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Derivatization of 5-fluorouracil With 4-bromomethyl-7-methoxycoumarin for Determination by Liquid Chromatography-Mass Spectrometry

Derivatization of 5-fluorouracil With 4-bromomethyl-7-methoxycoumarin for Determination by Liquid Chromatography-Mass Spectrometry

K Wang, M Nano, T Mulligan, E D Bush, R W Edom

J Am Soc Mass Spectrom. 1998 Sep;9(9):970-6.

PMID: 9725015

Abstract:

A robust new analytical method has been developed for the determination of 5-fluorouracil (5-FU) in human plasma samples using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The method is based on a liquid-liquid extraction procedure, precolumn derivatization, reversed-phase HPLC separation, and detection using atmospheric pressure chemical ionization and selected reaction monitoring. The derivatization agent used was 4-bromomethyl-7-methoxycoumarin. The internal standard for the assay procedure was a stable isotope labeled analog of 5-FU. The lower limit of quantitation was 1.0 ng/mL using 500 microL aliquots of plasma. Sample throughput on the mass spectrometer was approximately 17 samples/h (3.5 min/sample). The method was fully validated. The recovery of 5-FU averaged 76.1%. The accuracy of the assay, assessed from quality control samples, ranged from 99.1% to 104.3% (% theoretical). The overall interassay precision (% RSD) was 2.7%, and the intraassay precision (% RSD) ranged from 1.5% to 3.9%. The derivatized samples were found to be stable under sample analysis conditions and during refrigerator storage. The method was specific for the determination of 5-FU.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP35231448	4-Bromomethyl-7-methoxycoumarin		35231-44-8	Price

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