| By extraction and content determination methods,multi-index constituents of 8 kinds of traditional Chinese medicine(TCM), namely Jingzhiguanxin granules, Jingzhiguanxin tablets, Linaoxin capsules,Xinning tablets, Fuyankang tablets,Xiaokeping tablets,Yanyinjiangtang tablets and Shenshua- ining capsules etc.,compound preparations were studied in this paper. Multi-wavelength HPLC analysis on Danshensu,Protocatechuic aldehyde, Salvianolic acid B, TanshinoneⅡA,Paeoniflorin,Ferulic acid, Emodin, Polydatin, Berberine hydrochloride, Puerarin in TCM compound preparations were applied in quantitative analysis. A more economical, reliable, accurate and specific method of quality control was established. This paper was divided into eight parts, the main research contents include:Part one: Study on the methods of HPLC by Simultaneous Determination of the Five Compoents in Jingzhiguanxin GranulesObjective: By optimizing the chromatographic conditions, to establish a method of multi-index content analysis, the components of danshensu, protocatechuic aldehyde, salvianolic acid B,Paeoniflorin and Ferulic acid in Jingzhiguanxin granules were determined simultaneously.Methods:The Agilent Zorbax Eclipse XDB-C18(150mm×4.6mm, 5um) chromatographic separation column was used,mobile phase were composed of acetonitrile(A),methanol(B) and 0.5%H3PO4 aqueous(C)solution in a linear gradient elution mode( 0min : A4%, B1%, C95%; 7min: A4%, B2%, C94%;10min: A15%,B5%, C80%;30min: A22%,B11%,C67%;40min: A30%, B15%, C55%)The flow rate was 1 m L·min-1,and the column temperature was set at 30℃,injection volume was 10 u L.The detection wavelengths were set at 280 nm, 230 nm and 320 nm.Results: There was a good linear relationship over a rang of 33.07-530.00μg·m L-1 for Danshensu, 2.81-44.93μg·m L-1 for Protocatechuic aldehyde, 187.20-2995.20μg·m L-1for Salvianolic acid B, 23.70-379.39μg·m L-1 for Paeoniflorin, 0.20-3.12μg·m L-1 for Ferulic acid respectively. The average recovery were 98.90%, 98.95%, 98.91%, 98.59%, 97.76%, respectively.The average contents of danshensu, protocatechuic aldehyde, salvianolic acid B, Paeoniflorin and Ferulic acid in three different manufacturers were 1.6330 mg·g-1, 1.6640 mg·g-1, 1.6523 mg·g-1, 0.2131 mg·g-1, 0.2135 mg·g-1, 0.2143 mg·g-1, 11.7580 mg·g-1, 11.7529 mg·g-1, 11.7425 mg·g-1, 2.9067 mg·g-1, 2.9018 mg·g-1, 2.8995 mg·g-1, 6.0453×10-3 mg·g-1, 5.9989×10-3 mg·g-1, 5.8555×10-3 mg·g-1.Conclusion:The separation effect is good, operation is simple, convenient,and can achieve better control the quality of the products by the method. Compared the different manufacturers of Jingzhiguanxin granules of 5 kinds of component content, but the difference is not big.Part Two: Study on the methods of HPLC by Simultaneous Determi- nation of the Six Compoents in Jingzhiguanxin TabletsObjective:By optimizing the chromatographic conditions, to establish a method of multi-index content analysis, the components of danshensu, protocatechuic aldehyde, salvianolic acid B, TanshinoneⅡA,Paeoniflorin and Ferulic acid in Refined coronary tablets were determined simultaneously.Methods:The Agilent Zorbax Eclipse XDB-C18(150mm×4.6mm, 5μm) chromatographic separation column was used, mobile phase were composed of acetonitrile(A), methanol(B) and 0.5%H3PO4 aqueous(C)solution in a linear gradient elution mode(0min:A4%, B1%, C95%; 7min:A4%, B2%,C94%; 10min:A15%, B5%, C80%; 30min:A22%, B11%, C67%; 40min:A30%, B15%, C55%; 41min: A80%, C20%; 55min: A80%, C20%). The flow rate was 1 m L·min-1, and the column temperature was set at 30 ℃, injection volume was 10μL. The detection wavelengths were set at 280 nm, 230 nm, 250 nm and 320 nm.Results:There was a good linear relationship over a range of 16.54-530. 