辛烯基琥珀酸荸荠淀粉酯的制备与理化性质研究

以荸荠淀粉为原料,以辛烯基琥珀酸酐为酯化剂,湿法制备辛烯基琥珀酸荸荠淀粉酯,研究反应温度、反应时间、反应pH、辛烯基琥珀酸酐用量及反应初始淀粉乳浓度对辛烯基琥珀酸荸荠淀粉酯的取代度和反应效率的影响。通过单因素试验与正交试验方法,以取代度和反应效率为衡量指标,确定辛烯基琥珀酸荸荠淀粉酯最佳制备工艺。采用最优组合工艺条件制备改性淀粉酯,并与原荸荠淀粉进行理化性质比较分析。结果表明,以取代度为衡量指标,最佳制备工艺条件(优化组合1)为:反应温度40℃,反应时间6 h,pH 8.0,辛烯基琥珀酸酐用量5%,初始淀粉乳浓度40%。该条件下产品取代度为0.022 8,反应效率为59.14%。以反应效率为衡量指标,最佳制备工艺条件(优化组合2)为:反应温度40℃,反应时间6 h,pH 8.0,辛烯基琥珀酸酐用量2%,初始淀粉乳浓度40%。该条件下产品取代度为0.011 4,反应效率为73.75%。理化性质试验结果表明,与天然淀粉相比,优化组合1、优化组合2酯化改性淀粉的透明度,吸水率吸油率、抗老化性、抗凝沉性、冻融稳定性等理化性质均得到明显改善。     

乙酰化辛烯基琥珀酸蜡质玉米淀粉酯的制备及性质研究

以蜡质玉米淀粉为原料,选取乙酸酐和辛烯基琥珀酸酐对其进行双重酯化改性,以取代度为衡量标准,确定了蜡质玉米双重酯化淀粉的制备顺序是先进行乙酸酐的乙酰化再进行辛烯基琥珀酸酐的酯化,得到产物乙酰化辛烯基琥珀酸蜡质玉米淀粉酯。按照确定好的酯化顺序,以实验室自制取代度为0.0768的乙酰化淀粉为原料,采用单因素和正交实验的方法研究湿法工艺制备乙酰化辛烯基琥珀酸蜡质玉米淀粉酯,得出最佳工艺条件为:在辛烯基琥珀酸酐加入量为3%的情况下,淀粉乳初始浓度30%,反应体系pH8.5,反应温度35℃,反应时间4h。采用最佳工艺条件所得产品辛烯基琥珀酸酐酯化取代度为0.0197,利用红外光谱分析方法对乙酰化辛烯基琥珀酸蜡质玉米淀粉酯的结构进行了初步表征,并对产品的乳化性及乳化稳定性、透明度、表观黏度等性质做了测定和分析。     

辛烯基琥珀酸淀粉酯的制备及其酶法降解的研究

以蜡质玉米淀粉为原料,辛烯基琥珀酸酐为亲核试剂,用正交试验方法确定了在不同条件下,制备辛烯基琥珀酸淀粉酯的最佳工艺参数,着重研究了酯化反应条件对反应取代度的影响。实验结果表明:在辛烯基琥珀酸酐添加量(淀粉干基重的3%)不变的条件下,淀粉乳的浓度、反应温度、反应体系pH值、反应时间对反应取代度均有较大影响。对制备的淀粉酯中的辛烯基琥珀酸酐残留量进行了测定,结果表明,利用本文确定的最佳反应条件制得的淀粉酯辛烯基琥珀酸残留量低于规定标准。利用α-淀粉酶对制得的淀粉酯进行了降解处理,探讨了利用不同的酶解时间,获得不同DE值样品的酶解条件。利用最佳工艺条件,进行了辛烯基琥珀酸淀粉酯的中试放大并获得了预期产品。     

辛烯基琥珀酸淀粉酯的制备与性质研究

以木薯淀粉为原料,以取代度为衡量标准,采用单因素和正交试验方法研究湿法工艺制备辛烯基琥珀酸淀粉酯,从淀粉乳的初始浓度、体系pH、反应温度、反应时间和酸酐浓度5个方面研究辛烯基琥珀酸淀粉酯最佳制备工艺。其最佳条件为:淀粉乳浓度35%、pH8.5、反应温度35℃、反应时间3.5h、酸酐加入量为4%,采用最佳工艺所得产品取代度为0.02。在同类研究中,降低了淀粉乳初始浓度,提高了产品取代度。利用红外分析方法和差示量热扫描仪对辛烯基琥珀酸淀粉酯的结构进行了表征,并与木薯淀粉的结构做了对比。     

