Preparation and Properties of Octenyl Succinic Anhydride Modified Early Indica Rice Starch

Octenyl succinic anhydride (OSA) modified early indica rice starch was prepared in aqueous slurry systems and the major factors affecting the esterification were investigated systematically. The physicochemical properties of the products were determined by means of Fourier transform infrared (FT‐IR) spectroscopy, scanning electron microscopy (SEM), X‐ray diffraction and Rapid Visco Analyser (RVA). The results indicated that the suitable parameters for the preparation of OSA starch from early indica rice starch in aqueous slurry systems were as follows: concentration of starch slurry 35% (in proportion to water, w/w), reaction period 4 h, pH of reaction system 8.5, reaction temperature 35°C, amount of OSA 3% (in proportion to starch, w/w). The degree of substitution (DS) was 0 018 and the reaction efficiency (RE) was 78%. FT‐IR spectroscopy showed characteristic absorption of the ester carbonyl groups in the OSA starch at 1724 cm^‐1. SEM and X‐ray diffraction revealed that OSA groups acted by first attacking the surface and some pores formed, but OSA modification caused no change in the crystalline pattern of rice starch up to DS 0.046. RVA results indicated that the starch derivatives gelatinized at shorter time to achieve higher viscosities with increased OSA modification.     

大米抗性辛烯基琥珀酸淀粉酯的制备及特性分析

为探究抗性淀粉制备新途径,提高大米特别是碎米资源的利用价值,以大米淀粉为原料,水相法制备大米辛烯基琥珀酸淀粉酯（OSA淀粉）,以取代度DS和反应效率RE为考察指标,探讨反应温度、反应pH、酸酐滴加时间和淀粉浆浓度对DS和RE的影响。对OSA淀粉进行湿热处理,探究湿热处理时间对抗性淀粉含量和理化特性的影响,并进行体外消化试验。结果表明:制备OSA淀粉适合的工艺条件为反应温度40 ℃、反应pH为9.0、酸酐滴加时间为4 h、淀粉乳浓度30%,此条件下得到的OSA淀粉DS为1.3915,RE为78.2%。将此条件获得的OSA淀粉湿热处理18 h,抗性淀粉含量从25.2%增加至42.2%。在模拟胃肠道中消化水解率为58.8%。     

Preparation and properties of octenyl succinic anhydride modified potato starch

Potato starch was esterified with octenyl succinic anhydride (OSA) in aqueous slurry systems and the major factors affecting the esterification were systematically investigated. The physico-chemical properties of the products were determined by means of Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), X-ray diffraction and a viscosity analyser (VA). The results indicated that suitable parameters for the preparation of OSA starch from potato in aqueous slurry systems were as follows: concentration of starch slurry, 35% (in proportion to water, w/w), reaction period, 3 h, pH of reaction system, 8.0, reaction temperature, 35 °C, amount of OSA, 3% (in proportion to starch, w/w), OSA dilution-fold, 5. The degree of substitution (DS) was 0.017 and the reaction efficiency (RE) was 72 ± 1.8%. FT-IR spectroscopy showed characteristic absorption of the ester carbonyl groups in the OSA starch at 1724 cm⁻¹. SEM and X-ray diffraction revealed that OSA groups acted by first attacking the surface and some pores formed, but OSA modification caused little change in the crystalline pattern of potato starch (DS 0.045). Apparent pastiness measurement indicated that the starch derivatives gelatinized within a shorter time to achieve higher viscosities over the range of designed concentration of OSA potato starch.     

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。     

响应面法优化氧化辛烯基琥珀酸甘薯淀粉酯的制备工艺

以氧化甘薯淀粉(oxidation sweet potato starch,OSPS)为原料,制备氧化辛烯基琥珀酸甘薯淀粉酯(octenyl succinate anhydride-oxidation sweet potato starch,OSA-OSPS)。运用响应面分析(response surface method analysis,RSA)辛烯基琥珀酸酐(octenyl succinate anhydride,OSA)添加量、pH值、温度和时间对OSA-OSPS取代度(degree of substitution,DS)的影响,得出最佳制备工艺：酸酐添加量7%、pH8.40、温度40℃,反应时间10h。采用快速黏度分析仪(rapid viscosity analyzer,RVA)分析表明：氧化甘薯淀粉峰值黏度较低,而经过OSA酯化后,峰值黏度又会有一定程度的提高,且随DS的增加呈上升趋势。     

