通窍耳聋丸的质量标准研究
摘要
目的：
通窍耳聋丸是由龙胆、黄芩、栀子、芦荟、熟地黄、柴胡、木香等十二味中药制成的复方制剂,具有清肝泻火、通窍润便的功效,用于治疗肝经热盛,耳聋蝉鸣,耳底肿痛等症。通窍耳聋丸现有的标准收载于卫生部药品标准·中药成方制剂(第一册),其中的质量标准不完善,缺少鉴别及含量测定方法,不能满足中药现代化质量控制的要求。本论文研究的目的在于完善通窍耳聋丸的质量标准,提高本品质量的可控性。
方法：
采用薄层色谱法对制剂中木香、当归、黄芩、栀子、柴胡、龙胆、芦荟、青黛进行薄层鉴别研究。
采用高效液相色谱法,以龙胆苦苷为指标,建立君药龙胆药材的含量测定方法：采用Diamonsil C18分析柱(4.6*250mm,5μm),乙腈-水(15：85)为流动相,检测波长为275nm。以黄芩苷为指标,建立臣药黄芩药材的含量测定方法：采用Diamonsil C18分析柱(4.6*250mm,5μm),乙腈-0.2%磷酸(26：74)为流动相,检测波长为278nm。
结果：
在定性鉴别中,供试品色谱在与对照品色谱相应的位置上,显示相同颜色的斑点,斑点清晰,分离度良好,阴性对照品色谱中无干扰。
含量测定中,龙胆苦苷在0.24～2.7μg范围内与峰面积呈良好线性关系,回归方程为Y=20.375X-0.7398,r=0.9999；精密度、重复性、回收率的RSD<3%；同时确定了本品每1g含龙胆以龙胆苦苷(C16H20O9)计,不得少于1.5mg。
此外,黄芩苷在0.45～3.15μg范围内与峰面积呈良好线性关系,回归方程Y=39.403X-0.2359,r=0.9998；精密度、重复性、回收率的RSD<3%；同时确定了本品每1g含黄芩以黄芩苷(C21H18O11)计,不得少于12mg。
结论：
薄层色谱鉴别方法简便,专属性强,斑点清晰,重现性好；高效液相色谱法测定君药龙胆及臣药黄芩的含量,其方法专属性强,准确灵敏,稳定性好,可以作为本品的质量控制方法。
Object ive
Tongqiao Erlong pills is made up of12Chinese herbal medicines such as Radix Gentianae, Radix Scutellariae, Fructus Gardeniae, Aloe, Radix Angelicae Sinensis, Indigo Naturalis, Radix Bupleuri, Costus Root with effect of purging liver-fire and relaxing the bowels.It is used for the treatment of intense fire in liver, Deafness, tinnitus, Earache, and so on. The existing quality standard of Tongqiao Erlong Pills is written in the first Drug Standard of the Health Ministry. However, It is difficult to control the quality of Tongqiao Erlong pills completely due to the lacking of the qualitative and quantitative control methods of components in the medicine. The purpose of this research is to improve the quality standard of Tongqiao Erlong pills and control the quality effectively.
Methods
Use the thin-layer chromatography(TLC) to carry on the qualitative distinction of Costus Root, Radix Angelicae Sinensis, Radix Scutellariae, Fructus Gardeniae, Radix Bupleuri, Radix Gentianae, Aloe, Indigo Naturalis in the preparation.
Taking gentiopicrin as the target, A reversed-phase high performance liquid chromatography (HPLC) method was developed to determine Radix Gentianae in the preparation. HPLC analytical method was carried out by using a Diamonsil C18column(4.6mm×250mm,5um)and a mixture of acetonitrile-water (15:85) as the mobile phase. The detection wavelength was set at275nm. Taking baicalin as the target, A reversed-phase HPLC method was developed to determine Radix Scutellariae in the preparation. HPLC analytical method was carried out by using a Diamonsil C18column(4.6mmX250mm,5um)and a mixture of acetonitrile-0.2%phosphoric acid (26:74) as the mobile phase. The detection wavelength was set at278nm.
Results
In the identification, the sample displayed the same spots which were vivid and with high resolution as the reference substance did in the Chromatography, while the negative sample did not.
