摘要
利用微波为热源加工淀粉质食品或复热主食符合新型物理场技术发展的趋势，淀粉的结构、组成和聚集形态非常复杂，目前，针对淀粉质物料及其食品在微波场下响应行为的研究多停留在糊化应用层面。然而，微波加热的效果取决于物料的电磁性质，这方面研究的缺乏阻碍了对微波场中淀粉结构变化过程的认知，无法客观评价微波加热的安全性，限制了微波技术在淀粉质食品领域的应用。本文选取性状稳定的大米淀粉为研究对象，基于微波加热过程的作用机理，首先考察大米淀粉的基本电磁特性，确定物料在微波场下的损耗机制，建立和评价可对照的加热模型，研究微波对大米淀粉介电性质及吸波性能的影响，在此基础上，系统考察微波对淀粉各级结构、形态、热物性和水分布的影响，明确微波对淀粉质物料作用的主要机制，并开展大米淀粉质食品微波复热过程的温度分布规律以及传热模型的研究。论文的主要研究内容包括：
（1）大米淀粉的制备及其电磁响应特性的研究
以基本成分、糊化特性、颗粒形态和粒度分布为指标，比较碱法、碱性蛋白酶法和中性蛋白酶法对大米淀粉提取效果的影响，确定最优制备工艺，并对其开展电性能和磁性能的测试和表征，确立损耗类型，考察其水相体系的吸波性能。研究发现：中性蛋白酶法对淀粉颗粒有较小的破坏作用；干燥状态下，原淀粉和完全糊化淀粉的复介电常数实部（ε′）为2.7±0.1，虚部（ε″）处于0～0.2范围内，介电损耗角正切值（tanδε）均小于0.1，属于较弱的微波吸收材料；复磁导率的实部（μ′）为1.00±0.10，虚部（μ″）和磁损耗角正切值（tanδμ）均为0.19±0.02，表现为极弱的磁感应；传输线理论适用于液态混合物料的吸波特性的测试，试验结果与介质体系中电磁波波长的共振模型相匹配；淀粉乳的ε′随淀粉浓度的升高而下降，并呈现一维线性关系；ε″随其浓度的升高变化较小；2.45GHz频率下，原淀粉浓度从1％增加至30％，反射损耗从-5.1dB降至-1.2dB，电磁波吸收率从69.1％降至24.1％；原淀粉显著干预水在混合体系中的微波吸收作用，糊化后的淀粉对混合体系的微波吸收特性影响较小，预糊化淀粉乳的吸波特性由水主导。
（2）微波加热对大米淀粉介电及吸波性能的影响
基于微波加热与传导加热过程的升温规律，以快速传导加热为基准，建立与之匹配的微波加热模型，并以传统慢速加热为对照。研究微波加热过程对淀粉介电性质的影响，探讨基于体系复介电常数的Debye极化机制的干预，探讨体系吸波行为的消长。研究发现：微波加热促进淀粉乳在低温条件下产生重排，使体系表现出较为稳定的介电响应；微波加热后的样品表现出较为突出的介电特性，在45～65℃加热区间，ε′、ε″和tanδε值均高于快速和慢速传导方法；微波加热对淀粉乳的Cole-Cole简化曲线产生显著影响，表现为2.45±0.05GHz区间曲线规律显著区别于其它两种方法；微波加热改变了淀粉乳原有的极化规律，促使样品在±0.01GHz范围内，以2.45GHz为中心呈现明显转折，产生了双重极化现象；微波加热使淀粉乳的吸波性能在糊化温度以前呈现小幅降低，80℃后与传导加热趋于一致；虽然微波在低温过程就改变了物料在2.45GHz频率附近的极化特性，使物料的极化过程增加，但处理后物料的宏观微波吸收性能并未增强，与之相反，伴随升温过程表现出一定的阻碍效应。
（3）微波加热对大米淀粉结构特性的影响
采用傅里叶变换红外光谱（FTIR）、激光共聚焦显微拉曼光谱（FT Raman）、碳谱魔角旋转核磁共振（13C CP/MAS NMR）、广角X射线衍射（XRD）、小角X射线散射（SAXS）等技术，逐级研究微波加热对大米淀粉的分子结构、相对结晶度以及半结晶生长环层状结构等的影响。FTIR显示，微波加热不会在淀粉中形成新的化学键及化学基团，无序和有序结构的振动强度变化规律略有影响；FT Raman显示，微波对快速升温过程中骨架上C-H基团振动在糊化温度附近的增加起到抑制作用，微波加热对淀粉分子中如糖苷键、吡喃环等其他的骨架模式和C-O、C-O-H等其他骨架基团的振动强度没有明显影响；13C CP/MAS NMR显示，微波的快速加热效应是淀粉颗粒内的无定形态、双螺旋结构及V型单螺旋结构含量差异性的决定因素，微波对淀粉颗粒内部有序结构的影响不显著；XRD显示，微波的快速加热效应导致淀粉在低于糊化温度的范围结晶度降低；SAXS显示，微波的快速加热效应促使支链淀粉分子的双螺旋结构更加有序紧密地排列在结晶层，无定形层受到压缩；非热效应引起层状结构的不规律交替，并且对其快速升温界面层的破坏作用产生阻碍，高于60℃时，微波的非热效应则加速淀粉半结晶生长环层状结构的破坏。
（4）微波加热对大米淀粉形态、热物性及水状态的影响
采用粒径分布、偏光显微镜、扫描电子显微镜（SEM）、示差扫描量热仪（DSC）、热重分析仪（TG）、低场核磁共振仪（1H NMR）等手段，研究微波加热对大米淀粉偏光十字及颗粒形态的破坏，考察对淀粉活化能和热焓值的影响，采用IR和CPMG脉冲序列和反演得到的T1和T2探索对淀粉颗粒内部水分分布及动态的干预。研究发现：微波的快速加热效应是淀粉偏光十字消失及颗粒形态改变的主要原因，微波不会促使淀粉出现偏光十字消失与颗粒膨胀的异步性，不会影响支链淀粉的放射状组织结构产生的影像学效应；微波的快速加热效应促使活化能在50℃出现明显峰值，使热焓值
随着温度的升高呈现先升高再降低的趋势,较慢速加热处理显著不同,表明微波对糊化前淀粉热稳定性的影响主要取决于微波的快速升温作用；微波加热对淀粉颗粒内部水分分布及动态过程产生影响,快速加热效应抑制了淀粉分子之间和淀粉与水之间氢键的破坏作用,而微波的非热效应则加速了氢键的破坏。
(5)大米淀粉质食品微波复热温度分布规律以及传热模型的研究
