羧甲基壳聚糖的制备

以壳聚糖为原料,通过醚化后制得水溶性较好的羧甲基壳聚糖。实验确定的制备羧甲基壳聚糖的最适宜条件为v(异丙醇)∶m(壳聚糖)为10∶1,m(氯乙酸)∶m(壳聚糖)为1.2∶1,反应温度70℃,反应时间2h,碱化时间为1h。     

壳聚糖降解研究的最新进展

壳聚糖是迄今为止发现的天然多糖中唯一的碱性多糖,将壳聚糖降解到需要的分子量是其应用的前提。本文综述了壳聚糖化学降解(酸降解和氧化降解)、物理降解(辐射降解、超声波和微波降解、机械研磨降解、高压均质降解)、酶降解(专一性酶降解、非专一性酶降解、复合酶降解)以及复合降解法的最新进展,供相关领域人员参考。     

酶法降解壳聚糖工艺研究

采用非专一性酶(溶菌酶、纤维素酶)和专一性酶(壳聚糖酶)降解壳聚糖,探讨了不同条件对壳聚糖降解的影响.结果表明,溶菌酶降解壳聚糖的最佳条件为反应时间3.0 h、反应温度50℃、pH值4.0、酶用量40 U·mL-1;纤维素酶降解壳聚糖的最佳条件为反应时间1.5 h、反应温度55℃、pH值5.5、酶用量40 U·mL-1;壳聚糖酶降解壳聚糖的最佳条件为反应时间2.0 h、反应温度45℃、pH值5.0、酶用量30 U·mL-1.对壳聚糖酶酶解产物进行HPLC分析,发现得到了分子量分布较窄的壳寡糖.     

复合酶法提取牡丹种皮黄酮类化合物研究

利用正交实验和单因素实验方法获取复合酶(纤维素酶、半纤维素酶、果胶酶)辅助乙醇提取牡丹种皮中黄酮类化合物的最佳复合酶比例和最佳酶解工艺条件;分析了不同的加酶方式对总黄酮类化合物提取量的影响。结果表明三种复合酶最优比例为(纤维素酶∶半纤维素酶∶果胶酶=4∶1∶3);最佳提取工艺条件为:温度47.5℃、p H=5、酶解1.5 h、液料比20∶1,总黄酮提取量可达64.78 mg/g;最优分步加酶比同时加酶提取量增加了4.58 mg/g,总黄酮提取量可达69.36 mg/g。     

用于酶固定化的多胺化壳聚糖基载体的合成及性能表征

以构建性能优良的壳聚糖基固定化酶载体为目的,用反相悬浮交联法制备了壳聚糖微球,以其作为固定化载体基体,进一步制备了多胺化壳聚糖载体,分别优化了壳聚糖微球环氧化及胺化反应条件。最佳环氧化条件为:n(环氧氯丙烷)∶n(壳聚糖结构单元)=10∶1、50℃反应6 h,环氧基含量达3.32 mmol/g;最佳胺化条件为:n(四乙烯五胺)∶n(环氧基)=15∶1、55℃反应6 h,载体氨基含量可达4.55 mmol/g,高于未胺化微球的2.01mmol/g。用IR、SEM、XRD等对最终产物进行了表征。结果表明,制备的多胺化壳聚糖呈单分散球形,粒径220~300μm,表面较光滑,抗酸性能显著增强。采用该载体对木瓜蛋白酶进行固定化,固定化酶表观活力最高达146 U/g,活力回收率达51%,是采用未经多胺修饰的壳聚糖微球固定化的2~3倍。     

正交实验优化酶解预处理提取银杏叶黄酮和内酯的工艺

采用酶法预处理银杏叶,考察酶用量、酶解时间、酶解温度、pH值对银杏叶总黄酮和总内酯提取率的影响。结果表明,采用复合酶(纤维素酶∶果胶酶=1∶1)、用量为银杏叶的1/300、酶解4.0 h、温度50℃、初始pH为5.0时酶解效果最佳,该工艺条件下,总黄酮提取率为92.38%,总内酯提取率为91.74%。     

