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出 处:《中国药师》2016年第7期1397-1399,共3页China Pharmacist
基 金:河北省科技支撑计划项目(编号:10276430)
摘 要:目的:建立HPLC法同时测定甘草酸二铵原料中差向异构体18α-甘草酸和18β-甘草酸的含量。方法:色谱柱:Diamonsil C18柱(200 mm×4.6 mm,5μm);流动相:水相(水-60%高氯酸溶液为48∶0.5,用氨水调节p H至8.0)-甲醇(48∶52);检测波长:248 nm;流速:1.0 ml·min-1;柱温:30℃;进样量:20μl。结果:18α-甘草酸和18β-甘草酸得到良好分离;线性范围均为0.005 0~1.000 0 mg·ml-1(r分别为0.999 7和0.999 3);平均回收率分别为99.7%和99.1%,RSD分别为0.9%和0.4%(n=9)。结论:该法专属性强,准确度高,可用作甘草酸二铵原料中差向异构体的含量测定。Objective:To establish an HPLC method for the simultaneous determination of 18α-glycyrrhizic acid and 18β-glycyr-rhizic acid in diammonium glycyrrhizinate .Methods:A Diamonsil C18 column (200 mm ×4.6 mm, 5 μm) was used with the mobile phase of water (water-60%perchloric acid solution:48∶0.5, adjusting pH to 8.0 with ammonium hydroxide)-methanol (48∶52). The detection wavelength was set at 248 nm and the flow rate was 1.0 ml· min-1 .The column temperature was 30℃and the injection volume was 20 μl.Results:18α-Glycyrrhizic acid and 18β-glycyrrhizic acid were well separated .They had a good linear relationship within the range of 0.005 0-1.000 0 mg· ml-1(r=0.999 7 and 0.999 3).The average recovery was 99.7%and 99.1%, and RSD was 0.9%and 0.4%, respectively (n=9).Conclusion:The method is accurate, simple and reproducible, which can be used for the simultaneous determination of the two constituents in diammonium glycyrrhizinate .
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