果胶碱法脱酯工艺影响因素的研究

以商品柑橘高酯果胶为原料制取低酯果胶.重点探讨了低温碱法脱酯时间对果胶质量和得率的影响并比较了异丙醇、甲醇沉淀果胶的效果.以果胶的半乳糖醛酸含量、酯化度(DE值)、黏度、得率等为分析对象.结果表明,低温下(4℃)碱法脱酯可将影响果胶品质的β-消去反应控制在较小程度,所得产品黏度能最大程度得到保持.柑橘高酯果胶碱法脱酯的最佳工艺条件为pH 9.0,控制温度在4℃,处理30 min,沉淀果胶用异丙醇,该条件所得果胶半乳糖醛酸含量为86.57%,DE值为47.98%,得率为81.5%,指标达到低酯果胶产品的标准.     

果胶的酰胺化技术研究

以商品柑桔高酯果胶为原料,对其进行酰胺化处理,研究低温条件下酰胺化作用的氨水浓度和脱酯时间对产品质量的影响,以果胶的半乳糖醛酸含量、酯化度(DE值)、酰胺取代度(DA值)、特性粘度等指标为考察依据。结果表明,低温下(5℃)高浓度氨水(4N)脱酯可将影响果胶品质的β-消去反应控制在较小程度,所得产品特性粘度较高,酰胺化程度(DA值)较大;而低浓度氨水(1N)处理则得到酰胺化程度较低的产品。这两种方式配合短时间脱酯(40min)都可制得半乳糖醛酸含量,DE值,DA值等指标符合EU(欧盟)关于酰胺化果胶标准的产品。     

碱催化脱酯制取低甲氧基果胶的研究

以商品高酯果胶为原料,以脱酯率、产品粘度、得率为指标,对碱性条件下影响低甲氧基果胶制备的因素进行正交试验以获得制取低甲氧基果胶的最佳工艺。试验结果表明最佳工艺条件为:以浓度2%的高甲氧基果胶为原料,控制温度0℃和pH值9.0,搅拌反应45min进行脱酯;再在常温下利用pH为3.0的60%乙醇溶液搅拌5min以析出果胶。所得产品酯化度(DE)为42.56%、粘度116.2MPa·s、半乳糖醛酸含量(AGA)75.4%;果胶得率89.67%,各项指标符合低甲氧基果胶产品标准。     

柑橘果胶碱法脱酯动力学特征

为研究碱法脱酯机理以及温度和p H值对果胶酯化度(degree of esterification,DE)与脱酯速率的影响,以高酯柑橘果胶(DE为77.8%)为原料,研究不同温度(10、20、25℃和30℃)和不同p H值(10.0~11.3)条件下的脱酯动力学和热力学特征。为更精确控制p H值,在Na HCO3/Na2CO3缓冲体系中以Na OH调节果胶溶液p H值,以酯化度和甲氧基浓度为指标研究碱法脱酯规律。结果表明:温度和p H值都对碱法脱酯有显著影响,但p H值的影响大于温度,且它们的交互作用明显。果胶碱法脱酯符合一级动力学反应模型。脱酯速率常数(k)与p H值呈幂指数关系。当p H值从11.0轻微增加到11.3时脱酯速率显著增大。p H值为10.7、11.0和11.3时,脱酯活化能分别为136.97、122.37 k J/mol和104.20 k J/mol,脱酯活化焓分别为134.52、119.92 k J/mol和101.75 k J/mol,脱酯活化熵分别为141.86、100.28 J/(mol·K)和44.81 J/(mol·K),脱酯活化自由能分别为92.76、90.40 k J/mol和88.56 k J/mol。     

高酯果胶氨法降酯条件的研究

采用氨水对高酯速凝果肢进行降酯条件的研究，并对所得到的产品的半乳糖醛酸、酯化度、胶凝度等重要指标进行分析，通过正交实验确定了氨法降酯的最佳工艺条件：果胶浓度2％、反应pH值10．0、反应时间1h、反应温度15℃。     

利用果胶酯酶制备低酯果胶工艺研究

研究高酯果胶脱酯工艺的最佳条件;利用果胶酯酶对商品高酯果胶进行脱酯,采用L934正交试验法研究确定酶用量、脱酯温度、pH及脱酯时间对脱酯效果的影响.利用果胶酯酶进行脱酯的最佳工艺参数为:果胶酯酶0.06 g,脱酯温度45℃,脱酯pH 7,脱酯时间70 min,所得果胶甲氧基含量为4.96%.利用酶法制备低酯果工艺简单,脱酯效率较高.     

