scholarly journals Recent Development in Nuclear Magnetic Resonance as a Technique for Quantitative Method Validation

2021 ◽  
Vol 83 (6) ◽  
Author(s):  
R. Sahu ◽  
A. Kumar ◽  
Rakhi Mishra ◽  
Chandana Majee ◽  
R. Kumar
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Method Validation ◽  
Quantitative Method ◽  
Nuclear Magnetic

OBETICHOLIC ACID: AN INSIGHT INTO A QUANTITATIVE DETERMINATION AND METHODOLOGICAL VALIDATION THROUGH NUCLEAR MAGNETIC RESONANCE

2020 ◽  
pp. 179-190
Author(s):  
RAKESH SAHU ◽  
RAKHI MISHRA ◽  
CHANDANA MAJEE ◽  
AJAY KUMAR ◽  
RUPA MAZUMDER
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Quantitative Determination ◽  
Method Validation ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Proton Nuclear Magnetic Resonance ◽  
Obeticholic Acid ◽  
Relative Standard ◽  
Nuclear Magnetic

Objective: The research work unveils the use of nuclear magnetic resonance (NMR) technique for quantitative determination and method validation of obeticholic acid. As standard expository methodology for more up to date medications or formulations may not be available in pharmacopeias, hence it is fundamental need to create novel analytical procedures which should be precise and accurate. Methods: Proton (1H) and carbon (13C) NMR analysis were initially performed to confirm the preliminary authenticity of obeticholic acid API. Method validation was accomplished on the basis of standard guidelines for the parameters, in which tetramethylbenzene as an internal standard and deuterated dimethyl sulfoxide as a diluent were used to assess the obeticholic acid. Results: For the quantification of the drug, the proton nuclear magnetic resonance signals at 0.602 ppm and 6.86 ppm corresponding to the analyte proton of drug and internal standard respectively were used. The curve equation calculated from the regression method, the relative-standard-deviation and correlation-coefficient were found to be 0.743% and 0.9989 respectively, indicating good linearity. Consequently, the quantitative assay of the drug was found to be 99.91% in linearity with limit of detection and quantification values as 0.0773 mg and 0.2344 mg respectively, making successful the study of method validation for obeticholic acid. Conclusion: The advantage of the method was that no reference standard of analyte drug was required for quantification and method validation. The method is non-destructive and can be applied for quantification of drug in commercial pharmaceutical formulation products.

An emerging technology: Nuclear magnetic resonance microscopy

1988 ◽  
Vol 46 ◽  
pp. 1000-1001
Author(s):  
M.J. Hennessy ◽  
E. Kwok
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Relaxation Times ◽  
Basic Research ◽  
Local Environment ◽  
Magnetic Resonance Images ◽  
Nmr Microscopy ◽  
Mri Scans ◽  
Temperature Relaxation ◽  
Nuclear Magnetic

Much progress in nuclear magnetic resonance microscope has been made in the last few years as a result of improved instrumentation and techniques being made available through basic research in magnetic resonance imaging (MRI) technologies for medicine. Nuclear magnetic resonance (NMR) was first observed in the hydrogen nucleus in water by Bloch, Purcell and Pound over 40 years ago. Today, in medicine, virtually all commercial MRI scans are made of water bound in tissue. This is also true for NMR microscopy, which has focussed mainly on biological applications. The reason water is the favored molecule for NMR is because water is,the most abundant molecule in biology. It is also the most NMR sensitive having the largest nuclear magnetic moment and having reasonable room temperature relaxation times (from 10 ms to 3 sec). The contrast seen in magnetic resonance images is due mostly to distribution of water relaxation times in sample which are extremely sensitive to the local environment.

Nuclear magnetic resonance microscopy

1989 ◽  
Vol 47 ◽  
pp. 828-829
Author(s):  
Paul C. Lauterbur
Keyword(s):  
Magnetic Field ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Magnetic Fields ◽  
Signal To Noise ◽  
Field Gradients ◽  
Useful Signal ◽  
Magnetic Field Gradients ◽  
Observation Times ◽  
Nuclear Magnetic

Nuclear magnetic resonance imaging can reach microscopic resolution, as was noted many years ago, but the first serious attempt to explore the limits of the possibilities was made by Hedges. Resolution is ultimately limited under most circumstances by the signal-to-noise ratio, which is greater for small radio receiver coils, high magnetic fields and long observation times. The strongest signals in biological applications are obtained from water protons; for the usual magnetic fields used in NMR experiments (2-14 tesla), receiver coils of one to several millimeters in diameter, and observation times of a number of minutes, the volume resolution will be limited to a few hundred or thousand cubic micrometers. The proportions of voxels may be freely chosen within wide limits by varying the details of the imaging procedure. For isotropic resolution, therefore, objects of the order of (10μm) may be distinguished.Because the spatial coordinates are encoded by magnetic field gradients, the NMR resonance frequency differences, which determine the potential spatial resolution, may be made very large. As noted above, however, the corresponding volumes may become too small to give useful signal-to-noise ratios. In the presence of magnetic field gradients there will also be a loss of signal strength and resolution because molecular diffusion causes the coherence of the NMR signal to decay more rapidly than it otherwise would. This phenomenon is especially important in microscopic imaging.

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