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Predicate | Object |
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rdf:type | |
lifeskim:mentions | |
pubmed:issue |
9
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pubmed:dateCreated |
1998-9-24
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pubmed:abstractText |
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.
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pubmed:language |
eng
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pubmed:journal | |
pubmed:citationSubset |
IM
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pubmed:chemical |
http://linkedlifedata.com/resource/pubmed/chemical/4-bromomethyl-7-methoxycoumarin,
http://linkedlifedata.com/resource/pubmed/chemical/Antimetabolites,
http://linkedlifedata.com/resource/pubmed/chemical/Fluorouracil,
http://linkedlifedata.com/resource/pubmed/chemical/Indicators and Reagents,
http://linkedlifedata.com/resource/pubmed/chemical/Umbelliferones
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pubmed:status |
MEDLINE
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pubmed:month |
Sep
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pubmed:issn |
1044-0305
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pubmed:author | |
pubmed:issnType |
Print
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pubmed:volume |
9
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pubmed:owner |
NLM
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pubmed:authorsComplete |
Y
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pubmed:pagination |
970-6
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pubmed:dateRevised |
2006-11-15
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pubmed:meshHeading |
pubmed-meshheading:9725015-Antimetabolites,
pubmed-meshheading:9725015-Chromatography, High Pressure Liquid,
pubmed-meshheading:9725015-Fluorouracil,
pubmed-meshheading:9725015-Humans,
pubmed-meshheading:9725015-Indicators and Reagents,
pubmed-meshheading:9725015-Mass Spectrometry,
pubmed-meshheading:9725015-Quality Control,
pubmed-meshheading:9725015-Umbelliferones
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pubmed:year |
1998
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pubmed:articleTitle |
Derivatization of 5-fluorouracil with 4-bromomethyl-7-methoxycoumarin for determination by liquid chromatography-mass spectrometry.
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pubmed:affiliation |
Department of Drug Metabolism and Pharmacokinetics, Hoffmann-La Roche, Inc., Nutley, New Jersey 07110, USA. ka.wang@roche.com
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pubmed:publicationType |
Journal Article
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