Nuclear Magnetic Resonance (NMR) spectroscopy is an indispensable technique used in structure determination of small and macromolecules to study their physical properties, elucidation of characteristic interactions, dynamics and thermodynamic processes. Quantum mechanics defines the theoretical description of NMR spectroscopy and treatment of the dynamics of nuclear spin systems. The phenomenon of residual dipolar coupling (RDCs) has become a routine tool for accurate structure determination by providing global orientation information of magnetic dipole-dipole interaction vectors within a common reference frame. This offers accessibility of distance-independent angular information and insights to local relaxation. The measurement of RDCs requires an anisotropic orientation medium for the molecules to partially align along the magnetic field. This can be achieved by introduction of liquid crystals or attaching a paramagnetic center. Although anisotropic paramagnetic tags continue to mark achievements in the biomolecular NMR of large proteins, its application in small organic molecules remains unspread. Here, we propose a strategy for the synthesis of a lanthanide tag and the measurement of RDCs in organic molecules using paramagnetic lanthanide complexes.
High Resolution NMR Spectroscopy offers unique screening capabilities for food quality and safety by combining non-targeted and targeted screening in one analysis.
The objective is to demonstrate, that due to its extreme reproducibility NMR can detect smallest changes in concentrations of many components in a mixture, which is best monitored by statistical evaluation however also delivers reliable quantification results.
The methodology typically uses a 400 MHz high resolution instrument under full automation after minimized sample preparation.
For example one fruit juice analysis in a push button operation takes at maximum 15 minutes and delivers a multitude of results, which are automatically summarized in a PDF report.
The method has been proven on fruit juices, where so far unknown frauds could be detected. In addition conventional targeted parameters are obtained in the same analysis. This technology has the advantage that NMR is completely quantitative and concentration calibration only has to be done once for all compounds. Since NMR is so reproducible, it is also transferable between different instruments (with same field strength) and laboratories. Based on strict SOP`s, statistical models developed once can be used on multiple instruments and strategies for compound identification and quantification are applicable as well across labs.
Pure phase gallosilicate nitrite sodalite has been synthesized in a single step by low temperature (373 oK) hydrothermal technique. The product obtained was characterized using a combination of techniques including X-ray powder diffraction, IR, Raman spectroscopy, SEM, MAS NMR spectroscopy as well as thermogravimetry. Sodalite with an ideal composition was obtained after synthesis at 3730K and seven days duration using alkaline medium. The structural features of the Na8[GaSiO4]6(NO2)2 sodalite were investigated by IR, MAS NMR spectroscopy of 29Si and 23Na nuclei and by Reitveld refinement of X-ray powder diffraction data. The crystal structure of this sodalite has been refined in the space group P 4 3n; with a cell parameter 8.98386Å, V= 726.9 Å, (Rwp= 0.077 and Rp=0.0537) and Si-O-Ga angle is found to be 132.920 . MAS NMR study confirms complete ordering of Si and Ga in the gallosilicate framework. The surface area of single entity with stoichiometry Na8[GaSiO4]6(NO2)2 was found to be 8.083 x10-15 cm2/g.