A 96-well single-pot liquid-liquid extraction, hydrophilic interaction liquid chromatography-mass spectrometry method for the determination of muraglitazar in human plasma

Journal of Pharmaceutical and Biomedical Analysis
Y-J XueSteve Unger

Abstract

A single-pot liquid-liquid extraction (LLE) with hydrophilic interaction liquid chromatography/tandem mass spectrometry (HILIC/MS/MS) method has been developed and validated for the determination of muraglitazar, a hydrophobic diabetes drug, in human plasma. To 0.050 ml of each plasma sample in a 96-well plate, the internal standard solution in acetonitrile and toluene were added to extract the compound of interest. The plate was vortexed, followed by centrifugation. The organic layer was then directly injected into an LC/MS/MS system. Chromatographic separation was achieved isocratically on a Thermohypersil_Keystone, Hypersil silica column (3 mmx50 mm, 3 microm). The mobile phase contained 85% of methyl t-butyl ether and 15% of 90/10 (v/v) acetonitrile/water with 0.3% trifluoroacetic acid. Post-column mobile phase of 50/50 (v/v) acetonitrile/water containing 0.1% formic acid was added. Detection was by positive ion electrospray tandem mass spectrometry on a Sciex API 4000. The standard curve, ranged from 1 to 1000 ng/ml, was fitted to a 1/x weighted quadratic regression model. This single-pot LLE approach effectively eliminated time-consuming organic layer transfer, dry-down, and sample reconstitution steps, which are essentia...Continue Reading

References

Feb 28, 2002·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·M BernaS Glass
Aug 31, 2002·Rapid Communications in Mass Spectrometry : RCM·Wilson Z ShouWeng Naidong
Sep 25, 2002·Rapid Communications in Mass Spectrometry : RCM·Stacy D BrownMichael G Bartlett
Oct 29, 2003·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·Weng Naidong

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Citations

Jun 26, 2013·Bioanalysis·Yong Q Tang, Naidong Weng
Jan 31, 2007·Journal of Mass Spectrometry : JMS
Apr 23, 2008·Journal of Separation Science·Yunsheng Hsieh
Apr 11, 2008·Journal of Separation Science·Hien P Nguyen, Kevin A Schug
May 8, 2008·Journal of Separation Science·Bieke DejaegherYvan Vander Heyden
Feb 26, 2010·Journal of Separation Science·Bieke Dejaegher, Yvan Vander Heyden
Feb 16, 2010·Journal of Separation Science·Wenying JianNaidong Weng
Jan 4, 2012·Biomedical Chromatography : BMC·Y-J XueKarin M Keller

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