Heat-induced changes in myofibrillar protein structures and myowater of two pork qualities. A combined FT-IR spectroscopy and low-field NMR relaxometry study

Low-field NMR T(2) and Fourier transform infrared (FT-IR) measurements were performed on meat samples of two qualities (normal and high ultimate pH) during cooking from 28 degrees C to 81 degrees C. Pronounced changes in both T(2) relaxation data and FT-IR spectroscopic data were observed during cooking, revealing severe changes in the water properties and structural organization of proteins. The FT-IR data revealed major changes in bands in the amide I region (1700-1600 cm(-)(1)), and a tentative assignment of these is discussed. Distributed NMR T(2) relaxation data and FT-IR spectra were compared by partial least-squares regression. This revealed a correlation between the FT-IR peaks reflecting beta-sheet and alpha-helix structures and the NMR relaxation populations reflecting hydration water (T(2B) approximately 0-10 ms), myofibrillar water (T(21) approximately 35-50 ms), and also expelled "bulk" water (T(2) relaxation times >1000 ms). Accordingly, the present study demonstrates that definite structural changes in proteins during cooking of meat are associated with simultaneous alterations in the chemical-physical properties of the water within the meat.     

Myowater dynamics and protein secondary structural changes as affected by heating rate in three pork qualities: a combined FT-IR microspectroscopic and 1H NMR relaxometry study

The objective of this study was to investigate the influence of heating rate on myowater dynamics and protein secondary structures in three pork qualities by proton NMR T2 relaxation and Fourier transform infrared (FT-IR) microspectroscopy measurements. Two oven temperatures at 100 degrees C and 200 degrees C corresponding to slow and fast heating rates were applied on three pork qualities (DFD, PSE, and normal) to an internal center temperature of 65 degrees C. The fast heating induced a higher cooking loss, particularly for PSE meat. The water proton T21 distribution representing water entrapped within the myofibrillar network was influenced by heating rate and meat quality. Fast heating broadened the T21 distribution and decreased the relaxation times of the T21 peak position for three meat qualities. The changes in T21 relaxation times in meat can be interpreted in terms of chemical and diffusive exchange. FT-IR showed that fast heating caused a higher gain of random structures and aggregated beta-sheets at the expense of native alpha-helixes, and these changes dominate the fast-heating-induced broadening of T21 distribution and reduction in T21 times. Furthermore, of the three meat qualities, PSE meat had the broadest T21 distribution and the lowest T21 times for both heating rates, reflecting that the protein aggregation of PSE caused by heating is more extensive than those of DFD and normal, which is consistent with the IR data. The present study demonstrated that the changes in T2 relaxation times of water protons affected by heating rate and raw meat quality are well related to the protein secondary structural changes as probed by FT-IR microspectroscopy.     

1H nuclear magnetic resonance relaxometry study of water state in milk protein mixtures

1H NMR signal was used to characterize highly hydrated milk protein dispersions (3-20% dry matter) with various micellar casein concentrations (3-15%), whey protein concentrations (0-3%), lactose concentrations (0-7.5%), CaCl(2) concentrations (0-2 mM), and pH (6.2-6.6). The results showed the predominant effect of micellar casein concentration on water state and were consistent with the three-site relaxation model in the absence of lactose. The relaxation rates observed for these dispersions were explained by the free water relaxation rate, the hydration water relaxation rate, and the exchangeable proton relaxation rate. Hydration water was found to be mainly influenced by casein micelle concentration and structure. The variations in hydration with pH were consistent with those observed for classical measurement of voluminosity observed at this range of pH. The effects of lactose and whey protein content are discussed.     

Evaluation of 1H NMR relaxometry for the assessment of pore‐size distribution in soil samples

