马铃薯羧甲基淀粉的制备及结构分析

羧甲基淀粉是重要的变性淀粉之一,用途广泛。本文以马铃薯淀粉为原料,用乙醇溶剂法制备了马铃薯羧甲基淀粉钠,研究了氯乙酸、氢氧化钠、反应时间、反应温度、乙醇浓度、乙醇溶液体积等因素对反应的影响。以粘度为目标,用正交实验方法确定了最佳工艺条件。     

玉米羧甲基淀粉崩解剂的合成及性能改进

采用玉米淀粉为原料,以环氧氯丙烷为交联剂、氢氧化钠和氯化铵为复合催化剂、氯乙酸为醚化剂复合变性合成用作药片崩解剂的羧甲基淀粉,探讨了各种反应条件对淀粉的取代度、膨润性能及反应效率的影响,反应效率提高,反应时间大大缩短。原料最佳配比:n(脱水葡萄糖单元)∶n(环氧氯丙烷)∶n(氯乙酸)∶n(氢氧化钠)=1∶0.4∶0.6∶1.2,反应温度60°C左右,反应时间1～2h。     

羧甲基淀粉的快速制备工艺研究

用湿法制备出了具有较高取代度的羧甲基淀粉（CMS）。通过实验得到了取代度（DS＝0．19）的羧甲基淀粉。实验表明：此法工艺简单、设备投资低、耗时少。能够获得取代度较高,溶解性好,粘度高的羧甲基淀粉。     

紫外光照射对淀粉羧甲基化反应的影响

探索了紫外光照射对淀粉羧甲基化反应的影响。紫外光照射可以提高淀粉的反应活性,提高反应速率,增加替代度。     

羧甲基淀粉的应用与合成

综述了羧甲基淀粉的发展、合成方法、合成过程中的影响因素以及应用现状。羧甲基淀粉的合成主要分三种类型 :干法、半干法、湿法。综合了反应过程中的影响因素 ,例如醚化剂和催化剂的影响 ,反应时间和温度的关系 ,溶剂、设备对反应的影响 ,以及在食品、医药、钻井、纺织、日化工业中的应用前景     

羧甲基取代度对淀粉生物降解性能的影响

利用半生物体内模型和扫描电子显微技术系统地研究了取代度在0 05至0 40的羧甲基淀粉的生物降解性能,并用微生物降解代谢过程中CO2的净生成速度和剩余淀粉质量分数对羧甲基淀粉的生物降解速度和降解程度进行了表征。结果表明,淀粉经羧甲基化后,有利于微生物分泌的淀粉酶对淀粉分子链的水解。但随着羧甲基取代度的提高,水解产物中的羧甲基基团的质量分数增大,淀粉的生物降解速度和程度先增大后减少,说明羧甲基低聚糖不利于被微生物完全代谢。当取代度≤0 10时,羧甲基化促进玉米淀粉的生物降解速度和程度;当取代度为0 40时,羧甲基化抑制淀粉的生物降解,30d后其生物降解速度和程度分别为9 82mg·g-1·d-1和67 1%。淀粉的生物降解性能可以通过调节羧甲基取代度的大小来控制。     

羧甲基淀粉的合成研究

用淀粉与氯乙酸在碱性条件下发生醚化反应制备了较高取代度羧甲基淀粉。探讨了反应温度,反应时间,氢氧化钠用量,氯乙酸用量和水分含量等因素对羧甲基淀粉取代度的影,确定了最佳反应条件。结果表明,用乙醇溶剂法制备羧甲基淀粉工艺合理,操作简单,易于控制,产品具有良好的稳定性和较高的取代度,应用前景较好。     

高取代度木薯羧甲基淀粉的合成及表征

以机械活化60min的木薯淀粉为原料,采用乙醇溶剂法合成了高取代度的木薯羧甲基淀粉.通过正交实验优化羧甲基淀粉的合成工艺条件,探讨了反应时间、反应温度、催化剂用量、醚化剂用量、乙醇浓度及淀粉乳浓度等因素对羧甲基淀粉取代度的影响.结果表明,其合成的最优工艺条件为:反应温度50℃,乙醇浓度90%,反应时间120min,ClCH2COOH与淀粉摩尔比0.80,淀粉乳浓度35%(ω),NaOH与淀粉摩尔比0.80.在此条件下合成的羧甲基淀粉的取代度为1.24.并对产物的结构进行了表征.     

