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目的:优化超声-酶法提取两面针中白屈菜红碱及其6-烷氧基衍生物的工艺条件。方法:采用HPLC测定白屈菜红碱及其6-烷氧基衍生物提取率,流动相乙腈-水-磷酸-三乙胺(25∶75∶0.2∶0.25),检测波长284 nm。通过单因素试验考察溶剂加酸和酶解预处理对有效成分提取率的影响,利用正交试验优化提取次数、超声功率和溶剂用量,通过动态过程优化超声时间。结果:最佳工艺条件为复合酶预处理后,加40%乙醇(含盐酸0.5%)于250 W超声提取3次,每次的溶剂用量分别为6,3,3倍,提取时间依次为18,15,12 min。白屈菜红碱及其6-烷氧基衍生物提取率90.5%。结论:该工艺经济、高效、节能、省时,可为开发利用两面针中白屈菜红碱等成分提供实验基础。
OBJECTIVE: To optimize the ultrasonic and enzymatic conditions for the extraction of chelerythrine and its 6-alkoxy derivatives from two-sided needle. Methods: The extraction rate of chelerythrine and its 6-alkoxy derivatives was determined by HPLC. The mobile phase was acetonitrile-water-phosphoric acid-triethylamine (25:75:0.2:0.25). The detection wavelength was 284 nm. The effects of solvent addition and enzymolysis pretreatment on the extraction rate of active ingredients were investigated by single factor experiments. The orthogonal experiment was used to optimize the extraction times, ultrasonic power and solvent dosage, and the ultrasonic time was optimized by dynamic process. Results: The optimum conditions for the enzyme pretreatment, plus 40% ethanol (containing hydrochloric acid 0.5%) at 250 W ultrasonic extraction three times, each time the amount of solvent were 6,3,3 times, respectively, the extraction time was 18 , 15,12 min. Chelerythrine and its 6-alkoxy derivative extraction rate of 90.5%. Conclusion: The process is economical, efficient, energy-saving and time-saving, which can provide the experimental basis for the development and utilization of chelerythrine and other ingredients in the two-sided needles.