EPSRC NATIONAL MASS SPECTROMETRY SERVICE CENTRE AT SWANSEA 2007 to 2012

Lead Research Organisation: Swansea University
Department Name: Institute of Life Science Medical School

Abstract

The continuation of the EPSRC National Mass Spectrometry Service Centre (NMSSC) at Swansea will ensure that a proven high-quality mass spectrometry service at a very reasonable cost will be delivered to the UK Chemistry research base. This vital facility will help underpin the competitiveness of UK Science by providing excellent service quality with rapid sample turnaround time and high analytical success rate. The track record of the Centre at Swansea, extending over twenty years of exemplary service to the chemistry community, is attested with attainment of an unprecedented full set of six top-performance indicators from the Research Council's annual review panel in 2005. Most universities have their own mass spectrometers and the role of the service will shift to reflect this by: i) assisting departmental services to obtain good quality data on their own instruments; ii) assisting chemists to understand the data and use it appropriately and iii) analysing the samples that cannot be done in-house, either because of lack of technology or lack of expertise.Two new instruments are requested to replace three long-service mass spectrometers, both to maintain and to improve the present level of service, whilst increasing the capability for accurate mass measurement and complex sample analysis. Additionally, the limited remaining areas of analytical difficulty will be tackled by the purchase of relatively minor items of equipment, special spectrometer features and targeted research projects. These improvements will assist the National Centre to keep pace with the progress of modern chemistry and its broadening interface with other disciplines.Service activities such as matrix-assisted laser desorption/ionisation and other difficult analyses are expected to increase, and the publicity and training portfolios will increase concomitantly to extend the service into new areas of science and offset the growing usage and complexity of mass spectrometry. The training programme will assist departments to use the National Service and their own equipment more effectively, and thus also add value to previous research council investments. Outreach to the chemistry community will be by collaborations, shared doctoral training account studentships, and consultation on matters of the Centre's expertise, including instrument procurement, if required. The WWW will assist dissemination of knowledge.Scheduling time for use of the service will continue to be by a documented process monitored annually by the external Management Advisory Panel, and biased heavily towards EPSRC-funded research, ensuring that internationally competitive research is supported.The service will continue to provide high quality data, spectral interpretation and educational commentary on the results. Programmes for staying at the forefront of technology and maintaining professional standards of staff will also be in place.Another improvement to the Service will include extension of the Electronic Customer Interface whereby users log their samples for analysis and view the results electronically. The electronic interface will also allow future provision of an archive of mass spectral information of unique samples as a national resource. A key feature of the new Service will be routine accurate mass measurement of molecular and fragment ions with increased use of isotope information, these together will be a powerful tool for the unambiguous characterisation of chemical substances even when present in a mixture.Enhanced performance will be achieved by using key performance indicators to improve the quality of service and level of customer satisfaction.A strength of the Swansea NMSSC is its presence in the mass spectrometry-rich academic and research environment of the Institute of Mass Spectrometry.Resource accruing to the host institution from this grant will be used for further research in mass spectrometry and analytical chemistry.

Publications

10 25 50
 
Description A cost-effective Centre of Excellence in Mass Spectrometry using proven state-of-the-art techniques was provided to the UK scientific community to underpin high quality chemical research.

High quality mass spectra data with fast turnaround times were supplied to EPSRC-supported research groups in UK Universities.

Assistance with data interpretation was provided to these groups to ensure optimal use of the data obtained.

Specialist MS services, not readily available in other UK universities, were provided as well as general MS facilities to the user community that may have had no other access to mass spectrometry.

Developments in mass spectrometry were monitored, and advice provided, to the wider academic community on the scope of available techniques and new developments in the field.

Training courses in both technical and academic aspects of mass spectrometry were delivered to improve the knowledge of MS in the UK academic community (ie. Summer School courses, Outreach and arranging visits for training at the NMSSC at Swansea).

Students and technical staff from approved EPSRC-supported research groups in UK Universities were educated in various aspects of MS, as required, in order to optimise their use of MS.

Advice was given, as required, to institutions investigating the purchase of new mass spectrometers or other equipment in which the National Centre has expertise.
Exploitation Route The National MS Centre hosts work experience student visits, either as individuals or as groups visiting the Centre as part of a wider scheme run by the College of Medicine. The purpose of these visits is to introduce mass spectrometry to as wide a community as possible and to encourage potential young scientists on a career path in this area. As discussed above, the EPSRC National Mass Spectrometry Service Centre at Swansea provides a vital service in underpinning the competitiveness of UK science. In addition to supporting highly rated projects, the Centre provides time for young researchers and those with limited local facilities, as well as supporting local facilities that may be experiencing temporary failure or difficulties. Extensive training programmes, assessment of new technologies, and presentation of the Centre's own research at conferences and meetings are also within the Centre's remit.
Sectors Chemicals,Education,Energy,Environment,Healthcare,Pharmaceuticals and Medical Biotechnology,Other

 
Description Accommodation of local scholars and students requiring work experience: the NMSSC was certified by Careers Wales in 2011 to welcome year 10-13 students for work experience in a controlled, productive and safe scientific environment. The Centre has also provided demonstrations and presentations to numerous visiting groups of students from local schools as a means of raising awareness of, and interest in, the variety of careers available in science.
First Year Of Impact 2007
Sector Education
Impact Types Cultural,Societal

 
Title Accurate mass measurement of positive radical ions by MALDITOFMS using porphyrin based calibration standards 
Description Accurate mass measurement increases the certainty of analyte identification, and general background literature and operational guidelines are available. At the NMSSC, computer-assisted peak matching on a magnetic sector instrument with an electrospray (ESI) source is preferred for the wide range of samples received. Alternative sources are used where ESI is not appropriate, and while these systems generally give excellent results, some samples specifically require MALDI ionisation. A method for the accurate mass measurement of positive radical ions by MALDI-TOFMS was developed recently in our laboratory. Greater accuracy is achieved when radical ions are calibrated with radical ion standards, hence tetra-substituted porphyrin calibration standards have been developed. Sequential increase of the alkyl chain length, plus occasional phenyl groups, provides standards that cover the practical mass range of = 1000 Da. 
Type Of Material Improvements to research infrastructure 
Year Produced 2006 
Provided To Others? Yes  
Impact Enabled the challenging area of accurate mass measurement by MALDI using porphyrin based calibration standards to bracket the ion of interest. 
 
