Determination of MK‐0431 in human plasma using high turbulence liquid chromatography online extraction and tandem mass spectrometry

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Abstract
A robust and sensitive method using high turbulence liquid chromatography (HTLC) online extraction with tandem mass spectrometry (MS/MS) for the determination of MK‐0431 in human plasma was developed and validated to support the clinical studies. This HTLC online extraction method eliminated the time‐consuming offline sample extraction procedures and significantly increased productivity. A narrow bore large particle size reversed‐phase column (Cyclone, 50 × 1.0 mm, 60 µm) and a BDS Hypersil C18 column (30 × 2.1 mm, 3 µm) were used as extraction and analytical columns, respectively. The linear dynamic range of the calibration curve was 0.5 to 1000 ng/mL. Intraday validation was conducted using five calibration curves prepared in five lots of human control plasma, and the intraday precision (RSD%) was from 2.4 to 9.0% and the accuracy was from 98.0 to 103% of the nominal value. The intraday precision (RSD%, n = 5) for plasma quality control (QC) samples varied from 2.0 to 5.3% and accuracy from 103 to 105% of the nominal value. The interday precision (RSD%) for 100 sets of plasma QC samples in 29 analytical runs varied from 6.3 to 9.0% and the accuracy from 98.8 to 104% of the nominal value. No significant difference was observed between the interday and intraday precision and accuracy of the QC samples. Copyright © 2006 John Wiley & Sons, Ltd.

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