Document Detail


Development of a method for the direct analysis of peptide AM336 in monkey cerebrospinal fluid using liquid chromatography/electrospray ionization mass spectrometry with a mixed-function column.
MedLine Citation:
PMID:  14587085     Owner:  NLM     Status:  MEDLINE    
Abstract/OtherAbstract:
A liquid chromatography/mass spectrometry (LC/MS) analytical procedure, using a single column for sample clean-up, enrichment and separation, has been developed for the determination of the peptide AM336 in monkey cerebrospinal fluid (CSF). CSF samples were injected and analyzed using a polymer-coated mixed-function high-performance liquid chromatography (HPLC) column with gradient elution and application of a timed valve-switching event. The mass spectrometer was operated in the positive electrospray ionization (ESI(+)) mode with single ion recording (SIR) at m/z 920. The method was validated, yielding calibration curves with correlation coefficients greater than 0.9892. Assay precision and accuracy were evaluated by direct injection of AM336-fortified CSF samples at three concentration levels. Analyzed concentrations ranged from 99.93 to 113.1% of their respective theoretical concentrations with coefficients of variation below 9.0%. An evaluation of the signal-to-noise (S/N) ratio for a 200 ng/mL calibration standard, considered to be the lower limit of quantitation (LLOQ), resulted in an estimated limit of detection (LOD) of 31.2 ng/mL. Preliminary data suggest the possibility of using this method to analyze AM336 also in plasma samples, pending the successful outcome of additional investigations.
Authors:
Wei Bu; Scott D Freer; Shelly M Hollar; Philip L Stetson; Robert A Boyd; John B Kurek; Daniel W Sved
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Publication Detail:
Type:  Journal Article; Research Support, Non-U.S. Gov't    
Journal Detail:
Title:  Rapid communications in mass spectrometry : RCM     Volume:  17     ISSN:  0951-4198     ISO Abbreviation:  Rapid Commun. Mass Spectrom.     Publication Date:  2003  
Date Detail:
Created Date:  2003-10-30     Completed Date:  2003-12-12     Revised Date:  2006-11-15    
Medline Journal Info:
Nlm Unique ID:  8802365     Medline TA:  Rapid Commun Mass Spectrom     Country:  England    
Other Details:
Languages:  eng     Pagination:  2394-8     Citation Subset:  IM    
Copyright Information:
Copyright 2003 John Wiley & Sons, Ltd.
Affiliation:
WIL Research Laboratories, Inc., Ashland, OH 44805, USA. wbu@wilresearch.com
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MeSH Terms
Descriptor/Qualifier:
Animals
Calibration
Chromatography, Liquid / instrumentation,  methods*
Haplorhini / cerebrospinal fluid*
Spectrometry, Mass, Electrospray Ionization / instrumentation,  methods*
Venoms / cerebrospinal fluid*
Chemical
Reg. No./Substance:
0/AM336; 0/Venoms

From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine


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