芦苇浆纳米纤维素超声法制备工艺优化及表征

以芦苇浆为原料,采用超声辅助硫酸水解法制备了纳米纤维素.在单因素实验的基础上,响应面法优化纳米纤维素制备工艺条件,结果表明最佳制备工艺条件为超声时间32 min,硫酸浓度52％,反应温度54℃,纳米纤维素得率最高(78.67％);通过傅里叶变换红外(FTIR)、X射线衍射和透射电子显微镜(TEM)对最佳工艺条件制备的纳米纤维素进行性能表征,分析表明最佳工艺条件制备的纳米纤维素聚集态结构为纤维素Ⅰ型,呈棒状.     

扫描电镜技术在微晶纤维素的吸附性能研究中的应用

本文介绍了８１２树脂包埋微晶纤维素（ＭＣＣ）然后进行台面腐蚀的扫描电镜样品制备的方法，此方法制备了ＭＣＣ样品可在扫描电镜下观察到其内部的微观变化，是进行微晶纤维素吸附性能研究的理想方法。     

L-谷氨酸氧化酶与CBD的融合表达及其在微晶纤维素上固定化分析

酶的固定化作为一种重要的技术,已在生物催化领域得到了广泛的应用。现将来源于普拉特链霉菌3304(Streptomyces platensis NTU3304)产生的胞外L-谷氨酸氧化酶(L-glutamate oxidase,Gox)基因gox融合到来源于粪碱纤维单胞菌Cellulomonas fimi的纤维素结合域(CBDcex)的基因上,构建表达载体p ETM10-Gox-CBD,并在大肠杆菌中表达。通过蛋白纯化获得融合蛋白,并命名为Gox-CBD。利用CBD对微晶纤维素特异性吸附的特性将其固定在微晶纤维素上,并对固定化酶的制备条件、结合量、酶学性质及其微晶纤维素结合稳定性等进行了研究。在4℃条件下结合约1 h,融合蛋白Gox-CBD结合在纤维素上的结合量即可达到9.0 mg/g。通过对重组型、融合表达游离的以及固定化在微晶纤维素上的谷氨酸氧化酶的酶学性质进行比较发现,固定化酶的比酶活有所降低;但固定化酶的热稳定性相对于游离酶有了很大的提高,在60℃孵育30 min后还保留有约70%的活性,而游离的重组Gox在相同条件下几乎完全失去活性。当固定化结合蛋白在p H10或者盐浓度5 mmol/L的Na Cl条件下可以牢固结合。并且可以通过一步纯化方法固定化融合蛋白Gox-CBD于微晶纤维素上。因此,L-谷氨酸氧化酶与纤维素结合域融合表达的研究为蛋白的纯化及酶的固定化提供了一种新策略。     

以四甲基氢氧化铵为溶剂的磁性纤维素微球制备、表征及应用

以微晶纤维素和磁性Fe_3O_4纳米粒子为原料,四甲基氢氧化铵溶液为溶剂,通过乳化法制备了磁性纤维素微球。利用扫描电微镜、傅里叶变换红外光谱仪、X线衍射仪、振动样品磁强度计、比表面和孔径分析仪对磁性纤维素微球进行分析表征,结果表明磁性纤维素微球确为纤维素包裹Fe_3O_4纳米粒子形成,且表面粗糙,粒径约200 nm,比表面积13.6 m~2/g,表面微孔体积为0.5 cm~3/g,磁强度为2.0×10~(-3) T/g。磁性纤维素微球染料吸附试验表明,在pH 4～8时其对亚甲基蓝的去除率最大,达到70%以上。     

SO_3联合NH_3预处理稻草秸秆制备微晶纤维素

以稻草秸秆为原料考察SO3、NH3、SO3/NH3和NH3/SO3联合稀碱4种预处理方法制备稻草微晶纤维素(MCC)的可能性,并且选择出最优的制备方法,即SO3联合NH3预处理法制备稻草微晶纤维素。同时,利用X线衍射仪(XRD)和扫描电子显微电镜(SEM)等分析稻草MCC的结构。结果表明:预处理后的稻草秸秆中大部分木质素和半纤维素得到去除,制备得到的稻草微晶纤维素结晶度达到87.5%,并且所得的MCC产品仍然具有完整的纤维素链的结构和晶型。     

