摘要
建立超高效液相色谱-串联质谱联用法测定丹桂香颗粒中马兜铃酸Ⅰ的含量。采用ACQUITY UPLC®BHE C18柱(50 mm×2.1 mm,1.7μm)色谱柱分离,以0.1%(体积分数)甲酸水溶液(含5 mmol/L甲酸铵)-乙腈作为流动相进行梯度洗脱,柱温为30℃,流量为0.3 mL/min。在电喷雾离子源正离子模式,多反应监测模式下进行扫描检测,以外标法定量。马兜铃酸Ⅰ的质量浓度在0.1~40 ng/mL范围内与色谱峰面积线性关系良好,相关系数为0.9996。无糖型、含糖型样品的平均回收率分别为89.4%、91.3%,测定结果的相对标准偏差分别为3.2%、1.2%(n=9)。该方法操作简单、专属性强、准确度高,可实现对丹桂香颗粒中马兜铃酸Ⅰ的定量检测。
An ultra-high performance liquid chromatography-tandem mass spectrometry method was established for the determination of aristolochic acid Ⅰ in Danguixiang Granules.The separation was performed on ACQUITY UPLC®BHE C18 column(50 mm×2.1 mm,1.7μm),and gradient elution was performed on 0.1%(volume fraction)formic acid aqueous solution(including 5 mmol/L ammonium formate)-acetonitrile as mobile phase.The column temperature was 30℃,and the flow rate was 0.3 mL/min.Scanning detection was performed in the positive ion mode of electrospray ion source and multi reaction monitoring mode,and quantification was performed by external standard method.The mass concentrations of aristolochic acid Ⅰ were in the range of 0.1-40 ng/mL,and the correlation coefficient was 0.9996.The average recoveries of sugar-free and sugar-containing samples were 89.4%and 91.3%,respectively.The relative standard deviations of the results were 3.2%and 1.2%(n=9).The method has the advantages of simple operation,strong specificity and high accuracy,which can realize the quantitative detection of aristolochic acid I in Danguixiang Granules.
作者
程庆兵
汪海宣
郑正
袁杰
杨彬
王玮
张亚中
CHENG Qingbing;WANG Haixuan;ZHENG Zheng;YUAN Jie;YANG Bin;WANG Wei;ZHANG Yazhong(Hefei Food and Drug Inspection Center,Hefei 230071;Anhui Provincial Institute for Food and Drug Control,Hefei 230051)
出处
《化学分析计量》
CAS
2024年第11期52-57,共6页
Chemical Analysis And Meterage
基金
安徽省药品监督管理局药品监管科技创新项目(AHYJ-KJ-202222)。
关键词
超高效液相色谱-串联质谱法
丹桂香颗粒
马兜铃酸Ⅰ
ultra high performance liquid chromatography-tandem mass spectrometry
Danguixiang Granules
aristolochic acid Ⅰ
