反应条件对马铃薯羧甲基淀粉黏度和取代度的影响

以马铃薯淀粉为原料,通过与氯乙酸的反应和采用"两步碱化法"合成了羧甲基淀粉。探讨了在不同的反应条件下,羧甲基淀粉取代度和黏度之间的关系。结果表明,随着碱化时间、碱化温度、醚化时间、醚化温度、氢氧化钠以及氯乙酸用量的改变,羧甲基淀粉取代度的高低和其黏度的变化不呈单调关系。结论:由于氢氧化钠的双重作用,在一定范围内,取代度增大而粘度减小。     

红薯淀粉羧甲基化改性研究

以红薯淀粉为原料 ,用乙醇溶剂法制备羧甲基淀粉 ,通过正交实验探讨了影响羧甲基淀粉取代度的各种因素 ,获得制备条件为 :红薯淀粉用量 10 g、氢氧化钠 7g、氯乙酸 6g、乙醇浓度 75 %、乙醇体积 75mL、碱化温度 35℃、醚化温度 4 5℃、碱化时间 4 5min、醚化时间 80min。在该优化条件下 ,红薯羧甲基淀粉取代度(DS)达 0 .87,粘度达 0 .5 1Pa·S。     

高取代度羧甲基小麦淀粉制备工艺的优化及表征

摘 要：以小麦淀粉为原料,以氯乙酸作为醚化剂,采用两次加碱法制备了高取代度的羧甲基小麦淀粉。以4.05g淀粉为基准,采用正交实验对反应条件进行了优化,得到的最佳工艺条件为：水用量6mL,无水乙醇用量60mL,氯乙酸与淀粉摩尔比1.4,氢氧化钠与氯乙酸摩尔比1.8,碱化用氢氧化钠百分比70%,碱化温度35～40℃,碱化时间0.5～1h,醚化温度50～55℃,醚化时间2～3h,在此条件下制得了取代度高达1.21的羧甲基小麦淀粉。     

羧甲基绿豆淀粉合成工艺研究

以绿豆淀粉为原料,一氯乙酸作为醚化剂,乙醇为溶剂,制备羧甲基绿豆淀粉。以20 g绿豆淀粉为基准,采用正交和单因素试验对制备工艺进行优化,探讨氢氧化钠用量、一氯乙酸用量、醚化温度、醚化时间对产品取代度影响。试验结果表明,其最佳制备工艺条件为:氢氧化钠用量(氢氧化钠/淀粉摩尔比)1.3、一氯乙酸用量(一氯乙酸/淀粉摩尔比)1.0、醚化温度52℃、醚化时间120 min;在此条件下,制得羧甲基绿豆淀粉取代度为1.05。     

红薯粉制备特高黏度羧甲基淀粉工艺的研究

研究了制备工艺中的诸因素对红薯羧甲基淀粉(CMS)黏度的影响。结果表明,当红薯粉(C6H9O4OH)用量为1mol,乙醇用量为12mol,碱化时间为0.75h时,最佳工艺条件为n(C6H9O4OH)∶n(NaOH)∶n(ClCH2COOH)=1∶1.5∶0.75,碱化温度35℃,醚化温度45℃,醚化时间为2h,按此工艺可以制备黏度值高达2048mPa·s的红薯羧甲基淀粉。     

特高黏度交联(红薯)羧甲基淀粉的研究

研究了制备特高黏度交联红薯羧甲基淀粉(CMS)生产工艺的影响因素。通过加入环氧氯丙烷对红薯淀粉进行轻度交联,并在催化剂存在下交联与醚化一步完成,添加淀粉量0.12%(w/w)的环氧氯丙烷,在淀粉∶氯乙酸∶氢氧化钠=1∶1∶2.2(mol/mol),碱化温度30℃,碱化时间30m in,醚化温度45℃~50℃,醚化时间2.5h情况下,制备的交联红薯羧甲基淀粉具有高黏度(4500mPa.s)和较高的黏度稳定性。     

