复方山楂提纯液不同工艺的物质转移研究
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摘要
本文以复方山楂提取液为研究对象,运用HPLC法、紫外分光光度法以及HPLC-MS等方法对水提醇沉法和水提离心法各个环节的二苯乙烯苷和总黄酮进行了定量测定和转移率的研究比较,为优化口服液提取工艺和质量控制奠定了基础。主要内容如下:
1、根据所查阅的文献资料,研究传统的水提醇沉法和水提离心法各个环节的转移率,并以HPLC法和紫外分光光度法对各个步骤的二苯乙烯苷和总黄酮含量进行了测定,结果显示,水提醇沉法提取液二苯乙烯苷在水提液经旋蒸水浴45℃浓缩后损失率最大,为22.51%,其次在醇沉液经旋蒸水浴45℃浓缩回收乙醇后,为6.62%,其它环节损失很少;水提醇沉法水提液总黄酮在水提液经加乙醇静置过滤后损失率最大,为23.90%,其次是水提液经旋蒸水浴45℃浓缩后,损失率为12.47%,其它环节损失很少;两法比较,水提离心法制备的口服液中二苯乙烯苷和总黄酮含量分别提高了20.08%、29%。
2、根据实验室前期已完成对复方山楂口服液各成分定性工作的结论,进一步利用液质联用指纹图谱技术对主要药效成分进行了定量研究,与传统检测结果相对比,比较了各化学成分的含量差别,结果显示,两法提取液二苯乙烯苷、总黄酮主要的损失环节和其单成分检测是一致的;指纹图谱检测的二苯乙烯苷和总黄酮含量均小于单成分检测值;两法比较,水提离心法制备的口服液中二苯乙烯苷和总黄酮含量分别提高了22.92%、32.52%。结合生产成本和生产周期的考虑,认为水提离心法是比水提醇沉优化的提取工艺。
Hawthorn extract compound was studied using HPLC method, UVspectrophotometry and HPLC-MS methods, in which all aspects of centrifugationstilbene glycosides and total flavonoids through aqueous alcohol and water extractwere quantitatively determined and transfer rates were compared. The main workfocusedonthefollowingaspects:
1. According to the available literature, the transfer rates of the traditionalaqueous alcohol and centrifugation were studied. And the concentration of stilbeneglucoside and total flavonoids from the different steps was measured by HPLC andUV spectrophotometry. The results showed that aqueous extract alcohol stilbeneglucoside in water extracts by rotary steam condensed in a water bath 45℃is thebiggest loss for the 22.51%, followed by the liquid in the alcohol 45℃water bathrotary steam recycling ethanol concentration, the 6.62%;the other part of the loss issmall; water method alcohol aqueous extract of total flavonoids in the water extractby the increase of ethanol loss rate after holding the largest filter for 23.90%;followed by is the water extract by rotary steam condensed in a water bath 45℃, theloss rate of 12.47%; few other aspects of the loss; centrifugal water Preparation ofOralLiquidstilbeneglycosidesandtotalflavonoidswereincreasedby20.08%,29%.
2. On the basis of the former quality study on the components in the Hawthorncompound oral liquid components, the quantitative research was carried on. And theresults were compared with those of the traditional method. It showed that stilbeneglucoside extract, with a total loss of the main aspects of flavonoids and theirsingle-component testing is consistent; fingerprint detection stilbene glycosides andtotal flavonoids were less than the value of single-component testing; two method,centrifugal water Preparation of Oral Liquid stilbene glycosides and total flavonoidswere increased by22.92% , 32.52%. Combination of production costs and productioncycle of the consideration that the water is more than centrifugation alcohol waterextractionprocessoptimization.
