均质法联合超滤膜纯化侧柏叶黄酮成分的方法初探

Purification Method of Ultrasonic Emulsification Combined with Ultrafiltration Membrane Separation for Flavonoids in Cacumen Platycladi

目的:利用均质法和超滤膜获得侧柏叶中较高纯度的黄酮总量成分。方法:以侧柏叶中杨梅苷等7个化合物为对照品,采用HPLC法进行含量测定。采用单因素试验法,对比超声、微波、回流和均质提取法的提取含量;利用正交试验,对均质时间、乙醇浓度、料液比和次数4个因素进行考察,采用Biomax-5膜进行超滤膜分离。结果:单因素试验中以均质提取法提取含量最高。正交试验结果,均质时间15 min,乙醇浓度为50%,料液比1∶10,提取3次。超滤膜分离条件,以流量为1.5 L·min^(-1),压力为0.8 kg进行膜分离。结论:均质法和超滤膜的结合,对于侧柏叶中黄酮类化合物的纯化,方法可行,产品纯度高,该方法具有良好的应用前景。

Objective ： To obtain flavonoids of Cacumen Platycladi with high purity by using the method of ultrasonic emulsification combined with ultrafihration membrane separation. Methods： Seven compounds including myricetrin as the reference substances, an HPLC method was used for the content determination. Using the single factor experiments, ultrasound, microwave, reflux and ultrasonic emulsification were compared, and using the orthogonal experiments, the ultrasonic emulsification time, ethanol concentration, solidliquid ratio and times were studied. Biomax-5 membrane was adopted to improve the membrane separation. Results： The single factor experiments showed the homogeneous extraction method with the highest contents. The orthogonal experiments showed the optimal extracting conditions as follows： the ultrasonic emulsification time was 15 min, the ethanol concentration was 50%, the material-liquid ratio was 1 ： 10, and the extraction times was 3. The conditions of ultrafiltration membrane separation were as follows： the flow rate was 1.5 L· min^-1, and the membrane separation pressure was 0.8 kg. Conclusion： The combination of ultrasonic emulsification and ultrafiltration membrane separation is feasible in the extraction and purification of flavonoids in Cacumen Platycladi, and the product is with high purity, suggesting the method has good application prospect.