Document Detail


Quantitative determination of apogossypol, a pro-apoptotic analog of gossypol, in mouse plasma using LC/MS/MS.
MedLine Citation:
PMID:  16859853     Owner:  NLM     Status:  MEDLINE    
Abstract/OtherAbstract:
A simple and selective liquid chromatography/tandem mass spectrometry (LC/MS/MS) method based on internal standard quantitation using apigenin as the internal standard has been developed and validated for the analysis of the gossypol analog apogossypol, a pro-apoptotic compound, in mouse plasma. The methodology involves protein precipitation of plasma samples followed by LC/MS/MS analysis. Ascorbic acid was added to the spiking solutions and plasma samples to stabilize the easily oxidized compound. Separation of apogossypol and the internal standard from the plasma matrix was achieved using a C18 column with a gradient elution profile consisting of 5mM ammonium acetate and methanol. The validated range of the method extended from 10 to 2000 ng/mL with accuracies of 85-115% and precision of <15%. The average recovery of apogossypol at three concentrations (50, 200 and 1000 ng/mL) assayed in triplicate using this methodology was determined to be 90.8+/-12.9%. Recovery for the internal standard (apigenin) at a concentration of 500 ng/mL was found to be 99.9+/-6.41%. Apogossypol concentrations of 50 ng/mL and above were found to be stable in extracted plasma for 24h when stored at 25 degrees C. This method has been applied to the determination of apogossypol concentrations in plasma collected from mice given an IV dose of apogossypol.
Authors:
L Coward; G Gorman; P Noker; C Kerstner-Wood; M Pellecchia; J C Reed; L Jia
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Publication Detail:
Type:  Journal Article; Research Support, N.I.H., Extramural     Date:  2006-07-21
Journal Detail:
Title:  Journal of pharmaceutical and biomedical analysis     Volume:  42     ISSN:  0731-7085     ISO Abbreviation:  J Pharm Biomed Anal     Publication Date:  2006 Nov 
Date Detail:
Created Date:  2006-10-31     Completed Date:  2007-02-07     Revised Date:  2007-12-03    
Medline Journal Info:
Nlm Unique ID:  8309336     Medline TA:  J Pharm Biomed Anal     Country:  England    
Other Details:
Languages:  eng     Pagination:  581-6     Citation Subset:  IM    
Affiliation:
Southern Research Institute, 2000 Ninth Ave. South, Birmingham, AL 35205, USA. coward@sri.org
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MeSH Terms
Descriptor/Qualifier:
Animals
Apoptosis / drug effects*
Chromatography, Liquid
Gossypol / analogs & derivatives*,  blood,  pharmacology
Injections, Intravenous
Male
Mice
Mice, Inbred Strains
Reference Standards
Reproducibility of Results
Sensitivity and Specificity
Tandem Mass Spectrometry
Grant Support
ID/Acronym/Agency:
N01-CM-52203/CM/NCI NIH HHS
Chemical
Reg. No./Substance:
0/apogossypol; 303-45-7/Gossypol

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


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