Rapid, sensitive and specific methods were developed for the determination of diclofenac in pharmaceutical preparations by linear sweep voltammetry (LSV) and gas chromatography (GC) with mass spectrometry (MS) detection. The linearity was established over the concentration range of 5–35 μg/mL for LSV and 0.25–5 μg/mL for GC–MS method. The intra- and inter-day relative standard deviation (RSD) was less than 4.39% and 4.62% for LSV and GC–MS, respectively. Limits of quantification (LOQ) were determined as 4.8 and 0.15 μg/mL for LSV and GC–MS, respectively. No interference was found from tablet excipients at the selected assay conditions. The methods were applied for the quality control of commercial diclofenac dosage forms to quantify the drug and to check the formulation content uniformity.
A simple high-performance liquid chromatography method has been developed for the determination of naproxen in human plasma. The method was validated on an Ace C18 column using ultraviolet detection. The mobile phase consisted of 20 mM phosphate buffer (pH 7) containing 0.1% trifluoroacetic acid-acetonitrile (65:35, v/v). The calibration curve was linear between the concentration ranges of 0.10 and 5.0 µg/mL. Intra-day and inter-day precision values for naproxen in plasma were less than 4.84, and accuracy (relative error) was better than 3.67%. The extraction recovery values of naproxen from human plasma were between 91.0 and 98.9%. The limits of detection and quantification of naproxen were 0.03 and 0.10 µg/mL, respectively. Also, this assay was applied to determine the pharmacokinetic parameters of naproxen in six healthy Turkish volunteers who had been given 220 mg of naproxen.
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