1、根据所查阅的文献资料,研究传统的水提醇沉法和水提离心法各个环节的转移率,并以HPLC法和紫外分光光度法对各个步骤的二苯乙烯苷和总黄酮含量进行了测定,结果显示,水提醇沉法提取液二苯乙烯苷在水提液经旋蒸水浴45℃浓缩后损失率最大,为22.51%,其次在醇沉液经旋蒸水浴45℃浓缩回收乙醇后,为6.62%,其它环节损失很少;水提醇沉法水提液总黄酮在水提液经加乙醇静置过滤后损失率最大,为23.90%,其次是水提液经旋蒸水浴45℃浓缩后,损失率为12.47%,其它环节损失很少;两法比较,水提离心法制备的口服液中二苯乙烯苷和总黄酮含量分别提高了20.08%、29%。
2、根据实验室前期已完成对复方山楂口服液各成分定性工作的结论,进一步利用液质联用指纹图谱技术对主要药效成分进行了定量研究,与传统检测结果相对比,比较了各化学成分的含量差别,结果显示,两法提取液二苯乙烯苷、总黄酮主要的损失环节和其单成分检测是一致的;指纹图谱检测的二苯乙烯苷和总黄酮含量均小于单成分检测值;两法比较,水提离心法制备的口服液中二苯乙烯苷和总黄酮含量分别提高了22.92%、32.52%。结合生产成本和生产周期的考虑,认为水提离心法是比水提醇沉优化的提取工艺。
Hawthorn extract compound was studied using HPLC method, UVspectrophotometry and HPLC-MS methods, in which all aspects of centrifugationstilbene glycosides and total flavonoids through aqueous alcohol and water extractwere quantitatively determined and transfer rates were compared. The main workfocusedonthefollowingaspects:
1. According to the available literature, the transfer rates of the traditionalaqueous alcohol and centrifugation were studied. And the concentration of stilbeneglucoside and total flavonoids from the different steps was measured by HPLC andUV spectrophotometry. The results showed that aqueous extract alcohol stilbeneglucoside in water extracts by rotary steam condensed in a water bath 45℃is thebiggest loss for the 22.51%, followed by the liquid in the alcohol 45℃water bathrotary steam recycling ethanol concentration, the 6.62%;the other part of the loss issmall; water method alcohol aqueous extract of total flavonoids in the water extractby the increase of ethanol loss rate after holding the largest filter for 23.90%;followed by is the water extract by rotary steam condensed in a water bath 45℃, theloss rate of 12.47%; few other aspects of the loss; centrifugal water Preparation ofOralLiquidstilbeneglycosidesandtotalflavonoidswereincreasedby20.08%,29%.
2. On the basis of the former quality study on the components in the Hawthorncompound oral liquid components, the quantitative research was carried on. And theresults were compared with those of the traditional method. It showed that stilbeneglucoside extract, with a total loss of the main aspects of flavonoids and theirsingle-component testing is consistent; fingerprint detection stilbene glycosides andtotal flavonoids were less than the value of single-component testing; two method,centrifugal water Preparation of Oral Liquid stilbene glycosides and total flavonoidswere increased by22.92% , 32.52%. Combination of production costs and productioncycle of the consideration that the water is more than centrifugation alcohol waterextractionprocessoptimization.
引文
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[16]宋萍,李存仁,于军,分光光度法测定藏药鬼箭锦鸡儿中总黄酮的含量,时珍国医国药,2008,19(9):2076~2077
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[21]CMLai,SPLi,ArapidHPLC-ESI-MS/MSforqualitativeandquantitativeanalysisofsaponinsin“XUESETONG”injection,JournalofPharmaceuticalandBiomedicalAnalysis,2006,40:669~678
[22]J Han,M Ye,Analysis of multiple constituents in a Chinese herbal preparationShuang-Huang-Lian oral liquid by HPLC-DAD-ESI-MSn , Journal ofPharmaceuticalandBiomedicalAnalysis,2007,44(2):430~438
[23]康阿龙,GQl05-A型管式分离机在中药口服液生产中的应用,中成药,1999,21(2):94
