A: The group has extensive experience in host-guest chemistry. We are seeking novel supramolecular platforms/systems, in particular macrocyclic systems, which might find applications in the recognition of ionic and neutral guest molecules. The research consists of two main parts: synthesis of novel receptors and analysis of their supramolecular assemblies. The formation of supermolecules is monitored and analyzed by NMR, UV-vis and fluorescence spectrometry. X-ray analysis is used to determine structure of receptors and their complexes. We also work with dynamic combinatorial libraries (DCL) and occasionally synthesize isotopically labeled compounds.
Q: WHAT WAS YOUR PREVIOUS WORK FLOW OR CHALLENGES?
A: In the synthesis of molecules of complex structures we need fast and reliable feedback about the success of each synthetic step. For example, macrocyclisation reactions sometimes give very complex mixtures. In order to follow the reaction course and facilitate purification, we need a fast tool for the unambiguous confirmation in which TLC spot is the desired product. Also, distinguishing between [1+1] and [2+2] macrocycles is not possible by simple NMR measurements and for new dynamic combinatorial libraries any HPLC characterization method required validation by an LC-MS in the service laboratory which takes time.
Q: WHY DID YOU INCORPORATE THE EXPRESSION® CMS INTO YOUR LABORATORY?
A: We needed a versatile tool to speed up our synthesis processes and facilitate purification protocols. The expression® CMS is mainly applied with Plate Express™ for fast compound identification from TLC plates. Now the choice of synthetic protocol can be evaluated within minutes. The product unambiguously spotted on the TLC plate is much easier to isolate. In addition, whenever needed we connect CMS to our HPLC system to analyze complex mixtures and to validate the analytical protocols. Isotope composition of labeled compounds is also easy to follow using this system.
Q: WHO WOULD YOU RECOMMEND TO PURCHASE THE EXPRESSION® CMS?
A: We would recommend it to all groups dealing with synthesis of small molecules. The instant feedback about the reaction progress and aid in isolation of the product saves a lot of time. With the expression® CMS, the group is more independent, using the system as a stand-alone unit, coupled to the TLC plate reader or LC-system when needed.
A: Our company, SYNKOLA Ltd., is a chemical contract research company offering custom synthesis and research services for more than 24 years. Our clients are mostly global leaders in the industry. The focus of our laboratory research is the synthesis of organic substances, especially in the area of biologically active substances and chemical specialties. In term of structure, our targets are usually complicated molecules containing hetero- and multiple halogen atoms.
Q: WHY DID YOU INCORPORATE THE EXPRESSION CMS INTO YOUR LABORATORY?
A: We use the expression CMS for fast monitoring of reaction mixtures, to identify fractions and also to confirm structures in combination with other analysis methods. The analysis with CMS is very fast and any chemist is able to perform his own routine analysis. The ASAP®/APCI method is especially fast and simple (>2000 samples a year).
Q: TO WHOM WOULD YOU RECOMMEND THE EXPRESSION CMS?
A: We recommend the purchase of the expression CMS to all organic and synthetic chemists groups for its ease-of-use. With the ASAP option, chemists are enabled to analyze any sample in 2-3 minutes without the need for external services. A further advantage is that both positive/negative mode analysis is done at the same time and in a single run.
A: My group are actively researching the application of mass spectrometry to a range of problems in both chemical and biomedical science. In particular we are involved in the application of mass spectrometry based proteomics for label free quantitation of proteins from human tissue samples and also in the identification of trace analytes from environmental samples. We are also investigating the synthesis of novel co-polymeric monolithic phases for sample extraction and separation.
Q: WHAT WAS YOUR PREVIOUS WORK FLOW OR CHALLENGES?
A: The Chemistry Department at Hull have long recognised the need for practical training on a wide range of chemical instrumentation. In particular we recognise the requirement from many companies in the pharmaceutical and fine chemical sectors for practical training in GC/MS and LC/MS. The Advion expressionL compact mass spectromater (CMS) was purchased to provide such training at an undergraduate level and has been incorporated into the range of instrumental analysis practicals for final year students. The expressionL CMS fits tidily on the bench-top next to the HPLC system and gives students the chance experience at first hand the use of LCMS as an analytical technique. The ease of use and robust nature of the system means that the expressionL CMS lends itself to the undergraduate laboratory where users will not be experts in mass spectrometry at this point in their careers.
