Roed L, Lundanes E, Greibrokk T
Department of Chemistry, University of Oslo, Norway.
Electrophoresis. 1999 Sep;20(12):2373-8. doi: 10.1002/(SICI)1522-2683(19990801)20:12<2373::AID-ELPS2373>3.0.CO;2-3.
A nonaqueous packed capillary electrochromatographic reversed-phase method for separation of retinyl esters has been developed. The retinyl esters all-trans-retinyl acetate, palmitate, heptadecanoate, stearate, oleoate, and linoleoate were separated on a 180 microm ID column packed with 5 microm C30 particles with a mobile phase consisting of 2.5 mM lithium acetate in N,N-dimethylformamide-methanol (99:1, v/v). With this mobile phase, the electroosmotic flow was 0.8 mm/s at 650 V/cm and 40 degrees C, and the separation was completed in less than 30 min on 30 cm columns. To obtain electrostable frits of the hydrophobic C30 material both the preparation of the frits and the conditioning of the column prior to electroconditioning were of importance. Selectivity changes were introduced by replacing up to 70% v/v of the N,N-dimethylformamide by acetonitrile. The increase in the amount of acetonitrile was, however, accompanied by a significant increase in analysis time. Liver extracts obtained from arctic seal were analyzed.
已开发出一种用于分离视黄酯的非水填充毛细管电色谱反相方法。在填充有5微米C30颗粒的内径180微米的柱上,以由2.5 mM醋酸锂在N,N - 二甲基甲酰胺 - 甲醇(99:1,v/v)组成的流动相,分离视黄酯全反式视黄醇醋酸酯、棕榈酸酯、十七烷酸酯、硬脂酸酯、油酸酯和亚油酸酯。使用该流动相,在650 V/cm和40℃下电渗流为0.8 mm/s,在30 cm柱上不到30分钟即可完成分离。为了获得疏水C30材料的电稳定烧结物,烧结物的制备以及电调节之前柱的预处理都很重要。通过用乙腈替代高达70% v/v的N,N - 二甲基甲酰胺引入选择性变化。然而,乙腈量的增加伴随着分析时间的显著增加。对从北极海豹获得的肝脏提取物进行了分析。