正交实验优化酶解预处理提取银杏叶黄酮和内酯的工艺

采用酶法预处理银杏叶,考察酶用量、酶解时间、酶解温度、pH值对银杏叶总黄酮和总内酯提取率的影响。结果表明,采用复合酶(纤维素酶∶果胶酶=1∶1)、用量为银杏叶的1/300、酶解4.0 h、温度50℃、初始pH为5.0时酶解效果最佳,该工艺条件下,总黄酮提取率为92.38%,总内酯提取率为91.74%。     

壳聚糖-海藻酸钠微球固定化木瓜蛋白酶的工艺研究

以壳聚糖和海藻酸钠为原材料,采用乳化交联法制备空白微球,通过戊二醛固定木瓜蛋白酶,以固定化木瓜蛋白酶的活性回收率作为最终测定指标,并以星点设计-效应面法优化实验条件。通过一系列的实验,结果表明最优条件为:固定化时间是4 h,壳聚糖与海藻酸钠的质量配比(m/m)为5∶5、加酶量为700 U/mL、戊二醛浓度为1. 0%、固定化温度为40℃。木瓜蛋白酶的固定化效果良好,木瓜蛋白酶活性回收率为68. 9%。     

掺锌壳聚糖气凝胶的制备与表征

以壳聚糖作为模板剂,氯化锌作为前驱物通过溶胶-凝胶法制备出湿凝胶,经二氧化碳超临界干燥得到掺锌壳聚糖气凝胶。通过场发射扫描电镜(FESEM)和N2吸/脱附测试对气凝胶的微观结构和性能进行了表征。结果表明:掺锌壳聚糖气凝胶具有明显的三维纳米多孔结构;壳聚糖的含量对气凝胶的微观结构影响明显;当m(壳聚糖)∶m(氯化锌)=1∶1时,气凝胶骨架纤细,比表面积460 m2/g,平均孔径分布在3～10 nm。     

藜麦蛋白提取工艺优化及抗氧化活性研究

研究了藜麦蛋白提取的最佳工艺条件及抗氧化活性。以藜麦种子为原料,通过纤维素酶和糖化酶对其蛋白质进行复合酶解提取。以蛋白质的提取率为考察指标,在单因素试验的基础上,固定酶配比,利用响应面试验进行优化。得到最佳提取条件为:酶配比[m(纤维素酶)∶m(糖化酶)]为4∶6、酶解时间为70. 59 min、酶解温度为50. 06℃、pH为5. 03、总加酶量为427. 18 U/g,通过验证实验得到的蛋白质提取率为76. 82%。在此条件下得到的藜麦蛋白具有清除DPPH自由基、羟自由基的能力,说明藜麦蛋白具有一定的抗氧化活性。     

有机相中壳聚糖-海藻酸固定化脂酶的特性

研究了壳聚糖 海藻酸固定化脂酶在有机相反应中的稳定性与活性。考察了凝胶时间、壳聚糖浓度及壳聚糖分子质量对固定化脂酶包埋率与活性的影响 ,确定了适宜 pH值与批反应时间。同时讨论了溶剂极性和操作时间对固定化酶稳定性的影响。测定了固定化脂酶水解橄榄油反应的动力学参数。结果表明 ,壳聚糖 海藻酸聚电解质膜可提高固定化酶的包埋率与稳定性     

壳聚糖及丁二酸酐酰化壳聚糖双氧水降解行为的研究

在简单均相体系下．研究了壳聚糖及丁二酸酐酰化壳聚糖在双氧水中的降解特性。采用鸟氏粘度计，利用一点法测量了降解过程中壳聚糖及丁二酸酐酰化壳聚糖的分子量，讨论了该体系下壳聚糖及丁二酸酐酰化壳聚糖的降解速率．通过红外光谱分析了双氧水对低分子量壳聚糖和低分子量丁二酸酐酰化壳聚糖结构的影响。结果表明．在该体系下·壳聚糖及丁二酸酐酰化壳聚糖的降解主要发生在反应开始后的2～3h内．此后降解产物的分子量逐渐趋于20000；相同条件下，丁二酸酐酰化壳聚糖的降解程度高于壳聚糖；红外光谱表明．采用该降解体系制备的降解产物主链结构基本没有发生变化。     

