University of Cambridge
Abstract
We have developed a modular software system that enables researchers to monitor and control chemical reactions via the Internet, using any device from any location in the world. It facilitates the automation of synthetic procedures and is able to autonomously self-optimize reaction parameters to find the best conditions meeting customizable, multicomponent optimization functions. In this report, we demonstrate its utility as applied to reaction automation to maximize the output from a fixed volume of catalyst. We also showcase its ability to optimize a three-dimensional heterogeneous catalytic reaction and a five-dimensional Appel reaction against various target functions.
In this publication, the Advion expression Compact Mass Spectrometer (CMS) was paired with a flow reaction system for simple reaction monitoring.
An office colleague has stolen a prized chocolate bar, and Dr. Eikel with the help of his partner, Dr. Henion, use an Atmospheric Solids Analysis Probe (ASAP) enabled expression CMS to determine whodunnit. This application note describes the process, and points the finger at the guilty culprit!
This note covers work carried out at Leeds University with co-workers from Durham University in the area of flow chemical synthesis using the expression CMS (Advion, Ithaca, NY). Two different reactions are described.
P. P. Hurtado1, E., Palmer1, C. Aldcroft2, H. Moore2, A. Baker2. M. Allen2, J. Jones2, M.A. Turner1, J.C. Reynolds1
1Centre for Analytical Science, Department of Chemistry, Loughborough University, Ashby Road, Loughborough, Leicester, LE11 3TU, UK 2Advion UK Ltd
The development of new interfaces that enable direct analysis of VOCs represents an attractive and low cost alternative for rapid analysis. For example, the food industry is particularly interested in this type of analysis, where the freshness of different foods can be rapidly measured by the release of its volatiles. Numerous techniques have been used for this purpose. However, mass spectrometry remains the gold standard technique enabling chemical specificity of detection.
Q: WHAT IS THE FOCUS OF YOUR LAB’S RESEARCH?
A: The Liverpool School of Tropical Medicine (LSTM) is dedicated to research and teaching on tropical diseases. We are helping improve the health of some of the poorest people in the world by carrying out scientific research and developing treatments that will directly benefit them.
Specifically, I work in the department of parasitology, where our focus is on the key tropical parasites such as malaria, TB and filarial worms.
Q: WHY DID YOU INCORPORATE THE EXPRESSION CMS INTO YOUR LABORATORY?
A: The expression was originally purchased to save us from a 15-minute walk to get simple MS data at the University’s main analytical service. Also, it is compact and very easy to use, you do not need to be an expert in MS to generate very useful and meaningful data.
Q: HOW DO YOU USE THE EXPRESSION CMS?
A: We use the expression in the direct injection configuration for checking whether reactions have worked and whether the next purification and/or reaction steps are worth proceeding.
Before we got the expression, we either had to walk across campus to use the central service or continue without any knowledge as to whether our reactions had worked. The expression saves us time and boosts our overall research performance.
I am also planning to use it for some simple metabolism studies in the near future.
The analytical verification of compounds in organic syntheses is a challenging task. The sample is often directly taken out of the reaction mixture and therefore contains many impurities and matrix components. As a result, low-level sample preparation combined with a direct analysis method is highly beneficial. TLC/MS (thin layer chromatography – mass spectrometry) is such an analytical technique.
Co-authored with Merck Millipore in Darmstadt, Germany, this application note demonstrates a normal phase TLC/CMS technique for the rapid determination of 4-aminobiphenyl in its reaction mixture.
For the application note on the TLC/CMS determination of 4-aminobiphenyl in reverse phase, click here.
The analytical verification of compounds in organic syntheses is a challenging task. The sample is often directly taken out of the reaction mixture and therefore contains many impurities and matrix components. As a result, low-level sample preparation combined with a direct analysis method is highly beneficial. TLC/MS (thin layer chromatography – mass spectrometry) is such an analytical technique.
Co-authored with Merck Millipore in Darmstadt, Germany, this application note demonstrates a reverse phase TLC/CMS technique for the rapid determination of 4-aminobiphenyl in its reaction mixture.
For the application note on the TLC/CMS determination of 4-aminobiphenyl in normal phase, click here.
Q: WHAT IS THE FOCUS OF YOUR LAB’S RESEARCH?
A: As part of the Archibald research group our main research area is developing radiopharmaceutical compounds for medical imaging and targeted protein binding molecules for therapeutic applications.
Specifically, I am working on synthesising radiotracers to target the CXCR4 chemokine receptor which has been shown to be overexpressed in 23 different types of cancer.
Q: WHY DID YOU INCORPORATE THE EXPRESSION CMS INTO YOUR LABORATORY?
A: The expression CMS was purchased as we are a large research group and it is more cost and time effective to be able to carry out rapid MS analysis in situ for some sample and to use the University’s analytical service only for more complex analyses that are less time sensitive. The expression CMS fits nicely onto the bench top, performs all the functions needed for general day to day use, and is easy to use and maintain.
Q: HOW DO YOU USE THE EXPRESSION CMS?
A: We use the expression CMS to monitor chemical reactions, check for by-products and gauge the purity of our products. We have the TLC-MS interface which is extremely useful in identifying compounds straight from the TLC plate. Personally, I have used the expression CMS to examine fractions from a column to identify exactly when my product was being eluted, which would not have been possible previously. Purchasing the expression CMS has undoubtedly saved our group a great deal of time and has helped advance our research.
Advion has the cover story of the September 2015 issue of the Journal of Mass Spectrometry. We present a method requiring no sample preparation for the direct identification of indigoid colorants in tiny amounts in ancient historic fabrics using ASAP®-MS. Exact determinations were completed in less than 1 min.
