核磁共振技术在食品分析检测中的应用

核磁共振检测技术是一种新型的食品无损检测技术。介绍了核磁共振的基本原理和优势,综述了国内外核磁共振技术在食品中的水分、油脂、玻璃态转变、碳水化合物、蛋白质及品质鉴定等方面的研究进展,但该技术在实际应用中仍然存在一些问题,有待进一步研究。     

Application of quantitative nuclear magnetic resonance spectroscopy to biological acidification of barley mashes

Spontaneous biological acidification has long been a part of the German brewing tradition, and was historically used to optimize the pH of brewhouse mashes. By facilitating the growth of native barley flora, the production of lactic, acetic and succinic acids sours the mash, functioning in a similar way to the addition of food‐grade acids, which are prohibited under the Reinheitsgebot of 1516. Traditionally, sour mashes have been performed at the ‘optimum’ temperature of 49 °C. Quantitative proton nuclear magnetic resonance spectroscopy was used for the investigation and quantitation of organic acids produced by acidified mashes over a range of temperatures. All target metabolites demonstrated an inverse relationship with temperature, although lactic acid reached a relative maximum at 49 °C, which is in agreement with the customary sour mash temperature. Therefore, it would seem that the optimization of a sour mash is dependent not on absolute acid concentration, which would give the greatest pH regulation potential, but on the relative acid concentration, an important factor influencing the final flavour profile of a beer. Copyright © 2014 The Institute of Brewing & Distilling     

核磁共振技术在食品研究中的应用

介绍了核磁共振(NuclearMagneticResonance)技术的基本原理及其在食品分析和研究中的应用。     

Technical note: Evaluating nuclear magnetic resonance spectroscopy for determining body composition in Holstein dairy calves using deuterium oxide dilution methods

Deuterium oxide (D₂O) dilution methods have been used to assess body composition in live animals. Estimated body water content can be used to predict body fat and protein, and thus, the amount of energy reserves. It is an alternative method to direct chemical analysis and considered a noninvasive technique that is economical and repeatable. Deuterium oxide use is considered easy, safe, and accurate; however, the traditional methods of analyzing D₂O are expensive, tedious, and time consuming. The objective of this study was to evaluate the potential for using nuclear magnetic resonance spectroscopy (NMR) to determine body composition in Holstein dairy heifers. Nuclear magnetic resonance is less expensive and requires minutes to calculate the percentage of D₂O in the blood. This study used 24 newborn dairy heifer calves blocked by birth and randomly assigned to 1 of 3 treatments: (1) 446 g dry matter (DM) of a conventional milk replacer (MR) [CON; 20% crude protein (CP), 20% fat], (2) 669 g DM of a moderately high protein MR (MOD; 26% CP, 18% fat), or (3) 892 g DM of a moderately high protein MR (aggressive, AGG; 26% CP, 18% fat). All calves had free-choice access to starter and water. Both MR and starter were medicated with decoquinate. During weaning (d 43 to 49), the morning MR feeding ceased. On d 50, all MR feedings ended but starter and water intakes were continuously recorded until d 56. When calves were 50 d of age, a baseline blood sample was taken followed by injection of 300 mg of D₂O/kg of body weight in sterile physiological saline (0.9%). The syringes containing the D₂O in physiological saline were weighed before and after administration to record the actual dose of D₂O injected gravimetrically. After injection, the D₂O was allowed to equilibrate with body water for 1 h. Six blood samples were taken over 6 d (1/d) at 1630 h to estimate the dilution of the tracer. The plasma was aspirated and stored at ?20°C until further D₂O analysis. This new method was validated using 4 calf plasma samples that were sent to an outside laboratory for measurement using an independent validation method. We detected no differences in total body water, protein, fat, or mineral content in calves fed CON, MOD, or AGG; however, results demonstrated that the D₂O dilution technique and analysis by NMR is an appropriate and easy method to estimate water, protein, ash, and fat in young heifers.     