Effect of degree of deacetylation on solubility of low‐molecular‐weight chitosan produced via enzymatic breakdown of chitosan

Chitosan has emerged as a unique biomaterial, possessing scope in diverse applications in the biomedical, food and chemical industries. However, its high molecular weight is a concern when handling the polymer. Various techniques have been explored for depolymerization of this polymer, wherein enzymes have emerged as the most economic method having minimum degrading effect on the polymer and resulting in formation of side products. Chitosan can be depolymerized using a broad range of enzymes. In this study, various enzymes like α‐amylase, papain, pepsin and bromelain were employed to depolymerize chitosan and convert it into its lower molecular weight counterpart. Further, attempts were made to elucidate the process of depolymerization of chitosan, primarily by determining the change in its viscosity and hence its molecular weight. The process of depolymerization was optimized using a one‐factor‐at‐a‐time approach. The molecular weight of the resultant chitosan was estimated using gel permeation chromatography and infrared spectroscopy. These studies revealed a considerable decrease in molecular weights of chitosan depolymerized by pepsin, papain, bromelain and α‐amylase, resulting in recovery of the low‐molecular‐weight chitosan of 76.09 ± 5, 74.18 ± 5, 55.75 ± 5 and 49.18 ± 5%, respectively. Maximum yield and depolymerization were obtained using pepsin and papain due to their enzymatic recognition pattern, which was also validated using studies involving molecular dynamics. © 2019 Society of Chemical Industry     

降解壳聚糖的亚麻织物防皱整理作用研究

采用不同组分的降解壳聚糖作为亚麻织物无甲醛防皱整理剂,通过织物折皱回复率、白度、断裂强力保留率、断裂伸长率的变化,探讨降解壳聚糖用量及相对分子质量对整理效果的影响。实验结果显示,平均聚合度为9.787,平均相对分子质量为1 590.15,w(整理剂)%1%的降解壳聚糖进行亚麻织物整理后,折皱回复率为30.15%,白度为57.900%,断裂强力保留率为96.47%,断裂伸长率为12.73%。     

Effect of immobilized neutral protease on the preparation and physicochemical properties of low molecular weight chitosan and chito‐oligomers

Neutral protease was immobilized on glutaraldehyde‐pretreated N‐succinyl chitosan hydrogel beads and the biocatalyst obtained was used for the preparation of low molecular weight chitosan and chito‐oligomers with molecular weight of 1.9–23.5 kDa from commercial chitosan. Factors affecting the chitinolytic hydrolysis were described. The degradation was monitored by gel permeation chromatography. The structure of degraded chitosan was characterized by Fourier transform infrared, X‐ray diffraction and liquid chromatography‐mass spectrometry. Immobilized neutral protease showed optimal depolymerization at pH 5.7 and 50°C. The degree of deacetylation of the hydrolysates did not change compared to that of the initial chitosan. The decrease of molecular weight led to transformation of crystal structure but the chemical structures of residues were not modified. The degree of polymerization of chito‐oligomers was mainly from 3 to 8. The method allows cyclic procedures of immobilized enzyme and N‐succinyl chitosan support utilization, and is suitable for a large‐scale production of the low molecular weight chitosan and chito‐oligomers free of protein admixtures. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102:4185–4193, 2006     

明胶与壳聚糖复凝聚过程的研究

本文研究了四种明胶与两种壳聚糖组成的体系的复凝聚过程,对于复凝聚过程的主要影响参数(pH值、配比和盐类)与体系复凝聚产率的关系进行了探讨。发现选用二价金属盐类对体系复凝聚产率的影响明显不同于一价金属盐类,少量CaCl_2(≯0.30％)的加入可提高复凝聚产率;具有高冻力的RT-52354和RT-53808两种明胶较适用于进行复凝聚;采用分子量大、脱乙酰度较低(-NH_2含量较少)的壳聚糖有利于提高复凝聚产率;并且对上述两种明胶与壳聚糖体系确定了比较适宜的复凝聚条件。     

Medicated wound dressings based on poly(vinyl alcohol)/poly(N‐vinyl pyrrolidone)/chitosan hydrogels