柑橘果胶高效提取及其酰胺化改性制备

采用表面活性剂-超声辅助提取(S-UAE)柑橘果胶,研究pH值、超声时间和液固比(LSR)对果胶提取率(PY)、半乳糖醛酸(GA)含量和酯化度(DE)的影响。采用响应面法优化提取条件,在pH 0.6、超声时间15.0 min和LSR 21.0 m L/g的条件下,果胶提取率最高仅为17.1%。在此基础上,开展表面活性剂结合超声波辅助提取柑橘果胶的协同作用研究。S-UAE法是先向提取介质中加入8 g/L十二烷基硫酸钠(SDS),再进行超声提取;该法与单独的超声提取相比,果胶提取率高达26.4%±0.8%(增幅超过55.0%)。研究比较了传统酸法(CE)、超声辅助提取法(UAE)和S-UAE法柑橘果胶的提取率及产品的理化性质,如GA含量、DE值和平均分子质量(Mw)。另外,以获得的柑橘高酯果胶为原料,对其进行酰胺化改性处理,研究反应温度、pH值和果胶质量浓度对产品质量的影响,结果表明,在10℃、pH 11.5和果胶质量浓度20 g/L条件下反应100～180 min,获得不同类型的酰胺化产品,其酰胺化度(DA值)13%～22%,DE值29%～39%,GA含量69%～84%,黏度136～172 mPa·s,Mw 148～173 ku,符合国内外标准。本研究结果可为我国柑橘副产物高值化利用提供参考。     

超声波辅助提取柑橘幼果中果胶的工艺优化及其理化性质研究

为了探究柑橘幼果中果胶的种类及理化性质，并优化其超声波辅助提取工艺参数，进而提升柑橘幼果利用率，研究使用超声波辅助水提法提取柑橘幼果中的果胶，通过单因素试验结合正交试验法的设计得出结论。结果表明：柑橘幼果果胶的最佳提取工艺为料液比1:50 g/mL、超声频率50 kHz、提取时间40 min、提取温度70℃，在该条件下，柑橘幼果果胶得率最高，为6.11%。柑橘幼果中所含果胶为低酯果胶，与常见的柑橘高酯果胶不同，其中单糖组成占比最高的依次为半乳糖、阿拉伯糖以及葡萄糖醛酸，测得重均分子质量达583.66 ku，为高分子质量果胶。水分、灰分、酯化度以及半乳糖醛酸含量等理化指标均符合GB 25533—2010要求，冻干处理的果胶微观形态结构优于烘干处理。     

果胶酰胺化脱酯技术的研究

以高酯柑橘果胶为原料对高酯果胶酰胺化技术进行了研究,主要针对影响酰胺化脱酯速度以及反应中两对竞争性的反应-氨解反应和水解反应以及脱酯反应和β-降解反应的影响因素进行了探讨,并且以粘度为指标评价了将反应控制在一定低温条件和醇浓度下的必要性。实验结果表明,影响酰胺化过程的主要因素有氨水浓度、温度、反应时间以及体系中的醇浓度。通过控制体系的醇浓度和温度,既可以使酰胺化过程更有效率,又能使酰胺化果胶的酯化度和酰胺化度保持在一定所需范围之内,为工业化的生产打下良好的理论基础。     

