高效液相色谱-串联质谱法同时测定山楂中6个黄酮类功效成分  

Simultaneous determination of 6 flavonoids in hawthorn by high performance liquid chromatography-tandem mass spectrometry

作　　者：蒋娅兰 毋福海 黄芳 吴惠勤 黄晓兰 邓欣 JIANG Ya-lan;WU Fu-hai;HUANG Fang;WU Hui-qin;HUANG Xiao-lan;DENG Xin(College of Traditional Chinese Medicine,Guangdong Pharmaceutical University,Guangzhou 510006,China;School of Public Health,Guangdong Pharmaceutical University,Guangzhou 510024,China;Guangdong Provincial Public Laboratory of Analysis and Testing Technology,China National Analytical Center（Guangzhou）,Guangzhou 510070,China)

机构地区：[1]广东药科大学中药学院,广州510006 [2]广东药科大学公共卫生学院,广州510024 [3]广东省测试分析研究所(中国广州分析测试中心),广州510070

出　　处：《药物分析杂志》2018年第7期1139-1145,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：广东省科技成果转化启动项目(2011A060903001)

摘　　要：目的:建立山楂中6个黄酮类物质的液相色谱-串联质谱(LC-MS/MS)测定方法。方法:实验优化了液相色谱条件和质谱参数。采用C_(18)柱分离,流动相为乙腈-水(含0.1%甲酸),梯度洗脱,流速0.2 m L·min^(-1),以电喷雾离子源正离子多反应监测(MRM)模式进行MS/MS检测。结果:6个黄酮类物质在各自的线性范围内具有良好的线性关系,相关系数大于0.994,低、中、高3个添加水平的平均回收率在80.4%~105.0%之间,RSD小于10%。10批样品中6个黄酮成分的含量测定结果:儿茶素,0.03~5.39μg·g^(-1);牡荆素,0.11~1.02μg·g^(-1);木犀草素,0.02~0.09μg·g^(-1);槲皮素,3.72~14.02μg·g^(-1);芦丁,3.32~5.79μg·g^(-1);金丝桃苷,31.32~80.89μg·g^(-1)。结论:该方法可用于测定山楂中儿茶素、牡荆素、槲皮素、木犀草素、芦丁、金丝桃苷。Objective：To establish a high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）method for simultaneous determination of 6 functional components in hawthorn.Methods：The conditions of chromatography and mass spectrometry were optimized.The 6 flavonoids were separated on a C_（18）chromatographic column with acetonitrile and 0.1%formic acid as mobile phase under gradient elution at a flow rate of 0.2 m L·min^（-1）.The determination was conducted by tandem mass spectrometry in positive ESI mode under multiple reaction monitoring（MRM）mode.Results：Good linearities for all the compounds,with correlation coefficients over 0.994,were acquired.The recoveries（n=6）were in the range of 80.4%to 105.0%,while RSDs were less than 10%.The contents of 6 functional components in 10 batches of samples were as follows：catechin,0.03-5.39μg·g^（-1）;vitexin,0.11-1.02μg·g^（-1）;luteolin,0.02-0.09μg·g^（-1）;quercetin,3.72-14.02μg·g^（-1）;rutin,3.32-5.79μg·g^（-1）;hyperoside,31.32-80.89μg·g^（-1）.Conclusion：The established method can be used to determine catechin,vitexin,quercetin,luteolin,rutin and hyperoside in hawthorn.

关 键 词：液相色谱-串联质谱 多反应监测 儿茶素 牡荆素 槲皮素 木犀草素 芦丁 金丝桃苷 山楂 含量测定 

分 类 号：R917[医药卫生—药物分析学]