不同纤维素原料超临界水解的研究

分别以稻草秸秆、经预处理的稻草秸秆、脱脂棉、微晶纤维素和定性滤纸为原材料,利用间歇式的超临界反应设备,在400℃的盐浴中进行木质纤维素的超临界水解,采用3,5-二硝基水杨酸(DNS)法对产物中的还原糖进行测定,研究反应时间对不同纤维素原料水解产糖的影响。结果表明:在超临界条件下,不同原料在较短的时间内还原糖含量均出现峰值,随着反应时间的延长还原糖产量呈现下降的趋势;稻秆、预处理后的稻秆、脱脂棉、微晶纤维素和定性滤纸的最大产糖量分别为7.42、9.05、12.55、18.01和14.24 g/L;与此对应的最佳反应时间分别为3.5、4、3、3、4 min;对应的最大还原糖产率分别为14.84%、18.10%、25.10%、36.02%、28.48%。     

纳米生物活性玻璃的制备及其对人成纤维细胞增殖性能的影响

该文采用溶胶–凝胶结合碱性共沉淀法和冷冻干燥技术制备纳米生物活性玻璃(NBG),通过SEM、TEM、激光粒度考察NBG的形貌、分散性和粒径,并通过四唑盐比色法(MTT)研究其浸提液对人成纤维细胞(HDF)增殖性能的影响。结果显示, NBG颗粒粒径小于50 nm,激光粒度仪检测到的平均粒径为491.8 nm,相比于溶胶–凝胶生物活性玻璃(SGBG), NBG平均粒径更小,分散性更好。NBG与SGBG浸提液在5倍、10倍和15倍稀释的浓度下均有利于HDF的增殖,但SGBG在早期稍有利于细胞增殖但作用不明显,而NBG则在后期对细胞增殖作用更显著,因此NBG在创面修复方面更具有应用前景。     

响应面法优化酪蛋白酸钠-豌豆分离蛋白纳米乳液制备工艺

通过超声处理技术制备酪蛋白酸钠—豌豆分离蛋白纳米乳液,并利用响应面优化法确定了最优制备工艺为豌豆分离蛋白添加量4%（w/v）、酪蛋白酸钠添加量4%（w/v）、超声功率400 W、超声时间5min,此条件下,酪蛋白酸钠—豌豆蛋白纳米乳液的平均粒径为149.82 nm、TSI为3.008、乳化产率为91.28%。     

以米糠蛋白为乳化剂的β-胡萝卜素纳米乳液超声乳化制备工艺优化

为提高米糠蛋白的利用价值及应用意义,本研究拟采用超声乳化法制备以米糠蛋白为乳化剂的β-胡萝卜素纳米乳液,本研究采用响应面优化法获取了米糠蛋白纳米乳液超声乳化制备工艺:超声温度50℃,超声功率490 W,超声时间280 s和米糠蛋白浓度4.5%,在此条件下米糠蛋白纳米乳液的平均粒径为190 nm,乳化产率为88.1%,兼具较强的稳定性。研究结果将为新型功能性食品、纳米食品的开发提供技术途径及研发思路。     

对硝基苯硫酚分子内嵌的星形表面增强拉曼散射金 "套娃 "纳米颗粒用于肿瘤拉曼影像的初步研究

目的:制备对硝基苯硫酚(4-Nitrobenzenethiol,4-NBT)分子内嵌的星形表面增强拉曼散射(Surface enhanced Raman Scattering,SERS)金"套娃"纳米颗粒,测定其拉曼增强效果和应用于细胞以及活体肿瘤拉曼影像的可行性。方法:以种子介导法先后制备金纳米星及星形SERS金"套娃"纳米颗粒,采用透射电镜观察其形貌,激光粒度分析仪测定其粒径及Zeta电位,拉曼光谱仪测定其拉曼光谱,考察其对A549细胞的拉曼成像效果,建立A549皮下瘤模型,考察其对活体皮下瘤的成像效果。结果:制备并优化的金纳米星粒径较小,为60.5 nm,其针尖密度较高,以此为核心制备的星形SERS金"套娃"纳米颗粒形态规整,粒径约为66.7nm,Zeta电位约为-16.6 m V,拉曼增强效果提升至其前驱体金纳米星的5.3倍,能够实现对A549细胞及A549皮下瘤的拉曼成像。结论:所制备的星形SERS金"套娃"纳米颗粒形态规整均一,拉曼增强效果较好,能实现对细胞及活体肿瘤的拉曼影像。     

