| Objective:Investigate the technique of extracting and purifying aucubin from Aucuba japonica Variegata. Study on the quality standard of aucubin, and draw up quality standard draft. Evaluate the stability of aucubin.Method:Extract aucubin from Aucuba japonica Variegata through Loop scavenging, measure content of aucubin by HPLC.Adopt macroporous resin S-8and Silica gel separate aucubin, preference the best condition. Purify aucubin through crystallization method, and then make structural identification. Evaluate quality of aucubin by way of describing character, measuring physicochemical constants, establishing differential and checked method, also the way to measurement of the aucubin content. Adopt effect factor test evaluate stability of aucubin.Result:Taking aucubin as indexes, the best result of macroporous resin S-8is as follows: sample concentration2.76mg-mL-1, feed rate2BV/h, sample capacity9.56mg/g, eluant15%ethanol water, elution flow rate2BV/h, total quantity of eluant3BV. The best condition of silicagel column:eluant CH3OH-CHCl3(1:4,1:3), sample capacity35mg/ml, elution volume3BV, elution flow rate2BV/h. According to the method, the content and the recovery rate of79.19%and83.38%.After crystallization process, elaboration product would be got.Investigate physicochemical property, discrimination, examination, assay and stability of aucubin, draw up quality standard draft. Aucubin is white or almost white crystalline powder, odorless, water-soluble. It is water-soluble and methanol-soluble, ethanol sparingly soluble, but in organic solvent like CHCl3, petroleum ether is undissolved. It is easy to absorb moist. Specific rotation of aucubin is-117°. Qualitative identification is made by TLC, HPLC, and IR and so on. The test of release is according to China Pharmacopeia (2010edition), and provide the lowest contents of impurity. HPLC can be applied to determination of aucubin. The result shows that the method is satisfactory, well-repeatable. The result of stability test indicated that aucubin is unstable when it comes to high-temperature and high humidity.Conclusion:Separating aucubin by extraction of ethanol, macro porous resin S-8separation, silica column chromatography and crystallization method step by step, the purity of aucubin is over90%. It reaches the principle of raw material drug. Quality standard draft of aucubin is comprehensive and operable. Aucubin is unstable when it comes to high-temperature and high humidity, so it should be kept at low temperature and seal up completely. |