¹H NMR relaxometry is used in earth science as a non‐destructive and time‐saving method to determine pore size distributions (PSD) in porous media with pore sizes ranging from nm to mm. This is a broader range than generally reported for results from X‐ray computed tomography (X‐ray CT) scanning, which is a slower method. For successful application of ¹H NMR relaxometry in soil science, it is necessary to compare PSD results with those determined from conventional methods. The PSD of six disturbed soil samples with various textures and soil organic matter (SOM) content were determined by conventional soil water retention at matric potentials between −3 and −390 kPa (pF 1.5–3.6). These PSD were compared with those estimated from transverse relaxation time (T₂) distributions of water in soil samples at pF 1.5 using two different approaches. In the first, pore sizes were estimated using a mean surface relaxivity of each soil sample determined from the specific surface area. In the second and new approach, two surface relaxivities for each soil sample, determined from the T₂ distributions of the soil samples at different matric potentials, were used. The T₂ distributions of water in the samples changed with increasing soil matric potential and consisted of two peaks at pF 1.5 and one at pF 3.6. The shape of the T₂ distributions at pF 1.5 was strongly affected by soil texture and SOM content (R² = 0.51 − 0.95). The second approach (R² = 0.98) resulted in good consistency between PSD, determined by soil water retention, and ¹H NMR relaxometry, whereas the first approach resulted in poor consistency. Pore sizes calculated from the NMR data ranged from 100 μm to 10 nm. Therefore, the new approach allows ¹H NMR relaxometry to be applied for the determination of PSD in soil samples and for studying swelling of SOM and clay and its effects on pore size in a fast and non‐destructive way. This is not, or only partly, possible by conventional soil water retention or X‐ray CT.     

Mobility and distribution of water in cassava and potato starches by 1H and 2H NMR

Mobility and distribution of water in cassava (rainy and drought crops) and potato starches were studied by solid state and NMR relaxometry as a function of H(2)O and D(2)O contents ranging from 0 to 44% (dry basis). Measurements of relative mobility derived from (2)H solid state NMR were based on relative area and line shape analysis. The narrow peak (mobile component) started to show at 5% and increased with increasing D(2)O content. This increase in mobile fraction was accompanied by a line narrowing. The mobile fractions of deuterons reached a >98% level above 15% D(2)O, which is well below the water holding capacity of starch ( approximately 27%) and the previously assigned "glassy-rubbery transition point" (24.3%; Jouppila, K.; Roos, Y. H. The physical state of amorphous corn starch and its impact on crystallization. Carbohydr. Polym. 1997, 32, 95-104). This reconfirms the liquidlike nature of water in the so-called glassy state of starch granules. The plasticization effect of water on starch chains was observed at 14-17% for cassava and potato starches as indicated by the T(1) minimum. This, however, did not seem to relate to the difference observed in swelling among the starches studied.     

1H NMR diffusometry study of water in casein dispersions and gels

The self-diffusion coefficients of water in casein solutions and gels were measured using a pulsed-gradient spin-echo nuclear magnetic resonance technique (PGSE NMR). The dependence of the self-diffusion coefficient of water on the concentration and structure of casein is reported. The results were analyzed using a cell model. It was found that the water self-diffusion coefficient is insensitive to the structure of the casein in solution or in a gelled state. The influence of casein concentration on the water self-diffusion coefficient could be explained by obstruction from the casein molecule. Assuming a simple model with two water regions, each characterized by a specific water concentration and value of the water diffusion coefficient, the water mobility reduction induced by the casein can be rationalized.     

Effect of plant phenolics on protein and lipid oxidation in cooked pork meat patties

Rapeseed and pine bark are rich sources of phenolic compounds that have in previous studies been shown to exhibit antioxidant and anti-inflammatory properties. In this study, the antioxidant effect of rapeseed and pine bark phenolics in inhibiting the oxidation of lipids and proteins in meat was tested as a possible functional food application. The cooked pork meat with added plant material was oxidized for 9 days at 5 degrees C under light. The suitable level of plant material addition was first screened by following lipid oxidation only. For further investigations plant materials were added at a level preventing lipid oxidation by >80%. The oxidation was followed by measuring the formation of hexanal by headspace gas chromatography and the formation of protein carbonyls by converting them to 2,4-dinitrophenylhydrazones and measured by spectrophotometer. It was shown that rapeseed and pine bark were excellent antioxidants toward protein oxidation (inhibitions between 42 and 64%). These results indicate that rapeseed and pine bark could be potential sources of antioxidants in meat products.     

