Nonaqueous packed capillary electrochromatography on C18 columns: Separation of retinyl esters
β Scribed by Line Roed; Elsa Lundanes; Tyge Greibrokk
- Publisher
- John Wiley and Sons
- Year
- 1999
- Tongue
- English
- Weight
- 240 KB
- Volume
- 11
- Category
- Article
- ISSN
- 1040-7685
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β¦ Synopsis
A nonaqueous packed capillary electrochromatographic reversed-phase separation method for retinyl esters has been developed. The best performance was obtained using a 180-m-i.d. column packed with 3-m Hypersil ODS and a mobile phase consisting of 2.5 mM lithium acetate in N, N-dimethylformamideα Ε½ . methanol 99 : 1, vrv . This mobile phase composition gave an electroosmotic flow of 0.75 mmrs at 650 Vrcm and 40ΠC. The nonaqueous separation system produced low currents, enabling the use of larger i.d. columns. No loss in efficiency was observed when increasing the i.d. from 100 to 180 m, while the detection sensitivity increased by a factor of 6α7 resulting in a concentration limit of detection of 2 M. The separation system was evaluated in terms of the variation of retention times and peak areas. The within-day variation of retention times was Ε½ . Ε½ . Ε½ . 0.2α0.5% relative standard deviation RSD n s 3 and -0.1% RSD n s 3 without and with internal standard, respectively. Correspondingly, the between-day Ε½ . variation for 5 consecutive days was 1.5α1.6% RSD n s 5 and -0.1% RSD Ε½ . n s 5 . To obtain acceptable repeatability of the peak areas, internal standardization was necessary. The within-day and between-day variations of peak areas for Ε½ . Ε½ . retinyl palmitate were 0.5α1.4% RSD n s 3 and 9% RSD n s 5 , respectively. The method has been applied for the analysis of liver extracts obtained from arctic polar fox and seal.
π SIMILAR VOLUMES
A nonaqueous electrochromatographic reversed-phase separation method for retinyl esters using continuous bed columns has been developed. The Ε½ packing material was C modified material large-pore silica 5 m Nucleosil 4000 30 Λ. A . The continuous bed columns were prepared by solαgel bonding in 180 m