食品科学 ›› 2017, Vol. 38 ›› Issue (20): 112-118.doi: 10.7506/spkx1002-6630-201720016

• 成分分析 • 上一篇    下一篇

HPLC-DAD-FLD同时测定柑橘果汁中12 种多甲氧基黄酮和香豆素类物质

李贵节,谭祥,王华,吴厚玖,Russell Rouseff   

  1. (1.西南大学柑桔研究所,中国农业科学院柑桔研究所,重庆 400712;2.重庆第二师范学院,重庆市功能性食品协同创新中心,重庆市功能性食品工程技术研究中心,重庆 400067;3.西南大学食品科学学院,重庆 400715;4.重庆第二师范学院生物与化学工程学院,重庆 400067)
  • 出版日期:2017-10-25 发布日期:2017-09-29
  • 基金资助:
    公益性行业(农业)科研专项(201503142-12);重庆市功能性食品协同创新中心建设项目(167001); 中央高校基本科研业务费专项(XDJK2016E048);重庆市功能性食品协同创新中心科研项目(ccicff-rp-201604); 重庆市统筹城乡教师教育研究中心2015年工作室项目(JDGZS201507); 重庆第二师范学院2016年校级大学生创新创业训练计划项目(201605)

Simultaneous Determination of Twelve Compounds of Polymethoxyflavones, Coumarins and Furocoumarins in Citrus Juices by Using HPLC-DAD-FLD

LI Guijie, TAN Xiang, WANG Hua, WU Houjiu, Russell Rouseff   

  1. (1. Citrus Research Institute, Southwest University, Chinese Academy of Agricultural Sciences, Chongqing 400712, China;2. Chongqing Collaborative Innovation Center for Functional Food, Chongqing Engineering Research Center of Functional Food, Chongqing University of Education, Chongqing 400067, China;3. College of Food Science, Southwest University, Chongqing 400715, China;4. College of Biological and Chemical Engineering, Chongqing University of Education, Chongqing 400067, China)
  • Online:2017-10-25 Published:2017-09-29

摘要: 建立高效液相色谱-串联二极管阵列检测器和荧光检测器(high performance liquid chromatography-diode array detector-fluorescence detector,HPLC-DAD-FLD)同时检测柑橘果汁中12?种多甲氧基黄酮、香豆素及呋喃香豆素类物质的方法。以0.01%磷酸、甲醇、乙腈组成三元流动相进行梯度洗脱,12?种物质在30?min内实现基线分离。利用DAD和FLD获得各物质的紫外和荧光光谱信息,将柑橘果汁样品组分的光谱与之比对,并结合色谱保留时间,实现样品成分的定性分析。分别以320?nm和450?nm为紫外和荧光的检测波长,研究该方法的定量性能。结果显示:标准曲线线性关系良好;荧光定量限低至μg/L级,可作为紫外定量的重要补充手段;果汁回收率的紫外和荧光检测值分别为95.2%~104.8%和94.5%~103.5%。该方法对样品定性、定量分析准确,适合柑橘多甲氧基黄酮、香豆素等能发射荧光物质的检测。

关键词: 高效液相色谱, 荧光检测, 柑橘果汁, 多甲氧基黄酮, 香豆素

Abstract: A method using high performance liquid chromatography with diode array detection and fluorescence detection (HPLC-DAD-FLD) was developed to simultaneously analyze 12 compounds of polymethoxyflavones (PMFs), coumarins and furocoumarins in citrus juice samples. Baseline separation of twelve compounds was achieved within 30 min using gradient elution with a ternary mobile phase composed of 0.01% phosphoric acid, methanol and acetonitrile. Qualitative identification of the components in citrus juices was confirmed by comparing their UV and fluorescence (FL) spectra and retention times with those of the reference standards. Quantitative analysis of the juice components was operated at a UV wavelength of 320 nm (OD320 nm) and a fluorescence emission of 450 nm. The calibration curves showed good linearity. The limit of quantitation (LOQ) with FLD was at as low as μg/L level so that FLD could be an important complementary tool to UV detection. The recovery tests showed a good accuracy for both UV (95.2%–104.8%) and FL (94.5%–103.5%) examination. In general, this method is accurate and reliable for qualitative and quantitative analysis of citrus juice components, especially the ones having fluorescence emission like PMFs and coumarins.

Key words: high performance liquid chromatography (HPLC), fluorescence detection, citrus juice, polymethoxyflavones, coumarins

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