两面针的超声-酶法辅助半仿生提取工艺优选

Optimization of Ultrasonic Wave-enzymatic Assisted Semi-bionic Extraction Technology for Zanthoxyli Radix

目的:优选两面针的超声-酶法辅助半仿生提取工艺条件。方法:以氯化两面针碱、总生物碱得率和干膏收率为评价指标,通过正交试验考察超声功率、提取时间及溶剂用量对两面针半仿生超声提取工艺的影响,利用动态过程优选提取时间。运用HPLC测定氯化两面针碱含量,流动相乙腈-水-磷酸-三乙胺(30∶70∶0.15∶0.15),检测波长271 nm;采用UV测定总生物碱含量,检测波长328 nm。结果:最佳提取工艺为复合酶预处理后于250 W超声提取,第1次加5倍量pH2.0磷酸氢二钠-柠檬酸缓冲液提取18 min,第2次加5倍量pH 7.5缓冲液提取15 min,第3次加5倍量pH 8.3缓冲液提取12 min;氯化两面针碱得率0.135%(RSD 1.86%),总生物碱得率1.20%(RSD 1.75%),干膏收率14.65%(RSD1.23%)。结论:本法的氯化两面针碱和总生物碱得率与乙醇回流法接近或稍低,而干膏收率显著提高,可为两面针的大生产提供参考。

Objective：To optimize ultrasonic wave-enzymatic assisted semi-biotic extraction technology for Zanthoxyli Radix.Method：With yields of total alkaloids,nitidine chloride and dry extract as indexes,orthogonal test was adopted to optimize extraction technology by taking ultrasonic power,extraction time and solvent amount as factors,then extraction time was selected by dynamic process.HPLC was employed to determine the content of nitidine chloride with mobile phase of acetonitrile-water-phosphoric acid-triethylamine （30∶ 70∶ 0.15∶0.15） and detection wavelength at 271 nm ; UV was adopted to determine the content of total alkaloids at 328 nm.Result：Optimal extraction process of Zanthoxyli Radix was as follows：after pretreated by cellulase-pectinase,extracted thrice by 5 times the amount of sodium hydrogen phosphate-citric acid buffer with pH of 2.0,7.5 and 8.3,extraction time of 18,15,12 min,respectively; ultrasonic power of 250 W; yields of total alkaloids,nitidine chloride and dry extract were 1.20％,0.135％ and 14.65％ with RSD of 1.75％,1.86％ and 1.23％,respectively.Conclusion：Dry extract yield of this optimized process is significantly higher than ethanol reflux process,while extracting rates of nitidine chloride and total alkaloids are equal with or little lower than the later,this study could provide a reference for industrial production of Zanthoxyli Radix.