Separation and purification of furanocoumarins from Toddalia asiatica (L.) Lam. using microwave‐assisted extraction coupled with high‐speed counter‐current chromatography

Abstract

A method of microwave-assisted extraction coupled with high-speed counter-current chromatography was established for separation and purification of isopimpinellin, pimpinellin and phellopterin from Toddalia asiatica (L.) Lam. The conditions of MAE including the extraction solvent, size of sample, solid/liquid ratio, extraction temperature and extraction time were optimized by a mono-factor test. That is, 2.0 g dried powder of T. asiatica (L.) Lam of 0.30-0.15 mm size was extracted with 20 mL (solid/liquid ratio of 1:10, g/mL) methanol under 50 °C for 1 min. The crude extract was separated and purified by high-speed counter-current chromatography with hexane-ethyl acetate-methanol-water (5:5:5.5:4.5, v/v/v/v) solvent system. 0.85 mg/g of isopimpinellin, 2.55 mg/g of pimpinellin and 0.95 mg/g of phellopterin were obtained from original sample in one-step within 240 min, the purity determined by high performance liquid chromatography was 95.0%, 99.1% and 96.4%, respectively. Their chemical structures were further identified by mass spectroscopy and nuclear magnetic resonance spectroscopy. The results demonstrated that microwave-assisted extraction coupled with high-speed counter-current chromatography was a feasible, economical and efficient technique for rapid extraction, separation and purification of effective compounds from natural products.

Bioactivity-guided isolation of antimicrobial coumarins from Heracleum mantegazzianum Sommier & Levier (Apiaceae) fruits by high-performance counter-current chromatography

“…By applying this method pure pimpinellin and phellopterin were isolated rapidly for the first time. Previously, Qiu, Xiao, & Li (2012) purified these molecules from the roots of Toddalia asiatica (L.) Lam. (Rutaceae) using HSCCC, however the total run time was more than 200 min, while our method permitted the separation within 50 min.…”

Rapid preparative separation of six bioactive compounds fromGentiana crassicaulisDuthie ex Burk. using microwave-assisted extraction coupled with high-speed counter-current chromatography

“…Microwave-assisted extraction (MAE) is a process that enables solvent homogeneous heating and plant internal superheating which facilitates the extraction [14], its key advantages are shortened extraction time and high yield [15, 16]. Central composite design response surface methodology (CCD-RSM) is a collection of mathematical and statistical techniques that can be used for studying the effect of several factors at different level and their influence on each other [17, 18].…”

High‐performance countercurrent chromatography separation of Peucedanum cervaria fruit extract for the isolation of rare coumarin derivatives

“…A suitable solvent system is one in which the target components have a K value between approximately 0.2 and 5 . Results, which have been published so far, indicated mixtures of HEMW as the most suitable and the most often used . Nevertheless some authors successfully replaced alkanes with light petroleum ether and also mixtures of chloroform, methanol, and water have been applied for purification of simple coumarins and some chromone derivatives .…”