathi
B
Avula
Yan-Hong
YH
Wang
Cristina
C
Avonto
Amar G
AG
Chittiboyina
Philip L
PL
Wylie
Jon F
JF
Parcher
Ikhlas A
IA
Khan
D019587:Dietary Supplements / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D020441:Ginkgo biloba / Q000737:chemistry*; D015394:Molecular Structure; D010936:Plant Extracts / Q000737:chemistry* / Q000302:isolation & purification; D012459:Salicylates / Q000737:chemistry* / Q000302:isolation & purification
D010936:Plant Extracts; D012459:Salicylates; C112485:ginkgolic acid
Ginkgo biloba; TMSH derivatization; dietary supplements; gas chromatography/mass spectrometry; ginkgolic acids; ozonolysis