NMR Spectroscopy Services

Standard 1D, 2D and 3D experiments are available for the elucidation of protein, peptide and natural product structures. In addition, new techniques can be developed of for custom applications. Availability of the cryogenically cooled probes increases the sensitivity of the 700 MHz instrument and the 1.7 mm probe allows for the analysis of mass limited samples. Variable temperature experiments are available from 4 °C to 60 °C.

NMR spectroscopy is capable of accurately and precisely determining the concentration of small molecules within a purified sample or complex mixture. Protocols have been developed that use a single certified external or internal standard to calibrate to quantitate marine biotoxins and natural product extracts.

The NMR facility has the capability to analyze lipid extracts such as fatty acids and their derivatives, using multinuclear NMR techniques. Proton (¹H) 1D NMR can be used to profile saturated versus unsaturated fatty acid in mixtures. Carbon (¹³C) 1D NMR can be used to profile the regiospecific distribution of fatty acid chains in triacyl glycerols (TAG's). Phosphorous (³¹P) based NMR techniques (both 1D and 2D) can be used to characterize the headgroups of mixtures of glycerophospholipids.

High-resolution magic angle spinning (HR-MAS) technique is advantageous for studying semi-solids such as intact tissues, cells, raw materials or product formulations in their native environments by NMR spectroscopy. Valuable information can be obtained without time consuming and disrupting/degrading extractions or chemical modifications. Samples are spun at 3 to 5 kHz at the "magic angle" (54.7°) to the applied magnetic field reducing line broadening effects. Many of the nD experiments that are utilized for structural elucidation can be applied. Applications include:

• Lipid profiling of whole cells e.g. algae, yeast
• Extraction efficiencies from biomass
• Metabolite profiling of tissue e.g liver

NMR spectroscopy is suitable for metabolite analysis since it allows simultaneous detection of a diverse group of both primary metabolites (sugars, organic acids, amino acids etc.) and secondary ones (flavonoids, alkaloids tri-terpenes etc.). Availability of high throughput temperature controlled sample changer and automated data acquisition allows for acquisition of approximately 480 samples per weekend. Statistical analysis though principal component analysis (PCA) allows patterns associated with the variability in the levels of individual metabolites within several samples to be assessed. A Gilson Liquid Handler is available for high-throughput sample preparation. Applications include:

• serum and urine
• Cell and plant extracts

• Bruker Avance-III 700 MHz spectrometer
• Cooled (4 °C) sample changer that accommodates up to 5 × 96 tubes and 30 individual 5 mm tubes.
• Equipped with two helium-cooled probes (1.7 mm & 5.0 mm)
• 5 mm TCI CryoProbe with auto-tune and match and Z gradient, 1H signal to noise ratio 8000:1 13C signal to noise ratio 1200:1
• 1.7mm TCI CryoProbe with auto-tune and match and Z gradient, 1H signal to noise ratio 1300:1. 13C signal to noise ratio 150:1
• 5mm BBO probe with auto-tune and match and Z-gradient.
• TopSpin 2.1 for NMR data acquisition and processing

• Bruker Avance III 500 MHz spectrometer
• Medium through-put sample changer for acquisition of 60 samples
• 4 mm HR-MAS probe with Z gradient for semi solid samples
• 5 mm TXI probe with auto-tune and match and Z-gradient
• 5 mm BBFO probe (19F observe) with auto-tune and match and Z-gradient
• 1 mm inverse microprobe with auto-tune and match and Z gradient
• TopSpin 2.1 for NMR data acquisition and processing