A: Our group is interested in bacterial natural product chemistry, with projects ranging from the directed discovery of new natural products by genome mining and heterologous pathway expression, the elucidation of individual biocatalytic reactions by in vitro studies and the application of the respective biosynthetic enzymes in organic synthesis. This also involves significant synthetic work, for example to prepare enzyme substrates, validate natural product structure elucidation, or to realize chemo-enzymatic natural product total syntheses.
Q: WHAT WAS YOUR PREVIOUS WORK FLOW OR CHALLENGES?
A: While NMR spectroscopy is an analytical tool that is meanwhile accessible to chemical research practically at any time, making standard 1H NMR experiments available within minutes to few hours after a reaction work up, MS spectrometry can sometimes be challenging to conduct sufficiently fast to allow for an efficient work flow: MS equipment in academia is typically located in service units with relatively few machines for whole departments, often leading to waiting times of one to several days for an analysis. While MS would be the perfect tool to directly monitor the success of a chemical reaction in situ or to quickly evaluate the outcome of enzymatic transformations, above restrictions prevent this tool from being regularly and efficiently used.
Q: WHY DID YOU INCORPORATE THE EXPRESSION CMS INTO YOUR LABORATORY?
A: We integrated the expression CMS into our analytical equipment to obtain fast information on our synthetic and biocatalytic reactions, as well as on the content of whole bacterial raw extracts. While the machine is usually used for direct injections and for recording of MS spectra from TLC reaction controls using the Plate Express system, LC-MS measurements of enzymatic reaction set-ups and raw extracts are run overnight. To our surprise, even the detection of post-translational modifications on small proteins can accurately be detected with the CMS, providing us with an additional tool even for protein characterization. This now gives us fast initial MS data for all applications important to our lab, thus significantly streamlining our research work.
Q: WHO WOULD YOU RECOMMEND TO PURCHASE THE EXPRESSION CMS?
A: The expression CMS is the perfect MS system for any research laboratory involved in synthetic organic chemistry and chemical analytics of small molecules to proteins. The system is easy to use and maintain and can thus be used by many individuals. It is therefore particularly well-suited for academic research laboratories.
Ana A. Folgueiras-Amador, Kai Philipps, Sébastien Guilbaud, Jarno Polacker, Prof. Dr. Thomas Wirth
Flow electrochemistry is an efficient methodology to generate radical intermediates. An electrochemical flow microreactor has been designed and manufactured to improve the efficiency of electrochemical flow reactions. With this device only little or no supporting electrolytes are needed, making processes less costly and enabling easier purification. This is demonstrated by the facile synthesis of amidyl radicals used in intramolecular hydroaminations to produce isoindolinones. The combination with inline mass spectrometry facilitates a much easier combination of chemical steps in a single flow process.
The in-line MS analysis was carried out using Advion Expression® CMS (Atmospheric Pressure Ionisation Techniques (APCI)) and an MRA® valve.
Q: WHAT IS THE FOCUS OF YOUR LAB’S RESEARCH? A: Our work is focused on the development and implementation of chromatographic purification processes, ranging from mg to 100 kg scale. Many compounds of interest lack chromophores and cannot be detected by classical UV detection.
Q: WHAT WAS YOUR PREVIOUS WORKFLOW AND EXPERIENCED CHALLENGES?
A: In the past, the fraction collection during preparative HPLC was very time consuming as we had no indicator when the compound of interest was eluting in the chromatographic process in case it was not UV-active. All fractions had to be analyzed by TLC and in many cases additionally with HPLC and Corona detection before we could identify the fractions of interest.
Q: WHY DID YOU INCORPORATE THE EXPRESSION® CMS INTO YOUR LABORATORY?
A: We use the Advion Interchim Scientific expression® CMS as a robust and versatile detector in our chromatographic processes, both MPLC and HPLC. The data transfer into the control software of our prep HPLC systems was straightforward. The Advion MS is shared with our R&D department for more conventional applications and gave both departments very quick access to MS data. Both departments appreciated the quick set-up, the user-training, and the reliable after sales service whenever a question pops up.
Q: TO WHOM WOULD YOU RECOMMEND THE EXPRESSION® CMS?
A: The Advion MS is a robust instrument that can be used in different environments. It does not require a lot of training and is easy to understand. Whenever you have a need for MS data, be it online or offline, Advion MS might give you very easy access to the data you need.
