Solid-state NMR spectroscopy in pharmaceutical research and analysis

Berendt, Robert T.; Sperger, Diana M.; Munson, Eric J.; Isbester, Paul

doi:10.1016/j.trac.2006.07.006

Cited by 138 publications

(138 citation statements)

References 32 publications

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“…This NMR-based technique is non-destructive and can be beneficial to molecules in solution and solid state (Berendt et al, 2006). However, the most frequently used is hydrogen-1 NMR, because it is extremely rich and the most amenable isotope at natural abundance.…”

Section: Recent Techniques Used In Plant Metabolomics Profilingmentioning

confidence: 99%

Advances in detection of stress tolerance in plants through metabolomics approaches

Khan¹,

Ali²,

Shahid³

et al. 2017

Plant Omics

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Heat and drought stresses are presently the principal risk on world's food quantity, limiting yield. Both of these two stresses affect plants metabolism, physiological and morphological processes, which ultimately reduces the productivity. The plant cell develops different stress induced self-defence mechanisms to reduce the effect of stresses. These defence mechanisms are developed by modifying gene expression pattern, which results in qualitative and quantitative deviations in proteins synthesis, leading to the modulation of certain metabolic and defensive pathways. New metabolic profiling technologies offer a great opportunity for biologist to understand defence mechanism of plants under stress conditions. Metabolomics technologies presently enabled the using of different multi-variate analyses, generated from various hyphenated and chromatographic discovery systems, such as gas or liquid chromatography together with mass spectrometry, or nuclear magnetic resonance (NMR) based methods. Investigation and mining of metabolomics data can be done through a blend of different statistical methods, such as independent component analysis and analysis of variance. Metabolomics in combination with gene expression, protein interaction and other different regulatory pathways can be useful to diverse organisms with trivial alterations. In recent time, this technology has been used to investigate drought tolerance in plant crops to find particular stress related patterns in metabolic expression. These studies identified the vital roles of primary and secondary metabolites associated with abiotic stress tolerance.

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Section: Recent Techniques Used In Plant Metabolomics Profilingmentioning

confidence: 99%

Advances in detection of stress tolerance in plants through metabolomics approaches

Khan¹,

Ali²,

Shahid³

et al. 2017

Plant Omics

View full text Add to dashboard Cite

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“…Similar to the XRPD, the 13 C ssNMR has advantage of being nondestructive. However, it takes longer time to collect data; instrument is expensive and requires expertise to collect and analyze the data (7).…”

Section: Introductionmentioning

confidence: 99%

Comparison of Univariate and Multivariate Models of 13C SSNMR and XRPD Techniques for Quantification of Nimodipine Polymorphs

et al. 2015

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Abstract. The focus of the present investigation was to explore the use of solid-state nuclear magnetic resonance ( 13 C ssNMR) and X-ray powder diffraction (XRPD) for quantification of nimodipine polymorphs (form I and form II) crystallized in a cosolvent formulation. The cosolvent formulation composed of polyethylene glycol 400, glycerin, water, and 2.5% drug, and was stored at 5°C for the drug crystallization. The 13 C ssNMR and XRPD data of the sample matrices containing varying percentages of nimodipine form I and form II were collected. Univariate and multivariate models were developed using the data. Least square method was used for the univariate model generation. Partial least square and principle component regressions were used for the multivariate models development. The univariate models of the 13 C ssNMR were better than the XRPD as indicated by statistical parameters such as correlation coefficient, R 2 , root mean square error, and standard error. On the other hand, the XRPD multivariate models were better than the 13 C ssNMR as indicated by precision and accuracy parameters. Similar values were predicted by the univariate and multivariate models for independent samples. In conclusion, the univariate and multivariate models of 13 C ssNMR and XRPD can be used to quantitate nimodipine polymorphs.

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“…A major advantage of SSNMR spectroscopy is that it is a nondestructive and selective technique that allows characterization of the excipient directly in the physical state in which it is to be administered, even when in the presence of other excipients and the active pharmaceutical ingredient (3). Additionally, SSNMR spectroscopy can provide unique insight into the molecular dynamics of pharmaceutical solids such as excipients through the use of relaxation measurements (4).…”

Section: Introductionmentioning

confidence: 99%

Analysis of Structural Variability in Pharmaceutical Excipients Using Solid-State NMR Spectroscopy

Sperger

Munson

2011

AAPS PharmSciTech

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Abstract. Polysaccharide-based excipients comprise the majority of most solid dosage forms and can vary dramatically in terms of structural and functionally related properties. Analytical methods for characterizing these important formulation components are crucial. Solid-state NMR spectroscopy (SSNMR) can provide a wealth of information on these materials while offering the advantages of nondestructive sample preparation and selectivity. The overall objective of this work is to identify SSNMR parameters that can be used to detect differences among these excipients. Excipients were obtained from a wide range of suppliers and analyzed as received; 13 C SSNMR spectra were acquired using a Chemagnetics CMX-300 spectrometer operating at approximately 75 MHz. The resolution of SSNMR signals of many excipients allows for positive identification of the major form present. Alginic acid and sodium alginate can be differentiated based on carbonyl peak position. Analysis of relative peak intensities provides insight into the purity of a carrageenan sample compared to known standards. The SSNMR spectrum of starch can be used to identify the source and to quantitate the amorphous and crystalline content. Relaxation values and peak areas of starch derivatives can be related to the degree of hydrolysis, providing an alternative method for determining dextrose equivalent. Differences in peak intensities and relaxation time values of HPMC samples can be correlated to the amount of methoxy subsituent groups. Important characteristics of excipients such as form identification, structural differences, crystalline and amorphous content, and water content variations can be detected using SSNMR spectroscopy.

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Solid-state NMR spectroscopy in pharmaceutical research and analysis

Cited by 138 publications

References 32 publications

Advances in detection of stress tolerance in plants through metabolomics approaches

Advances in detection of stress tolerance in plants through metabolomics approaches

Comparison of Univariate and Multivariate Models of 13C SSNMR and XRPD Techniques for Quantification of Nimodipine Polymorphs

Analysis of Structural Variability in Pharmaceutical Excipients Using Solid-State NMR Spectroscopy

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