银杏辛烯基琥珀酸淀粉酯的制备及消化性能评价

以银杏淀粉为原料,对水相法制备辛烯基琥珀酸淀粉酯的工艺进行了研究。在辛烯基琥珀酸酐添加质量分数为3.0%不变的情况下,通过单因素试验考察淀粉乳浓度、反应时间、反应温度、p H等因素对产品取代度和反应效率的影响。在此基础上,通过正交试验优化了制备银杏辛烯基琥珀酸淀粉酯的最佳工艺参数:银杏淀粉质量分数40.0%,反应温度45.0℃,p H 8.0,反应时间4.0 h。在此工艺条件下,银杏辛烯基琥珀酸淀粉酯取代度可以达到0.019 36,反应效率74.42%。淀粉消化性能试验表明银杏辛烯基琥珀酸淀粉酯对胰淀粉酶水解作用具有良好的抵抗能力,慢消化及抗消化特性显著。     

辛烯基琥珀酸芋艿淀粉酯制备及性质研究

以芋艿淀粉为原料,采用湿法制备辛烯基琥珀酸芋艿淀粉酯。以辛烯基琥珀酸淀粉酯取代度(DS)为指标,研究芋艿淀粉浓度、辛烯基琥珀酸酐用量、反应温度、反应时间对辛烯基琥珀酸芋艿淀粉酯制备的影响。在单因素试验的基础上,通过正交试验优化辛烯基琥珀酸淀粉酯制备工艺。结果表明:辛烯基琥珀酸芋艿淀粉酯制备的适宜工艺条件:淀粉质量分数40%、辛烯基琥珀酸酐用量为2.0%芋艿淀粉干重、反应温度40℃、反应时间3 h。在该工艺条件下,制得的辛烯基琥珀酸芋艿淀粉酯颗粒结构发生变化,糊化温度由原淀粉的最高温度85.49℃变为82.15℃,红外光谱图中1 710~1 740 cm-1,1 550~1 610 cm-1区间分别出现酯羰基(C=O)伸缩振动吸收和RCOO-特征吸收,可断定辛烯基琥珀酸与淀粉酯化生成辛烯基琥珀酸淀粉酯。     

机械活化辛烯基琥珀酸西米淀粉酯的制备及其乳化性能分析

采用自制搅拌式球磨机对西米淀粉进行机械活化预处理,以辛烯基琥珀酸酐为酯化剂制备辛烯基琥珀酸西米淀粉酯。探讨活化时间、反应时间、辛烯基琥珀酸酐添加量、反应温度和pH等因素对辛烯基琥珀酸西米淀粉酯取代度的影响。结果表明,机械活化对西米淀粉辛烯基琥珀酸酐酯化反应有明显的增强作用;在相同反应条件下,活化淀粉的取代度和反应效率显著上升;通过正交试验确定了活化1.0 h西米淀粉酯的最佳工艺条件：反应时间为2.0 h,辛烯基琥珀酸酐用量为3%,pH为8.0,反应温度为35℃;在此条件下酯化得到的淀粉酯取代度为0.02294,反应效率为98.01%。FTIR、XRD、SEM测试结果表明,西米淀粉经过辛烯基琥珀酸酐处理后,产品的红外光谱在1570 cm^-1和1712 cm^-1处出现了新的吸收峰,淀粉结晶度下降,淀粉颗粒表面受到破坏,颗粒中间出现较大孔洞,进一步证实西米淀粉发生了酯化反应。取代度为0.02294的辛烯基琥珀酸西米淀粉酯的乳化性为26.43%,乳化稳定性为24.10%,均优于原西米淀粉酯。     

响应面制备辛烯基琥珀酸淀粉酯的工艺研究

通过响虚面分析(Response surface analysis,RSA)软件,采用boxbehnken中心组合设计方法对辛烯基琥珀酸淀粉酯(SSOS)的制备工艺条件进行优化,得到制备辛烯基琥珀酸淀粉酯的最佳工艺条件为:反应温度为34℃,时间1.5h,pH值为8.7,辛烯基琥珀酸酐添加量为淀粉干基的3%,反应取代度(DS)可达0.0144.     

辛烯基琥珀酸淀粉酯的合成及应用研究

以轻度水解淀粉为原料,以取代度为衡量标准,采用单因素和正交试验方法研究湿法工艺制备辛烯基琥珀酸淀粉酯,从淀粉乳的初始浓度、pH、反应温度、反应时间和酸酐浓度五个方面研究辛烯基琥珀酸淀粉酯最佳制备工艺。其结果为,淀粉乳浓度50％、pH8．5、反应温度35℃、反应时间4h。采用最佳工艺所得产品取代度为0．0495。利用红外分析方法对辛烯基琥珀酸淀粉酯的结构进行了验证。以合成的辛烯基琥珀酸淀粉酯为乳化剂应用在DHA藻油的微胶囊化中,取得了非常好的效果。     

响应面法优化辛烯基琥珀酸氧化甘薯淀粉酯的制备

用响应面法(RSA)对辛烯基琥珀酸氧化甘薯淀粉酯(OSA-OSPS)的制备工艺参数进行优化.以氧化甘薯淀粉(OSPS)为原材料,采用水相法制备高取代度辛烯基琥珀酸淀粉酯.通过工艺优化,在OSA添加量5％、pH值为8.5、反应温度35℃、反应时间8h的条件下,可得到取代度(DS)为0.0219的氧化辛烯基琥珀酸淀粉酯.     

