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比较并分析壳聚糖脱乙酰度的两种测定方法。通过一组正交试验来制备不同脱乙酰度的壳聚糖,同时采用碱量法和紫外分光光度法进行脱乙酰的测定。分别从测定的原理和影响因素进行比较分析并进行测定结果的t检验。碱量法操作简便,但干扰因素多,结果重现性差;紫外分光光度法干扰因素少,客观、准确,结果重现性好。两种方法测定的结果存在一定差异。 相似文献
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分别采用差示扫描量热法与红外吸收光谱法直接测定壳聚糖脱乙酰度,试验表明选择差示扫描量热曲线295℃处放热分解峰峰面积作为计算参数的结果与红外吸收光谱中A1320/A1420计算结果无统计学显著性差异,同时两种分析方法操作简便,分析时间短,故可满足相关工业生产实时分析要求。 相似文献
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甲壳素制备壳聚糖脱乙酰度可控性的研究 总被引:1,自引:0,他引:1
介绍了甲壳素(ehintin)和壳聚糖(ehitosan)的性质、用途及发展前景;分析了国内外对壳聚糖的研究状况及取得的成果;描述了制备壳聚糖的实验原理;初步研究了在保证能获得大分子量的情况下提高壳聚糖的脱乙酰度的实验方法;介绍了测定壳聚糖脱乙酰基的实验方法;分析了影响壳聚糖脱乙酰度(Degree of Deacetylation缩写:D.D.)的主要因素。 相似文献
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双突跃电位滴定法测定壳聚糖脱乙酰度 总被引:19,自引:0,他引:19
用 Microsoft Excel研究了电位滴定法测定壳聚糖的脱乙酰度的滴定曲线 ,利用两个突跃之间的氢氧化钠的用量计算了脱乙酰度。该方法具有准确可靠 ,重复性好等优点 ,相对标准偏差小于 0 .9%。 相似文献
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The objective of the study was to explore the effect of the degree of deacetylation (DD) of the chitosan used on the degradation rate and rate constant during ultrasonic degradation. Chitin was extracted from red shrimp process waste. Four different DD chitosans were prepared from chitin by alkali deacetylation. Those chitosans were degraded by ultrasonic radiation to different molecular weights. Changes of the molecular weight were determined by light scattering, and data of molecular weight changes were used to calculate the degradation rate and rate constant. The results were as follows: The molecular weight of chitosans decreased with an increasing ultrasonication time. The curves of the molecular weight versus the ultrasonication time were broken at 1‐h treatment. The degradation rate and rate constant of sonolysis decreased with an increasing ultrasonication time. This may be because the chances of being attacked by the cavitation energy increased with an increasing molecular weight species and may be because smaller molecular weight species have shorter relaxation times and, thus, can alleviate the sonication stress easier. However, the degradation rate and rate constant of sonolysis increased with an increasing DD of the chitosan used. This may be because the flexibilitier molecules of higher DD chitosans are more susceptible to the shear force of elongation flow generated by the cavitation field or due to the bond energy difference of acetamido and β‐1,4‐glucoside linkage or hydrogen bonds. Breakage of the β‐1,4‐glucoside linkage will result in lower molecular weight and an increasing reaction rate and rate constant. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 3526–3531, 2003 相似文献
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红外光谱法测定壳聚糖脱乙酰度 总被引:4,自引:0,他引:4
以碱量法为对比方法,考察了基于A1655/A3450和A1320/A1420的2种红外光谱计算壳聚糖脱乙酰度方法的准确性。结果表明,红外光谱法虽精密度低于碱量法,但基于A1655/A3450的红外测试结果与碱量法基本相吻合;基于A1320/A1420加的红外光谱计算结果略高于碱量法,与商家标注值相吻合,且不受样品含少量水、残酸或残碱的影响。红外光谱法是一种较为理想的壳聚糖脱乙酰度测定方法,同时采用A1655/A3450和A1320/A1420计算更利于得到准确的测定结果。 相似文献
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The objective of the study is to elucidate the effect of reaction time and temperature during heterogenous alkali reaction on degree of deacetylation (DD) and molecular weight (MW) of the resulting chitosans, and to establish the reaction conditions to obtain desired DD and MW chitosan products. Chitin was extracted from red shrimp process waste. DDs and MWs were determined by infrared spectroscopy (IR) and static light scattering, respectively. The results are as follow: The DD and MW of chitin obtained were 31.9% and 5637 kDa, respectively. The DD of the resulting chitosan increased along with reaction time and/or reaction temperature. The DDs of the resulting chitosan that were obtained from 140°C were higher than those reacted at 99°C. The highest DD of the resulting chitosans after alkali deacetylation at 99 and 140°C were 92.2 and 95.1%, respectively. The DDs of chitosans increased fast at the beginning of reaction process then slowed over time. The reaction rate and rate constant of the deacetylation reaction decreased with increasing DD of the reactant. The MWs of chitosans decreased along with the deacetylation time. MW of those chitosans reacted at 140°C are smaller than those at 99°C. The rate of chitosan degradation was above 43.6%/h in the initial stage, then decreased to about 20%/h. The degradation rate constants raised substantially in the late stage. