Microwave-assisted extraction coupled with countercurrent chromatography for the rapid preparation of flavonoids from Scutellaria barbata D. Don.

As a famous Chinese herb having good inhibitory effects on numerous human cancers both in vitro and in vivo, Scutellaria barbata D. Don attracts extensive attention worldwide. In this work, four flavonoids named scutellarin, baicalin, luteolin, and apigenin were simply and rapidly prepared from S. barbata by microwave-assisted extraction coupled to countercurrent chromatography. Extraction conditions including irradiation time, extraction temperature, liquid/solid ratio, and microwave power were optimized using an orthogonal array design method. The extract of S. barbata was separated and purified with a two-phase solvent system composed of hexane/ethyl acetate/methanol/acetic acid/water (1:5:1.5:1:4, v/v/v/v/v) and 4.5 mg of scutellarin, 4.6 mg of baicalin, 1.1 mg of luteolin, 2.1 mg of apigenin were obtained from 2.0 g original sample in a single run. The purities of scutellarin, baicalin, luteolin, and apigenin determined by HPLC were 93.6, 97.3, 97.6, and 98.4%, respectively. The targeted compounds were identified by LC with MS and (1) H NMR spectroscopy. The total time including extraction, separation, and purification was <300 min. Compared to traditional methods, microwave-assisted extraction coupled to countercurrent chromatography method is more simple and rapid for the extraction, separation, and purification of flavonoid compounds from natural products.

Ionic liquid aqueous solvent-based microwave-assisted hydrolysis for the extraction and HPLC determination of myricetin and quercetin from Myrica rubra leaves.

An ionic liquid aqueous solvent-based microwave-assisted hydrolysis (ILAS-MAH) approach was proposed for the rapid extraction and accurate determination of myricetin and quercetin from Myrica rubra (M. rubra) leaves for the first time. The effects of the ionic liquid class and concentration, liquid-solid ratio, hydrolysis temperature and time were investigated to obtain the optimal ILAS-MAH conditions. The optimized conditions were 2.0 mol/L [bmin][HSO4] or 2.5 mol/L acidified [bmin]Br solution, liquid-solid ratio 30:1 (mL : g), hydrolysis temperature 70°C and hydrolysis time 10 min. Under these conditions, the recoveries of myricetin and quercetin were in the range of 86.3-107.3% with relative standard deviation lower than 5.8%. Compared with conventional heating hydrolysis and regular MAH, the proposed approach reduced hydrolysis time and improved yields. The mechanism of ILAS-MAH was also investigated.

Application of ionic liquids in the microwave-assisted extraction of polyphenolic compounds from medicinal plants.

Ionic liquids (ILs) solutions as solvents were successfully applied in the microwave-assisted extraction (MAE) of polyphenolic compounds from medicinal plants. ILs, its concentration and MAE conditions were investigated in order to extract polyphenolic compounds effectively from Psidium guajava Linn. (P. guajava) leaves and Smilax china (S. china) tubers. The results obtained indicated that the anions and cations of ILs had influences on the extraction of polyphenolic compounds as well as the ILs with electron-rich aromatic pi-system enhanced extraction ability. Under the optimized conditions, the extraction yields of the polyphenolic compounds were in the range of 79.5-93.8% with one-step extraction, and meanwhile the recoveries were in the range of 85.2-103% with relative standard deviations (R.S.D.s) lower than 5.6%. Compared to conventional extraction procedures, the results suggested that the proposed method was effective and alternative for the extraction of polyphenolic compounds from medicinal plants. In addition, the extraction mechanisms and the structures of samples before and after extraction were also investigated. ILs solutions as green solvents in the MAE of polyphenolic compounds from medicinal plant samples showed a great promising prospect.

Study of vacuum microwave-assisted extraction of polyphenolic compounds and pigment from Chinese herbs.

Vacuum microwave-assisted extraction (VMAE), in which microwave-assisted extraction (MAE) was performed in vacuum, was specially designed and applied for the extraction of polyphenolic compounds and pigments from Chinese herbs. The extraction conditions including solid/liquid ratio, extraction time, extraction temperature and degree of vacuum were optimized. Subsequently, VMAE, MAE, and conventional heating reflux extraction (HRE) were evaluated with resveratrol and emodin extraction from Rhizma Polygoni Cuspidati, myricetin and quercetin extraction from Myrica rubra leaves, and safflomin A extraction from Flos Carthami. In addition, the different microstructures of those rhizome, leaf, and flower samples were investigated before and after extraction. It was obvious that the extraction yields of resveratrol, myricetin and safflomin A (thermosensitive compounds) with VMAE were higher than that with MAE or HRE by increments of 6.4-9.4% and 7.9-29.5%, respectively. In contrast, there was no obvious difference among the extraction yields for emodin and quercetin (thermo-stable compounds) with VMAE, MAE and HRE, except that the solvent consumption in VMAE was decreased. The results suggest that VMAE is a good alternative for the extraction of polyphenolic compounds and pigments, especially thermosensitive compounds, from Chinese herbs.