| Promoting blood circulation to remove blood stasis is one of theimportant theory and treatment principle of traditional Chinese medicine(TCM)."regulating the blood, recuperating the body " which is recorded inNeijing, has become the foundation of principle of diagnosis of promotingblood circulation to remove blood stasis for later generations.Following the further research of TCM for promoting blood circulation toremove blood stasis, which has discovered with the pharmacological effects inimproving hemodynamic disorder, hemorheological disorder, microcirculationdisturbance, anti-thrombus formation, anti-atherosclerosis, myocardialischemia, suppress tissue dysplasia. It is widely used in clinical departments,related to dozens of diseases including cardiovascular and cerebrovasculardiseases, diabetes, liver cirrhosis and tumor. The clinical efficacy is significant,showing a good application prospect.Just because of a wide range of applications in clinic, TCM preparation isalways with spotty quality. In order to guarantee the safety and efficacy ofcompound preparations of TCM, the quality control methods and means hasbecome one of the most important research topics for TCM modernization.The foreign chemical drug quality control mode is used by current TCMquality control pattern for reference. The chemicals with a specific molecularstructure and clearly structure-activity relationship, that identification,examination and content determination can be directly used as a qualityevaluation index. But for the guidance of TCM theory of Chinese medicine,especially compound preparations, detecting of any kind of composition can’treflect the overall quality. Hence, it is needed to re-examine and specific aims,strategies, patterns and methods of TCM quality, and set up a set of stable and controllable new TCM quality control management system which can directlyreflect safety and effectiveness."Chinese Pharmacopoeia"2010version TCMpart referred to content determination of the quality control of TCMcomposition that one is the active ingredient and one is the index composition,which is either active ingredient or inactive ingredient. Since the1970s, highperformance liquid chromatography (HPLC) with its unique advantages incontent determination (high separation efficiency, fast analysis speed, goodreproducibility, wide mobile phase selectivity, chromatographic column usedrepeatedly), applies massively in quality control of effective components andindex components which occupies very important position in quality controlof TCM. With the popularity of HPLC method application,2010"ChinesePharmacopoeia" carries up to709content determination method of TCM areused HPLC method.In order to make the compound preparation of TCM for promoting bloodcirculation to remove blood stasis to get safety and wide application, the indexcomponent of quality control is the major objective of our research. Thequality control of medicine is the basic attributes of it, of the foundation ofsafety and effectiveness of medicine.Quality standard is the important way to control the quality of medicine,which can effectively control the quality of the medicine and ensure the safetyof the medicine. It is the concrete reflection of the quality control. This subjectselects common TCM for promoting blood circulation to remove blood stasisin Tangshan worker Hospital as object of study, which containing variouscomponents of Danshensu，Protocatechuic aldehyde，Paeoniflorin，Ferulicacid，Dan phenolic acid B in Shenshao oral liquid (hospital preparation),Qilong capsule, Yixinshu capsule, Xiaoshuantongluo capsule（three kinds ofcommercially available varieties）. It is used HPLC to do comparativelymethodological systematic research on quality control of effective componentsin the compound preparations. It is with high specificity, good precision andstability, accurate and reliable experimental results which can providescientific and effective experimental method and basis for compound preparation of TCM for promoting blood circulation to remove blood stasis.Part one: Determinations of the Danshensu，Protocatechuic aldehydePaeonifl-orin，Ferulic acid，Dan phenolic acid B in Shenshao Oral Liquor byMultiple wavelength RP-HPLC methodObjective：A RP-HPLC was established for the quantitative analysis offive effective components (Danshensu，Protocatechuic aldehyde，Paeoniflorin，Ferulic acid，Dan phenolic acid B) in shenshao oral liquid, It provides thebasis for the quality control of shenshao oral liquid.Methods: The chromatographic column was Eclipse XDB-C18(4.6mm*150mm,5μm, agilent), the mobile phase was0.5%phosphoric acid aqueoussolution (A)-methanol (B)-acetonitrile (C) with gradient elution; The flowrate:1.0mL/min; The detection wavelength:280nm,230nm,320nm;Thecolumn temperature:30℃; The samplequantity for10μL.Results: Five kinds of components under the chromatographic conditionscan be completely separated, the linear range of Danshensu，Protocatechuicaldehyde，Paeoniflorin，Ferulic acid，Dan phenolic acid B respectively were:24~384μg/mL (r2=1),1.25~20μg/mL (r2=0.9998),40.5~648μg/mL (r2=0.9996),1.5~24μg/mL (r2=0.9999),145~2320μg/mL (r2=0.9999), theaverage recovery rate were100.8%(RSD=1.29%),100.2%(RSD=2.27%),99.6%(RSD=0.93%),100.2%(RSD=1.18%),99.3%(RSD=2.46%)respectively.Conclusions: The content determination method by multiple wavelengthRP-HPLC was established of the five effective components in shenshaoliquid (Danshensu，Protocatechuic aldehyde，Paeoniflorin，Ferulic acid，Danphenolic acid B). The method has good specificity, precision and accuracy,which can be used for the comprehensive quality control of shenshao oralliquid. Part two: The contents determination of Danshensu，Protocatechuicaldehyde，Paeoniflorin，Ferulic acid，Dan phenolic acid B in qilong capsule byMultiwa-velength reversed phase high performance liquid chromatographymethodObjective: A reversed phase high performance liquid chromatographymethod was established for the contents determination of Danshensu，Protocatechuic aldehyde，Paeoniflorin，Ferulic acid，Dan phenolic acid B inqilong capsule, It provides the reference for the quality control of thepreparations.Methods: The chromatographic column was Eclipse XDB-C18(4.6mm*150mm,5μm, agilent), the mobile phase was0.5%phosphoric acid aqueoussolution (A)-methanol (B)-acetonitrile (C) with gradient elution; The flowrate:1.0mL/min; The detection wavelength:280nm,230nm,320nm;Thecolumn temperature:30℃; The sample quantity for10μL.Results: Five kinds of components under the chromatographic conditionscan be completely separated, the linear range of Danshensu，Protocatechuicaldehyde，Paeoniflorin，Ferulic acid，Dan phenolic acid B respectively were:4.24~132.29μg/mL (r2=1),0.36~11.232μg/mL (r2=0.9998),23.712~379.392μg/mL (r2=1),0.7~11.2μg/mL (r2=0.9999),200~3200μg/mL (r2=0.9998), the average recovery rate were100.1%(RSD=1.40%),99.9%(RSD=2.70%),99.8%(RSD=1.47%),102.0%(RSD=3.11%),99.9%(RSD=1.41%) respectively.Conclusions: By the simple method,the five components showed a goodseparation effect,and the method can be used for the quality control of qilongcapsules. Part three: The contents determination of Danshensu， Protocatechuicaldehyde，Ferulic acid，Dan phenolic acid B in yixinshu capsule by Multiwave -length HPLC-DAD methodObjective: A HPLC-DAD method was established for the contentsdetermination of Danshensu，Protocatechuic aldehyde， Ferulic acid，Danphenolic acid B in yixinshu capsule, It provides the reference for the qualitycontrol of the preparations.Methods: The chromatographic column was Eclipse XDB-C18(4.6mm*150mm,5μm, agilent), the mobile phase was0.5%phosphoric acid aqueoussolution (A)-methanol (B)-acetonitrile (C) with gradient elution; The flowrate:1.0mL/min; The detection wavelength:280nm,320nm;The columntemperature:30℃; The sample quantity for10μL.Results: Four kinds of components under the chromatographic conditionscan be completely separated, the linear range of Danshensu，Protocatechuicaldehyde， Ferulic acid，Dan phenolic acid B respectively were:9~144μg/mL (r2=0.9999),0.5~8μg/mL (r2=0.9998),0.65~10.4μg/mL (r2=0.9997),221.25~3540μg/mL (r2=0.9997), the average recovery rate were100.7%(RSD=1.75%),100.3%(RSD=2.89%),100.2%(RSD=3.16%),99.7%(RSD=2.04%).Conclusions: The content determination method by multiple wavelengthHPLC-DAD was established of Danshensu，Protocatechuic aldehyde，Ferulicacid，Dan phenolic acid B in yixinshu capsule. The method has goodfeasibility and reproducibility, which can be used for the quality control ofyixinshu capsule. Part four: The contents determination of Danshensu，Protocatechuicaldehyde，Ferulic acid, Dan phenolic acid B in xiaoshuantongluo capsule byMultiwavel-ength high performance liquid chromatographyObjective:A Multiwavelength high performance liquid chromatographymethod was established for the Quantitative analysis of Danshensu，Protocatechuic aldehyde， Ferulic acid， Dan phenolic acid B in xiaoshuantongluo capsule, It provides the reference for the quality control ofthe preparations.Methods: The chromatographic column was Eclipse XDB-C18(4.6mm*150mm,5μm, agilent), the mobile phase was0.5%phosphoric acid aqueoussolution (A)-methanol (B)-acetonitrile (C) with gradient elution; The flowrate:1.0mL/min; The detection wavelength:280nm,320nm;The columntemperature:30℃; The sample quantity for10μL.Results: Four kinds of components under the chromatographic conditionscan be completely separated, the linear range of Danshensu，Protocatechuicaldehyde， Ferulic acid，Dan phenolic acid B respectively were:12~192μg/mL (r2=0.9998),1~16μg/mL (r2=0.9999),0.4~6.4μg/mL (r2=0.9999),62.5~1000μg/mL (r2=0.9999), the average recovery rate were100.8%(RSD=1.47%),100.3%(RSD=2.81%),101.4%(RSD=2.53%),99.9%(RSD=1.92%).Conclusions: The content determination method by multiple wavelengthhigh performance liquid chromatography was established of Danshensu，Protocatechuic aldehyde， Ferulic acid， Dan phenolic acid B inxiaoshuantongluo capsule. The method has good separation and accuracy,which can be used for the quality control of xiaoshuantongluo capsule. |
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