Spherical composite particles of rice starch and microcrystalline cellulose: A new coprocessed excipient for direct compression

Composite particles of rice starch (RS) and microcrystalline cellulose were fabricated by spray-drying technique to be used as a directly compressible excipient. Two size fractions of microcry stalline cellulose, sieved (MCS) and jet milled (MCJ), having volumetric mean diameter (D₅₀) of 13.61 and 40.51 μm, respectively, were used to form composite particles with RS in various mixing ratios. The composite particles produced were evaluated for their powder and compression properties. Although an increase in the microcrystalline cellulose proportion imparted greater compressibility of the composite particles, the shape of the particles was typically less spherical with rougher surface resulting in a decrease in the degree of flowability. Compressibility of composite particles made from different size fractions of microcrystalline cellulose was not different; however, using MCJ, which had a particle size range close to the size of RS (D₅₀=13.57 μm), provided more spherical particles than using MCS. Spherical composite particles between RS and MCJ in the ratio of 7∶3 (RS-MCJ-73) were then evaluated for powder properties and compressibility in comparison with some marketed directly compressible diluents. Compressibility of RS-MCJ-73 was greater than commercial spray-dried RS (Eratab), coprocessed lactose and microcrystalline cellulose (Cellactose), and agglomerated lactose (Tablettose), but, as expected, lower than microcrystalline cellulose (Vivapur 101). Flowability index of RS-MCJ-73 appeared to be slightly lower than Eratab but higher than Vivapur 101, Cellactose, and Tablettose. Tablets of RS-MCJ-73 exhibited low friability and good self-disintegrating property. It was concluded that these developed composite particles could be introduced as a new coprocessed direct compression excipient.     

Direct pelletization in a rotary processor controlled by torque measurements. III. Investigation of microcrystalline cellulose and lactose grade

The aim of the present study was to investigate the use of different grades of microcrystalline cellulose (MCC) and lactose in a direct pelletization process in a rotary processor. For this purpose, a mixed 2- and 3-level factorial study was performed to determine the influence of the particle size of microcrystalline cellulose (MCC), (≈60 and 105 μm) and lactose (≈30, 40, and 55 μm), as well as MCC type (Avicel and Emcocel) on the pelletization process and the physical properties of the prepared pellets. A 1∶4 mixture of MCC and lactose was applied, and granulation liquid was added until a 0.45 Nm increase in the torque of the friction plate was reached. All combinations of the 3 factors resulted in spherical pellets of a high physical strength. The particle size of MCC was found to have no marked effect on the amount of water required for agglomerate growth or on the size of the resulting pellets. An increasing particle size of lactose gave rise to more spherical pellets of a more narrow size distribution as well as higher yields. The MCC type was found to affect both the release of the model drug from the prepared pellets and the size distribution. Generally, the determined influence of the investigated factors was small, and direct pelletization in a rotary processor was found to be a robust process, insensitive to variations in the particle size and type of MCC and the particle size of lactose. Published: October 24, 2005     

Powder and mechanical properties of microcrystalline cellulose with different degrees of polymerization

This study investigated the influence of the degree of polymerization (DP) of cellulose materials (microcrystalline cellulose [MCC]) on some powder properties and the compression behavior of these materials. The DP was determined by measurements of viscosity (H). The weight average of molecular weight and the weight average of the different DPs were investigated after MCC was modified to cellulose tricarbanilate by light scattering measurements. The DP showed a remarkable influence on the physicochemical properties of the cellulose materials and, consequently, on the behavior of these materials during compression. MCC types with a high DP value showed greater water absorption than the types with a low DP value. No relevant relationship between the crystallinity index and the DP could be observed. DP 190 showed lower compactibility and compressibility parameters than DP 244 and 299. No significant differences could be observed between DP 244 and 299 when the same particle size fraction was compressed. Furthermore, the compressibility was increased by increasing the DP.     

