超高效液相色谱-串联质谱法测定蜂蜜中24种酚酸和黄酮类化合物  

Determination of 24 Kinds of Phenolic Acids and Flavonoids in Honey by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张敏 黄京平[1] 赵文[1] 王鹏[1] 金玥[1] 胡菡[1] 张金振[1] ZHANG Min;HUANG Jing-ping;ZHAO Wen;WANG Peng;JIN Yue;HU Han;ZHANG Jin-zhen(Bee Products Quality Supervision and Testing Center,Ministry of Agriculture and Rural Affairs,Institute of Apicultural Research,Chinese Academy of Agricultural Sciences,Beijing 100193,China)

机构地区：[1]中国农业科学院蜜蜂研究所农业农村部蜂产品质量监督检验测试中心(北京),北京100193

出　　处：《分析测试学报》2022年第11期1636-1643,共8页Journal of Instrumental Analysis

摘　　要：建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定蜂蜜中24种酚酸和黄酮类化合物的方法。样品经水溶解,SHIMSEN Styra MAX固相萃取柱净化,超高效液相色谱-串联质谱测定,外标法定量。结果表明,24种化合物在2~1000μg/L范围内线性关系良好,相关系数(r^(2))均大于0.998,方法定量下限为2~10μg/kg;在200、400、1000μg/kg加标水平下,平均回收率为60.3%~111%,相对标准偏差为0.80%~8.5%。采用该方法测定15批次5种植物源蜂蜜样品,结果显示样品中均含有不同浓度的没食子酸、短叶松素、高良姜素、松属素、原儿茶酸、对香豆酸、对羟基苯甲酸、咖啡酸、槲皮素、异鼠李素、莰菲醇和柯因等18种化合物,均不含有迷迭香酸和桑色素。该方法前处理简单、快速、灵敏、稳定,可用于蜂蜜中酚酸类和黄酮类物质的测定。An ultra-high performance liquid chromatography-tandem mass spectrometric method(UPLC-MS/MS)was established for the determination of 24 kinds of phenolic acids and flavonoids in honey.The target compounds were extracted with water,then purified and concentrated with a SHIMSEN Styra MAX solid phase extraction column,and finally analyzed by UPLC-MS/MS and quantified by external standard method.Under the optimal conditions,there were good linear rela⁃tionships for 24 target compounds in the range of 2-1000μg/L with correlation coefficients(r^(2))greater than 0.998.The limits of quantitation for the analytes were in the range of 2-10μg/kg.The average recoveries ranged from 60.3%to 111%,with relative standard deviations of 0.80%-8.5%.The established method was successfully applied to the rapid detection of 15 samples from five types of honey.It was found that 18 compounds including gallic acid,pinobanksin,galangin,pinocembrine,protocatechuic acid,p-coumaric acid,p-hydroxybenzoic acid,caffeic acid,quer⁃cetin,isorhamnetin,kaempferol and chrysin etc.were detected in all honeys,but there existed significant differences in their contents.Meanwhile,rosmarinic acid and morin were undetected in all honeys.The method is simple,rapid,sensitive and stable,and it could be used for the simulta⁃neous determination of various phenolic acids and flavonoids in various honeys.

关 键 词：蜂蜜 超高效液相色谱-串联质谱 固相萃取 酚酸 黄酮 

分 类 号：O657.7[理学—分析化学] TS201.6[理学—化学]