Title Analysis of functionalised fullerenes by MALDI-TOFMS, including accurate mass measurement 
Description Matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOFMS) allows the analysis of functionalised fullerenes with minimal fragmentation. In early experiments, the traditional polar acidic matrices did not perform well, and it was only with the development of the matrix 2-[(2E)-3-(4-tert-butylphenyl)-2-methylprop-2-enylidene]malononitrile (DCTB) that molecular ions were observed, irrespective of the analyte functional group. DCTB is an aprotic, electron-transfer matrix, so its' properties are similar to those of fullerenes, and may be used in both positive and negative ion modes. More recently, sulphur (S8), 9-nitroanthracene,trans-4-tert-butyl40-nitrostilbene (TBNS) and trihyroxyanthracene have all given acceptable data, but in our experience DCTB in negative ion mode gives consistent clean spectra with very good signal-to-noise ratiossupplied by Applied Biosystems. 
Type Of Material Improvements to research infrastructure 
Year Produced 2011 
Provided To Others? Yes  
Impact Analysis of functionalised fullerenes with minimal fragmentation by negative ion MALDI-TOF MS with DCTB matrix, an improvement on previous methodology. 
 
Title Application of solvent-free preparation methods for the analysis of organometallic and coordination complexes by MALDI-TOFMS 
Description Matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOF-MS) is an important and successful analytical technique for a wide variety of compounds. A traditional dried-droplet sample preparation technique relies on sample and matrix combinations that are soluble in the same volatile solvent or miscible solvents. However, many samples submitted to our Centre are insoluble or only soluble in less volatile solvents e.g. dimethyl sulphoxide. Development of a solvent-free MALDI method would complement other solvent-free ionisation techniques, offering a softer method of ionisation, and allowing analysis of compounds not suited to these other techniques. Previous work in this area has focussed mainly on synthetic polymers, but has also been applied to biochemical samples. Preliminary investigations into the analysis of various first-row transition metal acetylacetonate complexes using assorted literature and NMSSC solvent-free methods were summarised in a recent conference poster. The preparation method of ball-milling the sample and matrix mixture, followed by 'smearing' onto the target plate, including our own variations, is evaluated here for vanadium (III) acetylacetonate (V(acac)), in order to establish a reliable protocol. In addition, two insoluble samples submitted to the NMSSC are examined as case studies. 
Type Of Material Improvements to research infrastructure 
Year Produced 2007 
Provided To Others? Yes  
Impact Development of a solvent-free MALDI method that complements other solvent-free ionisation techniques, offering a softer method of ionisation, allowing analysis of compounds not suited to these other techniques such as solvent, air and moisture sensitive samples that often prove problematic to analyse successfully. 
 
Title Atmospheric Solids Analysis Probe (ASAP) on a Thermo Fisher LTQ Orbitrap XL 
Description The Atmospheric Solids Analysis Probe (ASAP) allows rapid and sensitive ionisation of samples obtained in solid or liquid forms. It can easily be fitted to any modern mass spectrometer with an atmospheric pressure chemical ionisation (APCI) source. 
Type Of Material Improvements to research infrastructure 
Year Produced 2011 
Provided To Others? Yes  
Impact Application of a rapid and sensitive technique for ionisation of a huge variety of samples obtained in solid or liquid forms. 
 
Title Boronic Acid Analysis by Mass Spectrometry - I: Cis-diol Derivatisation for EI and CI Analysis 
Description Mass spectrometry analysis of boronic acids by conventional methods, using a variety of ionisation modes, has often failed to show molecular species. In particular, EI and positive ion CI have generally been unsuccessful in our laboratory. We have therefore developed a derivatisation method to allow effective EI and CI analysis by characterisation of the less reactive ester from of the boronic acid. The esterification is based on a well documented reaction [1], commonly used in recent decades in affinity chromatography methods for the analysis of a wide variety of cis-diols [2]. In our application, the reaction is effectively used for the reverse effect, using the diol to facilitate analysis of the boronic acid, rather than using the acid to enable analysis of the diol. We recognise that it would be preferable to analyse the boronic acids without derivatisation, and research is currently in progress to establish more reliable methods for this. Electrospray, APCI and MALDI all show promise, and are the subject of initial studies. Any useful findings should be published on this website and more widely as they progress. 
Type Of Material Improvements to research infrastructure 
Year Produced 2008 
Provided To Others? Yes  
Impact Development of a simple derivatisation method to allow effective EI and CI analysis by characterisation of the less reactive ester from of previously porblematic boronic acids. 
 
Title Boronic Acid Analysis by Mass Spectrometry - II: Atmospheric Solids Analysis Probe (ASAP) 
Description Boronic acids have been notoriously difficult to analyse without the need for derivitisation. Until recently, the method utilised at the NMSSC required the use of 1,2-ethanediol to create an ester that could be analysed by electron ionisation (EI) or chemical ionisation CI. Previously, a study was instigated to investigate the ideal conditions for the generation of a molecular or pseudo-molecular species using atmospheric pressureionisation (API) techniques and mass spectrometry. Boronic acids are used widespread throughout the chemical, and biochemical world. The need for an easy, rapid method of generating an intact (pseudo-) molecular species has been a goal for many years. There has been a recent literature report of the analysis of boronic acids by nano liquid chromatography-direct electron ionization mass spectrometry, using a system built in-house. The authors showed that their system was able to produce a molecular species with the added benefit of chromatographic separation. Presented here is a method which any modern APCI instrument can be modified to perform. 
Type Of Material Improvements to research infrastructure 
Year Produced 2011 
Provided To Others? Yes  
Impact Development of an easy, rapid method of generating an intact (pseudo-) molecular species for Boronic Acids using an Atmospheric Solids Analysis Probe (ASAP). 
 