辛烯基琥珀酸交联淀粉酯合成工艺研究

以木薯淀粉为原料,用环氧氯丙烷作交联剂,辛烯基琥珀酸酐作酯化剂,采用湿法工艺合成辛烯基琥珀酸交联淀粉酯.探讨了淀粉乳浓度、反应温度、反应时间、pH和沉降积对辛烯基琥珀酸交联淀粉酯取代度的影响,确定制备辛烯基琥珀酸交联淀粉酯的最佳工艺参数为:淀粉乳浓度35%,酯化pH 8.0,酯化温度35℃,酯化时间3 h.交联淀粉的沉降积对酯化取代度影响较小,在生产中可根据最终产品的用途选用合适沉降积的交联淀粉进行酯化复合变性.复合变性淀粉符合食品行业标准,可以在食品工业中应用.扫描电镜对其结构进行观察显示淀粉中受侵蚀颗粒增多,颗粒表面的小凹痕数量增加.     

机械活化玉米淀粉的辛烯基琥珀酸酐酯化改性

采用行星式球磨机对玉米淀粉进行机械活化,再与辛烯基琥珀酸酐（octenyl succinic anhydride,OSA）发生酯化反应制备OSA淀粉酯。研究机械活化时间、反应温度、反应体系pH值、淀粉乳质量分数、反应时间因素对玉米淀粉酯化反应的影响,并采用二次回归正交旋转组合设计方法和响应面分析对制备条件进行优化。结果表明,机械活化对玉米淀粉OSA酯化反应有明显的增强作用,且反应不受pH值的影响;得到最优工艺条件为机械活化10 h、反应温度33.1 ℃、pH 8.45、淀粉乳质量分数12.2%、反应时间3 h,在此条件下制得机械活化辛烯基琥珀酸淀粉酯的平均取代度为0.020 3。     

Synthesis of Octenyl Succinic Derivative of Mechanically Activated Indica Rice Starch

Indica rice starch was mechanically activated by ball milling and then esterified by octenyl succinic anhydride (OSA) in aqueous slurry systems. The process of esterification was studied with respect to the time of mechanical activation, OSA/starch ratio, temperature, pH, starch slurry concentration and reaction time. The effects of these reaction conditions were evaluated on the basis of degree of substitution (DS) and reaction efficiency (RE). The results indicated that mechanical activation could enhance the reaction of OSA and starch. The DS and RE of OSA starch increased sharply when the time of mechanical activation increased from 0 h to 10 h, after which it was not significantly affected until 50h. The suitable conditions for the synthesis of OSA starch from Indica rice starch that was mechanically activated for 10 h (MAIS10) were an OSA/starch ratio 3%, temperature 35°C, pH 8.5, starch slurry concentration 12.5% and reaction time 3h. For native Indica rice starch (NIS), all conditions were identical to MAIS10 except for the starch slurry concentration of 40% and reaction time of 4 h. The maximum DS and RE of OSA‐MAIS10 (0.02037, 88.03%) was higher than that of OSA‐NIS (0.01700, 73.46%) at OSA/starch ratio 3%. The esterification of MAIS10 with OSA showed a low sensitivity to pH and a higher stability than OSA‐NIS. Scanning electron microscopy (SEM) revealed that the modified OSA starches did not show any detectable change in the morphological structural characteristics. The esterification between OSA and starch was confirmed by Fourier transform infrared (FT‐IR) spectroscopy.     

辛烯基琥珀酸芋头淀粉酯的制备工艺优化及理化性质分析

以奉化芋头淀粉为原料,辛烯基琥珀酸酐（Octenyl Succinic Anhydride,OSA）为酯化剂,制备了辛烯基琥珀酸芋头淀粉酯（Octenyl Succinicmodified Taro Starch,OSTS）。采用高效液相法测定淀粉酯的取代度(degree of substitution,DS),并以DS为响应值,通过单因素实验和响应面法优化酯化条件,然后测定了OSTS的疏水性、X射线衍射、微观形貌等理化性质。结果表明,最佳工艺为:淀粉浓度40%（w/v）,pH8.5,反应时间2.5 h,反应温度41 ℃,在此条件下获得的OSTS的取代度为0.02069。经酯化后,奉化芋头淀粉的表面疏水性增加,接触角从86.2°变为120.9°;淀粉晶型未受影响,即OSA与芋头淀粉的酯化反应优先发生在淀粉颗粒表面;相对结晶度由19.04%降至15.20%。该研究可为小粒径淀粉的高效辛烯基琥珀酸酐酯化提供理论依据。     

