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Micellar liquid chromatographic determination of nicotinic acid and nicotinamide after precolumn Konig reaction derivatization
被引:22
作者:
Capella-Peiró, ME
[1
]
Carda-Broch, S
[1
]
Monferrer-Pons, L
[1
]
Esteve-Romero, J
[1
]
机构:
[1] Univ Jaume 1, Area Quim Analit, Dept Ciencies Expt, Castellon de La Plana 12080, Spain
关键词:
Konig reaction;
precolumn derivatization;
micellar liquid chromatography;
nicotinic acid;
nicotinamide;
D O I:
10.1016/j.aca.2004.05.014
中图分类号:
O65 [分析化学];
学科分类号:
070302 ;
081704 ;
摘要:
In the Konig reaction, the heterocyclic nitrogen of a pyridine derivative reacts with cyanogen bromide and is afterwards coupled with an arylamine to give a polymethine dye. In the previous work, this reaction was automated using a flow injection system, and in this study we have coupled this system to a chromatograph to determine nicotinic acid and nicotinamide, after precolumn derivatization, using the Konig reaction. First, we checked the micellar chromatography behavior of the polymethines using a C 18 column, a flow of I mL min(-1) and detection at 440 nm. After modeling, the composition of the selected mobile phase was 150 mM sodium dodecyl sulfate (SDS)-6% (v/v) pentanol pH 3. In this mobile phase, the analysis time was below 17 min, the calibrations were lineal in the range 0.05 to 50 mug mL(-1) with regression coefficients above 0.999, and intra- and inter-day imprecision were below 5%. The method developed here was applied to the determination of nicotinamide and nicotinic acid in pharmaceuticals, serum and urine samples and the amounts determined were similar to those obtained using a reference method. (C) 2004 Elsevier B.V. All rights reserved.
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页码:81 / 87
页数:7
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