Title Electrospray Accurate Mass Measurement Using Polyethylenimine as an Internal Reference Standard 
Description The determination of the elemental formulae of small molecules can be achieved by accurate mass measurement. Accurate mass spectrometry has been summarised elsewhere and guides are available. At Swansea, computer-assisted peak-matching accurate mass spectrometry is the preferred method, using polyethylenimine (PEI) as the internal reference standard. PEI is suitable for measurements between m/z 150 and 1200. 
Type Of Material Improvements to research infrastructure 
Year Produced 2006 
Provided To Others? Yes  
Impact Implementation of a simple, readily available polymer, polyethylenimine (PEI) as an internal reference standard for accurate mass electrospray for measurements between m/z 150 and 1200. PEI is a superior polymer to use for this purpose as it crates a good distribution of ions across the m/z range without creating lasting carryover when not required. 
 
Title The advantageous use of stepped in-source (cone) voltages in electrospray mass spectrometry for compound characterisation and the identification of mixtures. 
Description The relative abundances of ions in electrospray are affected by the in-source voltages (e.g. cone voltage) applied. This phenomenon can be used to advantage in the characterisation of chemical compounds, the identification of unknown species and the recognition of mixtures, and is used routinely in our laboratory for all electrospray (ESI) analyses for these purposes. The method should be generally useful on almost any ESI instrument, in either polarity, but in this illustration, for simplicity, we just describe it on the Waters ZQ4000 in positive ion mode. 
Type Of Material Improvements to research infrastructure 
Year Produced 2006 
Provided To Others? Yes  
Impact Facilitating characterisation of chemical compounds, identification of unknown species and recognition of mixtures using a simple application of in-source cone voltage in electrospray MS analysis. 
 
Title The use of 2-[(2E)-3-(4-tert-Butylphenyl)-2-methylprop-2- enylidene]malononitrile (DCTB) matrix in MALDI-TOFMS 
Description DCTB is a nonpolar, aprotic matrix, and may be used in the analysis of a variety of compounds by MALDITOFMS.The classes of compounds include coordination compounds, organometallics, conjugated non-polar organic compounds, and polar organic compounds. Comparisons are made with spectra acquired with the use of 1,8,9-trihydroxyanthracene (dithranol), 2,5-dihydroxybenzoic acid (DHB) matrices. DCTB is a charge-transfer matrix, therefore, radical ions are observed. Exceptions to this are salts, when constituent positive and negative ions, usually singly charged, are observed, and polar samples, when metal adduct formation is promoted. Certain limitations of DCTB are noted and good working practices for the use of the matrix are also outlined. 
Type Of Material Improvements to research infrastructure 
Year Produced 2006 
Provided To Others? Yes  
Impact Improved MALDI data generated for a variety of compounds by a simple preparation procedure using DCTB matrix. 
 
Description A statistically rigorous framework for the analysis of biological mass spectrometry data 
Organisation Swansea University
Department Institute of Mass Spectrometry (IMS)
Country United Kingdom 
Sector Academic/University 
PI Contribution MRC Fellowship to develop a mathematical model to describe a pulse-height distribution arising as a result of a single ion arrival on a mass spectrometer's detector system and investigate mathematical methods for understanding their superposition.
Start Year 2012
 
Description Advanced solid-state multi-stage biomolecule separations 
Organisation Porvair Filtration Group Ltd
Country United Kingdom 
Sector Private 
PI Contribution The development of tools/technologies underpins advances in our understanding of biological systems. A key approach is proteomics. Advances in proteomic technologies have occurred in recent years with e.g. differentially-labelled proteins analysed through 2D gel electrophoresis, and sophisticated liquid chromatography such as MudPit. Both have been coupled with mass spectrometry developments, for "bottom up" and "top down" approaches, for biomolecule analysis that continues to offer improvements in accuracy/sensitivity for protein identification/structure. Disposable pre-LC column based technologies have proved important in proteomics, yet are largely limited to functionalised agarose/sepharose 'beads' for mainstream application. Such systems are limited by the requirement for specialist packing, loss of free 'beads' and therefore surface availability, and sample loss through 'dead space' in columns. To attain the necessary throughput, proteomics continues to advance, requires a step change in early process separation technologies. We propose to develop a solution through the rational application of functionalised solid state, agarose free, separations. Base technology, BioVyon, has been developed Porvair (CASE partner). This project will develop a high-throughput serial-filtration approach for the rapid sample preparation necessary in advanced proteomics. Columns assembled for differential multi-stage biomolecule separation will be developed for separation of complex protein samples. Simulation of online separation strategies will enable optimal online column design, and inform future functionalisation strategies. The flexibility of this solid-state approach has the potential to impact significantly on high throughput proteomics. This project will develop a high-throughput serial-filtration approach for the rapid sample preparation necessary in advanced proteomics. Columns assembled for differential multi-stage biomolecule separation will be developed for separation of complex protein samples. Simulation of online separation strategies will enable optimal online column design, and inform future functionalisation strategies.
Start Year 2012
 
Description Collaboration with Manchester University Mass Spectrometry Service 
Organisation University of Manchester
Country United Kingdom 
Sector Academic/University 
PI Contribution A Collaboration with Manchester University Mass Spectrometry Service was established to exchange staff expertise, use of equipment and training. Staff from Manchester Mass Spectrometry Service (Gareth Smith, Rehana Sung, Carole Webb) have received training at NMSSC; Samples have been analysed for the service at times of instrument breakdown or backlog.
Start Year 2007
 
