贮藏过程中棕榈油基塑性脂肪结晶网络结构与宏观物理性能变化研究
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摘要
随着国家经济及食品工业的发展以及人均消费水平的提高，塑性脂肪作为现代食品工业中新型食用油脂制品的需求量愈来愈大，对产品的质量要求也愈来愈高。塑性脂肪在贮藏过程中品质将会由于温度的不适或波动而劣化，品质的变化与其内部结构变化密切相关。了解塑性脂肪品质变化与内部结构变化规律对高品质塑性脂肪的生产有重要指导作用。有鉴于此，本论文以两种棕榈油基起酥油为研究对象，通过研究温度恒定贮藏（0°C、10°C、20°C、30°C、40°C）与温度波动贮藏（0°C12h-20°C12h、10°C12h-20°C12h、30°C12h-20°C12h、40°C12h-20°C12h，分别作为周期温度往复）模式下贮藏温度和时间对这两种起酥油样品的组成、宏观物理性能、热特性、结晶网络结构的变化规律，探讨贮藏过程中温度和时间对这类塑性脂肪的微观结构和宏观性能的影响机理，建立贮藏过程中结晶网络结构与宏观物理性能之间的关联，为高品质塑性脂肪的可控化生产及贮藏建立科学的理论基础。主要研究内容与结果如下：
一、贮藏过程中棕榈油基起酥油的分子组成、固体脂肪含量、质构及流变性能变化
采用HPLC、pNMR、TA和Hakee流变仪分别研究温度恒定及波动贮藏下模型起酥油样品的分子组成、固体脂肪含量、硬度及弹性模量的变化。研究发现，在两种温度作用模式下，两种模型起酥油的分子组成均未发生明显变化。在恒温贮藏时，随贮藏温度的升高，两种起酥油样品的固体脂肪含量呈线性下降，硬度呈指数关系下降，弹性模量逐渐下降；随贮藏时间的延长，二者的固体脂肪含量及弹性模量变化不显著，当温度≤20°C时硬度随时间的延长逐渐变大，当温度>20°C时硬度随时间的延长逐渐变小。在温度波动贮藏时，随波动温度的升高，两种样品的固体脂肪含量呈现先稳定（0°C-20°C）后下降的趋势（30°C-40°C），硬度呈先平稳（0°C-10°C）后降低（30°C-40°C）的趋势，弹性模量呈先下降（0°C-10°C）后趋于稳定（30°C-40°C）；随贮藏时间的延长，二者的固体脂肪含量及弹性模量无显著变化，硬度呈对数下降。
二、贮藏过程中棕榈油基起酥油的热性质及晶型的变化
采用DSC和XRD方法分别研究温度恒定及波动贮藏下两种模型起酥油样品的热性质及晶型的变化。研究发现，在恒温及温度波动贮藏时，随着贮藏温度的升高，吸热峰的峰温升高，表明，样品中晶体内高熔点甘油三酯含量增加。通过对XRD谱图中β晶型相对强度进行计算得到，在恒温贮藏时，随着时间的延长及温度的升高，起酥油样品中β晶型的含量均逐渐上升。在温度波动贮藏时，随时间延长，其β型晶体含量显著增加，与温度恒定贮藏相比，两种样品在温度波动模式下贮藏时β'晶型向β晶型转变速率明显较快。
三、贮藏过程中棕榈油基起酥油结晶网络结构的变化
采用PLM及SEM对温度恒定及波动贮藏下两种模型起酥油样品的晶体形态、大小及网络结构进行研究，并对温度作用下塑性脂肪结晶网络变化机制进行了推测。结果表明，在恒温贮藏时，随贮藏时间的延长，晶体尺寸逐渐增大，两种起酥油样品的结晶网络中出现部分晶体聚集块，网络的不均匀性增大，在温度≤20°C时，Db值逐渐增大，在温度>20°C时，Db值逐渐减小；随着温度的升高，两种模型起酥油样品的晶体尺寸先增大（0-20°C）后减小（30°C-40°C），这一现象在低熔点起酥油样品中更为明显，同时，两种起酥油样品的Db值逐渐降低，网络坍塌较多。在温度波动贮藏时，两种起酥油样品的在四种波动模式下晶体随着时间的延长逐渐聚集；同时，随着波动温度的升高，Db值逐渐下降。与恒温贮藏相比，温度波动模式对两种样品的结晶网络及晶体尺寸影响更大。
四、贮藏过程中起酥油结晶网络结构与宏观物理性能关系的探讨
对温度恒定及波动贮藏过程中两种模型起酥油的结晶网络结构及宏观物理性能之间关系进行探讨，并建立人工神经网络模型。结果表明，在贮藏过程中，无论恒温还是温度波动贮藏，两种模型起酥油样品的固体脂肪含量、结晶网络结构及β晶型的含量为宏观物理性能变化的重要影响因素。同时，建立了精度较高的人工神经网络模型，该模型可以很好地用于关联及预测类模型起酥油塑性脂肪宏观物理性能及微观结构在贮藏过程中的变化，为高品质塑性脂肪的可控化生产及贮藏提供依据。
With the development of the national economy and food industry, and the rising percapita consumption, as a new type of edible oils and fats for products in the modern foodindustry, a large number of plastic fats with higher product quality are required.The impropertemperature or the fluctuant temperature during storage will induce deterioration in the qualityof plastic fats such as consistency and plasticity, which is related to the change of the internalstructure in plastic fats. Learning the variation of the quality and internal structure of plasticfats has an important guiding role on the production of high-quality plastic fat. Two kinds ofpalm oil-based shortening were employed to explore the effect of storage temperature andtime on the composition, physical properties, thermal characteristics, the structure of crystalnetwork under different storage modes for28days including constant temperatures (0°C,10°C,20°C,30°C,40°C, repectively) and fluctuant temperatures (0°C12h-20°C12h,10°C12h-20°C12h,30°C12h-20°C12h,40°C12h-20°C12h, repectively for a cycle), as wellas their relations. In addition, mathematic model between the microstructure and physicalproperties of palm oil-based shortenings during storage has been further built to proposescientific theory foundation for control administration production and storage of plastic fatswith high quality. The main contents and results of this study were as follows:
(1) The variation of the triglyceride (TAG) composition, solid fat content, texture andrheological properties of two model palm oil-based shortenings during storage
