MSU NMR Facility 

The MSU Nuclear Magnetic Resonance (NMR) Facility is a user-supported facility operating under the Office of the Vice President of Research and Economic Development. The NMR facility is located on the first floor of the Chemistry and Biochemistry building in room 18on the MSU campus in Bozeman, MT. The facility provides both on-campus and off-campus industry/start-up researchers in the biological, chemical and physical sciences 24/7 open-access availability to state-of-the-art solution NMR spectroscopy instrumentation, training and sample preparation resources.The facility can be accessed individually or as a full service center. The NMR Facility has a total space of ~2,500 sq ft. divided among 3 rooms fully constructed with considerations for cooling, in-place floor dampening infrastructure and space for wet lab/sample preparation. The facility specializes in small molecule structure determination, small molecule characterization, biomolecular/protein structure determination, qualitative and quantitative NMR analysis, and small molecule purification from a wide variety of sample sources.

Facility Instrumentation

The NMR spectroscopy facility operates four solution NMR spectrometers and wet lab instrumentation, each with advantages for specific types of analyses and preparative work. The following list highlights the present installed instrumentation and example applications.

Bruker 300 MHz UltraShield DPX AVANCE I NMR Spectrometer (actively shielded) equipped with a 300 MHz QNP Probe (room temperature). Available working temperature range: -80oC to +130oC with two channel acquisition for 1H/19F/13C/31P and lock. The instrument is ideal for basic 1H, 19F, 13C and 31P direct detection, training and temperature studies.

Bruker 400 MHz Ascend AVANCE NEO NMR Spectrometer (actively shielded) with a 400 MHz PI HR-BBO400S1-BBF/H/D-5.0-Z SP N (room temperature SmartProbe) or PI HR-TBO400S1-BBF/H/P/D-5.0-Z FB N DP SmartProbe. Available working temperature range: -150oC to +150oC with two channel acquisition for 1H/BB19F and lock. Auto-tune/Auto-shim capabilities. SampleCaseTM automated sample loading system (24-position). The instrument is used for high-through-put 1H and 19F dual nuclei experiments, X nuclei direct detection, temperature and kinetic studies.

Bruker 500 MHz Ascend Avance III HD Spectrometer (actively shielded) with 500 MHz Prodigy (liquid nitrogen cooled) CPP BBO (BB-H+F-05Z) ProdigyTM Cryoprobe. Available working temperature range: -40oC+80oC. Two channel 1H/19F, XBB and lock. Auto-tune/Auto-shim capabilities. SampleJetTM automated sample loading system. Best system for X nucleus direct detection and high-resolution/low abundance structure elucidation experiments.

Bruker 600 MHz Avance III NMR Spectrometer (actively shielded) with 600 MHz TCI (H-C/N-D05Z) LT (liquid helium cooled) Helium CryoProbeTM. Available working temperature range: -40oC+80oC. Three channels: 1H, X1=13C, X2=15N, lock. Auto-tune/Auto-shim. SampleJetTM automated sample loading system. Best system for direct detection of 1H and indirect detection of 13C and 15N. Routinely used for high-throughput metabolomics sample analysis and protein structure determination.

LC-SPE-NMR-MS (a hyphenated LC-NMR spectroscopy system with enhanced sample recovery combined with real-time MS analysis and high-through-put capabilities). The system consists of an Agilent 1260 HPLC with DAD detection coupled to a Bruker NMR-MS-Bridge (splitter), a Bruker micrOTOF mass spectrometer (shared resource), a Bruker ProspekII SPE (solid phase extraction) unit and a Gilson 215 liquid handler. The system allows for NMR analysis of known and unknowns following reversed-phased or HILIC chromatography. Analytes can be trapped as fractions or on solid-phase-support (SPE) cartridges for drying, elution with deuterated NMR solvents and NMR analysis with real-time collected MS analysis.

Bruker InsightMR software and 5 mm flow probe/pump unit (4m) with chiller/heater bath for on-line kinetic/reaction monitoring by NMR analysis. Working temperature range -20oC to +200oC. Working flow rate ranges 0.001-10ml/min. The Bruker InsightMR package allows for real-time reaction monitoring by NMR analysis.

Bruker micrOTOF - Agilent 1260 HPLC. The Bruker micrOTOF ESI instrument with a time-of-flight (TOF) detector (shared instrument resource) can be interfaced directly t the Agilent 1260 HPLC system which can deliver solvent flow rates between 50 microliters and 5000 microliters per minute, appropriate for standard analytical HPLC analyses as well as rapid high-performance HPLC protocols. The micrOTOF-HPLC configured system is regularly used for evaluating recombinant protein masses (SEC), providing accurate mass for organic synthesis products undergoing NMR analysis, and identification/validation of known metabolites.

Agilent 1100 HPLC (with analytical pumps), DAD detector and columns (reversed phased and HILIC chromatography) for preparative and analytical services.

JASCO FT/IR-4100 Fourier Transform Infrared Resonance spectrometer with analysis software. For chemical functional group detection and characterization.  

LABCONCO 12plus freeze-zone freeze dryer. Used for drying/recovery of samples following purification by HPLC and preparative methods.

Software

The NMR Facility houses on-site computers with access to the following software: Bruker Topspin (spectra processing and analysis). Bruker Dynamics Center (spectra processing and kinetic analysis). Bruker CMCse (Small Molecule Structure Elucidation analysis). ACD Labs (spectral processing and analysis). ChenomxTM - Metabolite profiling and quantification. MVAPCK (statistical analysis of spectra).

Sample preparation

The NMR facility includes standard wet lab accessories, microfuges, scale, FPLC and off-line fraction collectors to support a wide variety of NMR sample purification/fractionation and recovery protocols.