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补肺丸的质量标准研究
Study on the quality standard of Bufei pills
【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0.020 9~0.522 5μg(r=0.999 9),0.030 1~0.752 0μg(r=0.999 9),0.1459~3.646 4μg(r=1.000),0.094 3~2.358 4μg(r=1.000),0.141 6~3.539 2μg(r=0.999 9)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0.049 2~0.075 7、0.079 2~0.112 3、0.279 8~0.358 5、0.047 6~0.0693、0.146 2~0.182 1 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。
【Abstract】 Objective:To develop an HPLC method for the simultaneous determination of verbascoside(Rehmannia Glutinosa),scopoletin(Mori Cortex),schisandrin,deoxyschizandrin and γ-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,5 μm)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 and γ-schisandrin had good linearity within the range of 0.020 9-0.522 5 μg(r=0.999 9),0.030 1-0.752 0 μg(r=0.999 9),0.145 9-3.646 4 μg(r=1.000 0),0.094 3-2.358 4 μg(r=1.000 0)and 0.141 6-3.539 2 μg(r=0.999 9),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 0.049 2~0.075 7 mg·g-1 for acteoside,0.079 2~0.112 3 mg·g-1 for scopoletin,0.279 8~0.358 5 mg·g-1 for schisandrin,0.047 6~0.069 3 mg·g-1 for deoxyschizandrin and 0.146 2~0.182 1 mg·g-1 for γ-schisandrin.Conclusion:The methods standard are specific,accurate,which can be used for quality control of Bufei pills.
【Key words】 Bufei pills; acteoside; scopoletin; schisandrin; deoxyschizandrin; γ-schisandrin; TLC; HPLC; quality standard;
- 【文献出处】 药物分析杂志 ,Chinese Journal of Pharmaceutical Analysis , 编辑部邮箱 ,2019年11期
- 【分类号】R286.0
- 【被引频次】1
- 【下载频次】298