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通过二维液相色谱法分离和鉴定洗涤剂中的聚合分散剂。

Separation and identification of polymeric dispersants in detergents by two-dimensional liquid chromatography.

机构信息

The Dow Chemical Company, Analytical Sciences, Collegeville, PA 19426, USA.

The Dow Chemical Company, Analytical Sciences, Collegeville, PA 19426, USA.

出版信息

J Chromatogr A. 2018 Sep 7;1566:111-117. doi: 10.1016/j.chroma.2018.06.063. Epub 2018 Jun 26.

Abstract

Polymeric dispersants are an important ingredient in many consumer products. Their separations and identifications in final product formulation can be very challenging due to the presence of multiple polymeric dispersants at different levels and the presence of other polymeric and small-molecule components. In this study, using nearly comprehensive two-dimensional liquid chromatography (2D-LC), various water-soluble polymer and co-polymer dispersants were separated with aqueous size exclusion chromatography (SEC) in the first dimension (D) and gradient elution reversed-phase liquid chromatography (RPLC) in the second dimension (D). Detection of the polymeric dispersants was accomplished by evaporative light scattering detector (ELSD). A large ID (8.0 mm) SEC column used in common one-dimensional SEC practices was directly adopted in the 2D setup for rapid method development. A close representation of fully comprehensive 2D separation was achieved even with 60% of D eluent diverted to waste, demonstrating the flexibility and versatility of having SEC in D for two dimensional separation of polymers. Important method parameters, such as D column dimensions and flow rate, gradient conditions, and buffer pH were studied. Practical aspects of routine industrial applications such as solvent consumption and analysis time were also considered. This method was exploited for quick identification of polymeric dispersants in commercial detergent samples. Nine detergent samples were screened and polymeric dispersants and additional polymer features were detected in the samples.

摘要

聚合物分散剂是许多消费品的重要成分。由于存在多种不同水平的聚合物分散剂以及其他聚合物和小分子成分,因此在最终产品配方中对其进行分离和鉴定极具挑战性。在这项研究中,使用近乎全面的二维液相色谱(2D-LC),通过第一维(D)的水性尺寸排阻色谱(SEC)和第二维(D)的梯度洗脱反相液相色谱(RPLC)对各种水溶性聚合物和共聚物分散剂进行了分离。通过蒸发光散射检测器(ELSD)检测聚合物分散剂。在 2D 配置中,直接采用了在常见一维 SEC 实践中使用的大 ID(8.0mm)SEC 柱,用于快速方法开发。即使将 60%的 D 洗脱液分流到废物中,也实现了完全全面的 2D 分离的紧密再现性,证明了 SEC 在 D 中用于聚合物二维分离的灵活性和多功能性。研究了 D 柱尺寸和流速、梯度条件和缓冲液 pH 等重要方法参数。还考虑了溶剂消耗和分析时间等常规工业应用的实际方面。该方法用于快速识别商业洗涤剂样品中的聚合物分散剂。筛选了 9 个洗涤剂样品,并在样品中检测到了聚合物分散剂和其他聚合物特征。

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