用响应面法优化四黄止痢复方中药提取工艺
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摘要
为制备四黄止痢复方中药并建立其高效液相色谱(HPLC)检测方法,在单因素试验的基础上,以浸渍时间、料液比[质量(g)体积(mL)比]、甲醇体积分数为自变量,黄芩苷、盐酸小檗碱质量浓度及干膏率综合评分为因变量,采用HPLC法测定其质量浓度,响应面法进行试验设计、建立数学模型,并进行预测分析。结果显示,四黄止痢复方中药的最佳提取工艺为浸渍时间146 min、料液比1︰333、甲醇体积分数80%。建立的HPLC色谱条件为色谱柱Kromasil C18柱(250 mm×4.6 mm,5 m),流动相甲醇(A)-0.1%磷酸水(B)梯度洗脱,检测波长278 nm,流速1.0 mL/min,进样体积10 L,柱温25℃。结果表明,用响应面法优化的四黄止痢复方中药提取工艺,方法简单,精密度高;所建立的HPLC法可用于四黄止痢复方中药的检测。
The aim was to prepare Sihuangzhili Compound,and to establish a detection method of high performance liquid chromatography(HPLC).On the basis of single-factor experiment,taking extraction time,solid-liquid ratio and methanol concentration as the independent variables,comprehensive score of concentration of baicalin and berberine,dry extract yield as the dependent variables,concentration of Sihuangzhili Compound was determined by HPLC,mathematical model was established by response surface methodology,forecast and analyze.The results showed that optimization of extraction conditions of Sihuangzhili Compound:extraction time146 min,solid-liquid ratio 1 ︰ 333,methanol concentration 80%.HPLC chromatographic conditions:a C18 column(250 mm ×4.6 mm,5 m) with methanol(A)-0.1% phosphoric acid water(B) as mobile phase for gradient elution,detection wavelength was 278 nm,flow rate was 1.0 mL/min,and the column temperature was25 ℃ with injection volume of 10 L.These results suggested that the optimized extraction process of Sihuangzhili Compound by response surface methodology was simple and precise.The determination method can be used for Sihuangzhili Compound test.
The aim was to prepare Sihuangzhili Compound,and to establish a detection method of high performance liquid chromatography(HPLC).On the basis of single-factor experiment,taking extraction time,solid-liquid ratio and methanol concentration as the independent variables,comprehensive score of concentration of baicalin and berberine,dry extract yield as the dependent variables,concentration of Sihuangzhili Compound was determined by HPLC,mathematical model was established by response surface methodology,forecast and analyze.The results showed that optimization of extraction conditions of Sihuangzhili Compound:extraction time146 min,solid-liquid ratio 1 ︰ 333,methanol concentration 80%.HPLC chromatographic conditions:a C18 column(250 mm ×4.6 mm,5 m) with methanol(A)-0.1% phosphoric acid water(B) as mobile phase for gradient elution,detection wavelength was 278 nm,flow rate was 1.0 mL/min,and the column temperature was25 ℃ with injection volume of 10 L.These results suggested that the optimized extraction process of Sihuangzhili Compound by response surface methodology was simple and precise.The determination method can be used for Sihuangzhili Compound test.
引文
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[12]郎利敏,王克领,张力宪,等.中药复方对鸡常见病原菌的体外抗菌试验[J].中兽医学杂志,2014(3):7-10.LANG Li-min,WANG Ke-ling,ZHANG Li-xian,et al.In vitro antibacterial test of traditional Chinese medicine compound on fowl common pathogenic bacteria[J].Chinese Journal of Traditional Veterinary Science,2014(3):7-10.(in Chinese)
[13]王敏,王逢春,郭琪.高效液相色谱法测定半夏泻心口服液中黄芩苷和盐酸小檗碱的含量[J].解放军医药杂志,2013,25(10):76-78.WANG Min,WANG Feng-chun,GUO Qi.Content determination of baicalin and berberine hydrochloride in Banxia Xiexin Oral solution by high performance liquid chromatography[J].Medical&Pharmaceutical Journal of Chinese People’s Liberation Army,2013,25(10):76-78.(in Chinese)
[14]王晖,陈丽,陈垦,等.多指标综合评价方法及权重系数的选择[J].广东药学院学报,2007(5):583-589.WANG Hui,CHEN Li,CHEN Ken,et al.Multi-index comprehensive evaluation method and selection of weight coefficient[J].Journal of Guangdong Pharmaceutical University,2007(5):583-589.(in Chinese)
[15]袁继勇,李炜,葛斌,等.基于层次分析法的中药注射剂安全性评价[J].兰州大学学报(医学版),2012,38(4):23-26.YUAN Ji-yong,LI Wei,GE Bin,et al.Safety evaluation of traditional Chinese medicine injections based on analytical hierarchy process[J].Journal of Lanzhou University(Medical sciences),2012,38(4):23-26.(in Chinese)
[16]陈华.响应面法优化天麻中天麻素提取工艺研究[D].遵义:遵义医学院,2011.CHEN Hua.Optimization of extraction of gastrodin from Rhizoma Gastrodia by response surface methodology[D].Zunyi:Zunyi Medical University,2011.(in Chinese)
