HPLC法同时测定复方法莫替丁胃内滞留漂浮型缓释片中法莫替丁、阿莫西林和盐酸小檗碱的含量

目的:建立同时测定复方法莫替丁胃内滞留漂浮型缓释片中法莫替丁、阿莫西林和盐酸小檗碱含量的方法。方法:采用高效液相色谱法,使用Kromasil C₁₈色谱柱(4.6 mm×150 mm, 5μm),以0.05 mol·L^-1磷酸二氢钾溶液(用2 mol·L^-1氢氧化钠溶液调pH至5.0)-乙腈-0.01 mol·L^-1庚烷磺酸钠溶液(用冰醋酸调pH至3.9)为流动相,梯度洗脱[0~3 min,A-B-C(47:6:47);3~11 min,A-B-C(47:6:47)→A-B-C(41:18:41);11~15 min,A-B-C(41:18:41)→A-B-C(37.5:25:37.5);15~16 min,A-B-C(37.5:25:37.5)→A-B-C(27.5:45:27.5);16~23 min,A-B-C(27.5:45:27.5)],流速1 mL·min^-1,检测波长230 nm,柱温30℃。结果:法莫替丁质量浓度在31~106 μg·mL^-1范围内,与其峰面积呈良好的线性关系,平均回收率(n=3)分别为99.5%、99.0%和99.6%,RSD分别为1.9%、1.8%和1.8%;阿莫西林质量浓度在67~229 μg·mL^-1范围内,与其峰面积呈良好的线性关系,平均回收率(n=3)分别为101.0%、99.0%和99.2%,RSD分别为1.6%、1.0%和2.3%;盐酸小檗碱质量浓度在49~168 μg·mL^-1范围内,与其峰面积呈良好的线性关系,平均回收率(n=3)分别为101.1%、98.7%和99.2%,RSD分别为1.6%、1.5%和2.3%。3批样品中法莫替丁的含量分别为43.2、42.6和43.9 mg·g^-1,阿莫西林的含量分别为332.8、329.3和335.9 mg·g^-1,盐酸小檗碱的含量分别为329.2、327.1和330.1 mg·g^-1。结论:本法经方法学验证,可用于复方法莫替丁胃内滞留漂浮型缓释片的质量控制。

Objective: To establish a method for determination of famotidine, amoxicillin and berberinein hydrochloride in compound famotidine gastric floating sustained-release tablets. Methods: The HPLC analysis was performed on a Kromasil C₁₈ column (4.6 mm×150 mm, 5 μm) with a mobile phase of monopotassium phosphate (the pH value was adjusted to 5.0 by 2 mol·L^-1 sodium hydroxide solution)-acetonitrile-sodium heptanesulfonate (the pH value was adjusted to 3.9 by glacial acetic acid) using gradient elution [0-3 min, A-B-C(47:6:47); 3-11 min, A-B-C(47:6:47)→A-B-C(41:18:41); 11-15 min, A-B-C(41:18:41)→A-B-C(37.5:25:37.5); 15-16 min, A-B-C(37.5:25:37.5)→A-B-C(27.5:45:27.5); 16-23 min, A-B-C(27.5:45:27.5)] at a flow rate of 1.0 mL·min^-1, the detection wavelength was 230 nm, and the column temperature was 30℃. Results: Good linearig of amotidine, amoxicillin and berberine hydrochloride was achieved in the concentration ranges of 31-106 μg·mL^-1, 67-229 μg·mL^-1 and 49-168 μg·mL^-1, respectively. The average recovery of famotidine (n=3) was 99.5%, 99.0%, 99.6%, and the relative standard deviation was 1.9%, 1.8%, 1.8%, respectively. The average recovery of amoxicillin (n=3) was 101.0%, 99.0%, 99.2%, and the relative standard deviation was 1.6%, 1.0%, 2.3%, respectively. The average recovery of berberine hydrochloride (n=3) was 101.1%, 98.7%, 99.2%, and the relative standard deviation was 1.6%, 1.5%, 2.3%, respectively. In three batches of samples, the content of famotidine was 43.2 mg·g^-1, 42.6 mg·g^-1 and 43.9 mg·g^-1, the content of amoxicillin was 332.8 mg·g^-1, 329.3 mg·g^-1 and 335.9 mg·g^-1, and the content of berberine hydrochloride was 329.2 mg·g^-1, 327.1 mg·g^-1 and 330.1 mg·g^-1. Conclusion: The method is proved to be simple, accurate and reproducible. It can effectively control the quality of compound famotidine gastric floating sustained-release tablets.