Poly(vinyl alcohol)/poly(N‐vinyl pyrrolidone) (PVP)/chitosan hydrogels were prepared by a low‐temperature treatment and subsequent ⁶⁰Co γ‐ray irradiation and then were medicated with ciprofloxacin lactate (an antibiotic) and chitosan oligomer (molecular weight = 3000 g/mol). The gel content, swelling ratio, tensile strength, and crystallinity of the hydrogels were determined. The effects of the chitosan molecular weight, the low‐temperature treatment procedure, and the radiation dosage on the hydrogel properties were examined. The molecular weight of chitosan was lowered by the irradiation, but its basic polysaccharide structure was not destroyed. Repeating the low‐temperature treatment and γ‐ray irradiation caused effective physical crosslinking and chemical crosslinking, respectively, and contributed to the mechanical strength of the final hydrogels. The incorporation of PVP and chitosan resulted in a significant improvement in the equilibrium swelling ratio and elongation ratio of the prepared hydrogels. The ciprofloxacin lactate and chitosan oligomer were soaked into the hydrogels. Their in vitro release behaviors were examined, and they were found to follow diffusion‐controlled kinetics. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 2453–2463, 2006     

Preparation and characterization of poly(ethylene glycol) crosslinked chitosan films

Poly(ethylene glycol) (PEG) crosslinked chitosan films with various PEG to chitosan ratio and PEG molecular weight were successfully prepared via the epoxy‐amine reaction between chitosan and PEG‐epoxy. The thermal and mechanical properties and swelling behavior were studied for the PEG crosslinked chitosan films. The mechanical strength of chitosan films were greatly enforced by the introduction of PEG‐epoxy, achieving an elongation of about 80%. It was found that the crosslinked chitosan films form hydrogel in water, achieving a swelling ratio higher than 20 times of original weight. The swelling behavior of chitosan films relied greatly on the molecular weight of the crosslinker PEG‐epoxy and the weight percent of PEG‐epoxy. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2008     

Valorization of chitins extracted from North Morocco shrimps: Comparison of chitin reactivity and characteristics

Huge quantities of waste discharged by the gray and pink shrimp decortication units in the North of Morocco can be valorized by producing about 950 tons of pure chitin, which can be transformed into 700 tons of highly to totally deacetylated chitosan. During the preparation of chitin and chitosan from gray and pink shrimps, differences in reaction behavior were observed even though these are taxonomically close species. The presented results concern several chitinous sources, and they show that the progress in the N-deacetylation reactions of chitin would be linked to the crystallinity index of the starting chitin. Following the kinetic study of the polymer hydrolysis during N-deacetylation, the difference in the molecular weights of the chitosan samples obtained under identical reaction conditions was related to the differences between molecular weights of the native chitin, 478 000 g.mol⁻¹ for pink shrimp and 562 000 for gray shrimp. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47804.     

Effect of preparation method and characteristics of chitosan on the mechanical and release properties of the prepared capsule

The objective of this study is to elucidate the effect of preparation method and the characteristics of chitosan used on the mechanical and release properties of the prepared capsule. The characteristics of the chitosan explored include molecular weight (1.8, 5.6, 20.2, and 31.8 × 10⁵ Dalton) and chain flexibility parameter (B), which was manipulated by a varying degree of deacetylation (DD, 67.9, 81.3, 90.5, and 92.2%), and sodium chloride concentration (0 or 0.3%). The orifice method was used to encapsulate hemoglobin, whereas complex coacervation was used to encapsulate the bovine serum albumin (BSA). The axial ratio was measured to characterize the appearance of the capsule. Break strength was used as an index of mechanical strength. Release percent of protein was used as a pore size indicator. The results show axial ratio and hemoglobin release percent of the capsule prepared by the orifice method increased with the increase of the chain flexibility parameter (B), but decreased with the increase of the chitosan molecular weight. However, break force behaved just opposite from that of the axial ratio and release percent of hemoglobin. The capsule cannot be prepared from 92.2% DD chitosan. Break strength and BSA release percent of the capsule prepared by complex coacervation did not vary with different DD, molecular weight of chitosan, and sodium chloride concentration. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 66: 161–169, 1997