In the essay, the liner ranges of gentiopicrin was0.24-2.7μg, liner regression equation was Y=20.375X-0.7398, r=0.9999. The RSD of precision, repeatability and recovery were less than3%. We finally determined that gentiopicrin (C16H20O9) should not be less than1.5mg pergrams of Tongqiao Erlong pills; the liner ranges of baicalin was0.45-3.15μ g, liner regression equation was Y-39.403X-0.2359, r=0.9998. The RSD of precision, repeatability and recovery were less than3%. We finally determined that baicalin (C21H18O11) should not be less than12mg pergrams of Tongqiao Erlong pills.
Conclusion
The TLC methods for identification and the HPLC assay methods were simple, sensitive, specific, repeatable and accurate. These analysis method can be applied to the quality control of preparation.
通窍耳聋丸是由龙胆、黄芩、栀子、芦荟、熟地黄、柴胡、木香等十二味中药制成的复方制剂,具有清肝泻火、通窍润便的功效,用于治疗肝经热盛,耳聋蝉鸣,耳底肿痛等症。通窍耳聋丸现有的标准收载于卫生部药品标准·中药成方制剂(第一册),其中的质量标准不完善,缺少鉴别及含量测定方法,不能满足中药现代化质量控制的要求。本论文研究的目的在于完善通窍耳聋丸的质量标准,提高本品质量的可控性。
方法：
采用薄层色谱法对制剂中木香、当归、黄芩、栀子、柴胡、龙胆、芦荟、青黛进行薄层鉴别研究。
采用高效液相色谱法,以龙胆苦苷为指标,建立君药龙胆药材的含量测定方法：采用Diamonsil C18分析柱(4.6*250mm,5μm),乙腈-水(15：85)为流动相,检测波长为275nm。以黄芩苷为指标,建立臣药黄芩药材的含量测定方法：采用Diamonsil C18分析柱(4.6*250mm,5μm),乙腈-0.2%磷酸(26：74)为流动相,检测波长为278nm。
结果：
在定性鉴别中,供试品色谱在与对照品色谱相应的位置上,显示相同颜色的斑点,斑点清晰,分离度良好,阴性对照品色谱中无干扰。
含量测定中,龙胆苦苷在0.24～2.7μg范围内与峰面积呈良好线性关系,回归方程为Y=20.375X-0.7398,r=0.9999；精密度、重复性、回收率的RSD<3%；同时确定了本品每1g含龙胆以龙胆苦苷(C16H20O9)计,不得少于1.5mg。
此外,黄芩苷在0.45～3.15μg范围内与峰面积呈良好线性关系,回归方程Y=39.403X-0.2359,r=0.9998；精密度、重复性、回收率的RSD<3%；同时确定了本品每1g含黄芩以黄芩苷(C21H18O11)计,不得少于12mg。
结论：
薄层色谱鉴别方法简便,专属性强,斑点清晰,重现性好；高效液相色谱法测定君药龙胆及臣药黄芩的含量,其方法专属性强,准确灵敏,稳定性好,可以作为本品的质量控制方法。
Object ive
Tongqiao Erlong pills is made up of12Chinese herbal medicines such as Radix Gentianae, Radix Scutellariae, Fructus Gardeniae, Aloe, Radix Angelicae Sinensis, Indigo Naturalis, Radix Bupleuri, Costus Root with effect of purging liver-fire and relaxing the bowels.It is used for the treatment of intense fire in liver, Deafness, tinnitus, Earache, and so on. The existing quality standard of Tongqiao Erlong Pills is written in the first Drug Standard of the Health Ministry. However, It is difficult to control the quality of Tongqiao Erlong pills completely due to the lacking of the qualitative and quantitative control methods of components in the medicine. The purpose of this research is to improve the quality standard of Tongqiao Erlong pills and control the quality effectively.
Methods
Use the thin-layer chromatography(TLC) to carry on the qualitative distinction of Costus Root, Radix Angelicae Sinensis, Radix Scutellariae, Fructus Gardeniae, Radix Bupleuri, Radix Gentianae, Aloe, Indigo Naturalis in the preparation.
