低场核磁共振法测定猪肉中脂肪含量

为避免索氏抽提法使用有机溶剂带来的环境污染与危害,提高猪肉中脂肪含量的检测效率,采用低场核磁共振技术研究测定猪肉中脂肪含量。首先优化回波时间、重复扫描次数等信号采集参数和样品质量、烘干时间、检测温度等样品相关参数,然后对方法重复性和精密度进行考察验证。结果表明,4 g肉糜烘干6 h,在检测温度50 ℃、回波时间0.3 ms、重复扫描次数64 次条件下,以纯猪油为标准样品,检测结果良好,标准曲线R2达到0.999 9,重复性相对标准偏差为1.69%～2.72%,日内、日间精密度分别为3.07%、2.57%。该低场核磁法与GB 5009.6—2016《食品中脂肪的测定》中索氏抽提法之间相关系数高达0.999 5。因此,该方法可用于猪肉中脂肪含量的准确定量,同时可为其他畜禽肉脂肪含量的测定提供参考。     

核磁共振磷谱法测定乳制品中的酪蛋白含量

基于插值法建立乳制品中酪蛋白的核磁共振磷谱定量检测方法.结果表明,该方法的检出限为0.38 g/L(信噪比(RSN)=3),定量限为1.25 g/L(RSN=10);在5.00～35.00 g/L质量浓度范围内线性良好,相关系数R2大于0.999;加标回收率在91.94％～105.10％范围区间;日内精密度在0.65％...     

基于低场核磁共振技术的注胶肉快速检测

目的:探索并建立一种新的注胶猪肉快速检测方法.方法:以正常猪肉及注射不同种类胶(黄原胶、卡拉胶、明胶、琼脂)的注胶肉为对象,利用低场核磁共振并结合主成分分析法分析处理的检测数据,根据肉品中的水分存在状态及分布结果,对猪肉进行快速检测.结果:正常肉与注胶肉之间、各类注胶肉及不同注胶量之间在主成分得分图上具有很好的区分效果.结论:低场核磁共振技术结合主成分分析法可以快速区分正常肉与注胶肉.     

NMR氢谱定量测定奶酪中总共轭亚油酸的含量

目的：建立用核磁共振定量法测定奶酪中总共轭亚油酸含量的方法,并与紫外分光光度法进行比较。方法：以1,2,4,5-四甲基苯为内标,采用5 mm BBO探头、脉冲序列noesyig1d、探头温度300 K、扫描次数128 次、脉冲延迟时间（D1）10 s。结果：该方法的加样回收率为93.33%,相对标准偏差（relative standard deviation,RSD）为4.20%;精密度RSD为0.99%,重复性RSD为3.17%,稳定性RSD为1.81%。结论：该方法前处理简单,无需标准品做参比,在对目标物完成定性、定量分析的同时还可以实现对非目标物的定性分析。与紫外分光光度法相比,该方法具有更好的专属性。     

Two-Dimensional Nuclear Magnetic Resonance Studies of Starch and Starch Products

The use of two-dimensional Nuclear Magnetic Resonance (NMR) spectroscopy as applied to studies of starch, starch products and glycogen is reported. The use of both homonuclear correlation (COSY, relay-COSY and HOHAHA) and heteronuclear correlation (HMQC, HETCOR) experiments is discussed. This approach makes it possible to obtain complete assignments of the proton NMR spectra of these polysaccharides. This is not possible from 1-D spectra due to excessive overlap of the non-anomeric proton signals. The resulting assignments are useful in obtaining structural information regarding starch and related products. Moreover, the greater inherent resolution of the two-dimensional spectra can reveal the presence of low molecular weight carbohydrates (glucose, maltose etc.) in dextrin samples, thus providing information about carbohydrate composition.     

One-Dimensional Nuclear Magnetic Resonance Studies of Starch and Starch Products

The use of one-dimensional Nuclear Magnetic Resonance (NMR) spectroscopy as applied to structural studies of starch, starch products and glycogen is reviewed. Proton, carbon-13 and phosphorus-31 NMR spectra of a range of starches and starch products are described. These spectra, particularly carbon-13 NMR spectra, permit one to obtain structural information regarding these molecules. From the proton NMR spectra, which can be obtained with greater sensitivity, it is possible to determine the DP (degree of polymerization, the average number of glucose units per molecule) and the degree of branching (the proportion of glucose units which are (1→6) linked) without recourse to chemical or enzymatic methods. Moreover, the anomer distribution of the reducing sugars can be determined by ¹H or ¹³C NMR. Finally, some examples of the application of NMR to follow the time course of enzymatic digestion and sugar anomerization are discussed, as is the solid-state NMR of starch and glycogen. The phosphorus-31 NMR spectra provide information about the nature of the phosphate groups in potato starch.     