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[30]宋逍,唐志书,崔春利等,中药复方制剂中黄芩苷转移率影响因素研究,陕西中医,2008,29(6):730~731
[31]董洁,郭立玮,陈丹丹等,0.2μm无机陶瓷膜微滤对黄芩等7种中药主要指标性成分转移率的影响,南京中医药大学学报,2003,19(3):148~149
[32]黄夏敏,彭中芳,邓祝玲,白芍在中成药生产过程中芍药甙含量变化的研究,中药新药与临床药理,1998,9(4):236~237
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[34]薛冬,杨根寿,益心酮片的制备与疗效观察,中成药,1999,21(8):436
[35]李贵海,孙敬勇,张希林,等,山楂降血脂有效成分的实验研究,中草药,2002,33(1):50~53
[36]ZZuo,LZhang,LMZhou,etal,Intestinalabsorptionofhawthornflavonoids-invitro,insituandinvivocorrelationsLifeSciences,2006,79:2455~2462
[37]SLAnna,OJan,WAneta,Antioxidantactivityofthephenoliccompoundsofhawthorn,pineandskullcap,FoodChemistry,2007,103:853~859
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[2]白乐溪,中药质量面临的问题与解决的措施,海峡药学,2003,15(2):102~103
[3]马丽丹,薛东生,探讨制约中药发展及其现代化的因素与策略研究,时珍国医国药,2006,17(12):2610~2612
[4]李忠红,杜冠华,中药质量监控之我见,世界科学技术——中医药现代化,2005,6(6):67~71
[5]韩桂茹,水提醇沉对中药各类有效成分的影响,中国中药杂志,1993,18(2):286~287
[6]史宇翔,苏嫦娥,传统中药新剂型的研究概况,药学研讨,2001,10(5):64
[7]RBauer,Qualitycriteriaandphytopharmaceutical:Canacceptabledrugstandardsbeachieved,DrugInformationJournal,1998,32:101
[8]NLazarowych,Useoffingerprintingandmarkercompoundsforidentificationofbotanicaldrug:StrategiesforapplyingpharmaceuticalHULKanalysistoherbalproducts,DrugInformationJournal,1998,32:497
[9]丰加涛,金郁,王金成等,基于定量指纹图谱技术的中药质量控制,色谱,2008,3:180~185
[10]李云梅,中药复方制剂工艺分离纯化技术的现状与展望,农垦医学,2001,23(5):341~343
[11]刘春海,李跃辉,杨永华,离心技术在中药研究中的应用,中成药,2004,26(1):68~70
[12]孔德营,刘力,指纹图谱技术及其在中药质量鉴定中的应用,吉林畜牧兽医,2007(1):12~14
[13]郑燕鹏,段春改,运用高新技术为中药搭建“腾飞台”,中国医药报,2006,4:8
[14]孙彩华,指纹图谱在中药研究领域的应用,中国药业,2006,15(17):25~27
[15]李亚林,张浩,HPLC法测定何首乌中二苯乙烯苷的含量,内蒙古中医药,2007,26(12):24~25
[16]宋萍,李存仁,于军,分光光度法测定藏药鬼箭锦鸡儿中总黄酮的含量,时珍国医国药,2008,19(9):2076~2077
[17]严启新,李萍,王迪,鸡血藤脂溶性化学成分的研究,中国医科大学学报,2001,32(5):6
[18]卢闻,贺浪冲,杨广德等,白川降压胶囊HPLC指纹图谱定性与定量分析方法研究,中国中药杂志,2006,31(23):64~65
[19]李亦蕾,晏媛,谈亚非等,复方蒲公英灌肠液指纹图谱定性和有效成分定量分析方法研究,南方医科大学学报,2006,26(10):1503~1505
[20]施超欧,陶萍,丹参注射液主要成分的HPLC及LC-MS定性分析,世界科学技术-中药现代化,2001,3(5):50~52
[21]CMLai,SPLi,ArapidHPLC-ESI-MS/MSforqualitativeandquantitativeanalysisofsaponinsin“XUESETONG”injection,JournalofPharmaceuticalandBiomedicalAnalysis,2006,40:669~678
[22]J Han,M Ye,Analysis of multiple constituents in a Chinese herbal preparationShuang-Huang-Lian oral liquid by HPLC-DAD-ESI-MSn , Journal ofPharmaceuticalandBiomedicalAnalysis,2007,44(2):430~438
[23]康阿龙,GQl05-A型管式分离机在中药口服液生产中的应用,中成药,1999,21(2):94
[24]张超,壮腰健肾口服液制剂工艺研究,中药材,1997,20(8):409
[25]谢秀娟,高速离心法与水醇法制备清热解毒口服液的比较研究,中成药,1997,17(8):3
[26]孙红月,低温离心法制备生脉口服液的工艺优选,中国中药杂志,1999,24(3):156~157
[27]奉建芳,罗杰英,高速离心法制备归脾口服液工作条件选择,中成药,1997,19(1):1~2
[28]娄如菊,中成药生产中离心薄膜浓缩技术的初步研究,中成药,1993,15(1):4~5
[29]刘春海,李跃辉,杨永华,离心技术在中药研究中的应用,中成药,2004,26(1):68~70
[30]宋逍,唐志书,崔春利等,中药复方制剂中黄芩苷转移率影响因素研究,陕西中医,2008,29(6):730~731
[31]董洁,郭立玮,陈丹丹等,0.2μm无机陶瓷膜微滤对黄芩等7种中药主要指标性成分转移率的影响,南京中医药大学学报,2003,19(3):148~149
[32]黄夏敏,彭中芳,邓祝玲,白芍在中成药生产过程中芍药甙含量变化的研究,中药新药与临床药理,1998,9(4):236~237
[33]徐承水,王文房,何首乌提取物对大鼠血脂水平的影响,曲阜师范大学学报,2004,30(3):5~86
[34]薛冬,杨根寿,益心酮片的制备与疗效观察,中成药,1999,21(8):436
[35]李贵海,孙敬勇,张希林,等,山楂降血脂有效成分的实验研究,中草药,2002,33(1):50~53
[36]ZZuo,LZhang,LMZhou,etal,Intestinalabsorptionofhawthornflavonoids-invitro,insituandinvivocorrelationsLifeSciences,2006,79:2455~2462
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