Ultra (high) performance liquid chromatography (UPLC/UHPLC) is a relatively new technique, and is valued for its speed, efficiency and the quality of information provided. Many synthetic and medicinal chemistry laboratories are moving to this process to improve their workflows and save time.
Mass Directed Fraction Collection
The Advion expression Compact Mass Spectrometer (CMS) was coupled to a Normal Phase Flash Chromatography system for mass directed fraction collection. Typically a UV detector is used to monitor compounds eluting from Normal Phase columns. A limitation of the UV detector is that it relies on compounds having a chromophore in the chemical structure, hence an analyte of interest may not be detectable if it lacks a suitable UV chromophore or coelutes with another compound. In addition, solvent systems can interfere with and hinder UV absorbance. The Advion expression CMS provides the ultimate in selectivity, unambiguously identifying residual starting materials, desired product ions, side reactants and impurities by their molecular weight despite co-eluting compounds and solvent peaks. Mass directed fraction collection greatly speeds up the chemist’s work flow with confidence in the content and purity of the collected fractions by eliminating off-line TLCs, workup and core lab LC/MS assays.
Northeastern State University, Natural Sciences Department
Q: What is the focus of your lab’s research?
A: Our laboratory is primarily a teaching laboratory for undergraduate and graduate students to gain exposure to current chemistry technology. Several techniques are practiced for medicinal chemistry and synthetic organic chemistry applications including TLC, reaction monitoring, and UV-vis.
Q: Why did you incorporate the expression cMs into your laboratory?
A: As a small university, we face unique challenges of limited resources in both space and funding. Mass spectrometers are a powerful detector, and it is important that our students gain exposure to this analytical technique; however, purchasing one was out of our reach. The expression CMS has allowed us to not only bring this commonly used technology to the hands of our students, but also has resulted in faster data. Our students no longer have to wait up to a month for results from an outsourced partner. They know right away whether what they set to accomplish was successful.
Q: Who Would you recoMMend to purchase the expression cMs?
A: I recommend the expression CMS to all teaching labs that wish to expose their students to this technology in a fast and easy-to-use platform.
Rapid Screening of ‘White Powders’ for Unknown Agents Using a DART-Equipped Compact Mass Spectrometer
The expression® compact mass spectrometer (CMS) was developed based on decades of chemistry and mass spectrometry experience specifically to meet the needs of chemists. Many chemists are asked to perform their work in the field, and the CMS was built to be versatile. It is available with a TACOM-compliant Mobile Attenuation Mounting (MAM) system. This allows the CMS to be placed in a mobile laboratory environment and driven for the equivalent of the life of the vehicle while remaining fully functional to all specifications. Many global FDA agencies, state labs, Level 1 responders, and others wish to install CMS in a mobile laboratory setting taking the CMS to a field-based point-of-assay. In certain instances, large corporations wish to have the unit fully transportable within large plant settings. The MAM system is developed to international operating standards.
The flexibility of the CMS can be seen in a recent poster presentation given at this year’s ASMS meeting in Minneapolis. The poster is available for download.
Max Planck Institute for Coal Research, Germany
Q: What is the focus of youR lab’s ReseaRch?
A: Our activities on lignin chemistry cover the extraction of lignin by the organosolv process, characterization of lignin and development of catalysts for lignin hydrogenolysis, oxidation and depolymerization.
The similarity between the chemical structures of low ranking coals and lignin encourages us to develop integrated strategies to process coal and biomass together. Our activities on coal chemistry cover the direct coliquefaction of low ranking coals and biomass to produce liquid fuels.
Furthermore, we are aiming at understanding the process of dissolution of cellulose in nonconventional solvent systems and are exploring the reactivity of cellulose in new solvent systems.
Q: What pRevious WoRkfloW challenges DiD you expeRience?
A: Many scientists generating a high number of diverse compounds need fast and direct access to the exact mass data for those compounds. Thus, we had to find a way to conduct most of the mass determination directly in our laboratory in a timely and cost-efficient way.
Q: Why DiD you incoRpoRate the expRession cMs into youR laboRatoRy?
A: The purchase of Advion expression compact mass spectrometer reveals to be an excellent investment. We are performing analyses of complex samples (e.g., lignin, cellulose and coal products) in a multi-user environment. As such, the Advion device is very easy to operate as well as a robust and very reliable mass spectrometer, surpassing all the expectations that we had for an affordable device.
