2026-04-14T02:15:44Zhttps://recercat.cat/oai/request

oai:recercat.cat:10459.1/4677442025-09-15T18:52:20Zcom_2072_3622col_2072_479130

00925njm 22002777a 4500 dc Escribà i Gelonch, Marc author Shahbazali, E. author Honing, M. author Hessel, Volker author 2018 Process intensification commonly enables reaction acceleration and therefore continuous-flow/PAT is urgently needed. The low volumes typical for micro-flow pose challenges for online sampling operations in analytics. In this paper, a very fast process is combined with a modified ultra-high-performance liquid chromatography (UHPLC) system allowing for very fast sampling and analysis. Low-volume online sampling according to the needs posed by PAT for pharma quality control, is introduced here for UHPLC analysis of the photo-Claisen rearrangement in micro-flow. Chances and challenges are critically reviewed, including the reproducibility and robustness of the sampling. Furthermore, the ability and speed of the chosen set-up in order to capture process changes and adjust the process parameters properly is investigated. With the applied online sampling system, it was possible to perform, almost unattended and spending 12 times less sampling volume, a full factorial analysis of all relevant reaction conditions (243 experiments) in three days. Such quality-in-the-process-line (QuIProLi) online sampling avoided random errors due to automation. This project was funded by the Horizon 2020: Marie Skolodowska-Curie Individual Fellowship awarded by Dr. Marc Escribà Gelonch under grant agreement number 659233. Process automation Flow chemistry Fast-sampling UHPLC Photo-Claisen rearrangement Quality-in(Process)Line (QuIProLi) process intensification for a micro-flow UV-photo synthesis enabled by online UHPLC analysis