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.
With the emergence of new protein therapeutics, including biosimilars, biobetters and ADCs, peptide mapping by LC/MS is becoming more commonly used for the identification of post-translational modifications (PTMs), glycosylation, and conjugation sites, as well as primary sequence confirmation.
The purpose of this study is to provide guidelines for developing optimal LC running conditions with Aeris™ PEPTIDE core-shell HPLC/UHPLC columns and determine the feasibility of transferring a method developed on UV to MS simply by adjusting the acidic modifier in the mobile phase.
Q: WHAT IS THE FOCUS OF YOUR LAB’S RESEARCH?
A: The Drug Discovery Unit (DDU), based at the University of Dundee, is an independent, fully integrated Drug Discovery Group that works across multiple disease areas. We are active in areas of unmet medical need and bridge the gap between academic research and industrial drug discovery. Our staff are multi-disciplinary and come from both Academic and Industrial backgrounds.
Q: WHY DID YOU INCORPORATE THE EXPRESSION CMS INTO YOUR LABORATORY?
A: We needed a mass spectrometer that was easy to install, operate and move as well as available at a reasonable price. We have had the instrument for over a year now and are very happy with it.
Q: HOW DO YOU USE THE EXPRESSION CMS?
A: We have the expression linked to an HPLC instrument and it is used as an open access system. The combination of UV purity data along with MS confirmation is incredibly powerful for our chemists. The instrument is networked so our chemists can then process and review data from their desks.
Q: WHAT IS THE FOCUS OF YOUR LAB’S RESEARCH?
A: At SynZeal Research Pvt Ltd, with state of the art synthesis laboratory, we are focused on custom synthesis of high purity secondary reference standards of API Impurities and metabolites. SynZeal also provides chemistry research services and products to synergize the drug discovery and development.
Q: WHAT PREVIOUS WORKFLOW CHALLENGES DID YOU EXPERIENCE?
A: The major challenge to our workflow is to have fast decision on success or failure of targeted chemical transformation to decide further course of action and to complete the projects on time.
Q: WHY DID YOU INCORPORATE THE EXPRESSION CMS INTO YOUR LABORATORY?
A: We selected expression CMS as one of the affordable alternative for Mass Spectroscopy which can be operated even by an inexperienced person in mass spectrometry. Our productivity was increased many fold after installation of this system.
There have been a few reports on thin layer chromatography/mass spectrometry (TLC/MS) and thin layer chromatography/tandem mass spectrometry (TLC/MS/MS). The merits of TLC/MS (i.e., without MS/MS or high-resolution mass measurement) include lower-cost mass spectrometers, ease of operation and molecular weight (MW) information when applicable. TLC/MS/MS offers additional benefits, but requires more expensive instrumentation and more challenging operational requirements.
This article describes the direct coupling of TLC plates or other planar surfaces to a compact, single-quadrupole mass spectrometer that can provide routine electrospray ionization (ESI) or atmospheric pressure chemical ionization (APCI) in both the positive and negative ionization modes.
The scientific investigation of cultural heritage objects is the only access to knowledge about long-gone, ancient societies and their cultural, technological as well as their social stage of development. In addition, the materials used by our ancestors, e.g. their textiles and the organic dyestuff to colorize these materials, allow researchers to draw some conclusions about cultural exchanges and trading routes. But in-depth knowledge about materials and dyestuff is also of highest importance for proper conservation and restauration of these materials. Specimens, however, are rare and available only in minute amounts. For their investigation preferentially non-destructive or at least minimal invasive methods have to be used.
A direct analysis using the Atmospheric Solids Analysis Probe (ASAP®) on the expression® compact mass spectrometry (CMS) technique offers a minimally invasive method allowing for a rapid and direct sampling without any sample preparation prior to analysis.
