In this study, a green extraction and purification process for the rapid preparation of corilagin from Phyllanthus has been designed using an aqueous ionic liquid coupled with preparative high-performance liquid chromatography (prep-HPLC) and precipitation. The results showed that the optimum extraction process for corilagin involved mixing Phyllanthus tenellus Roxb. with 0.4 M [BMIm]Br at a liquid–solid ratio of 10 : 1 and dispersing the mixture by ultrasonication at 50 °C for 15 min. Macroporous resin D101 and prep-HPLC were employed for [BMIm]Br removal and corilagin separation to yield corilagin of 86.49% purity. Subsequently, corilagin was further purified by water precipitation to achieve 99.12% purity. The results indicated the successful development of a new rapid and green process to prepare corilagin on a large scale from plants using [BMIm]Br. This promising process can be applied for the preparative separation and purification of other active compounds from complex plant systems.

Herein, we reported a novel approach for the preparative separation and purification of loliolide and epiloliolide from Ascophyllum nodosum. An amine-based microporous organic polymer (MOP) was used for the pretreatment of the nodosum extract via solid-phase extraction (SPE). The obtained extract was further purified using macroporous resin chromatography and preparative high-performance liquid chromatography (prep-HPLC). The loading and elution parameters of the MOP were evaluated using standard loliolide, and the optimized conditions were used during the SPE of the nodosum extract (37.5 g). After the pretreatment with MOP, the extract (2.79 g) was obtained and further purified using a D101 resin column followed by prep-HPLC. A pair of epimers were isolated and identified as loliolide (5.83 mg) and epiloliolide (2.50 mg) using high-resolution electrospray ionization tandem mass spectrometry (HRESI-MS), 1D- and 2D-nuclear magnetic resonance (NMR) spectroscopy. This study demonstrates the potential of MOPs in the separation and purification of monoterpenoids from complex plant samples.