Analysis of acid-soluble glycogen in pork extracts of two PRKAG3 genotypes by 1H liquid-state NMR spectroscopy and biochemical methods

Meat extracts with acid-soluble glycogen (macroglycogen) from M. longissmus dorsi of carriers and noncarriers of the PRKAG3 mutation (RN(-) and rn(+) genotype) were analyzed by both (1)H liquid-state NMR spectroscopy and a biochemical method. The (1)H NMR analysis revealed that shorter polymers (dimers, trimers, etc.) of α-1,4-linked glucose were generated 24-48 h post-mortem. This is not possible to elucidate with the biochemical method, by which only the total amount of hydrolyzed glucose residues is determined. The shorter polymers were primarily formed in carriers of the PRKAG3 mutation, suggesting different post-mortem glycogen degradation mechanisms in the two genotypes.     

用低场核磁研究烫漂对甜玉米水分布和状态影响

该文旨在用低场核磁（NMR）及其成像技术（MRI）研究甜玉米粒中的水分布和水状态,为探讨烫漂后甜玉米失重和热特性参数变化的原因提供理论依据。试验通过T2加权成像技术,观察到烫漂后的甜玉米粒出现新的水信号分布区;通过研究烫漂时间和温度对甜玉米粒横向弛豫信号的影响,发现弛豫时间为450～750 ms和50～70 ms的结合水的百分比例明显变化,并具有一定规律,这种变化是由于淀粉糊化造成的。研究表明,烫漂改变了甜玉米中水的分布和结合状态;低场核磁技术揭示了甜玉米水状态的变化规律,为食品加工过程中物性参数的研究提供了一种有效方法。     

Water distribution in brine salted cod (Gadus morhua) and salmon (Salmo salar): a low-field 1H NMR study

Low-field (LF) (1)H NMR T 2 relaxation measurements were used to study changes in water distribution in lean (Atlantic cod) and fatty (Atlantic salmon) fish during salting in 15% NaCl and 25% NaCl brines. The NMR data were treated by PCA, continuous distribution analysis, and biexponential fitting and compared with physicochemical data. Two main water pools were observed in unsalted fish, T 21, with relaxation times in the range 20-100 ms, and T 22, with relaxation times in the range 100-300 ms. Pronounced changes in T 2 relaxation data were observed during salting, revealing changes in the water properties. Salting in 15% brine lead to a shift toward longer relaxation times, reflecting increased water mobility, whereas, salting in saturated brines had the opposite effect. Water mobility changes were observed earlier in the salting process for cod compared to salmon. Good linear correlations ( F 相似文献   

Effect of fertilizers on galanthamine and metabolite profiles in Narcissus bulbs by 1H NMR

Narcissus bulbs contain the biologically active alkaloid galanthamine, and Narcissus is being developed as a natural source of the molecule for the pharmaceutical industry. The effect of fertilizer on galanthamine production was investigated in a field study using a (1)H nuclear magnetic resonance (NMR) metabolite profiling approach. Galanthamine was quantitated and major metabolites in the bulbs were identified. The application of standard fertilization levels of nitrogen and potassium caused a significant increase in galanthamine as compared to a control. Multivariate data analysis of the (1)H NMR data revealed that applying double the standard level of nitrogen fertilizer resulted in production of more amino acids and citric acid cycle intermediates, but not more galanthamine. The results indicated that standard levels of fertilizer currently applied in The Netherlands are sufficient for optimal galanthamine accumulation in the bulbs. This study shows how (1)H NMR-based metabolic profiling can provide insight into the response of plant metabolism to agricultural practices.     

Analysis of protein structures and interactions in complex food by near-infrared spectroscopy. 1. Gluten powder

The potential of near-infrared (NIR) spectroscopy in detailed food analysis was tested in a model system consisting of gluten powder treated with moisture and heat. Second-derivative transformation and extended multiplicative signal correction were applied for improving the band resolution and removing physical and quantitative spectral variations. Subsequent chemometric analyses gave loading spectra, which were interpreted as spectral effects of altered protein structures, induced by the treatments. Moistening of the gluten powder resulted in shifts and intensity changes in the protein bands, which could be explained by a combination of minor secondary structure changes, water binding, and changed microenvironments of the amino acid side chains. Heat denaturation induced increases at 2209 nm and decreases at 2167-2182 nm, indicating an alpha-helix to beta-sheet transformation, in agreement with the expectations.     

