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.
This application note suggests that a simple LC/MS screen of a relatively fresh sample of human whole blood collected from a lavender capped potassium EDTA anticoagulant blood sample applied to a cotton swab can be analyzed by full-scan positive ion or negative ion LC/MS using a compact single quadrupole mass spectrometer (expression® CMS). A presumptive positive determination from such a test would benefit from confirmation by LC/MS/MS or other definitive confirmative analytical technique.
D. Tranchemontagne, N. Sousou, S. J. Prosser, J.D. Henion – Advion, Inc. & S. Orlowicz, S. Sadjadi, L. Snow – PhenoLogix
The Advion Interchim Scientific expression® Compact Mass Spectrometer (CMS) coupled with Liquid Chromatography (LC) was used as a qualitative screening tool. This application note will demonstrate the screening of various drugs, including amphetamines, benzodiazepines, antidepressants, opiates and opioid drugs as well as their common metabolites. It will show that the expression® CMS can easily be implemented in a doctor’s office to provide fast and easy drug screening.
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.
Using Thin-Layer Chromatography with Compact Mass Spectrometry
A sprig of mistletoe symbolizes a tradition of romance; however, reputed to be the “kiss of death,” mistletoe is said by some to be so poisonous that humans can be killed if they ingest the leaves or berries.
In the spirit of the Holiday season and to ensure that mistletoe kisses are enjoyed and are ‘non-toxic’, Nigel Sousou and Jack Henion employed the Advion TLC/CMS system to analyze a commercial Tincture of Mistletoe ethanolic extract to determine whether tyramine is present in the extract of mistletoe.
A: Our exclusively undergraduate program in chemistry is fortunate to have a nice inventory of analytical instrumentation for use in various lab courses and student/faculty research. As the department’s analytical chemist, I coordinate the use of these instruments and the development of laboratory projects for use in our curricular labs. I also direct a group of undergraduate student assistants in research aimed at developing new devices and methodologies for microscale spectroelectrochemical measurements.
Q: WHAT WAS YOUR PREVIOUS WORK FLOW OR CHALLENGES?
A: Our department’s mass spectrometry instrumentation (two GCMS systems and an ambient pressure gas analyzer) was limited to EI ionization of gaseous and volatile liquid samples until we purchased the Advion CMS.
Q: WHY DID YOU INCORPORATE THE EXPRESSION CMS INTO YOUR LABORATORY?
A: Our faculty agreed the need existed to incorporate additional MS capabilities to our instrumentation holdings for both our undergraduate lab curriculum and several of our faculty members’ research efforts. The Advion CMS was an ideal choice with regard to cost, portability and flexibility. In particular, the ASAP probe available for APCI mode was an attractive feature supporting our development of lab projects with forensic and pharmaceutical emphasis.
Q: WHO WOULD YOU RECOMMEND TO PURCHASE THE EXPRESSION CMS?
A: I think the Advion system is well suited for a variety of undergraduate curricular and research lab applications.
Q: DO YOU HAVE ANY PUBLICATIONS OR PRESENTATIONS USING THE EXPRESSION CMS?
A: None to report yet, but I’m optimistic – at present, a student in my instrumental analysis course is satisfying her independent project requirement by working with the ASAP probe to develop a simple internal standard approach to permit quantitation of components in pharmaceutical preparations.
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.
