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A Stability Indicating LC Method for Amtolmetin Guacyl

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Abstract

A simple, sensitive gradient RP-LC assay method has been developed for the quantitative determination of amtolmetin guacyl in bulk drug, used as anti-inflammatory drug. The developed method is also applicable for related substances determination. Efficient chromatographic separation was achieved on a C18 stationary phase with simple mobile phase combination delivered in a gradient mode and quantification was carried out using ultraviolet detection at 313 nm at a flow rate of 1.0 mL min−1. In the developed LC method the resolution between Amtolmetin Guacyl and its three potential impurities was found to be greater than 2.0. Regression analysis shows an r value (correlation coefficient) greater than 0.99 for amtolmetin guacyl and its three impurities. This method was capable to detect all three impurities of amtolmetin guacyl at a level of 0.002% with respect to test concentration of 0.5 mg mL−1 for a 10 μL injection volume. The inter- and intra-day precision values for all three impurities and for amtolmetin guacyl was found to be within 2.0% RSD at its specification level. The method has shown good and consistent recoveries for amtolmetin guacyl (99.2–101.5%) and its three impurities (94.5–104.8%). The test solution was found to be stable in diluent for 48 h. The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. Considerable degradation was found to occur in oxidative stress conditions. The stress samples were assayed against a qualified reference standard and the mass balance was found close to 99.6%. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness.

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Acknowledgment

The authors wish to thank the management of United States Pharmacopeia laboratory- India for supporting this work.

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Authors and Affiliations

  1. United States Pharmacopeia India Private Limited, Reference Standard Laboratory, ICICI Knowledge Park, Turkapally, Shameerpet, Hyderabad, 500 078, India

    D. V. Subba Rao, P. Radhakrishnanand & K. V. Surendranath

  2. Hetero Laboratories Limited, Hetero House, Erragadda, Hyderabad, 500 078, India

    P. Raghuram

  3. Department of Chemistry, Jawaharlal Nehru Technological University, Kukatpally, Hyderabad, 500 072, India

    D. V. Subba Rao & V. Himabindu

Authors
  1. D. V. Subba Rao
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  2. P. Radhakrishnanand
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  3. K. V. Surendranath
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  4. P. Raghuram
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  5. V. Himabindu
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Correspondence to D. V. Subba Rao.

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Subba Rao, D.V., Radhakrishnanand, P., Surendranath, K.V. et al. A Stability Indicating LC Method for Amtolmetin Guacyl. Chroma 68, 567–577 (2008). https://doi.org/10.1365/s10337-008-0743-y

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  • DOI: https://doi.org/10.1365/s10337-008-0743-y

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