补肺丸的质量标准研究

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，5 μm），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 5 μg（r=0.999 9），0.030 1~0.752 0 μg（r=0.999 9），0.1459~3.646 4 μg（r=1.000），0.094 3~2.358 4 μg（r=1.000），0.141 6~3.539 2 μg（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 6~0.069 3、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。

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.

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