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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p H至5.0)-乙腈-0.01 mol·L-1庚烷磺酸钠溶液(用冰醋酸调p H至3.9)为流动相,梯度洗脱[0~3 min,A-BC(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 m L·min-1,检测波长230 nm,柱温30℃。结果:法莫替丁质量浓度在31~106μg·m L-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67~229μg·m L-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49~168μg·m L-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 the simultaneous determination of famotidine, amoxicillin and berberine hydrochloride in gastric floating sustained release tablets of compound famotidine. Methods: Kromasil C18 column (4.6 mm × 150 mm, 5 μm) was used in this study. High performance liquid chromatography (HPLC) was performed on a Kromasil C18 column with 0.05 mol·L -1 potassium dihydrogen phosphate solution (adjusted with 2 mol·L -1 sodium hydroxide solution H to 5.0) -acetonitrile-0.01 mol·L -1 sodium heptanesulfonate solution (adjusted to pH 3.9 with glacial acetic acid) as the mobile phase gradient elution [0-3 min, A-BC (47: 6: 47); ABC (47:6:47) → ABC (41:18:41); 11-15 min, ABC (41:18:41) → ABC (37.5:25:37.5); 3 to 11 min; (16.5:45:27.5), ABC (27.5:45:27.5), flow rate 1 m L · min-1, detection wavelength 230 nm The column temperature was 30 ℃. Results: The concentration of famotidine in the range of 31 ~ 106μg · m L-1 showed a good linear relationship with the peak area. The average recoveries (n = 3) were 99.5%, 99.0% and 99.6%, respectively Were 1.9%, 1.8% and 1.8%, respectively. The amoxicillin concentration ranged from 67 to 229μg · m L-1, with a good linear relationship with the peak area. The average recoveries (n = 3) were 101.0% and 99.0% % And 99.2% respectively. The RSDs were 1.6%, 1.0% and 2.3%, respectively. The berberine hydrochloride concentration ranged from 49 to 168μg · m L-1 and had a good linear relationship with the peak area. 3) were 101.1%, 98.7% and 99.2%, respectively, with RSDs of 1.6%, 1.5% and 2.3%, respectively. The contents of famotidine in three batches of samples were 43.2, 42.6 and 43.9 mg · g-1, respectively, the contents of amoxicillin were 332.8, 329.3 and 335.9 mg · g-1, respectively, and the contents of berberine hydrochloride were 329.2 , 327.1 and 330.1 mg · g -1, respectively. Conclusion: This method is validated by methodology, and can be used for quality control of floating sustained release tablets of compound famotidine in stomach.