延胡索中生物碱类化合物的分离纯化及指纹图谱研究
|
摘要
本文以延胡索中生物碱类化合物为模式物,针对延胡索有效成分延胡索乙素传统生产工艺存在收率低、能耗高、耗时长、质量控制不稳定等问题,提出了提取—层析分离—高速逆流色谱快速纯化的延胡索乙素生产新工艺,并建立了基于数字化指纹图谱技术评价元胡止痛片的质量控制标准,要点如下:
在提取过程中,考察了提取工艺的主要参数,建立了适合不同分离纯化要求的延胡索提取工艺;在层析分离过程中,通过静态吸附和动态吸附相关参数对离子交换树脂进行优化,筛选出适合于延胡索分离的D152树脂。在优化的条件下,延胡索乙素的纯度从原料中峰面积百分比的4.11%提高到21.13%,收率为65.50%,相比于液液萃取及沉淀法分离延胡索乙素,离子交换树脂分离法具有收率高、处理能力大、操作简便和再生利用容易等优点;粗制样品通过高速逆流色谱一步分离获得高纯度延胡索乙素。由于在高速逆流色谱中溶剂体系的筛选占了90%以上的工作量,本文提出了一种新概念,建立了新方法(平均极性~(P′)),这种新的溶剂体系筛选方法,可以一步从上百种溶剂体系中中筛选到几种合适的溶剂体系,极大地缩短了工作量,提高了工作效率,有利于高速逆流技术的推广。上机实验对新方法进行了验证,采用正已烷:乙酸乙酯:甲醇:水(4-6-5-5)一步分离成功延胡索乙素,纯度为92.7%,回收率达到95.1%。
根据美国FDA、WHO、欧洲药典以及国家药品监督管理局的要求,草药制剂生产商提供原料、半成品及成品的指纹图谱以保证其品种的真实性和批次间质量的稳定性。本文建立了一种适合于含生物碱化合物指纹图谱分析的流动相,并对原理进行了讨论。通过改变流动相的梯度建立了两种以生物碱类化合物为指标物的中成药高效液相指纹图谱,进一步以相对保留时间作为定性依据,相对峰面积作为定量依据,以及特征指纹总差异率和重叠率等构建了高效液相色谱数字化指纹谱,消除了操作过程中各种操作因素的影响,有效地降低了色谱保留值的波动性,使不同样品之间可以进行量化比较;绘制了特征指纹曲线,直观表现了不同样品之间的近似程度;以图像式指纹图谱和数字化指纹谱评价了不同厂家的元胡止痛片和黄连上清丸,对各样的质量差异进行了定量的鉴别,对产生差异的原因也作了初步剖析。不同厂家和批次药品的质量进行对比,其差异分明,可供应用时参考。该分离纯化及质量控制方法可推广应用于其他中草药及天然产物的研究。
This paper took alkaloids of Corydalis yahusuo W.T.Wang(C.yanhusuo) as the research mode.According to the problems need to be solved in separation and quality control of alkaloids,we developed a new process for producing alkloids with high purity using ion-exchange resins separation and high-speed counter-current chromatography(HSCCC) purification.Furthermore,the digitized fingerprints were constructed for quality control of alkaloids-containing products.The main results are listed as follows:
After examined the extraction methods of C.yanhusuo,ion-exchanger resin D152 was selected for dl-tetrahydropalmatine(dl-THP) separation from crude extract of C.yanhusuo. Under the optimized sorption-desorption conditions,the area percent of dl-THP in crude extreact increased from 4.11%to 21.13%with a recovery of 65.50%using D152 packed column.Compared with liquid/liquid extraction and deposition method,ion-exchange resin showed obvious advantages of high recovery,high treatment capability,easy operation and easy regeneration.In the high-speed counter-current chromatography(HSCCC) technique, solvent screening took over 90%work time.We established a fast solvent screening method named average polarity(p').Using the new method,a HSCCC separation was further constructed to purify dl-THP with n-hexane-ethyl acetate-methanol-water(4:6:5:5,v/v) as solvent systems,and the purity of dl-THP reached 92.7%with a recovery of 95.1%after one run HSCCC purification.
Fingerprint becomes a popular and authoritative method for the quality control of natureal product,which was recommended by authorities including SFDA,FDA,WHO and the European Agency.A HPLC fingerprint has been developed for the purpose of quality control of TCM product.In order to eliminate the effect of operation and reduce the fluctuation of chromatography information,a digitized fingerprint was further constructed using RRT as nature determination criterion,RPA as quantification criterion,n main peaks, difference ratio,superpose ratio and correlation coefficient as parameters,and character curve was plotted to show visual representation the similarity of different sample.This technique was expected to apply to the fingerprinting research of other natureal products.
