高效液相色谱法测定芦荟大黄素的有关物质  

Determination of aloe-emodin related substances by HPLC

作　　者：姚倩 邓远雄[1] 李岩 罗剑 夏志强 杜乐 YAO Qian;DENG Yuan-xiong;LI Yan;LUO Jian;XIA Zhi-qiang;DU Le(School of Medicine,Hunan Normal University,Changsha 410013;Changsha King-eagle Medical Science and Technology Co.,Ltd.,Changsha 410013;Department of Pharmacy,Ordos Central Hospital,Ordos Inner Mongolia 017000)

机构地区：[1]湖南师范大学医学院,长沙410013 [2]长沙晶易医药科技股份有限公司,长沙410013 [3]鄂尔多斯市中心医院药剂科,内蒙古鄂尔多斯017000

出　　处：《中南药学》2024年第4期1076-1079,共4页Central South Pharmacy

基　　金：湖南省自然科学基金项目(No.2020JJ4437)。

摘　　要：目的 建立HPLC法测定芦荟大黄素中有关物质的含量。方法 采用HPLC法分析,色谱柱为Welch Xtimate C18(150 mm×4.6 mm,5μm)柱;以pH 2.0磷酸盐缓冲液-甲醇-乙腈为流动相,梯度洗脱;流速为1.2 mL·min^(-1),进样量为20μL,柱温为30℃,检测波长为254 nm。结果 芦荟大黄素与其有关物质的色谱峰均能良好分离,精密度试验表明,当杂质含量<0.1%,12份样品的RSD<13%;当杂质含量≥0.1%,12份样品的RSD<4.0%,方法精密度良好。同一厂家6批芦荟大黄素样品测定结果显示,最大单杂为已知杂质大黄醛,含量1.42%,杂质总含量小于5.0%,但不同批样品间杂质存在差异。结论 建立的方法灵敏、专属性强,准确度高,可用于芦荟大黄素有关物质的测定。Objective To determine the related substances in aloe-emodin by HPLC.Methods A Welch Xtimate C18 column(150 mm×4.6 mm,5μm)was used with a mobile phase consisted of pH 2.0 phosphate buffer-methanol-acetonitrile in the gradient elution.The flow rate was maintained at 1.2 mL·min^(-1),with an injection volume of 20μL,a column temperature of 30℃,and detection wavelength at 254 nm.Results Aloe-emodin and its related substances were well separated.Experiments revealed excellent precision,with a maximum relative standard deviation(RSD)below 13%when the impurity content was below 0.1%.When the impurity content≥0.1%,the maximum RSD among the 12 parts tested was below 4.0%.The predominant single impurity as rhubarb aldehyde was identified in 6 batches of aloe-emodin samples from the same manufacturer,with a content of 1.42%.The total impurity content in these samples was less than 5.0%,with variations in the impurity profiles among different batches.Conclusion This method is sensitive,specific,and accurate,which is suitable for the detection of related substances in aloe-emodin and control its quality.

关 键 词：芦荟大黄素 高效液相色谱 多组分含量测定 质量控制 

分 类 号：R917[医药卫生—药物分析学]