Box-Behnken响应面法优化徐长卿配方颗粒挥发油-β-CD包合物制备工艺
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摘要
为了解决徐长卿挥发油加油难及加入后的稳定性问题,采用Box-Behnken响应面法,优选出徐长卿配方颗粒挥发油-β-CD包合物的制备工艺。在单因素试验的基础上,采用3因素3水平Box-Behnken设计对徐长卿配方颗粒挥发油-β-CD包合工艺进行优选,以挥发油包合率及包合物收率为考察指标,考察挥发油与β-CD比例、包合温度、包合时间对结果的影响。结果表明:优选的包合工艺条件为挥发油与β-CD质量比为1∶8.34,包合温度为50.2℃,包合时间为2.17 h。在此条件下,挥发油包合率为72.19%,包合物收率为75.06%,综合评分为96.41,RSD值为1.1%。优选的包合工艺包合率高,工艺稳定可行,可为配方颗粒挥发油的工业化生产提供数据支持。
In order to solve the problems of refuel difficulty and the stability of volatile oil from Cynanchum paniculatum,the preparation technology is optimized for volatile oil from Cynanchum paniculatum formula granule-β-CD inclusion complex by Box-Behnken design-response surface method. A three-factor and three-level Box-Behnken experimental design is employed to optimize the preparation process of volatile oil from Cynanchum paniculatum formula granule-β-Cyclodextrin inclusion complex on the basis of single factor experiments. With the inclusion ratio of volatile oil and the yield of the inclusion complex as investigate targets,the effect of the ratio of volatile-oil and β-CD,the inclusion temperature and the inclusion time on the result are investigated. The optimal inclusion technologies are as follows: The ratio of volatile oil-β-CD is 1 ∶ 8.34,the inclusion temperature is 50.2 ℃ and the inclusion time is 2.17 h. Underthese conditions,the inclusion ratio is 72.19%,and the yield of the inclusion complex is 75.06%. The composite score is 96.41,and RSD is 1.1%. The optimum inclusion condition is stable and reproducible with a high inclusion yield,providing data support for industrial production of formula granule volatile oil.
In order to solve the problems of refuel difficulty and the stability of volatile oil from Cynanchum paniculatum,the preparation technology is optimized for volatile oil from Cynanchum paniculatum formula granule-β-CD inclusion complex by Box-Behnken design-response surface method. A three-factor and three-level Box-Behnken experimental design is employed to optimize the preparation process of volatile oil from Cynanchum paniculatum formula granule-β-Cyclodextrin inclusion complex on the basis of single factor experiments. With the inclusion ratio of volatile oil and the yield of the inclusion complex as investigate targets,the effect of the ratio of volatile-oil and β-CD,the inclusion temperature and the inclusion time on the result are investigated. The optimal inclusion technologies are as follows: The ratio of volatile oil-β-CD is 1 ∶ 8.34,the inclusion temperature is 50.2 ℃ and the inclusion time is 2.17 h. Underthese conditions,the inclusion ratio is 72.19%,and the yield of the inclusion complex is 75.06%. The composite score is 96.41,and RSD is 1.1%. The optimum inclusion condition is stable and reproducible with a high inclusion yield,providing data support for industrial production of formula granule volatile oil.
引文
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[13]杨欢,詹雪艳,林宏英,等.中药挥发油环糊精包合物研究现状[J].中国中医药信息杂志,2015,22(10):129-133.YANG Huan,ZHAN Xueyan,LIN Hongying,et al.Research status of cyclodextrin inclusion compound of TCM volatile oil[J].Chinese Journal of Information on TCM,2015,22(10):129-133.
[14]冯玉康,王文鹏,郝鹏彬,等.响应曲面法优化银杏叶提取物柱层析精制工艺[J].中国现代中药,2015,17(12):1321-1326.FENG Yukang,WANG Wenpeng,HAO Pengbin,et al.Study on optimization of refining process of column chromatography of Ginkgo Biloba leaves extracts by response surface methodology[J].Modern Chinese Medicine,2015,17(12):1321-1326.
[15]李哲,蔡向杰,李菲,等.Box-Behnken响应面法优化玄麦甘桔含片浸膏真空低温连续干燥工艺[J].现代中药研究与实践,2017,31(5):56-59.LI Zhe,CAI Xiangjie,LI Fei,et al.Optimization of vacuum belt drying process of Xuanmaiganju tablets by Box-Behnken design-response surface methodology[J].Research and Practice on Chinese Medicines,2017,31(5):56-59.
[2]赵超,杨再波,张前军,等.固相微萃取/气相色谱/质谱法分析徐长卿挥发性化学成分[J].贵州大学学报(自然科学版),2007,24(4):407-409.ZHAO Chao,YANG Zaibo,ZHANG Qianjun,et al.Analysis of the essentia oil from Cynanchum paniculatum by SPME/GC/MS[J].Journal of Guizhou University(Natural Sciences),2007,24(4):407-409.