己酰酯化羧甲基淀粉的制备及粘度性质研究

以羧甲基淀粉(CMS)为原料,己酰氯为酯化试剂,二甲基亚砜(DMSO)为溶剂,吡啶为有机碱合成了己酰酯化羧甲基淀粉(HCMS)。研究了反应温度、反应时间、催化剂用量、溶剂用量对己酰酯化取代度(DS)和反应效率(RE)的影响,确定了最佳反应条件为:5 g CMS,40 mL DMSO,反应温度为50℃,反应时间为30 min,有机碱用量为1.0 g。通过IR、流变仪对产物进行了结构及溶液黏度性质研究。通过对不同质量分数和己酰酯化取代度(DShexyl)的羧甲基淀粉溶液黏度性质(剪切速率0～500 s-1)的研究表明,达到临界聚集质量分数2.0%时,适当己酰基取代度(DShexyl=0.3)的HCMS,可以使羧甲基淀粉溶液的黏度由420 mPa.s提高到34 000 mPa.s(γ=5 s-1)。     

改性蜡质玉米淀粉稳定Pickering乳液的制备及应用

采用辛烯基琥珀酸酐(OSA)对蜡质玉米淀粉(WS)疏水改性制得辛烯基琥珀酸酐改性蜡质玉米淀粉(OSA-WS),以不同取代度OSA-WS制备了稳定的Pickering乳液。测定了OSA-WS取代度(DS)、反应效率(RE)及三相接触角,对其进行了FT-IR、XRD和SEM表征。结果表明,OSA通过与淀粉表面羟基反应对其进行改性并未改变淀粉颗粒结构;随着取代度的增大,淀粉颗粒乳化性增加,制得Pickering乳液稳定性增强;以OSA-WS为乳化剂制得包埋辅酶Q10的Pickering乳液,通过透皮运输实验可知,与辅酶Q10的油溶液相比,包埋辅酶Q10的Pickering乳液更有利于辅酶Q10的透皮运输。     

Synthesis,characterization, and anticoagulant activity of carboxymethyl starch sulfates

To develop a renewable and compatible anticoagulant as potential heparin alternative, carboxymethyl starch sulfate (CMSS) was prepared by the reaction of carboxymethyl starch (CMS) and sulfating reagent [N(SO₃Na)₃]. The chemical structures of CMS and CMSS were characterized by Fourier transform infrared spectroscopy and ¹³C nuclear magnetic resonance. The influences of reaction parameters, including the pH of sulfating reagent, the molar ratio of sulfating reagent to CMS, reaction time, and temperature on the degree of substitution of sulfate groups (DS) of CMSS were studied. Meantime, the DS of each CMSS was determined by barium sulfate–glutin nephelometery method. Moreover, the anticoagulant activity of CMSS was investigated by the coagulation assays of activated partial thromboplastin time, thrombin time, and prothrombin time. The results revealed that the anticoagulant activity of CMSS was closely related to the DS value and concentration. The anticoagulant activity was promoted with the increasing of the DS and concentration. The molecular weight (M_w) in measured range had little impact on anticoagulant activity in contract to the DS and concentration. In this article, the CMSS with the DS of 1.91, concentration of 75 μg/mL and the M_w of 2.61 × 10⁴ had the best blood anticoagulant activities. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Effects of drying process for amorphous waxy maize starch on theophylline release from starch‐based tablets

Physical properties and theophylline‐release profiles of compressed tablets prepared with amorphous waxy maize starches dried using different methods were examined. A gelatinized waxy maize starch paste (10% solids in water) was either freeze‐dried or oven‐dried (40 or 105°C) until the moisture content reached to <5%. To form the tablets, the dried amorphous starch powders, either with or without theophylline (3 : 10, w/w), were remoistened to a water content of (17 ± 0.2)%, and compressed into tablets. The drying process applied to the amorphous starch powders affected both the compactness and swelling behavior of the tablets. Although no crystallinity was detected in all the starches tested, X‐ray diffraction patterns indicated that starch chains dried at the lower temperature (40°C) are allowed more time to re‐associate during the drying process than those dried at the higher temperature (105°C). The freeze‐dried starch powders formed tablets characterized by greater compactness and rigidity than was observed in the oven‐dried starch samples. The drug release of the tablets prepared with the starch dried at the higher temperature (105°C) occurred at a much slower rate than that of the tablets made with the starch dried at the lower temperature (40°C). The drug release characteristics of the freeze‐dried starch tablets were nearly identical to those of the tablets prepared with the starch dried at 105°C. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007     

