参浮化痰丸质量标准的研究

Quality standard for Shenfu Huatan Pills

目的建立参浮化痰丸(党参、浮小麦、陈皮、防风、黄芩、制半夏等)的质量标准。方法采用薄层色谱法对参浮化痰丸中的陈皮、防风、黄芩进行定性鉴别;采用高效液相色谱法测定制剂中橙皮苷、5-O-甲基维斯阿米醇苷、升麻素苷的质量浓度。橙皮苷和5-O-甲基维斯阿米醇苷的色谱条件为SYMMETRY C18色谱柱(4.6 mm×150 mm,5μm),流动相为乙腈-0.1%磷酸(17∶83),检测波长分别为283 nm和254 nm,柱温为30℃,体积流量为1.0mL/min;升麻素苷的色谱条件为SYMMETRY C18色谱柱(4.6 mm×150 mm,5μm)色谱柱,流动相为甲醇-水(33∶67),检测波长254 nm,柱温30℃,体积流量1.0 mL/min。结果制剂中陈皮、防风、黄芩的薄层斑点清晰,分离度好,专属性强,阴性对照无干扰。橙皮苷在150.0～750.0μg/mL范围内,峰面积与进样质量浓度具有良好的线性关系(r=0.999 9),平均加样回收率为102.63%,RSD为1.29%;5-O-甲基维斯阿米醇苷在99.1～495.6μg/mL范围内,峰面积与进样质量浓度线性关系良好,r=0.999 9,平均加样回收率为102.62%,RSD为1.17%;升麻素苷在7.7～38.6μg/mL范围内,峰面积与进样质量浓度有良好的线性关系(r=0.999 9),平均加样回收率为97.02%,RSD为1.25%。结论所建立的方法可靠、准确、专属性强,可以用于该制剂的质量控制。

AIM To establish the quality standard for Shenfu Huatan Pills （Codonopsis Radix, Tritici Fructus Levis, Cirri reticulatae Pericarpium, Saposhnikoviae Radix, Scutellariae Radix, Pinelliae Rhizoma preparatum, etc. ）. METHODS The TLC method was used to identify Citri reticulatae Pericarpium, Saposhnikoviae Radix and Scutellariae Radix in Shenfu Huatan Pills. The contents of hesperidin, 4＇-0-β -D-glucosyl-5-O-methylvisam-minol and prim-O-glucosylcimifugin were determined by HPLC. The separation of hesperidin and 4＇-O-β-D-glu- cosyl-5-O-methylvisamminol was performed on SYMMETRY Cls column at 30 .C with acetonitrile -0. 1% phos- phoric acid （ 17 ： 83 ） as mobile phase, The detection wavelengthes were set at 283 nm and 254 nm, respectively. The flow rate was at 1.0 mL/min. The separation of prim-O-glucosylcimifugin was performed on SYMMETRY Cis column at 30 .C with methanol-water （33 ： 67） as mobile phase. The detection wavelength was set at 254 nm, and the flow rate was at 1.0 mL/min. RESULTS The developed TLC spots were clear, separation was good, specif- ic, and the negative test showed no interference. Hesperidin in Shenfu Huatan Pills showed a good linear relation- ship in the range of 150.0-750. 0 μg/mL （r = 0. 999 9）. Its average recovery was 102.63% , and RSD was 1.29%. 4＇-O-β-D-glueosyl-5-O-methylvisamminol showed a good linear relationship in the range of 99. 1-495.6 μg/mL （r = 0. 999 9）. Its average reeovery was 102.62% , and RSD was 1.17%. Prim-O-glucosylcimifugin showed a good linear relationship in the range of 7.7-38.6μg/mL （ r = 0. 999 9 ）. Its average recovery was 97.02% , and RSD was 1.25% . CONCLUSION The method is reliable, accurate and specific, and can be used for the quality eontrol of Shenfu Huatan Pills.