天然产物研究与开发 ›› 2019, Vol. 31 ›› Issue (8): 1365-1371.doi: 10.16333/j.1001-6880.2019.8.009

• 研究简报 • 上一篇    下一篇

SPE-HPLC-DAD法同时检测柑橘药用资源中黄烷酮类和川陈皮素成分

谢辉1,陈亚1,雷爱玲1,朱春燕1,李杨梅1,白玉婷1,孙鹏1*,李贵节1,2*   

  1. 1重庆第二师范学院生物与化学工程学院 重庆市功能性食品协同创新中心,重庆 400067;2西南大学柑桔研究所 中国农业科学院柑桔研究所 国家柑桔工程技术研究中心,重庆 400712
  • 出版日期:2019-09-10 发布日期:2019-09-10
  • 基金资助:

    重庆市教育委员会科学技术研究项目(KJQN201801613);国家柑桔工程技术研究中心开放项目(NCERC2019004);重庆第二师范学院大学生科研项目(XK20170220,KY20180256);重庆市功能性食品协同创新中心科研项目(ccicff-srp-201608)

Simultaneous determination of flavanones and nobiletin in citrus medicinal resources by using SPE-HPLC-DAD methods

XIE Hui1,CHEN Ya1,LEI Ai-ling1,ZHU Chun-yan1,LI Yang-mei1,BAI Yu-ting1,SUN Peng1*,LI Gui-jie1,2*   

  1. 1School of Biological and Chemical Engineering,Chongqing University of Education,Chongqing Collaborative Innovation Center for Functional Food,Chongqing 400067,China; 2Citrus Research Institute of Southwest University & Chinese Academy of Agricultural Sciences,National Citrus Engineering Research Center,Chongqing 400712,China
  • Online:2019-09-10 Published:2019-09-10

摘要: 为检测柑橘类5种药用资源中芸香柚皮苷、柚皮苷、橙皮苷、柚皮素和橙皮素等5个黄烷酮物质和川陈皮素的含量。实验用70%乙醇水溶液分别浸提化橘红、陈皮、青皮、橘络和橘核,提取液经稀释后利用C18固相萃取柱除杂和浓缩,再以0.5%醋酸水溶液和甲醇为流动相进行反相梯度洗脱,用串联二极管阵列检测器(DAD)扫描紫外光谱做定性分析,并分别在283、285、290、335 nm波长处做定量检测。在该条件下6个类黄酮成分均实现基线分离;外标法定量,线性相关性好(R2≥0.999 8);加标回收率为95.83%~103.56%,相对标准偏差为2.90%~8.78%。含量分析结果显示:芸香柚皮苷10.49 mg/g、柚皮素0.327 mg/g、橙皮素0.129 mg/g在青皮中含量最高,橙皮苷10.78 mg/g、川陈皮素1.74 mg/g在陈皮中含量最高,柚皮苷19.20 mg/g在化橘红中含量最高。该方法适用于柑橘药用资源中微量类黄酮成分的准确定性和定量检测。

关键词: 柑橘药用资源, 高效液相色谱, 固相萃取, 川陈皮素, 黄烷酮

Abstract: Contents of five flavanones such as narirutin,naringin,hesperidin,naringenin and hesperetin as well as nobiletin in five citrus medicinal resources were analyzed.Huajuhong,Chenpi (dried tangerine peel),Qingpi,Juluo and Juhe were extracted with 70% ethanol aqueous solution;extract solution was diluted and then cleaned and concentrated by C18 solid phase extraction column.A reverse-phase HPLC gradient elution with 0.5% acetic acid (aq.) and methanol as mobile phase was developed for separation;a diode array detector (DAD) was hyphenated to scan UV spectra for the qualitative analysis;quantitation was achieved respectively at 283,285,290 and 335 nm.Under above conditions,the six flavonoids were base-isolated;the external standard method for quantitation showed good linear correlation (R2≥0.999 8);recovery rate was between 95.83%-103.56%;the relative standard deviation was between 2.90%-8.78%.The results of sample content analysis showed that Qingpi had the highest concentration of narirutin 10.49 mg/g,naringenin 0.327 mg/g and hesperetin 0.129 mg/g;Chenpi had the highest concentration of hesperidin 10.78 mg/g and nobiletin 1.74 mg/g;Huajuhong had the highest concentration of naringin 19.20 mg/g.This method is suitable for accurate qualitative and quantitative detection of flavonoids in citrus medicinal resources.

Key words: citrus medicinal resources, high performance liquid chromatography, solid phase extraction, nobiletin, flavanone

中图分类号: 

R284.2 O657.3