在提取过程中,考察了提取工艺的主要参数,建立了适合不同分离纯化要求的延胡索提取工艺;在层析分离过程中,通过静态吸附和动态吸附相关参数对离子交换树脂进行优化,筛选出适合于延胡索分离的D152树脂。在优化的条件下,延胡索乙素的纯度从原料中峰面积百分比的4.11%提高到21.13%,收率为65.50%,相比于液液萃取及沉淀法分离延胡索乙素,离子交换树脂分离法具有收率高、处理能力大、操作简便和再生利用容易等优点;粗制样品通过高速逆流色谱一步分离获得高纯度延胡索乙素。由于在高速逆流色谱中溶剂体系的筛选占了90%以上的工作量,本文提出了一种新概念,建立了新方法(平均极性~(P′)),这种新的溶剂体系筛选方法,可以一步从上百种溶剂体系中中筛选到几种合适的溶剂体系,极大地缩短了工作量,提高了工作效率,有利于高速逆流技术的推广。上机实验对新方法进行了验证,采用正已烷:乙酸乙酯:甲醇:水(4-6-5-5)一步分离成功延胡索乙素,纯度为92.7%,回收率达到95.1%。
根据美国FDA、WHO、欧洲药典以及国家药品监督管理局的要求,草药制剂生产商提供原料、半成品及成品的指纹图谱以保证其品种的真实性和批次间质量的稳定性。本文建立了一种适合于含生物碱化合物指纹图谱分析的流动相,并对原理进行了讨论。通过改变流动相的梯度建立了两种以生物碱类化合物为指标物的中成药高效液相指纹图谱,进一步以相对保留时间作为定性依据,相对峰面积作为定量依据,以及特征指纹总差异率和重叠率等构建了高效液相色谱数字化指纹谱,消除了操作过程中各种操作因素的影响,有效地降低了色谱保留值的波动性,使不同样品之间可以进行量化比较;绘制了特征指纹曲线,直观表现了不同样品之间的近似程度;以图像式指纹图谱和数字化指纹谱评价了不同厂家的元胡止痛片和黄连上清丸,对各样的质量差异进行了定量的鉴别,对产生差异的原因也作了初步剖析。不同厂家和批次药品的质量进行对比,其差异分明,可供应用时参考。该分离纯化及质量控制方法可推广应用于其他中草药及天然产物的研究。
This paper took alkaloids of Corydalis yahusuo W.T.Wang(C.yanhusuo) as the research mode.According to the problems need to be solved in separation and quality control of alkaloids,we developed a new process for producing alkloids with high purity using ion-exchange resins separation and high-speed counter-current chromatography(HSCCC) purification.Furthermore,the digitized fingerprints were constructed for quality control of alkaloids-containing products.The main results are listed as follows:
After examined the extraction methods of C.yanhusuo,ion-exchanger resin D152 was selected for dl-tetrahydropalmatine(dl-THP) separation from crude extract of C.yanhusuo. Under the optimized sorption-desorption conditions,the area percent of dl-THP in crude extreact increased from 4.11%to 21.13%with a recovery of 65.50%using D152 packed column.Compared with liquid/liquid extraction and deposition method,ion-exchange resin showed obvious advantages of high recovery,high treatment capability,easy operation and easy regeneration.In the high-speed counter-current chromatography(HSCCC) technique, solvent screening took over 90%work time.We established a fast solvent screening method named average polarity(p').Using the new method,a HSCCC separation was further constructed to purify dl-THP with n-hexane-ethyl acetate-methanol-water(4:6:5:5,v/v) as solvent systems,and the purity of dl-THP reached 92.7%with a recovery of 95.1%after one run HSCCC purification.
Fingerprint becomes a popular and authoritative method for the quality control of natureal product,which was recommended by authorities including SFDA,FDA,WHO and the European Agency.A HPLC fingerprint has been developed for the purpose of quality control of TCM product.In order to eliminate the effect of operation and reduce the fluctuation of chromatography information,a digitized fingerprint was further constructed using RRT as nature determination criterion,RPA as quantification criterion,n main peaks, difference ratio,superpose ratio and correlation coefficient as parameters,and character curve was plotted to show visual representation the similarity of different sample.This technique was expected to apply to the fingerprinting research of other natureal products.
引文
[1]陈友梅.中药化学.济南:山东科学技术出版社,1988.
[2]肖崇厚.中药化学.上海:上海科学技术出版社,1997.
[3]王宪楷,赵同芳.千金藤属植物中的生物碱.华西药学杂志,1990,5(2):87-93.
[4]周军,李德兴.左旋四氢巴马汀及其同类物的心血管药理作用.中国药理学通报,1992,8(4):253-256.
[5]钟平,杨任民.中药川芎嗪治疗急性脑缺血机理的实验研究.实用全科医学,2003,1(1):19-20.
[6]洪山海,马广恩.石蒜科生物碱的研究Ⅱ紫花石蒜和其他两种石蒜中的生物碱及新生物碱紫花石蒜碱.药学学报,1964,11(1):1-14.
[7]张兰珍,李家实等.苦豆子种子生物碱成分研究[J].中国中药杂志,1997,22(12):740-743
[8]赵博光.苦豆草生物碱的研究.药学学报,2004,15(3):23-28.
[9]郑洪艳,徐为人.小檗碱药理作用研究进展.中草药,2004,35(6):708-711.
[10]张群英,贺广远.四氢小檗碱抗心律失常作用及其机理探讨.江苏医药,1993,19(3):138-140.
[11]陈祝霞.中药降压的研究进展.中医药信息,2000,4:20-21.
[12]贺道华,马廉亭.罂粟碱,尼莫同治疗脑血管痉挛的疗效比较.暨南大学学报,2000,21(1):105-108.
[13]骆顺安,王晓贤.山莨菪碱舌下给药治疗急性痉挛性腹痛100例.新药与临床,1996,15(3):176-176.
[14]王丽平.包公藤甲素及其类似物的缩瞳活性.中草药,1992,23(4):205-208.
[15]李十中,王淀佐,亭晓岩.中药研究与开发现代化探讨.中草药,2001,32(5):385-387.
[16]Elena E,Stashenko,Ricardo A et al.High-resolution gas-chromatographic analysis of the secondary metabolites obtained by subcritical-fluid extraction from Colombian rue (Ruta graveolens L.).Journal of Biochemical and Biophysical Methods,2000,43(1):379-390.
[17]赵宋亮,陶春元,吴海英.超临界萃取技术在生物碱提取中的研究新进展.江西化工,2008(3):1-4.
[18]李化.超声技术在中草药成分提取中的应用.中药材,2001,24(4):299-300.
[19]蒲含林,郑元升,麻建军.超声法提取金鸡纳生物碱的工艺,暨南大学学报:自然科学与医学版,2008(3):329-330.
[20]范华均,栾伟,李攻科.微波辅助提取/HPLC分析石蒜中的生物碱.分析测试学报,2006,25(3):27-30.
[21]鲁传华,何平笙.麻黄及黄连生物碱膜提取方法的研究.中成药,2002,24(4):251-254.
[22]秦学功,元英进.苦豆子种子中生物碱的冷浸提取实验研究.中草药,2001,(32)7:604-606.
[23]刘颖,张燕玲,王雁.从天然植物龙葵中提取生物碱的工艺研究.辽宁丝绸,2003(2):4-5.
[24]王玉芹,李晓静,法洋.峨眉千里光生物碱乙醇提取工艺研究.中成药,2004,16(10):002-003.
[25]龙德清,饶贞学,丁宗庆.酸性醇浸渍法提取魔芋中的总生物碱.2003,24(10):126-127.
[26]迟玉明,赵唏瑛,吉泽丰吉等.角蒿总生物碱提取工艺的研究.天然产物研究与开发,2005,17(4):475-477.
[27]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(2):41-42.
[28]陈永刚,林励.魏燕华等超声波提取法与索氏提取法提取化橘红柚皮苷的比较研究中药新药与临床药理,2008(4):309-311.
[29]甄攀,杨风珍.吴茱萸总生物碱提取条件的考察.中国中药杂志,2000,(8):504-505.
[30]冷薇.超声提取技术的新探索,中国现代实用医学杂志,2006(5):43-45.
