Mass spectrometry and separations

The Department has a wide variety of mass spectrometry and separations equipment.

Mass Spectrometry

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

Mass Spectrometry Service for Small Molecule Mass Assignment

Mass assignments of small molecule samples are typically performed using the Shimadzu LCMS-IT-TOF in ESI or APCI, but without the initial chromatography step; contact Dr David Rochester for details on sample submission.

Axima Performance MALDI-TOF

Shimadzu Axima iDplus Performance MALDI-TOF is located in Faraday A70 Mass Spectrometry and bookable here.

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 provides information rich MS spectra for a broad mass range 100–12,000 Da or 12,000–100,000 Da respectively; whilst MS/MS capabilities further facilitate compound characterisation. Software tools specifically designed for biomolecule or polymer analysis enable 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.

The MALDI-TOF analytical work-flow can be integrated with robotic sample preparation enabling LC-MALDI-TOF analytical procedures in combination with the Shimadzu GPC and NexeraX2 separation systems. Also available is a SunCollect MALDI spray chamber for tissue imaging.

 

Liquid Chromatography

Shimadzu LCMS-IT-TOF

The Shimadzu LCMS-IT-TOF mass spectrometer is fronted by a Shimadzu NexeraX2 UHPLC system; the instrument is designed for high resolution accurate mass MSn experiments. Currently located in Faraday A71 Mass Spectrometry, the booking timetable is here.

Coupled to HPLC/UHPLC separation the LCMS-IT-TOF combines a QIT (ion trap) and TOF (time-of-flight) mass spectrometer system. The unique combination of ion-trap and time-of-flight technologies allows mass spec fragmentation experiments, MSn, up to MS10 with high accuracy mass assignment of precursor and product ions.

Shimadzu LC-TQ8040

The Shimadzu LCMS-8040 triple quadrupole mass spectrometer fronted by a Shimadzu NexeraX2 UHPLC system; for SRM/MRM quantitative LCMS analysis. This instrument is installed in cTAP B06 Instrument Room, and is bookable here.

The LCMS-8040 enables high sensitivity mass analysis of HPLC/UHPLC separations. A combined MS probe enables simultaneous ESI and APCI for highly sensitive and specific quantitative analysis of samples. Triple quad mass analysis is common in applications such as omics studies, environmental and biological analysis requiring very low levels of detection and quantitation.

Shimadzu NexeraX2 UHPLC-PDA

Ultra-high performance liquid chromatography with PDA detection, and optional AccuSpot MALDI spotting robot. One is located in Faraday A70 Mass Spectrometry (bookable here), and the other in cTAP B06 Instrument Room (timetable here).

For the separation, identification and quantitation of components dissolved in liquid samples, the Shimadzu NexeraX2 system is capable of ultra-high pressure chromatography of a range of sample types. High sensitivity, multi-wavelength analysis is achieved with the PDA detector. Analysis is routinely conducted using reverse-phase conditions and consumables, however, with appropriate selection of mobile and stationary phases alternative LC experiments can be conducted.

Shimadzu GPC/SEC

Gel permeation / size exclusion chromatography specific equipment with detection via RID, Wyatt Technologies MALS and viscometry detectors. Also available is an AccuSpot MALDI spotting robot. Currently located in Faraday A70 Mass Spectrometry and bookable here.

Gel permeation chromatography (GPC), or size exclusion chromatography (SEC), equipment for the measurement of molecular weight values of synthetic polymers and biomolecules (such as proteins, etc.). The combination of size fractionation with refractive index (RID), light scattering (MALS) and viscometry detection allows the on-line measurement of molecular weight, molecular weight distribution and molecular interactions without the need for extensive instrument/column calibration.

Basic analysis routinely conducted by this instrument for polymer analysis uses THF solvent, a broad molecular weight column, and the three detector system for the analysis of molecular weight and molecular weight distribution. Typical sample submission requires 1–10 mg of sample dissolved in 1 ml mobile phase.

Agilent 6120B LCMS

The Agilent 1260 Infinity HPLC with 6120B Single Quad MS offers robust, versatile, sensitive and selective analysis of a broad range of compounds for routine characterization of complex mixtures. A quaternary gradient HPLC coupled with a choice of chromatographic stationary phases (C8, C18, phenyl-hexyl, SB-aq) and the specificity of MS detection enables LCMS to cover a broad range of analytical requirements for liquid soluble, polar or non-polar compounds.

Agilent 1220 Infinity HPLC

The Agilent 1220 Infinity HPLC instrument comprises a binary gradient solvent pump and single-wavelength UV-vis detection. Robust, reproducible HPLC analysis is provided with a single unit capable of full automation. This instrument is currently located in the non-synthetic teaching lab (Faraday B32 Teaching Laboratory).

HPLC analysis is conducted using a range of available column chemistries including C8, C18, phenyl-hexyl, SB-aq phases. Samples submitted in a range of concentrations from <1 mg/ml dissolved in analytical solvent. Instrument detection limited to UV-vis spectroscopy, but this is likely to cover most analytical requirements.

Thermo Scientific Dionex ICS-5000+ HPIC

Thermo Scientific Dionex ICS-5000+ Reagent Free Ion Chromatography dual microbore analysis for anions (organic, inorganic, transition metal oxides) and cations. Currently located in cTAP B01 Laboratory, and bookable here.

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 offers high sensitivity analysis for a range of ions. Dual IC channels, complete with separate pumps, eluent generation, stationary phase and detection enables simultaneous cation and anion detection of the same sample.

The modular system with all-PEEK flow path contains 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 i.d.) 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

Located in cTAP B06 Instrument Room and bookable here.

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

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. One is located in cTAP B06 Instrument Room and bookable here, while the other is in Faraday B32 Teaching Lab, but is not yet on the booking system.

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 suitable volatile solvent.

Agilent GC-MSD

An Agilent GC-7820A with an MSD 5975C for reliable, robust, easy-to-use GCMS analysis. Single quadrupole mass analysis offers reliable rapid data collection in either full scan or selected ion monitoring mode. This is currently located in Faraday B32 Teaching Lab, but is not yet on the booking system.