Taking gentiopicrin as the target, A reversed-phase high performance liquid chromatography (HPLC) method was developed to determine Radix Gentianae in the preparation. HPLC analytical method was carried out by using a Diamonsil C18column(4.6mm×250mm,5um)and a mixture of acetonitrile-water (15:85) as the mobile phase. The detection wavelength was set at275nm. Taking baicalin as the target, A reversed-phase HPLC method was developed to determine Radix Scutellariae in the preparation. HPLC analytical method was carried out by using a Diamonsil C18column(4.6mmX250mm,5um)and a mixture of acetonitrile-0.2%phosphoric acid (26:74) as the mobile phase. The detection wavelength was set at278nm.
Results
In the identification, the sample displayed the same spots which were vivid and with high resolution as the reference substance did in the Chromatography, while the negative sample did not.
In the essay, the liner ranges of gentiopicrin was0.24-2.7μg, liner regression equation was Y=20.375X-0.7398, r=0.9999. The RSD of precision, repeatability and recovery were less than3%. We finally determined that gentiopicrin (C16H20O9) should not be less than1.5mg pergrams of Tongqiao Erlong pills; the liner ranges of baicalin was0.45-3.15μ g, liner regression equation was Y-39.403X-0.2359, r=0.9998. The RSD of precision, repeatability and recovery were less than3%. We finally determined that baicalin (C21H18O11) should not be less than12mg pergrams of Tongqiao Erlong pills.
Conclusion
The TLC methods for identification and the HPLC assay methods were simple, sensitive, specific, repeatable and accurate. These analysis method can be applied to the quality control of preparation.
引文
[1]王玉美.针刺治疗聋哑病129例[J].山东中医杂志,1993,12(1)：25.
[2]周德安,严华.针刺治疗神经性耳聋98例[J].上海针灸杂志,1999,18(5)：29.
[3]乔佳彬,乔占林,宋晓平,等.中两结合治疗感音神经性耳聋48例研究分析[J].全国疑难性心脑血管病诊疗新进展研讨会：41-42.
[4]钟渠,彭顺林,冯大志,等.中两医结合治疗感音神经性耳聋疗效观察.山两中医,2002,18(3)：32.
[5]李展宗,李云英.突发性耳聋中医病因病机现代研究概况[J],辽宁中医药大学学报,2011,13(7)：71-73.
[6]张东霞.中医药在突发性耳聋综合治疗中的应用概况[J].中医导报,2010,25(3)：584-585.
[7]李凡成.论神经性耳鸣的辨证施治[J].湖南中医药大学学报,2011,31(1)：12-14.
[8]魏榕清.辨证治疗感音神经性耳聋32例疗效观察[J].新中医,1996,4：23-25.
[9]卫生部药品标准[S].中药成方制剂.第一册.WS3-B-0122-89.
[10]郑晓黎,张荣华,周赛南.从肝论治耳鸣耳聋[J].山东中医药大学学报,32(2),2008：113.
[11]贾琦,张如益.柴胡属植物中皂苷化学研究进展[J].药学学报,1989,24(12)：961.
[12]谭利,张庆英,李教社,等.南柴胡根中木脂素苷类化合物的研究[J].药学学报,2005,40(5)：428.
[13]戴克敏,杭秉菁,袁吕齐.常用中药的药理和应用[M].南京：江苏科学技术出版社,1981：1931.
[14]梅全喜.现代中药药理与临床应用手册[M]北京：中国中医药出版社,2008：801.
[15]孙南君,夏春芳.坚龙胆中化学成分的研究[J].中药通报,1984,9(1)：33.
[16]刘明韬,韩志超,章漳,等.龙胆化学成分研究[J].沈阳药科大学学报,2005,22(2)：103.
[17]国家中医药管理局《中华本草》编委会.中华本草(精选本)：下册[Z].上海：上海科技出版社,1998.1489-1496.
[18]Atherton,Peter MB ChB,DObst,et al.Aloe vera:magic or medicine[J].Nurs Stand,1998,12(41):49.
[19]万金志,乔悦.芦荟的化学成分及其研究[J].中草药,1999,30(2)：151-153.
[20]冯力,州正海.芦荟的化学成分及药用价值研究研究进展[J].西北药学杂志,2008,10(23)：332-333.