The TAG composition, solid fat content, texture and rheological properties of two modelpalm oil-based shortenings stored at constant and fluctuant temperatures for28days wereanalyzed by pNMR, TA and Hakee rheometer. The results indicated that the TAG compositiondid not change during constant and fluctuant temperature storage. When stored at constanttemperature, as the temperature increased, the solid fat content values of two palm oil-basedshortenings have been found to decrease linearly, the hardness decreased in an exponentialmanner, the elasticity modulus decreased with the rising temperature; with the extension ofthe storage time, the solid fat content values and the elasticity modulus of the two modelshortenings did not change, the hardness increased when the temperature≤20°C anddecreased when the temperature>20°C. When stored at fluctuant temperatures, as the temperature increased, the solid fat content values of two model palm oil-based shorteningswere constant in the temperature range from0°C to20°C and then decreased (30°C-40°C),the hardness decreased when the temperature was higher than10°C, the elasticity modulusdecreased initially when the temperature was lower than10°C and then turned to be stable;with the extension of the storage time, the solid fat content values and the elasticity modulusof the two model shortenings did not change and the hardness decreased in a logarithmicmanner.
(2) The variation of the thermal characteristics and crystal form of two model palmoil-based shortenings during storage
The thermal characteristics and crystal form of two model palm oil-based shorteningsstored at constant and fluctuant temperatures for28days were analyzed by DSC and XRD.When the model shortenings were stored at constant and fluctuant temperatures, the peaktemperature in the melting curves shifted to higher temperature, suggesting higher content ofhigh-melting TAG in the crystals of the two model shortenings. When storing at constanttemperatures, the content of the β form crystal increased with the increasing storagetemperature and time. When the two model shortenings were stored at fluctant temperatures,the content of the β form crystal increased with the extension of the storage time. Comparedwith the constant temperature storage, the β-type crystal conversion rate of the twoshortenings stored at fluctuant temperatures was faster.
(3) The variation of the crystal network structure of two model palm oil-basedshortenings during storage
The crystal morphology, size, and fractal dimensions of the crystal network in the twomodel palm oil-based shortenings stored at constant and fluctuant temperatures for28dayswere analyzed by PLM and SEM, and the mechanisms of the crystal network variation underdifferent temperatures were summarized. When the two model shortenings were stored atconstant temperatures, with the extension of the storage time, the crystal size increased, somecrystal aggregates appeared, resulting in the increasing of the crystal network inhomogeneity,the fractal dimensions Dbincreased when the temperature was higher than20°C anddecreased when the temperature was lower than20°C. When the two model shortenings werestored at fluctuant temperatures, with the extension of the storage time, the different crystal aggregates appeared, and the size of the crystal aggregates increased. Meanwhile, the fractaldimensions Dbof the two model shortenings decreased as the fluctuant temperature increased.Compared with the constant temperature storage, the fluctuant temperature storage showed agreater impact on the crystal network and crystal size.
