补肺丸的质量标准研究  

Study on the quality standard of Bufei pills

作　　者：蔡蕤 陈忠东[1] 张寒娟[1] 洪岩 CAI Rui;CHEN Zhong-dong;ZHANG Han-juan;HONG Yan(Department of Pharmacy,Zhengzhou No.7 People’s Hospital,Zhengzhou 450016,China)

机构地区：[1]郑州市第七人民医院药学部

出　　处：《药物分析杂志》2019年第11期2098-2105,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立同时测定补肺丸中毛蕊花糖苷(熟地黄)、东莨菪内酯(桑白皮)、五味子醇甲、五味子甲素、五味子乙素(五味子)的高效液相色谱方法和党参、黄芪、紫菀、桑白皮的薄层鉴别方法,为全面控制和提高补肺丸的质量标准提供实验依据。方法:Agilent-C18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈(A)-0.1%磷酸(B),梯度洗脱(0~5 min,15%A→25%A;5~20 min,25%A→26%A;20~30 min,26%A→40%A;30~40 min,40%A→46%A;40~41 min,46%A→55%A;41~71 min,55%A→63%A;71~75 min,63%A),流速1.0 mL·min^-1;柱温30℃,检测波长0~30 min(334 nm),30~75 min(215 nm)。结果:各药材薄层色谱斑点清晰,阴性无干扰;毛蕊花糖苷、东莨菪内酯、五味子醇甲、五味子甲素和五味子乙素分别在0.0209~0.5225μg(r=0.9999),0.0301~0.7520μg(r=0.9999),0.1459~3.6464μg(r=1.000),0.0943~2.3584μg(r=1.000),0.1416~3.5392μg(r=0.9999)范围内线性关系良好,平均回收率分别为92.2%(RSD=1.6%)、92.6%(RSD=2.1%)、96.9%(RSD=2.4%)、96.8%(RSD=2.9%)和88.8%(RSD=1.3%),6批样品中上述5个成分的含量范围分别为0.0492~0.0757、0.0792~0.1123、0.2798~0.3585、0.0476~0.0693、0.1462~0.1821 mg·g^-1。结论:本法具有较强的专属性,准确度高,可以用于补肺丸药品质量的控制。Objective:To develop an HPLC method for the simultaneous determination of verbascoside(Rehmannia Glutinosa),scopoletin(Mori Cortex),schisandrin,deoxyschizandrin andγ-schisandrin(Schisandra Chinensis Fructus)and a TLC method for identification of Codonopsis Radix,Astragali Radix,Asteris Radix et Rhizoma and Mori Cortex,in order to provide experimental data for comprehensive control and improvement of Bufei pills quality standard.Methods:The separation was performed on an Agilent Welch-C18(4.6 mm×250 mm,5μm)column with acetonitrile(A)-0.1%phosphoric acid(B)as the mobile phase in the gradient elution(0-5 min,15%A→25%A;5-20 min,25%A→26%A;20-30 min,26%A→40%A;30-40 min,40%A→46%A;40-41 min,46%A→55%A;41-71 min,55%A→63%A;71-75 min,63%A).The flow rate was 1.0 mL·min^-1,the detection wavelength was 334 nm(0-30 min)and 215 nm(30-75 min),and the column temperature was maintained at 30℃.Results:The TLC spots of each crude drug were clear without interference from negative samples.Verbascoside,scopoletin,schisandrin,deoxyschizandrin andγ-schisandrin had good linearity within the range of 0.0209-0.5225μg(r=0.9999),0.0301-0.7520μg(r=0.9999),0.1459-3.6464μg(r=1.0000),0.0943-2.3584μg(r=1.0000)and 0.1416-3.5392μg(r=0.9999),respectively.The average recoveries were 92.2%(RSD=1.6%),92.6%(RSD=2.1%),96.9%(RSD=2.4%),96.8%(RSD=2.9%)and 88.8%(RSD=1.3%),respectively.The contents of five components in six batches of samples were 0.0492~0.0757 mg·g^-1 for acteoside,0.0792~0.1123 mg·g^-1 for scopoletin,0.2798~0.3585 mg·g^-1 for schisandrin,0.0476~0.0693 mg·g^-1 for deoxyschizandrin and 0.1462~0.1821 mg·g^-1 forγ-schisandrin.Conclusion:The methods standard are specific,accurate,which can be used for quality control of Bufei pills.

关 键 词：补肺丸 毛蕊花糖苷 东莨菪内酯 五味子醇甲 五味子甲素 五味子乙素 薄层色谱 高效液相色谱 质量标准 

分 类 号：R917[医药卫生—药物分析学]