[21]吕明庄,陈波,张遵真,等.芦荟提取物对衰老模型鼠抗自由基氧化损伤DNA作用的试验研究[J].中国医药学报,2003,18(3)：136-138.
[22]赵素容,卢茺伟,陈金龙,等.地黄梓醇降糖作用的实验研究[J].时珍国医国药,2009,20(1)：171-172.
[23]江苏新医学院编.中药大辞典[M].上海科学技术出版社,2005,4：217.
[24]李玉山.黄芩的化学成分及黄芩营的提取方法[J].西北药学杂志,2008,23(6)：410.
[25]陈雪梅.青黛炮制过程基本原理研究[D].成都：成都中医药大学,2008：11.
[26]向阳,常晓慧,程慧,等.“复方青黛片为主治疗急性早幼粒细胞白血痫的临床研究”引证文献分析[J].中国中医药信息杂志,2010,17(9)：97.
[27]姜晓昆.青黛临床新用[J].黑龙江中医药,2009(4)：45.
[28]Prakash S,Sinha G K.Chemical examination of Arisaema curvatum Kunth (Part I) [J].Nat Appl Sci Bull,1974,26(2):25-27.
[29]Miglani B D,Chawla A S,Gaind K N.Chemical investigation of Arisaema tortuosum corm [J].Indian J Pharm,1978,40(1):24-26.
[30]杜树山,徐艳春,魏璐雪.天南星化学成分研究[J].中草药,2003,34(4)：310.
[31]Dhuna V,Bains JS,Kamboj SS,et al.Purification and characterization of a lectin from Arisaema tortuosum Schott having in-vitro anticancer activity against human cancercell lines[J]. Biochem Mol Biol,2005,38(5):526.
[32]王关林,蒋丹,方宏筠.天南星的抑菌作用及其机理研究[J].畜牧兽医学报,2004,35(3)：280.
[33]侯鹏飞,陈文星,赵新慧,等.木香挥发性成分气质联用分析及其抑制血小板聚集作用的研究[J].2008,14(7)：26-30.
[34]Talwar KK,Singh IP,Kalsi PS.A sesquiterpenoid with plant growth regulat ory activity from Sarssurea lappa [J].Phytochem istry,1992,31(1):336-338.
[35]蔡少青,郑汉臣.药用植物学与生药学[M].北京：人民卫生出版社,2004：430.
[36]韩坚,林煌权,钟志勇,等.木香超临界提取物抗实验性胃溃疡的研究[J].中药材,2005,28(11)：1017-1019.
[37]Lee MG,Lee KT,Chi SG,et al.Costunolide induces apoptosis by ROS mediated mitochondrial permeability transition and cytochrome C release[J].BiolPharm Bull,2001,24:303-306.
[38]郑学钦,沈小燕,刘紫英.陈皮、青皮、枳实和枳壳的气相色谱研究[J].海峡药学,1995,7(4)：4-5.
[39]陈康,叶桥.炮制对青皮中黄酮类成分的影响[J].中药材,1996,19(4)：185-186.
[40]丁春光,孙素琴,周群,等.应用HPLC-DAD及HPLC-HRMS技术研究不同贮存年限陈皮的指纹图谱[J].中国新药杂志,2008,17(11)：927.
[41]Molnar P, Kawase M,Satoh K,et al.Biological activity of carotenoids in red paprika,Vnlencia orange and Golden delicious apple[J].Phytother Res,2005,19(8):700-707.
[42]Tanaka T,Makita H,Kawabata K,et al.Chemoprevention of azoxymethane induced rat colon carcinogenesis by the naturally occurring flavonoids,diosmin and hesperidin[J].Carcinogenesis,1997,18(5):957-965.
[43]国家药典委员会.中华人民共和国药典：一部[M].北京：化学工业出版社,2010：124.
[44]柳永青.当归的化学成分与生物活性[J].航空航天医药,2009,20(11)：127-128.
[45]夏邦旗.栀子深加工综合利用研究[J].安徽科技,1998(4)：31-32.
[46]刘海萍.栀子的化学成分及其质量研究[D].北京：首都师范大学,2007.
[47]马双成,戴忠,J‘丽霞.中药质量标准的研究进展[J].中国药师,2006,9(1)：29.
