J. Lipid Res. Please sign the JLR Guestbook
HOME HELP FEEDBACK SUBSCRIPTIONS ARCHIVE SEARCH
QUICK SEARCH:   [advanced]


     

A more recent version of this article appeared on March 1, 2007

Papers In Press, published online ahead of print January 10, 2007
J. Lipid Res., doi:10.1194/jlr.D600040-JLR200
This Article
Right arrow Full Text (Accepted Manuscript)
Right arrow All Versions of this Article:
D600040-JLR200v1
48/3/733    most recent
Right arrow Alert me when this article is cited
Right arrow Alert me if a correction is posted
Services
Right arrow Similar articles in this journal
Right arrow Similar articles in PubMed
Right arrow Alert me to new issues of the journal
Right arrow Download to citation manager
Right arrow reprints & permissions
Citing Articles
Right arrow Citing Articles via Google Scholar
Google Scholar
Right arrow Articles by Zhang, B.
Right arrow Articles by Saku, K.
Right arrow Search for Related Content
PubMed
Right arrow PubMed Citation
Right arrow Articles by Zhang, B.
Right arrow Articles by Saku, K.
Social Bookmarking
Add to CiteULike   Add to Complore   Add to Connotea   Add to Del.icio.us   Add to Digg   Add to Reddit   Add to Technorati  
What's this?

Submitted on October 2, 2006
Revised on November 2, 2006
Accepted on December 14, 2006

Control of matrix effects in the analysis of urinary F2-isoprostanes using novel multidimensional solid-phase extraction and LC-MS/MS

Bo Zhang and Keijiro Saku

Dept. of Cardiology, Fkuoka University, Fukuoka 814-0180

Corresponding Author: bozhang{at}fukuoka-u.ac.jp

Objective: F<2-Isoprostanes (iPs), an established marker of oxidative stress, exist as 4 sets of stereoisomers. Simultaneous and specific determination of F2-iPs can be achieved by liquid chromatography-tandem mass spectrometry (LC-MS/MS). We developed novel methods for urine sample preparation and HPLC to control matrix-related ion suppression effects in the LC-MS/MS analysis of F2-iPs. Methods and Results: A selective solid-phase extraction (SPE) wash protocol was developed with an Oasis HLB SPE cartridge using an elution profile of [3H]-8-iso-PGF2alpha(iPF22alpha-III) when the methanol concentration was increased under acidic and base wash conditions. A multidimensional (MD) SPE method that incorporated size-exclusion, reverse-phase chromatography, and normal-phase chromatography was developed using an Oasis HLB SPE cartridge and an HLB mu Elution SPE plate. Average extraction recoveries of the deuterated internal standards of iPF2alpha-III and iPF2alpha-VI were 62+/-8 and 60+/-10%. A buffer-free HPLC method for the separation of F2-iP isomers was developed on base-deactivated C8 columns. Average matrix effects for iPF2alpha-III and iPF2alpha-VI were 95+/-6 and 103+/-5%. Conclusion: The clean extraction of urine F2-iPs using MD-SPE and the separation of F2-iP isomers using a novel HPLC method did not cause apparent ion suppression in the analysis of iPF2alpha-III and iPF2alpha-VI using LC-MS/MS. This finding should be useful for establishing a routine LC-MS/MS method for the analysis of F2alpha-iPs.


Add to CiteULike CiteULike   Add to Complore Complore   Add to Connotea Connotea   Add to Del.icio.us Del.icio.us   Add to Digg Digg   Add to Reddit Reddit   Add to Technorati Technorati    What's this?




HOME HELP FEEDBACK SUBSCRIPTIONS ARCHIVE SEARCH
 All ASBMB Journals   Journal of Biological Chemistry 
 Molecular and Cellular Proteomics   ASBMB Today 
Copyright © 2007 by the American Society for Biochemistry and Molecular Biology.