Liu X Michael, Gao Wei, Maziarz E Peter, Salamone Joseph C, Duex John, Xia Erning
Bausch & Lomb, Inc., Global Research & Development, 1400 N. Goodman Street, Rochester, NY 14609, USA.
J Chromatogr A. 2006 Feb 3;1104(1-2):145-53. doi: 10.1016/j.chroma.2005.11.094. Epub 2005 Dec 19.
A more complete understanding of polymeric, cationic cellulose derivatives, including polyquaterium-10 (Polymer JR), has become increasingly important in the eye care industry as thorough characterization of raw materials helps promote product quality and process control. Often such detailed information requires utilization of a combination of analytical techniques. In this work three Polymer JR samples with different viscosities were characterized using aqueous size exclusion chromatography (SEC) with a light scattering detector, a differential viscometer, and a differential refractometer (triple detection). Detailed molecular information such as absolute molecular weights, molecular weight distributions, intrinsic viscosities, and molecular conformations were obtained. One major challenge of analyzing cationic polymers is abnormal size exclusion separation, which could be caused by the ionic interaction between sample molecules and the column packing material. A selection of mobile phases varying in pH, buffer, organic solvent content, and molar concentration of salts was employed to evaluate the correlation of obtained molecular weight values and mobile phase composition. Universal calibration concept was used to examine the abnormal size exclusion separation phenomenon of Polymer JR samples when using different mobile phases. It was observed that the abnormal size exclusion was dependent on both the separation conditions and molecular weights of the samples. Despite the changes in separation parameters and uncharacteristic polymeric structure compared to conventional SEC samples, the use of aqueous SEC with triple detection provided reproducible and valuable molecular information of Polymer JR samples with low to medium molecular weights. By using a combination of high buffer content and adding organic solvent, the abnormal exclusion separation of high molecular weigh Polymer JR could be considerably reduced.
在眼保健行业中，更全面地了解聚合阳离子纤维素衍生物，包括聚季铵盐-10（Polymer JR）变得越来越重要，因为对原材料进行全面表征有助于提高产品质量和过程控制。通常，此类详细信息需要综合运用多种分析技术。在这项工作中，使用配备光散射检测器、差示粘度计和差示折光仪的水性尺寸排阻色谱（SEC）（三重检测）对三种不同粘度的Polymer JR样品进行了表征。获得了诸如绝对分子量、分子量分布、特性粘度和分子构象等详细的分子信息。分析阳离子聚合物的一个主要挑战是异常的尺寸排阻分离，这可能是由样品分子与柱填料之间的离子相互作用引起的。选用了pH值、缓冲液、有机溶剂含量和盐的摩尔浓度各不相同的流动相，以评估所得分子量值与流动相组成之间的相关性。采用通用校准概念来研究使用不同流动相时Polymer JR样品的异常尺寸排阻分离现象。观察到异常尺寸排阻既取决于分离条件，也取决于样品的分子量。尽管与传统SEC样品相比，分离参数和聚合物结构具有非典型性，但使用配备三重检测的水性SEC仍能为低至中等分子量的Polymer JR样品提供可重复且有价值的分子信息。通过使用高缓冲液含量并添加有机溶剂的组合，可以显著减少高分子量Polymer JR的异常排阻分离。
