Determination of pramipexole (U-98,528) in human plasma by high-performance liquid chromatography with atmospheric pressure chemical ionization tandem mass spectrometry.
A highly sensitive and selective HPLC-MS-MS method was developed for the determination of pramipexole in human plasma. The analytes, pramipexole and BHT-920 (internal standard), were extracted from plasma at basic pH with methyl tert.-butyl ether (MTBE). MTBE was evaporated to dryness and reconstituted in 100 microliters of (95:5) methanol-water. Chromatographic separation was achieved on a Zorbax SB-CN column with a mobile phase of (15:5:80) water-0.1 M ammonium acetate-methanol. The analytes were detected utilizing HPLC in conjunction with atmospheric pressure chemical ionization (APCI) tandem mass spectrometry (MS-MS). The assay was linear in the concentration ranges of 50 to 5000 pg/ml. The analysis of pooled quality controls (150, 750, and 3000 pg/ml) demonstrated excellent precision with relative standard deviations (R.S.D.) (n = 18) of 7.2%, 5.3% and 5.2%, respectively. The method is accurate with all intra-day (n = 6) and overall (n = 18) mean values being less than 11.7% from theoretical.
Department of Biopharmaceutics, Corning Hazleton Inc., Madison, WI 53704, USA.
Y Y
YY
Lau
J M
JM
Selenka
G D
GD
Hanson
R
R
Talaat
N
N
Ichhpurani
D000284:Administration, Oral; D001274:Atmospheric Pressure; D001381:Azepines / Q000032:analysis / Q000737:chemistry; D052160:Benzothiazoles; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D018491:Dopamine Agonists / Q000008:administration & dosage / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics; D006801:Humans; D016014:Linear Models; D013058:Mass Spectrometry; D000077487:Pramipexole; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013844:Thiazoles / Q000008:administration & dosage / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics
D001381:Azepines; D052160:Benzothiazoles; D018491:Dopamine Agonists; D013844:Thiazoles; C024763:talipexole; D000077487:Pramipexole