新鲜与干制柑橘皮果胶物化特性比较分析

以柑橘皮为原料,分析、比较新鲜柑橘皮果胶（fresh citrus pectin,FCP）与干制柑橘皮果胶（dried citruspectin,DCP）的物化特性差异。采用传统酸法结合金属螯合剂（六偏磷酸钠）分别从新鲜、干制柑橘皮中提取得到果胶FCP、DCP,测定FCP和DCP的物化特性参数,包括水分、灰分、酸不溶灰分和蛋白含量等基本理化指标,以及半乳糖醛酸含量、酯化度、胶凝度、分子质量和表观黏度等果胶品质评价指标。结果表明：FCP与DCP的基本理化性质相差不大,FCP半乳糖醛酸含量、酯化度、胶凝度和分子质量分别为77.29%、67.5%、179.8和158.8 kD,而DCP对应的值依次为74.98%、66.7%、153和109.1 kD,FCP表观黏度值高于DCP。新鲜和干制柑橘皮果胶品质存在一定差异,特别是作为果胶品质重要参考指标的胶凝度,FCP要高于DCP,而这可能与FCP的分子质量较高有关,但两者的半乳糖醛酸含量和酯化度均符合果胶品质的国家标准GB25533-2010《食品安全国家标准 食品添加剂》要求。     

黄秋葵果胶理化特性的研究

以商品柑橘果胶为对照,研究黄秋葵果胶的理化特性及果胶质量浓度、加热温度、pH值、蔗糖质量浓度和CaCl2质量浓度等因素对黄秋葵果胶黏度的影响。结果表明：黄秋葵果胶总半乳糖醛酸含量为86.68%,酯化度为75.45%,溶解度为82%,pH值为4.63,属于弱酸性高酯果胶;黄秋葵果胶的黏度随着加热时间的延长而下降,但其热稳定性优于商品柑橘果胶;黄秋葵果胶的黏度与其质量浓度、蔗糖质量浓度均成正相关,与加热温度成负相关,而随pH值、CaCl2质量浓度的增大呈先上升后下降的趋势,表现出一般果胶的黏度特性。黄秋葵果胶的黏度及热稳定性能优于商品柑橘果胶,是一种优质果胶。     

偏最小二乘回归法预测酰胺化低酯果胶性能

利用均匀设计法进行橘皮酰胺化低酯果胶提取的工艺条件试验。考察反应pH、反应时间、反应温度3个因素对酰胺化低酯果胶得率、酰胺化度和酯化度的影响,通过试验数据的偏最小二乘回归分析得到可对酰胺化低酯果胶得率、酰胺化度和酯化度3个指标进行预测的二次多项式数学模型。此数学模型描述各种反应因素与橘皮低酯果胶得率、酰胺化度和酯化度之间的关系,预测得率时有较好的效果,预测酯化度和酰胺化度时存在一定误差。     

Ester Content and Jelly pH Influences on the Grade of Pectins

SUMMARY— A series of samples with percent esterification ranging from 73.7 to 28.6 was prepared under acid conditions at room temperature from lemon peel pectin that had been precipitated with aluminum. Molecular weight, as determined by viscosity in 1% Calgon, and galacturonic acid content remained unaltered during demethylation while equivalent weight decreased. Setting time increased until an ester content of around 50% was reached. At lower ester values setting time decreased again.
Maximum jelly grades were obtained at an ester content of ca. 45%. However, at this ester level the pH at which a high jelly grade was obtained was very low and the grade decreased very rapidly as the jelly pH was increased to values above pH 2.2. The maximum grade obtained with a particular sample decreased and the pH at which this maximum grade could still be obtained increased as the ester content was increased above ca. 45%. Below this ester level, the maximum grade as well as the maximum pH at which this grade could be obtained decreased with ester content.     

酸提工艺对果胶品质的影响

选用福建特产琯溪蜜柚果皮为原料,考察酸提工艺条件对果胶的酯化度、黏均分子质量和半乳糖醛酸含量的影响,设计正交试验L9(34)考察各因素的影响。结果表明:在试验范围内,酸提工艺条件对果胶的酯化度基本无影响,对半乳糖醛酸的含量有明显的影响,对果胶的分子质量影响最显著。9个不同试验条件下,酸提果胶的酯化度63.5%～63.8%,半乳糖醛酸含量74.2%～88.5%,果胶的黏均分子质量101～202ku。     

Prediction of Pectin Yield and Quality by FTIR and Carbohydrate Microarray Analysis