Detection of pits in olives under motion by nuclear magnetic resonance

One-dimensional magnetic resonance projections of pickled olives were acquired while they were travelling on a conveyor belt which passed through a 2-tesla NMR magnet and a 150-mm imaging coil. The projections were used to distinguish between pitted and non-pitted olives. The effect of fruit position in the coil was tested and coil end effects were noticed when projections were generated under dynamic conditions. Sorting of 300 pitted and non-pitted olives at various belt speeds was tested. Classification errors (pitted olives classified as non-pitted and vice versa) were 4·3, 4·7, 2·3 and 4·0% at 0, 5, 15 and 25 cm s⁻¹ belt speeds, respectively. ©1997 SCI     

Determination of fat and water content in vitro and in vivo by proton nuclear magnetic resonance

Proton NMR spectroscopy was performed on a series of pork samples containing varying proportions of fat and muscle and on a series of control and obese mice. Initial measurements were made using a 0.5 T (21 MHz) whole body imaging system and the results were expressed as the ratio of water and lipid hydrogen peak areas. With pork samples the NMR results correlated well with per cent water or lipid in the tissue (r = 0.99 for 20- and 50-g samples). For the mice the correlation between per cent water or lipid in the body and the NMR measurement was 0.92. Subsequent measurements were made using a 4.7 T (200 MHz) imaging/spectrometer from which separate integral values were obtained for the water and lipid hydrogen peaks. The separation of the water and lipid peaks was 3.5 ppm. For pork samples measured with the 4.7 T system the correlation between the peak area and the amount of water or lipid in the sample was 0.997 with the standard error of the estimate being ±0.72 g for water and ±1.00g for lipid. NMR imaging was used to determine the relative amount of fat and muscle in a cross-section of a control and an obese rat.     

Optimization of nuclear magnetic resonance and gas chromatography-mass spectrometry-based fingerprinting methods to characterize goat milk powder

This study is the first to provide a comprehensive characterization of the liquid and volatile fractions of whole goat milk powder (GMP). Robust nuclear magnetic resonance (NMR)- and gas chromatography-mass spectrometry (GC-MS)-based chemical fingerprinting methods were optimized and implemented. The untargeted ¹H-NMR analysis resolved 44 metabolites in the liquid fractions of GMP. The NMR fingerprinting technique effectively identified metabolites coming from the aliphatic, sugar, and aromatic regions that can be important in defining the technological properties and quality of the GMP. The untargeted headspace gas chromatography-mass spectrometry fingerprinting was able to detect a total of 50 volatiles including alkanes, ketones, alcohols, aromatics, alkenes, aldehydes, esters, acid, and sulfur compounds. The GMP was dominated by volatiles in the alkane group, while only a few esters were detected. Goat milk is a premium product and vulnerable to fraudulent activities such as adulteration or counterfeit. Therefore, proper characterization and identification is a crucial first step to verify its authenticity and quality.     

Oxidation of corn oil at room temperature: Primary and secondary oxidation products and determination of their concentration in the oil liquid matrix from H nuclear magnetic resonance data

The oil liquid matrix of several corn oil samples that have been stored at room temperature in closed receptacles for different periods of time is studied by means of ¹H nuclear magnetic resonance (¹H NMR), in order to further knowledge about this type of edible oil oxidation. As expected, the degradation of linoleic acyl groups predominates. In samples at early oxidation stages the presence of hydroperoxides and of (Z,E) conjugated-dienic systems is demonstrated, the concentration of the first group being higher than that of the second. In addition to these compounds, the presence of hydroxy derivatives supporting (Z,E) conjugated-dienic systems, as well as of hydroperoxy derivatives supporting (E,E) conjugated-dienic systems, in samples at intermediate and advanced oxidation stages, is also shown. Corn oil samples at advanced stages of oxidation also contain aldehydes, among which there are alkanals, (E)-2-alkenals, (E,E)-2,4-alkadienals, 4-hydroxy-(E)-2-alkenals, 4-hydroperoxy-(E)-2-alkenals and 4,5-epoxy-(E)-2-alkenals. The concentrations of the different kinds of intermediate compounds above mentioned as well as of the different kinds of aldehydes present in the oil liquid matrix were determined. These latter compounds can be either free or joined to truncated structures of triglycerides. In addition, a principal component analysis between storage conditions and oxidation level of the samples was carried out.