开展米饭成分以及与微波加热有关的物性参数和介电特性的研究,以圆柱型物料为考察形态,探讨样品自身特征对微波复热过程温度分布规律的影响,通过对加热均匀性进行分析,选取最优的米饭尺寸,并根据能量守衡定律、傅里叶方程等传热理论构建圆柱型米饭微波复热的传热模型,采用朗伯定律计算微波吸收功率,结合符合米饭特性的初值和边界条件,根据数值算法有限差分法(FDM)处理数学模型,运用计算机软件MATLAB进行编程,实现数值预测米饭微波加热过程中的温度分布规律。研究发现：温度对米饭的比热和介电损耗影响显著,对导热系数和介电常数影响较小；用温度的二次多项式可以很好的反映米饭介电损耗的变化规律(R2=0.9785),导热系数在温度4～80℃时可取平均值0.760W/(m·℃)；在相同温度下,频率为0.915GHz时米饭的介电常数大于频率为2.45GHz时的介电常数,介电损耗因数则相反；圆柱形米饭温度分布规律揭示：样品在轴向上温度对称分布且随高度/直径比的增大出现边角和表面加热趋势；高度直径比(L/D)对样品内部温度分布规律影响显著；采用基于标准偏差的温度变化系数(COV)作为温度均匀性的评价方法,得到L/D和半径对于COV的变化关系,确定了微波加热均匀性最好的圆柱型米饭(半径4cm,高度4cm)；预测模型的拟合度较高(R2在0.996和0.999之间)。
微波对淀粉及淀粉乳产生的影响贯穿于整个处理过程；微波的非热效应仅限于对淀粉的分子极化机制、骨架间紧密度和层状结构水分分布等微观层面产生干预；微波的快速加热效应是决定淀粉宏观物理化学特性显著差异的主要因素；淀粉质食品的微波加热过程可根据物料的热物性和介电特征进行模型描述。
The application of microwave for heat processing or reheating of starchy food fits the current trend ofthe development of new technology of physical field. As a carbohydrate polymer, the structure,composition, and morphology of starch are very complex. Up to now the research on starchy materials andfoods in the microwave field mainly focus on the behavior related to gelatinization and its application, andthe lack of research on the influence of electromagnetic properties on the microwave heating effectfundamentally hinder the cognition of the structural change of starch in the microwave field, fail to makeobjective safety evaluation, and limit the development of microwave technology in the field of starchy food.In this study we selected stable rice starch as the object, examined the fundamental electromagneticproperties of the rice starch based on the mechanism of the microwave heating process, determined the lossmechanism of the material in the microwave field, established and evaluated the control heating model,investigated the effect of microwave on dielectric properties and absorbing properties of rice starch.Moreover, we investigated the effect of microwave on the structure, morphology, thermal properties andwater distribution of starch at all levels, elucidated the major mechanism of microwave on starchy material,and conducted research on the temperature distribution and heat transfer model of rice starchy foods duringthe microwave reheating process. The major results of the current study are as follows:
（1）Preparation of rice starch and electromagnetic response characteristics
With the basic components, pasting properties, particle morphology and particle size distribution asindicators, the effect of alkaline, alcalase and neutrase on the extraction of rice starch was investigated todetermine the optimal preparation process, and the electrical properties and the magnetic properties wereexamined to establish the loss type and inspect the absorbing properties of the water system. The resultsshowed that neutrase had minor influence on the starch granule. In the dry state, for the complexpermittivity of both the native and completely gelatinized starch, ε′was2.7±0.1, and ε″lied in the range of0～0.2, with tanδε