HPD-100大孔树脂分离纯化延胡索总生物碱的工艺研究
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摘要
目的:优选HPD-100大孔吸附树脂分离纯化延胡索总生物碱的工艺条件,为工业化生产提供依据。方法:采用酸性染料比色法测定延胡索总生物碱的含量,并以此为评价指标,以延胡索醇提浓缩液上样流速、吸附柱径高比、药液浓度3个影响树脂的载样量的因素设计正交试验,对延胡索总生物碱解吸性能进行考察,从而确定延胡索总生物碱解吸剂的类型和用法及洗脱流速。结果:HPD-100大孔吸附树脂有较大吸附量、易吸附、易解吸附,延胡索提取液浓度为0.25g/mL,流速为2BV/h,吸附柱径高比为1∶15,洗脱液体积定为先用60%乙醇5BV再用80%乙醇1BV,洗脱流速为3BV/h,为最优分离纯化工艺条件。结论:该延胡索总生物碱的分离纯化工艺科学、合理、稳定、可行、无环境污染、绿色环保、成本低,适合工业化生产。
Objective: To optimize the process conditions ofmacroporous adsorption resin HPD-100 for separation and purification of total alkaloids from Corydalis, and to provide basis for industrial production. Methods: The content of total alkaloids in Corydalis was determined by acid dye colorimetry, and it was used as an evaluation index. The orthogonal experiment was carried out with three factors affecting the loading of the resin, such as the loading flow rate of the extract of the fumarate,the diameter ratio of the adsorption column, and the concentration of the liquid. The desorption performance of the total alkaloids of Corydalis was investigated to determine type and usage of desorbent and elution flow rate. Results: HPD-100 macroporous adsorption resin had larger adsorption amount, easy adsorption and desorption. The optimum separation and purification process conditions were: the concentration of drug solution from Corydalis was 0.25 g/mL, velocity of absorption was 2 BV/h, ratio of diameter and height from adsorption column was 1 : 15, first solvent of elution was 5 BV 60% of alcohol and then 1 BV 80% of alcohol, and velocity of elution was 3 BV/h. Conclusion: The separation and purification process of total alkaloids of Corydalis is scientific, reasonable, stable, feasible, environmentally friendly, environmentally friendly and low cost, which is suitable for industrial production.
Objective: To optimize the process conditions ofmacroporous adsorption resin HPD-100 for separation and purification of total alkaloids from Corydalis, and to provide basis for industrial production. Methods: The content of total alkaloids in Corydalis was determined by acid dye colorimetry, and it was used as an evaluation index. The orthogonal experiment was carried out with three factors affecting the loading of the resin, such as the loading flow rate of the extract of the fumarate,the diameter ratio of the adsorption column, and the concentration of the liquid. The desorption performance of the total alkaloids of Corydalis was investigated to determine type and usage of desorbent and elution flow rate. Results: HPD-100 macroporous adsorption resin had larger adsorption amount, easy adsorption and desorption. The optimum separation and purification process conditions were: the concentration of drug solution from Corydalis was 0.25 g/mL, velocity of absorption was 2 BV/h, ratio of diameter and height from adsorption column was 1 : 15, first solvent of elution was 5 BV 60% of alcohol and then 1 BV 80% of alcohol, and velocity of elution was 3 BV/h. Conclusion: The separation and purification process of total alkaloids of Corydalis is scientific, reasonable, stable, feasible, environmentally friendly, environmentally friendly and low cost, which is suitable for industrial production.
引文
[1]刘俊红,魏峻峰.大孔吸附树脂在延胡索生物碱提取分离中的应用.中草药,2002,33(1):37-38
[2]江苏新医学院.中药大辞典.上海:上海科学技术出版社,1975:921-921
[3]王绪颖,贾晓斌,陈彦.延胡索总生物碱的提取纯化工艺研究.中成药,2010,32(11):1899-1904
[4]桑彤,谢培德.延胡索渗漉提取工艺的优选.基层中药杂志,2000,14(3):35-36
[5]姜欣欣,李跃金,陈维.超临界CO2萃取技术在中药有效成分提取中的应用.广东化工,2015,42(1):53-54
[6]孙百虎,尚平,卜欣立.元胡中生物碱的醇回流提取.河北化工,2008,31(2):41-44
[7]秦秀蓉,汤燕.超声法提取延胡索有效部分的工艺研究.成都中医药大学学报,2005,28(4):47-52
[8]袁红波,彭国平,郑云枫.p SFC色谱法分离夏天无中的原阿片碱和延胡索乙素.华西药学杂志,2007,22(2):133-135
[9]王婷,胡凤英,潘桂湘.延胡索生物碱的高速逆流分离制备和纯化.时珍国医国药,2014,25(10):2403-2404
[10]吕子明,刘文娟,于向红.大孔吸附树脂纯化延胡索总生物碱工艺研究.中国医药导报,2012,9(20):109-112
[11]李雪丽,刘建勋.延胡索大孔吸附树脂的分离纯化工艺研究.中华中医药杂志,2014,29(4):1021-1024
[12]冀德富,冯凯,张勇,等.粉防己总生物碱的提取与纯化研究.中华中医药杂志,2017,32(12):5656-5658
[2]江苏新医学院.中药大辞典.上海:上海科学技术出版社,1975:921-921
[3]王绪颖,贾晓斌,陈彦.延胡索总生物碱的提取纯化工艺研究.中成药,2010,32(11):1899-1904
[4]桑彤,谢培德.延胡索渗漉提取工艺的优选.基层中药杂志,2000,14(3):35-36
[5]姜欣欣,李跃金,陈维.超临界CO2萃取技术在中药有效成分提取中的应用.广东化工,2015,42(1):53-54
[6]孙百虎,尚平,卜欣立.元胡中生物碱的醇回流提取.河北化工,2008,31(2):41-44
[7]秦秀蓉,汤燕.超声法提取延胡索有效部分的工艺研究.成都中医药大学学报,2005,28(4):47-52
[8]袁红波,彭国平,郑云枫.p SFC色谱法分离夏天无中的原阿片碱和延胡索乙素.华西药学杂志,2007,22(2):133-135
[9]王婷,胡凤英,潘桂湘.延胡索生物碱的高速逆流分离制备和纯化.时珍国医国药,2014,25(10):2403-2404
[10]吕子明,刘文娟,于向红.大孔吸附树脂纯化延胡索总生物碱工艺研究.中国医药导报,2012,9(20):109-112
[11]李雪丽,刘建勋.延胡索大孔吸附树脂的分离纯化工艺研究.中华中医药杂志,2014,29(4):1021-1024
[12]冀德富,冯凯,张勇,等.粉防己总生物碱的提取与纯化研究.中华中医药杂志,2017,32(12):5656-5658