HPLC法同时测定甘草酸二铵制剂中18α和18β甘草酸二铵含量  

Simultaneous Determination of 18α-Glycyrrhizic Acid and 18β-Glycyrrhizic Acid in Diammonium Glycyrrhizinate Preparation by HPLC

作　　者：张轶华 田晓彤 孙婷 高燕霞 李挥 ZHANG Yihua;TIAN Xiaotong;SUN Ting;GAO Yanxia;LI Hui(Hebei Institute for Drug and Medical Device Control,Shijiangzhuang,Hebei,China 050200)

机构地区：[1]河北省药品医疗器械检验研究院,河北石家庄050200

出　　处：《中国药业》2021年第12期56-59,共4页China Pharmaceuticals

基　　金：河北省科学技术研究与发展计划项目[10276430]。

摘　　要：目的建立同时测定甘草酸二铵制剂中差向异构体18α甘草酸二铵和18β甘草酸二铵含量的高效液相色谱法。方法色谱柱为Diamonsil C18柱(200 mm×4.6 mm,5μm),流动相为水-60%高氯酸溶液(48∶0.5,V/V,用氨水调pH至8.0)-甲醇(48∶52,V/V),流速为1.0 m L/min,检测波长为248 nm,柱温为25℃,进样量为20μL。结果18α甘草酸二铵和18β甘草酸二铵的质量浓度均在0.005~1.000 mg/m L范围内与峰面积线性关系良好(r=0.9997,0.9993,n=7),精密度、稳定性、重复性试验结果的RSD均小于1.0%;不同厂家、不同批号(剂型)3批制剂样品中18α甘草酸二铵和18β甘草酸二铵的平均回收率分别为99.57%和99.70%,99.80%和99.66%,99.48%和99.55%,RSD分别为0.81%和0.95%,0.47%和0.71%,0.49%和0.90%;不同制剂中18α甘草酸二铵和18β甘草酸二铵的含量均不同。结论所建立的方法专属性强,准确度高,可为控制甘草酸二铵制剂中的差向异构体提供参考,也为甘草酸二铵差向异构体的进一步研究奠定了基础。Objective To establish a high-performance liquid chromatography(HPLC)method for simultaneous determination of epimer(18α-glycyrrhizic acid and 18β-glycyrrhizic acid)in Diammonium Glycyrrhizinate Preparation.Methods The chromatographic column was Diamonsil C18 column(200 mm×4.6 mm,5μm),the mobile phase was water-60%perchloric acid solution(48∶0.5,V/V,p H was adjusted to 8.0 with ammonium hydroxide)-methanol(48∶52,V/V),the flow rate was 1.0 m L/min,the detection wavelength was248 nm,the column temperature was 25℃,and the injection volume was 20μL.Results The linear range of 18α-glycyrrhizic acid and 18β-glycyrrhizic acid was 0.005-1.000 mg/m L(r=0.9997,0.9993,n=7).The RSDs of precision,stability and repeatability tests were less than 1.0%.The average recoveries of 18α-glycyrrhizic acid and 18β-glycyrrhizic acid in the samples with different lot numbers(dosage forms)from different manufacturers were 99.57%,99.70%,99.80%,99.66%,99.48%,99.55%with RSDs of0.81%,0.95%,0.47%,0.71%,0.49%,0.90%,respectively.The contents of 18α-glycyrrhizic acid and 18β-glycyrrhizic acid in different preparations were different.Conclusion The established method has strong specificity and high accuracy,which can provide a reference for the control of epimers in diammonium glycyrrhizinate preparations and provide a basis for the further study of diammonium glycyrrhizinate epimers.

关 键 词：高效液相色谱法 甘草酸二铵 差向异构体 18α甘草酸二铵 18β甘草酸二铵 含量测定 

分 类 号：R927.2[医药卫生—药学]