Major characteristics of the cellulolytic system of Clostridium thermocellum coincide with those of the purified cellulosome

The properties of the cellulosome (a cellulose-binding, multiple cellulase-containing protein complex isolated from Clostridium thermocellum) have been compared with the previously reported characteristics for crude cellulase [see 1,4-(1,3;1,4)-β-d-glucan 4-glucanohydrolase, EC 3.2.1.4] preparations. Similar to the crude enzyme system, true cellulolytic activity was demonstrated for the purified cellulosome on the basis of extensive solubilization of microcrystalline cellulose. The cellulolytic activity of the purified cellulosome was enhanced both by calcium ions and by thiols, and was inhibited by cellobiose (the major end product of the cellulosome-mediated cellulose degradation). In addition, at low ionic strength, cellulose-adsorbed cellulosome was detached intact from the cellulose matrix. Using controlled conditions, maximum enzymatic activity was shown to correspond to suboptimal conditions of cellulosome adsorption to cellulose. The results suggest that previous data accumulated for the crude cellulase system in C. thermocellum essentially reflect the contribution of the cellulosome.     

裂褶菌纤维二糖脱氢酶吸附纤维素性质

纤维二糖脱氢酶（ＣＤＨ）可以吸附棉花、微晶纤维素和酸处理纤维素,４ｍｉｎ便都达到平衡。与纤维素酶明显不同,该酶的Ｓｃａｔｃｈａｒｄ吸附曲线都是一条直线,为典型的单结合位点模型（ｏｎｅ－ｂｉｎｄｉｎｇ－ｓｉｔｅ ｍｏｄｅｌ）。观察到ｐＨ值、温度、乙二醇和ＮａＣｌ对ＣＤＨ吸附微昌纤维素有影响,并进行了讨论。     

Effect of beating on recycled properties of unbleached eucalyptus cellulose fiber

The effects of beating on recycled properties of eucalyptus cellulose fiber were studied by analyzing the changes of morphological parameters (fiber length and the fines content), physical properties (tensile strength, breaking length and the stretch), WRV, crystal structure of cellulose and pore structure of cellulose fiber. The results showed that beating caused the fine content increase. Tensile strength, breaking length and the stretch increased with the increasing beating time. WRV of the first cycle beaten eucalyptus pulp was increased by 32.1%, compared to the first cycle unbeaten pulp. WRV increased with the increase in beating degree. However, crystallinity of cellulose increased, and then decreased with an increase in beating degree. FTIR spectra showed that there were no drastic changes in the functional groups of the eucalyptus pulp cellulose during beating. Fiber pore size was gradually diverted into macropore with the increase in beating degree, resulting in the mean pore volume increased.     

Ultrasound mediated enzymatic hydrolysis of cellulose and carboxymethyl cellulose

A recombinant Trichoderma reesei cellulase was used for the ultrasound‐mediated hydrolysis of soluble carboxymethyl cellulose (CMC) and insoluble cellulose of various particle sizes. The hydrolysis was carried out at low intensity sonication (2.4–11.8 W cm^?2 sonication power at the tip of the sonotrode) using 10, 20, and 40% duty cycles. [A duty cycle of 10%, for example, was obtained by sonicating for 1 s followed by a rest period (no sonication) of 9 s.] The reaction pH and temperature were always 4.8 and 50°C, respectively. In all cases, sonication enhanced the rate of hydrolysis relative to nonsonicated controls. The hydrolysis of CMC was characterized by Michaelis‐Menten kinetics. The Michaelis‐Menten parameter of the maximum reaction rate V_max was enhanced by sonication relative to controls, but the value of the saturation constant K_m was reduced. The optimal sonication conditions were found to be a 10% duty cycle and a power intensity of 11.8 W cm^?2. Under these conditions, the maximum rate of hydrolysis of soluble CMC was nearly double relative to control. In the hydrolysis of cellulose, an increasing particle size reduced the rate of hydrolysis. At any fixed particle size, sonication at a 10% duty cycle and 11.8 W cm^?2 power intensity improved the rate of hydrolysis relative to control. Under the above mentioned optimal sonication conditions, the enzyme lost about 20% of its initial activity in 20 min. Sonication was useful in accelerating the enzyme catalyzed saccharification of cellulose. © 2013 American Institute of Chemical Engineers Biotechnol. Prog., 29:1448–1457, 2013     