Simple, high-performance coupling of SFC to CMS for mass-directed fraction collection
This is one from a set of two application notes. In this application note, we review recovery and purity determination of two, three component standard mixtures by supercritical fluid chromatography (SFC) couped with the Advion expression Compact Mass Spectrometer (CMS).
For the other application note on the fraction collection of a 0.2% impurity, click here.
Advion co-authored with a major pharmaceutical partner to create two application notes highlighting the benefits of supercritical fluid chromatography (SFC) coupled to a compact mass spectrometer for mass directed fraction collection. These application notes conclude that mass‐directed fraction collection with a simplified passive splitter on the Preparative JASCO SFC coupled with expression CMS system increases purification selectivity by mass directed fraction collection while maintaining excellent recovery and purity. The MS accepted high concentrations of sample material with peak shapes trailing edges almost indistinguishable from the UV trace. Low, Middle and High isocratic flow rates all showed comparable MS source clearance leading to minimal tailing beyond the UV. Gradients further minimized peak tailing as expected on the UV and this was also seen on the TIC and XIC. Peak purities for all main band purifications were ≥99.9% pure and minor impurity collections showed equivalent success yielding 100% pure fractions. Acceptable recoveries for all collected fractions were 94% or better.
Ultimate in Analytical Flexibility. Multi-Mode expression CMS
The expression CMS was developed with the chemist’s objectives and laboratory workflow in mind. Organic, Natural Product and Peptide chemists utilize many techniques to determine the progress, yield and purity of their reactions.
Prep scale SFC/CMS Interface – passive split
Supercritical fluid chromatography (SFC) is a fast growing technique. Initially used almost exclusively for only thermally labile and chiral compounds it is now becoming accepted as a versatile analytical technique applied across a broad range of compounds. It is faster and higher-throughput than regular HPLC and Preparative LC and becoming popular as a ‘green’ technique, with far lower solvent consumption and lower consumable cost than HPLC. SFC is also compatible with a wide range of detection methods including electrospray (ESI) and atmospheric pressure chemical ionization (APCI) mass spectrometry.
Download this product note to see how SFC combined with compact mass spectrometry (CMS) offers chemists several benefits.
Terminalia Tomentosa Roxb (ex DC) Wight & Arn: Phytochemical Investigatio
Goa College of Pharmacy
Abstract
The present study was undertaken to carry out phytochemical investigation of the ethanolic extract of the stem bark of Terminalia tomentosa Roxb (ex DC) Wight & Arnbelonging to the family Combreteaceae. The plant is known in Sanskrit as Asana, in English as Black murdah, in Hindi as Asan, Saj, Sain and in Marathi as Ain.The plant has been known to possess various pharmacological activities like antifungal, antioxidant, antihyperglycaemic, antidiarrhoeal, antileucorrheal etc. The bark of the plant is astringent& useful in ulcers, vata, fractures, haemorrhages, bronchitis, diarrhoea etc.Preliminary phytochemical screening of the ethanolic extract of stem bark revealed the presence of carbohydrates, flavonoids, triterpenoids,steroids, tannins and saponins. The chemical entities isolated and characterised includes 4 – methy l – 4 – hydroxymethylene – 6β – (10 – methyl octanyl) cyclohexane (Arjuna homoses quiterpenol), di-n-octyl phthalate, di isobutyl phthalate and dibutyl phthalate. All these phytoconstituents are reported for the first time from the ethanolic extract of stem bark of T.tomentosa.
Mass spectra was obtained by ESI ionization using the Advion expression Compact Mass Spectrometer (CMS).
Application with Mass Directed Preparative SFC Utilizing the JASCO Preparative SFC platform and Advion expression® Compact Mass Spectrometer
In this study we evaluated the performance of a Preparative SFC‐MS system combining the JASCO Preparative SFC with the Advion expression® CMS (Compact Mass Spectrometer) utilizing a simplified passive splitter for mass‐directed fraction collection. The initial test explored a wide range of flow rates both isocratic and gradient to test performance and reliability of the passive splitter, coinciding timing of MS and UV signal and the clearance of the source with highly concentrated samples.