Mass Spectrometry and Separations

Academics using the mass spec equipment

Mass Spectrometry

LCMS and GCMS capabilities are described below with the relevant chromatography technique.

Shimadzu Axima iDplus Performance MALDI-TOF

Location: Chemistry A70 Mass Spectrometry

Shimadzu Axima iDplus Performance MALDI-TOF mass spectrometer performs laser ionisation of matrix co-crystallised solid samples which are analysed by time-of-flight mass spectrometry with MS/MS capabilities.

MALDI-TOF mass spec. is used for “soft” ionisation of fragile compounds such as complex biological samples and/or synthetic polymers. Extremely versatile MALDI-TOF analysis can be performed in either reflectron or linear detector modes which provide information-rich MS spectra for a broad mass range 100–12,000 Da or 12,000–100,000 Da respectively; while MS/MS capabilities further facilitate compound characterisation. Software tools specifically designed for biomolecule or polymer analysis enable an in-depth understanding of samples.

MALDI-TOF requires bespoke sample preparation procedures to maximise instrument performance. The co-crystallisation of samples with matched matrix material is required to optimise MS data and analytical sensitivity; however, generic analytical work-flows yield information-rich data for sample concentrations as low as picomolar concentration.

Liquid Chromatography

Thermo Scientific Dionex ICS-5000+ HPIC

Location: Chemistry A70 Mass Spectrometry

Thermo Scientific Dionex ICS-5000+ Reagent Free Ion Chromatography dual microbore analysis for anions (organic, inorganic, transition metal oxides) and cations.

The ICS-5000+, with all-PEEK flow path capable of operating at high pressures (2000-3000 psi), for the analysis of anions and cations in sample mixtures. Reagent-free eluent generation, ion suppression and conductivity detection offer high-sensitivity analysis for a range of ions. Dual IC channels, complete with separate pumps, eluent generation, stationary phase and detection enable simultaneous cation and anion detection of the same sample.

The modular system with all-PEEK flow path contains a dual system to run two different analyses concurrently on a single sample. The system is configured for analysis with dual pump, Reagent-free eluent generation, microbore (3–7 mm id) separation, eluent ion suppression and conductivity detection. Aqueous components detected routinely in the parts per million range. Organic mobile phase analysis is also possible with instrument re-configuration.

Gas Chromatography

Shimadzu GCMS-TQ8040

Location: cTAP B06 Instrument Room

GCMS is a powerful tool for a range of analytical requirements particularly the separation and identification of volatile and semi-volatile compounds. With a triple quadrupole GCMS detector, trace-level analysis in complex matrices is possible with liquid or headspace injections. Operation in multiple reaction monitoring (MRM) mode provides exceptional sensitivity, selectivity, and specificity for detection and quantitation of targeted compounds.

Automated sample preparation for liquid, headspace and SPME applications can be performed with the PAL3 autosampler.

Agilent GC-7890B GC-FID

Location: cTAP B06 Instrument Room, and Faraday B32 Teaching Lab

Conventional GC-FID system for reliable robust analysis of GC samples; currently configured with He carrier gas and standard stationary phase chemistries. Full sample automation is achieved through the PAL Systems CTC for 24/7 sample analysis in liquid or headspace injection modes.

GC-FID with PAL RTC sample automation. Current configuration utilises He carrier gas and methylpolysiloxane column chemistry. Other carrier gases and column chemistry are available with correct specification of consumable items. Samples are provided as 1–10 mg of material dissolved in a suitable volatile solvent.

Contact

David Rochester

Dr David Rochester

Deputy Superintendent, Experimental Officer in Separations/Mass Spectrometry