Liquid chromatography/mass spectrometry for the quantitation of muraglitazar in monkey plasma

Biomedical Chromatography : BMC
Ming Yao, Nuggehally R Srinivas

Abstract

A high-performance liquid chromatographic-mass spectrometric (LC/MS) assay was developed and validated for the determination of muraglitazar, a novel alpha/gamma, dual PPAR activator, in monkey plasma. The method utilized trazodone as the internal standard (IS). The extraction scheme involved a simple protein precipitation procedure with the use of a mixture of acetonitrile and methylene chloride. Separation was carried out on a BDS Hypersil C(18) analytical column (2 x 50 mm, 3 microm) and an effective chromatographic separation of muraglitazar (3.31 min) and trazadone (2.27 min) was achieved at a ssow rate of 0.3 mL/min. The mobile phase, used in an isocratic mode, consisted of 90% A (acetonitrile: 0.1% formic acid, 50:50 v/v) and 10% B (acetonitrile: 0.1% formic acid, 95:5 v/v). Detection of muraglitazar and trazodone was by positive ion turbo-ion spray mass spectrometry in the SIM mode. The mass spectrometer was programmed to admit the protonated molecules at m/z 372.0 (IS) and m/z 517.1 (muraglitazar). The standard curve, which ranged from 2 to 500 ng/mL, was fitted to a 1/x weighted linear regression model. The between run precision and within-run precision values of the assay was within 6.2% RSD. The assay accuracy was w...Continue Reading

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