UPLC-MS/MS同时测定鱼腥草中3个马兜铃内酰胺类成分的含量  

Simultaneous Determination of Three Aristolactams from Houttuyniae Herba by UPLC-MS/MS

作　　者：武营雪 康帅[1] 刘静[1] 戴忠[1] 马双成[1] WU Ying-xue;KANG Shuai;LIU Jing*;DAI Zhong*;MA Shuang-cheng(National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《中国现代中药》2022年第4期616-621,共6页Modern Chinese Medicine

基　　金：国家“重大新药创制”科技重大专项(2018ZX09735006)。

摘　　要：目的:建立同时测定不同产地鱼腥草中马兜铃内酰胺AⅡ、马兜铃内酰胺FⅠ和马兜铃内酰胺BⅡ3个马兜铃内酰胺类成分的超高效液相色谱-质谱法(UPLC-MS/MS)。方法:选用Agilent SB-C;柱(50 mm×2.1 mm,1.8μm),以乙腈-0.1%甲酸为流动相等度洗脱,流速为0.3 mL·min^(-1),多反应监测模式,建立鱼腥草中3个马兜铃内酰胺类成分的UPLC-MS/MS,在方法学验证的基础上对所有样品进行检测分析。运用SPSS 26.0和SIMCA14.1进行差异性、聚类、相关性和主成分分析。结果:在考察的质量浓度范围内,3个马兜铃内酰胺类成分的线性关系良好(r≥0.9998),加样回收率为83.77%~105.61%,RSD为1.14%~11.46%。14批鱼腥草中马兜铃内酰胺AⅡ、马兜铃内酰胺FⅠ和马兜铃内酰胺BⅡ的质量分数分别为0.757~19.538、1.418~15.971、2.893~70.131μg·g^(-1)。差异性分析表明,3个成分的含量与鱼腥草的产地、野生或种植无关。相关性分析表明,3个成分的含量成正相关。结论:所建立的方法准确、可靠,能够用于鱼腥草中3个马兜铃内酰胺类成分的检测分析。Objective:To establish the ultra-performance liquid chromatography-tandem mass spectrometry(UPLCMS/MS)method for simultaneous determination of three aristolactams(AⅡ,FⅠ,and BⅡ)in Houttuyniae Herba from different habitats.Methods:UPLC-MS/MS conditions are as follows:Agilent SB-C;column(50 mm×2.1 mm,1.8μm),isocratic elution with mobile phase of acetonitrile-0.1%formic acid at flow rate of 0.3 mL·min^(-1),multiple reaction monitoring(MRM).After methodological verification,all the samples were determined.Then SPSS 26.0 and SIMCA 14.1 were used for difference analysis,correlation analysis,hierarchical cluster analysis(HCA),and principal component analysis(PCA).Results:Three aristolactams showed good linear relationships within the investigated concentration ranges(r≥0.9998).The overall recoveries were in the range of 83.77%-105.61%,with RSD of 1.14%-11.46%.The content of aristolactam AⅡ,FⅠ,and BⅡin 14 batches of Houttuyniae Herba was in the ranges of 0.757-19.538,1.418-15.971,2.893-70.131μg·g^(-1),respectively.Difference analysis showed that the content of the three components had no correlation with the origin or the cultivation method(wild or cultivated)of Houttuyniae Herba.Pearson’s correlation analysis suggested the content of the three was in positive correlation.Conclusion:The established method is accurate and reliable,which can be applied for analysis of aristolactams in Houttuyniae Herba.

关 键 词：鱼腥草 超高效液相色谱-质谱法 马兜铃内酰胺 

分 类 号：R284[医药卫生—中药学]