Use of NMR relaxometry to assess physicochemical characteristics of seeds and grains

2022-8
Ünal, Kübra
Nuclear Magnetic Resonance (NMR) relaxometry is a widely used characterization method for the analysis of physiological and biochemical changes in a huge variety of samples. Time domain NMR (TD-NMR) relaxometry provides structural analysis at low magnetic fields. It is basically relies on the relaxation times of proton signals coming from the entire sample. Thus, it provides quantification of water absorption and analyzing its distribution within the biological systems. In this dissertation, plant tissues and starch-water interaction systems were investigated using TD-NMR relaxometry. In the first part of the study, TD-NMR relaxometry was used to investigate the changes in the cell integrity of plant tissues. For plant tissues, tomato seed was selected and subjected to osmotic stress (OS) (10, 20, 30% NaCl solutions), ultrasonication (US) (5, 10 and 20 minutes) at 75% amplitude and high hydrostatic pressure (HHP) (300, 400 and 500 MPa for 15 min at 20°C). NMR relaxation spectra of tomato seed gave four peaks each corresponding to different water compartments due to multiexponential relaxation behavior of the plant cell. According to the results, all the three treatments resulted in cell permeabilization and disruption of cellular compartmentalization. Among the treatments, HHP at 500 MPa for 15 min at 20°C resulted in the most detrimental effect in the cell structure and OS treatment with 10% NaCl solution caused the least changes in the cell structure. Seeds exposed to different treatments were also analyzed by Scanning Electron Microscope (SEM) to determine the extent of damage to the cell. These results have proved that NMR relaxometry is an effective method to analyze the cell membrane integrity of tomato seeds exposed to selected treatments. Use of NMR relaxometry to assess physicochemical characteristics of starch-water interactions was the second part of the study. Quinoa starch was chosen to study starch-water interactions. Following starch isolation, NMR relaxometry was used to investigate the physiological changes in quinoa starch dispersions induced by HHP and US. HHP at 250, 350 and 500 MPa at 20°C and 40°C; ultrasonication (US) at 100% power with constant pulse for 15 min were applied as modification methods. Following the treatments, functional, rheological, particle size, morphological and structural analysis were carried out. Results showed that swelling power and water solubility index of quinoa starch was decreased significantly with both HHP and US treatments (p<0.05). Apparent viscosity of the starch samples decreased with increasing pressure and US treatment. The particle size distribution revealed a more apparent increase in the volume mean diameter (D [4,3]) with HHP treatment (p<0.05) compared to US. Time domain (TD) NMR relaxometry experiments confirmed that HHP treatment caused less granule swelling of starch. NMR relaxation spectra of quinoa seeds revealed mainly two distinct proton populations and HHP treatment at 500 MPa resulted in faster exchange of proton populations compared to the US treatment. DSC results are correlated with the results of NMR relaxometry. SEM images visualized the change in the morphology of the quinoa starches after treatments and structural changes were observed through FTIR and XRD experiments. These results have demonstrated that HHP treatment had a strong modification effect on quinoa starch compared to US and provide modified quinoa starch with better quality. Moreover, the investigation of the quinoa starch and water interactions under these conditions was demonstrated to be effective with the use of NMR relaxometry. To conclude, this dissertation has proved that TD-NMR relaxometry is an effective method for characterization of cell integrity of tomato seeds and physiological changes in quinoa starch dispersions. This study may provide information for further research in food applications.

Suggestions

The Effect of Ultrasonication on the Size and Morphology of Iron Oxide - Chitosan Nano and Microparticles
Akin, Deniz; YAKAR, ARZU; Gündüz, Ufuk (2013-04-28)
The aim of this study is to synthesize magnetic Fe3O4-chitosan nano and microparticles (Fe3O4-CPs) by suspension cross-linking and ionic gelation methods and investigate the effect of ultrasonication on the size, morphology and magnetic properties. The synthesized particles were characterized by transmission electron microscopy (TEM), dynamic light scattering (DLS) and vibrating sample magnetometry (VSM). The results showed that the ultrasonication decreased the mean particle diameter and enhanced magnetic ...
Controlled assemble and microfabrication of zeolite particles on SiO2 substrates for potential biosensor applications
Öztürk, Semra; Turan, Raşit; Akata Kurç, Burcu (2008-12-04)
Zeolite nanoparticles were organized into functional entities on SiO2 substrates and microfabrication technique was tested to form patterns of zeolite nanoparticles on SiO2 using the electron beam lithography (EBL). The effect of different techniques for efficient zeolite assembly on the SiO2 substrates was investigated. For this purpose, three different assembly techniques were tested. The first two methods are spin-coating (SC) and ultrasound aided strong agitation (US) methods, which were tested using ba...
Development of sensitive analytical methods for the determination of thallium at trace levels by slotted quartz tube flame atomic absorption spectrometry
Ari, Betul; BAKIRDERE, Sezgin; Ataman, Osman Yavuz (Elsevier BV, 2020-09-01)
A simple, sensitive and economical technique is needed for the determination of thallium and this study demonstrates the different analytical strategies were developed using atomic absorption spectrometry (AAS). In order to improve the sensitivity of flame atomic absorption spectrometry (FAAS), a basic slotted quartz tube (SQT) was used for the thallium determination. In the first strategy, mixing propanol (100 mu L) and Tl standard solution (500 mu L) under the optimum conditions, namely solvent assisted S...
Experimental and mathematical investigation of mass transfer in food andhydrogel systems using magnetic resonance imaging and NMR relaxometry
Çıkrıkcı, Sevil; Öztop, Halil Mecit; Department of Food Engineering (2019)
Nuclear magnetic resonance (NMR) and Magnetic Resonance Imaging (MRI) are well-known non-invasive characterization methods used in a wide range of areas; from medical to food applications. NMR experiments are conducted either through spectroscopy with high resolution systems or with relaxometery (Time Domain NMR) through mid or low field systems. Time domain NMR is primarily based on relaxation times and diffusion measurements from the signal coming from the whole sample while MRI enables to visualize the i...
Preparation and thermal characterization of poly(2-vinylpyridine) copolymers coordinated to Cr nanoparticles
Öztürk, Yurdagül; Kayran, Ceyhan; Hacaloğlu, Jale (2015-06-01)
In this study, polystyrene-block-poly(2-vinylpyridine), PS-b-P2VP, polyisoprene-block-poly(2-vinylpyridne), PI-b-P2VP and poly(methyl metacrylate)-block-poly(2-vinylpyridine), PMMA-b-P2VP, coordinated to Cr metal were synthesized and characterized by Fourier transform infrared, transmission electron microscopy and direct pyrolysis mass spectrometry techniques. Both thermal degradation mechanism and thermal stability of P2VP blocks were affected by the coordination of Cr nanoparticles to nitrogen of pyridine...
Citation Formats
K. Ünal, “Use of NMR relaxometry to assess physicochemical characteristics of seeds and grains,” Ph.D. - Doctoral Program, Middle East Technical University, 2022.