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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 simultaneous determination of 18α-glycyrrhizic acid and 18β-glycyrrhizic acid in diammonium glycyrrhizinate raw materials. Methods: The column was Diamonsil C18 (200 mm × 4.6 mm, 5 μm). The mobile phase consisted of aqueous phase (48: 0.5 in water-60% perchloric acid solution and pH 8.0 with aqueous ammonia) 52); detection wavelength: 248 nm; flow rate: 1.0 ml · min-1; column temperature: 30 ℃; injection volume: 20μl. The results showed that 18α-glycyrrhizic acid and 18β-glycyrrhizic acid were separated well. The linear range was 0.005 0-1.000 0 mg · ml-1 (r = 0.999 7 and 0.999 3, respectively). The average recoveries were 99.7% and 99.1% , RSD 0.9% and 0.4% respectively (n = 9). Conclusion: The method is highly specific and accurate, and can be used as the determination of epimers in diammonium glycyrrhizinate raw materials.