Q: WHY DID YOU INCORPORATE THE EXPRESSION CMS INTO YOUR LABORATORY?
A: We use the expressionL CMS to give undergraduate students practical experience of using LC/MS to prepare and analyse a ‘mock’ urine sample. The sample has to be prepared by adding the internal standard and extracting the analytes using Solid Phase Extraction (SPE) to obtain a sample suitable for LC/MS analysis. The aim is to identify and quantify the compounds found in the sample by reference to the internal standard added. The HPLC separation is a rapid 10 min gradient elution and the ability to incorporate the data from the UV detector into the MS data provides an additional benefit. Purchasing the expression L CMS has allowed us to provide practical training in LC/MS for our undergraduate students at a time when prospective employers are actively seeking such skills.
A recent development in mass spectrometry is the design of smaller sized MS systems with full analytical capability (compact mass spectrometry, CMS). CMS systems with fragmentation analysis are very cost eff ective analysis solutions and ideally suited for reaction and quality control in SPPS including detailed product characterization3. Here, we evaluate the utility of a system comprised of an automated peptide synthesizer, Prelude X
(Protein Technologies Inc.) and the LC/CMS analysis system expression-L (Advion Inc.) based on two peptides selected for their known synthetic challenge.
The CheMS user interface simplifies the mass spectrometry experience and makes it more accessible in chemistry and biochemistry laboratories. This allows the chemist to obtain optimal data without needing to be an expert in mass spectrometry.
Available with the Advion expression® compact mass spectrometer (CMS) is a fast and easy tool that is ideal for the teaching environment — Students simply select an ionization method for effortless instrument setup at the click of a button.
Fill out the form to download the full CheMS product note now.
N. Holmes, G.R. Akien, R.J.D. Savage, C. Stanetty, I.R. Baxendale, A.J. Blacker, B.A. Taylor, R.L. Woodward, R.E. Meadows, and R.A. Bourne
An automated continuous reactor for the synthesis of organic compounds, which uses online mass spectrometry (MS) for reaction monitoring and product quantification, is presented. Quantitative and rapid MS monitoring was developed and calibrated using HPLC. The amidation of methyl nicotinate with aqueous MeNH2 was optimised using design of experiments and a self-optimisation algorithm approach to produce >93% yield.
Q: What is the focus of your lab’s research? A: Our research is focused on developing and exploiting chemical tools and principles to address questions in plant and microbial carbohydrate biochemistry. Projects typically involve some combination of chemical and enzymatic synthesis, inhibitor design and assessment, biochemistry, structural biology and omics analyses.
Q: What was your previous workflow or challenges? A: We synthesize a lot of different molecules in the lab, many of which have relatively low molecular weights. To acquire low resolution MS spectra of purified compounds we relied on MALDI-TOF or on direct injection into an expensive LC-MS system (ESI). Access to these instruments required booking in advance and there was also often a delay in obtaining results.
Q: Why did you incorporate the expression® CMS into your lab? A: We wanted an instrument that would allow rapid access to low resolution MS data for low molecular weight compounds. Immediate access to this instrument allows rapid confirmation of product formation in chemical and ezymatic syntheses; the Compact Mass Spectrometer (CMS) is particularly useful for rapid identification of analytes from LC separations. All of this can be done by direct injection but in our lab the injection from a TLC silica plate using the Advion Interchim Scientific Plate Express™ is being increasingly used as a faster alternative. The APCI ion source is another great capability of the CMS, particularly for analysis of lipophilic compounds such as triterpenes, which we have experienced difficulties in analysing by other ionisation techniques.
Q: Who would you recommend to purchase the expression® CMS? A: Any group working with organic molecules that requires fast access to low resolution MS spectra. We would especially recommend coupling the expression® CMS with the Plate Express™ for labs that routinely use TLC for monitoring chemical syntheses and biotransformations.
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.
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.
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.
