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Clinical Chemistry 36: 538-540, 1990;
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Clinical Chemistry, Vol 36, 538-540, Copyright © 1990 by American Association for Clinical Chemistry

Improved sample preparation in determination of urinary metanephrines by liquid chromatography with electrochemical detection

RN Gupta
Department of Laboratory Medicine, St. Joseph's Hospital, Hamilton, Ontario, Canada.

In this relatively simple procedure for extracting metanephrines from urine, after an internal standard (4-hydroxy-3-methoxybenzylamine in 1 mmol/L HCl) is added, the sample is hydrolyzed in a boiling water bath, then treated with ammonia and alumina. Excess ammonia is removed under reduced pressure and the sample is applied to a 1-mL Bond Elut SCX column, which is washed, and metanephrines and internal standard are eluted with 0.5 mmol/L sodium acetate/acetonitrile (3/1 by vol). Of this elute, 5 microL is injected into a 15 cm x 4.6 mm (i.d.) column packed with 5-microns octadecylsilyl silica particles, which is eluted with a mobile phase containing tetramethylammonium perchlorate. Peaks are detected coulometrically at +0.28 V. In the resulting chromatogram, metanephrines give sharp peaks, well resolved from peaks for solvent and internal standard. There are no extraneous peaks for catechols or mono-oxygenated phenylethylamines. Results correlated well (r = 0.999, n = 13) with those by earlier described liquid-chromatography.


The following articles in journals at HighWire Press have cited this article:


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 Clin. Chem.Home page
D. K. Crockett, E. L. Frank, and W. L. Roberts
Rapid Analysis of Metanephrine and Normetanephrine in Urine by Gas Chromatography-Mass Spectrometry
Clin. Chem., February 1, 2002; 48(2): 332 - 337.
[Abstract] [Full Text] [PDF]


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