Quantitative Determination of Water and Lipid in Sunflower Oil and Water/Meat/Fat Emulsions by Nuclear Magnetic Resonance Imaging

A Dixon NMR imaging experiment was used to map the spatial distribution of either the water or lipid protons in sunflower oil and water and meat and fat emulsions. A phase correction algorithm was applied to the experimental image data compensate for regional inhomogeneities of the magnetic field and allowed the water and lipid concentrations from any region in the image to be measured quantitatively.     

低场核磁共振技术快速检测鲜乳水分方法研究

运用低场核磁共振技术研究鲜乳变质过程中水分的变化规律,选取反转恢复脉冲序列和Carr-Purcell-
Meiboom-Gill序列测定鲜乳样品在不同贮藏时间的弛豫参数,根据纵向弛豫时间T1、横向弛豫时间T2观测样品的水
分含量,并通过T2反演数据的拟合结果得出自由水和结合水的变化趋势。研究表明,随着贮藏时间的延长直至鲜乳
变质腐败,鲜乳中的总水分先减少后增加,其中自由水减少,结合水先减少后增加。结果表明,低场核磁共振技术
可用于快速、有效地判定鲜乳的新鲜程度,并有助于在鲜乳贮运过程中品质的实时监控。     

Visualisation of Liquid Triacylglycerol Migration in Chocolate by Magnetic Resonance Imaging

This study has demonstrated that magnetic resonance imaging can be used to visualise the migration of liquid triacylglycerols in composite chocolate confectionery. Migration was observed between a layer of hazelnut oil filling (oil+icing sugar) and a layer of dark chocolate used as a model of composite chocolate confectionery products. In addition, low-resolution nuclear magnetic resonance measurements of the solid fat content (%) were also made. Substantial differences were observed between the migration profiles at 19 and 28°C, and in the distribution of liquid triacylglycerols across the chocolate layer after migration. It is suggested that the mechanism of migration involves both diffusion of the liquid triacylglycerols and capillary attraction of the hazelnut oil into the chocolate matrix. © 1997 SCI.     

低场核磁共振法快速检测炸油质量

由于在高温油炸过程中的快速劣变,市场上油炸用油的质量问题日益受到人们的关注. 为了研究低场核磁共振技术在市场上复杂油炸条件下的油炸用油质量快速检测中的表现,共从上海市10个行政区的市场上共采集油炸用油样品107个,包括大豆油96个,起酥油11个. 通过测定油样的极性组分和黏度,发现6个(占总样品数56%)油样的极性组分超过国家标准,说明市场上油炸用油存在一定的安全问题. 通过线性分析发现极性组分和黏度之间的线性关系良好,R2为0892,除去样品中11个起酥油后R2则达到0927. 用低场核磁共振仪测定各油样后,通过对多组分T2弛豫图谱中T21峰面积(S21)比例的分析发现,S21比例与极性组分和黏度呈现良好的相关性,R2值分别为0860和0840,除去油样中的起酥油后R2值略有上升,分别达到0865和0854. 这说明可以利用低场核磁共振技术达到快速检测市场上油炸用油品质的目的.     

核磁共振波谱法分析淀粉中含有的蛋白质和脂肪

淀粉、蛋白质和脂肪由于结构复杂使解析其结构非常繁琐和困难,致使对各种淀粉中含有的蛋白质、脂肪的深入研究受限。随着高分辨核磁共振波谱(NMR)技术飞速发展,它在淀粉的结构研究中发挥了日益重要的作用。综述了淀粉、蛋白质和脂肪一维核磁共振(1HNMR,13CNMR)的特征和应用核磁共振波谱法分析淀粉中含有的蛋白质、脂肪。     

基于单边核磁共振技术的乳制品品质分析

运用单边全开放式核磁共振技术对常见掺假牛乳进行快速检测,并对室温条件下贮藏的市售盒装酸奶进行跟踪监测。在非均匀磁场下采用SGSE-CPMG（static gradient spin echo carr-purcell-meiboom-gill）序列测量各个样品的横向弛豫时间（记为T2CPMG）,经弛豫校正可得到测试样品的横向弛豫时间T2。研究表明,在恒定梯度磁场中不同掺假比例样品随掺假质量浓度的升高其T2CPMG逐渐增大,经弛豫矫正后盒装酸奶样品T2峰位的变化可间接反映其新鲜度。运用单边核磁共振技术可实现乳制品品质的快速无损检测,被测样品无需复杂预处理,其系统硬件结构简单可便携（或安装）至现场进行实时检测。     