Effect of Hydroxypropylation on Retrogradation and Water Dynamics in Wheat Starch Gels Using 1H NMR

The water dynamics in gels made from native wheat starch, control (alkali‐treated) starch, and hydroxypropylated starch were studied using ¹H NMR relaxometry. Transverse relaxation studies showed that at least two domains of water exist in the starch gel, one with a T₂ of 0.5–8 msec and one with a T₂ at 8–200 msec. For starch gels held at 5°C for up to 15 days, the peak T₂ of both regions decreased with time for gels made from native starch, but not for those made from hydroxypropylated starch. Changes in integrated signal in each region suggests that water migrates out of the lower T₂ domain during retrogradation. Gels made from isolated amylose had a single, relatively mobile water domain, with T₂ dependent on gel concentration. This fraction did not change during storage at 5°C. Granule‐rich gels showed two water domains, one with a T₂ range similar to that for amylose gels, which varied over time and were thermally reversible. During storage, most significant changes occurred in the relatively low T₂ region associated with granule remnants. These studies show that, in addition to changes in starch during retrogradation, water dynamics are also affected by recrystallization and chemical modification of starch molecules.     

Detection of primary and secondary oxidation products by Fourier transform infrared spectroscopy (FTIR) and 1H nuclear magnetic resonance (NMR) in sunflower oil during storage

The oxidation of sunflower oil, stored in closed receptacles at room temperature for a period of 10 years, was monitored using Fourier transform infrared spectroscopy (FTIR) and 1H nuclear magnetic resonance (NMR). The objective was to understand the evolution of the oxidation process in sunflower oil under the conditions above mentioned. These techniques provide information about the oxidative status of several oil samples and the primary and some of the secondary oxidation products formed in the oxidation process. The results obtained show that, under these conditions, sunflower oxidation takes place in a different way to that at higher temperatures with aeration. The 1H NMR spectra show that in the first oxidation stages of the process only hydroperoxides supporting cis, trans-conjugated double bonds are formed and that at more advanced stages hydroperoxides having trans, trans-conjugated double bonds are generated, with the latter always being in a smaller proportion than the former. In addition, the presence of hydroxy derivatives supporting cis, trans-conjugated double bonds among the primary oxidation compounds is shown for the first time. Also, from early oxidation stages onward and unlike the process at 70 degrees C with aeration, it is noticeable that 4-hydroxy- trans-2-alkenals are formed in much higher proportions than 4-hydroperoxy- trans-2-alkenals. This fact could be associated with the presence of hydroxy derivatives with cis, trans-conjugated double bonds among the primary oxidation products and the limited concentration of oxygen during the oxidation. Furthermore, relationships between some oxidation conditions and the oxidation level of the samples were statistically analyzed.     

13C NMR studies of organic matter in whole soils: H. A case study of some Rothamsted soils

Nuclear magnetic resonance (NMR) spectra were obtained for solid samples of whole soils from three long–term field sites at Rothamsted Experimental Station, UK. In all sites, soil organic matter content was either increasing or decreasing due to contrasted long–continued treatments. Two soils were from Highfield, one from under old grassland (47 g organic C kg^?1) and one from an area kept as bare fallow following ploughing of grass 21 years previously (14 g organic C kg^?1). Three soils were taken from Broadbalk, two from plots within the Broadbalk Continuous Wheat Experiment which had received no fertilizer or animal manure annually for 148 years (7 and 27 g organic C kg^?1, respectively) and one from Broadbalk Wilderness, wooded section (38 g organic C kg^?1). Broadbalk Wilderness was arable until 1881 and has reverted to deciduous woodland in the subsequent 110 years. Two soils were from Geescroft, one from an arable field (9 g organic C kg^?1) and one from Geescroft Wilderness (35 g organic C kg^?1) which began reversion to deciduous woodland at the same time as Broadbalk Wilderness but is now acid (pH = 4.2) in contrast to Broadbalk which is calcareous (pH = 7.3). Solid–state ¹³C NMR spectra were obtained on a 300–MHz instrument using cross polarization (CP) and magic angle spinning (MAS). All samples exhibited peaks in the following spectral regions: 0–45 ppm (alkyl), 45–60 ppm (methoxyl, carbohydrate and derivatives), 60–110 ppm (carbohydrates and derivatives, C–α of peptides), 110–160 ppm (aromatics) and 160–185 ppm (carboxyl groups and derivatives). Within the spectrum of a specific sample it was not possible to determine the relative proportions of soil organic carbon in the different forms identified because a range of factors can potentially alter the relative areas of peaks in different regions of the spectrum. However, from a comparison of relative peak areas within a set of soils from a given site, differing only in organic matter content, information can be deduced regarding the forms of C that are more or less subject to change in response to land use or management. At all sites carbohydrate C appears to be the form that is most subject to change, suggesting that it is an ‘active’ fraction compared with the other forms. It was greatest where organic matter inputs were greatest (due to inputs of farmyard manure or reversion to woodland) and declined relative to other forms following ploughing of old grassland. Alkyl C increased as total C accumulated but did not decline relative to other forms following ploughing of grass. One reason for the non–quantitative nature of the soil ¹³C CPMAS spectra was a short (approximately 1 ms) component of the rotating–frame T_I relaxation time for H nuclei (T_1pH). This problem was not overcome by acquiring data at – 60°C. In principle, solid–state spectra of soils obtained by direct polarization (i.e. without CP) might produce quantitative results, but the low C content of most mineral soils (10–50 g C kg^?1) precludes this, given current instrumentation.     