below0.1, indicating that starch is a weak absorbing material in microwave. For thecomplex permeability, μ′was1.00±0.10，and μ″and tanδμ were both0.19±0.02，showing weak magneticinduction. Transmission line theory is suitable for the examination of absorbing characteristics of complexliquid materials, and the results matched the resonance model of the electromagnetic wavelength. The ε′ofthe starch emulsion decreased with the increase of the concentration with linear relationship, and ε″showedlittle change with the increase of the concentration. Under2.45GHz, when the concentration of the nativestarch increased from1%to30%, the reflection loss decreased from-5.1dB to-1.2dB，and theelectromagnetic absorbability decreased from69.1％to24.1％. Native starch significantly interfere withthe microwave absorbing characteristics of water in the mixed system, and the gelatinized starch showedlittle influence on the microwave absorbing characteristics, whereas water dominated the microwaveabsorbing characteristics of the pre-gelatinized starch system.
（2）Effect of microwave heating on the dielectric and absorbing properties of rice starch
Based on the heating law of the microwave and the conduction heating, the microwave heating modelwas established with the slow heating conduction as the control. The effect of the microwave heatingprocess on starch, the intervention based on the Debye polarization mechanism of the complex permittivityof the system, and the absorbing behavior of the system were investigated. The results showed thatmicrowave heating promoted the rearrangement of the starch emulsion under the low temperatureconditions, so that the system exhibited a relatively stable dielectric response. After microwave heating thesamples showed prominent dielectric characteristics, and ε ', ε "and tanδε values were higher than those atthe rapid and slow conduction methods in the heating range of45~65℃. Microwave heating processshowed significant influence on the simplified Cole-Cole plot curves of starch emulsion with a significantvariation of the curves from those of the other two methods at2.45±0.05GHz. The microwave heatedsample changed the original polarization law at2.45GHz±0.01GHz, and showed a dual polarizationphenomenon. Microwave processing of starch showed a slight decrease in the absorbing performancebefore gelatinization temperature, which was in line with the conduction heating process afterwards.Although microwave processing at low temperature changed the polarization characteristics of the materialin the vicinity of the frequency of2.45GHz, after processing the microwave absorption characteristics ofthe material were not enhanced.