00μg·m L-1 for Danshensu,1.44-44.93μg·m L-1 for Protocatechuic aldehyde, 93.60-2995.20μg·m L-1 for Salvianolic acid B, 6.56-210.00μg·m L-1 for TanshinoneⅡA,11.86-379.39μg·m L-1 for Paeoniflorin,0.40-12.48μg·m L-1 Ferulic acid respectively. The average recovery were 98.69%, 8.49%, 98.06%, 98.90%,99.33%,98.24%,respectively.Comparison of the three different manufacturers,the content of 6 kinds of ingredients in Danshen, Danshensu, Protocatechuic aldehyde, Salvianolic acid B,TanshinoneⅡA large difference.Conclusion:The separation effect is good, operation is simple, convenient,and can achieve better control the quality of the products by the method.Different manufacturers of Jingzhiguanxin tablets of 6 kinds of component content have very big difference.Part Three: Study on the methods of HPLC by Simultaneous Determina- tion of the Six Compoents in Linaoxin CapsulesObjective:By optimizing the chromatographic conditions, to establish a method of multi-index content analysis, the components of danshensu, protocatechuic aldehyde, salvianolic acid B,Paeoniflorin, Ferulic acid and Puerarin in Linaoxin capsules were determined simultaneously.Methods:The Agilent Zorbax Eclipse XDB-C18(150mm×4.6mm, 5μm) chromatographic separation column was used, mobile phase were composedof acetonitrile(A), methanol(B)and 0.5%H3PO4 aqueous(C)solution in a linear gradient elution mode( 0min:A4%,B1%, C95%;7min:A4%, B2%,C94%; 10min:A10%,B5%,C85%;35min: A20%,B10%,C70%; 45min: A35%, B10%, C55%; 47min: A35%, B10%, C55%).The flow rate was 1 m L·min-1, and the column temperature was set at 30℃, injection volume was 10μL.The detection wavelengths were set at 280 nm, 230 nm, 250 nm and 320 nm.Results:There was a good linear relationship over a rang of 16.54-264. 58μg·m L-1 for Danshensu,1.44-22.46μg·m L-1 for Protocatechuic aldehyde, 187.20-1497.60μg·m L-1 for Salvianolic acid B,23.71-379.39μg·m L-1 for Paeoniflorin,0.20-1.56μg·m L-1 for Ferulic acid,2.72-42.43μg·m L-1 for Puerarin respectively.The average recovery were 98.37%,98.28%, 98.74%, 98.15%, 98.38%, 98.29%, respectively.Conclusion:The separation effect is good,operation is simple, convenient,and can achieve better control the quality of the products by the method.Part Four:Study on the methods of HPLC by Simultaneous Determin- ation of the Five Compoents in Xinning TabletsObjective:By optimizing the chromatographic conditions, to establish a method of multi-index content analysis, the components of danshensu, protocatechuic aldehyde, salvianolic acid B, Paeoniflorin and Ferulic acid in Xinning tablets were determined simultaneously.Methods:The Agilent Zorbax Eclipse XDB-C18(150mm×4.6mm,5μm) chromatographic separation column was used, mobile phase were composed of acetonitrile(A),methanol(B) and 0.5%H3PO4 aqueous(C)solution in a linear gradient elution mode(0min:A4%,B1%,C95%;7min:A4%, B2%, C94%; 10min:A10%,B5%,C85%;35min:A20%,B10%,C70%;45min:A35%,B10%,C55%;47min: A35%, B10%, C55%).The flow rate was 1 m L·min-1,and the column temperature was set at 30℃, injection volume was 10 u L.The detection wavelengths were set at 280 nm, 230 nm and 320 nm.Results:There was a good linear relationship over a range of 66.14-1060.00μg·m L-1 for Danshensu,5.62-88.86μg·m L-1 for Protocatechuic aldehyde,187.20-2 995.20μg·m L-1for Salvianolic acid B,23.70-379.39μg·m L-1 for Paeoniflorin, 0.20-3.12μg·m L-1 for Ferulic acid respectively. The average recovery were 98.67%, 98.22%, 98.94%, 98.15%,98.96%, respectively.Conclusion:The separation effect is good,operation is simple, convenient,and can achieve better control the quality of the products by the method.Part Five:Study on the methods of HPLC by Simultaneous Determin- ation of the Six Compoents in Fuyankang TabletsObjective:By optimizing the chromatographic conditions, to establish a method of multi-index content analysis, the components of danshensu, protocatechuic aldehyde, salvianolic acid B, Paeoniflorin, Ferulic acid and Berberine hydrochloride in Fuyankang tablets were determined simultaneously.Methods: The Agilent Zorbax Eclipse XDB-C18(150mm×4.6mm, 5μm) chromatographic separation column was used, mobile phase were composed of acetonitrile(A), methanol(B) and 0.5%H3PO4 aqueous(C)solution in a linear gradient elution mode(0min:A4%, B1%, C95%; 7min: A4%, B2%, C94%; 10min: A10%, B5%, C85%;35min: A20%, B10%, C70%; 45min: A35%, B10%, C55%; 50min: A35%, B10%, C55%). The flow rate was 1 m L·min-1, and the column temperature was set at 30 ℃, injection volumewas 10μL. The detection wavelengths were set at 280 nm, 265 nm, 230 nm and 320 nm.Results:There was a good linear relationship over a range of 33.02-528.41μg·m L-1 for Danshensu,2.88-46.13μg·m L-1 for Protocatechuic aldehyde, 187.26-2996.10μg·m L-1for Salvianolic acid B, 11.89-190.22μg·m L-1 for Paeoniflorin, 0.20-3.12μg·m L-1 for Ferulic acid, 39.06-625.00μg·m L-1 for Berberine hydrochloride respectively. The average recovery were 98.71%, 99.04%, 98.83%, 98.50%, 97.08%, 