HPLC-FLD测定辛芩颗粒中的马兜铃酸I  

Determination of Aristolochic Acid I in Xinqin Granules by HPLC-FLD

作　　者：颜淑婷 马铭[2] 丁芳林[1] 文星星 周芳 姜放军[1] 张朝辉[1] YAN Shuting;MA Ming;DING Fanglin;WEN Xingxing;ZHOU Fang;JIANG Fangjun;ZHANG Zhaohui(Hunan Biological and Electromechanical Polytechnic,Changsha 410127,China;Key Lab.of Chemical Biology and Traditional Chinese Medicine Research,Hunan Normal University,Changsha 410081,China)

机构地区：[1]湖南生物机电职业技术学院,湖南长沙410127 [2]湖南师范大学化学生物学及中药分析教育部重点实验室,湖南长沙410081

出　　处：《中国野生植物资源》2025年第2期41-47,共7页Chinese Wild Plant Resources

基　　金：湖南省自然科学基金科教联合项目(2022JJ60070);湖南省教育厅科学研究一般项目(22C1054)。

摘　　要：目的:建立锌粉还原衍生、高效液相色谱-荧光检测法(HPLC-FLD)测定辛芩颗粒中马兜铃酸I(AA-I)的分析方法。方法:采用超声波法提取样品后,在酸性条件下用锌粉将提取液中无荧光的AA-I还原衍生成具有荧光的马兜铃内酰胺I(AL-I),再通过比较衍生前后HPLC-FLD检测结果之差求得AA-I的含量。结果:最佳衍生反应条件为:酸性条件下,室温反应15 min。在最佳条件下,AA-I在0.001~0.400μg/mL范围内线性关系良好,R^(2)为0.9936,低、中、高3个浓度基质加标的相对回收率在91.9%~107.8%之间,RSD小于8.1%。采用该方法测得3批次辛芩颗粒样品中AA-I的平均含量在0.59~0.66μg/g之间。结论:本研究建立的方法灵敏、快速,可为中药制剂中AA-I含量的准确测定提供参考。Objective:To establish a method for the determination of aristolochic acid I(AA-I)in Xinqin granules by zinc powder reduction derivatization and high-performance liquid chromatographyfluorescence detection(HPLC-FLD).Methods:After extracting the samples using the ultrasonic method,the extract was subjected to a reduction-derivatization process under acidic conditions with zinc powder to convert non-fluorescent AA-I into fluorescent aristololactam I(AL-I).By comparing the differences in HPLC-FLD detection results before and after derivatization,the content of AA-I could be determined.Results:The optimal derivatization reaction conditions were established as follows:the reaction was conducted at room temperature for 15 min under acidic conditions.Under optimal conditions,the method demonstrated a broad linear range of 0.001 to 0.400μg/mL,with a correlation coefficient(R²)of 0.9936.The relative recoveries for matrix spiking experiments at low,medium,and high concentrations ranged from 91.9%to 107.8%,with a relative standard deviation(RSD)of less than 8.1%.The method was applied to determine the AA-I content in three batches of Xinqin granules,with the average content ranging from 0.59 to 0.66μg/g.Conclusion:The method established in this study was found to be highly sensitive and rapid,serving as a reference for the accurate determination of AA-I content in traditional Chinese medicinal preparations.

关 键 词：马兜铃酸I 辛芩颗粒 高效液相色谱 荧光检测 含量测定 

分 类 号：R286.0[医药卫生—中药学]