本文選題：葡萄糖酸內(nèi)酯 + 魚糜凝膠　； 參考：《江南大學(xué)》2017年博士論文

【摘要】：近年來,隨著科技的進(jìn)步以及經(jīng)濟(jì)的快速增長,人們對(duì)社會(huì)的需求逐漸增加,食品加工行業(yè)的高度工業(yè)化水平不斷提升。三維打印技術(shù)是基于增材制造法原理的一種高新技術(shù),是快速成型技術(shù)的延續(xù)與發(fā)展,其以制造技術(shù)和信息技術(shù)深度融合為特征的現(xiàn)代智能制造模式,為我國食品加工行業(yè)的發(fā)展提供了不同于傳統(tǒng)制造技術(shù)的新思路。打印材料是三維打印技術(shù)發(fā)展的重要基礎(chǔ),也是制約三維打印技術(shù)獲得廣泛應(yīng)用的瓶頸。對(duì)于廣泛應(yīng)用于食品加工領(lǐng)域的擠壓式三維打印技術(shù),其對(duì)食品物料有著準(zhǔn)確嚴(yán)格的要求:應(yīng)具備一定的流動(dòng)性、成型性,并具有合格的物理、化學(xué)性質(zhì)。魚糜凝膠體系具有一定的凝膠強(qiáng)度、黏度和流變特性,因此本論文以葡萄糖酸內(nèi)酯(GDL)誘導(dǎo)形成的魚糜凝膠體系為擠壓式三維打印食品材料,通過輔料添加改善凝膠體系的力學(xué)特性以適用于三維打印技術(shù)。在此基礎(chǔ)之上,研究擠壓式三維打印工藝參數(shù)對(duì)魚糜凝膠體系打印品質(zhì)及精度的影響。并進(jìn)一步研究貯藏條件對(duì)魚糜打印特性的影響,探究貯藏過程中脂肪過氧化產(chǎn)物對(duì)魚糜凝膠打印效果的影響,探究魚糜肌原纖維蛋白氧化聚形成的內(nèi)在機(jī)制。以期深入闡明加工及貯藏過程中食品物料結(jié)構(gòu)狀態(tài)、打印特性與打印工藝三者之間的關(guān)系。本研究對(duì)于了解肉制品凝膠體系在擠壓式三維打印技術(shù)中的應(yīng)用奠定了理論依據(jù)和實(shí)際運(yùn)用基礎(chǔ)。首先初步研究了葡萄糖酸內(nèi)酯(GDL)誘導(dǎo)鰱魚糜凝膠體系的形成過程。通過分析不同GDL濃度對(duì)魚糜凝膠的持水性、質(zhì)構(gòu)特性及水分分布的影響。進(jìn)一步通過GDL作用于魚肉肌原纖維蛋白(MP),研究GDL誘導(dǎo)魚糜凝膠化過程中分子間作用力的變化。結(jié)果表明,促進(jìn)魚糜凝膠體系建立的GDL最佳濃度為1.5%。在此條件下,魚糜凝膠化4 h內(nèi),魚糜pH值快速降至4.5左右。GDL可改變魚肉蛋白結(jié)構(gòu)。隨著GDL濃度的增加,蛋白結(jié)構(gòu)展開,α-螺旋轉(zhuǎn)化為β-折疊或無規(guī)則卷曲,疏水基團(tuán)外露促進(jìn)蛋白發(fā)生交聯(lián)形成凝膠,凝膠強(qiáng)度及持水性提高。而過量的GDL添加反而會(huì)降低魚糜凝膠的凝膠特性,導(dǎo)致凝膠劣化。低濃度的GDL誘導(dǎo)肌原纖維蛋白凝膠形成的作用力主要是疏水作用和共價(jià)二硫鍵,而當(dāng)GDL濃度進(jìn)一步增加時(shí),出現(xiàn)疏水作用降低的現(xiàn)象。通過添加NaCl和固體脂肪改善魚糜凝膠體系的松弛應(yīng)力、蠕變特性、表觀粘度以及動(dòng)態(tài)學(xué)流變等打印特性,以期得到可用于三維打印的魚糜凝膠體系。結(jié)果表明NaCl添加能夠顯著提高魚糜凝膠的松弛應(yīng)力、蠕變特性及動(dòng)態(tài)學(xué)流變特性,有利于提高打印線條的抗壓力,改善魚糜凝膠的成型性,同時(shí)表觀粘度的提高也有利于擠壓式三維打印出料系統(tǒng)供料順暢。10.0%的脂肪能夠顯著提高魚糜凝膠的松弛應(yīng)力、蠕變特性及動(dòng)態(tài)流變學(xué)特性,但表觀粘度呈逐漸下降的趨勢。當(dāng)加入過量的脂肪,魚糜凝膠體系的粘度降低,不利于打印系統(tǒng)出料,并且打印完成后,樣品結(jié)構(gòu)容易塌陷變形。通過工藝參數(shù)試驗(yàn)研究了層高值、打印速率、噴嘴直徑、出料速率及打印溫度等參數(shù)對(duì)擠出成型質(zhì)量的影響,并確定了關(guān)鍵工藝參數(shù)之間的相互制約關(guān)系。結(jié)果表明:層高值1.5 mm、打印高度5.0 mm,噴嘴直徑2.0 mm、打印速率28 mm/s、打印溫度45°C以及出料速率0.003 cm3/s條件下,打印魚糜凝膠樣品的成型質(zhì)量較好,成型件表面光滑沒有突起,層層之間結(jié)合較為緊密,沒有缺口,搭接的量較少。其中,出料速率Vd、打印速率Vn與噴嘴直徑Dn三個(gè)打印參數(shù)之間存在著一定的制約關(guān)系,因此在打印過程中應(yīng)綜合調(diào)控這三個(gè)參數(shù),以提高打印精度。另外,對(duì)三維打印螺桿擠壓出料的過程中螺桿轉(zhuǎn)速與打印速率的關(guān)系進(jìn)行建模及數(shù)值分析,并設(shè)計(jì)簡單打印模型驗(yàn)證數(shù)值分析的結(jié)果。結(jié)果顯示利用此模型,螺桿轉(zhuǎn)速與打印速率更加匹配,擠出物料過程的穩(wěn)定性顯著提高,減少了打印誤差,有效的提高了打印精度�？疾炝唆~糜在不同貯藏溫度下脂肪氧化、蛋白氧化、魚糜持水性、凝膠強(qiáng)度及三維打印相關(guān)特性的變化規(guī)律,結(jié)果表明隨著貯藏時(shí)間的延長,魚糜肌肉蛋白氧化增加和脂肪氧化加速,整體新鮮度會(huì)下降。同時(shí)持水性、凝膠強(qiáng)度、凝膠彈性、松弛應(yīng)力、蠕變特性及表觀粘度顯著性降低。三種貯藏溫度下,各指標(biāo)整體變化趨勢相似,而在相對(duì)較高溫度下較長時(shí)間貯藏,會(huì)加速氧化劣變的發(fā)生,脂肪氧化與蛋白氧化具有一定的相關(guān)性,脂肪氧化能夠促進(jìn)蛋白氧化的發(fā)生。另外,建立基于整體穩(wěn)定性指數(shù)法(GSI)預(yù)測不同溫度貯藏下魚糜凝膠的蛋白氧化程度及打印特性變化的數(shù)學(xué)模型,GSI=1-5.6161texp(-20.9159/RT),該模型能夠準(zhǔn)確有效地預(yù)測貯藏鰱魚糜解凍后的基本品質(zhì)及三維打印特性的變化規(guī)律。建立亞油酸(OLA)與丙二醛(MDA)脂質(zhì)過氧化物氧化體系并作用于魚糜凝膠,通過對(duì)肌原纖維蛋白結(jié)構(gòu)變化的影響及促進(jìn)肌原纖維蛋白氧化程度的研究,闡明貯藏過程中脂肪氧化對(duì)魚糜凝膠打印效果的影響機(jī)制。并以MDA作用于肌原纖維蛋白,通過測定蛋白凝膠強(qiáng)度、持水力、水分狀態(tài)及微觀結(jié)構(gòu)等研究蛋白氧化聚集形成凝膠的過程。研究表明脂質(zhì)過氧化物OLA和和MDA可提高魚糜的表觀粘度、屈服應(yīng)力以及動(dòng)態(tài)流變特性,表現(xiàn)了一定的凝膠黏彈特性,從而促進(jìn)魚糜漿料順利出料,減小出絲斷條的幾率。MDA誘導(dǎo)蛋白凝膠化的效果要明顯高于OLA體系,當(dāng)MDA濃度達(dá)到0.03%時(shí),魚糜在短時(shí)間內(nèi)就可表現(xiàn)出固態(tài)特性,在料斗剪切進(jìn)料時(shí)發(fā)生凝膠大分子聚集,并且提高剪切速度仍無法使?jié){料均勻進(jìn)料,在螺桿縫隙極易出現(xiàn)堵塞的現(xiàn)象,導(dǎo)致打印無法正常進(jìn)行。OLA和和MDA引起了肌原纖維蛋白的結(jié)構(gòu)變化,即蛋白溶解度下降,蛋白羰基值、表面疏水性呈先增加后緩慢下降的趨勢,肌原纖維蛋白內(nèi)源熒光強(qiáng)度下降并且出峰位置發(fā)生藍(lán)移。NMR結(jié)果顯示MDA作用于魚肉肌原纖維蛋白可促進(jìn)蛋白結(jié)構(gòu)舒展,隨著MDA濃度的增大,MDA-MP形成剛性的凝膠結(jié)構(gòu),蛋白中不易流動(dòng)水發(fā)生藍(lán)移,自由水比例降低。加熱作用結(jié)合適量的共價(jià)鍵有利于加固凝膠結(jié)構(gòu),使得多余的自由水排除在凝膠結(jié)構(gòu)之外。
