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采用核壳颗粒填充毛细管柱的纳米液相色谱法分析茶样中的多酚和甲基黄嘌呤。

Analysis of polyphenols and methylxantines in tea samples by means of nano-liquid chromatography utilizing capillary columns packed with core-shell particles.

机构信息

Università Campus-Biomedico, Centro Integrato di Ricerca, Via Alvaro del Portillo 21, 00128 Roma, Italy.

出版信息

J Chromatogr A. 2012 Apr 20;1234:38-44. doi: 10.1016/j.chroma.2011.12.103. Epub 2012 Jan 9.

Abstract

In this study, a rapid separation of eleven polyphenols and three methylxanthines was obtained by means of nano-liquid chromatography (nano-LC), employing a 100 μm I.D. capillary column packed with C18 core-shell particles (2.7 μm) for 10 cm. All compounds were baseline resolved with a step gradient elution in less than 15 min. The developed analytical method was validated and the resulting RSD% for intra-day and inter-day repeatability, related to retention time, retention factor and peak area, were below 5.1 and 5.7%. LOD and LOQ values corresponded to 0.300 and 0.625 μg/mL, while linearity range assessed gave R² no lower than 0.990. Then, the method was used to determine studied compounds in tea extracts. Further, the nano-LC system was coupled with a mass spectrometer to confirm the components present in real samples. Finally the results were compared with those obtained using a capillary column (100 μm I.D. × 10 cm) packed with C18 sub-2 μm particles, applying the same nano-LC experimental conditions.

摘要

在这项研究中,通过纳米液相色谱(nano-LC),采用 100μm ID 的毛细管柱,填充 C18 核壳颗粒(2.7μm),长度为 10cm,实现了对 11 种多酚和 3 种甲基黄嘌呤的快速分离。所有化合物均采用分步梯度洗脱,在 15 分钟内实现了基线分离。所开发的分析方法经过验证,日内和日间重复性的 RSD%(与保留时间、保留因子和峰面积相关)均低于 5.1%和 5.7%。LOD 和 LOQ 值分别对应于 0.300 和 0.625μg/mL,而评估的线性范围给出的 R² 不低于 0.990。然后,该方法用于测定茶提取物中的研究化合物。此外,将纳米 LC 系统与质谱仪耦合,以确认实际样品中存在的成分。最后,将结果与使用填充有 C18 亚 2μm 颗粒的毛细管柱(100μm ID×10cm),应用相同的 nano-LC 实验条件得到的结果进行了比较。

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