RP-HPLC method validation for fast extraction and quantification of Levonorgestrel drug from silicone based intrauterine device intended for in-process and finished formulation

Abstract

Background

To develop and validate a simple and consistent reversed phase high performance liquid chromatography (RP-HPLC) method for the estimation of Levonorgestrel (LNG) drug from silicone based intrauterine device.

Methods

Sample solution was prepared using tetrahydrofuran (THF) as solvent for the drug extraction, and RP-HPLC analysis was performed using Luna C18 analytical column (150 × 4.6 mm, 5 μm, 100 Å – Phenomenex), with a mobile phase consisting of a mixture of acetonitrile and water (50:50, v/v) at a flow rate of 1.0 ml/min and injection volume of 20 μl. Detection was carried out at 241 nm in PDA detector, with a total run time of 15 min. The method was validated in accordance with ICH guidelines. Method applicability was tested for optimizing formulation using quality-by-design approach, to check the stability and content uniformity of levonorgestrel-silicone mixture (core blend), and quantifying the amount of LNG from commercially available silicone based formulation.

Results

The retention time for LNG drug was obtained at 8.5 min (± 0.3 min). A linear relationship was observed over the concentration range of 2.6–15.6 μg/ml with the correlation coefficient (r) value 0.9999. The method was found to be precise within the acceptable limit (RSD < 2%) and the drug recovery from the intrauterine device was found in the range 99.78–100.0%. Content uniformity for different prototypes developed was observed in the range of 91.6–101.4%, and assay of optimized core blend was in the range of 97.78–106.79% during the 10 days of retention period for stability studies.

Conclusion

The validated method is found to be a simple, accurate, precise, reproducible, and hence can be used for the routine analysis of LNG such as in-process, quality control and stability assays of silicone based intrauterine devices by RP-HPLC.

Graphical abstract

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Acknowledgements

The authors acknowledge HLL Lifecare Limited, Trivandrum, Kerala, India for financial support and for providing research facilities.

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Correspondence to Diksha Painuly.

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Veeran, M.G., C., K., B., B. et al. RP-HPLC method validation for fast extraction and quantification of Levonorgestrel drug from silicone based intrauterine device intended for in-process and finished formulation. DARU J Pharm Sci (2021). https://doi.org/10.1007/s40199-021-00396-7

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Keywords

  • Levonorgestrel
  • Silicone
  • Intrauterine device
  • Validation
  • Quality by design (QbD)