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目的:分别建立高效液相色谱法和非水电位滴定法测定盐酸艾咪朵尔含量。方法:高效液相色谱法:色谱柱为KromasilC18(250 mm×4.6 mm,5μm);流动相为甲醇-水-甲酸(36∶64∶0.5,v/v/v),流速1.0 mL.min-1;检测波长为254 nm;柱温30℃。非水电位滴定法以冰醋酸和醋酐为溶剂,用0.1 mol.L-1高氯酸溶液进行滴定。结果:高效液相色谱法:盐酸艾咪朵尔在2.02～50.4μg.mL-1范围内线性关系良好,r=0.9999;方法精密度RSD为0.45%(n=5);平均回收率为100.0%(n=9)。非水电位滴定法:方法精密度RSD为0.13%(n=5);平均回收率为99.8%,RSD为0.15%(n=5)。结论:高效液相色谱法和非水电位滴定法的测定结果在统计学上无显著性差异。高效液相色谱法分离能力高,专属性强,消耗样品量少;非水电位滴定法简单、快速,测定结果精密,准确度高。
OBJECTIVE: To establish HPLC and non-aqueous potentiometric titration method for the determination of amiloride hydrochloride. METHODS: High performance liquid chromatography (HPLC) was performed on a Kromasil C18 column (250 mm × 4.6 mm, 5 μm) with a mobile phase of methanol-water-formic acid (36:64:0.5, v / v / v) 1; detection wavelength is 254 nm; column temperature is 30 ℃. Non-aqueous potentiometric titration with glacial acetic acid and acetic anhydride as solvent, with 0.1 mol.L-1 perchloric acid solution titration. Results: High performance liquid chromatography (HPLC): Amidol hydrochloride showed a good linearity in the range of 2.02 ~ 50.4μg.mL-1, r = 0.9999. The precision RSD was 0.45% (n = 5) % (n = 9). Non-aqueous potentiometric titration: The method has a precision RSD of 0.13% (n = 5), an average recovery of 99.8% and a RSD of 0.15% (n = 5). Conclusion: There is no statistically significant difference between HPLC and non-aqueous potentiometric titration. High performance liquid chromatography with high specificity, strong specificity and low sample consumption; non-aqueous potentiometric titration method is simple, rapid, accurate determination of results, high accuracy.