[48]黄巧文.红外光谱技术对中药鉴别的研究进展[J].海峡药学,2008,20(12)：151-153.
[49]时维静,王甫成,俞浩,等.中药分析与检测[M].北京：化学工业出版社,2010,24-25.
[50]国家药典委员会.中国药典2010年版一部[S].北京：中国医药科技出版社,2009：前言.
[51]高学敏,张建军,张德芹,等.中成药质量标准化建设的现状及展望[J].中国中药杂志,2007,32(9)：868-871.
[52]刘万仓,孙磊,于孟琦,等.中药指纹图谱模式识别研究进展.国际药学研究杂志,2010,37(6)：446-449.
[53]Qiu YQ,Lu X,Pang T,et al.Study of traditional Chinese medicine volatile oils from different geographical origins by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry(GC×GC-TOFMS)in combination with multivariate analysis[J].J Pharm Biomed Anal,2007,43(5):1721.
[54]Cai M,Zhou Y,Gesang S,Chemical fingerprint analysis of rhizomes of Gymnadenia conopsea by HPLC-DAN-MS[J].Chromatogr B Analyt Technol Biomed Life Sci,2006,844:301-307.
[55]Lu HM,Liang YZ,Chen S.Identification and quality as-sessment of houttuynia cordata injection using GC-MS fingerprint:A standardization approach[J].J Ethnopharmacol,2006,105(3):436.
[56]Ren MT,Che J,Song Y,et al. Identification and quantification of 32 bioactive compounds in lonicera species by high performance liquid chromatography coupled with tine-of-fiight mass spectrometry[J].J Pharm Biomed Anal,2008,48(5):1351.
[57]国家药典委员会.中华人民共和国药典(一部)[S]北京：中国医药科技出版社,2010：778.
[58]刘梅,陈其华,刘满祥.显得清冲剂主要成分的薄层鉴别[J].西北药学杂志,1996,11(4)：156-157.
[59]国家药典委员会.中华人民共和国药典(一部)[S]北京：中国医药科技出版社,2010：729.
[60]赵志军,王连水.小柴胡颗粒薄层鉴别及黄芩苷含量测定方法的研究[J].中国实验方剂学杂志,2005, 11(3)：22-23.
[61]苏丽静,吴伟东,余星云小儿清热止咳口服液薄层鉴别方法的改进[J].今日药学,2010,20(6)：45.
[62]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：597.
[63]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：1210.
[64]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：1105.
[65]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：1002.
[66]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：1172.
[67]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：185.
[68]李馨,王金宏,金迪,等.HPLC法测定龙胆中龙胆苦苷的含量[J].黑龙江医药,2010,23(3)：319-321.
[69]张建春,张华,施瑛,等.黄岑苷的研究近况[J].时珍国医国药,2005,16(3)：247-249.
[70]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：89,969,1172.
[71]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：282,1134.
[2]周德安,严华.针刺治疗神经性耳聋98例[J].上海针灸杂志,1999,18(5)：29.
[3]乔佳彬,乔占林,宋晓平,等.中两结合治疗感音神经性耳聋48例研究分析[J].全国疑难性心脑血管病诊疗新进展研讨会：41-42.
[4]钟渠,彭顺林,冯大志,等.中两医结合治疗感音神经性耳聋疗效观察.山两中医,2002,18(3)：32.
[5]李展宗,李云英.突发性耳聋中医病因病机现代研究概况[J],辽宁中医药大学学报,2011,13(7)：71-73.
[6]张东霞.中医药在突发性耳聋综合治疗中的应用概况[J].中医导报,2010,25(3)：584-585.
[7]李凡成.论神经性耳鸣的辨证施治[J].湖南中医药大学学报,2011,31(1)：12-14.
[8]魏榕清.辨证治疗感音神经性耳聋32例疗效观察[J].新中医,1996,4：23-25.
[9]卫生部药品标准[S].中药成方制剂.第一册.WS3-B-0122-89.
[10]郑晓黎,张荣华,周赛南.从肝论治耳鸣耳聋[J].山东中医药大学学报,32(2),2008：113.
[11]贾琦,张如益.柴胡属植物中皂苷化学研究进展[J].药学学报,1989,24(12)：961.