Pectin production is complex, and final product quality assessment is generally accomplished at the end of the process using time-consuming off-line laboratory analysis. In this study, pectin was extracted from lime peel either by acid or by enzymes. Fourier transform infrared spectroscopy and carbohydrate microarray analysis were performed directly on the crude lime peel extracts during the time course of the extractions. Multivariate analysis of the data was carried out to predict final pectin yields. Fourier transform infrared spectroscopy (FTIR) was found applicable for determining the optimal extraction time for the enzymatic and acidic extraction processes, respectively. The combined results of FTIR and carbohydrate microarray analysis suggested major differences in the crude pectin extracts obtained by enzymatic and acid extraction, respectively. Enzymatically extracted pectin, thus, showed a higher degree of esterification (DE 82 %) than pectin extracted by acid (DE 67 %) and was moreover found to be more heterogeneously esterified when probed with the monoclonal antibodies JIM5, JIM7, and LM20. The data infer that enzymatic pectin extraction allows for extraction of complex, high DE pectin, and that FTIR and carbohydrate microarray analysis have potential to be developed into online process analysis tools for prediction of pectin extraction yields and pectin features from measurements on crude pectin extracts.     

Pectin changes in the pre-cooking step of dehydrated mashed potato production

Some in-vivo and in-vitro characteristics of pectin methylesterase (PME) from cell wall and whole potato tuber were determined and its role was elucidated in the pre-cooking and cooling steps of commercial dehydrated mashed potato production. The isolated cell walls contained 16.3% anhydrogalacturonic acid with a degree of esterification (DE) of 56, and 25% of tuber total PME. Cell wall pre-cooking in model systems resulted in a DE of 53.2. Native cell wall pectin solubilisation was much less than that of H-cell walls devoid of metal cations. Calcium but not Mg, supplied as Ca(Mg)-starches, retarded pectin solubilisation, while Ca-uptake by retained pectin was high when cooling followed pre-cooking. Texture measurements of potato slices pre-cooked, cooled and cooked suggested a firming effect which could be attributed to Ca-release from gelatinised starch during pre-cooking, and stabilisation of Cabridges with free COO^? groups of cell wall pectin duringcooling. The role ascribed to PME in causing firming is de-emphasised.     

Changes in Molecular Weight of Pectin During Methylation with Diazomethane

SUMMARY– Acid and enzymatic demethylation procedures suggest that the change in molecular weight during methylation is a result of depolymerization and that a change in the percent methoxyl groups probably has very little effect on the change in molecular weight during methylation or demethylation with pectins having an ester content between 60% and 95%.
Samples of a commercially prepared citrus pectin were acid washed, dissolved and neutralized to different levels with dilute NaOH. These samples were treated with isopropanol to yield an open gel-like precipitate, the alcohol was replaced with ether and the pectin treated with diazomethane at < −30°C. The samples methylated to 70%, 85% and 95% had molecular weight values which decreased with increasing degrees of esterification. Molecular weight was determined by measuring the viscosity of a 0.1 % sol in 1 % Calgon.     

豆腐柴叶低甲氧基果胶提取工艺优化及其加工特性和微观结构研究

采用响应面法研究了提取温度、pH、提取时间和液料比对豆腐柴果胶得率和酯化度(DE)的影响,并对最佳提取条件下的果胶进行了微观结构和加工特性的研究。最佳提取条件为:提取温度90 ℃,pH6,提取时间67 min,液料比24:1 mL/g,果胶得率为17.8%。在最佳条件下获得的果胶为低甲氧基果胶(DE=43.1%),半乳糖醛酸含量为65.8%,具有果胶多糖典型的红外光谱图,扫描电镜显示果胶呈多褶皱的团聚状。其持水力和持油力分别为6.52和6.03 g/g,在2%和4%时的起泡能力分别为52.7%和72.4%,30 min后的泡沫稳定性为18.5%和44.6%。综上所述,豆腐柴叶为低甲氧基酯果胶的良好来源,且具有作为乳化剂、稳定剂、起泡剂用于高脂食品体系感官品质改善的潜在应用价值。