Ruddy S B, Hadzija B W
Division of Pharmaceutics, School of Pharmacy, University of North Carolina at Chapel Hill.
J Chromatogr B Biomed Appl. 1994 Jul 1;657(1):83-92. doi: 10.1016/0378-4347(94)80073-1.
The isocratic, reversed-phase, high-performance liquid chromatographic (HPLC) method presented provides a simple and rapid analytical technique for the simultaneous determination of low-molecular-mass oligomers of polyethylene glycol (PEG) in aqueous polymer samples containing polar contaminants of biologic origin. In the present case, individual molecular mass species were quantitated in aqueous skin extracts arising from the investigation of PEG transport through mammalian skin. PEGs were isolated and purified by solid-phase extraction using large-pore kieselguhr (Extrelut QE) cartridges, which selectively retained polar contaminants from excised skin specimens. Sample recoveries were found to be dependent upon molecular mass, ranging from 18.28% to 86.10%, but were highly reproducible. The mean inter-sample error (n > or = 5) for the extraction of twenty-six molecular mass species of PEG was less than 3%. Satisfactory resolution of primary molecular mass components was accomplished using a base-deactivated, C8 column (Supelcosil LC-8-DB) and a mobile phase consisting of methanol and water. Corresponding run times for the complete separation of individual oligomers ranged from 8 to 30 min, while the limit of detection for a particular molecular mass species was approximately 5 micrograms/ml. The method was further employed to determine the weight-average (Mw) and number-average (Mn) molecular mass distributions and polydispersity for three commercial PEG blends, as well as to characterize the methylene chloride/water distribution coefficients for twenty-two molecular mass species ranging from 282 to 1206 Da.
本文介绍的等度反相高效液相色谱（HPLC）方法，为同时测定含有生物来源极性污染物的水性聚合物样品中的聚乙二醇（PEG）低分子量低聚物提供了一种简单快速的分析技术。在本研究中，通过对PEG透过哺乳动物皮肤的研究，对水性皮肤提取物中的各个分子量物种进行了定量分析。PEG通过使用大孔硅胶（Extrelut QE）柱进行固相萃取进行分离和纯化，该柱可选择性地保留切除皮肤标本中的极性污染物。发现样品回收率取决于分子量，范围为18.28%至86.10%，但具有高度的重现性。提取26种PEG分子量物种的平均样品间误差（n≥5）小于3%。使用碱钝化C8柱（Supelcosil LC-8-DB）和由甲醇和水组成的流动相，实现了主要分子量成分的满意分离。单个低聚物完全分离的相应运行时间为8至30分钟，而特定分子量物种的检测限约为5微克/毫升。该方法进一步用于测定三种市售PEG混合物的重均分子量（Mw）和数均分子量（Mn）分布以及多分散性，以及表征22种分子量范围从282至1206 Da的物种的二氯甲烷/水分配系数。