流量对河水滴灌重力沉沙过滤池内流速分布的影响

为研究流量对河水滴灌重力沉沙过滤池流速分布规律的影响,该文对5种不同流量下的水沙两相流流场进行了数值模拟。通过对不同流量下流速沿程分布规律、流速沿水深方向分布规律及水沙分离效率的对比与分析,可知河水滴灌重力沉沙过滤池的适宜流量范围为0.05~0.2 m3/s,进水流量越小,流速变化幅度也就越小,越有利于泥沙沉降,水沙分离效率不小于72.5%。不同流量下沉淀池中流速沿程变化规律可分成3个阶段:流速迅速增加阶段、流速缓慢减小阶段和流速迅速减小阶段。清水池中流速方向与沉淀池的相反,流速沿程减小。受进水口、出水口和固体边界,以及侧向溢流堰的影响,不同流量下河水滴灌重力沉沙过滤池中的流速沿水深方向分布规律有差别。当流量为0.05和0.1 m3/s时,远离进水口、出水口及侧向溢流堰的位置,流速沿水深方向的分布规律包含流速迅速增加、流速缓慢减小和流速恒定3个阶段,而清水池则只包括流速迅速增加和流速恒定阶段。研究可对大首部的应用提供参考。     

水土保持措施对无定河流域沟道-河道系统泥沙收支平衡的影响

流域系统可以分为坡面系统和沟道-河道系统2大单元,可以分别建立泥沙收支平衡关系。结果表明：1）实施水土保持措施以后,无定河流域系统泥沙收支平衡中各变量均随时间而变化。沟道-河道系统泥沙输移比发生了极显著的减小趋势,泥沙存储量发生了显著的增大趋势,流域产沙量的变化发生了较显著的减小趋势,坡面净侵蚀量有所减少,但变化趋势不显著。2）对于不同的泥沙收支平衡变量的变化而言,水土保持措施变化和降雨变化的贡献率是不同的;对坡面净侵蚀量的变化而言,汛期降雨的变化起着决定性的作用,贡献率高达90.82%,坡面水土保持措施的贡献率仅为9.18%;对沟道河道系统泥沙存储量的变化而言,淤地坝拦沙的变化起着决定性的作用,贡献率高达76.16%,汛期降雨变化的贡献率仅为23.81%;对流域产沙量的变化而言,汛期降雨和水土保持措施的变化都起着重要作用,前者贡献率为57.84%,后者贡献率为42.16%。3）对沟道-河道系统泥沙输移比RSDRc的变化而言,淤地坝拦沙的变化起着决定性的作用,贡献率高达87.27%,汛期降雨变化的贡献率仅为12.73%。     

山西省农牧结构及其协调发展研究

在对山西省农牧结构发展变化及现状评价的基础上，以农牧协调发展为前提，运用系统分析方法提出3套山西省种植业及畜牧业结构调整方案，并对调整后的农牧协调性作了系统分析。     

我国西部地区水土资源匹配模式与政策研究

研究分析我国西部地区水土资源时空分布及其利用结构等现状与问题 ,指出西部水土资源利用的根本问题不是资源匮乏 ,而是土地资源和水资源利用结构不合理、时空分布不均和利用效率低等原因造成匹配不当。并提出西部水土资源合理匹配主要模式和政策措施。