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

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Abstract

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 °C in a 10 min linear ramp. The chromatographic separation was performed on a Discovery RP-Amide C16 column (250 × 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.

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Acknowledgments

This research was supported by a grant of the Italian Medicines Agency (AIFA).

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Authors and Affiliations

  1. Dipartimento del Farmaco, Istituto Superiore di Sanità, Viale Regina Elena 299, 00161, Rome, Italy

    Stefano Labbozzetta, Luisa Valvo, Paola Bertocchi, Stefano Alimonti, Maria Cristina Gaudiano & Livia Manna

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  1. Stefano Labbozzetta
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  2. Luisa Valvo
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  3. Paola Bertocchi
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  4. Stefano Alimonti
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  5. Maria Cristina Gaudiano
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  6. Livia Manna
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Correspondence to Livia Manna.

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Labbozzetta, S., Valvo, L., Bertocchi, P. et al. Focused Microwave-Assisted Extraction and LC Determination of Ketoprofen in the Presence of Preservatives in a Pharmaceutical Cream Formulation. Chroma 69, 365–368 (2009). https://doi.org/10.1365/s10337-008-0892-z

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  • DOI: https://doi.org/10.1365/s10337-008-0892-z

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