Oil Migration in a Chocolate Confectionery System Evaluated by Magnetic Resonance Imaging

ABSTRACT: Oil migration is a common problem in composite chocolate confectionery products resulting in softening of chocolate and hardening of the filling. Spatial and temporal changes in the liquid oil content of a 2-layer peanut butter and chocolate model system were evaluated using a magnetic resonance imaging (MRI) technique. The experimental factors were chocolate particle size, milk fat content, emulsifier concentration, degree of temper, and storage temperature. The responses were migration rate and overall change in signal intensity (amount of migration). Based on analysis of variance (ANOVA), particle size, milk fat content, and storage temperature were significant factors for oil migration rates. Milk fat content and temperature were significant factors for overall change in signal intensity.     

利用1H NMR分析小龙虾的特征性滋味组成

为深入研究小龙虾的非挥发性滋味活性物质,利用1H核磁共振（nuclear magnetic resonance,NMR）对小龙虾中游离氨基酸、核苷酸、有机酸、可溶性糖和生物碱等滋味成分进行定性定量分析,并采用味道强度值（taste activity value,TAV）分析其味觉活性成分,以及通过味精当量（equivalent umami concentration,EUC）评价鲜味。结果表明,使用1HNMR共检测到小龙虾中33种滋味化合物,其中精氨酸、组氨酸、谷氨酸、丙氨酸、赖氨酸、甘氨酸、5’-单磷酸腺苷二钠、5’-单磷酸肌苷二钠、琥珀酸和乳酸的TAV大于1,它们对小龙虾的滋味有重要影响。EUC值以谷氨酸钠质量计,发现小龙虾样品的EUC值为9.1 g/100 g,说明小龙虾具有非常强烈的鲜味。     

低场核磁共振技术在肉与肉制品水分测定及其相关品质特性中的应用

低场核磁共振技术以其检测迅速、无损、样品需要量少等优点已在肉类科学领域得到一定的研究和应用。本文介绍了低场核磁共振技术基本原理,归纳了肉与肉制品水分组成及测定方法,并详细综述了低场核磁共振技术在肉与肉制品水分测定及相关特性中的应用研究进展。     

核磁共振磷谱定量测定肉制品中磷酸盐的含量

建立了核磁共振磷谱(31P-qNMR)技术快速定量测定肉制品中磷酸盐含量的方法.样品采用碱性缓冲盐振荡提取2次,离心过膜后,以六甲基磷酰三胺为内标进行定量分析.结果表明:该方法加标回收率为97.0％～112.0％,相对标准偏差0.87％～3.15％.日内精密度为0.68％～3.55％,日间精密度为1.12％～4.51％...     

Structural Studies of Pullulan by Nuclear Magnetic Resonance Spectroscopy

Nuclear Magnetic Resonance (NMR) spectroscopy was used to probe the primary structure of the glucan pullulan. Carbon-13, proton and phosphorus-31 NMR spectra in aqueous solution of the intact poly-saccharide obtained from three different sources indicate that significant structural differences can occur among these samples. In particular, two samples consist solely of α(1 → 6) linked maltotriose units, in accord with the generally accepted structure. However a third sample has fewer α(1 → 6) linkages and appears to consist of higher α(1 → 6) linked maltooligosaccharides in addition to maltotriose. Unlike the other samples, this sample was also phosphorylated. Enzymatic digestion of pullulan followed by NMR spectroscopy using pullulanase confirmed these results, as did HPLC analysis of the resulting digest, which showed the presence of maltooligosaccharides consisting of ten and more glucose units. However, HPLC analysis of acid hydrolysed pullulan indicated that no sugars other than glucose were present in any of the samples examined.     

Mobility of Water in Starch Powders Determined by Nuclear Magnetic Resonance

The molecular mobility of water in corn starch powders (71 to 96% solids) was determined by deuterium (²H) and oxygen-17 (¹⁷O) high-field Nuclear Magnetic Resonance (NMR) spectroscopy, in deuterium (D₂O) and oxygen-17 enriched water (H₂¹⁷O), respectively. The NMR transverse relaxation rate (R₂) was related to both the concentration and activity of water (a_w). The concentration plot showed two regions of water mobility; trapped and monolayer water. The water activity plot showed two linear regions of water mobility; Region A, from 0.99 to 0.23 a_w, and Region B, from 0.23 to 0.11 a_w. The linear relationship in Region A between water mobility, as measured by R₂ and water activity is hypothesized to be due to the hydrophobic nature of the starch granules which results in diffusion limited water motion. Relaxation rates for ²H and ¹⁷O at high a_w were compared with one another and literature data.