Evaluation of temperature programming for gradient elution in packed capillary liquid chromatography coupled to electrochemical detection
✍ Scribed by O. Nordström; P. Molander; T. Greibrokk; R. Blomhoff; E. Lundanes
- Publisher
- John Wiley and Sons
- Year
- 2001
- Tongue
- English
- Weight
- 118 KB
- Volume
- 13
- Category
- Article
- ISSN
- 1040-7685
- DOI
- 10.1002/mcs.1039
No coin nor oath required. For personal study only.
✦ Synopsis
Abstract
A miniaturized amperometric detector compatible with temperature‐programmed packed capillary liquid chromatography has been constructed and evaluated. Temperature programming could successfully be used as a tool for retention control, providing gradient action that did not influence the detector performance. A 7‐μm single carbon fiber was utilized as working electrode and detection was performed in a 50‐μm i.d. fused silica detection capillary which also functioned as restriction capillary. Separation of tyrosine, 3‐(3,4‐dihydroxyphenyl)alanine, 3‐chloro‐tyrosine and 3‐NO~2~‐tyrosine was achieved in 6 min using a temperature program from 30°C to 100°C with a ramp of 8°C/min on a 25 cm 0.32 mm i.d. column packed with 3 μm Hypersil ODS. The mobile phase consisted of 50 mM citric acid (pH 3.10)‐methanol (95+ 5, v/v), and the mass limit of detection was in the range 1–5 pg using 1.2 V vs the Ag/AgCl reference electrode. © 2001 John Wiley & Sons, Inc. J Micro Sep 13: 179–185, 2001