Synthesis and characterization of modified chitosan microspheres: Effect of the grafting ratio on the controlled release of nifedipine through microspheres

The grafting of acrylamide onto a chitosan backbone was carried out at three acrylamide concentrations (polymer/monomer ratio = 1:1, 1:2, and 1:3). The synthesis of the grafted polymer was achieved by K₂S₂O₈‐induced free‐radical polymerization. Microspheres of polyacrylamide‐g‐chitosan crosslinked with glutaraldehyde were prepared to encapsulate nifedipine (NFD), a calcium channel blocker and an antihypertensive drug. The microspheres of polyacrylamide‐g‐chitosan were produced by a water‐in‐oil emulsion technique with three different concentrations of glutaraldehyde as the crosslinking agent. Fourier transform infrared (FTIR) spectroscopy and differential scanning calorimetry (DSC) were used to characterize the grafted copolymers, and the microspheres were prepared from them. FTIR and DSC were also used to analyze the extent of crosslinking. The microspheres were characterized by the particle size; the water transport into these microspheres, as well as the equilibrium water uptake, were studied. Scanning electron microscopy confirmed the spherical nature of the particles, which had a mean particle size of 450 μm. Individual particle dynamic swelling experiments suggested that with an increase in crosslinking, the transport became case II. The release of NFD depended on the crosslinking of the network and on the amount of drug loading. Calculating the drug diffusion coefficients with the initial time and later time approximation method further supported this. The drug release in all 27 formulations followed case II transport, and this suggested that the time dependence of the NFD release followed zero‐order kinetics. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 2940–2949, 2003     

2-氯-5-氯甲基-1,3-噻唑提纯新方法

2-氯-5-氯甲基-1,3-噻唑(CCMT)是一种重要的农药中间体。介绍了以1-异硫氰酸基-2-氯-2-丙烯和氯气反应制备2-氯-5-氯甲基-1,3-噻唑的方法,并重点介绍了通过合成2-氯-5-氯甲基噻唑盐酸盐的方法进行产品提纯的新方法,产品含量大于99%,提纯收率95%。     

相转移催化法合成2-甲氧基-5-乙磺酰基苯甲酸

以4－甲氧基－3－羧基苯磺酰氯为原料，用相转移催化方法合成盐酸舒托必利中间体2－甲氧基－5－乙磺酰基苯甲酸，工艺简便，条件温和。 总收率54％。     

Preparation and characterization of eugenol‐grafted chitosan hydrogels and their antioxidant activities

The hydrogels composed of chitosan and eugenol were prepared to enhance and sustain antioxidant activities. The vinyl groups of eugenol monomer were directly grafted on the amino groups of chitosan, using ceric ammonium nitrate. The graft of eugenol onto chitosan was confirmed by using Fourier‐transform infrared and proton nuclear magnetic resonance spectroscopies. Results from the swelling behavior, thermal stability, and wide‐angle X‐ray diffraction revealed that the equilibrium water content decreased with increase of graft yields, because of the hydrophobicity of eugenol, although the introduction of eugenol as a side chain disturbed the ordered arrangement of chitosan's crystalline structure. The eugenol‐grafted chitosan hydrogels showed lower pH sensitivity in comparison with chitosan alone, because the amino groups, which were pH sensitive, of chitosan were grafted with eugenol. The scavenging activity of the tested hydrogels increased with graft yield of eugenol, because phenolic groups in the eugenol could play a major role as potent free‐radical terminators, in the results of improved antioxidant activity in eugenol‐grafted chitosan hydrogel in comparison with chitosan alone. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 99:3500–3506, 2006     

Rheological study on O−carboxymethylated chitosan/cellulose polyblends from LiCl/N,N‐dimethylacetamide solution