[2]熊玥,宋慧敏,贾纪萍,等.四黄止痢颗粒质量标准研究[J].中国兽药杂志,2015,49(6):45-48.XIONG Yue,SONG Hui-min,JIA Ji-ping,et al.Studies on quality standard of Sihuangzhili granules[J].Chinese Journal of Veterinary Drug,2015,49(6):45-48.(in Chinese)
[3]杨志雄,莫志江.RP-HPLC法测定复方金银花颗粒中黄芩苷的含量[J].中国民族民间医药,2010(19):41-42.YANG Zhi-xiong,MO Zhi-jiang.Determination of the contents of scutellarin in Fufang Jinyinhua Keli by HPLC[J].Chinese Journal of Ethnomedicine and Ethnopharmacy,2010(19):41-42.(in Chinese)
[4]国家药典委员会.中华人民共和国药典二〇一五年版:四部[M].北京:中国医药科技出版社,2015:374-376.Chinese Pharmacopoeia Commission.Pharmacopoeia of People’s Republic of China(2015):VolumeⅣ[M].Beijing:China Medical Science Press,2015:374-376.(in Chinese)
[5]任爱农,卢爱玲,田耀洲,等.层次分析法用于中药复方提取工艺的多指标权重研究[J].中国中药杂志,2008(4):372-374.REN Ai-nong,LU Ai-ling,TIAN Yao-zhou,et al.AHP application to study of weighted coefficient on multicriteria optimization of extraction technology about Chinese traditional compound drug[J].China Journal of Chinese Materia Medica,2008(4):372-374.(in Chinese)
[6]石振武,赵敏.运用层次分析法确定指标的权值[J].科技和产业,2008(2):23-25.SHI Zhen-wu,ZHAO Min.Making index proportion on analytical hierarchy process(AHP)method[J].Science Technology and Industry,2008(2):23-25.(in Chinese)
[7]许子竞,黎贵卿,黄丽,等.响应面法优化微波辅助提取滇桂艾纳香多糖工艺研究[J].食品工业科技,2010,31(1):220-223.XU Zi-jing,LI Gui-qing,HUANG Li,et al.Optimization of microwave-assisted extraction technique of Blumea ripaia polysaccharide by response surface methodology[J].Science and Technology of Food Industry,2010,30(1):220-223.(in Chinese)
[8]李春慧,蒲万霞,吴润,等.响应面法对啤酒酵母菌制剂培养条件的优化[J].中国兽医科学,2014,44(10):1095-1100.LI Chun-hui,PU Wan-xia,WU Run,et al.Optimization of culturing condition of Saccharomyces cerevisiae preparation by response surface methodology[J].Chinese Veterinary Science,2014,44(10):1095-1100.(in Chinese)
[9]陈君琛,赖谱富,周学划,等.响应面法优化大球盖菇粗多糖提取工艺[J].食品科学,2012,33(2):139-142.CHEN Jun-chen,LAI Pu-fu,ZHOU Xue-hua,et al.Optimization of extraction process for crude polysaccharides from Stropharia rugoso-annulata by response surface methodology[J].Food Science,2012,33(2):139-142.(in Chinese)
[10]易军鹏,朱文学,马海乐,等.牡丹籽油超声波辅助提取工艺的响应面法优化[J].农业机械学报,2009,40(6):103-110.YI Jun-peng,ZHU Wen-xue,MA Hai-le,et al.Optimization on ultrasonic-assisted extraction technology of oil from Paeonia suffruticosa Andr seeds with response surface analysis[J].Transactions of the Chinese Society for Agricultural Machinery,2009,40(6):103-110.(in Chinese)
[11]丘富安,张建龙,丁育诗,等.车前子黄酮的响应面法优化微波提取及其对鸡抗氧化能力的影响[J].中国兽医科学,2017,47(10):1315-1325.QIU Fu-an,ZHANG Jian-long,DING Yu-shi,et al.Optimization of microwave-assisted extraction of plantain seed flavonoids by response surface method ology and its effects on antioxidant activities in chickens response to oxidative stress[J].Chinese Veterinary Science,2017,47(10):1315-1325.(in Chinese)
[12]郎利敏,王克领,张力宪,等.中药复方对鸡常见病原菌的体外抗菌试验[J].中兽医学杂志,2014(3):7-10.LANG Li-min,WANG Ke-ling,ZHANG Li-xian,et al.In vitro antibacterial test of traditional Chinese medicine compound on fowl common pathogenic bacteria[J].Chinese Journal of Traditional Veterinary Science,2014(3):7-10.(in Chinese)
[13]王敏,王逢春,郭琪.高效液相色谱法测定半夏泻心口服液中黄芩苷和盐酸小檗碱的含量[J].解放军医药杂志,2013,25(10):76-78.WANG Min,WANG Feng-chun,GUO Qi.Content determination of baicalin and berberine hydrochloride in Banxia Xiexin Oral solution by high performance liquid chromatography[J].Medical&Pharmaceutical Journal of Chinese People’s Liberation Army,2013,25(10):76-78.(in Chinese)
[14]王晖,陈丽,陈垦,等.多指标综合评价方法及权重系数的选择[J].广东药学院学报,2007(5):583-589.WANG Hui,CHEN Li,CHEN Ken,et al.Multi-index comprehensive evaluation method and selection of weight coefficient[J].Journal of Guangdong Pharmaceutical University,2007(5):583-589.(in Chinese)
[15]袁继勇,李炜,葛斌,等.基于层次分析法的中药注射剂安全性评价[J].兰州大学学报(医学版),2012,38(4):23-26.YUAN Ji-yong,LI Wei,GE Bin,et al.Safety evaluation of traditional Chinese medicine injections based on analytical hierarchy process[J].Journal of Lanzhou University(Medical sciences),2012,38(4):23-26.(in Chinese)
[16]陈华.响应面法优化天麻中天麻素提取工艺研究[D].遵义:遵义医学院,2011.CHEN Hua.Optimization of extraction of gastrodin from Rhizoma Gastrodia by response surface methodology[D].Zunyi:Zunyi Medical University,2011.(in Chinese)
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