[31]陈志慧,周家容.不同提取方法对断肠草总生物碱提取率的影响.2007,46(3):176-177.
[32]王洪新,王键.苦豆子种子生物碱离子交换分离的因素研究.中草药,2002,33(12):1080-1083.
[33]周先礼,陈东林,王锋鹏.三小叶翠雀花中生物碱成分的研究.华西药学杂志,2005,20(1):1-3.
[34]李义平,杨广德,贺浪冲.红毛七总生物碱提取工艺研究.中药材,2007,30(2):220-223.
[35]刘逆夫,李瑞明.阳离子树脂纯化苦参生物碱的工艺研究.中国中医药现代远程教育,2006,4(12):22-24.
[36]廖小雪,查丽杭,刘骁等.吸附层析分离麻黄生物碱的过程优化.天然产物研究与开发,2004,16(4):281-285.
[37]迟玉明,赵唏瑛,吉泽丰吉.离子交换树脂用于角蒿总生物碱的纯化研究.天然产物研究与开发,2005,17(5):617-621.
[38]霍务贞,李苑新,姜红宇.阳离子交换树脂纯化喘平复方总生物碱的工艺研究.中药新药与临床药理,2005,16(6):446-449.
[39]顾铭,欧阳藩,苏志国.高速逆流色谱法分离纯化丹参并尝试制订中药指纹图谱.生物工程学报,2003,19(6):740-744.
[40]谭龙泉,张所明,欧庆瑜.薄层色谱在高速逆流色谱溶剂系统选择过程中的应用.分析化学,1996,24(12):1448-1451.
[41]袁黎明,傅若农,张天佑等.高速逆流色谱分离苦参中的总生物碱.北京理工大学学报,1997,17(2):244-247.
[42]谭龙泉,阮宗琴,欧庆瑜.高效毛细管电泳在高速逆流色谱的溶剂系统选择过程的应用.分析化学,1997,25(5):515-518.
[43]蔡定国,顾明娟,张吉德等.高速逆流层析分离中药苦参和洋金花总碱.中成药,1990,12(6):32-33.
[44]蔡定国,顾明娟,金涛.应用高速逆流层析分离峨眉千里光生物碱.中国中药杂志,1992,17(10):616-618.
[45]蔡定国,顾明娟,张吉德等.应用高速逆流层析仪分离三杉总碱的主要成分.中国医药工业杂志,1991,22(2):72-73.
[46]袁黎明,吴平,夏滔等.高速逆流色谱制备分离中药黄柏中的生物碱.色谱,2002,20(2):185-186.
[47]Liu Z L,Jin Y,Shen P N et al.Separation and purification of verticine and verticinone from Bulbus Fritillariae Thunbergii by high-speed counter-current chromatography coupled with evaporative light scattering detection.Talanta,2007,71(5):1873-1876
[48]饶畅,刘欣,张佩玲等.高速逆流色谱在天然产物分离中的应用-紫杉烷类二萜及二萜生物碱的制备分离.药学学报,1991,26(7):510-514.
[49]Li H B,Chen F.Preparative isolation and purification of chuanxiongzine from the medicinal plant Ligusticum chuanxiong by high-speed counter-current chromatography.Journal of Chromatography A,2004,1047(2):249-253.
[50]Wang X,Geng Y L,Li F W,et al.Large-scale separation of alkaloids from Corydalis decumbens by pH-zone-refining counter-current chromatography.Journal of Chromatography A,2006,1115(1-2):267-270.
[51]甘师俊,李振吉,邹健强.中药现代化发展战略.北京:科学技术文献出版社,1998.
[52]FDA Guidance for Industry-Botanical Drug Products(Draft Guidance).US Food and Drug Administration,Rockville,2000:18-22.
[53]Note for Guidance on Quality of Herbal Medicinal Products.European Medicines Agency,London,2001.
[54]科技部,国家计委,国家经贸委,卫生部,药品监管局,知识产权局,中医药局和中科院.药现代化发展纲要,2002.
[55]任德权.中药指纹图谱质控技术的意义与作用.中药材,2001,24(4):235-239.
[56]苏薇薇,吴忠,全健.中药指纹图谱的构建及计算机解析.中药材,2001,24(4):295-298.
[57]周玉新,雷海明,徐永红等.中药指纹图谱研究技术.北京:化学工业出版社,2002.
[58]梁逸曾.浅议中药色谱指纹图谱的意义、作用及可操作性.中药新药与临床药理,2001,5(12):196-200.
[59]周玉新,雷海明,徐永红等.中药指纹图谱研究技术.北京:化学工业出版社,2002.
[60]Snyder L R,Kirkland J J,Glajch J L.实用高效液相色谱法的建立(第二版).北京:华文出版社,2001.
[61]王俊德.高效液相色谱法.北京:石油化工出版社,1992.
[62]郑荣庆,李光秀.高效液相色谱法及其在中药研究中的应用.中草药,1993,24(5):265-268.
[63]Chen S B,Liu H P,Tian R T.High-performance thin-layer chromatographic fingerprints of isoflavonoids for distinguishing between Radix Puerariae Lobate and Radix Puerariae Thomsonii.Journal of Chromatography A,2006,1121(1):114-119.
[64]Yan S K,Xin W F,Luo G A.An approach to develop two-dimensional fingerprint for the quality control of Qingkailing injection by high-performance liquid chromatography with diode array detection.Journal of Chromatography A,2005,1090 (1-2):90-97.
[65]Gu M,Ouyang F,Su Z G.Comparison of high-speed counter-current chromatography and high-performance liquid chromatography on fingerprinting of Chinese traditional medicine.Journal of Chromatography A,2004,1022(1-2):139-144.
[66]Lu H M,Liang Y Z,Chen S.Identification and quality assessment of Houttuynia cordata injection using GC-MS fingerprint:A standardization approach.Journal of Ethnopharmacology,2006,105 (3):436-440.
[67]Yu K,Gong Y F,Lin Z Y.Quantitative analysis and chromatographic fingerprinting for the quality evaluation of Scutellaria baicalensis Georgi using capillary electrophoresis.Journal of Pharmaceutical and Biomedical Analysis,2006.
