烷基酚聚氧乙烯醚在不同液相色谱分离模式中的分离研究

考察了烷基酚聚氧乙烯醚在反相色谱、正相键合色谱、硅胶吸附色谱、体积排阻色谱4种不同液相色谱分离模式中的分离效果,分别采用Kromasil C_(18)(250 mm× 4.6 mm,5 μm)、Agilent ZORBAX NH2(250 mm× 4.6 mm,5 μm)、Waters Spherisorb S3W(150 mm×2.0 mm,3 μm)和Shodex MSpak GF-310 2D(150 mm×2.0 mm,5 μm)色谱柱,以225 nm为紫外检测波长,对不同液相色谱分离模式的流动相组成、梯度洗脱条件、柱温、流速等进行了优化,并对烷基酚聚氧乙烯醚在不同液相色谱分离模式中的保留机理进行了初步探讨.结果表明,正相键合色谱实现了烷基酚聚氧乙烯醚的最佳分离;硅胶吸附色谱和体积排阻色谱的分离效果较正相键合色谱稍差.

Study on Separation of Alkylphenol Ethoxylates in Different Liquid Chromatography Modes

The separation effects of alkylphenol ethoxylates in different liquid chromatography modes, such as reversed-phase liquid chromatography, bonded normal-phase liquid chromatography, silica adsorption chromatography and size exclusion chromatography were investigated. The chromatographic columns including Kromasil C_(18)(250 mm × 4.6 mm, 5 μm) , Agilent ZORBAX NH_2(250 mm × 4.6 mm, 5 μm), Waters Spherisorb S3W(150 mm × 2.0 mm, 3 μm) and Shodex MSpak GF-310 2D( 150 mm × 2. 0 mm, 5 μm) were utilized and detection wavelength was set at 225 nm. The chro-matographic conditions, including mobile phase composition, gradient elution, column temperature, flow rate, etc, were optimized. The retention mechanism of alkylphenol ethoxylates in different liq-uid chromatography modes was discussed. The best resolution of alkylphenol ethoxylates was achieved by bonded normal-phase liquid chromatography, which was slightly better than the resolution in silica adsorption chromatography and size exclusion chromatography. However, the reversed-phase mobile phase in silica adsorption chromatography and size exclusion chromatography possessed excellent com-patibility with ESI mass spectrometry. Both the structural information of alkyl chains and ethoxylation distribution of alkylphenol ethoxylates, and the quantitation of alkylphenol ethoxylates with different polymerization degrees can be achieved by chromatography - mass spectrometry technology.