[Objectives] To establish a high performance liquid chromatography (HPLC) wavelength switching method for the simultaneous determination of content of six constituents (phellodendrine chloride, gentiopicrin, paeoniflo...[Objectives] To establish a high performance liquid chromatography (HPLC) wavelength switching method for the simultaneous determination of content of six constituents (phellodendrine chloride, gentiopicrin, paeoniflorin, tetrandrine, berberine hydrochloride and paeonol) in Cangbaiqutong capsules, and provide a scientific basis for the comprehensive evaluation of the quality of Cangbaiqutong capsule.[Methods] The chromatographic column of Waters XSELECT CSH-C 18 (4.6 mm × 150 mm, 5 μm), the mobile phase of acetonitrile-0.1% phosphate solution, gradient elution (0-15 min,10%-18% A;15-30 min,18%-50% A;30-35 min, 50%-10% A);the flow rate of 1.0 mL/min, wavelength switching of 284 (0-7 min, phellodendrine), 274 (7-10 min, gentiopicrin), 230 (10-14 min, paeoniflorin) and 274 nm (14-35 min, tetrandrine, berberine hydrochloride, paeonol), the injection volume of 10 μL.[Results] There was a good linear relationship between the area of chromatographic peak and the injection volume of phellodendrine chloride, gentiopicrin, paeoniflorin, tetrandrine, berberine hydrochloride and paeonol in the range of 0.150-1.504, 0.768-7.680, 1.096-10.960, 0.220-2.200, 0.296-2.956, 0.0345-0.345 μg, respectively;the average recovery rates ( n =6) were 98.3%, 99.2%, 98.8%, 98.8%, 99.1% and 98.2%, respectively;the RSD value was 1.32%, 1.46%, 1.08%, 1.31%, 1.26% and 1.21%, respectively.[Conclusions] The method can be used to determine many kinds of constituents at the same time, and the operation is simple, accurate and reproducible, and can be used for the quality control of compound Cangbaiqutong capsules.展开更多
[Objectives]This study was conducted to establish the quality standard of Danshen Jianxin Capsules.[Methods]Orthogonal design was adopted to optimize the water extraction process by taking the amount of water added,ex...[Objectives]This study was conducted to establish the quality standard of Danshen Jianxin Capsules.[Methods]Orthogonal design was adopted to optimize the water extraction process by taking the amount of water added,extraction time and extraction times as factors,and the content of tanshinone I as the index.Salviae Miltiorrhizae,Notoginseng Radix Et Rhizoma and Radix Astragali in the capsules were qualitatively identified by TLC,and the content of tanshinone I in the capsules was determined by HPLC.[Results]The best water extraction process included the steps of adding 12 times of water each time,extracting the materials twice,for 1 h each time.In TLC identification,the test samples showed spots of the same color at the positions corresponding to tanshinone II A,ginsenoside Rg1,notoginsenoside R1 and astragaloside IV reference samples.[Conclusions]Danshen Jianxin Capsules was prepared by the water extraction method,which is characterized by high efficiency and being suitable for mass production.The quality control method is reliable,fast and accurate,which can effectively control the quality of the product.展开更多