Description Collaboration with Mass Spectrometry Service, Department of Chemistry University of Edinburgh 
Organisation University of Edinburgh
Country United Kingdom 
Sector Academic/University 
PI Contribution Training and exchange of ideas has been ongoing with the Mass Spectrometry Service, Department of Chemistry University of Edinburgh. Alan Taylor, a senior mass spectrometrist at the Mass Spectrometry Service in Edinburgh, spent 5 days at the EPSRC NMSSC to improve his expertise with the MAT 900 and MAT95 to ensure optimal sample analysis.
Start Year 2009
 
Description DTA PhD Studentship I 
Organisation University of Oxford
Department Department of Chemistry
Country United Kingdom 
Sector Academic/University 
PI Contribution Establishment of DTA PhD Studentship with Dr Simon Aldridge in the Department of Chemistry, University of Oxford. Ms Victoria Chislett was the successful graduate to attain the studentship.The project involves the synthesis of organometallic polymers and the use of a range of techniques, including mass spectrometry to assess polymer electronic/physical properties and applications. The DTA student has not completed this studentship due to ill health, but much progress was made in the first two years of her studies.The project involved the synthesis of organometallic polymers and the use of a range of techniques, including mass spectrometry to assess polymer electronic/physical properties and applications.
Start Year 2007
 
Description DTA PhD Studentship II 
Organisation University of Cambridge
Country United Kingdom 
Sector Academic/University 
PI Contribution Establishment of DTA PhD Studentship with Prof Carol Robinson, Project: Dissecting the assembly of heterogenous multi-protein complexes using mass spectrometry. Mass Spectrometry was used to study large multi-protein complexes: Yeast Nucleosome Assembly Protein (NAP1), Heat shock protein 90 (Hsp90) and transcription factor II D (TFIID). Interactions of NAP1 with histones H2A and H2B were characterised, and insights gained on subunit interactions in TFIID complex. An informative interaction network between Hsp90 and its co-chaperones was obtained, simultaneously unravelling the heterogeneity, kinetics and dynamics of fourteen Hsp90 chaperone complexes.
Start Year 2008
 
Description DTA PhD Studentship II 
Organisation University of Oxford
Country United Kingdom 
Sector Academic/University 
PI Contribution Establishment of DTA PhD Studentship with Prof Carol Robinson, Project: Dissecting the assembly of heterogenous multi-protein complexes using mass spectrometry. Mass Spectrometry was used to study large multi-protein complexes: Yeast Nucleosome Assembly Protein (NAP1), Heat shock protein 90 (Hsp90) and transcription factor II D (TFIID). Interactions of NAP1 with histones H2A and H2B were characterised, and insights gained on subunit interactions in TFIID complex. An informative interaction network between Hsp90 and its co-chaperones was obtained, simultaneously unravelling the heterogeneity, kinetics and dynamics of fourteen Hsp90 chaperone complexes.
Start Year 2008
 
Description DTA PhD Studentship III 
Organisation Swansea University
Department Institute of Mass Spectrometry (IMS)
Country United Kingdom 
Sector Academic/University 
PI Contribution Shared DTA PhD Studenship with Dr Yuqin Wang: Ian Richard Gilmore Chemical Proteomics to characterise the emerging roles of oxysterols and oxysterol-mediated protein-protein interactions.
Start Year 2008
 
Description DTA PhD Studentship IV 
Organisation Swansea University
Department Institute of Mass Spectrometry (IMS)
Country United Kingdom 
Sector Academic/University 
PI Contribution Shared DTA PhD Studentship with Prof Brenton (IMS). Andrew David John Williams Development of atmospheric pressure ionization techniques using a novel liquid sampling system based on a miniature electrophoretic liquid focussing device. This thesis describes the development of a prototype liquid electrohydrodynamic sampling device, based on existing spotting and sampling systems. The hypothesis relates to the development of devices that could both control and shape a liquid meniscus by applying an electrostatic field of appropriate strength.
Start Year 2009
 
Description DTA PhD Studentship V 
Organisation Swansea University
Country United Kingdom 
Sector Academic/University 
PI Contribution Shared DTA PhD Studentship with Prof William Griffiths (IMS): Micheal Ogundare Lipodomics of the Central Nervous system About 25% of the body?s cholesterol is found in the central nervous system (CNS). This is true for all animals. Cholesterol is metabolised in brain to sterols and steroids, these are present at very low levels in comparison to cholesterol. Despite their low level, sterol and steroid metabolites are biologically active molecules, and are believed to be important in memory and cognition. Deranged cholesterol metabolism is suggested to be responsible for many neurodegenerative diseases including Alzheimer?s disease and Huntington?s disease. Sterols and steroids are present at ng/g - _g/g levels in brain as compared to cholesterol which is present at the mg/g level, and their analysis by conventional methods is challenging. Because of this, their profile in CNS has been poorly characterised. In this project we used newly developed ultra sensitive mass spectrometry methods to analyse sterols and steroids in CNS. We identified the molecular species present and their concentrations. We similarly explored the sterol/steroid content of plasma. Sterol and steroid metabolites are biologically active molecules, believed to be important in memory and cognition. Deranged cholesterol metabolism is suggested to be responsible for many neurodegenerative diseases including Alzheimer?s disease and Huntington?s disease. Newly developed ultra sensitive mass spectrometry methods were used to analyse sterols and steroids in CNS. Molecular species and their concentrations were identified.
Start Year 2008
 
Description DTA PhD Studentship VI 
Organisation Swansea University
Department College of Medicine
Country United Kingdom 
Sector Academic/University 
PI Contribution Shared DTA PhD Studentship with Dr Paul Lewis (College of Medicine): Sion Bayliss Investigation of metabolomics: biomarkers for early detection of lung cancer by GC/MS and LC/MS
Start Year 2008
 