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。     

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。     

机械活化协同微波法制备高取代度柠檬酸酯淀粉

在微波辐射条件下,以不同机械活化时间的木薯淀粉为原料,柠檬酸为酯化剂,氢氧化钠为催化剂制备柠檬酸酯淀粉。以取代度和反应效率为指标,分别探讨机械活化时间、微波功率、微波辐射时间、淀粉含水量、柠檬酸用量及氢氧化钠用量对木薯淀粉柠檬酸酯化反应的影响,并对影响因素进行了正交优化。结果表明,木薯淀粉经机械活化后,对微波功率、微波辐射时间、酯化剂用量、催化剂用量、淀粉含水量的依赖性明显降低,取代度和反应效率均为原木薯淀粉的2倍多。通过正交试验确定了制备柠檬酸酯淀粉的最佳工艺条件:微波功率800 W、微波辐射5.0 min、淀粉含水量35%、柠檬酸质量分数50%、氢氧化钠质量分数6%,所得产品的取代度为0.399 8,反应效率为88.84%。并采用红外光谱和X-射线衍射对木薯淀粉、活化淀粉及高取代度柠檬酸酯淀粉进行了表征。     

基于响应面法氧化辛烯基琥珀酸糯玉米淀粉酯制备的优化研究

以糯玉米淀粉为原料,先对其氧化处理,然后用辛烯基琥珀酸酐对氧化淀粉进行酯化.在单因素基础上选取影响酯化取代度明显的四个因素(pH值、反应温度、淀粉乳浓度、反应时间)在酸酐加入量为3%及酸酐用乙醇稀释5倍的前提下进行响应面设计,得出了最优条件:pH值为8.4,反应温度为36%,淀粉乳质量分数为40%,反应时间为3.5 h,酯化剂用量3%(占淀粉干基比),此时制备产品的取代度可达0.0196.     

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。     

Characterisation of 2-octen-1-ylsuccinylated waxy rice amylodextrins prepared by dry-heating

Waxy rice amylodextrins substituted with 2-octen-1-ylsuccinic acid (OSA) were prepared by heating a dried mixture of waxy rice starch and OSA (3% OSA based on starch solids) at 130–150 °C and pH 3–5 for 1–3 h. The effects of the heating conditions, such as pH, temperature and heating time on the degrees of substitution (DS) and dextrinisation, and the physical properties of the dextrins were evaluated. Substitution and dextrinisation were more affected by the reaction pH than by the physical conditions (temperature and time). Heating under a more acidic condition resulted in a higher DS and a lower molecular weight (M_w). Pasting viscosity profiles showed reduced pasting temperatures but increased peak viscosities, due to the presence of OSA, compared to unsubstituted dextrin counterparts. The X-ray diffraction patterns of the OSA dextrins were similar to that of the native starch, indicating that the dextrinisation occurred mainly in the amorphous regions of the starch granules. Fat-free whipped creams were prepared with the OSA dextrins and skim milk powder to examine the fat-replacing effects of the dextrins. The OSA dextrins effectively substituted the fat in dairy cream, providing good foaming ability and storage stability.     

辛烯基琥珀酸碎米淀粉酯的制备

以碎米淀粉为原料,采用湿法制备辛烯基琥珀酸碎米淀粉酯,以取代度为评价指标,确定辛烯基琥珀酸酐添加量为3%,通过单因素与正交试验确定辛烯基琥珀酸碎米淀粉酯的最佳制备工艺。结果显示：淀粉乳质量分数30%、pH8.5、反应时间5h、反应温度35℃为最佳工艺条件,在此条件下所得产品取代度可达0.01445。     

辛烯基琥珀酸淀粉的干法制备及其黏度性质

以木薯淀粉为原料,研究了辛烯基琥珀酸淀粉的干法制备工艺及其性质.结果表明,反应体系的碱性范围对酯化反应的影响较大,提高反应温度和延长反应时间都能增加产物取代度,但取代度增加到一定程度后趋于稳定.干法制备的辛烯基琥珀酸淀粉具有较低的糊化温度、峰值黏度和热糊黏度,糊的崩溃性减弱,冷糊稳定性有所提高,凝胶性增强.     

非晶态辛烯基琥珀酸淀粉酯的结构与理化性质关系研究

以非晶态蜡质玉米淀粉与辛烯基琥珀酸酐反应制备了系列不同取代度(DS)的辛烯基琥珀酸淀粉酯,用红外、核磁进行了表征。研究了淀粉酯制备效率及其内部结构、取代度及分子量与乳化、包埋性能的关系。结果表明:与原淀粉相比较,非晶态淀粉和辛烯基琥珀酸酐的反应效率得到明显提高,DS也增大;非晶态淀粉酯的乳化和包埋性能明显高于具有相近DS的晶态淀粉酯,当DS=0.0203时,其乳化能力、乳化稳定性以及包埋率分别达到68%、67.3%及55.2%。乳化能力和乳化稳定性随着DS和分子量的增加没有明显对应关系,而包埋率则随着DS和分子量的增加逐渐升高,呈明显正相关。     

Production and physicochemical properties of 2-octen-1-ylsuccinic derivatives from waxy corn starch

