UPLC-Q-TOF-HRMS技术结合SWATH采集方法同时测定柠檬果实中26种生物活性成分的含量  

Simultaneous determination of 26 bioactive components in lemon fruits based on UPLC-Q-TOF-HRMS and SWATH acquisition mode

作　　者：赵希娟[1,2] 庞雯辉 谭涛[1,2] 张耀海 焦必宁[1,3] ZHAO Xijuan;PANG Wenhui;TAN Tao;ZHANG Yaohai;JIAO Bining(Key Laboratory of Quality and Safety Control for Citrus Fruits,Ministry of Agriculture and Rural Affairs,Supervision&Inspection&Testing Center for Quality of Citrus and Nursery Trees,Ministry of Agriculture and Rural Affairs,Chongqing 400715,China;College of Horticulture and Landscape Architecture,Southwest University,Chongqing 400715,China;Citrus Research Institute,Southwest University,Chongqing 400712,China)

机构地区：[1]农业农村部柑橘类果品质量安全控制重点实验室,农业农村部柑桔及苗木质量监督检验测试中心(西南大学),重庆400715 [2]西南大学园艺园林学院,重庆400715 [3]西南大学柑桔研究所,重庆400712

出　　处：《食品与发酵工业》2022年第23期306-314,共9页Food and Fermentation Industries

基　　金：国家现代农业(柑桔)产业技术体系建设专项(CARS-26)。

摘　　要：利用超高效液相色谱-四极杆-飞行时间高分辨质谱(ultra performance liquid chromatography-quadrupole-time of flight high resolution mass spectrometry,UPLC-Q-TOF-HRMS)技术结合所有理论碎片离子的连续窗口采集(sequential window acquisition of all theoretical fragment ions,SWATH)模式,采用特征二级碎片离子峰面积进行外标法定量,建立了一种快速、灵敏同时测定柠檬中13种类黄酮、8种香豆素和呋喃香豆素、2种类柠檬苦素和3种酚酸物质的方法,并对6个品种柠檬果实的果皮、果肉和果汁中这26种生物活性成分进行了定量分析。方法学考察结果显示,该方法具有良好的线性关系、灵敏度、精密度和准确度:线性方程的相关系数均在0.99以上;定量限最低可达0.001μg/L;日间相对标准偏差和日内相对标准偏差分别不超过5.33%和6.39%;加标回收率为(84.27±3.02)%~(114.25±1.77)%。定量结果表明,不同品种与不同部位的柠檬样品中生物活性物质的含量存在较大差异。26种物质在6种柠檬果实中的含量排序为:柯尔提粗柠檬>里斯本柠檬>尤力克柠檬>美国粗柠檬>扁红柠檬>北京柠檬;果皮中的含量显著高于果肉和果汁,所测类黄酮的总含量在26种生物活性成分中占比最高,是柠檬生物活性成分的主要来源之一,其中橙皮苷的含量居首位;柠檬油素、橙皮油内酯、伞形花内酯是柠檬果实中含量较高的香豆素类物质。该研究建立的同时测定26种生物活性成分含量的方法适用于柠檬果实不同部位多类型生物活性物质的筛查和定量分析,方法灵敏、可靠、具有通用性,可用于植物源性产品中多类型生物活性物质的分析研究。Lemon fruits have good nutritional and medicinal values owing to their rich bioactive components such as flavonoids,coumarins,limonoids and phenolic acids.However,the current quantitative analysis methods of bioactive components in lemon fruits have some disadvantages such as the relatively single kind of components or too long detection time.The objective of this study is to establish a rapid and sensitive method to determine the content of multiple bioactive components in lemon fruits,and further compare and analyze the types and contents of bioactive components in different tissues of different lemon varieties,which can provide a reference for evaluating the nutritional quality of lemon and the development of functional products.Based on UPLC-Q-TOF-HRMS and sequential window acquisition of all theoretical fragment ions(SWATH)mode,a rapid and sensitive method was established for the simultaneous determination of 13 flavonoids,8 coumarins,2 limonoids and 3 phenolic acids in lemon fruits by using the peak area of characteristic secondary fragment ions with the external standard method.The 26 bioactive components in the peel,pulp and juice of six lemon varieties were further analyzed quantitatively.The method showed good linear relationships,high sensitivity,precision and accuracy.The correlation coefficients of linear equations for all the compounds were more than 0.99.The minimum limit of quantitation(LOQ)was as low as 0.001μg/L.The interday RSD and intraday RSD were no more than 5.33%and 6.39%,respectively.The recoveries were between(84.27±3.02)%and(114.25±1.77)%.The quantitative results showed that there were great differences in the content of bioactive components in lemon samples of different varieties and parts.The contents of 26 compounds in 6 kinds of lemon fruits were as follows:Keerti Cuningmeng>Lisbon lemon>Eureka lemon>Meiguo Cuningmeng>Bianhong Ningmeng>Meyer Lemon;The contents of the 26 compounds in the peel were significantly higher than those in the pulp and fruit juice.The total contents of fl

关 键 词：柠檬 超高效液相色谱-四级杆飞行时间质谱(UPLC-Q-TOF-HRMS) 理论碎片离子连续窗口采集(SWATH) 类黄酮 香豆素 酚酸 类柠檬苦素 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]