Objective To establish a quality control method for simultaneous determination of multiple components in gamboge. Methods A single reference standard for the determination of multiple components （SSDMC） with HPLC wa...Objective To establish a quality control method for simultaneous determination of multiple components in gamboge. Methods A single reference standard for the determination of multiple components （SSDMC） with HPLC was proposed. Seven major components of gamboge including gambogenic acid （S）, β-morellic acid （C1）, 2R-30-hydroxygambogic acid （C2）, isogambogenic acid （C3）, gambogellic acid （C4）, 2R-gambogic acid （C5）, and 2S-gambogic acid （C6） were simultaneously analyzed using gambogenic acid as reference standard. The credibility and feasibility of SSDMC method were validated with respect to linearity, limits of detection and quantification, precision, stability, repeatability, accuracy, ruggedness, and robustness. The relative conversion factors （RCFs） of S and C1-6 were calculated. Twelve batches of gamboge including crude and processed products were successfully analyzed by applying the SSDMC and traditional external standard （ES） methods. Results The SSDMC method was credible and feasible. The RCFs of S and C1-6 were 1.000, 0.913, 0.864, 1.064, 0.777, 0.921, and 0.919, respectively. No significant difference was observed in the contents of the seven components between SSDMC and ES methods. The heat-processing technique caused a reduction in the seven components. Conclusion SSDMC is a simple, reliable, and effective method for the analysis of the complex multiple components in gamboge, and it is also a practical and economical approach.展开更多
目的：建立黄地安消胶囊质量控制的方法。方法：采用薄层色谱法（TLC）对黄地安消胶囊中的黄连、麦冬、葛根、枇杷叶进行定性鉴别研究;采用高效液相色谱法（HPLC）对黄地安消胶囊中君药黄连的活性成分盐酸小檗碱进行含量测定,色谱条件：...目的：建立黄地安消胶囊质量控制的方法。方法：采用薄层色谱法（TLC）对黄地安消胶囊中的黄连、麦冬、葛根、枇杷叶进行定性鉴别研究;采用高效液相色谱法（HPLC）对黄地安消胶囊中君药黄连的活性成分盐酸小檗碱进行含量测定,色谱条件：Agilent Eclipse Plus C18色谱柱（4.6 mm×250 mm,5μm）,流动相：乙腈-0.05 mol·L^-1磷酸二氢钾（30∶70）,流速：1 m L·min^-1,柱温：30℃,检测波长：345 nm。结果：薄层色谱鉴别斑点清晰,易于鉴别;采用HPLC法对黄地安消胶囊中的盐酸小檗碱进行含量测定,盐酸小檗碱在0.235-3.760μg范围内呈良好的线性关系,r=0.9999;平均加样回收率为99.84%,RSD=0.27%。结论：定性鉴别和含量测定方法操作简单,重现性、精密度及稳定性均良好,可用作黄地安消胶囊的质量控制研究方法。展开更多
基金Supported by Lanzhou Talent Innovation and Entrepreneurship Science and Technology Plan Project(2015-RC-22)
文摘[Objectives] To establish a high performance liquid chromatography (HPLC) wavelength switching method for the simultaneous determination of content of six constituents (phellodendrine chloride, gentiopicrin, paeoniflorin, tetrandrine, berberine hydrochloride and paeonol) in Cangbaiqutong capsules, and provide a scientific basis for the comprehensive evaluation of the quality of Cangbaiqutong capsule.[Methods] The chromatographic column of Waters XSELECT CSH-C 18 (4.6 mm × 150 mm, 5 μm), the mobile phase of acetonitrile-0.1% phosphate solution, gradient elution (0-15 min,10%-18% A;15-30 min,18%-50% A;30-35 min, 50%-10% A);the flow rate of 1.0 mL/min, wavelength switching of 284 (0-7 min, phellodendrine), 274 (7-10 min, gentiopicrin), 230 (10-14 min, paeoniflorin) and 274 nm (14-35 min, tetrandrine, berberine hydrochloride, paeonol), the injection volume of 10 μL.[Results] There was a good linear relationship between the area of chromatographic peak and the injection volume of phellodendrine chloride, gentiopicrin, paeoniflorin, tetrandrine, berberine hydrochloride and paeonol in the range of 0.150-1.504, 0.768-7.680, 1.096-10.960, 0.220-2.200, 0.296-2.956, 0.0345-0.345 μg, respectively;the average recovery rates ( n =6) were 98.3%, 99.2%, 98.8%, 98.8%, 99.1% and 98.2%, respectively;the RSD value was 1.32%, 1.46%, 1.08%, 1.31%, 1.26% and 1.21%, respectively.[Conclusions] The method can be used to determine many kinds of constituents at the same time, and the operation is simple, accurate and reproducible, and can be used for the quality control of compound Cangbaiqutong capsules.
