Development and validation of a sensitive LC-MS/MS method with electrospray ionization for quantitation of pramipexole in human plasma: application to a clinical pharmacokinetic study

✍ Scribed by D. Vijaya Bharathi; Kishore Kumar Hotha; P. V. Vidya Sagar; S. Sirish Kumar; A. Naidu; Ramesh Mullangi

• Publisher: John Wiley and Sons
• Year: 2009
• Tongue: English
• Weight: 396 KB
• Volume: 23
• Category: Article
• ISSN: 0269-3879
• DOI: 10.1002/bmc.1108

✦ Synopsis

Abstract

A highly sensitive and specific LC‐MS/MS method has been developed and validated for the estimation of pramipexole (PPX) with 500 µL human plasma using memantine as an internal standard (IS). The API‐4000 was operated under multiple‐reaction monitoring mode (MRM) using the electrospray ionization technique. Solid‐phase extraction was used to extract PPX and IS from human plasma. The resolution of peaks was achieved with 0.01 m ammonium acetate buffer (pH 4.4):acetonitrile (30:70, v/v) on a Discovery CN column. The total chromatographic run time was 3.0 min and the elution of PPX and IS occurred at approximately 2.32 and 2.52, respectively. The MS/MS ion transitions monitored were 212.10 → 153.10 for PPX and 180.20 → 107.30 for IS. The method was proved to be accurate and precise at linearity range of 20–3540 pg/mL with a correlation coefficient (r) of ≥0.999. The intra‐ and inter‐day precision and accuracy values found to be within the assay variability limits as per the FDA guidelines. The developed assay method was applied to a pharmacokinetic study in human volunteers following oral administration of 0.25 mg PPX tablet. Copyright © 2008 John Wiley & Sons, Ltd.