[68]Laura M B,Betty A L,Dan L B.Characterisation of phenolics by LC-UV/Vis,LC-MS/MS and sugars by GC in Melicoccus bi jugatus Jacq.‘Montgomery’ fruits,Food Chemistry,2008,111(4):1017-1024
[69]Sebnem G,Aysegul C G,Feride S.Use of Fourier transform infrared spectroscopy for rapid comparative analysis of Bacillus and Micrococcus isolates,Food Chemistry,2009,113(4):1301-1307
[70]Alonso-Salces R M,H(?)berger K,Holland M V,Multivariate analysis of NMR fingerprint of the unsaponifiable fraction of virgin olive oils for authentication purposes,Food Chemistry,2008
[71]Avula B,Wang Y H,Pawar R S,A rapid method for chemical fingerprint analysis of Hoodia species,related genera,and dietary supplements using UPLC-UV-MS,Journal of Pharmaceutical and Biomedical Analysis,2008,48(3) 722-731.
[72]聂晶,颂九,王国荣．中药指纹图谱的研究现状．中草药,2000,31(12)：881-884．
[73]Yu R M,Ye B,Yan C Y.Fingerprint analysis of fruiting bodies of cultured Cordyceps militaris by high-performance liquid chromatography-photodiode array detection,Journal of Pharmaceutical and Biomedical Analysis.2007,44(3):818-823.
[74]Chen C,Zhang H,Xiao W et al.High-performance liquid chromatographic fingerprint analysis for different origins of sea buckthorn berries.Journal of Chromatography A,2007,1154(1-2):250-259.
[75]Yi L Z,Yuan D L,Liang Y Z.Quality control and discrimination of Pericarpium Citri Reticulatae and Pericarpium Citri Reticulatae Viride based on high-performance liquid chromatographic fingerprints and multivariate statistical analysis.Analytica Chimica Acta,2007,588(2):207-215.
[76]Ma L J,Zhang X Z,Zhang H P.Development of a fingerprint of Salvia miltiorrhiza Bunge by high-performance liquid chromatography with a coulometric electrode array system.Journal of Chromatography B,2007,846(1-2):139-146.
[77]国家药典委员会.中华人民共和国药典.2005年版,一部[M],北京:人民卫生出版社,2005:94.
[78]奚镜清,金联城,忻纳新等.中药材延胡索的品种整理及文献考证.现代应用药学,1995,12(4):12-15.
[79]金正均,王永铭,苏定冯.药理学进展.北京:科学出版社,1999,64-73.
[80]Hidehikok,Neko,Shunsuke N.Studies on the Constituents of Corydalis sp.Ⅵ.Alkaloids from Chinese Corydalis and the Identity of d-Corydalmine with d-Corybulbine.1969,3(9) 2803-2804.
[81]刘俊红,魏峻峰,王洪志等.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.
[82]马家骅,杨明,许润春等.醋延胡索炮制工艺的研究.中草药,2005,36(11):1657-1659.
[83]李银林.影响延胡索疗效因素的分析.河南中医学院学报,2005,3(2):76-77.
[84]南京药学院《中草药》编写组.《中草药学》(中册).江苏人民出版社,1976.
[85]金国章.延胡索乙素的药理研究ⅩⅢ:延胡索乙素对动物成瘾性的实验,生理学报,1978,30(1):67-72.
[86]吕清文,丛雅勤.延胡索药理作用及临床应用浅议.内蒙古中医药:26-27.
[87]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.
[88]周瑞,陆兔林.延胡索的提取工艺优选.时珍国医国药,2003,14(11):662-663.
[89]邱蓉丽,李祥,陈建伟等.延胡索总碱提取方法研究.中医药研究,2000,16(5):50-51.
[90]谢彩娟,张志琪.超声提取延胡索总生物碱的研究.西北药学杂志,2005,20(4):153-154.
[91]范斌,刘泓,杨亚莉.HPLC法测定延胡索药材中季胺型生物碱的含量.中国中医基础医学杂志,2006,12(1):59-60.
[92]姜舜尧.高效液相色谱法测定元胡止痛片中脱氢延胡索碱的含量.中国中药杂志,2000,25(8):479-480.
[93]Cheng Z H,Guo Y L,Wang H Y,et al.Qualitative and quantitative analysis of quaternary ammonium alkaloids from Rhizoma Corydalis by matrix-assisted laser desorption/ionization Fourier transform mass spectrometry coupled with a selective precipitation reaction using Reinecke salt.Analytica Chimica Acta,2006,555(2):269-277.
[94]程志红,陈国强,王昊阳等.延胡索中季铵生物碱的高分辨基质辅助激光解吸电离质谱研究.2004,2(2):99-102.
[95]陈洪燕,万明,孙金霞.均匀设计延胡索提取工艺的研究.湖北中医杂志,2006,28(7):54-55.
[96]黄山,陈峰,郭立伟.延胡索提取工艺的优选.中国中医药信息杂志,2006,13(1):47-48.
[97]涂文升.用不同溶剂、不同提取方法测定金不换中延胡索乙素的含量.广西医科大学学报,2006,23(1):105-106.
[98]廖维,夏新华.延胡索提取工艺的研究.中成药,2004,26(10):6-8.
[99]房方,丁选胜.延胡索药材中延胡索乙素的含量测定.现代中药研究与实践,2005,19(1):54-56.
[100]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):47-48.
[101]陈峰,郭立伟,井山林等.超临界C02流体萃取延胡索中延胡索乙素的正交试验研究.中药新药与临床药理,2005,16(2):137-138.
[102]刘龙忠.优选延胡索生物碱提取工艺.遵义医学院学报,2004,27(6):595-596.
[103]龚青,周蒂,王碧娟.HPLC法测定延胡索乙素的含量.中国现代应用药学杂志,2000,17(4):315-317.
[104]马临科.高效液相色谱法测定延胡索中延胡索乙素的含量.药学实践杂志,2003,21(6):351-353.
[105]方东军,赵润琴,张鹏.HPLC法测定安胃片中延胡索乙素的含量.中医药学报,2004,32(5):36-37.
[106]石上梅,高天兵,田金.HPLC法测定消痛片中延胡索乙素的含量.中国药事,2003,17(1):42-43.
[107]顾秀琰.RP-HPLC测定元胡止痛丸中延胡索乙素的含量.2006,28(4):606-608.
[108]方强,陈晓龙,陈彬.反相高效液相色谱法测定安胃片中有过延胡索乙素的含量.2006,25(8):827-828.
[109]Ou J J,Kong L,Pan C S et al.Determination of Dl-tetrahydropalmatine in Corydalis yanhusuo by L-tetrhydropalmatine inprinted monolithic column coupling with reversed-phase high performance liquid chromatography.Journal of Chromatography A,2006,1117(1):163-169.
