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通过高效液相色谱-串联质谱法同时测定浆果中的32种多酚类化合物

Simultaneous Determination of 32 Polyphenolic Compounds in Berries via HPLC-MS/MS.

作者信息

Wang Yuan, Xing Lijie, Zhang Jinlei, Chen Yongfa, Lu Shiling

机构信息

College of Food Science, Shihezi University, Shihezi 832000, China.

Analysis and Testing Center, Xinjiang Academy of Agriculture and Reclamation Science, Shihezi 832000, China.

出版信息

Molecules. 2025 Apr 30;30(9):2008. doi: 10.3390/molecules30092008.

Abstract

An HPLC-MS/MS method for the simultaneous determination of 32 polyphenolic compounds in berries was established. For method validation, the berry samples were extracted with 80% ethanol, purified on an HLB column, and separated on a C18 column via gradient elution with an acetonitrile-water mobile phase system before mass spectrometry detection with electrospray ionization in negative mode and multiple reaction monitoring. The results revealed that the 32 polyphenolic compounds had a good linear relationship in the concentration range of 1-500 μg/L, with R > 0.99, limits of detection, limits of quantitation, and recoveries of 0.2-0.6 μg/kg, 0.3-1.0 μg/kg, and 82.8-104.8%, respectively, and RSDs < 5.8%. The contents of polyphenolic compounds in the berries were determined, with 23 polyphenolic compounds in sea buckthorn, 18 in mulberry, 17 in black wolfberry, and 12 in red wolfberry. Eight polyphenolic compounds were found in all 4 kinds of berries, including 4-hydroxybenzoic acid, p-coumaric acid, ferulic acid, erucic acid, rutin, hypericin, kaempferol-3-O-rutinoside, and daffinoside. Additionally, six polyphenolic compounds, catechin, syringic acid, isorhamnetin-3-O-galactoside, isorhamnetin-3-O-glucoside, cinnamic acid, and isorhamnetin, were detected only in sea buckthorn.

摘要

建立了一种同时测定浆果中32种多酚类化合物的高效液相色谱-串联质谱法。为进行方法验证,将浆果样品用80%乙醇提取,在HLB柱上纯化,然后在C18柱上通过乙腈-水流动相系统进行梯度洗脱分离,最后采用电喷雾电离负离子模式和多反应监测进行质谱检测。结果表明,32种多酚类化合物在1 - 500 μg/L浓度范围内具有良好的线性关系,相关系数R > 0.99,检测限、定量限和回收率分别为0.2 - 0.6 μg/kg、0.3 - 1.0 μg/kg和82.8 - 104.8%,相对标准偏差RSDs < 5.8%。测定了浆果中多酚类化合物的含量,沙棘中含有23种多酚类化合物,桑椹中含有18种,黑枸杞中含有17种,红枸杞中含有12种。在所有4种浆果中均发现了8种多酚类化合物,包括4 - 羟基苯甲酸、对香豆酸、阿魏酸、芥酸、芦丁、金丝桃素、山柰酚-3-O-芸香糖苷和水仙苷。此外,仅在沙棘中检测到6种多酚类化合物,即儿茶素、丁香酸、异鼠李素-3-O-半乳糖苷、异鼠李素-3-O-葡萄糖苷、肉桂酸和异鼠李素。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/6c62/12073267/d2b6c45bdb08/molecules-30-02008-g001.jpg

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