A rapid, accurate and precise LC-MS method is described for the quantitative determination of pramipexole in human plasma matrix using ropinirole as internal standard. Pramipexole and ropinirole were extracted from plasma by liquid-liquid extraction technique. The method was validated over the concentration range of 100-2514 pg/mL. The method was found to have acceptable accuracy, precision, linearity and selectivity. The mean extraction recovery from spiked plasma samples was in the range of 79.415-87.00 %. The intra-day accuracy of the assay ranged from 98.924 to 112.236 % and intra-day precision ranged from 3.489 to 6.756 %. Inter-day accuracy and precision results for quality control samples ranged between 100.340 and 107.443% of nominal and precision is observed to be 3.970-5.714 %. The pramipexole was found to be stable after several stability studies. The proposed method yielded a quick, simple and reliable protocol for estimating pramipexole concentrations in human plasma.
Three new spectrophotometric methods (A, B and C) and one new high performance liquid chromatography (HPLC) method (D) for the quantitative analysis of bosentan (BSN) in pharmaceutical dosage forms have been described. The method A involves the oxidation of bosentan with ammonium molybdate in acidic medium which results in a blue-colored product. The methods B and C are based on the formation of yellow colored ion-pair complexes with 2, 4-dinitrophenol and bromocresol green, respectively. In method D, the determination of bosentan was carried out on Agilent C18 column (150 mm × 4.6 mm I.D., 5 μm ) in isocratic mode with methanol and ammonium acetate buffer (60:40 v/v) as mobile phase . The flow rate was 1.0 mL/min and eluent was monitored at 227 nm. The retention time of bosentan was 2.449 min. Under the optimized experimental conditions, Beer's plot showed good correlation in the concentration ranges of 2-30, 5-30, 2.5-50 and 5-100 μg/mL for methods A, B, C and D respectively. The methods were validated in accordance with the International Conference on Harmonization (ICH) guidelines. These methods were found to be sensitive, accurate, precise and robust and were successfully applied to the estimation of tablet dosage forms containing bosentan. There was no interference from the tablet excipients.
A rapid, accurate and precise LC-MS method is described for the quantitative determination of pramipexole in human plasma matrix using ropinirole as internal standard. Pramipexole and ropinirole were extracted from plasma by liquid-liquid extraction technique. The method was validated over the concentration range of 100-2514 pg/mL. The method was found to have acceptable accuracy, precision, linearity and selectivity. The mean extraction recovery from spiked plasma samples was in the range of 79.415-87.00 %. The intra-day accuracy of the assay ranged from 98.924 to 112.236 % and intra-day precision ranged from 3.489 to 6.756 %. Inter-day accuracy and precision results for quality control samples ranged between 100.340 and 107.443% of nominal and precision is observed to be 3.970-5.714 %. The pramipexole was found to be stable after several stability studies. The proposed method yielded a quick, simple and reliable protocol for estimating pramipexole concentrations in human plasma.
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