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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

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【作者】 颜淑婷马铭丁芳林文星星周芳姜放军张朝辉

【Author】 YAN Shuting;MA Ming;DING Fanglin;WEN Xingxing;ZHOU Fang;JIANG Fangjun;ZHANG Zhaohui;Hunan Biological and Electromechanical Polytechnic;Key Lab.of Chemical Biology and Traditional Chinese Medicine Research, Hunan Normal University;

【通讯作者】 张朝辉;

【机构】 湖南生物机电职业技术学院湖南师范大学化学生物学及中药分析教育部重点实验室

【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/m L范围内线性关系良好,R2为0.993 6,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。

【Abstract】 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/m L,with a correlation coefficient (R2)of 0.993 6.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.

【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)
  • 【文献出处】 中国野生植物资源 ,Chinese Wild Plant Resources , 编辑部邮箱 ,2025年02期
  • 【分类号】R286.0;O657.3
  • 【下载频次】34
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