[12]谭利,张庆英,李教社,等.南柴胡根中木脂素苷类化合物的研究[J].药学学报,2005,40(5)：428.
[13]戴克敏,杭秉菁,袁吕齐.常用中药的药理和应用[M].南京：江苏科学技术出版社,1981：1931.
[14]梅全喜.现代中药药理与临床应用手册[M]北京：中国中医药出版社,2008：801.
[15]孙南君,夏春芳.坚龙胆中化学成分的研究[J].中药通报,1984,9(1)：33.
[16]刘明韬,韩志超,章漳,等.龙胆化学成分研究[J].沈阳药科大学学报,2005,22(2)：103.
[17]国家中医药管理局《中华本草》编委会.中华本草(精选本)：下册[Z].上海：上海科技出版社,1998.1489-1496.
[18]Atherton,Peter MB ChB,DObst,et al.Aloe vera:magic or medicine[J].Nurs Stand,1998,12(41):49.
[19]万金志,乔悦.芦荟的化学成分及其研究[J].中草药,1999,30(2)：151-153.
[20]冯力,州正海.芦荟的化学成分及药用价值研究研究进展[J].西北药学杂志,2008,10(23)：332-333.
[21]吕明庄,陈波,张遵真,等.芦荟提取物对衰老模型鼠抗自由基氧化损伤DNA作用的试验研究[J].中国医药学报,2003,18(3)：136-138.
[22]赵素容,卢茺伟,陈金龙,等.地黄梓醇降糖作用的实验研究[J].时珍国医国药,2009,20(1)：171-172.
[23]江苏新医学院编.中药大辞典[M].上海科学技术出版社,2005,4：217.
[24]李玉山.黄芩的化学成分及黄芩营的提取方法[J].西北药学杂志,2008,23(6)：410.
[25]陈雪梅.青黛炮制过程基本原理研究[D].成都：成都中医药大学,2008：11.
[26]向阳,常晓慧,程慧,等.“复方青黛片为主治疗急性早幼粒细胞白血痫的临床研究”引证文献分析[J].中国中医药信息杂志,2010,17(9)：97.
[27]姜晓昆.青黛临床新用[J].黑龙江中医药,2009(4)：45.
[28]Prakash S,Sinha G K.Chemical examination of Arisaema curvatum Kunth (Part I) [J].Nat Appl Sci Bull,1974,26(2):25-27.
[29]Miglani B D,Chawla A S,Gaind K N.Chemical investigation of Arisaema tortuosum corm [J].Indian J Pharm,1978,40(1):24-26.
[30]杜树山,徐艳春,魏璐雪.天南星化学成分研究[J].中草药,2003,34(4)：310.
[31]Dhuna V,Bains JS,Kamboj SS,et al.Purification and characterization of a lectin from Arisaema tortuosum Schott having in-vitro anticancer activity against human cancercell lines[J]. Biochem Mol Biol,2005,38(5):526.
[32]王关林,蒋丹,方宏筠.天南星的抑菌作用及其机理研究[J].畜牧兽医学报,2004,35(3)：280.
[33]侯鹏飞,陈文星,赵新慧,等.木香挥发性成分气质联用分析及其抑制血小板聚集作用的研究[J].2008,14(7)：26-30.
[34]Talwar KK,Singh IP,Kalsi PS.A sesquiterpenoid with plant growth regulat ory activity from Sarssurea lappa [J].Phytochem istry,1992,31(1):336-338.
[35]蔡少青,郑汉臣.药用植物学与生药学[M].北京：人民卫生出版社,2004：430.
[36]韩坚,林煌权,钟志勇,等.木香超临界提取物抗实验性胃溃疡的研究[J].中药材,2005,28(11)：1017-1019.
[37]Lee MG,Lee KT,Chi SG,et al.Costunolide induces apoptosis by ROS mediated mitochondrial permeability transition and cytochrome C release[J].BiolPharm Bull,2001,24:303-306.
[38]郑学钦,沈小燕,刘紫英.陈皮、青皮、枳实和枳壳的气相色谱研究[J].海峡药学,1995,7(4)：4-5.
[39]陈康,叶桥.炮制对青皮中黄酮类成分的影响[J].中药材,1996,19(4)：185-186.