[Abstract]:In recent years, with the progress of science and technology and the rapid growth of economy, the demand for society is increasing gradually. The high level of industrialization in the food processing industry is increasing. The three-dimensional printing technology is a new and high technology based on the principle of material increasing manufacturing. It is the continuation and development of rapid prototyping technology, and its manufacturing technology and information technology are deep. The modern intelligent manufacturing mode characterized by degree fusion provides a new idea different from the traditional manufacturing technology for the development of the food processing industry in China. Printing material is an important basis for the development of 3D printing technology, and also a bottleneck restricting the wide application of three-dimensional printing technology. For the extrusion type three widely used in the field of food processing. It has a precise and strict requirement for food materials: it should have certain fluidity, formability and qualified physical and chemical properties. The gelatin gel system has a certain gel strength, viscosity and rheological properties. Therefore, the gelatin gel system induced by gluconate (GDL) in this paper is a three dimensional extrusion. To print the food materials, the mechanical properties of the gel system were added to improve the mechanical properties of the gel system to apply to the three-dimensional printing technology. On this basis, the influence of the extrusion parameters on the printing quality and precision of the surimi gel system was studied. The effects of storage conditions on the printing characteristics of the surimi were further studied and the fat in the storage process was explored. The effect of peroxide products on the printing effect of surimi gel, and to explore the internal mechanism of the formation of the oxidative polymerization of myofibrillar protein of surimi, in order to clarify the relationship between the structure state of the food materials and the relationship between the printing characteristics and the printing process in the process of processing and storage. This study is to understand the three-dimensional printing technique of the meat gel system in the extrusion type. The application in the operation laid a theoretical basis and practical basis. First, the formation process of gluconate (GDL) induced silver carp surimi gel system was first studied. The effects of different GDL concentrations on the water holding, texture and water distribution of the surimi gel were analyzed. The effect of GDL on fish myofibrillar protein (MP) was further studied. GDL induced changes in the intermolecular force during the gelation of fish surimi. The results showed that the optimum concentration of GDL to promote the surimi gel system was 1.5%. under this condition. The gelation of surimi was 4 h, and the pH value of