The comprehensive analysis of phenolic compounds from natural products comprises critical steps, including quantitative extraction, extract preparation, and chromatographic procedure. Performing these steps off-line requires a long time to obtain results, besides being laborious and more error-prone. This work discusses the concept and presents the details of assembling and validating a new system to comprehensively analyze phenolic compounds in natural products. The system is based on a bidimensional separation through the combination of pressurized liquid extraction with in-line solid-phase extraction coupled online with HPLC-PDA. The system proved to be able to perform a bidimensional separation to characterize the sample and ensure quantitative extraction of all detected components using the most appropriate extraction solvent gradient depending on the raw sample analyzed. The 1^st dimension separation is achieved by PLE-SPE with a solvent gradient and differential interactions of extracted compounds with the adsorbent. The 2^nd dimension presents the HPLC-PDA separation. The extraction/separation process can be monitored in real-time, and kinetic extraction curves for individual compounds can also be obtained to ensure quantitative extraction. Thus, the 2D PLE-SPE×HPLC-PDA may provide fast and precise comprehensive analyses of a large plethora of phenolic compounds, finding relevant applications in the chemical, food, pharmaceutical, and agricultural fields.

天然产物中酚类化合物的综合分析包括关键步骤，包括定量提取、提取物制备和色谱程序。离线执行这些步骤需要很长时间才能获得结果，而且费力且更容易出错。这项工作讨论了这个概念，并介绍了组装和验证一个新系统的细节，以全面分析天然产物中的酚类化合物。该系统基于二维分离，通过将加压液体萃取与在线固相萃取结合在线与 HPLC-PDA 相结合。事实证明，该系统能够进行二维分离以表征样品并确保根据所分析的原始样品使用最合适的萃取溶剂梯度对所有检测到的成分进行定量萃取。1使用溶剂梯度和萃取化合物与吸附剂的不同相互作用，通过 PLE-SPE 实现^st维分离。的2^所维呈现的HPLC-PDA的分离。提取/分离过程可以实时监控，还可以获得单个化合物的动力学提取曲线，以确保定量提取。因此，二维 PLE-SPE×HPLC-PDA 可以对大量酚类化合物进行快速、精确的综合分析，在化学、食品、制药和农业领域找到相关应用。