基金Supported by Self-financed Scientific Research Project of Administration of Traditional Chinese Medicine of Guangxi Zhuang Autonomous Region(GXZYZ20210290)The First Batch of High-level Talent Research Project of Affiliated Hospital of Youjiang Medical University for Nationalities in 2019(Y20196311)Basic Scientific Research Ability Improvement Project for Young and Middle-aged Teachers in Guangxi Universities in 2020(2020KY13034).
文摘[Objectives]This study was conducted to establish the quality standard of Danshen Jianxin Capsules.[Methods]Orthogonal design was adopted to optimize the water extraction process by taking the amount of water added,extraction time and extraction times as factors,and the content of tanshinone I as the index.Salviae Miltiorrhizae,Notoginseng Radix Et Rhizoma and Radix Astragali in the capsules were qualitatively identified by TLC,and the content of tanshinone I in the capsules was determined by HPLC.[Results]The best water extraction process included the steps of adding 12 times of water each time,extracting the materials twice,for 1 h each time.In TLC identification,the test samples showed spots of the same color at the positions corresponding to tanshinone II A,ginsenoside Rg1,notoginsenoside R1 and astragaloside IV reference samples.[Conclusions]Danshen Jianxin Capsules was prepared by the water extraction method,which is characterized by high efficiency and being suitable for mass production.The quality control method is reliable,fast and accurate,which can effectively control the quality of the product.
基金Science and Technology Commission of Shanghai Municipality(13ZR1442000)Shanghai Municipal Education Commission(2014YSN20)Support Program
文摘Objective To establish a quality control method for simultaneous determination of multiple components in gamboge. Methods A single reference standard for the determination of multiple components （SSDMC） with HPLC was proposed. Seven major components of gamboge including gambogenic acid （S）, β-morellic acid （C1）, 2R-30-hydroxygambogic acid （C2）, isogambogenic acid （C3）, gambogellic acid （C4）, 2R-gambogic acid （C5）, and 2S-gambogic acid （C6） were simultaneously analyzed using gambogenic acid as reference standard. The credibility and feasibility of SSDMC method were validated with respect to linearity, limits of detection and quantification, precision, stability, repeatability, accuracy, ruggedness, and robustness. The relative conversion factors （RCFs） of S and C1-6 were calculated. Twelve batches of gamboge including crude and processed products were successfully analyzed by applying the SSDMC and traditional external standard （ES） methods. Results The SSDMC method was credible and feasible. The RCFs of S and C1-6 were 1.000, 0.913, 0.864, 1.064, 0.777, 0.921, and 0.919, respectively. No significant difference was observed in the contents of the seven components between SSDMC and ES methods. The heat-processing technique caused a reduction in the seven components. Conclusion SSDMC is a simple, reliable, and effective method for the analysis of the complex multiple components in gamboge, and it is also a practical and economical approach.
文摘目的：建立黄地安消胶囊质量控制的方法。方法：采用薄层色谱法（TLC）对黄地安消胶囊中的黄连、麦冬、葛根、枇杷叶进行定性鉴别研究;采用高效液相色谱法（HPLC）对黄地安消胶囊中君药黄连的活性成分盐酸小檗碱进行含量测定,色谱条件：Agilent Eclipse Plus C18色谱柱（4.6 mm×250 mm,5μm）,流动相：乙腈-0.05 mol·L^-1磷酸二氢钾（30∶70）,流速：1 m L·min^-1,柱温：30℃,检测波长：345 nm。结果：薄层色谱鉴别斑点清晰,易于鉴别;采用HPLC法对黄地安消胶囊中的盐酸小檗碱进行含量测定,盐酸小檗碱在0.235-3.760μg范围内呈良好的线性关系,r=0.9999;平均加样回收率为99.84%,RSD=0.27%。结论：定性鉴别和含量测定方法操作简单,重现性、精密度及稳定性均良好,可用作黄地安消胶囊的质量控制研究方法。
