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Substituent Distribution and Clouding Behavior of Hydroxypropyl Methyl Cellulose Analyzed Using Enzymatic Degradation

机译:酶促降解法分析羟丙基甲基纤维素的取代基分布和混浊行为

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摘要

The distribution of substituents along the polymer backbone will have a strong influence on the properties of modified cellulose.Endoglucanases were used to degrade three different batches of hydroxypropyl methyl cellulose (HPMC) derivatives with similar chemical properties.The phase separation of the HPMCs as a function of temperature,i.e.,the clouding behavior,was analyzed prior to degradation.The total amount of unsubstituted glucose was determined using total acid hydrolysis followed by high-performance anion-exchange chromatography with pulsed amperometric detection (HPAEC-PAD).The products after enzymatic degradation were analyzed with size-exclusion chromatography with online multiangle light scattering and refractive index detection and also with reducing end determination.To further characterize the formed products,matrix-assisted laser desorption/ ionization time-of-flight mass spectrometry was employed for analysis of short-chained oligosaccharides.The different endoglucanases showed varying degradation capability of HPMC derivatives,depending on structure of the active site.The investigated HPMCs had different susceptibility to degradation by the endoglucanases.The results showed a difference in substituent distribution between HPMC batches,which could explain the differing clouding behaviors.The batch with the lowest cloud point was shown to contain a higher number of non-degradable,highly substituted regions.
机译:取代基沿聚合物主链的分布将对改性纤维素的性能产生重大影响,使用内切葡聚糖酶降解三批化学性质相似的不同批次的羟丙基甲基纤维素(HPMC)衍生物。降解之前先分析温度的变化,即混浊行为。先采用总酸水解,然后采用高效阴离子交换色谱和脉冲安培检测法(HPAEC-PAD)测定未取代的葡萄糖的总量。使用尺寸排阻色谱,在线多角度光散射和折射率检测以及减少末端测定法分析降解。为进一步表征形成的产物,采用矩阵辅助激光解吸/电离飞行时间质谱分析短链寡糖es显示HPMC衍生物的降解能力各不相同,取决​​于活性位点的结构。所研究的HPMC对内切葡聚糖酶的降解敏感性不同。结果表明各批次之间HPMC的取代基分布不同,这可以解释不同的混浊行为。浊点最低的批次显示出包含更多数量的不可降解,高度取代的区域。

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