Validated ultra-performance liquid chromatography tandem mass spectrometry method for the determination of pramipexole in human plasma.
A sensitive and high throughput ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS-MS) method has been developed for the determination of pramipexole, a dopamine agonist, in human plasma. Sample preparation involved liquid-liquid extraction of pramipexole and ranitidine as the internal standard (IS) in ethyl acetate from 100 μL human plasma. The chromatographic separation is achieved on a Waters Acquity UPLC BEH C18 (100 mm × 2.1 mm, 1.7 μm) analytical column using an isocratic mobile phase, consisting of 10 mM ammonium formate (pH 7.50)-acetonitrile (15:85, v/v), at a flow-rate of 0.5 mL/min. The precursor → product ion transition for pramipexole (m/z 212.1 → 153.0) and IS (m/z 315.0 → 176.1) were monitored on a triple quadrupole mass spectrometer, operating in the multiple reaction monitoring (MRM) and positive ion mode. The method was validated over a wide dynamic concentration range of 20-4020 pg/mL. Matrix effect is assessed by post-column infusion experiment and the process efficiency were 91.9% and 85.7% for pramipexole and IS, respectively. The method is rugged and rapid with a total run time of 1.5 min and is applied to a bioequivalence study of 0.25 mg PPX tablet formulation in 30 healthy Indian male subjects under fasting condition.
Bioanalytical Research Department, Veeda Clinical Research, Ambawadi, Ahmedabad 3800015, India.
Manish
M
Yadav
Rajasekhar
R
Rao
Hemal
H
Kurani
Jaysukh
J
Rathod
Rakesh
R
Patel
Puran
P
Singhal
Pranav S
PS
Shrivastav
D052160:Benzothiazoles / Q000097:blood*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D018491:Dopamine Agonists / Q000097:blood*; D006801:Humans; D000077487:Pramipexole; D053719:Tandem Mass Spectrometry / Q000379:methods*
D052160:Benzothiazoles; D018491:Dopamine Agonists; D000077487:Pramipexole