An analytical method based on liquid-liquid extraction has been developed and validated for analysis of agomelatine in human plasma. Fluoxetine was used as an internal standard for agomelatine. A Betasil C18 (4.0 × 100 mm, 5 µm) column provided chromatographic separation of analytes followed by detection with mass spectrometry. The method involves simple isocratic chromatographic conditions and mass spectrometric detection in the positive ionization mode using an API-4000 system. The proposed method has been validated with linear range of 0.050-8.000 ng/ml for agomelatine. The intra-run and inter-run precision values are within 12.12% and 9.01%, respectively, for agomelatine at the lower limit of quantification level. The overall recovery for agomelatine and fluoxetine was 67.10% and 72.96%, respectively. This validated method was used successfully for analysis of plasma samples from a pharmacokinetic study.
A simple, fast and precise reversed phase high performance liquid chromatographic method is developed for the simultaneous determination of aceclofenac, paracetamol and chlorzoxazone. Chromatographic separation of the three drugs was performed on an Intersil C18column (250 mm × 4.6 mm, 5µm) as stationary phase with a mobile phase comprising of 10 mM potassium dihydrogen phosphate (pH adjusted to 5.55 with ammonia): acetonitrile in the ratio 60:40 (v/v) at a flow rate of 1.0 mL/min and UV detection at 205 nm. The linearity of aceclofenac, paracetamol and chlorzoxazone were in the range of 5.00-15.00 µg/µL, 25.00-75.00 µg/µL and 25.00-75.00 µg/µL respectively. The limit of detection for aceclofenac, paracetamol and chlorzoxazone was found to be 18.0 ng/mL, 22.0 ng/mL and 9.0 ng/mL respectively whereas, the limit of quantification was found to be 55 ng/mL, 65 ng/mL and 27.0 ng/mL respectively. The recovery was calculated by standard addition method. The average recovery was found to be 99.04%, 99.57% and 101.63% for aceclofenac, paracetamol and chlorzoxazone respectively. The proposed method was found to be accurate, precise and rapid for the simultaneous determination of aceclofenac, paracetamol and chlorzoxazone
The mixed ligand complexes of Co(II), Ni(II), Cu(II) and Zn(II) with Schiff bases N-(2-hydroxy-1-naphthylidene)-4-methylaniline (L 1 H) and N-(2-hydroxybenzylidene)-2,3-dimethylaniline (L 2 H) have been synthesized and characterized. The resulting complexes were characterized by elemental analysis, thermogravimetric analysis, magnetic moment measurements, conductivity measurements, 1 H NMR, IR, UV-visible and ESR spectral studies. The Schiff bases acts as bidentate monobasic ligands, coordinating through deprotonated phenolic oxygen and azomethine nitrogen atoms. The complexes are non-electrolytic in DMSO. The presence of the two coordinated water molecules in these complexes was indicated by IR spectra and thermogravimetric analysis of the complexes. From the analytical and spectral data the stoichiometry of these complexes have been found to be [M(L 1 )(L 2 )(H 2 O) 2 ] {where M = Co(II) , Ni(II), Cu(II) and Zn(II)}. It is found that Co(II), Ni(II), Cu(II) and Zn(II) complexes exhibited octahedral geometry. The antimicrobial activities of ligands and their mixed ligand complexes were screened by disc diffusion method. It is found that the metal complexes have higher antimicrobial activity than the free ligand.
A simple, precise and rapid isocratic reverse phase high performance liquid chromatographic method was developed for the simultaneous determination of paracetamol, chlorzoxazone and diclofenac sodium from tablet dosage form. The chromatographic separation was performed on an inertsil C18column (250 mm × 4.6 mm i.d 5 µm particle size). Mobile phase consisted of a mixture of phosphate buffer (0.02 M KH2PO4, pH adjusted to 3.7 using orthophosphoric acid), acetonitrile and methanol in the ratio of (25: 25: 50) at a flow rate of 1.0 mL/min. The wavelength was set at 220 nm. The proposed method was validated for linearity, accuracy, precision, LOD and LOQ. The calibration was linear over the range of 50-150 µg/mL for paracetamol, 50-150 µg/mL for chlorzoxazone and 5-15 µg/mL for diclofenac sodium. The retention times were found as 2.8 min for paracetamol, 4.2 min for chlorzoxazone and 6.4 min for diclofenac sodium. The method can be easily adopted for quality control analysis.
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