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 2917–2923, 2003 相似文献
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Effects of the degree of deacetylation (DDA) and the molecular mass of chitosan oligosaccharides (CTS-OS), obtained from the enzymatic hydrolysis of high molecular weight chitosan (HMWC), on antitumor activity was explored. The DDA and molecular weights of CTS-OS were determined by matrix-assisted laser desorption/ionization-mass spectrometry (MALDI-TOF MS) analysis. The CTS-OS were found to be a mixture of mainly dimers (18.8%), trimers (24.8%), tetramers (24.9%), pentamers (17.7%), hexamers (7.1%), heptamers (3.3%), and octamers (3.4%). The CTS-OS were further fractionated by gel-filtration chromatography into two major fractions: (1) COS, consisting of glucosamine (GlcN)(n), n = 3-5 with DDA 100%; and (2) HOS, consisting of (GlcN)(5) as the minimum residues and varying number of N-acetylglucosamine (GlcNAc)(n), n = 1-2 with DDA about 87.5% in random order. The cytotoxicities, expressed as the concentration needed for 50% cell death (CC(50)), of CTS-OS, COS, and HOS against PC3 (prostate cancer cell), A549 (lung cancer cell), and HepG2 (hepatoma cell), were determined to be 25 μg·mL(-1), 25 μg·mL(-1), and 50 μg·mL(-1), respectively. The HMWC was approximately 50% less effective than both CTS-OS and COS. These results demonstrate that the molecular weight and DDA of chitosan oligosaccharides are important factors for suppressing cancer cell growth. 相似文献
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Yanming Dong Congyi Xu Jianwei Wang Yusong Wu Mian Wang Yonghong Ruan 《应用聚合物科学杂志》2002,83(6):1204-1208
We prepared chitosans with various degrees of deacetylation (DDAs) by mixing completely deacetylated chitosan and acetic anhydride at room temperature without serious degradation and O‐substitution. We obtained a standard curve to measure DDA by plotting the IR absorbance ratio of A1560/A2880 against the known DDAs (from 1–100%) of 10 specimens. The effect of DDA on the critical concentration (C*) of chitosan/dichloroacetic acid solutions required to form mesophase was investigated by optical methods. A maximum C* value of 23 wt % appeared at a relative medium DDA (~20%). The effect was explained by the disordering of chains with medium composition ratios of the copolymer of glucosamine and N‐acetyl glucosamine. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 1204–1208, 2002 相似文献
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Several sea sources for chitin have been investigated, and the chitin content and crystallographic polymorph of the extracted chitin determined. Deacetylation of the chitin was carried out and the physicochemical characteristics of the resulting chitosan studied. The influence of the reaction parameters (reaction duration, temperature, nature of alkaline reagent, etc) was followed. Thus it became possible to determine adequate reaction conditions for obtaining chitosans with the required properties. The physicochemical characteristics of the obtained chitosan are closely related to the taxonomy of the source. New sea sources for chitin have been investigated and considered for industrial purposes. © 2000 Society of Chemical Industry 相似文献
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