基于一测多评法的长城感冒片质量控制

目的：建立一测多评法同时测定长城感冒片中连翘酯苷B、连翘酯苷A、连翘苷、木犀草苷、木犀草素、紫花前胡苷、羌活醇、异欧前胡素的含量，并验证此方法用于长城感冒片中8个指标成分测定的可行性。方法：该药物70%甲醇提取液的分析采用Kromasil C₁₈色谱柱（250 mm×4.6 mm，5 μm）；流动相乙腈-0.2%磷酸溶液，梯度洗脱；流速1.0 mL·min^-1；检测波长275 nm（连翘酯苷B、连翘酯苷A、连翘苷）、350 nm（木犀草苷、木犀草素）、315 nm（紫花前胡苷、羌活醇、异欧前胡素）；柱温30℃；以连翘苷为内参物，建立其他7个待测成分的相对校正因子，并用2台不同品牌的色谱仪和3种不同的色谱柱对建立的相对较正因子的耐用性进行考察，用建立的校正因子进行计算，完成一测多评法含量测定。同时采用常规的外标法对这8个成分进行含量测定。结果：连翘酯苷B、连翘酯苷A、连翘苷、木犀草苷、木犀草素、紫花前胡苷、羌活醇和异欧前胡素质量浓度分别在3.780~94.50、14.67~366.8、4.860~121.5、1.990~49.75、1.660~41.50、4.070~101.8、1.090~27.25、9.470~236.8 μg·mL^-1范围内线性关系良好；以连翘苷为内参物，测得的相对校正因子值分别为1.052 3、1.384 9、1.381 9、1.840 1、0.904 3、2.322 9和1.216 9，且建立的一测多评法与外标法测定结果无显著性差异，一测多评法可以替代外标法。结论：利用相对校正因子对长城感冒片中8个成分的含量测定是可行的，一测多评法可以用于长城感冒片的质量评价研究。

Objective: To establish a simultaneous determination method of forsythoside B,forsythoside A,forsythin,luteolin-7-glucoside,luteolin,nodakenin,notopterol and isoimperatorin in Changcheng Ganmao tablets with strategy of multi-components by single-marker(QAMS)and validate its feasibility. Methods: The analysis of 70% methanol extract of this drug was performed on a thermostatic Kromasil C₁₈ column(250 mm×4.6 mm,5 μm)at 30℃. The mobile phase consisted of acetonitrile-0.2% phosphoric acid solution at a flow rate of 1.0 mL·min^-1 in a gradient elution manner. The detection wavelength were set at 275 nm(forsythoside B,forsythoside A and forsythin),350 nm(luteolin-7-glucoside and luteolin)and 315 nm(nodakenin,notopterol and isoimperatorin). The relative correction factors(RCFs)of other components were calculated with forsythin as the internal reference. Then durability of the RCFs was investigated with 2 different HPLC instruments and 3 columns. Meanwhile,contents of 8 components were determined by conventional external standard method. Results: The standard curves of forsythoside B,forsythoside A,forsythin,luteolin-7-glucoside,luteolin,nodakenin,notopterol and isoimperatorin showed good linearity in 3.78-94.50,14.67-366.75,4.86-121.50,1.99-49.75,1.66-41.50,4.07-101.75,1.09-27.25,9.47-236.75 μg·mL^-1,respectively. With forsythin as the internal reference standard,the relative correction factors were 1.052 3,1.384 9,1.381 9,1.840 1,0.904 3,2.322 9 and 1.216 9,respectively. The results determined by two methods were compared without significant differences. So QAMS can replace external standard method. Conclusion: The use of relative correction factor is feasible to determine the contents of eight components in Changcheng Ganmao tablets. The QAMS method can be used for the quality evaluation of Changcheng Ganmao tablets.

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