响应曲面法优化钩藤叶中钩藤碱和异钩藤碱的提取条件
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摘要
以钩藤叶为材料,在干燥温度、提取时间和提取剂浓度3个单因素试验的基础上,采用Box-Behnken中心组合进行3因素3水平试验设计,建立回归方程,优化出钩藤叶中钩藤碱和异钩藤碱的最佳提取条件。模拟得到钩藤叶干燥温度为54.95℃时,钩藤碱和异钩藤碱的最优提取条件为超声时间60 min、甲醇浓度73.35%。在此条件下,钩藤碱的最高提取率为133.342μg·g~(-1),异钩藤碱的最高提取率为429.746μg·g~(-1)。为了方便实际操作,校正条件为干燥温度55℃、超声提取60 min、甲醇浓度73%。通过验证试验得到钩藤碱平均提取率为130.8μg·g~(-1),异钩藤碱平均提取率为425.6μg·g~(-1),与模型预测值较为接近。因此响应曲面法可以对钩藤叶中钩藤碱和异钩藤碱的提取条件进行优化。
The leaves of U. rhynchophylla were used as test materials, on the basis of three single factor tests, the effects of drying temperature, extracting time and extractant concentration were studied by three-factor and three-level test developed by Box-Behnken central composite test design and the relative equations were established, which optimized the extraction conditions. When the drying temperature of leaves is 54.95 ℃, the optimal extraction conditions of rhynchophylline and isorhynchophylline were 60 mins of ultrasound time, 73.35% of methanol, and the extraction value of rhynchophylline was 133.342 μg·g~(-1) and of isorhynchophylline was 429.746 μg·g~(-1). In order to facilitate the practice, the conditions were modified as follows: drying temperature was 55 ℃, ultrasound time was 60 min, the volume of methanol was 73%. From the verification test, the average yield of rhynchophylline was 130.8 μg·g~(-1) and of isorhynchophylline was 425.6 μg·g~(-1), which is close to the model predicted value. Thus the response surface method can be used to optimize the extraction conditions of rhynchophylline and isorhynchphylline in the leaves of U. rhynchophylla.
The leaves of U. rhynchophylla were used as test materials, on the basis of three single factor tests, the effects of drying temperature, extracting time and extractant concentration were studied by three-factor and three-level test developed by Box-Behnken central composite test design and the relative equations were established, which optimized the extraction conditions. When the drying temperature of leaves is 54.95 ℃, the optimal extraction conditions of rhynchophylline and isorhynchophylline were 60 mins of ultrasound time, 73.35% of methanol, and the extraction value of rhynchophylline was 133.342 μg·g~(-1) and of isorhynchophylline was 429.746 μg·g~(-1). In order to facilitate the practice, the conditions were modified as follows: drying temperature was 55 ℃, ultrasound time was 60 min, the volume of methanol was 73%. From the verification test, the average yield of rhynchophylline was 130.8 μg·g~(-1) and of isorhynchophylline was 425.6 μg·g~(-1), which is close to the model predicted value. Thus the response surface method can be used to optimize the extraction conditions of rhynchophylline and isorhynchphylline in the leaves of U. rhynchophylla.
引文
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[20]张荣,刘睿,刘启德,等.钩藤中钩藤碱、异钩藤碱的提取与含量测定[J].中药新药与临床药理,2009,20(4):338-341.
[21]刘清华,葛尔宁.RP-HPLC法测定钩藤煎剂中钩藤碱含量及变化[J].浙江中医药大学学报,2010,34(2):270-272.
[22]刘卫,杨雪萍,王中师,等.钩藤总碱的热稳定研究[J].药学实践杂志,2011,29(6):442-444.
[23]黄卓谦,刘建利,王玉英,等.钩藤煎煮过程中化学成分变化[J].西北大学学报(自然科学版),2008,38(5):787-789.
