ABSTRACT
This study was aimed to optimize the extraction technology of Wei-Kang (WK) Capsule. Orthogonal test and comprehensive evaluation were used to optimize the extraction process of compound preparation. The icarrin, to-tal ginkgo flavone glycosides and the dried decocting rates were used as index components for optimizing the effect of ethanol concentration, ethanol volume, extraction duration and extraction frequency. The results showed that the opti-mal ethanol extraction technology was adding 12 times of 60% ethanol and extract for 3 times with 1 h for each ex-traction time. It was concluded that the optimized extraction technology was stable, practical, scientific and reason-able, which can be used in the large-scale industrial production.
ABSTRACT
Object To develop a capillary GC-MS analytical method for identification and deter- mination of ginkgolide A, B, C and bilobalide (GA, GB, GC and BB) in Ginkgo biloba L. leaves. Methods The leave samples were extracted in ultrasonic bath with ethanol-water (20∶80). The extract was purified by liquid-liquid extraction with ethyl acetate followed by solid-phase extraction on a column mixed with acid Al 2O 3, active carbon and celite. The terpenes were trimethylsilylated by BSTFA (with 1% TMCS) for 60 min at 100 ℃ and determined by GC-MS with HP-5 MS capillary column in the selected-ion monitoring mode. The intense fragment ions were chosen as monitoring ions for quantitative analysis. Cholesterol was used as an internal standard. Column temperature gradient: initial temperature 180 ℃, maintained 1 min, and then increased at 20 ℃/min to 260 ℃, and finally at 2 ℃/min up to 300 ℃, maintained 2 min. Results The retention times of GA, GB, GC and BB were 13.7,14.3,15.3 and 6.8 min, the major fragmentation ions (monitoring) were at m/z 537, 625, 713 and 455 (299), the average recoveries of GA, GB, GC and BB were 102.0%, 99.4%, 96.0%, 96.3%, RSD were 0.54%, 2.40%, 1.98% and 2.43%, respectively. Conclusion This method is repeatable, specific, accurate and easy to operate. It is adoptable for quality and quantity analysis of terpene lactones from G. biloba leaves.