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Validation of an HPLC Method for the Determination of Valdecoxib and its Degradation Product: a Mixture of α- and β-n-Lactosyl Sulfonamide Anomers

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An Erratum to this article was published on 29 June 2007

Abstract

An HPLC method has been developed for the separation of valdecoxib and a degradation product consisting of α and β-N-lactosyl sulfonamide, i.e. α and β anomers (SC-77852). Best results were achieved with a Chromolith Performance RP-18e column (100 mm × 4.6 mm), macropore size 2 μm, mesopore size 13 nm, with an eluent of methanol:water containing a 1% solution of TEA (36:64 v/v), pH 7.4 (adjusted with 85% orthophosphoric acid), at 22 °C. Detection was at 220 nm. The method was validated for its selectivity, linearity, precision (repeatability) and robustness. Quantitation and detection limits were determined for both valdecoxib and SC-77852. Method robustness was further evaluated by performing 23 full factorial design experiments. The final step, optimisation of the variables, was performed using response surface design. The validated method was used for assay of valdecoxib and SC-77852 in Bextra® film-coated tablets.

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Authors and Affiliations

  1. Medicines and Medical Devices Agency of Serbia, Vojvode Stepe 458, 11152, Belgrade, Serbia

    G. Savić

  2. Institute of Pharmaceutical Chemistry and Drug Analysis, Faculty of Pharmacy, Vojvode Stepe 450, P.O.Box 146, 11000, Belgrade, Serbia

    M. Zečević, B. Jocić & Lj. Živanović

Authors
  1. G. Savić
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  2. M. Zečević
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  3. B. Jocić
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  4. Lj. Živanović
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Corresponding author

Correspondence to M. Zečević.

Additional information

An erratum to this article can be found at http://dx.doi.org/10.1365/s10337-007-0328-1

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Savić, G., Zečević, M., Jocić, B. et al. Validation of an HPLC Method for the Determination of Valdecoxib and its Degradation Product: a Mixture of α- and β-n-Lactosyl Sulfonamide Anomers. Chroma 66, 29–35 (2007). https://doi.org/10.1365/s10337-007-0276-9

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