高取代度柠檬酸酯淀粉制备研究

柠檬酸酯淀粉是一种具有抗性作用酯化变性淀粉,在国外广泛应用于面包、饼干及其它食品中,以改善食品品质。该研究以玉米淀粉为原料,采用酯化变性方法,在干法条件下制备高取代度柠檬酸酯淀粉,探讨反应时间、反应温度、pH值、柠檬酸浓度对淀粉酯化过程影响;并获得高取代度柠檬酸酯淀粉最佳实验条件为:反应时间7．4h、反应温度140℃、pH为2．51、柠檬酸浓度为43．16％,样品最高取代度可达0．1776。     

Properties of Low‐substituted Cationic Starch Derivatives Prepared by Different Derivatisation Processes

Cationic starch ethers prepared by the chemical reaction of starch with a quaternary ammonium reagent are commercially important derivatives. Cationic potato starch derivatives were produced under pilot‐scale conditions, employing four different principles. Wet cationisation was carried out by the slurry and paste processes, in which the cationic reagent and catalyst are added to the starch. Besides being prepared by these more commonly used processes, cationic starches were also produced by dry cationisation and by adding the cationic reagent during extrusion of starch. The cationic reagent used was 2,3‐epoxypropyltrimethylammonium chloride. Derivatives with three graded degrees of substitution (DS) between 0.03 and 0.12 were prepared by each process. The physical properties of the derivatives were analysed by the following methods: polarised light microscopy, X‐ray scattering, differential scanning calorimetry (DSC), solubility and swelling behaviour, and High‐Performance Size‐Exclusion Chromatography‐Multiangle Laser Light Scattering (HPSEC‐MALLS). The degree of substitution was determined by high resolution ¹³C‐NMR spectroscopy after hydrolysis with trifluoroacetic acid. The properties of the cationic starch derivatives were highly dependent on the derivatisation method. The granular structure of the starch was not visibly affected by the slurry process. Products from the semi‐dry reaction showed some granular damage, which was particularly evident after suspension of the granules in water. In the paste and extrusion processes, the starch granules were completely destroyed. Swelling temperatures and enthalpies can be determined only for starch derivatives that still retain a granular structure. As a result, samples from the paste and extrusion reactions exhibited no swelling endotherm in DSC. The samples from the slurry process showed a shift in the swelling temperature range towards lower temperature and a decrease in swelling enthalpy both as compared to native potato starch and also with increasing DS. Similar behaviour was found for the samples from the semi‐dry process. The swelling temperature region was comparable to that of the slurry samples for the same DS but the swelling enthalpy was distinctly lower, indicating that the granular structure of the starch was altered far more by the semi‐dry than the slurry process. Swelling in excess water and solubility were affected primarily by the cationisation process, while the influence of DS was of minor importance. The extrusion products had pronounced cold‐water solubility, the semi‐dry products showed increasing cold‐water solubility with increasing DS, the paste products were highly swollen in cold water and the slurry products were insoluble in cold water. All products were soluble in hot water but the state of dissolution was different. The molar mass distributions of the samples were determined after dissolution by pressure cooking. The different derivatisation methods resulted in characteristic molar mass distributions. The average molar mass decreased in the order slurry, semi‐dry‐, paste and extrusion process.     

脂肪酶催化月桂酸淀粉酯的合成

在无溶剂体系中,用脂肪酶Novozym 435催化合成月桂酸玉米淀粉酯。考察时间、底物配比、酶添加量、水活度等因素对淀粉酯合成的影响。确定最适反应条件为反应时间24h、温度60℃、月桂酸与淀粉质量比4:1、酶添加量3%,取代度可达到0.1339。并使用FT-IR谱图对产物结构进行表征,说明月桂酸玉米淀粉酯合成成功。     

半干法制备低取代度阳离子淀粉的工艺研究

以玉米淀粉为原料,以3-氯-2羟丙基三甲基氯化铵(CHPTMA)为醚化剂,以NaOH为催化剂的条件下,半干法制备了低取代度阳离子淀粉。确定了半干法制备低取代度阳离子淀粉的工艺路线,研究了各反应因素对阳离子淀粉反应效率的影响,并以反应效率为指标,利用二次通用旋转试验建立了相应的回归方程,确定了最佳工艺参数为:NaOH与醚化剂的摩尔比1.85∶1,体系含水量20.49%,反应温度60.65℃,反应时间4.49h,最佳条件下制备的阳离子淀粉反应效率可达到89.48%,取代度为0.0335。