Analytical Instrument Documents

JEOL RESONANCE Inc has developed a new NMR system, the JNM-ECZ series (* Notice) . Building on the experience of the JNM-ECAII/ECXII/ECS series, the JNM-ECZ series uses fully integrated cutting-edge digital technologies. In this report, some of the hardware features of the JNM-ECZ spectrometers (ZETA) are introduced.

University of Massachusetts Lowell’s NMR Spectroscopy Facility Manager, Wendy Gavin, discusses the importance of an NMR vendor that supports the constant challenge to be innovative. With over 13 years spent working in industry, 11 in a large pharmaceutical company, it is safe to say that Wendy Gavin knows the secret to successful nuclear magnetic resonance (NMR). Wendy has worked at the university for over six years and, as well as being the NMR Core Research Facility Manager, she also manages the University’s Analytical Chemistry lab. Her experience working in industry has provided unique insights into a customer’s requirements and enables her to ensure that the NMR facility at the University of Massachusetts Lowell is providing high quality data. Here, she explains the difference it makes to have an instrumentation vendor that goes the extra mile to support all users.

Last Updated: September 2013

Since 1998 the serious public health problem in South East Asia of counterfeit artesunate, containing no or subtherapeutic amounts of the active antimalarial ingredient, has led to deaths from untreated malaria, reduced confidence in this vital drug, large economic losses for the legitimate manufacturers, and concerns that artemisinin resistance might be engendered.

Last Updated: December 2014

High-resolution mass spectrometry (HRMS) continues to play an important role in the compositional characterization of larger organic molecules. In the field of polymer characterization, however, the application of HRMS has made only slow progress because of lower compatibility between matrix-assisted laser desorption/ionization (MALDI) and ultrahigh-resolution Fourier transform ion cyclotron resonance mass spectrometry (FT-ICRMS). In this study, a newly developed type of MALDI high-resolution time-of-flight mass spectrometry (TOFMS) with a spiral ion trajectory (MALDI spiral-TOFMS) was applied to the structural and compositional characterization of polymers. To create a graphical distribution of polymer components on a two-dimensional plot converted from complex mass spectra, we adopted a slightly modified Kendrick mass defect (KMD) analysis based on accurate masses determined using spiral-TOFMS. By setting the Kendrick mass scale based on the mass of the repeating units of a given polymer, components with common repeat units lined up in the horizontal direction on the KMD plot, whereas those components with different structures were shifted vertically. This combination of MALDI spiral-TOFMS measurement and KMD analysis enabled the successful discrimination of the polymer components in a blend of poly(alkylene oxide)s, the compositional analysis of poly(ethylene oxide)/poly(propylene oxide) block copolymers, and profiling of the end-group distribution of poly(ε- caprolactone)s synthesized under different conditions.

Traceability and authenticity of olive oils in Croatia were probed by a versatile analytical approach using spiral MALDI-TOF MS system for the triacylglycerol (TAG) analysis. Molecular ion patterns were shown to represent specific data for statistical analysis, in which differences of cultivar regions of Croatian coast were recognized. This pilot project allows indications to be followed in high throughput procedures with high number of samples to get statistically relevant data for discrimination of olive oils from different geographic sites. Additionally, the fragmentation in the TOF/TOF MS provided distinct highly valuable data for assignment of acyl residues. In this way molecular species with different fatty acid substituents can be clearly assigned and possible isomeric mixtures identified.

The structural characterization of copolymers by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) remains a challenging task, since their random comonomer distribution creates very complicated mass spectra. In this study, a high-resolution TOF mass spectrometer with a spiral ion trajectory was applied to the structural and compositional characterization of free radical copolymerized poly(methyl methacrylate-co-tert-butyl methacrylate), poly(MMA-co-tBMA)s in ethyl lactate acting as a chain transfer agent. Virtually complete peak assignments of the isobaric components within the poly(MMA-co-tBMA)s served to identify the end-group combinations and copolymer compositions of individual copolymer components, allowing the distributions of comonomer compositions and six types of end-group combinations to be evaluated.

Last Updated: September 2013

PaperSpray Principle: Samples and a polar solvent such as methanol are deposited onto a porous substrate such as filter paper or chromatography paper cut into a triangle. When a high voltage (typically ~3000V) is applied, Electrospray Ionization (ESI) occurs at the tip of the paper triangle. PaperSpray is simpler than ESI and does not require a pump, spray needle, desolvating gas or precise alignment.