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Eco-friendly and green chromatographic method for the simultaneous determination of chlorocresol and betamethasone dipropionate in topical formulations using Box–Behnken design

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Abstract

Betamethasone dipropionate topical formulations are using to treat anti-inflammatory skin diseases such as dermatitis, eczema, and psoriasis. The current research study confers the eco-friendly toward green chemistry and stability-indicating RP-UHPLC method for the simultaneous determination of chlorocresol (CCL) and betamethasone dipropionate (BTD) in topical formulations (cream and ointment). The CCL and BTD were accurately quantitated by employing beclomethasone dipropionate (BCD) as an internal standard. The developed method was optimized utilizing QbD-based Box–Behnken Design (BBD) prior to method validation for the intended purpose. The critical quality attributes (CQAs) and critical method parameters (CMPs) identified and executed 15 design of experiments (DoEs). The foremost influencing factors were fine-tuned and optimized using graphical and numerical evaluation. The chromatographic separation was accomplished on Acquity UPLC BEH C18, 100 mm × 2.1 mm, 1.7 µm column with potassium phosphate buffer (0.02 M) and acetonitrile (ACN) using gradient elution with a runtime of 8 min. The set flow rate and injection volumes were 0.4 mL/min and 5 µL, respectively. The detection was made at 240 nm and maintained column oven temperature at 40 °C. The analytical method was validated as per the current ICH guideline Validation of Analytical Procedures: Text and Methodology Q2(R1). The linearity ranges for CCL, BTD, and BCD were 20.4–61.1, 10.3–30.8, and 10.4–31.1 µg/mL with correlation coefficients of > 0.999. As revealed, the method was superior accuracy with % recovery for CCL 98.6–101.5 and BTD 99.6–101.6 at three different levels. The results dictate the fitness of the method for the routine quality control determination of CCL and BTD from its commercial topical formulations. The proposed method with a low flow rate and less runtime benefits to analyze high throughput quality control samples with less solvent consumption, and it helps the environment by supporting the green chemistry concept.

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Acknowledgements

Authors would like to thank Douglas Pharma US Inc management for approving the publication of this article.

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Authors and Affiliations

  1. Analytical Research and Development, Douglas Pharma US Inc, 1035 Louis Drive, Warminster, PA, 18974, USA

    Siva Krishna Muchakayala & Raju V. K. Vegesna

  2. Department of Chemistry, School of Science, GITAM Deemed To Be University, Rudraram, Sangareddy, Hyderabad, Telangana, 502329, India

    Siva Krishna Muchakayala & Naresh Kumar Katari

  3. Analytical Research and Development, Cambrex High Point Inc, 4170 Mendenhall Oaks Parkway, High Point, NC, USA

    Thirupathi Dongala

  4. Analytical Research and Development, ScieGen Pharmaceuticals Inc, 89 Arkay drive, Hauppauge, NY, 11788, USA

    Vishnu Murthy Marisetti

  5. R&D and Regulatory Compliance, Invahealth Inc, 1212 South River Road, Cranbury, NJ, 08512, USA

    Govind Vyas

Authors
  1. Siva Krishna Muchakayala
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  2. Naresh Kumar Katari
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  3. Thirupathi Dongala
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  4. Vishnu Murthy Marisetti
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  5. Govind Vyas
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  6. Raju V. K. Vegesna
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Contributions

SKM performed a literature search, development of the RP-UHPLC method, data interpretation, QbD experimentation and data analysis, method validation, and original draft preparation. TD involved in QbD experiments planning, data analysis, and original draft preparation. VMM participated in manuscript review and editing. GV supported us to improve the quality of draft during revision and to address the comments in systemic way. RVKV helped with resources and proofreading. NKK provided guidance on the selection of journal and supervision of the entire process. All authors have read and agreed to the published version of the manuscript.

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Correspondence to Naresh Kumar Katari.

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Muchakayala, S.K., Katari, N.K., Dongala, T. et al. Eco-friendly and green chromatographic method for the simultaneous determination of chlorocresol and betamethasone dipropionate in topical formulations using Box–Behnken design. J IRAN CHEM SOC 19, 1397–1412 (2022). https://doi.org/10.1007/s13738-021-02388-5

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  • DOI: https://doi.org/10.1007/s13738-021-02388-5

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