surimi decreased rapidly to about 4.5.GDL to change the structure of fish protein. With the increase of GDL concentration, the structure of protein was expanded and the alpha helix was transformed into beta. Folding or irregular curling, hydrophobic group exposure promotes protein crosslinking to form gelatin, gel strength and water holding capacity increases. But excessive GDL addition can reduce gel properties of surimi gel and lead to gel deterioration. Low concentration of GDL induced myofibrillar gel formation force is mainly hydrophobic and covalent two sulfur bond, When the concentration of GDL is further increased, the hydrophobicity is reduced. By adding NaCl and solid fat to improve the relaxation stress, creep property, apparent viscosity and dynamic rheological properties of the surimi gel system, it is expected that the fish chyle gel system can be used for three-dimensional printing. The results show that the addition of NaCl can improve the fish significantly. The relaxation stress, creep properties and dynamic rheological properties of the chygels are beneficial to improve the pressure resistance of the printing lines and improve the formability of the surimi gel. At the same time, the increase of apparent viscosity is also beneficial to the smooth.10.0% fat of the extruded three dimensional printing and discharging system, which can significantly raise the relaxation stress, creep properties and dynamics of the fish surimi gel. The rheological properties, but the apparent viscosity decreases gradually. When the excess fat is added, the viscosity of the surimi gel system decreases, which is not conducive to the printing of the system. After the printing is completed, the structure of the sample is easily collapsed and deformed. Through the process parameter test, the layer height, the printing rate, the nozzle diameter, the feed rate and printing temperature are studied. The influence of the number on the quality of the extrusion molding was determined and the interaction between the key technological parameters was determined. The results showed that the molding quality of the printed surimi gel samples was better and the surface light of the molded parts was better under the conditions of the height of 1.5 mm, the printing height of 5 mm, the diameter of the nozzle 2 mm, the printing rate 28 mm/s, the printing temperature 45 degree C and the feed rate 0.003 cm3/s. There is no protruding, there is no gap between the layers, there is no gap, and the amount of lap joint is less. Among them, there is a certain restriction relationship between the feeding rate Vd, the printing rate Vn and the three printing parameters of the nozzle diameter Dn. Therefore, in the printing process, the three parameters should be adjusted to improve the printing precision. In addition, the three-dimensional printing screw extruder is used. The relationship between the screw speed and the printing rate is modeled and analyzed, and a simple printing model is designed to verify the results of the numerical analysis. The results show that the screw speed is more matched with the printing rate, the stability of the extrusion material process is greatly improved, the printing error is reduced, and the printing precision is effectively improved. The