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Development and Validation of a Stability-Indicating HPLC Method for Assay of Milbemycin Oxime and Estimation of Its Related Compounds

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Abstract

A stability-indicating reversed-phase HPLC method for assay of milbemycin oxime (MO) and estimation of its related compounds has been developed and validated as per VICH and ICH method validation guidelines. The stability-indicating capability of this method has been demonstrated by adequate separation of all process-related impurities including all potential degradation products of milbemycin oxime (MO) that were generated using stress degradation conditions that are prescribed in ICH guideline. The stability-indicating capabilities of this method were further challenged by analyzing aged stability samples of MO active pharmaceutical ingredient (API). Chromatographic separation of MO and its related compounds was achieved using an isocratic elution at a flow rate of 0.5 mL/min on a Supelco Ascentis Express C18 column (100 mm × 3.0 mm, 2.7 µm particle size, 90 Å pore size) maintained at 50 °C. The isocratic mobile phase was composed of 30% v/v of 0.05% phosphoric acid in aqueous solution and 70% v/v of a mixture of methanol and acetonitrile (6:4, v/v). UV detection at 244 nm was employed to monitor the analytes.

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Acknowledgements

The authors would like to thank BIAH and all the analytical scientists in Global Pharmaceutical Technical Support (GPTS) of BIAH at North Brunswick, New Jersey (R&D site) for their support of this study.

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This research did not receive any specific grant from funding agencies in the public, commercial, or not-for-profit sectors.

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Authors and Affiliations

  1. Boehringer Ingelheim Animal Health (BIAH), 631 US Route 1 South, North Brunswick, NJ, 08902, USA

    Junmin Huang, Jiangtao He & Abu M. Rustum

Authors
  1. Junmin Huang
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  2. Jiangtao He
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  3. Abu M. Rustum
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Correspondence to Jiangtao He.

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Huang, J., He, J. & Rustum, A.M. Development and Validation of a Stability-Indicating HPLC Method for Assay of Milbemycin Oxime and Estimation of Its Related Compounds. Chromatographia 84, 483–498 (2021). https://doi.org/10.1007/s10337-021-04028-9

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