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Integrative Validation Method of Roflumilast by Quantification and Detection in Lipid-Nanoparticles via Reverse Phase HPLC

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Abstract

Purpose

The aim of current study is to develop an accurate, ideal, and precise Reverse-Phase HPLC (High-Performance Liquid Chromatography) method for detecting and quantifying roflumilast (ROF) in Lipid-nanoparticles for the very first time. Nowadays, HPLC is an extensively utilized quantitative analytical technology in the pharmaceutical sciences.

Method

RP HPLC (Shimadzu 20A) ROF detection method was validated with a mobile phase of distilled water and acetonitrile having 40:60 concentrations. Samples were analyzed via isocratic elution of 10 μl injection volumes, a PDA detector, using a C18 Backmann column silica column (4.6*250-mm-wide) as the stationary phase and the ambient temperature of the column was sustained at 45 °C with 35 MPa max pressure. A flow rate of 1 ml/min was run over 15 min (run time) and ROF was observed at a wavelength of 254 nm with a linearity range of 70–130% (40–300 µg).

Results

All HPLC analytical parameters accuracy, precision, linearity, and range were studied and optimized according to ICH guidelines. The retention time of Lipid-nanoparticles of Rof was 7.1 ± 0.02 min and approximately 100 percent accuracy, specificity and precision were achieved with this method. The values of limit-of-detection (LOD) and limit-of-quantification-(LOQ)-were found to be  – 0.0041 and 0.031 µg/ml respectively.

Conclusion

This validated analytical method was so sensitive and site-specific for the verification of roflumilast in lipid-based formulations.

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Authors and Affiliations

  1. Department of Pharmacy, Quaid-I-Azam University, Islamabad, 45320, Pakistan

    Iqra Chaudhery, Marya Nawaz Malik, Tofeeq Ur-Rehman, Humaira Fatima, Asim Ur-Rehman & Naveed Ahmed

  2. Univercity of Lyon, University Claude Bernard Lyon-1, CNRS, ISA-UMR 5280, 69622, Villeurbanne, France

    Abdelhamid Elaissari

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Chaudhery, I., Malik, M.N., Ur-Rehman, T. et al. Integrative Validation Method of Roflumilast by Quantification and Detection in Lipid-Nanoparticles via Reverse Phase HPLC. Chemistry Africa 7, 131–140 (2024). https://doi.org/10.1007/s42250-023-00719-y

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