Description DTA PhD Studentship VII 
Organisation Swansea University
Department DNA Damage Research Group
Country United Kingdom 
Sector Academic/University 
PI Contribution Shared DTA PhD Studentship with Dr George Johnson (College of Medicine): Adam David Thomas. Investigations of points of departure (PoD) for potent DNA reactive mutagenic substances. Investigations points of departure (PoD) for potent DNA reactive mutagenic substances. This work focused on the super-mutagen methyl-nitrosourea (MNU) and the DNA repair mechanism involved with the PoD. The experiments were carried out in vitro using the HPRT gene mutation assay in human lymphoblastoid cells, and mass spectrometry was used to quantify DNA adduct levels at different concentrations through the mutation dose response.
Start Year 2009
 
Description DTA Studentship Environmental Analysis Team (Mr David Atkins) 
Organisation Swansea University
Country United Kingdom 
Sector Academic/University 
PI Contribution This is a studentship with Dr A R Godfrey concerning the environmental fate and impact of pharmaceuticals in environmental samples. In particular the aims of this work will be to investigate the products of commonly prescribed pharmaceuticals generated from secondary sewage treatment using ion trap liquid chromatography-mass spectrometry (LC-MSn). The project will involve considerable method development; successful method(s) will potentially be used in assessing the levels of commonly prescribed pharmaceuticals in these samples and used within the Environment Agency screening programme. We have supported this work through research supervision and training, providing access to specialist equipment when required.
Collaborator Contribution Funding of PhD and contribution to some small items of equipment and support of travel to conferences.
Impact This is a multidisciplinary collaboration covering analytical science (sample preparation, chromatography, mass spectrometry) and environmental science. This studentship is on-going with work only disseminated as research presentations up to this point.
Start Year 2012
 
Description DTA Studentship Environmental Analysis Team (Ms Rachel Townsend) 
Organisation Swansea University
Country United Kingdom 
Sector Academic/University 
PI Contribution This is a studentship with Dr A R Godfrey concerning the environmental fate and impact of pharmaceuticals in environmental samples for the Chemical Investigation Programme II. In particular the aims of this work will be to investigate the pharmaceutical content of wastewater within urban and semi-urban catchments containing several hospitals and relevant biota using LC-MS. This work will help underpin future environmental and public health policy for pharmaceutical pollutants with potential risk to human health supporting the inclusion/exclusion of the chosen pharmaceuticals on the 'watch list' in accordance with the EU timeline (i.e. by 2017). We have supported this work through research supervision and training, providing access to specialist equipment when required.
Collaborator Contribution Funding of PhD and contribution to some small items of equipment and support of travel to conferences.
Impact This is a multidisciplinary collaboration covering analytical science (sample preparation, chromatography, mass spectrometry) and environmental science. This studentship is on-going with work only disseminated as research presentations up to this point.
Start Year 2014
 
Description DTA Studentship Ionization group development on flowing afterglow atmospheric pressure sources (Ms Charlotte Davies) 
Organisation Swansea University
Country United Kingdom 
Sector Academic/University 
PI Contribution Expertise in designing sources, equipment contributions, time on instrumentation (Orbitrap and Xevo). A Flowing Atmospheric Pressure Afterglow (FAPA) ionisation source to extend the capability of an Orbitrap MS to cover compounds that are difficult to ionize or could benefit from an alternative ionization method.
Collaborator Contribution Funding of PhD and contribution to some small items of equipment and support of travel to conferences.
Impact Patent in preparation with commercial company and Swansea Innovations Ltd.
Start Year 2014
 
Description DTA Studentship Mr Andrew Williams 
Organisation University of Rwanda
Country Rwanda 
Sector Academic/University 
PI Contribution MS instrumentation Orbitrap time to undertake the project analysis, supply of some materials connected to the application of some items from the Advion Triversa sampling system to the research. We helped design an Electro-Focusing Liquid Extractive Surface Analysis (EF-LESA) Coupled to Mass Spectrometry whereby analysis of the chemical composition of surfaces by liquid sampling devices interfaced to mass spectrometry is made from a sample stream continuously monitored at good sensitivity and selectivity. A sampling probe has been constructed that takes discrete liquid samples (typically <100 nL) of a surface. It incorporates an electrostatic lens system, comprising three electrodes, to which static and pulsed voltages are applied to form a conical "liquid tip", employed to dissolve analytes at a surface. A prototype system demonstrates spatial resolution of 0.093 mm2.
Collaborator Contribution Swansea University - Funding of PhD and contribution to some small items of equipment and support of travel to conferences. Some advice and materials were supplied by Advion Corporation, supplier for the Triversa, primarily from the UK agent Dr Mark Allen, and support engineer time.
Impact dx.doi.org/10.1021/ac4035136
Start Year 2009
 
Description DTA Studentship TESA Toroidal Team (Mr Will Johnson) 
Organisation Swansea University
Country United Kingdom 
Sector Academic/University 
PI Contribution Design of instrumentation and ion optics experience, programmes and instrumentation development in laboratory with donation of equipment to build a prototype system
Collaborator Contribution Funding of PhD and contribution to some small items of equipment and support of travel to conferences.
Impact 1. Patent in preparation with Swansea University Ventures. 2. Papers in preparation will be submitted for publication once patent process is complete and safe.
Start Year 2013
 
Description Identification of novel bioactive compounds from natural sources and investigation of the bioavailability and interaction of these molecules in their specified target organisms / biochemical pathways. 
Organisation Swansea University
Country United Kingdom 
Sector Academic/University 
PI Contribution Application of Fasttrack MALDI, GC/MS and nanoelectrsopray on the Orbitrap for identification of novel bioactive compounds from natural sources and investigation of the bioavailability and interaction of these molecules in their specified target organisms / biochemical pathways. Dr Dudley collaborates with NMSSC to share facilities and exchange knowledge to aid in the identification of novel bioactive compounds from natural sources and invesigate the bioavailability and interaction of these molecules in their specified target organisms/biochemical pathways. Additionally, Dr Dudley studies modified nucleosides that are naturally produced in nucleic acid structures, their role in tRNA function and their occurrence and excretion under different metabolic conditions.
Start Year 2007
 
