RESUMEN
An efficient, selective, sensitive, and rapid ultra-performance liquid chromatography tandem mass spectrometry method was established and validated for the quantification of pramipexole dihydrochloride monohydrate and levodopa simultaneously in human plasma with the aid of diphenhydramine as an internal standard. A simple protein precipitation technique with HPLC grade acetonitrile was efficiently utilized for the cleanup of plasma. The analysis was performed using a Hypersil gold 50 mm × 2.1 mm (1.9 µm) column and a mobile phase of 0.2% formic acid and methanol (90: 10 v/v). The triple-quadrupole mass spectrometer equipped with an electrospray source operated in the positive mode was set up in the selective reaction monitoring mode (SRM) to detect the ion transitions m/z 212.15 â153.01, m/z 198.10â 135.16, and m/z 255.75 â 166.16 for pramipexole dihydrochloride monohydrate, levodopa, and diphenhydramine, respectively. The method was thoroughly validated according to FDA guidelines and proved to be linear, accurate, and precise over the range 100-4000 pg/mL for pramipexole dihydrochloride monohydrate and 60-4000 ng/mL for levodopa. The proposed method was effectively applied for monitoring both drugs in plasma samples of healthy volunteers.
Asunto(s)
Agonistas de Dopamina/sangre , Levodopa/sangre , Pramipexol/sangre , Espectrometría de Masas en Tándem/métodos , Administración Intravenosa , Cromatografía Líquida de Alta Presión/métodos , Agonistas de Dopamina/administración & dosificación , Agonistas de Dopamina/química , Estabilidad de Medicamentos , Humanos , Levodopa/administración & dosificación , Levodopa/química , Pramipexol/administración & dosificación , Pramipexol/químicaRESUMEN
A facile, fast and specific method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous quantitation of paracetamol, chlorzoxazone and aceclofenac in human plasma was developed and validated. Sample preparation was achieved by liquid-liquid extraction. The analysis was performed on a reversed-phase C18 HPLC column (5 µm, 4.6 × 50 mm) using acetonitrile-10 mM ammonium formate pH 3.0 (65:35, v/v) as the mobile phase where atrovastatin was used as an internal standard. A very small injection volume (3 µL) was applied and the run time was 2.0 min. The detection was carried out by electrospray positive and negative ionization mass spectrometry in the multiple-reaction monitoring mode. The developed method was capable of determining the analytes over the concentration ranges of 0.03-30.0, 0.015-15.00 and 0.15-15.00 µg/mL for paracetamol, chlorzoxazone and aceclofenac, respectively. Intraday and interday precisions (as coefficient of variation) were found to be ≤12.3% with an accuracy (as relative error) of ±5.0%. The method was successfully applied to a pharmacokinetic study of the three analytes after being orally administered to six healthy volunteers.
Asunto(s)
Acetaminofén/sangre , Clorzoxazona/sangre , Cromatografía Liquida/métodos , Diclofenaco/análogos & derivados , Espectrometría de Masas en Tándem/métodos , Acetaminofén/química , Acetaminofén/farmacocinética , Clorzoxazona/química , Clorzoxazona/farmacocinética , Diclofenaco/sangre , Diclofenaco/química , Diclofenaco/farmacocinética , Humanos , Límite de Detección , Modelos Lineales , Masculino , Reproducibilidad de los ResultadosRESUMEN
Recently, mirabegron has been added to tamsulosin to treat overactive bladder in men with benign prostatic hypertrophy. A Rapid, selective, sensitive, and green high-performance thin-layer chromatography (HPTLC) approach was developed for the simultaneous determination of tamsulosin (TAM) and mirabegron (MIR) in pure and laboratory-prepared mixture. Complete separation was obtained on silica gel F254 using the solvent system methanol-ethyl acetate-ammonia (3:7:0.1, v/v). Short-wave ultraviolet light at 270 nm was used to view the chromatographic bands. For MIR and TAM, the suggested technique revealed compact spots with retention factor Rf values of 0.42 and 0.63, respectively. Within concentration ranges of 0.15-7.5 µg/band and 0.05-2.5 µg/band, good linearity was observed, with mean percentage recoveries of 100.04 ± 0.56 and 99.98% ± 0.95 for MIR and TAM, respectively. Green assessment of the developed HPTLC technique was estimated using different green analytical chemistry metrics such as Analytical eco-scale Analytical GREEness (AGREE), and Green Analytical Procedure Index (GAPI) metrics. The proposed method was effectively used as a stability-indicating assay to assess the presence of MIR and TAM in the pharmaceutical dosage form in the presence of their degradation product. The statistical analysis showed high precision and accuracy.
RESUMEN
A highly sensitive spectrofluorimetric method is developed for the determination of prucalopride succinate (PRU). The method depends on lanthanide-sensitized luminescence due to complex formation between the drug and terbium chloride (Tb+3) which is enhanced by the addition of 8 hydroxyquinoline (8HQ) and phosphate buffer (0.02 M, pH 3.2). The calibration curve was constructed over the linear range 10-300 ng/mL after excitation at 226 nm and measuring the emission of the ternary complex at 544 nm. The method was validated according to ICH Q2 (R1) guidelines and showed a good recovery ± RSD of 100.41% ± 1.26, the limits of detection and quantitation were found to be 2.81 and 8.53 ng/mL, respectively. The proposed method was successfully applied for the determination of the drug marketed tablet dosage form and the results were in good agreement with the reference method. Also, the method greenness was evaluated according to Complex-GAPI and analytical Eco-Scale.
RESUMEN
In this work, resolution and quantitation of spectral signals are achieved by several univariate and multivariate techniques. The novel pure component contribution algorithm (PCCA) along with mean centering of ratio spectra (MCR) and the factor based partial least squares (PLS) algorithms were developed for simultaneous determination of chlorzoxazone (CXZ), aceclofenac (ACF) and paracetamol (PAR) in their pure form and recently co-formulated tablets. The PCCA method allows the determination of each drug at its λmax. While, the mean centered values at 230, 302 and 253nm, were used for quantification of CXZ, ACF and PAR, respectively, by MCR method. Partial least-squares (PLS) algorithm was applied as a multivariate calibration method. The three methods were successfully applied for determination of CXZ, ACF and PAR in pure form and tablets. Good linear relationships were obtained in the ranges of 2-50, 2-40 and 2-30µgmL(-1) for CXZ, ACF and PAR, in order, by both PCCA and MCR, while the PLS model was built for the three compounds each in the range of 2-10µgmL(-1). The results obtained from the proposed methods were statistically compared with a reported one. PCCA and MCR methods were validated according to ICH guidelines, while PLS method was validated by both cross validation and an independent data set. They are found suitable for the determination of the studied drugs in bulk powder and tablets.