[110]方子季,徐霞,王春燕.高效液相色谱法测定良参胃安片中延胡索乙素的含量.解放军药学学报,2006,22(3):222-223.
[111]王慕邹.常用中草药高效液相色谱分析.北京:科学出版社,1999,139-146.
[112]俞雁,金艳,徐超.应用高速逆流色谱技术从延胡索中分离制备延胡索乙素.世界科学技术-中医药现代化,2006,8(2):17-19.
[113]王海燕,穆惠军.元胡止痛片提取工艺研究.山东中医杂志,2002,21(12):739-740.
[114]Ito Y.Golden rules and pitfalls in selecting optimum conditions for high-speed counter-current chromatography.Journal of Chromatography A,2005,1065(2):145-168.
[115]江和源,程启坤,杜琪珍.高速逆流色谱法分离纯化茶黄素.天然产物研究和开发,2000,12(4):30-35.
[116]缪平,蔡定国.分析型逆流色谱的应用.中国重要杂志,1995,20(9):569-670.
[117]Gu M,Wang XL,Su Z G et al.One-step separation and purification of 3,4-dihydroxy phenylactic acid,salvianolic acid B and protocatechualdehyde from Salvia miltiorrhiza Bunge by high-speed counter-current chromatography.Journal of Chromatography A,2007,1140(1-2):107-111.
[118]Li H B,Chen F.Preparative isolation and purification of phillyrin from the medicinal plant Forsythia suspensa by high-speed counter-current chromatography.Journal of Chromatography A,2005,1083(1-2):102-105.
[119]Gao M,Gu M,Liu C Z.Two-step purification of scutellarin from Erigeron breviscapus (vant.)Hand.Mazz.by high-speed counter-current chromatography.Journal of Chromatography B,2006,838(2):139-143.
[120]Peng J Y,Jiang Y Y,Fan G R et al.Optimization suitable conditions for preparative isolation and separation of curculigoside and curculigoside B from Curculigo orchioides by high-speed counter-current chromatography.Separation and Purification Technology,2006,52(1):22-28.
[121]Yu Y,Jin Y,Cu C et al.Separation and Preparation of dl-tetrahydropalmatine from Crude Extract of Corydalis Yanhusuo W.T.Wang by High-speed Countercurrent Chromatography Technology.World science and technology-modernization of traditional Chinese medicine and materia medica,2006,8(2):17-19.
[122]曹学丽．高速逆流色谱分离技术及应用．化学工业出版社,北京,2005,40-41．
[123]Ito Y.Golden rules and pitfalls in selecting optimum conditions for high-speed counter-current chromatography.Journal of Chromatography A,2005,1065(2):145-168.
[124]Tong S Q,Yan J Z,Lou J Z.Preparative isolation and purification of alkaloids from Corydalis yanhusuo W.T.Wang by high speed counter-current chromatography.Journal of Liquid Chromatography and Related Technologies,2005,28(18) 2979-2989.
[125]Liu ZL,JinY,ShenPNetal.Separation and purification of verticine and verticinone from Bulbus Fritillariae Thunbergii by high-speed counter-current chromatography coupled with evaporative light scattering detection.Talanta,2007,71(5):1873-1876.
[126]FDA Guidance for Industry-Botanical Drug Products (Draft Guidance).US Food and Drug Administration.Rockville,2000:18-22.
[127]Note for Guidance on Quality of Herbal Medicinal Products.European Medicines Agency.London,2001.
[128]Committee of National Pharmacopoeia.In:Pharmacopoeia of P.R.China,Press of Chemical Industry,Beijing,2005.
[129]Wang M Z.HPLC Analysis of Some Common Chinese Traditional Medicine.Beijing:Science Press,2000:139～146.
[130]周元瑶,李芳.用反向高效液相色谱法考察盐酸黄连素的质量,药物分析杂志,1984,4(3):131-133.
[131]袁久荣,魏英勤,袁浩等.RP-HPLC法同时测定黄连中四种原小檗碱型生物碱的含量.世界科学技术-中医药现代化2006,8(6):36-39.
[132]Tetsuo M,Kazuhiko S,Mitsuharu O et al.Simultaneous determnation of berberine,palmatine and coptisine in crude drugs and oriental pharmaceutical preparation by ion-pair high-performance liquid chromatography.ChemPharm Bull,1987,30(1):354-357.
[133]洪筱坤,王智华.中药数字化色谱指纹谱.上海:上海科学技术出版社,2003.
[2]肖崇厚.中药化学.上海:上海科学技术出版社,1997.
[3]王宪楷,赵同芳.千金藤属植物中的生物碱.华西药学杂志,1990,5(2):87-93.
[4]周军,李德兴.左旋四氢巴马汀及其同类物的心血管药理作用.中国药理学通报,1992,8(4):253-256.
[5]钟平,杨任民.中药川芎嗪治疗急性脑缺血机理的实验研究.实用全科医学,2003,1(1):19-20.
[6]洪山海,马广恩.石蒜科生物碱的研究Ⅱ紫花石蒜和其他两种石蒜中的生物碱及新生物碱紫花石蒜碱.药学学报,1964,11(1):1-14.
[7]张兰珍,李家实等.苦豆子种子生物碱成分研究[J].中国中药杂志,1997,22(12):740-743
[8]赵博光.苦豆草生物碱的研究.药学学报,2004,15(3):23-28.
[9]郑洪艳,徐为人.小檗碱药理作用研究进展.中草药,2004,35(6):708-711.
[10]张群英,贺广远.四氢小檗碱抗心律失常作用及其机理探讨.江苏医药,1993,19(3):138-140.
[11]陈祝霞.中药降压的研究进展.中医药信息,2000,4:20-21.
[12]贺道华,马廉亭.罂粟碱,尼莫同治疗脑血管痉挛的疗效比较.暨南大学学报,2000,21(1):105-108.
[13]骆顺安,王晓贤.山莨菪碱舌下给药治疗急性痉挛性腹痛100例.新药与临床,1996,15(3):176-176.
[14]王丽平.包公藤甲素及其类似物的缩瞳活性.中草药,1992,23(4):205-208.
[15]李十中,王淀佐,亭晓岩.中药研究与开发现代化探讨.中草药,2001,32(5):385-387.
