Separation of nicotinic acid and six metabolites within 60 seconds using high-flow gradient chromatography on silica column with tandem mass spectrometric detection

被引：31

作者：

Li, AC ^{[1
]}

Chen, YL ^{[1
]}

Junga, H ^{[1
]}

Shou, WZ ^{[1
]}

Jiang, X ^{[1
]}

Naidong, W ^{[1
]}

机构：

[1] Covance Labs Inc, Madison, WI 53704 USA

来源：

CHROMATOGRAPHIA | 2003年 / 58卷 / 11-12期

关键词：

column liquid chromatography; high flow gradient elution; tandem ms detection; nicotinic acid and metabolites; rapid analysis;

D O I：

10.1365/s10337-003-0117-4

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

Separation of nicotinic acid and its six metabolites (nicotinamide, nicotinuric acid, 1-methy-2pyridone-5-carboxamide, 1-methy-4-pyridone-5-carboxamide, 1-methyl-nicotinamide, and nicotinamide-N-oxide) within 60 seconds was achieved by using a gradient chromatography at a flow rate of 4 mL min(-1) on silica column and aqueous/organic mobile phases with tandem mass spectrometric detection. The fourth metabolite, 1-methyl-4-pyridone-5-carboxamide, did not show isotopic or cross channel interference, even though it co-eluted with nicotinamide-N-oxide. This method was validated to analyze all seven compounds in human plasma and urine samples which were extracted with Waters Oasis MCX 96-well plate. The linearity of the method is 10 to 2000 ng mL(-1) for each analyte. The relative standard deviation and relative error for the standards were less than 17% and 8.4%, respectively. The relative standard deviation and relative error for the quality control samples were less than 12% and 13% respectively.

引用

页码：723 / 731

页数：9

共 12 条

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