Lavoisier Anaïs, Vilgis Thomas A, Aguilera José Miguel
Department of Chemical and Bioprocess Engineering, Pontificia Universidad Católica de Chile, Av. Vicuña Mackenna, 4860, Macul, Santiago, Chile.
Max Planck Institute for Polymer Research, Ackermannweg 10, 55128, Mainz, Germany.
Curr Res Food Sci. 2019 Oct 18;1:31-42. doi: 10.1016/j.crfs.2019.10.001. eCollection 2019 Nov.
A model gel of whey protein isolate (WPI) was prepared by cold gelation with calcium. This system was modified by the addition of free cysteine residues (Cys) at different steps of the process. The WPI cold-set gels obtained were then subjected to heat treatment at 90°C. First, the effect of Cys addition on the heat-induced aggregation of WPI was studied through Atomic Force Microscopy (AFM) and infrared spectroscopy (ATR-FTIR), while Cys' effect on cold gelation was observed by AFM, Confocal Laser Scanning Microscopy (CLSM) and oscillatory rheology (amplitude sweeps). The impact of heating on the microstructure and the viscoelastic properties of the WPI cold-set gels were finally investigated through several techniques, including DSC, ATR-FTIR, CLSM, cryo-SEM, and rheological measurements (temperature sweeps). When added during the first step of cold gelation, Cys modified heat-induced aggregation of WPI, resulting in the formation of a denser gel network with a fractal dimension (Df) of 2.8. However, the addition of Cys during the second step of cold gelation led to the formation of highly branched clusters of WPI and a looser gel network was observed (Df = 2.4). In this regard, the use and limitations of oscillatory rheology and the "Kraus model" to determine the Df of WPI cold-set gels was discussed. The viscoelastic properties and the microstructure of the WPI cold-set gels were irreversibly modified by heating. Gels were stiffer, more brittle, and coarser after heat treatment. New disulfide bonds and calcium bridges formed, as well as H-bonded β-sheets, all contributing to the formation of the final gel network structure.
通过钙冷凝胶法制备了乳清分离蛋白(WPI)模型凝胶。在该过程的不同步骤中添加游离半胱氨酸残基(Cys)对该体系进行了改性。然后将得到的WPI冷置凝胶在90°C下进行热处理。首先,通过原子力显微镜(AFM)和红外光谱(ATR-FTIR)研究了添加Cys对WPI热诱导聚集的影响,同时通过AFM、共聚焦激光扫描显微镜(CLSM)和振荡流变学(振幅扫描)观察了Cys对冷凝胶化的影响。最后,通过差示扫描量热法(DSC)、ATR-FTIR、CLSM、低温扫描电子显微镜(cryo-SEM)和流变学测量(温度扫描)等多种技术研究了加热对WPI冷置凝胶微观结构和粘弹性的影响。在冷凝胶化的第一步添加Cys时,Cys改变了WPI的热诱导聚集,导致形成了分形维数(Df)为2.8的更致密的凝胶网络。然而,在冷凝胶化的第二步添加Cys导致形成了高度分支的WPI簇,并观察到更松散的凝胶网络(Df = 2.4)。在这方面,讨论了振荡流变学和“克劳斯模型”用于确定WPI冷置凝胶Df的用途和局限性。加热不可逆地改变了WPI冷置凝胶的粘弹性和微观结构。热处理后凝胶更硬、更脆且更粗糙。形成了新的二硫键和钙桥,以及氢键连接的β-折叠,所有这些都有助于最终凝胶网络结构的形成。