Overview:
Direct sample analysis is possible via an Atmospheric Solids Analysis Probe (ASAP®) combined with atmospheric pressure chemical ionization (APCI) on a compact mass spectrometer. This technique allows for the rapid investigation (<30 sec) of material suspected of containing trace amounts of explosive residues.
The expression® Compact Mass Spectrometer (CMS) with an Atmospheric Solids Analysis Probe (ASAP®) is a high performance instrument with a small footprint that allows for efficient liquid and solid screening at the point of need. The CMS provides rapid and accurate detection with significantly reduced false-positives and false-negatives than other techniques.
Here, we demonstrate the use of the ASAP® probe and expression® CMS detector for explosives screening. Sampling via the ASAP® probe is then inserted in to the APCI source of the mass spectrometer, initiating in a fast ionization reaction that provides rapid results.
Bacteria can be benign, beneficial and harmful, for more than 70 years we have been combatting these microscopic creatures with antibiotics. Increasingly though strains of antimicrobial resistant bacteria are becoming commonplace. This has motivated numerous studies aimed at deciphering the evolution of antibiotic resistance. Volatile Organic Compounds (VOCs) are ubiquitous in nature and are produced through various metabolic and catabolic processes. The profile of bacterial VOCs could therefore offer an insight into the detection of the type of bacteria and how they grow. This research utilizes a Volatile Atmospheric Pressure Chemical Ionization (vAPCI) source coupled to a Advion CMS instrument for detection of bacterial VOCs from in-vitro samples. This rapid and non-invasive approach of sampling VOCs and the implementation of a metabolomics workflow discriminates between E.coli and staphylococcus aureus and demonstrates how bacterial profiles can change over time.
Many chemical reactions carried out by synthetic chemists involve air-sensitive compounds such as metal catalysts and organometallics and must therefore be carried out in a glove box or using a Schlenk line to prevent oxidation and hydrolysis. Sampling and transportation of these samples to a mass spectrometer by an Atmospheric Solids Analysis Probe (ASAP®) without exposure to the air presents a problem.
Here, the inert ASAP probe (iASAP), a modification of the technique developed by Professor Ingo Krossing’s group at the Albert-Ludwigs-University of Freiburg, allows sampling and transportation in an environment of inert gas to prevent decomposition of the compound.
Shared live at the 254th ACS National Meeting in Washington, D.C. –
John Matson, Ph. D., Matson Research Group on Macromolecular and Supramolecular Chemistry, Assistant Professor, Virginia Tech.
Listen to the recorded workshop session highlighting the role of H2S in the human body and how compact mass spectrometry is used to assay peptides via direct injection for reaction monitoring, and coupled with HPLC for purification.
Many chemical reactions carried out by synthetic chemists involve air-sensitive compounds such as metal catalysts and organometallics and must therefore be carried out in a glove box or using a Schlenk line to prevent oxidation and hydrolysis. Sampling and transportation of these samples to a mass spectrometer by an Atmospheric Solids Analysis Probe (ASAP ®) without exposure to the air presents a problem. Here, the inert ASAP probe (iASAP), a modification of the technique developed by Professor Ingo Krossing’s group at the Albert-Ludwigs-University of Freiburg, allows sampling and transportation in an environment of inert gas to prevent decomposition of the compound.
Introducing a new type of mass spectrum, available exclusively in the Advion Peak Express™ software suite: the Delta Spectrum (ΔS). The ΔS is available with the expression® compact mass spectrometer (CMS) to look beyond chemical noise and automatically detect even the smallest peaks without knowing the m/z in advance.
With the Peak Express™ software featuring ΔS, you can:
Obtain clear detection of peaks without knowing their mass
Find adducts, dimers, fragments, side-reactions and other unexpected compounds at the click of a button, in real-time or with post-processing
Highlight minor components in complex mixtures and dirty matrices
Control mass-directed purification without providing the compound mass
Acquire XIC-quality data while scanning the entire mass range, allowing Peak Express™ to tell you the m/z
Advion Interchim Scientific’s range of AVANT®, high performance, liquid chromatography systems can be used standalone with UV and UV/Vis detector options, or with the expression® compact mass spectrometer to provide seamlessly integrated LC/CMS under the full control of Advion Interchim Scientific’s simple, intuitive Mass Express software suite.
Modular, stackable design, with many options, provides custom solutions for both HPLC and UHPLC needs. From the simplest manual injection HPLC to a fully automated, streamlined UHPLC system and everything in-between, the AVANT® series can be configured to fit your analytical requirements and your budget.
