Separation of aceclofenac and diclofenac in human plasma by free zone capillary electrophoresis using N-methyl-d-glucamine as an effective electrolyte additive (original) (raw)
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2020
Method development is the process to prove that the analytical methods employed to measure the concentration of active pharmaceutical drug in a particular compounded dosage form is acceptable. This must be validated to provide accurate data for regulatory submissions. Aceclofenac (ACE) is an analog of diclofenac, a non-steroidal anti-inflammatory drug (NSAIDs). The drug is used in osteoarthritis, rheumatoid arthritis, ankylosing spondylitis ankylosing spondylitis, inflammation and relief of pain. The high importance of this class of drugs has prompted us to review the most important recent spectrophotometric methods for analyzing Aceclofenac in pure formulations, in various types of pharmaceutical dosage and in biological fluids published in the literature to date. They include spectrophotometry, high performance liquid chromatography, high performance thin layer chromatography, liquid chromatography-mass spectrometry, ultra high-performance liquid chromatography, mass spectrometry,...
Studia Universitatis Babeș-Bolyai Chemia, 2019
The purpose of this study was the development and validation of an LC-MS/MS method, for the determination of diclofenac from human plasma. The sample workup involved a simple protein precipitation procedure. A core/shell type analytical column (50×2,1 mm, 2.6 Å) was used with C18 stationary phase. The mobile phase consisting of 52.5% acetonitrile and 47.5% water provided good peak shape, accuracy and precision (stable ionization). The mass spectrometer was operated in negative electrospray ionization mode for analyte and internal standard. The following parameters were evaluated for validation purpose: Selectivity, sensitivity, matrix effect, anticoagulant effect, linearity, precision and accuracy, recovery, short and long term analyte/IS stability in solvent/matrix and carryover. The validated calibration range was 3.9-1194 ng/ml. The correlation coefficient R 2 was at least 0.999 in all validation batches. The validated method has been successfully used for the evaluation of bioequivalence of a generic diclofenac potassium formulation of 12.5 mg strength.
Journal of AOAC International, 2002
Two novel analytical methodologies using capillary electrophoresis (CE) and liquid chromatography (LC) were developed and compared for the determination of diclofenac sodium in commercial and simulated tablet formulations. The CE analysis was performed in a bare fused-silica capillary with 75 microm id and total length of 50 cm (28 cm to the detector) with a buffer solution of 20 mM sodium tetraborate, pH 9.23. The applied voltage was 20 kV, and acetaminophen was used as the internal standard (IS). The LC analysis was performed with a LiChrospher 100 RP-18 (5 microm) column and a mobile phase of methanol-diluted glacial acetic acid (0.3 parts in 2500; 75 + 25) at a flow rate of 0.9 mL/min with propylparaben as the IS. In both analyses, detection was by ultraviolet absorption at 276 nm. Under optimized conditions, the CE migration times for the diclofenac sodium standard and acetaminophen (IS) were 2.07 and 1.59 min, respectively, and the LC retention times for the diclofenac sodium ...
Journal of Pharmacy and Chemistry, 2010
A fast, sensitive and specific LC-MS/MS method for the determination of Aceclofenac in human plasma has been developed and validated over the range of 0.106 μg/ml to 14.060 μg/ml (r2 >0.999). Samples (200 μL) were buffered (pH 6.8), extracted using acetonitrile and 5 μL of sample extract was injected into the LC-MS/MS system. Analysis was performed using anal micro C18 (4.6 X 50 mm, 50μm, 60AO) column by gradient elution at a flow rate of 0.350 ml/min over a 2min’s run-time. Retention times of Aceclofenac and Diclofenac (Internal Standard) were observed at 1.20 and 1.21 min’s respectively. Detection was achieved by using Thermo, Triple Quadruple mass spectrometer, in positive electro spray ionization mode. Ion transitions were monitored using MRM (multiple reaction monitoring) for drug (m/z 354 –> 250) and for IS (m/z 296.1 –> 215). This validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic, bioavailability or bioequivalence studies.
Rapid determination of diclofenac in pharmaceutical formulations by capillary zone electrophoresis
Scientia pharmaceutica, 2012
Capillary electrophoresis is competitive to HPLC and other chromatographic methods, predominantly when charged analytes have to be separated. The time of analysis can be reduced by the use of very short capillaries applying a high voltage. In most instruments which are commercially available the so-called 'short end' of the capillary can be used for separation, leading to very rapid separations. In this contribution we want to demonstrate this approach by using Diclofenac Sodium as an analyte.
Journal of Chromatography B: Biomedical Sciences and Applications, 1989
sodium, sodmm o-(2,6-dlchlorophenyl )ammophenylacetate (Voltaren 1, 1s a potent non-steroidal anti-inflammatory and analgesic drug, which has been used successfully for several years m the treatment of rheumatic deseases [l-3] This compound 1s metabolized m animals and humans to the corresponding mono-and dlhydroxy and conjugated derlvatlves [4,5] Several methods have been described for its determmatlon m body flulds, includmg gas chromatography with electron-capture detection [ 6,7], gas chromatography-mass spectrometry and high-performance llquld chromatography (HPLC) with VV detection [lo-21
Journal of Chromatography B: Biomedical Sciences and Applications, 2001
A novel high-performance liquid chromatographic (HPLC) method for the quantification of diclofenac in human plasma was set up. Samples, added with ibuprofen (used as internal standard) were purified by solid-phase extraction using Abselut Nexus cartridges (Varian) not requiring pre-conditioning. Drugs of interest were eluted directly into the autosampler vials and injected. The recovery of diclofenac was 92%, the analysis lasted
Journal of chromatography, 1993
An assay using reversed-phase high-performance liquid chromatography with ultraviolet detection, at 278 nm, was developed to measure diclofenac in human plasma and urine at concentrations suitable for biopharmaceutical studies. Indomethacin was used as internal standard and separation was performed at 40 degrees C on a C18 Spherisorb column with acetonitrile-0.1 M sodium acetate (35:65, v/v) (pH 6.3) as mobile phase. The sample preparation is simple and rapid (extractionless), and the total run time is less than 5 min. The retention time is 2.8 min for diclofenac and 3.6 min for indomethacin. The detection limit is 0.2 microgram/ml using a 20-microliters loop.
A new RP-HPLC-UV method for the simultaneous quantification of aceclofenac in bulk & its tablets
Asimple, selective, linear, precise, and accurate RP-HPLC method was developed and validated for the estimation of Aceclofenac from bulk drug. Chromatographic separation was achieved isocratically on a Phenomenex, C8 column (250×4.6 mm, 3 µ particle size) using a mobile phase, (0.01M ammoniumacetate bufferwith 2ml triethylamine, (v/v)-acetonitrile (68:32 v/v) pH was adjusted to 6.5 with glacialAcetic acid. The flowrate was 1.2 ml/min and effluent was detected at 270 nm and 20ìl of sample was injected. The retention time of Aceclofenac was 6.4 min. Linearity was observed in the concentration range of 8-16 µg/ml. Percent recoveries obtained for Aceclofenac was 99.65-99.93%. The percentage RSD for precision and accuracy of the method was found to be less than 1%. The method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy, precision, LOD and LOQ. The method developed was successfully applied for the analysis& estimation of Aceclofenac in bulk drug.