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
姚倩 1邓远雄 2李岩 3罗剑 4夏志强 4杜乐4
作者信息
- 1. 湖南师范大学医学院,长沙 410013;长沙晶易医药科技股份有限公司,长沙 410013
- 2. 湖南师范大学医学院,长沙 410013
- 3. 鄂尔多斯市中心医院药剂科,内蒙古 鄂尔多斯 017000
- 4. 长沙晶易医药科技股份有限公司,长沙 410013
- 折叠
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,5 μm)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1.2mL·min-1,进样量为20 μL,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.
Abstract
Objective To determine the related substances in aloe-emodin by HPLC.Methods A Welch Xtimate C18 column(150 mm × 4.6 mm,5 μm)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 20 μL,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Key words
aloe-emodin/HPLC/muti-component content determination/quality control引用本文复制引用
基金项目
湖南省自然科学基金(2020JJ4437)
出版年
2024
NETL
NSTL
万方数据