羧甲基大米淀粉的半干法制备及表征

以大米淀粉和氯乙酸钠为原料,采用半干法制备羧甲基淀粉(CMS)。考察了氯乙酸钠用量、NaOH用量、醚化温度、醚化时间和碱化温度等条件对产物取代度的影响,并对得到的CMS的红外光谱和晶型进行了表征分析。结果表明:半干法合成CMS的单因素优化条件为:nMCA/nAGU=1,nNaOH/nAGU=1.25,碱化温度35℃,碱化时间1h,醚化温度70℃,醚化时间2.5h,在该条件下得到取代度为0.45的产物,其红外光谱在1 300~1 600cm~(-1)处出现了新的吸收峰,为羧基官能团特征峰,其晶型由多晶颗粒结构转变为无定型结构。     

高取代度羧甲基玉米淀粉制备工艺的研究

以玉米淀粉为原料,乙醇为溶剂,氯乙酸为醚化剂,研究高取代度羧甲基淀粉的制备工艺。还比较了不同淀粉、醚化剂的种类以及Na OH状态对取代度的影响。结果表明,最佳工艺为:二次加碱法,95%(质量分数)的乙醇作溶剂,淀粉乳浓度为25%,氯乙酸用量为115 g,Na OH用量为2.25(摩尔比,碱∶酸),碱化温度为40℃,碱化时间为10 h,碱化Na OH用量为1(摩尔比,碱∶酸),醚化温度为40℃,醚化时间为10 h,醚化阶段用14 g Na_2CO_3代替部分Na OH。一步法制备了取代度(DS)=1.21,反应效率(RE)=61.38%的羧甲基淀粉(CMS),非晶颗粒态淀粉的取代度比原淀粉略高,四种淀粉制备CMS取代度从高到低依次为马铃薯淀粉、木薯淀粉、蜡质玉米淀粉、玉米淀粉,氯乙酸作醚化剂时取代度远高于氯乙酸钠,固体碱制备CMS的取代度比液体碱高。     

蜡质玉米淀粉羧基化的工艺优化探究

为了解决海藻酸钠逐步向食用品转化,价格提高,导致印花生产成本上升的问题,新型、低成本的改性糊料便成为了近年研究的热点。研究了低成本、印制性能较优的羧甲基淀粉的合成工艺。以蜡质玉米淀粉为原料,运用乙醇和异丙醇复配溶剂制得了能溶于水的高取代度羧甲基淀粉钠,考察了溶剂配比、碱化时间、碱化温度、醚化时间、醚化温度、碱用量、氯乙酸用量及含水量对产品取代度的影响,通过正交试验得出了最佳工艺条件:溶剂[V(乙醇)∶V(异丙醇)=5∶5]用量3.4 m L/g,含水量5%,碱化时间90 min,碱化温度35℃,醚化时间4.5 h,醚化温度55℃,n(氯乙酸)∶n(淀粉)=1.15∶1,n(NaOH)∶n(淀粉)=2.55∶1,在此条件下制备的羧甲基淀粉取代度最大,为1.162。     

响应面分析优化菊粉的羧甲基改性工艺

研究菊粉的羧甲基改性工艺条件,以碱化时间、醚化温度、醚化时间、碱用量以及氯乙酸用量为影响因素,以羧甲基的取代度为考察指标,运用Plackett-Burman设计筛选出3个对菊粉羧甲基取代度影响显著因素,即碱化时间、醚化温度和氯乙酸用量,采用响应面分析试验优化菊粉的羧甲基改性工艺。菊粉的羧甲基改性最优工艺条件为菊粉用量6.8g、碱化时间30min、醚化温度81℃、氯乙酸用量2.96g,此时菊粉的羧甲基取代度为0.66±0.000167。     