Description Intercomparison Study of Mass Spectrometric Analysis of Boronic Acids 
Organisation AstraZeneca
Country United Kingdom 
Sector Private 
PI Contribution Implementation of an Intercomparison study involving ESI, MALDI, APPI and APCI on a variety of analysers to establish a more reliable method of analysis of boronic acids. The aim of collaboration was to establish methodolgy for successful mass spectrometric analysis of challenging boronic acids.
Start Year 2008
 
Description Intercomparison Study of Mass Spectrometric Analysis of Boronic Acids 
Organisation Durham University
Country United Kingdom 
Sector Academic/University 
PI Contribution Implementation of an Intercomparison study involving ESI, MALDI, APPI and APCI on a variety of analysers to establish a more reliable method of analysis of boronic acids. The aim of collaboration was to establish methodolgy for successful mass spectrometric analysis of challenging boronic acids.
Start Year 2008
 
Description Intercomparison Study of Mass Spectrometric Analysis of Boronic Acids 
Organisation University of Bath
Country United Kingdom 
Sector Academic/University 
PI Contribution Implementation of an Intercomparison study involving ESI, MALDI, APPI and APCI on a variety of analysers to establish a more reliable method of analysis of boronic acids. The aim of collaboration was to establish methodolgy for successful mass spectrometric analysis of challenging boronic acids.
Start Year 2008
 
Description Investigation of agarose gel mediated silver nanoparticles by MALDI-TOFMS 
Organisation University of Liverpool
Country United Kingdom 
Sector Academic/University 
PI Contribution Investigation of agarose gel mediated silver nanoparticles by MALDI-TOFMS. Dr Brust?s group had been using agarose gel to control the size silver, gold and ruthenium nanoparticles, and had hoped to analyse them directly from embedded within the gel. Dr Brust?s group had been using agarose gel to control the size silver, gold and ruthenium nanoparticles, and had hoped to analyse them directly from within the gel by MALDI-TOF MS.
Start Year 2009
 
Description Investigation of phosphacenes encapsulating fullerenes or carboranes by MALDI-TOFMS. 
Organisation University of Regensburg
Department Institute of Inorganic Chemistry
Country Germany 
Sector Academic/University 
PI Contribution Prof. Scheer?s research involves macro coordination complex nanospheroids based upon pentaphosphaferrocene copper(I) chloride that can encapsulate small fullerenes or carboranes; major problems in characterising these materials led to initiation of a collaboration to investigate phosphacenes encapsulating fullerenes or carboranes by MALDI-TOFMS.
Start Year 2009
 
Description Investigation of polymer stabilizers for size-controlled synthesis of monodisperse gold nanoparticles by MALDI-TOFMS. 
Organisation University of Liverpool
Country United Kingdom 
Sector Academic/University 
PI Contribution Prof. Andrew Cooper initiated a collaboration in 2006, requiring NMSSC facilities and expertise to study polymer stabilizers used to control the size of gold nanoparticles during aqueous-based synthesis, and the resulting polymer-protected nanoparticles. The polymers themselves, being poly acids with a pendant carboxylic acid on each repeat unit prone to proton exchange with metal cations, provided an initial challenge. Several strategies were attempted until a sample preparation protocol was refined, and this work led to a paper with Dr Wyatt as lead-author in 2007. The methodology was extended to analyse the polymer-protected gold nanoparticles leading to a second paper, co-authored by Dr Wyatt in 2007.
Start Year 2006
 
Description Investigation of synthetic routes for various fluorinated analogues of the MALDI-TOFMS matrix 2-[(2E)-3-(4-tert-butylphenyl)-2-methylprop-2-enylidene]malononitrile (DCTB). 
Organisation University of Manchester
Department School of Chemistry Manchester
Country United Kingdom 
Sector Academic/University 
PI Contribution Dr Wyatt initiated a collbaoration to synthesise and study rationally-designed novel MALDI charge-transfer matrices, based upon the highly successful charge-transfer matrix, DCTB. By incorporating fluorine into a molecule, the ionisation energy of that molecule is increased and this should allow analysis of analytes with relatively high ionisation energies. Seven novel fluorinated analogues of DCTB (F-DCTBs) were designed by Dr Wyatt, who then initiated the use of the sister National Computational Chemistry Service Centre (NCCSS) at Imperial in 2008, with the help of Dr Sarah Wilsey and Dr Helen Tsui. Dr Wyatt required the NCCSS to run some ab initio density functional theory (DFT) calculations for the ionisation energies for the F-DCTBs, to see how they fitted with the charge-transfer ionisation mechanism theory, and to further identify which analogues were most suitable to attempt to synthesize. The resulting calculations achieved these targets, and the aim was to publish them along with the synthesis. Dr Wyatt initiated a collaboration with Dr Alan Brisdon of The Fluorine Group at University of Manchester to synthesize these compounds. Synthesis of rationally-designed novel MALDI charge-transfer matrices, based upon the highly successful charge-transfer matrix, DCTB. Icorporating fluorine into a molecule increases the ionisation energy of that molecule allowing analysis of analytes with relatively high ionisation energies.
Start Year 2008
 
Description Investigation of very high molecular weight iridium polydendrimers, and novel dendrimers and polymers by MALDI-TOFMS. 
Organisation University of Queensland
Country Australia 
Sector Academic/University 
PI Contribution A collaboration with Prof. Paul Burn, originally from the University of Oxford until moving his group to University of Queensland in 2007, and Dr Jeremy Robertson at University of Oxford that required NMSSC facilities and expertise in studying challenging polydendrimers, with each repeat unit containing an iridium coordination complex, and with an average molecular weight over 100kDa. This work led to a publication co-authored by Dr Wyatt in 2010, and the work was also presented at the 2010 BMSS meeting in Cardiff. Prof. Paul Burn from University of Oxford (OXFBUR) was a standard user for the analysis of small iridium complexes, until moving his group to University of Queensland in 2007. He continued to work with the NMSSC via a collaboration that also involved Dr Jeremy Robertson at University of Oxford (OXFROB,) requiring our facilities and expertise in studying challenging polydendrimers, with each repeat unit containing an iridium coordination complex, and with an average molecular weight over 100kDa.
Start Year 2007
 