[16]Elena E,Stashenko,Ricardo A et al.High-resolution gas-chromatographic analysis of the secondary metabolites obtained by subcritical-fluid extraction from Colombian rue (Ruta graveolens L.).Journal of Biochemical and Biophysical Methods,2000,43(1):379-390.
[17]赵宋亮,陶春元,吴海英.超临界萃取技术在生物碱提取中的研究新进展.江西化工,2008(3):1-4.
[18]李化.超声技术在中草药成分提取中的应用.中药材,2001,24(4):299-300.
[19]蒲含林,郑元升,麻建军.超声法提取金鸡纳生物碱的工艺,暨南大学学报:自然科学与医学版,2008(3):329-330.
[20]范华均,栾伟,李攻科.微波辅助提取/HPLC分析石蒜中的生物碱.分析测试学报,2006,25(3):27-30.
[21]鲁传华,何平笙.麻黄及黄连生物碱膜提取方法的研究.中成药,2002,24(4):251-254.
[22]秦学功,元英进.苦豆子种子中生物碱的冷浸提取实验研究.中草药,2001,(32)7:604-606.
[23]刘颖,张燕玲,王雁.从天然植物龙葵中提取生物碱的工艺研究.辽宁丝绸,2003(2):4-5.
[24]王玉芹,李晓静,法洋.峨眉千里光生物碱乙醇提取工艺研究.中成药,2004,16(10):002-003.
[25]龙德清,饶贞学,丁宗庆.酸性醇浸渍法提取魔芋中的总生物碱.2003,24(10):126-127.
[26]迟玉明,赵唏瑛,吉泽丰吉等.角蒿总生物碱提取工艺的研究.天然产物研究与开发,2005,17(4):475-477.
[27]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(2):41-42.
[28]陈永刚,林励.魏燕华等超声波提取法与索氏提取法提取化橘红柚皮苷的比较研究中药新药与临床药理,2008(4):309-311.
[29]甄攀,杨风珍.吴茱萸总生物碱提取条件的考察.中国中药杂志,2000,(8):504-505.
[30]冷薇.超声提取技术的新探索,中国现代实用医学杂志,2006(5):43-45.
[31]陈志慧,周家容.不同提取方法对断肠草总生物碱提取率的影响.2007,46(3):176-177.
[32]王洪新,王键.苦豆子种子生物碱离子交换分离的因素研究.中草药,2002,33(12):1080-1083.
[33]周先礼,陈东林,王锋鹏.三小叶翠雀花中生物碱成分的研究.华西药学杂志,2005,20(1):1-3.
[34]李义平,杨广德,贺浪冲.红毛七总生物碱提取工艺研究.中药材,2007,30(2):220-223.
[35]刘逆夫,李瑞明.阳离子树脂纯化苦参生物碱的工艺研究.中国中医药现代远程教育,2006,4(12):22-24.
[36]廖小雪,查丽杭,刘骁等.吸附层析分离麻黄生物碱的过程优化.天然产物研究与开发,2004,16(4):281-285.
[37]迟玉明,赵唏瑛,吉泽丰吉.离子交换树脂用于角蒿总生物碱的纯化研究.天然产物研究与开发,2005,17(5):617-621.
[38]霍务贞,李苑新,姜红宇.阳离子交换树脂纯化喘平复方总生物碱的工艺研究.中药新药与临床药理,2005,16(6):446-449.
[39]顾铭,欧阳藩,苏志国.高速逆流色谱法分离纯化丹参并尝试制订中药指纹图谱.生物工程学报,2003,19(6):740-744.
[40]谭龙泉,张所明,欧庆瑜.薄层色谱在高速逆流色谱溶剂系统选择过程中的应用.分析化学,1996,24(12):1448-1451.
[41]袁黎明,傅若农,张天佑等.高速逆流色谱分离苦参中的总生物碱.北京理工大学学报,1997,17(2):244-247.
[42]谭龙泉,阮宗琴,欧庆瑜.高效毛细管电泳在高速逆流色谱的溶剂系统选择过程的应用.分析化学,1997,25(5):515-518.
[43]蔡定国,顾明娟,张吉德等.高速逆流层析分离中药苦参和洋金花总碱.中成药,1990,12(6):32-33.
[44]蔡定国,顾明娟,金涛.应用高速逆流层析分离峨眉千里光生物碱.中国中药杂志,1992,17(10):616-618.
[45]蔡定国,顾明娟,张吉德等.应用高速逆流层析仪分离三杉总碱的主要成分.中国医药工业杂志,1991,22(2):72-73.
[46]袁黎明,吴平,夏滔等.高速逆流色谱制备分离中药黄柏中的生物碱.色谱,2002,20(2):185-186.
[47]Liu Z L,Jin Y,Shen P N et al.Separation and purification of verticine and verticinone from Bulbus Fritillariae Thunbergii by high-speed counter-current chromatography coupled with evaporative light scattering detection.Talanta,2007,71(5):1873-1876
[48]饶畅,刘欣,张佩玲等.高速逆流色谱在天然产物分离中的应用-紫杉烷类二萜及二萜生物碱的制备分离.药学学报,1991,26(7):510-514.
[49]Li H B,Chen F.Preparative isolation and purification of chuanxiongzine from the medicinal plant Ligusticum chuanxiong by high-speed counter-current chromatography.Journal of Chromatography A,2004,1047(2):249-253.
[50]Wang X,Geng Y L,Li F W,et al.Large-scale separation of alkaloids from Corydalis decumbens by pH-zone-refining counter-current chromatography.Journal of Chromatography A,2006,1115(1-2):267-270.
[51]甘师俊,李振吉,邹健强.中药现代化发展战略.北京:科学技术文献出版社,1998.
[52]FDA Guidance for Industry-Botanical Drug Products(Draft Guidance).US Food and Drug Administration,Rockville,2000:18-22.
[53]Note for Guidance on Quality of Herbal Medicinal Products.European Medicines Agency,London,2001.
[54]科技部,国家计委,国家经贸委,卫生部,药品监管局,知识产权局,中医药局和中科院.药现代化发展纲要,2002.
[55]任德权.中药指纹图谱质控技术的意义与作用.中药材,2001,24(4):235-239.
[56]苏薇薇,吴忠,全健.中药指纹图谱的构建及计算机解析.中药材,2001,24(4):295-298.
[57]周玉新,雷海明,徐永红等.中药指纹图谱研究技术.北京:化学工业出版社,2002.
[58]梁逸曾.浅议中药色谱指纹图谱的意义、作用及可操作性.中药新药与临床药理,2001,5(12):196-200.