槲皮素-羧甲基甘薯淀粉酯的合成

以甘薯淀粉为原料,依次经过羧甲基化、槲皮素共价修饰两步改性,得到槲皮素-羧甲基甘薯淀粉酯,并采用单因素及响应面试验考察制备工艺条件对产物取代度的影响。单因素试验结果表明,其取代度随反应底物配比（N槲皮素/AGU）（X1）的增加而增加,随活化试剂与羧甲基甘薯淀粉脱水葡萄糖基的物质的量比（NEDC/AGU）（X2）及反应体系pH值（X3）的增加呈先增加后降低的趋势;响应面试验结果表明,NEDC/AGU及反应体系pH值对取代度有极显著影响（P＜0.01）,而N槲皮素/AGU以及二次项和交互项对取代度的影响不显著（P＞0.05）。得到最佳工艺条件为羧甲基甘薯淀粉质量浓度51?g/L、N槲皮素/AGU?2∶1,NEDC/AGU?1.8∶1、反应体系pH?7.4,可制得最大取代度（0.114?9）的槲皮素-羧甲基甘薯淀粉酯。通过检测槲皮素从产物的水解释放确认产物的合成。     

红薯淀粉水凝胶制备及吸水特性研究

以红薯淀粉为原料,以4-二甲基氨基吡啶为催化剂,于水相中经过醋酸酐酯化处理制备红薯淀粉水凝胶。确定了制备红薯淀粉水凝胶的最佳工艺条件,红外光谱确认在淀粉中引入了羧甲基。红薯淀粉水凝胶吸水性增强,黏度增大,糊透明度得到改善,说明红薯淀粉水凝胶具有优良吸水特性。     

交联-羧甲基红薯淀粉的制备及性质研究

以红薯淀粉为原料,用环氧氯丙烷作交联剂,氯乙酸作羧甲基化试剂,合成交联-羧甲基复合变性淀粉。确定了交联-羧甲基复合变性红薯淀粉合成工艺的最佳条件——反应温度55℃,反应时间4 h,配料比m(淀粉)∶m(氯乙酸):m(NaOH)=1∶0.48∶0.44。交联-羧甲基复合变性红薯淀粉的粘度增大,糊化温度降低、糊化时间缩短、糊透明度得到改善。红外光谱分析证实在淀粉中引入了羧甲基。     

Starch Derivatives of High Degree of Functionalization. 13. Novel Amphiphilic Starch Products

Amphiphilic starch derivatives of high degree of substitution (DS) were prepared by benzylation of pea, potato and waxy maize starch followed by the introduction of hydroxypropyltrimethylammonium and carboxymethyl moieties. The conversions were carried out under heterogeneous conditions leading to products with a total DS of up to 1.8. The starch composition regarding amylose and amylopectin influences the DS value. The structure of the products was characterized by means of elemental analysis, FTIR and NMR spectroscopy, and, in case of benzyl carboxymethyl starch by means of HPLC after complete chain degradation. The tensioactive properties depend on the DS values of hydrophilic and lipophilic groups and can be adjusted by controlling the molar ratio anhydroglucose unit to reagent during the synthesis. Surface tensions as low as 48.6 mN/m were found for benzyl hydroxypropyltrimethylammonium starch and 38.6 mN/m for benzyl carboxymethyl starch. The lowest critical micelle concentration determined is 2.1 mmol/L.     

Experimental Studies on the Carboxymethylation of Arrowroot Starch in Isopropanol‐Water Media

The reaction between granular arrowroot starch and sodium monochloroacetate (SMCA) in isopropanol‐water mixtures has been studied in a systematic way using experimental design strategies. The effect of six factors, i.e. the theoretical degree of substitution (DS_t), reaction time, weight fraction of water in the mixture, NaOH/SMCA ratio, temperature and weight fraction of starch on three responses, i.e. the degree of substitution (DS), the conversion of SMCA and the selectivity of SMCA towards carboxymethyl starch, has been determined in a systematic manner. Granular carboxymethyl arrowroot starch with a maximum DS of 1.4 could be prepared in a singlestep procedure. The results are compared with data obtained for potato starch. Similar trends for all responses were observed, suggesting close similarities between the chemical composition and the topochemistry of granular arrowroot‐ and potato‐starch.     

