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目的:研究了离子对反相高效液相色谱法测定小柴胡胶囊制剂中黄芩苷的含量。方法:用50 % 甲醇作溶剂,超声波振荡法提取样品。色谱条件用μBondpak C18 作分析柱,Waters GuardPAK C18 作保护柱,水相( 取庚烷磺酸钠0 .40g ,磷酸二氢钠3 .90g ,冰醋酸20ml ,加水溶解并稀释至1000ml)甲醇(56∶44) 作流动相,流速1ml/min ,UV检测波长为275nm 。结果:黄芩苷与其它组份峰分离良好,柱效高,保留时间约为12min ,在浓度0 .03 ~0 .20mg/ml之间与峰面积(A/107) 呈良好线性关系,回归方程为:A= 0 .008 + 5 .608c ,r = 0 .99996 ,5 次的加样回收率为100 .2 % ,RSD= 0 .84 % ,日内、日间变异( RSD) 分别为0 .86 % 和1 .42 % 。结论:本法简便、准确,适合于制剂中黄芩苷含量的测定
Objective: To study the determination of baicalin in Xiaochaihu Capsules by ion-exchange RP-HPLC. Method: The sample was extracted by ultrasonic shaking with 50% methanol as the solvent. Chromatographic conditions using μ-Bondpak C18 as an analytical column, Waters Guard-PAK C18 as a guard column, and aqueous phase (taking 0.54 g of sodium heptane sulfonate, 3.90 g of sodium dihydrogen phosphate, 20 ml of glacial acetic acid, and adding water to dissolve and dilute to 1000ml)-methanol (56:44) was used as the mobile phase, flow rate was 1ml/min, UV detection wavelength was 275nm. RESULTS: Baicalin was well separated from other components, peak efficiency was high, retention time was about 12 min, and concentration was 0. 03 ~ 0 . A good linear relationship between peak area (A/107) and 20 mg/ml was obtained. The regression equation was: A = 0. 008 + 5 . 608c ,r = 0 . 99996, 5 times the recovery rate of 100. 2%, RSD = 0. 84%, daytime, daytime variation (RSD) were 0. 86% and 1. 42%. Conclusion: This method is simple, accurate and suitable for the determination of baicalin in preparations.