补肺颗粒质量控制研究  

Quality standard of Bufei Granules

作　　者：刘淑[1] 闫晓楠[2] 袁婷婷[1] LIU Shu;YAN Xiao-nan;YUAN Ting-ting(Darentang Pharmaceutical Factory,Tianjin Zhongxin Pharmaceutical Group Co.,Ltd.,Tianjin 300457,China;Institute of Pharmaceutical Research,Tianjin Zhongxin Pharmaceutical Group Co.,Ltd.,Tianjin 300457,China)

机构地区：[1]天津中新药业集团股份有限公司达仁堂制药厂,天津300457 [2]天津中新药业集团股份有限公司药物研究院,天津300457

出　　处：《中草药》2020年第16期4201-4207,共7页Chinese Traditional and Herbal Drugs

基　　金：国家科技重大新药创制专项(2017ZX09301023);天津市科技计划项目新药创制科技重大专项(15ZXXYSY00060)。

摘　　要：目的通过对补肺颗粒进行薄层色谱(TLC)鉴别、含量测定等定性与定量的研究,建立科学合理的补肺颗粒质量控制方法。方法依据处方中各药味的主要化学成分,应用TLC法对其处方中山萸肉、蜜麻黄、赤芍、黄芩、陈皮、甘草进行了定性分析;应用HPLC法测定了补肺颗粒中马钱苷、黄芩苷的含量,并进行了方法学研究,其中马钱苷采用Agilent Eclipse XDB-C18(250 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-甲醇-水-甲酸(10∶1∶89∶0.1),检测波长为236 nm;黄芩苷采用Dikma Diamonsil C18(250 mm×4.6 mm,5μm)色谱柱,流动相为甲醇-水-甲酸(49∶51∶0.1),检测波长为280nm。结果 TLC鉴别方法能特征地鉴别蜜麻黄、赤芍、黄芩、陈皮、甘草,各斑点清晰,阴性无干扰,分离度良好,专属性强。以马钱苷、黄芩苷为指标成分进行方法学研究,马钱苷平均回收率为98.49%,RSD为0.80%;重复性试验RSD为0.83%,符合要求;线性范围在4.76~50.70μg/mL,线性关系良好(r=0.999 9)。黄芩苷平均回收率为101.20%,RSD为0.77%;重复性试验RSD为0.90%,符合要求;线性范围在6.00~96.00μg/mL,线性关系良好(r=0.999 9)。3批样品(批号001、002、003)中马钱苷的含量测定结果分别为12.04、9.78、11.81 mg/袋;黄芩苷的含量测定结果分别为121.13、101.31、103.14 mg/袋。结论该方法易于操作,专属性强,准确灵敏,重复性好,可用于补肺颗粒的质量控制。Objective To establish a scientific and reasonable quality control method of Bufei Granules through the qualitative and quantitative research of thin layer identification and content determination of Bufei Granules. Methods Based on the main chemical constituents of each drug in Bufei Granules, TLC method was used to analyze Corni Fructus, Ephedrae Herba, Paeoniae Radix Rubra, Scutellariae Radix, Citri Reticulatae Pericarpium, and Glycyrrhizae Radix et Rhizoma;HPLC was used to determine the content of loganin and baicalin. The content of loganin was analyzed by Agilent Eclipse XDB-C18 column(250 mm × 4.6 mm, 5 μm) with the mobile phase of acetonitrile-methanol-water-formic acid(10∶1∶89∶0.1). The detection wavelength was set at 236 nm;The content of baicalin was analyzed by Dikma Diamonsil C18 column(250 mm × 4.6 mm, 5 μm) with the mobile phase of methanol-water-formic acid(49∶51∶0.1). The detection wavelength was set at 280 nm. Results The TLC identification method can distinguish Ephedrae Herba, Paeoniae Radix Rubra, Scutellariae Radix, Citri Reticulatae Pericarpium, and Glycyrrhizae Radix et Rhizoma with clear spots, no negative interference, good separation and strong specificity. Loganin and baicalin were used as index components in methodological study. The average recovery of loganin was 98.49% and the RSD was 0.80%;The repeatability test RSD was 0.83% which met the requirement. The linear range was from 4.76 μg/mL to 50.70 μg/mL and the linear relationship was good(r = 0.999 9). The average recovery of baicalinrate was 101.20% and the RSD was 0.77%. The repeatability test RSD was 0.90%, which met the requirements. The linear range was from 6.00 μg/mL to 96.00 μg/mL and the linear relationship was good(r = 0.999 9). The loganin content of three bantches of samples was 12.04, 9.78 and 11.81 mg/bag;And the content determination result of baicalin was 121.13, 101.31 and 103.14 mg/bag. Conclusion The method is easy to operate, strong in specificity, accurate and sensitive, with good repeatabil

关 键 词：补肺颗粒 质量控制 马钱苷 黄芩苷 薄层色谱 HPLC 

分 类 号：R286.02[医药卫生—中药学]