[59]周玉新,雷海明,徐永红等.中药指纹图谱研究技术.北京:化学工业出版社,2002.
[60]Snyder L R,Kirkland J J,Glajch J L.实用高效液相色谱法的建立(第二版).北京:华文出版社,2001.
[61]王俊德.高效液相色谱法.北京:石油化工出版社,1992.
[62]郑荣庆,李光秀.高效液相色谱法及其在中药研究中的应用.中草药,1993,24(5):265-268.
[63]Chen S B,Liu H P,Tian R T.High-performance thin-layer chromatographic fingerprints of isoflavonoids for distinguishing between Radix Puerariae Lobate and Radix Puerariae Thomsonii.Journal of Chromatography A,2006,1121(1):114-119.
[64]Yan S K,Xin W F,Luo G A.An approach to develop two-dimensional fingerprint for the quality control of Qingkailing injection by high-performance liquid chromatography with diode array detection.Journal of Chromatography A,2005,1090 (1-2):90-97.
[65]Gu M,Ouyang F,Su Z G.Comparison of high-speed counter-current chromatography and high-performance liquid chromatography on fingerprinting of Chinese traditional medicine.Journal of Chromatography A,2004,1022(1-2):139-144.
[66]Lu H M,Liang Y Z,Chen S.Identification and quality assessment of Houttuynia cordata injection using GC-MS fingerprint:A standardization approach.Journal of Ethnopharmacology,2006,105 (3):436-440.
[67]Yu K,Gong Y F,Lin Z Y.Quantitative analysis and chromatographic fingerprinting for the quality evaluation of Scutellaria baicalensis Georgi using capillary electrophoresis.Journal of Pharmaceutical and Biomedical Analysis,2006.
[68]Laura M B,Betty A L,Dan L B.Characterisation of phenolics by LC-UV/Vis,LC-MS/MS and sugars by GC in Melicoccus bi jugatus Jacq.‘Montgomery’ fruits,Food Chemistry,2008,111(4):1017-1024
[69]Sebnem G,Aysegul C G,Feride S.Use of Fourier transform infrared spectroscopy for rapid comparative analysis of Bacillus and Micrococcus isolates,Food Chemistry,2009,113(4):1301-1307
[70]Alonso-Salces R M,H(?)berger K,Holland M V,Multivariate analysis of NMR fingerprint of the unsaponifiable fraction of virgin olive oils for authentication purposes,Food Chemistry,2008
[71]Avula B,Wang Y H,Pawar R S,A rapid method for chemical fingerprint analysis of Hoodia species,related genera,and dietary supplements using UPLC-UV-MS,Journal of Pharmaceutical and Biomedical Analysis,2008,48(3) 722-731.
[72]聂晶,颂九,王国荣．中药指纹图谱的研究现状．中草药,2000,31(12)：881-884．
[73]Yu R M,Ye B,Yan C Y.Fingerprint analysis of fruiting bodies of cultured Cordyceps militaris by high-performance liquid chromatography-photodiode array detection,Journal of Pharmaceutical and Biomedical Analysis.2007,44(3):818-823.
[74]Chen C,Zhang H,Xiao W et al.High-performance liquid chromatographic fingerprint analysis for different origins of sea buckthorn berries.Journal of Chromatography A,2007,1154(1-2):250-259.
[75]Yi L Z,Yuan D L,Liang Y Z.Quality control and discrimination of Pericarpium Citri Reticulatae and Pericarpium Citri Reticulatae Viride based on high-performance liquid chromatographic fingerprints and multivariate statistical analysis.Analytica Chimica Acta,2007,588(2):207-215.
[76]Ma L J,Zhang X Z,Zhang H P.Development of a fingerprint of Salvia miltiorrhiza Bunge by high-performance liquid chromatography with a coulometric electrode array system.Journal of Chromatography B,2007,846(1-2):139-146.
[77]国家药典委员会.中华人民共和国药典.2005年版,一部[M],北京:人民卫生出版社,2005:94.
[78]奚镜清,金联城,忻纳新等.中药材延胡索的品种整理及文献考证.现代应用药学,1995,12(4):12-15.
[79]金正均,王永铭,苏定冯.药理学进展.北京:科学出版社,1999,64-73.
[80]Hidehikok,Neko,Shunsuke N.Studies on the Constituents of Corydalis sp.Ⅵ.Alkaloids from Chinese Corydalis and the Identity of d-Corydalmine with d-Corybulbine.1969,3(9) 2803-2804.
[81]刘俊红,魏峻峰,王洪志等.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.
[82]马家骅,杨明,许润春等.醋延胡索炮制工艺的研究.中草药,2005,36(11):1657-1659.
[83]李银林.影响延胡索疗效因素的分析.河南中医学院学报,2005,3(2):76-77.
[84]南京药学院《中草药》编写组.《中草药学》(中册).江苏人民出版社,1976.
[85]金国章.延胡索乙素的药理研究ⅩⅢ:延胡索乙素对动物成瘾性的实验,生理学报,1978,30(1):67-72.
[86]吕清文,丛雅勤.延胡索药理作用及临床应用浅议.内蒙古中医药:26-27.
[87]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.
[88]周瑞,陆兔林.延胡索的提取工艺优选.时珍国医国药,2003,14(11):662-663.
[89]邱蓉丽,李祥,陈建伟等.延胡索总碱提取方法研究.中医药研究,2000,16(5):50-51.
[90]谢彩娟,张志琪.超声提取延胡索总生物碱的研究.西北药学杂志,2005,20(4):153-154.
[91]范斌,刘泓,杨亚莉.HPLC法测定延胡索药材中季胺型生物碱的含量.中国中医基础医学杂志,2006,12(1):59-60.
[92]姜舜尧.高效液相色谱法测定元胡止痛片中脱氢延胡索碱的含量.中国中药杂志,2000,25(8):479-480.
[93]Cheng Z H,Guo Y L,Wang H Y,et al.Qualitative and quantitative analysis of quaternary ammonium alkaloids from Rhizoma Corydalis by matrix-assisted laser desorption/ionization Fourier transform mass spectrometry coupled with a selective precipitation reaction using Reinecke salt.Analytica Chimica Acta,2006,555(2):269-277.
[94]程志红,陈国强,王昊阳等.延胡索中季铵生物碱的高分辨基质辅助激光解吸电离质谱研究.2004,2(2):99-102.
[95]陈洪燕,万明,孙金霞.均匀设计延胡索提取工艺的研究.湖北中医杂志,2006,28(7):54-55.
