Quality-In(Process)Line (QuIProLi) process intensification for a micro-flow UV-photo synthesis enabled by online UHPLC analysis

Marc Escriba-Gelonch; Elnaz Shahbazali; Maarten Honing; Volker Hessel

doi:10.1016/j.tet.2018.02.016

Quality-In(Process)Line (QuIProLi) process intensification for a micro-flow UV-photo synthesis enabled by online UHPLC analysis

Marc Escriba-Gelonch^*, Elnaz Shahbazali, Maarten Honing, Volker Hessel^*

^*Corresponding author for this work

Research output: Contribution to journal › Article › Academic › peer-review

Abstract

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. (C) 2018 Elsevier Ltd. All rights reserved.

Original language	English
Pages (from-to)	3143-3151
Number of pages	9
Journal	Tetrahedron
Volume	74
Issue number	25
DOIs	https://doi.org/10.1016/j.tet.2018.02.016
Publication status	Published - 21 Jun 2018

Keywords

Process automation
Flow chemistry
Fast-sampling
UHPLC
Photo-Claisen rearrangement
NEAR-INFRARED SPECTROSCOPY
INTEGRATED MICROREACTOR SYSTEM
ORGANIC-SYNTHESIS
REACTOR SYSTEM
IN-LINE
CLAISEN REARRANGEMENT
LIQUID-CHROMATOGRAPHY
SELF-OPTIMIZATION
PROCESS WINDOWS
PARTICLE-SIZE

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10.1016/j.tet.2018.02.016

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title = "Quality-In(Process)Line (QuIProLi) process intensification for a micro-flow UV-photo synthesis enabled by online UHPLC analysis",

abstract = "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. (C) 2018 Elsevier Ltd. All rights reserved.",

keywords = "Process automation, Flow chemistry, Fast-sampling, UHPLC, Photo-Claisen rearrangement, NEAR-INFRARED SPECTROSCOPY, INTEGRATED MICROREACTOR SYSTEM, ORGANIC-SYNTHESIS, REACTOR SYSTEM, IN-LINE, CLAISEN REARRANGEMENT, LIQUID-CHROMATOGRAPHY, SELF-OPTIMIZATION, PROCESS WINDOWS, PARTICLE-SIZE",

author = "Marc Escriba-Gelonch and Elnaz Shahbazali and Maarten Honing and Volker Hessel",

year = "2018",

month = jun,

day = "21",

doi = "10.1016/j.tet.2018.02.016",

language = "English",

volume = "74",

pages = "3143--3151",

journal = "Tetrahedron",

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AU - Escriba-Gelonch, Marc

AU - Shahbazali, Elnaz

AU - Honing, Maarten

AU - Hessel, Volker

PY - 2018/6/21

Y1 - 2018/6/21

N2 - 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. (C) 2018 Elsevier Ltd. All rights reserved.

AB - 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. (C) 2018 Elsevier Ltd. All rights reserved.

KW - Process automation

KW - Flow chemistry

KW - Fast-sampling

KW - UHPLC

KW - Photo-Claisen rearrangement

KW - NEAR-INFRARED SPECTROSCOPY

KW - INTEGRATED MICROREACTOR SYSTEM

KW - ORGANIC-SYNTHESIS

KW - REACTOR SYSTEM

KW - IN-LINE

KW - CLAISEN REARRANGEMENT

KW - LIQUID-CHROMATOGRAPHY

KW - SELF-OPTIMIZATION

KW - PROCESS WINDOWS

KW - PARTICLE-SIZE

U2 - 10.1016/j.tet.2018.02.016

DO - 10.1016/j.tet.2018.02.016

M3 - Article

SN - 0040-4020

VL - 74

SP - 3143

EP - 3151

JO - Tetrahedron

JF - Tetrahedron

IS - 25

ER -

Quality-In(Process)Line (QuIProLi) process intensification for a micro-flow UV-photo synthesis enabled by online UHPLC analysis

Abstract

Keywords

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