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[高效液相色谱法测定水果中的21种多酚]

[Determination of 21 polyphenols in fruits by high performance liquid chromatography].

作者信息

Niu Jingqi, Zhang Xuesong, Liu Yuehan, Song Shuang, Wang Guodong, Wang Zhu, Xu Weisheng

机构信息

National Institute for Nutrition and Health, Chinese Center for Disease Control and Prevention, Beijing 100050, China.

National Institute for Nutrition and Health, Chinese Center for Disease Control and Prevention, Beijing 100050, China NHC Key Laboratory of Trace Element Nutrition, Beijing 100050, China.

出版信息

Wei Sheng Yan Jiu. 2023 May;52(3):474-482. doi: 10.19813/j.cnki.weishengyanjiu.2023.03.023.

Abstract

OBJECTIVE

To establish a high performance liquid chromatography(HPLC) method for simultaneous determination of flavonoids(epicatechin, isoorientin, eriocitrin, hyperoside, narirutin, naringin, hesperidin, neohesperidin, quercetin, didymin, naringenin and hesperetin), phenolic acids(gallic acid, chlorogenic acid, caffeic acid, ferulic acid, sinapic acid and p-coumaric acid), terpenoids(limonin), stilbenes(piceatannol and resveratrol) in fruits.

METHODS

Add ethanol-water(4∶1, V/V) solution to the fruit pulp sample, ultrasonic extraction at 55 ℃ for 10 min, after centrifugation, the supernatant was dried and re-dissolved, and then eluted with ZORBAX Eclipse XDB-C_(18)(4.6 mm×100 mm, 3.5 μm) as chromatographic column, polyphenols are determined by HPLC under switching wavelength, and quantified by external standard method.

RESULTS

The 21 polyphenols can be detected within 45 min and well separated from baseline, with linear correlation coefficients greater than 0.999, the detection limit of the method was 0.03-0.31 μg/g, and the limit of quantitation of the method was 0.09-1.03 μg/g. The intra-day precision was 0.5%-9.3%, the inter-day precision was 2.0%-9.6%. The recoveries of more than 90% polyphenols in the three fruits at three levels were between 80.0% and 119.8%. The relative standard deviation of spiked recoveries of three samples was less than 10.8%. The detection result of citrus, mango, blueberry, persimmon and other samples proved that the composition of polyphenols in different fruits was different.

CONCLUSION

The method is sensitive, accurate and reproducible, and is suitable for the determination of polyphenols in fruits.

摘要

目的

建立一种高效液相色谱法(HPLC),用于同时测定水果中的黄酮类化合物(表儿茶素、异荭草素、圣草次苷、金丝桃苷、橙皮芸香苷、柚皮苷、橙皮苷、新橙皮苷、槲皮素、二氢山奈酚、柚皮素和橙皮素)、酚酸(没食子酸、绿原酸、咖啡酸、阿魏酸、芥子酸和对香豆酸)、萜类化合物(柠檬苦素)、芪类化合物(白皮杉醇和白藜芦醇)。

方法

向果肉样品中加入乙醇 - 水(4∶1,V/V)溶液,于55℃超声提取10分钟,离心后,将上清液干燥并重新溶解,然后以ZORBAX Eclipse XDB - C₁₈(4.6 mm×100 mm,3.5μm)为色谱柱进行洗脱,采用切换波长的HPLC法测定多酚类化合物,并以外标法进行定量。

结果

21种多酚类化合物可在45分钟内被检测到,且基线分离良好,线性相关系数大于0.999,该方法的检测限为0.03 - 0.31μg/g,定量限为0.09 - 1.03μg/g。日内精密度为0.5% - 9.3%,日间精密度为2.0% - 9.6%。三种水果中三个加标水平下90%以上多酚类化合物的回收率在80.0%至119.8%之间。三个样品加标回收率的相对标准偏差小于10.8%。柑橘、芒果、蓝莓、柿子等样品的检测结果证明不同水果中多酚类化合物的组成不同。

结论

该方法灵敏、准确、重现性好,适用于水果中多酚类化合物的测定。

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