Università Campus-Biomedico, Centro Integrato di Ricerca, Via Alvaro del Portillo 21, 00128 Roma, Italy.
J Chromatogr A. 2012 Apr 20;1234:38-44. doi: 10.1016/j.chroma.2011.12.103. Epub 2012 Jan 9.
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.
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。