A Comparison of Some Methods for the Determination of the Degree of Substitution of Carboxymethyl Starch

The degree of substitution (DS) markedly affects the properties of sodium carboxymethyl starch (Na‐CMS). In this work Na‐CMS samples with different DS starting from both potato and corn starch were synthesized in an ethanol/water mixture and their DS was determined using three methods: direct titration of the acid form of the carboxymethyl starch (H‐CMS), Cu salt precipitation and back titration. It was found that direct titration gave smaller DS values, while the Cu salt precipitation method gave higher DS values than the back titration method, which was found to be the most accurate. The values of the DS obtained by these methods were similar for lower DS while for higher values the discrepancy was more pronounced. Under the same experimental conditions the CMS obtained from corn starch had a higher DS than the one obtained from potato starch and on average, the discrepancies between the DS values obtained by the employed analytical methods were smaller for the CMS samples synthesized from corn starch.     

食品胶对甘薯淀粉膜性能的响应面法优化实验

以机械性能(抗张强度、断裂拉伸应变)和透湿性为指标,研究食品胶对甘薯淀粉膜性能的优化。结果表明：羟丙基羧甲基纤维素(HPCMC)添加量为3.5～4.0g/100g 淀粉、甘油添加量小于2.0g/100g 淀粉及黄原胶添加量小于2.0g/100g 淀粉时,膜的机械性能较好;HPCMC 添加量小于2.0g/100g 淀粉、甘油添加量大于4.0g/100g 淀粉和黄原胶添加量小于1.5g/100g 淀粉时,膜的透湿性较小。由于不同性能的优化值范围不完全相同,在实际应用中可根据对不同性能的要求进行选择。     

食品胶协同干热处理对马铃薯淀粉理化特性的影响

为了改善马铃薯淀粉加工特性,选用瓜尔胶、羧甲基纤维素钠和黄原胶3种食品胶分别与马铃薯淀粉复配后进行干热处理,研究食品胶协同干热处理对马铃薯淀粉糊化、老化和流变特性的影响。研究发现,中3种食品胶协同干热处理均能够降低糊化温度与糊化焓,并且均能增强淀粉体系稳定性,使其呈现出弹性流体性质,不仅如此还均能提高淀粉糊热稳定性以及耐剪切能力,此外均能增强淀粉凝胶的冻融稳定性。结果表明,3种食品胶协同干热处理均能起到改善马铃薯淀粉加工特性的作用,对其改善程度对比分析发现,黄原胶协同干热处理改善马铃薯淀粉特性效果最好。     

乙醇溶剂法制备羧甲基马铃薯淀粉及特征分析

以乙醇为溶剂通过单步反应和多步反应制备了羧甲基马铃薯淀粉,并采用红外光谱、X-衍射、热重分析、扫描电镜、13C核磁共振、紫外扫描对产品进行了分析.单步反应时取代度可以达到0.75,反应效率75%,多步反应时取代度可以达到1.06,反应效率35.3%.分析显示:淀粉微观结构发生了显著变化,结晶度大幅下降,热稳定性上升,取代位点主要分布在C-2、C-6位点上,C-3位点取代度很小,产品溶液在可见光区的透光性相对于原淀粉有极大提高.     

Synthesis,characterisation and in vitro digestibility of carboxymethyl potato starch rapidly prepared with microwave-assistance

Carboxymethyl potato starch was synthesised with the aid of microwave. Optimal degree of substitution (DS) of 0.32 was obtained at 45 °C in 25 min using aqueous ethanol media with water/solvent of 0.15 at 200 W. The molar ratio of sodium hydroxide and monochloroacetic acid to anhydroglucose unit for optimal DS were 2.5 and 1.0, respectively. FT-IR spectrometry revealed the carboxymethyl starch to show new bands at ν = 1614 cm⁻¹ and ν = 1429 cm⁻¹. Wide angle X-ray diffractometry and DSC revealed a remarkable reduction in starch crystallinity after carboxymethylation, which was consistent with destroyed surface observed in SEM. The digestibility of carboxymethyl starch (CMS) was lower than that of native starch. With similar DS, there was no difference in digestibility of carboxymethyl starch prepared with and without microwave. As DS increased from 0.05 to 0.32, the amount of resistant starch in microwave-assisted carboxymethyl starch was elevated from 14.6% to 20.0%, which was much higher than that of native starch (10.8%).