八角枫中总生物碱的含量测定、提取及大孔树脂纯化工艺优化  

Determination of total alkaloids in Alangium sinensis,optimization of extraction process and purification process of macroporous resin

作　　者：肖思羽 张永萍 徐剑 程纯 刘杰 曹国琼 刘耀 XIAO Siyu;ZHANG Yongping;XU Jian;CHENG Chun;LIU Jie;CAO Guoqiong;LIU Yao(College of Pharmaceutical Sciences,Guizhou University of Traditional Chinese Medicine,Guiyang 550025,China;National Engineering Technology Research Center for Miao Medicine,Guiyang 550025,China;Guizhou Engineering Technology Research Center for Processing and Preparation of Traditional Chinese Medicineand Ethnic Medicine,Guiyang 550025,China)

机构地区：[1]贵州中医药大学药学院,贵阳550025 [2]国家苗药工程技术研究中心,贵阳550025 [3]贵州中药炮制与制剂工程技术研究中心,贵阳550025

出　　处：《吉林中医药》2024年第12期1456-1463,共8页Jilin Journal of Chinese Medicine

基　　金：国家苗药工程技术研究中心能力提升项目(黔科合中引地〔2023〕006);贵州省高等学校中药民族药(苗药)新剂型新制剂工程研究中心项目(黔教技〔2022〕022);贵州省高层次创新型人才项目(黔科合平台人才-GCC〔2023〕037)。

摘　　要：目的建立八角枫[Alangium chinese(Lour.)Harms]中总生物碱的含量测定方法,并对其提取工艺及大孔树脂的纯化工艺进行优化。方法采用酸性染料比色法测定八角枫中总生物碱的含量;在单因素实验基础上,利用Box-Behnken设计-响应面法,以提取溶剂浓度、提取溶剂体积、提取时间为考察因素,总生物碱含量为评价指标,设计三因素三水平实验,以优化八角枫总生物碱(alangium total alkaloids)的提取工艺;采用静态吸附和解吸实验对5种大孔树脂进行筛选,以吸附、解吸性能为考察指标,确定大孔树脂类型,利用单因素实验考察静态吸附时间、上样液质量浓度、上样液体积等因素,优化大孔树脂纯化工艺。结果在含量测定中确定酸性染料为溴甲酚绿,用量为5 mL,磷酸氢二钠-柠檬酸缓冲溶液pH为5.0,检测波长为415 nm;优化提取工艺参数为:提取溶剂浓度为80%,10倍量提取溶剂体积,提取时间为2.0 h;最优大孔树脂纯化工艺为:采用D101型大孔吸附树脂,上样液质量浓度3.02 mg/mL,上样液pH=6.0,上样液体积45 mL,上样液流速1.0 mL/min,树脂柱径高比为1:3,静置60 min;乙醇洗脱液体积分数90%,洗脱流速2 mL/min,乙醇洗脱液体积120 mL。结论所建含量测定方法灵敏度高、稳定性好;优化后的提取、纯化工艺稳定、可行,为其临床应用开发与工业化生产提供依据。Objective To establish a method for the determination of total alkaloids in Alangium chinese(Lour.)Harms,and to optimize its extraction process and the purification process of macroporous resin.Methods Acid dye colorimetry was used to determine the content of total alkaloids in Alangium sinensis.On the basis of single factor experiment,Box-Behnken design-response surface method was used to optimize the extraction process of total alkaloids from Alangia L.with concentration,volume and time of extraction solvent as factors and total alkaloid content as evaluation indexes.Static adsorption and desorption tests were used to screen 5 kinds of macroporous resins,and the types of macroporous resins were determined based on their adsorption and desorption properties.The static adsorption time,mass concentration of sample liquid and volume of sample liquid were investigated by single factor experiments to optimize the purification process of macroporous resins.Results The content of the acid dye was determined as bromocresol green,the dosage was 5 mL,the pH of disodium hydrogen phosphate and citrate buffer solution was 5.0,and the detection wavelength was 415 nm.The optimized extraction parameters were as follows:the extraction solvent concentration was 80%,the extraction solvent volume was 10 times,and the extraction time was 2.0 h.The optimal macroporous resin purification process was as follows:D101 macroporous adsorption resin was used,the mass concentration of sample liquid was 3.02 mg/mL,the pH of sample liquid was 6,the volume of sample liquid was 45 mL,the flow rate of sample liquid was 1.0 mL/min,the ratio of resin column diameter to height was 1:3,and the purification process was left for 60 minutes.The integral number of ethanol elution liquid was 90%,the elution flow rate was 2 mL/min,and the volume of ethanol elution liquid was 120 mL.Conclusion The method is sensitive and stable.The optimized extraction and purification process is stable and feasible,which provides a basis for clinical application developmen

关 键 词：八角枫 总生物碱 含量测定 提取工艺 大孔树脂 纯化工艺 

分 类 号：R284.2[医药卫生—中药学]