98.12%,respectively.Conclusion:The separation effect is good,operation is simple, convenient, and can achieve better control the quality of the products by the method.Part six:Study on the methods of HPLC by Simultaneous Determination of the Five Compoents in Xiaokeping TabletsObjective:By optimizing the chromatographic conditions, to establish a method of multi-index content analysis, the components of danshensu, protocatechuic aldehyde, salvianolic acid B,Puerarin and Berberine in Xiaokeping tablets were determined simultaneously. TheMethods:Agilent Zorbax Eclipse XDB-C18(150mm×4.6mm,5μm) chromatographic separation column was used, mobile phase were composed of acetonitrile(A),methanol(B) and 0.5%H3PO4 aqueous(C)solution in a linear gradient elution mode(0min: A4%, C96%; 7min: A4%, B1%, C95%; 20min:A10%, B3%, C87%;30min: A15%,B3%,C82%; 45min: A25%, B10%, C65%; 60min: A30%, B10%, C60%).The flow rate was 1 m L·min-1, and the column temperature was set at 30 ℃,injection volume was 10μL. The detection wave length were set at 280 nm,250 nm and 265 nm.Results:There was a good linear relationship over a rang of33.02-528.41μg·m L-1 for Danshensu, 1.44-22.46μg·m L-1 for Protocatechuic aldehyde,374.51-5992.20μg·m L-1for Salvianolic acid B,84.86-1357.82 μg·m L-1for Puerarin,312.50-5000.00μg·m L-1 for Berberine hydrochloride respectively. The average recovery were 98.24%, 98.37%, 98.86%, 98.93%, 99.04%, respectively.Conclusion:The separation effect is good, operation is simple, convenient,and can achieve better control the quality of the products by the method.Part Seven:Study on the methods of HPLC by Simultaneous Determin- ation of the Four Compoents in Yangyinjiangtang TabletsObjective: By optimizing the chromatographic conditions, to establish a method of multi-index content analysis, the components of Puerarin,Polydatin, Ferulic acid and emodin in Yangyinjiangtang tablets were determined simultaneously.Methods:The Agilent Zorbax Eclipse XDB-C18(150mm×4.6mm, 5μm) chromatographic separation column was used, mobile phase were composed of acetonitrile(A),methanol(B) and 0.5%H3PO4 aqueous(C)solution in a linear gradient elution mode(0min:A10%, B5%, C85%; 10min: A20%, B5%, C75%; 20min:A25%, B5%,C70%;30min: A30%, B7%, C53%; 40min:A50%, B30%, C20%; 55min: A50%, B30%,C20%).The flow rate was 0.6 m L·min-1, and the column temperature was set at 30 ℃, injection volume was 10μL.The detection wave length were set at 250 nm, 306 nm,254nm and 320 nm.Results:There was a good linear relationship over a rang of 42.43-678. 91μg·m L-1 for Puerarin,150.00-2400.00μg·m L-1 for Polydatin, 0.39-6.26 μg·m L-1for Ferulic acid, 62.50-1000.00μg·m L-1 for Emodin respectively.Theaverage recovery were 98.59%, 99.12%, 98.96%, 98.89%, respectively.Conclusion:The separation effect is good, operation is simple, convenient, and can achieve better control the quality of the products by the Method.Part eight:Study on the methods of HPLC by Simultaneous Determin- ation of the Four Compoents in Shenshuaining CapsulesObjective: By optimizing the chromatographic conditions, to establish a method of multi-index content analysis, the components of danshensu, protocatechuic aldehyde, salvianolic acid B and emodin in Shenshuaining capsules were determined simultaneously.Methods: The Agilent Zorbax Eclipse XDB-C18(150mm×4.6mm, 5μm) chromatographic separation column was used, mobile phase were composed of acetonitrile(A), methanol(B) and 0.5%H3PO4 aqueous(C) solution in a linear gradient elution mode(0min:A3%, C97%; 10min: A5%, C95%; 15min: A10%, B2%, C88%; 20min:A20%, B5%, C75%; 30min: A30%, B10%, C60%; 40min: A35%, B10%, C55%;50min: A45%,B15%, C40%; 60min: A55%, B20%, C25%). The flow rate was 1 m L·min-1, and the column temperature was set at 30 ℃, injection volume was 10μL. The detection wave-length were set at 280 nm and 254 nm.Results:There was a good linear relationship over a range of 66.79-1068.64μg·m L-1 for Danshensu,5.63-90.15μg·m L-1 for Protocatechuic aldehyde,748.80-11980.80μg·m L-1for Salvianolic acid B,500.00- 8067.68 μg·m L-1 for Emodin respectively. The average recovery were 98.24%, 98.55%, 98.37%, 99.44%, respectively.Conclusion:The separation effect is good, operation is simple, convenient,and can achieve better control the quality of the products by themethod. |
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