(4) The relationship between the crystal network structure and macroscopic physicalproperties of the two model palm oil-based shortenings during storage
The relationship between the crystal network structure and macroscopic physicalproperties of the two model palm oil-based shortenings were discussed and the artificialneural network models were built. The results indicated that the solid fat content, the crystalnetwork structure and the content of β form crystalline had an important fluence on themacroscopic physical properties of the model shortenings whether during constanttemperature storage or fluctuant temperature storage. Meanwhile, two artificial neuralnetwork models with a high precision between the crystal network structure and macroscopicphysical properties of the two model palm oil-based shortenings during storage wereestablished, and the models could be used to relate and predict the crystal network structureand macroscopic physical properties of the shortenings.
一、贮藏过程中棕榈油基起酥油的分子组成、固体脂肪含量、质构及流变性能变化
采用HPLC、pNMR、TA和Hakee流变仪分别研究温度恒定及波动贮藏下模型起酥油样品的分子组成、固体脂肪含量、硬度及弹性模量的变化。研究发现，在两种温度作用模式下，两种模型起酥油的分子组成均未发生明显变化。在恒温贮藏时，随贮藏温度的升高，两种起酥油样品的固体脂肪含量呈线性下降，硬度呈指数关系下降，弹性模量逐渐下降；随贮藏时间的延长，二者的固体脂肪含量及弹性模量变化不显著，当温度≤20°C时硬度随时间的延长逐渐变大，当温度>20°C时硬度随时间的延长逐渐变小。在温度波动贮藏时，随波动温度的升高，两种样品的固体脂肪含量呈现先稳定（0°C-20°C）后下降的趋势（30°C-40°C），硬度呈先平稳（0°C-10°C）后降低（30°C-40°C）的趋势，弹性模量呈先下降（0°C-10°C）后趋于稳定（30°C-40°C）；随贮藏时间的延长，二者的固体脂肪含量及弹性模量无显著变化，硬度呈对数下降。
二、贮藏过程中棕榈油基起酥油的热性质及晶型的变化
采用DSC和XRD方法分别研究温度恒定及波动贮藏下两种模型起酥油样品的热性质及晶型的变化。研究发现，在恒温及温度波动贮藏时，随着贮藏温度的升高，吸热峰的峰温升高，表明，样品中晶体内高熔点甘油三酯含量增加。通过对XRD谱图中β晶型相对强度进行计算得到，在恒温贮藏时，随着时间的延长及温度的升高，起酥油样品中β晶型的含量均逐渐上升。在温度波动贮藏时，随时间延长，其β型晶体含量显著增加，与温度恒定贮藏相比，两种样品在温度波动模式下贮藏时β'晶型向β晶型转变速率明显较快。
三、贮藏过程中棕榈油基起酥油结晶网络结构的变化
采用PLM及SEM对温度恒定及波动贮藏下两种模型起酥油样品的晶体形态、大小及网络结构进行研究，并对温度作用下塑性脂肪结晶网络变化机制进行了推测。结果表明，在恒温贮藏时，随贮藏时间的延长，晶体尺寸逐渐增大，两种起酥油样品的结晶网络中出现部分晶体聚集块，网络的不均匀性增大，在温度≤20°C时，Db值逐渐增大，在温度>20°C时，Db值逐渐减小；随着温度的升高，两种模型起酥油样品的晶体尺寸先增大（0-20°C）后减小（30°C-40°C），这一现象在低熔点起酥油样品中更为明显，同时，两种起酥油样品的Db值逐渐降低，网络坍塌较多。在温度波动贮藏时，两种起酥油样品的在四种波动模式下晶体随着时间的延长逐渐聚集；同时，随着波动温度的升高，Db值逐渐下降。与恒温贮藏相比，温度波动模式对两种样品的结晶网络及晶体尺寸影响更大。
四、贮藏过程中起酥油结晶网络结构与宏观物理性能关系的探讨
对温度恒定及波动贮藏过程中两种模型起酥油的结晶网络结构及宏观物理性能之间关系进行探讨，并建立人工神经网络模型。结果表明，在贮藏过程中，无论恒温还是温度波动贮藏，两种模型起酥油样品的固体脂肪含量、结晶网络结构及β晶型的含量为宏观物理性能变化的重要影响因素。同时，建立了精度较高的人工神经网络模型，该模型可以很好地用于关联及预测类模型起酥油塑性脂肪宏观物理性能及微观结构在贮藏过程中的变化，为高品质塑性脂肪的可控化生产及贮藏提供依据。
With the development of the national economy and food industry, and the rising percapita consumption, as a new type of edible oils and fats for products in the modern foodindustry, a large number of plastic fats with higher product quality are required.The impropertemperature or the fluctuant temperature during storage will induce deterioration in the qualityof plastic fats such as consistency and plasticity, which is related to the change of the internalstructure in plastic fats. Learning the variation of the quality and internal structure of plasticfats has an important guiding role on the production of high-quality plastic fat. Two kinds ofpalm oil-based shortening were employed to explore the effect of storage temperature andtime on the composition, physical properties, thermal characteristics, the structure of crystalnetwork under different storage modes for28days including constant temperatures (0°C,10°C,20°C,30°C,40°C, repectively) and fluctuant temperatures (0°C12h-20°C12h,10°C12h-20°C12h,30°C12h-20°C12h,40°C12h-20°C12h, repectively for a cycle), as wellas their relations. In addition, mathematic model between the microstructure and physicalproperties of palm oil-based shortenings during storage has been further built to proposescientific theory foundation for control administration production and storage of plastic fatswith high quality. The main contents and results of this study were as follows:
(1) The variation of the triglyceride (TAG) composition, solid fat content, texture andrheological properties of two model palm oil-based shortenings during storage