Description NALDI analysis collaboration with NanoSys Inc. USA) 
Organisation Nanosys Inc
Country United States 
Sector Private 
PI Contribution Collaboration with NanoSys Inc. (USA) to examine the use of NALDI plate technology for the analysis of samples in the NMSSC. NALDI plates were supplied by Nanosys Inc for assessment as suitable targets for the various analytical challenges dealt with at the NMSSC. The collaboration led to publication.
Start Year 2008
 
Description Sterol Analysis by GC/MS 
Organisation Swansea University
Department Centre for P450 Biodiversity
Country United Kingdom 
Sector Academic/University 
PI Contribution Collaboration with Dr Steve Kelly (College of Medicine): GC/MS analysis of the sterol composition of agriculturally important fungal stains prior to and following their treatment with anti-fungal compounds.
Start Year 2007
 
Description Theoretical calculations for various fluorinated analogues of the MALDI-TOFMS matrix 2-[(2E)-3-(4-tert-butylphenyl)-2-methylprop-2-enylidene]malononitrile (DCTB). 
Organisation Imperial College London
Department National Computational Chemistry Service Centre
Country United Kingdom 
Sector Academic/University 
PI Contribution Dr Wyatt had the idea for rationally-designed novel MALDI charge-transfer matrices, based upon the highly successful charge-transfer matrix, DCTB. By incorporating fluorine into a molecule, the ionisation energy of that molecule is increased and this should allow analysis of analytes with relatively high ionisation energies. Seven novel fluorinated analogues of DCTB (F-DCTBs) were designed by Dr Wyatt, who then initiated the use of the sister National Computational Chemistry Service Centre (NCCSS) at Imperial in 2008, with the help of Dr Sarah Wilsey and Dr Helen Tsui. Dr Wyatt required the NCCSS to run some ab initio density functional theory (DFT) calculations for the ionisation energies for the F-DCTBs, to see how they fitted with the charge-transfer ionisation mechanism theory, and to further identify which analogues were most suitable to attempt to synthesize.
Start Year 2007
 
Description Theoretical calculations for various fluorinated analogues of the MALDI-TOFMS matrix 2-[(2E)-3-(4-tert-butylphenyl)-2-methylprop-2-enylidene]malononitrile (DCTB). 
Organisation Imperial College London
Country United Kingdom 
Sector Academic/University 
PI Contribution Dr Wyatt had the idea for rationally-designed novel MALDI charge-transfer matrices, based upon the highly successful charge-transfer matrix, DCTB. By incorporating fluorine into a molecule, the ionisation energy of that molecule is increased and this should allow analysis of analytes with relatively high ionisation energies. Seven novel fluorinated analogues of DCTB (F-DCTBs) were designed by Dr Wyatt, who then initiated the use of the sister National Computational Chemistry Service Centre (NCCSS) at Imperial in 2008, with the help of Dr Sarah Wilsey and Dr Helen Tsui. Dr Wyatt required the NCCSS to run some ab initio density functional theory (DFT) calculations for the ionisation energies for the F-DCTBs, to see how they fitted with the charge-transfer ionisation mechanism theory, and to further identify which analogues were most suitable to attempt to synthesize.
Start Year 2008
 
Description Trondheim University Collaboration/training 
Organisation Norwegian University of Science and Technology (NTNU)
Country Norway 
Sector Academic/University 
PI Contribution A Senior Engineer from the MS service in the Department of Chemistry, Norwegian University of Science and Technology, Trondheim, Ms Susana Gonzales, was trained in specialist MS techniques for 10 working days following the 2009 summer school. Susana was provided with training and advice on the optimal MS analysis of a wide range of molecules on the Centre's MAT 95.
Start Year 2009
 
Description Washington-Baltimore Discussion Group 
Organisation Washington-Baltimore Mass Spectrometry Discussion Group
Country United States 
Sector Academic/University 
PI Contribution Delivery of course on "Interpretation of Mass Spectra" at ASMS conferences. Mrs Stein joined the Washington-Baltimore Discussion Group to deliver a course on "Interpretation of Mass Spectra" at the annual American Society of Mass Spectrometry meeting.
Start Year 2007
 
Company Name AberMs Ltd 
Description Manufacturer of ion sources and ion optics consultancy company. It has expertise in programming and interfacing equipment and has previously developed software 21 CFR Part 11 Compliance. 
Year Established 2015 
Impact Developer of novel ion source and mass analysers.
 
Description "Collaborative" mass spectrometry course (Edinburgh) 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Undergraduate students
Results and Impact The collaborative course presented at Edinburgh was a useful publicity exercise as well an a primary educational aim.
Year(s) Of Engagement Activity 2008
 
Description "Outreach" visit to Hull and Loughborough advertising services offered by NMSSC 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Undergraduate students
Results and Impact Questions and informal discussions were given with small group of 1-10.
Year(s) Of Engagement Activity 2008
 
Description 6 hour lectures designed for "Outreach" training programme 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Undergraduate students
Results and Impact A new course of 6 hours of lectures designed for the "Outreach" training programme to be taken into university departments.
Year(s) Of Engagement Activity 2008
 
Description AAMG/RSC meeting at Burlington House (London) 
Form Of Engagement Activity A formal working group, expert panel or dialogue
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Other audiences
Results and Impact Attended RSC meeting.
Year(s) Of Engagement Activity 2009
 
Description ASMS Conference (Philadelphia) 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Other audiences
Results and Impact Presenting the Interpretation of Mass Spectra course.
Year(s) Of Engagement Activity 2009
 
Description ASMS conference in Indianapolis 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Industry/Business
Results and Impact A course on "Interpretation of Mass Spectra" was given. Collaboration with the Washington-Baltimore Discussion Group (USA).
Year(s) Of Engagement Activity 2007
 