Effect of particle size on the rate of enzymatic hydrolysis of cellulose

The effect of particle size on enzymatic hydrolysis of cellulose has been investigated. The average size of microcrystalline cotton cellulose has been reduced to submicron scale by using a media mill. The milled products were further subjected to hydrolysis using cellulase. High cellulose concentration (7%) appeared to retard the size reduction and resulted in greater particles and smaller specific surface areas than those at low concentration (3%) with the same milling time. Initial rate method was employed to explore the rate of enzymatic hydrolysis of cellulose. The production rate of cellobiose was increased at least 5-folds due to the size reduction. The yield of glucose was also significantly increased depending upon the ratio of enzyme to substrate. A high glucose yield (60%) was obtained in 10-h hydrolysis when the average particle size was in submicron scale.     

Biohydrogen generation by mesophilic anaerobic fermentation of microcrystalline cellulose

Sixteen batch experiments were performed to evaluate the stability, kinetics, and metabolic paths of heat-shocked digester (HSD) sludge that transforms microcrystalline cellulose into hydrogen. Highly reproducible kinetic and metabolic data confirmed that HSD sludge could stably convert microcrystalline cellulose to hydrogen and volatile fatty acids (VFA) and induce metabolic shift to produce alcohols. We concluded that clostridia predominated the hydrogen-producing bacteria in the HSD sludge. Throughout this study the hydrogen percentage in the headspace of the digesters was greater than 50% and no methanogenesis was observed. The results emphasize that hydrogen significantly inhibited the hydrogen-producing activity of sludge when initial microcrystalline cellulose concentrations exceeded 25.0 g/L. A further 25 batch experiments performed with full factorial design incorporating multivariate analysis suggested that the ability of the sludge to convert cellulose into hydrogen was influenced mainly by the ratio of initial cellulose concentration (So) to initial sludge density (Xo), but not by interaction between the variables. The hydrogen-producing activity depended highly on interaction of So x (So/Xo). Through response surface analysis it was found that a maximum hydrogen yield of 3.2 mmol/g cellulose occurred at So = 40 g/L and So/Xo = 8 g cellulose/g VSS. A high specific rate of 18 mmol/(g VSS-d) occurred at So = 28 g/L and So/Xo = 9 g cellulose/g VSS. These experimental results suggest that high hydrogen generation from cellulose was accompanied by low So/Xo.     

Importance of Small Pores in Microcrystalline Cellulose for Controlling Water Distribution during Extrusion–Spheronization

The purpose of this research was to investigate the effects of particle size on the wet massing behavior of microcrystalline cellulose (MCC). In this study, a series of six fractionated MCC grades were customized and specially classified to yield different particle size varieties of the standard grade, Comprecel M101. All seven MCC grades were extensively characterized for the physical properties and wet massing behavior using mixer torque rheometry. Effects of MCC physical properties on the maximum torque (Torque_max) were determined using partial least squares (PLS) analysis. Most physical properties varied systematically with particle size and morphological changes. Marked differences were observed in the small pore volumes (V _highP) and BET surface areas of the MCC grades. Variables that exerted dominant influences on Torque_max were identified. In particular, the significance of V _highP in governing wet mass consistency was established. The role of V _highP has not been reported in any study because this small but significant variation is likely to be obliterated or compensated by variation in other physical properties from MCC grades from different suppliers. The findings demonstrated the role of small pores in governing the wet mass consistency of MCC and provide a better understanding of MCC’s superior performance as a spheronization aid by the ability to fulfill the function as a molecular sponge to facilitate pellet formation during wet granulation processes.