[40]丁春光,孙素琴,周群,等.应用HPLC-DAD及HPLC-HRMS技术研究不同贮存年限陈皮的指纹图谱[J].中国新药杂志,2008,17(11)：927.
[41]Molnar P, Kawase M,Satoh K,et al.Biological activity of carotenoids in red paprika,Vnlencia orange and Golden delicious apple[J].Phytother Res,2005,19(8):700-707.
[42]Tanaka T,Makita H,Kawabata K,et al.Chemoprevention of azoxymethane induced rat colon carcinogenesis by the naturally occurring flavonoids,diosmin and hesperidin[J].Carcinogenesis,1997,18(5):957-965.
[43]国家药典委员会.中华人民共和国药典：一部[M].北京：化学工业出版社,2010：124.
[44]柳永青.当归的化学成分与生物活性[J].航空航天医药,2009,20(11)：127-128.
[45]夏邦旗.栀子深加工综合利用研究[J].安徽科技,1998(4)：31-32.
[46]刘海萍.栀子的化学成分及其质量研究[D].北京：首都师范大学,2007.
[47]马双成,戴忠,J‘丽霞.中药质量标准的研究进展[J].中国药师,2006,9(1)：29.
[48]黄巧文.红外光谱技术对中药鉴别的研究进展[J].海峡药学,2008,20(12)：151-153.
[49]时维静,王甫成,俞浩,等.中药分析与检测[M].北京：化学工业出版社,2010,24-25.
[50]国家药典委员会.中国药典2010年版一部[S].北京：中国医药科技出版社,2009：前言.
[51]高学敏,张建军,张德芹,等.中成药质量标准化建设的现状及展望[J].中国中药杂志,2007,32(9)：868-871.
[52]刘万仓,孙磊,于孟琦,等.中药指纹图谱模式识别研究进展.国际药学研究杂志,2010,37(6)：446-449.
[53]Qiu YQ,Lu X,Pang T,et al.Study of traditional Chinese medicine volatile oils from different geographical origins by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry(GC×GC-TOFMS)in combination with multivariate analysis[J].J Pharm Biomed Anal,2007,43(5):1721.
[54]Cai M,Zhou Y,Gesang S,Chemical fingerprint analysis of rhizomes of Gymnadenia conopsea by HPLC-DAN-MS[J].Chromatogr B Analyt Technol Biomed Life Sci,2006,844:301-307.
[55]Lu HM,Liang YZ,Chen S.Identification and quality as-sessment of houttuynia cordata injection using GC-MS fingerprint:A standardization approach[J].J Ethnopharmacol,2006,105(3):436.
[56]Ren MT,Che J,Song Y,et al. Identification and quantification of 32 bioactive compounds in lonicera species by high performance liquid chromatography coupled with tine-of-fiight mass spectrometry[J].J Pharm Biomed Anal,2008,48(5):1351.
[57]国家药典委员会.中华人民共和国药典(一部)[S]北京：中国医药科技出版社,2010：778.
[58]刘梅,陈其华,刘满祥.显得清冲剂主要成分的薄层鉴别[J].西北药学杂志,1996,11(4)：156-157.
[59]国家药典委员会.中华人民共和国药典(一部)[S]北京：中国医药科技出版社,2010：729.
[60]赵志军,王连水.小柴胡颗粒薄层鉴别及黄芩苷含量测定方法的研究[J].中国实验方剂学杂志,2005, 11(3)：22-23.
[61]苏丽静,吴伟东,余星云小儿清热止咳口服液薄层鉴别方法的改进[J].今日药学,2010,20(6)：45.
[62]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：597.
[63]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：1210.
[64]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：1105.
[65]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：1002.
[66]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：1172.
[67]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：185.
[68]李馨,王金宏,金迪,等.HPLC法测定龙胆中龙胆苦苷的含量[J].黑龙江医药,2010,23(3)：319-321.
[69]张建春,张华,施瑛,等.黄岑苷的研究近况[J].时珍国医国药,2005,16(3)：247-249.
[70]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：89,969,1172.
[71]国家药典委员会.中华人民共和国药典(一部)[S].北京：中国医药科技出版社,2010：282,1134.