Focused Microwave-Assisted Extraction and LC Determination of Ketoprofen in the Presence of Preservatives in a Pharmaceutical Cream Formulation

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• 作者：Stefano Labbozzetta ; Luisa Valvo ; Paola Bertocchi ; Stefano Alimonti ; Maria Cristina Gaudiano and Livia Manna
• 关键词：Column liquid chromatography ; Microwave ; Assisted extraction ; Counterfeit drugs ; Ketoprofen
• 刊名：Chromatographia
• 出版年：2009
• 出版时间：February, 2009
• 年：2009
• 卷：69
• 期：3-4
• 页码：365-368
• 全文大小：264.7 KB

文摘

A simple and rapid open-vessel focused microwave-assisted extraction (FMAE) method followed by LC analysis was developed for the determination of ketoprofen lysine salt in the presence of methyl p-hydroxybenzoate and propyl p-hydroxybenzoate preservatives in topical cream. Extraction were performed in acetone/potassium dihydrogenphosphate (25 mM, pH 3.0) (70:30 v/v) by reaching a target temperature of 65 ¡ãC in a 10 min linear ramp. The chromatographic separation was performed on a Discovery RP-Amide C16 column (250 ¡Á 4.6 mm I.D., 5 μm particle size). The optimal mobile phase consisted of acetonitrile/potassium dihydrogen phosphate 25 mM adjusted to pH 3.0 with phosphoric acid (50:50 v/v). The complete analytical procedure was validated with regard to limit of quantification, linearity, precision and accuracy. The method was linear over the concentration range of 0.08–0.12 mg mL−1; the relative standard deviations of intra- and inter-day assays were 1.9–2.3 and 1.8 % respectively. The limit of quantification was 0.54 μg mL−1. The proposed method shows many advantages as short extraction time, little solvent consumption without requiring further sample clean-up steps before liquid chromatographic analysis and is proposed for vast scale screening of cream dosage forms aimed to the detection of counterfeit and substandard drugs.