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.
A highly sensitive and specific LC-MS/MS method has been developed and validated for the estimation of pramipexole (PPX) with 500 microL 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 > or =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.
Bharathi
D Vijaya
DV
Bioanalytical Department, Integrated Product Development, Dr Reddy's Laboratories Ltd, Bachupalli, Hyderabad-500 072, India.
Hotha
Kishore Kumar
KK
Sagar
P V Vidya
PV
Kumar
S Sirish
SS
Naidu
A
A
Mullangi
Ramesh
R
D052160:Benzothiazoles / Q000008:administration & dosage / Q000032:analysis* / Q000493:pharmacokinetics; D002853:Chromatography, Liquid / Q000379:methods*; D018491:Dopamine Agonists / Q000008:administration & dosage / Q000032:analysis* / Q000493:pharmacokinetics; D004355:Drug Stability; D006801:Humans; D016014:Linear Models; D008559:Memantine / Q000032:analysis; D000077487:Pramipexole; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*
D052160:Benzothiazoles; D018491:Dopamine Agonists; D000077487:Pramipexole; D008559:Memantine