Carboxymethylation of γ‐irradiated starch

Low viscosity carboxymethyl corn starch was prepared by the reaction of γ‐irradiated starch with monochloroacetic acid in the presence of alkali. It was found that irradiation dose influences the product viscosity remarkably. The viscosity decreases as the irradiation dose level increases; however, the viscosity increases with the increasing dose rate and the degree of substitution (DS). γ‐Irradiation can activate the starch to react with monochloroacetic acid, and the more of the irradiation dose, the higher of the DS and the reaction efficiency. The product has the character of low viscosity at high concentration, and the more of the irradiation dose, the more similar of the rheological behavior to a Newtonian liquid. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 2210–2215, 2006     

高黏度、高热稳定性羧甲基淀粉己酸酯的溶液性质

以羧甲基淀粉(CMS)为原料制备了高黏度、高热稳定性的羧甲基淀粉己酸酯(CMSH)。用IR和TG对产物进行了结构和热稳定性质研究;通过Brookfield R/S-CC流变仪对羧甲基淀粉己酸酯溶液黏度性质和影响因素,如己酰基质量分数、浓度、剪切力、温度及溶液黏度的剪切恢复性质、温度敏感性质等进行了详细研究。结果表明,引入己酰基基团后,可以降低黏度对温度的敏感性,显著提高羧甲基淀粉的热稳定性和溶液的黏度值。但己酰基团的引入,不能提高CMS溶液黏度的抗剪切性和剪切恢复性。当己酰基质量分数为11.8%时,羧甲基淀粉己酸酯的初始热分解温度由260℃提高到300℃;溶液的黏度值由420 mPa·s提高到32000 mPa·s。     

羧甲基淀粉研究进展

介绍了羧甲基淀粉的合成原理和方法,综述了淀粉的种类、溶剂、醚化剂、催化剂、反应时间和反应温度等因素对制备羧甲基淀粉的影响及最新的研究进展情况。     

聚乳酸改性糯玉米淀粉的制备及表征

以糯玉米淀粉为原料、异辛酸亚锡为催化剂,在丙交酯熔融体系中制备了聚乳酸改性糯玉米淀粉。建立了聚乳酸改性糯玉米淀粉取代度的1HNMR测试方法,以取代度为响应值,反应时间、反应温度、丙交酯添加量为考察因素,通过单因素和响应面实验优化了聚乳酸改性糯玉米淀粉的合成工艺,得到最优工艺为：反应时间12.46 h,反应温度111.75℃,丙交酯添加量为淀粉质量的258%,预测最大取代度为0.0253,通过实际操作条件调整后实际取代度为0.0238。对最优条件下制备的聚乳酸改性淀粉进行了系列表征,证实聚乳酸改性糯玉米淀粉的颗粒结构没有被完全破坏,晶型、相对分子质量等性能优于溶剂法传统技术制备的聚乳酸改性糯玉米淀粉。     

Optimization of preparation conditions of carboxymethyl potato starch through orthogonal experimental design

To optimize the preparation conditions of carboxymethyl potato starch (CMPS), the effects of relevant factors on viscosity (η) of 2% CMPS aqueous solution and degree of substitution (DS) were investigated. These condition parameters included etherification temperature, alkalization and etherification time, water content in the mixed solvent, ratio of liquid volume to starch mass, molar ratio of sodium hydroxide to monochloroacetic acid, and molar ratio of monochloroacetic acid to anhydroglucose unit. After individual parameter influencing η and DS was researched one by one, an orthogonal experiment of L₁₈ (2 × 3⁷) was designed to identify the main factors affecting them. In light of range analysis, the comparative importance of factors impacting η and DS was obtained, separately. Results of variance analysis showed that the most effective factor to control DS was etherification temperature, whereas the influences of all factors on η were not significant. Meanwhile, η and DS of the optimized final product were found to be 12,000 mPa.s and 0.68, respectively. In addition, the structure of CMPS was characterized by Fourier transform infrared (FTIR) spectrophotometer. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

高取代度羧甲基淀粉的制备

用玉米淀粉、氯乙酸和氢氧化钠为原料，在乙醇溶剂中反应制备了取代度为０．６的羧甲基淀粉。采用正交设计试验考察了物料配比、反应温度、反应时间对产物取代度的影响，确定了最佳反应条件。