MICROWAVE-ASSISTED HYDROLYZATION OF THE FLAVONOIDS IN EPIMEDIUM KOREAMUM NAKAI

In the present paper, icariside I has been prepared by hydrolyzing the flavonoids extract of Epimedium Koreamum Nakai in acid solution. Two heating methods, reflux and microwave irradiation, were used in the hydrolysis reaction and hydrolyzed products were analyzed by high performance liquid chromatography-diode array detection-electrospray ionization tandem mass spectometry (HPLC-DAD-ESI-MSn). The four flavonoids in the extracts have been identified as epimedin A, epimedin B, epimedin C, and icariin, and the hydrolysis product was icariside I. Icariside I has been evaluated by comparing with the peak areas of HPLC-DAD spectra obtained using different heating methods. The experimental results demonstrate that the advantage of microwave irradiation over conventional reflux is validated, and the hydrolysis time is dramatically reduced, and the yield of icariside I is effectively improved. Also, optimum conditions for microwave hydrolysis are established. As a result, the optimum yield of icariside I can be reached under the following conditions: the reaction temperature is 70°C; the microwave irradiation power is 600 W; and the microwave irradiation time is 10 min. The optimum yield by this method was (300.46 ± 0.41 µg), which was 2.3 times more than the classical way (128 ± 0.86 µg). In view of the efficiency, energy saving, and environmental protection in the procedures of microwave-assisted hydrolyzation, this method will have a bright future in the industrial application.

[1]  Wu Shaohui,et al.  Research advance in the pharmacological effects of icariin. , 2013 .

[2]  Lianmei Zhao,et al.  [The effects of ICA on the cell-immunosuppressive and bone-marrow-suppressive mice after chemotherapy]. , 2010, Xi bao yu fen zi mian yi xue za zhi = Chinese journal of cellular and molecular immunology.

[3]  Weiwei Zhai,et al.  Optimization of microwave-assisted extraction of anthocyanins from purple corn (Zea mays L.) cob and identification with HPLC–MS , 2010 .

[4]  Zhang Xiao-yu Mechanism of resisting exercise fatigue by Epimedium flavones in mice , 2009 .

[5]  Elsevier Sdol,et al.  World Science and Technology – Modernization of Traditional Chinese Medicine and Materia Medica , 2009 .

[6]  Xiaosong Hu,et al.  Optimization of microwave-assisted extraction of anthocyanins in red raspberries and identification of anthocyanin of extracts using high-performance liquid chromatography – mass spectrometry , 2007 .

[7]  Yogesh Mohan,et al.  Microwave Assisted Extraction-An Innovative and Promising Extraction Tool for Medicinal Plant Research , 2007 .

[8]  G. Lin,et al.  Effects of icariin on phosphodiesterase-5 activity in vitro and cyclic guanosine monophosphate level in cavernous smooth muscle cells. , 2006, Urology.

[9]  Tsu-Ming Chien,et al.  Epimedium brevicornum Maxim extract relaxes rabbit corpus cavernosum through multitargets on nitric oxide/cyclic guanosine monophosphate signaling pathway , 2006, International Journal of Impotence Research.

[10]  Li Ling HPLC determination of icariin in Shenbao capsules , 2006 .

[11]  Yumin Yang,et al.  Studies on preparation of oligoglucosamine by oxidative degradation under microwave irradiation , 2003 .

[12]  Sheng-Feng Lai,et al.  Studies on synthesis and adsorption properties of chitosan cross-linked by glutaraldehyde and Cu(II) as template under microwave irradiation , 2001 .

[13]  R. Gedye,et al.  The rapid synthesis of organic compounds in microwave ovens , 1988 .

[14]  Z. Bacq The metabolism of adrenaline. , 1949, The Journal of pharmacology and experimental therapeutics.