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Simultaneous estimation of nimesulide and chlorzoxazone in pharmaceutical formulations by a RP-HPLC method
Abstract
A rapid and sensitive high performance liquid chromatography method for determination of nimesulide and chlorzoxazone has been developed. The chromatography system used a reversed phase C18 column (Inertsil C18, 5μ , 150 mm x 4.6 mm). The sample was analyzed using Acetonitrile: Methanol: Phosphate buffer, in the ratio of 50:30:20: (pH adjusted to 4.50 with orthophosphoric acid) as a mobile phase at a flow rate of 1.0 ml/min and detection at 280 nm. The retention time for nimesulide and chlorzoxazone was found to be 3.24 and 4.85 min respectively, and recoveries from tablet were between 99 and 101 %. The method can be used for estimation of combination of these drugs in tablets.
... For CHZ, UV method [15,16,18,[35][36][37] RP-HPLC method [38,39], HPLC/UV method for analysis of plasma/serum samples [40,41] and HPTLC [33] methods have been reported. ...
... Similarly, for NIM UV method [37,42,43], RP-HPLC [38,[44][45][46][47] and HPTLC [33,48] methods have been reported. ...
A simple, precise, and accurate reversed-phase liquid chromatographic method has been developed for the simultaneous determination of paracetamol (PCM), chlorzoxazone (CHZ), and nimesulide (NIM) in pharmaceutical dosage form. The chromatographic separation was achieved on a Thermo Hypersil GOLD C18 column (250 × 4.6 mm i.d., 5 μm particle size). The mobile phase consisted of water : acetonitrile (55 : 45 v/v). The flow rate was set to 1.2 mL min−1 and UV detection was carried out at 275 nm. The retention time () for PCM, CHZ, and NIM was found to be 2.69 ± 0.02, 4.61 ± 0.01, and 9.55 ± 0.02 min, respectively. The validation of the proposed method was carried out for linearity, precision, robustness, limit of detection, limit of quantitation, specificity, and accuracy. The linear dynamic ranges were 32.5–65.0 μg mL−1 for PCM, 37.5–75.0 μg mL−1 for CHZ, and 10.0–20.0 μg mL−1 for NIM. The developed method can be used for routine quality control analysis of titled drugs in pharmaceutical dosage form.
The voltammetric behavior of chlorzoxazone at gold electrode has been investigated for the first time using cyclic, linear sweep, and square wave voltammetric techniques. The dependence of the current on pH, concentration, and scan rate was investigated to optimize the experimental conditions for the determination of chlorzoxazone. The effect of surfactants was studied. The anodic peak was characterized and process was diffusion controlled. The number of electrons transferred in the oxidation process was calculated, and a plausible oxidation mechanism was proposed. In the range of 5.0 x 10(-6) to 1.0 x 10(-4) M, the current measured by square wave voltammetry presents a good linear property as a function of the concentration of chlorzoxazone with a detection limit of 0.45 x 10(-7) M with good selectivity and sensitivity. The proposed method was successfully applied to chlorzoxazone determination in pharmaceutical samples and for the detection of chlorzoxazone in urine as a real sample. This method can be employed in clinical analysis, quality control, and routine determination of drugs in pharmaceutical formulations.
The electrochemical behavior of chlorzoxazone drug at glassy carbon electrode has been investigated for the first time using cyclic and square wave voltammetric techniques. The dependence of the current on pH, concentration, and scan rate was investigated to optimize the experimental conditions for determination of chlorzoxazone. The anodic peak was characterized and the process was diffusion-controlled. The number of electrons transferred in the oxidation process was calculated and a plausible oxidation mechanism was proposed. In the range of 8.0 × 10–7 to 1.0 × 10–5 M, the current measured by square wave voltammetry presents a good linear property as a function of the concentration of chlorzoxazone with a detection limit of 4.41 × 10–8 M with good selectivity and sensitivity. The proposed method was successfully applied to chlorzoxazone determination under physiological condition in pharmaceutical samples and for the detection of chlorzoxazone in human biological fluids. This method can be employed in clinical analysis, quality control, and routine determination of drugs in pharmaceutical formulations.
A simple, selective, rapid, precise and economical reverse phase HPLC method has been developed for the simultaneous estimation of nimesulide and diclofenac sodium from capsules. The analyte was resolved by using a mobile phase (methanol and water in the ratio 50:50) at a flow rate of 1 mi/min. on an isocratic HPLC system consisting of LC-10 AT liquid pump, SPD-10A UV/ Visible detector, a ODS C-18 RP column (4.6 mm I.D. x 25 cm) at a wavelength of 230 nm. The linear dynamic range for both nimesulide and diclofenac sodium was 0.5-30 μg/ml and 2.0-30 μg/ mi respectively by this method. Paracetamol was used as an internal standard.