An O?carboxymethylated chitosan (O? CMCh) water solution (I) and N,N‐dimethylacetamide (DMAc) emulsion (II) were blended with a cellulose LiCl/DMAc solution, and corresponding polyblends (Polyblends I and II) were obtained. The rheology of the three fluids, that is, the cellulose solution and Polyblends I and II, was investigated. The cellulose solution was characterized by a power‐law fluid. When an O‐CMCh water solution or DMAc emulsion was added to the cellulose solution, the power‐law curve was preserved. The power‐law indexes (n) of all three fluids increased along with the temperature. Polyblend I displays an n close to but a little higher than that of the cellulose solution, while Polyblend II shows a much higher power index than those of the other two fluids. The values of the apparent viscosity (η_a) for all the three fluids are close and decrease along with an increase in the temperature. Adding O‐CMCh microparticles into Polyblends I and II results in a decrease in the structural viscosity index (Δη) in comparison to that of the cellulose solution, and this effect is very obvious for Polyblend I. A cellulose solution's Δη declines with the augmentation of temperature, while the Δη's of both Polyblends I and II show minimum values at about 323 K. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 1719–1725, 2003     

一种含壳聚糖的有机硅纺织柔软剂的研制

以三甲胺、环氧氯丙烷、壳聚糖为原料，合成了N-壳聚糖季铵盐；并将其与氨基硅油、三种非离子型表面活性剂、一种有机硅两性表面活性剂进行复配，制成了一种新型有机硅柔软剂。经检测，产品的离心稳定性、酸碱稳定性及阴离子型表面活性剂稳定性较好；经其整理的纯棉白布不仅具有良好的柔软性和吸湿性，而且具有一定的抗茵活性。     

壳聚糖对化学镀镍废液中Ni^2＋吸附

研究了用壳聚糖吸附化学镀镍废液中Ni^2＋的最佳条件及其脱附和再生方法，以及镀液中络合剂等其他组分对吸附率的影响。结果表明，壳聚糖对化学镀镍废液中的Ni^2＋具有较好的吸附能力，pH是影响吸附的主要因素。在室温、pH=5．0时，Ni^2＋质量浓度为4．6952g／L的化学镀镍废液被0．9390g壳聚糖吸附2h后，Ni^2＋的去除率达72．25％。     

壳聚糖硫酸盐催化丙酸丁酯的绿色合成研究

研究了丙酸与丁醇在壳聚糖硫酸盐催化剂作用下的酯化反应,考察了反应时间、催化剂用量、醇酸摩尔比等因素对丙酸丁酯酯化率的影响。实验结果表明反应的最佳条件为:丙酸用量为0.1mol,醇酸摩尔比为1.4,壳聚糖硫酸盐用量为1.2g,反应时间为1.5h,酯化率达97.2%,催化剂重复使用5次仍保持较高活性。无污染产生,具有绿色合成的特点。产品经折光率、红外光谱进行了表征。     

改性磁性壳聚糖微球的制备、表征及性能研究

以(NH4)2Fe(SO4)2.6H2O、NH4Fe(SO4)2.12H2O和壳聚糖为原料,经羟丙基化、胺基化,采用一步包埋法制备了一种新型的多胺基化磁性壳聚糖微球。通过正交实验法确定了磁性微球的最佳制备条件,即搅拌速度1200r/min,壳聚糖用量3.0g,环氧氯丙烷用量2.5mL,乙二胺用量2.5mL。并用IR、TG、XRD和SEM对其结构及形貌进行了表征。结果表明,Fe3O4磁性粒子已包埋了一层胺基化壳聚糖。磁性微球胺基含量为2.302mmol/g;呈较规则的球形,平均粒径为209nm,且具有顺磁性和良好的耐酸性。     

壳聚糖固定化脲酶生物传感器选择性测定铜离子

基于重金属对脲酶的抑制作用,研制了用于测定铜离子的生物传感器。该生物传感器的制备以壳聚糖为载体,将脲酶固定于pH电极表面。由于壳聚糖对Cu2+的富集,该生物传感器展现出高灵敏度。在样品溶液中加入5 mmol/L NaI,可以消除Hg2+和Ag+的干扰,从而实现Cu2+的选择性检测。在0.005～0.5μg/mL的浓度范围内,脲酶活性的抑制率与Cu2+浓度的对数呈良好的线性响应关系,其检出限为0.002μg/mL。将使用后的生物传感器浸泡于0.5 mmol/L的EDTA溶液再生5 min,被Cu2+抑制的脲酶的活性可以得到恢复。