[3]李颖,曾茂贵,郑笈,等.星点设计-效应面法优化鱼腥草挥发油-β-环糊精包合物的制备工艺[J].中草药,2014,45(13):1855-1862.LI Ying,ZENG Maogui,ZHENG Ji,et al.Optimization of preparation of volatile oil from Houttuynie Herba-β-cyclodextrin inclusion complex by central composite design-response surface method[J].Chinese Traditional and Herbal Drugs,2014,45(13):1855-1862.
[4]赵慧,张骥,闫路娜.响应面法优化杏鲍菇粗多糖提取工艺的研究[J].河北科技大学学报,2017,38(1):80-86.ZHAO Hui,ZHANG Ji,YAN Luna.Study on optimization of extraction process of crude polysaccharides from Pleurotuseryngii by response surface method[J].Journal of Hebei University of Science and Technology,2017,38(1):80-86.
[5]姜国志,屈云萍,李哲,等.舒筋通络颗粒矫味剂的筛选与评价[J].西北药学杂志,2017,32(3):337-340.JIANG Guozhi,QU Yunping,LI Zhe,et al.Screening and evaluation of the flavors of Shujintongluo Granules[J].Northwest Pharmaceutical Journal,2017,32(3):337-340.
[6]张芹,钱芳.清肠化湿颗粒中肉桂挥发油的提取及β-环糊精包合工艺研究[J].现代中药研究与实践,2016,30(5):43-45.ZHANG Qin,QIAN Fang.Study on extraction process of volatile oil from cinnamomum cassia and inclusion preparation ofβ-cyclodextrin in Qingchanghuashi granule[J].Research and Practice on Chinese Medicines,2016,30(5):43-45.
[7]屠寒,卢金清,江汉美,等.星点设计-效应面法优化β-环糊精包合薄荷挥发油的工艺[J].中药材,2016,39(11):2579-2581.
[8]屈云萍,李哲,王娇,等.舒筋通络颗粒中乳香挥发油提取及包合工艺研究[J].河北工业科技,2018,35(4):294-298.QU Yunping,LI Zhe,WANG Jiao,et al.Study on extraction and inclusion process of volatile oil from frankincense in Shujintongluo granules[J].Hebei Journal of Industrial Science and Technology,2018,35(4):294-298.
[9]代丽萍,谢小龙,鲁艳清,等.HPLC测定丹芍方提取物中丹皮酚、芍药苷的含量[J].中国实验方剂学杂志,2013,19(17):127-129.DAI Liping,XIE Xiaolong,LU Yanqing,et al.Quantitative determination of Paeonol and Paeoniflorin in extraction of Danshao formula by HPLC[J].Chinese Journal of Experimental Traditional Medical Formulae,2013,19(17):127-129.
[10]周桂清,张楠,孙紫薇,等.HPLC法测定徐长卿根和根茎及地上部分丹皮酚的含量[J].人参研究,2017(6):11-12.ZHOU Guiqing,ZHANG Nan,SUN Ziwei,et al.HPLC was used to determine the content of the root and Rhizomaand the ground part of Paeonol on Cynanchum paniculatum[J].Ginseng Research,2017(6):11-12.
[11]马宏伟,田汝芳,魏爱云.正交试验优选藏药六味大托叶云实散中挥发油的包合工艺[J].中国民族民间医药,2015,24(18):23-24.MA Hongwei,TIAN Rufang,WEI Aiyun.Optimization of the inclusion technology for volatile oil from Liuwei Datuoyeyunshi powder by orthogonal experment[J].Chinese Journal of Ethnomedicine and Ethnopharmacy,2015,24(18):23-24.
[12]汪文来,杨立新,赵红霞.青皮挥发油β-环糊精包合工艺优选[J].中国实验方剂学杂志,2010,16(18):38-40.WANG Wenlai,YANG Lixin,ZHAO Hongxia.Study on optimization forβ-cyclodextrin including technology of volatile oils from pericarpium citri reticulatae viride[J].Chinese Journal of Experimental Traditional Medical Formulae,2010,16(18):38-40.
[13]杨欢,詹雪艳,林宏英,等.中药挥发油环糊精包合物研究现状[J].中国中医药信息杂志,2015,22(10):129-133.YANG Huan,ZHAN Xueyan,LIN Hongying,et al.Research status of cyclodextrin inclusion compound of TCM volatile oil[J].Chinese Journal of Information on TCM,2015,22(10):129-133.
[14]冯玉康,王文鹏,郝鹏彬,等.响应曲面法优化银杏叶提取物柱层析精制工艺[J].中国现代中药,2015,17(12):1321-1326.FENG Yukang,WANG Wenpeng,HAO Pengbin,et al.Study on optimization of refining process of column chromatography of Ginkgo Biloba leaves extracts by response surface methodology[J].Modern Chinese Medicine,2015,17(12):1321-1326.
[15]李哲,蔡向杰,李菲,等.Box-Behnken响应面法优化玄麦甘桔含片浸膏真空低温连续干燥工艺[J].现代中药研究与实践,2017,31(5):56-59.LI Zhe,CAI Xiangjie,LI Fei,et al.Optimization of vacuum belt drying process of Xuanmaiganju tablets by Box-Behnken design-response surface methodology[J].Research and Practice on Chinese Medicines,2017,31(5):56-59.
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