Description Advances in LC/MS and Related Hypenated Techniques Conference (Sunderland) 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Industry/Business
Results and Impact A poster was displayed and staff on hand to answer questions.
Year(s) Of Engagement Activity 2009
 
Description Advertising NMSSC by email 
Form Of Engagement Activity A magazine, newsletter or online publication
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Other audiences
Results and Impact NMSSC advertised it services by email to all chemistry and releated departments.
Year(s) Of Engagement Activity 2007,2008,2009
 
Description American Society of Mass Spectrometry Conference (Denver) 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Industry/Business
Results and Impact Advertising NMSSC to the wider international community. Posters were also presented.
Year(s) Of Engagement Activity 2008
 
Description American Society of Mass Spectrometry Conference in Indianapolis 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Industry/Business
Results and Impact The American Society of Mass Spectrometry Conference in Indianapolis. Contacts were made and the NMSSC advertised to the wider international community.
Year(s) Of Engagement Activity 2007
 
Description Annual Summer School 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Undergraduate students
Results and Impact An annual Summer School with two full days of lectures and tutorials and half a day on specialist topics agreed with delegates.
Year(s) Of Engagement Activity 2007,2008,2009,2010,2011
 
Description BMSS Conference at Heriot-Watt University 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Industry/Business
Results and Impact BMSS conference at Heriot-Watt University where posters were presented.
Year(s) Of Engagement Activity 2007
 
Description BioWales Conference (Cardiff) 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Industry/Business
Results and Impact Attendance was to advertise NMSSC to another community.
Year(s) Of Engagement Activity 2009
 
Description Dalton Discussion 10 Conference (DD10) in Durham 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Undergraduate students
Results and Impact A stall was set up wih promotional material of the NMSSC.
Year(s) Of Engagement Activity 2008
 
Description Distribution of NMSSC brochure 
Form Of Engagement Activity A magazine, newsletter or online publication
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Media (as a channel to the public)
Results and Impact The NMSSC brochure has been distributed to interested parties throughout the year to raise awareness and knowledge of the National Service.
Year(s) Of Engagement Activity 2007,2008
 
Description Education material on NMSSC website (Swansea) 
Form Of Engagement Activity Engagement focused website, blog or social media channel
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Undergraduate students
Results and Impact Educational material on NMSSC's new website.
Year(s) Of Engagement Activity 2009
 
Description IMSC in Bremen (Germany) 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Other audiences
Results and Impact Posters were presented.
Year(s) Of Engagement Activity 2009
 
Description Lecture at Queen's University Belfast 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Undergraduate students
Results and Impact A lecture presented to the chemistry department at Queen's University Belfast.
Year(s) Of Engagement Activity 2009
 
Description NMSSC "Corporate posters" displayed in Swansea University 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Postgraduate students
Results and Impact NMSSC corporate posters displayed in public areas of Swansea University which had been previously presented at conferences and meetings.
Year(s) Of Engagement Activity 2007
 
Description New course of lectures (two mornings, 7 hours) (Edinburgh) 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Undergraduate students
Results and Impact New course of lectures (two mornings, 7 hours) implemeted in a collaborative effort with the chemistry dept at Edinburgh University.
Year(s) Of Engagement Activity 2008
 
Description Presentation of PhD student (Swansea University) 
Form Of Engagement Activity A talk or presentation
Part Of Official Scheme? No
Geographic Reach Local
Primary Audience Postgraduate students
Results and Impact Presentation presented by PhD student from Oxford at Postgraduate fair in the School of Medicine.
Year(s) Of Engagement Activity 2009
 
Description RSC Advances in GC Technology meeting in Runcorn 
Form Of Engagement Activity A formal working group, expert panel or dialogue
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Other audiences
Results and Impact Attended meeting re advances in GC Technology.
Year(s) Of Engagement Activity 2009
 
Description RSC Co-ordination Chemistry Conference (Leeds) 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Other audiences
Results and Impact Conference was attended to publicise NMSSC and its activities to new users.
Year(s) Of Engagement Activity 2009
 
Description RSC/BMSS combined meeting, "Structure2010" (Leicestershire) 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Other audiences
Results and Impact A stand was hosted with NMSSC publicity material.
Year(s) Of Engagement Activity 2010
 
Description Research Networking Event in the School of Environment and Society (Swansea university) 
Form Of Engagement Activity A formal working group, expert panel or dialogue
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Undergraduate students
Results and Impact Staff were networking with other deparments. Publicity material was displayed.
Year(s) Of Engagement Activity 2007
 
Description School visits from Swansea and Cardiff schools 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach Regional
Primary Audience Schools
Results and Impact Students from different schools attended for demonstrations on the activities of NMSSC.
Year(s) Of Engagement Activity 2009
 
Description Technician's training at Queen's University Belfast 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Other audiences
Results and Impact A week's MS training given to technicians of the chemistry department at Queen's University Belfast which was highly successful.
Year(s) Of Engagement Activity 2009
 
Description Training given to visiting academic from University of Witwatersrand (Johannesburg) 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Other audiences
Results and Impact Fundamental training given as part of a collabrative exercise.
Year(s) Of Engagement Activity 2007
 
Description Visit to Mass Spectrometry Service in Edinburgh university 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Undergraduate students
Results and Impact Following this visit a training course for the chemistry department was arranged.
Year(s) Of Engagement Activity 2008
 
Description Visit to Mass Spectrometry facilities in York and Manchester 
Form Of Engagement Activity A formal working group, expert panel or dialogue
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Other audiences
Results and Impact Discussion of mutual interest with staff members.
Year(s) Of Engagement Activity 2008
 
Description Work experience for local student (Swansea) 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach Local
Primary Audience Schools
Results and Impact One week work experience with one local student.
Year(s) Of Engagement Activity 2009
 
Description Work experience students from local schools (Swansea) 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach Local
Primary Audience Schools
Results and Impact Two students attended a two week work experience.
Year(s) Of Engagement Activity 2009