摘要
目的:为了建立椪柑陈皮的高效液相色谱指纹图谱及多成分含量测定方法,并结合化学计量学分析研究不同陈化时长对椪柑陈皮8种黄酮类成分的影响。方法:以乙腈(A相)-0.1%磷酸水溶液(B相)为流动相,使用梯度洗脱,进样体积为10μL;检测波长分别为283 nm(橙皮苷、新橙皮苷、柚皮苷、芸香柚皮苷)、310 nm(指纹图谱)、330 nm(川陈皮素、3,5,6,7,8,3’,4’-七甲氧基黄酮(3,5,6,7,8,3’,4’-heptamethoxyflavone,HMF)、桔皮素、5-羟基-6,7,8,3’,4’-五甲氧基黄酮(5-hydroxy-6,7,8,3’,4’-pentamethoxyflavone,5-HPMF))。采用高效液相色谱法建立10批次不同陈化时长(0~126 d)椪柑陈皮的指纹图谱,并进行相似度评价;结合聚类分析、主成分分析、正交偏最小二乘判别分析等化学计量学分析方法对10批次椪柑陈皮8种黄酮类成分变化差异性进行综合分析。结果:10批次椪柑陈皮样品指纹图谱相似度均大于0.995,标定了32个共有峰,说明不同陈化时长椪柑陈皮质量相对稳定,建立的指纹图谱稳定可靠;柚皮苷、橙皮苷、川陈皮素、桔皮素、5-HPMF等五种成分含量在陈化阶段呈波动下降趋势,新橙皮苷含量呈先波动上升后下降趋势,而芸香柚皮苷和HMF两种成分含量呈上升趋势;聚类分析将10批次椪柑陈皮分为2类,其中加速陈化56、70 d与陈化0 d的样品聚为一类,其他加速时长的样品聚为一类;主成分分析提取了3个主成分,累计方差贡献率为85.740%,通过正交偏最小二乘判别分析,确定了橙皮苷、新橙皮苷、5-HPMF及桔皮素4种黄酮类成分是区分不同陈化时长椪柑陈皮的差异性标志物。结论:本研究构建的椪柑陈皮指纹图谱和多成分含量测定方法稳定性高、重复性好,可结合聚类分析、主成分分析以及正交偏最小二乘判别分析对不同陈化时长的椪柑陈皮成分变化和质量进行监测和评价,为椪柑陈皮的开发和利用提供理论与方法基础。
Objective:To establish a high performance liquid chromatographic(HPLC)fingerprint and multi-component content determination methods of Ponkan Chenpi,the effects of different aging durations on 8 kinds of flavonoid components of Ponkan Chenpi were investigated by chemometric analysis.Methods:The injection volume was 10μL and gradient elution was applied with acetonitrile(A)-0.1% phosphoric acid aqueous solution(B)as the mobile phase.The detection wavelengths were 283 nm for hesperidin,neohesperidin,naringin,and narirutin,310 nm for fingerprint,and 330 nm for nobiletin,3,5,6,7,8,3',4'-heptamethoxyflavone(HMF),tangeretin,5-hydroxy-6,7,8,3',4'-pentamethoxyflavone(5-HPMF).The fingerprint profiles of 10 batches of Ponkan Chenpi with different aging periods(0~126 d)were established by HPLC and their similarities were evaluated.The variability of 8 flavonoid components was analyzed by combined chemometric methods,including hierarchical cluster analysis(HCA),principal component analysis(PCA)and orthogonal partial least squares discriminant analysis(OPLS-DA).Results:The similarities of fingerprint profiles of 10 batches of Ponkan Chenpi samples were all greater than 0.995,and 32 common peaks were marked.The result indicated that the quality of Ponkan Chenpi was relatively stable during different aging periods and the established fingerprint profiles were reliable and credible.The contents of five components,including naringin,hesperidin,nobiletin,tangeretin and 5-HPMF,showed a fluctuating decreasing trend,and neohesperidin showed a fluctuating upward and then downward trend,while those of narirutin and HMF showed a fluctuating increasing one during the aging.The result of HCA indicated that 10 batches of Ponkan Chenpi samples could be divided into two categories.The samples with accelerated aging of 56,70 d and aging 0 d were clustered into one category,while the rest were clustered into another one.The PCA result revealed that three principal components with a cumulative variance contribution of 85.740%could be extracted.Four flavonoid components,including hesperidin,neohesperidin,5-HPMF and tangeretin,were identified as the differential markers to distinguish between different aging periods of Ponkan Chenpi samples.Conclusion:The fingerprint profile and multicomponent content determination methods constructed in this study were highly stable and reproducible.Combined with HCA,PCA and OPLS-DA,the methods could be applied to monitor and evaluate the changes in chemical components and quality of Ponkan Chenpi with different aging periods.The study would provide a theoretical and methodology basis for the development and utilization of Ponkan Chenpi.
作者
张慧静
陆胜民
朱卫东
王佳俊
王阳光
ZHANG Huijing;LU Shengmin;ZHU Weidong;WANG Jiajun;WANG Yangguang(School of Food and Pharmacy,Zhejiang Ocean University,Zhoushan 316022,China;Institute of Food Science,Zhejiang Academy of Agricultural Science,Hangzhou 310021,China;Quzhou Institute of Agricultural and Forestry Sciences,Quzhou 324000,China)
出处
《食品工业科技》
CAS
北大核心
2023年第24期23-33,共11页
Science and Technology of Food Industry
基金
浙江省市级农科院联盟区域示范性项目实施计划(2022SJLM7)。