（3）Effect of microwave heating on structural characteristics of rice starch
The FTIR, InVia Reflex Raman microscope sys-tem,13C CP/MAS NMR, wide-angle and smallangle X-ray diffraction techniques were applied to investigate the effect of microwave heating process onthe molecular structure such as molecule structure, the relative degree of crystallinity, the ordered structureand disordered structure contents of rice starch. The FTIR results showed that microwave heating does notproduce new chemical bonds and the chemical group in starch, and the vibration energy of the disorderedand ordered structure slight changed, indicating the rapid heating effect was the major factor for thechanges in the chemical bonds in starch under microwave. The Raman spectroscopy showed an inhibitoryeffect of microwave on the increase in the skeleton of the CH group vibration near the gelatinization temperature during the rapid heating process, and microwave heating of starch molecules showed nosignificant effect on the vibration intensity of the glycosidic linkage, pyranose ring, and-C-O, C-O-Hgroups on the skeleton. The results of13C CP/MAS NMR showed that the rapid heating effect ofmicrowave is the major factor for the differences in the amorphous starch granules, double-helix structureand V-type single helix structure contents, and the effect of microwave on the ordered internal structure ofstarch granules was not significantly. Small angle X-ray diffraction indicated that the rapid heating effect ofthe microwave resulted in tighter arrangement of the double helix structure of the amylopectin molecules inthe crystalline layer and compression of the amorphous layer. Electromagnetic effect is obviously resultedin irregular alternation of the layered structure, and destructive effects on the rapid heating. When thetemperature was above60°C，the molecular vibration mechanism of microwave accelerated the destructionof the lamellar repeats architecture of starch. The results of the wide angle X-ray diffraction showed thatthe rapid heating effect of microwave caused the decrease of the degree of crystallinity of starch below thegelatinization temperature.
（4） Effect of microwave heating on the morphology, thermal properties and water status of ricestarch
The particle size distribution, polarizing microscope, SEM, TG, DSC, the1H NMR were applied tostudy the destruction of birefringence and granule morphology of rice starch by microwave, and theinfluence on the activation energy and enthalpy. The IR and CPMG results indicated that the rapid heatingeffect is the main reason for the disappearance of birefringence and change in granule morphology, andmicrowave did not procure the asynchronous nature of the disappearance of birefringence and change ingranule morphology, and did not affect the imaging effect of the radial arrangement of amylopectin chains.The rapid heating effect of the microwave prompted the apparent peak of activation energy at50℃, andthe rapid heating effect of the microwave resulted in the enthalpy value first increased and then decreasedwith the increases of the temperature, different from the slow heating treatment, indicating that the effect ofmicrowave on thermal stability of the pre-gelatinized starch mainly depended on the rapid heating effect ofthe microwave. Microwave heating affected the internal water distribution and dynamics of starch granules,and the rapid heating effects limited the damaging effects of hydrogen bonds between starch molecules andstarch with water. However the molecular vibration mechanism of microwave accelerated the destructionof the hydrogen bonds, and the vibration mechanism showed stronger effect then the rapid heating effect.
（5）Temperature distribution and heat transfer model of rice starchy food under microwave reheating
The physical parameters and dielectric properties of rice components under microwave heating wasinspected with cylindrical material, and the influence of the sample features on the temperature distributionin the microwave reheating process was investigated through the heating uniformity analysis. The optimalsize of the rice was selected, and the heat transfer model was built according to the law of conservation ofenergy, the Fourier equation. Lambert law was used to calculate the microwave absorption power, togetherwith the initial and boundary conditions of the rice and the finite difference method (FDM) numericalalgorithm, MATLAB was applied for the numerical prediction of the temperature distribution in rice undermicrowave heating process. The results showed that temperature showed a significant impact on thespecific heat and dielectric loss on rice, with little effect on the thermal conductivity and the dielectricconstant. Polynomials can show a good reflection on the variation of the rice dielectric loss withtemperature（R2=0.9785），and the thermal conductivity averaged at0.760W/(m℃) in the range of4~80℃.At the same temperature, the rice permittivity is greater at a frequency of0.915GHz than at the frequencyof2.45GHz, whereas the dielectric loss factor is the opposite. The temperature distribution pattern ofcylindrical rice revealed that temperature distribution of the sample in the axial direction distributedsymmetrically, showing increased corner and surface heating trend with the increase in the height/diameter ratio, and L/D had a significant impact on the internal temperature distribution of the sample.With the temperature coefficient of variation (COV) as the evaluation indicator of the temperatureuniformity of, the L/D and the radius for the COV was obtained to determine the optimal cylindrical-typerice with uniformity of microwave heating (a radius of4cm, height4cm), with high fitness of thepredictive model（R2between0.996and0.999）.
Microwave showed impact on starch and starch emulsion throughout the entire process. Themicrowave electromagnetic effects were only limited in molecule polarization mechanism, skeletontightness, and water distribution of the layered structure at the micro level intervention. Rapid microwaveheating effect was the principal factors for macro differences in physical and chemical properties of starch.The microwave heating process of starchy foods can be described based on the thermal properties and thedielectric characteristics of the material.
引文
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