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[3]吴卫,周娜,刘梅.HPLC法测定钩藤提取物中钩藤碱的含量[J].安徽农业科学,2012,40(11):6442-6443.
[4]Bertol G,Franco L,Oliveira BH.HPLC Analysis of Oxindole Alkaloids in Uncaria Tomentosa:Sample Preparation and Analysis Optimisation by Factorial Design[J].Phytochemical Analysis,2012,23(2):143-151.
[5]Kushida H,Fukutake M,Tabuchi M,et al.Simultaneous quantitative analyses of indole and oxindole alkaloids of Uncaria Hook in rat plasma and brain after oral administration of the traditional Japanese medicine Yokukansan using high‐performance liquid chromatography with tandem mass spectrometry[J].Biomedical Chromatography,2013,27(12):1647-1654.
[6]Ganzera M,Muhammad I,Khan R,et al.Improved Method for the Determination of Oxindole Alkaloids in Uncaria tomentosa by High Performance Liquid Chromatography[J].Planta Medica2001,67(5):447-450.
[7]宋纯清,樊懿,黄伟晖,等.钩藤中不同成分降压作用的差异[J].中草药,2000,31(10):762-764.
[8]SakakibaraΙ,Terabayashi S,Kubo M,et al.Effectson locomotionof indole alkaloids from the hooks of uncaria plants[J].Phytomedicine,1999,6(3):163-168.
[9]田丽娜,高华武,龙子江,等.钩藤碱对自发性高血压大鼠的降压作用及其对血管的调节机制探讨[J].中草药,2014,45(15):2210-2213.
[10]汪冰,袁丹,马斌,等.钩藤叶化学成分的研究[J].中国药物化学杂志,2006,16(6):369-372.
[11]刘遂库.钩藤叶生物碱有效部位的制备工艺、药理活性和急性毒性研究[D].沈阳:沈阳药科大学,2008.
[12]李汝鑫,程锦堂,焦梦娇,等.钩藤叶化学成分研究[J].中草药,2017,48(8):1499-1505.
[13]Bezerra MA,Santelli RE,Oliveira EP,et al.Responsesurface methodology(RSM)as a tool for optimization in analytical chemistry[J].Talanta,2008,76(5):965.
[14]肖娟,孙智达,谢笔钧,等.荷叶生物碱提取工艺响应曲面优化研究[J].食品科学,2009,30(22):157-161.
[15]杨立芳,刘洪存,姜明国,等.响应曲面法优选毛果鱼藤中香豆素类成分提取工艺的研究[J].药物分析杂志,2015,35(3):506-511.
[16]仲耘,冯瑞芝.钩藤及其同属植物生物碱含量的紫外分光、HPLC测定[J].中国药学杂志,1993,24(9):462-46.
[17]杨秀娟,洪燕龙,吴飞,等.HPLC测定钩藤中钩藤碱和异钩藤碱的方法学探究[J].中国中药杂志,2013,38(5):720-724.
[18]王克英,郭思妤,祝晶,等.黔产钩藤药材不同采收期及不同加工方法有效成分含量对比研究[J].中国民族民间医药,2012,21(13):27-28.
[19]于淼,柏云娇,代岐昌,等.响应曲面法优化文殊兰中生物碱的提取工艺[J].中草药,2013,44(10):1286-1289.
[20]张荣,刘睿,刘启德,等.钩藤中钩藤碱、异钩藤碱的提取与含量测定[J].中药新药与临床药理,2009,20(4):338-341.
[21]刘清华,葛尔宁.RP-HPLC法测定钩藤煎剂中钩藤碱含量及变化[J].浙江中医药大学学报,2010,34(2):270-272.
[22]刘卫,杨雪萍,王中师,等.钩藤总碱的热稳定研究[J].药学实践杂志,2011,29(6):442-444.
[23]黄卓谦,刘建利,王玉英,等.钩藤煎煮过程中化学成分变化[J].西北大学学报(自然科学版),2008,38(5):787-789.