Validation of capillary gas chromatographic method for determination of bilobalide and ginkgolides A, B, C in Ginkgo biloba dry and liquid extracts.
A method for identification and quantitative determination of ginkgolides A, B, and C and bilobalide in liquid and dry extracts of Ginkgo biloba extracts has been developed. Determinations made by employing capillary gas chromatography technique with FID detection were preceded by derivatization using BSTFA with TMCS addition at 120 degrees C. Cholesterol was used as an internal standard. Validation of the method shows no interferences with concurrent constituents; average resolution (R), controlled for peaks of cholesterol and ginkgolide A was 1.53 (SD = 0.06). In the temperature program used (from 50 degrees C to 300 degrees C) the analyte retention times range from 11.2 min. (bilobalide) to 13.8 min. (ginkgolide C) and are of high repeatability of relative values (RRT): RSD = 0.05% / 0.07% for ginkgolides. High correlation coefficients (r), detector signal linearity: from 0.99962 for ginkgolide C to 0.99985 for ginkgolide A were obtained within the concentration range under investigation. The method is of high sensitivity: limits of detection and limits of determination are 35 pg and 44 pg for bilobalide, respectively, while for ginkgolides (Gk) are: 78 pg and 92 pg for GkA, 57 pg and 68 pg for GkB, and 213 pg and 320 pg for GkC.
Department of Inorganic and Analytical Chemistry, Collegium Medicum, Jagiellonian University, 9 Medyczna St., 30-688 Kraków, Poland. jankrzek@cm-uj.krakow.pl
Jan
J
Krzek
Janusz S
JS
Czekaj
Włodzimierz
W
Rzeszutko
Radosław J
RJ
Ekiert
D002849:Chromatography, Gas / Q000379:methods*; D003517:Cyclopentanes / Q000032:analysis / Q000302:isolation & purification; D005410:Flame Ionization; D005663:Furans / Q000032:analysis / Q000302:isolation & purification; D020441:Ginkgo biloba / Q000737:chemistry*; D046934:Ginkgolides / Q000032:analysis / Q000302:isolation & purification; D007783:Lactones / Q000032:analysis / Q000302:isolation & purification; D010936:Plant Extracts / Q000737:chemistry*; D018515:Plant Leaves; D015203:Reproducibility of Results; D013696:Temperature
D003517:Cyclopentanes; D005663:Furans; D046934:Ginkgolides; D007783:Lactones; D010936:Plant Extracts; C058295:ginkgolide C; C045856:ginkgolide B; C073710:bilobalide; C477042:ginkgolide A