The TAG composition, solid fat content, texture and rheological properties of two modelpalm oil-based shortenings stored at constant and fluctuant temperatures for28days wereanalyzed by pNMR, TA and Hakee rheometer. The results indicated that the TAG compositiondid not change during constant and fluctuant temperature storage. When stored at constanttemperature, as the temperature increased, the solid fat content values of two palm oil-basedshortenings have been found to decrease linearly, the hardness decreased in an exponentialmanner, the elasticity modulus decreased with the rising temperature; with the extension ofthe storage time, the solid fat content values and the elasticity modulus of the two modelshortenings did not change, the hardness increased when the temperature≤20°C anddecreased when the temperature>20°C. When stored at fluctuant temperatures, as the temperature increased, the solid fat content values of two model palm oil-based shorteningswere constant in the temperature range from0°C to20°C and then decreased (30°C-40°C),the hardness decreased when the temperature was higher than10°C, the elasticity modulusdecreased initially when the temperature was lower than10°C and then turned to be stable;with the extension of the storage time, the solid fat content values and the elasticity modulusof the two model shortenings did not change and the hardness decreased in a logarithmicmanner.
(2) The variation of the thermal characteristics and crystal form of two model palmoil-based shortenings during storage
The thermal characteristics and crystal form of two model palm oil-based shorteningsstored at constant and fluctuant temperatures for28days were analyzed by DSC and XRD.When the model shortenings were stored at constant and fluctuant temperatures, the peaktemperature in the melting curves shifted to higher temperature, suggesting higher content ofhigh-melting TAG in the crystals of the two model shortenings. When storing at constanttemperatures, the content of the β form crystal increased with the increasing storagetemperature and time. When the two model shortenings were stored at fluctant temperatures,the content of the β form crystal increased with the extension of the storage time. Comparedwith the constant temperature storage, the β-type crystal conversion rate of the twoshortenings stored at fluctuant temperatures was faster.
(3) The variation of the crystal network structure of two model palm oil-basedshortenings during storage
The crystal morphology, size, and fractal dimensions of the crystal network in the twomodel palm oil-based shortenings stored at constant and fluctuant temperatures for28dayswere analyzed by PLM and SEM, and the mechanisms of the crystal network variation underdifferent temperatures were summarized. When the two model shortenings were stored atconstant temperatures, with the extension of the storage time, the crystal size increased, somecrystal aggregates appeared, resulting in the increasing of the crystal network inhomogeneity,the fractal dimensions Dbincreased when the temperature was higher than20°C anddecreased when the temperature was lower than20°C. When the two model shortenings werestored at fluctuant temperatures, with the extension of the storage time, the different crystal aggregates appeared, and the size of the crystal aggregates increased. Meanwhile, the fractaldimensions Dbof the two model shortenings decreased as the fluctuant temperature increased.Compared with the constant temperature storage, the fluctuant temperature storage showed agreater impact on the crystal network and crystal size.
(4) The relationship between the crystal network structure and macroscopic physicalproperties of the two model palm oil-based shortenings during storage
The relationship between the crystal network structure and macroscopic physicalproperties of the two model palm oil-based shortenings were discussed and the artificialneural network models were built. The results indicated that the solid fat content, the crystalnetwork structure and the content of β form crystalline had an important fluence on themacroscopic physical properties of the model shortenings whether during constanttemperature storage or fluctuant temperature storage. Meanwhile, two artificial neuralnetwork models with a high precision between the crystal network structure and macroscopicphysical properties of the two model palm oil-based shortenings during storage wereestablished, and the models could be used to relate and predict the crystal network structureand macroscopic physical properties of the shortenings.
引文
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