Waxy corn starch was esterified with 2-octen-1-ylsuccinic anhydride (OSA) using response surface methodology. The molecular structure and paste properties were also investigated. Results indicated that the optimum parameters for esterification were as follows: reaction period 4 h, temperature 36.7 °C, pH of reaction system 8.3, concentration of starch slurry 36.9%, and amount of OSA 3%. The degree of substitution was 0.0187 and the reaction efficiency was 80.6%. The ester carbonyl group in OSA starch was characterized by Fourier Transform Infrared Spectroscopy at 1723 cm(-1). Compared with native starch, OSA derivative had higher peak viscosity, better freeze-thaw stability, and decreased gelatinization temperature and digestibility by porcine pancreatic alpha-amylase. Scanning electron microscopy showed that the gels from OSA starch had less and smaller pores; however, the native starch gels changed to sponge-like structure after 4 freezing/thawing cycles. The OSA modified waxy corn starch offered a potential to be used in frozen foods. PRACTICAL APPLICATION: (a) To optimize operating conditions to achieve OSA modified waxy corn starch with a high degree of substitution; (b) to give a deeper insight into the physicochemical properties of OSA modified waxy corn starch, which offered a potential to be used in frozen foods.     

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.     

Gelatinization and pasting properties of rice starch modified with 2‐octen–1‐ylsuccinic anhydride

Rice starch was modified with various levels of 2‐octen‐1‐ylsuccinic anhydride (OSA). Treatments with OSA at 3, 5, and 10% resulted in starch derivatives with 0.016, 0.033, and 0.070 degrees of substitution (DS( respectively. Thermovisco properties of the derivatives were investigated by differential scanning calorimetry (DSC) and rapid visco analysis (RVA). Water content in the sample was found to have a significant effect on the characteristics of the DSC endotherm. Pasting properties of the OSA‐starch and the effect of pH and salt on the RVA profiles were also studied. In general, with increased OSA‐modification, the starch derivatives swelled and gelatinized at lower temperatures to achieve higher viscosities. Specifically, based on DSC analysis at 80% water, the peak temperature of gelatinization decreased from 68.5 to 63.2°C as the OSA modification increased in DS from 0 (intact starch) to 0.070. On the other hand, RVA results indicate that, for samples undergoing similar increase in OSA modification, the pasting temperature decreased from 88.7 to 51.5°C and the peak viscosity increased from 668 to 6822 cP.     

Synthesis and Characterization of low DS Succinate Derivatives of Cassava (Manihot esculenta Crantz) Starch

Succinylation of cassava starch was carried out in aqueous medium to prepare derivatives with low degree of substitution (DS) and the physicochemical properties of the products were determined. A response surface design was used for the experiment with three levels of each of the three variables viz., concentration of succinic anhydride, reaction time and pH of the reaction medium. The reaction was followed in terms of the DS of the products and reaction efficiency (RE). The degree of substitution of the derivatives varied from 0.001 to 0.022 and reaction efficiency from 2.2 to 46.8%. The DS and RE showed an adequate fit to a second order polynomial model of the variables used. Succinylation brought about increase in the swelling volume, peak viscosity and paste clarity of the starch. However, the pasting temperature and solubility did not show any significant change. The in‐vitro α‐amylase digestibility of the succinylated derivatives decreased in comparison to that of native starch and this decrease correlated with a corresponding increase in DS.     

Preparation and characterisation of octenyl succinate starch as a delivery carrier for bioactive food components

The octenyl succinic anhydride (OSA) modified corn starch (OSAS) was synthesised with different degrees of substitution (DS) and the influences of three factors namely OSA/starch ratio, reaction temperature, and reaction time on the DS of OSAS were studied by response surface methodology (RSM). As a delivery carrier material, the characteristics of OSAS were investigated. The resistant starch (RS) content of OSAS was increased with increasing DS, indicating the improvement of colon-targeting property. The swelling ratio (SR) of the OSAS in simulated gastrointestinal fluids was higher than that of native starch and its hydrophilicity was decreased with increasing DS. For in vitro release study, the percentage of released bioactive components was less than 7% within the first 8 h and close to 100% over a period of 36 h when the DS was 0.60. These results demonstrate that OSAS can be a potential carrier for colon-targeted delivery of bioactive food components.     

十二烷基苯磺酸酯淀粉的制备

为拓展玉米淀粉的用途,以玉米淀粉为原料,十二烷基苯磺酸钠为酯化剂,干法制备十二烷基苯磺酸酯淀粉,并用红外光谱对其结构进行表证。分别以十二烷基苯磺酸钠与玉米淀粉物质的量的比、反应时间和反应pH值对十二烷基苯磺酸酯化淀粉的取代度、黏度和黏度热稳定性的影响进行实验。结果表明：在十二烷基苯磺酸钠与玉米淀粉物质的量的比0.06、反应时间4h、反应pH14 条件下制备的十二烷基苯磺酸酯淀粉的取代度较适宜,黏度最高,黏度热稳定性最好。