[96]黄山,陈峰,郭立伟.延胡索提取工艺的优选.中国中医药信息杂志,2006,13(1):47-48.
[97]涂文升.用不同溶剂、不同提取方法测定金不换中延胡索乙素的含量.广西医科大学学报,2006,23(1):105-106.
[98]廖维,夏新华.延胡索提取工艺的研究.中成药,2004,26(10):6-8.
[99]房方,丁选胜.延胡索药材中延胡索乙素的含量测定.现代中药研究与实践,2005,19(1):54-56.
[100]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):47-48.
[101]陈峰,郭立伟,井山林等.超临界C02流体萃取延胡索中延胡索乙素的正交试验研究.中药新药与临床药理,2005,16(2):137-138.
[102]刘龙忠.优选延胡索生物碱提取工艺.遵义医学院学报,2004,27(6):595-596.
[103]龚青,周蒂,王碧娟.HPLC法测定延胡索乙素的含量.中国现代应用药学杂志,2000,17(4):315-317.
[104]马临科.高效液相色谱法测定延胡索中延胡索乙素的含量.药学实践杂志,2003,21(6):351-353.
[105]方东军,赵润琴,张鹏.HPLC法测定安胃片中延胡索乙素的含量.中医药学报,2004,32(5):36-37.
[106]石上梅,高天兵,田金.HPLC法测定消痛片中延胡索乙素的含量.中国药事,2003,17(1):42-43.
[107]顾秀琰.RP-HPLC测定元胡止痛丸中延胡索乙素的含量.2006,28(4):606-608.
[108]方强,陈晓龙,陈彬.反相高效液相色谱法测定安胃片中有过延胡索乙素的含量.2006,25(8):827-828.
[109]Ou J J,Kong L,Pan C S et al.Determination of Dl-tetrahydropalmatine in Corydalis yanhusuo by L-tetrhydropalmatine inprinted monolithic column coupling with reversed-phase high performance liquid chromatography.Journal of Chromatography A,2006,1117(1):163-169.
[110]方子季,徐霞,王春燕.高效液相色谱法测定良参胃安片中延胡索乙素的含量.解放军药学学报,2006,22(3):222-223.
[111]王慕邹.常用中草药高效液相色谱分析.北京:科学出版社,1999,139-146.
[112]俞雁,金艳,徐超.应用高速逆流色谱技术从延胡索中分离制备延胡索乙素.世界科学技术-中医药现代化,2006,8(2):17-19.
[113]王海燕,穆惠军.元胡止痛片提取工艺研究.山东中医杂志,2002,21(12):739-740.
[114]Ito Y.Golden rules and pitfalls in selecting optimum conditions for high-speed counter-current chromatography.Journal of Chromatography A,2005,1065(2):145-168.
[115]江和源,程启坤,杜琪珍.高速逆流色谱法分离纯化茶黄素.天然产物研究和开发,2000,12(4):30-35.
[116]缪平,蔡定国.分析型逆流色谱的应用.中国重要杂志,1995,20(9):569-670.
[117]Gu M,Wang XL,Su Z G et al.One-step separation and purification of 3,4-dihydroxy phenylactic acid,salvianolic acid B and protocatechualdehyde from Salvia miltiorrhiza Bunge by high-speed counter-current chromatography.Journal of Chromatography A,2007,1140(1-2):107-111.
[118]Li H B,Chen F.Preparative isolation and purification of phillyrin from the medicinal plant Forsythia suspensa by high-speed counter-current chromatography.Journal of Chromatography A,2005,1083(1-2):102-105.
[119]Gao M,Gu M,Liu C Z.Two-step purification of scutellarin from Erigeron breviscapus (vant.)Hand.Mazz.by high-speed counter-current chromatography.Journal of Chromatography B,2006,838(2):139-143.
[120]Peng J Y,Jiang Y Y,Fan G R et al.Optimization suitable conditions for preparative isolation and separation of curculigoside and curculigoside B from Curculigo orchioides by high-speed counter-current chromatography.Separation and Purification Technology,2006,52(1):22-28.
[121]Yu Y,Jin Y,Cu C et al.Separation and Preparation of dl-tetrahydropalmatine from Crude Extract of Corydalis Yanhusuo W.T.Wang by High-speed Countercurrent Chromatography Technology.World science and technology-modernization of traditional Chinese medicine and materia medica,2006,8(2):17-19.
[122]曹学丽．高速逆流色谱分离技术及应用．化学工业出版社,北京,2005,40-41．
[123]Ito Y.Golden rules and pitfalls in selecting optimum conditions for high-speed counter-current chromatography.Journal of Chromatography A,2005,1065(2):145-168.
[124]Tong S Q,Yan J Z,Lou J Z.Preparative isolation and purification of alkaloids from Corydalis yanhusuo W.T.Wang by high speed counter-current chromatography.Journal of Liquid Chromatography and Related Technologies,2005,28(18) 2979-2989.
[125]Liu ZL,JinY,ShenPNetal.Separation and purification of verticine and verticinone from Bulbus Fritillariae Thunbergii by high-speed counter-current chromatography coupled with evaporative light scattering detection.Talanta,2007,71(5):1873-1876.
[126]FDA Guidance for Industry-Botanical Drug Products (Draft Guidance).US Food and Drug Administration.Rockville,2000:18-22.
[127]Note for Guidance on Quality of Herbal Medicinal Products.European Medicines Agency.London,2001.
[128]Committee of National Pharmacopoeia.In:Pharmacopoeia of P.R.China,Press of Chemical Industry,Beijing,2005.
[129]Wang M Z.HPLC Analysis of Some Common Chinese Traditional Medicine.Beijing:Science Press,2000:139～146.
[130]周元瑶,李芳.用反向高效液相色谱法考察盐酸黄连素的质量,药物分析杂志,1984,4(3):131-133.
[131]袁久荣,魏英勤,袁浩等.RP-HPLC法同时测定黄连中四种原小檗碱型生物碱的含量.世界科学技术-中医药现代化2006,8(6):36-39.
[132]Tetsuo M,Kazuhiko S,Mitsuharu O et al.Simultaneous determnation of berberine,palmatine and coptisine in crude drugs and oriental pharmaceutical preparation by ion-pair high-performance liquid chromatography.ChemPharm Bull,1987,30(1):354-357.
[133]洪筱坤,王智华.中药数字化色谱指纹谱.上海:上海科学技术出版社,2003.