changes in lipid oxidation, protein oxidation, water retention of surimi, gel strength and three dimensional printing related characteristics were investigated at different storage temperatures. The results showed that with the prolongation of storage time, the muscle protein oxidation and lipid oxidation accelerated, and the whole new freshness decreased. Meanwhile, water holding, gel strength and gel elasticity were also found. Relaxation stress, creep property and apparent viscosity decrease significantly. Under three storage temperatures, the overall change trend of each index is similar, while storage at a relatively high temperature will accelerate the occurrence of oxidative deterioration, fat oxidation and protein oxidation have a certain correlation, fat oxidation can promote the occurrence of protein oxidation. In addition, it is built. Based on the integral stability index method (GSI), a mathematical model for predicting the changes of protein oxidation and printing properties of surimi gel at different temperatures was established. GSI=1-5.6161texp (-20.9159/RT). The model can accurately and effectively predict the basic quality and the three dimensional printing characteristics of silver carp surimi after the storage of silver carp and establish linoleic acid (OLA). The effect of the lipid peroxide oxidation system with malondialdehyde (MDA) on the surimi gel and the influence of the structure of myofibrillar protein and the improvement of the oxidation degree of myofibrillar protein were studied. The effect of lipid oxidation on the printing effect of surimi gel during storage was elucidated, and the effect of MDA on the myofibrillar protein and the determination of the egg was carried out. The results show that the apparent viscosity, yield stress and dynamic rheological properties of the surimi OLA and MDA can increase the apparent viscosity of the gelatin, thus promoting the smooth production of the surimi slurry and reducing the filaments. The effect of.MDA induced protein gelation is obviously higher than that of the OLA system. When the MDA concentration reaches 0.03%, the surimi can show a solid state in a short time. The gelation of the gelatin can occur when the hopper is cut into the material, and the shear speed can not be evenly made into the slurry. The phenomenon of blocking in the screw gap is easy. .OLA and MDA caused the structural change of myofibrillar protein, that is, protein solubility decreased, protein carbonyl value, surface hydrophobicity first increased and then decreased slowly. The endogenous fluorescence intensity of myofibrillar protein decreased and the peak position was blue shift.NMR results showed that MDA acted on the myofibrils of fish flesh. Protein can promote the expansion of protein structure. With the increase of MDA concentration, MDA-MP forms a rigid gel structure. The flow water in the protein is not easy to move blue, and the proportion of free water is reduced. The heating effect combined with a proper covalent bond is beneficial to the strengthening of the gel structure, and the excess free water is excluded from the gel structure.
【學(xué)位授予單位】：江南大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2017
【分類號(hào)】：TS254.4

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