A MASS COMPATIBLE UPLC METHOD FOR THE QUANTIFICATION OF IMPURITIES IN FLUTICASONE PROPIONATE NASAL SPRAY

  • MUGADA RAVI PRASADA RAO Analytical Research and Development, Integrated Product Development, Dr. Reddy’s Laboratories Ltd., Bachupally, Hyderabad 500090, India
  • RAMA KRISHNA THOTA Analytical Research and Development, Integrated Product Development, Dr. Reddy’s Laboratories Ltd., Bachupally, Hyderabad 500090, India
  • MAHIBALAN SENTHI Analytical Research and Development, Integrated Product Development, Dr. Reddy’s Laboratories Ltd., Bachupally, Hyderabad 500090, India
  • PAUL MOGADATI AR and D Consultant, Innovative Scientific Services Inc., Rutgers University, East Greenbush, New York, USA
  • SRINIVAS ARUTLA Head Product Development, Apotex Research Pvt. Ltd., Bengaluru, India

Abstract

Objective: The objectives of the present study were to develop and validate a mass compatible ultra-performance liquid chromatography (UPLC) method to quantify the impurities in fluticasone nasal spray, and to establish a suitable container-closure system for the formulation.


Methods: A gradient method was optimized with a flow rate of 0.5 ml/min, detector wavelength-240 nm, run time-25 min and 0.1% Trifluoroacetic acid (TFA) in water as solvent A and Methanol as solvent B.


Results: The developed method was linear over the range of 0.07-1.10 µg/ml for impurity-I, 0.16-2.47 µg/ml for impurity-II, 0.67-10.0 µg/ml for impurity-III, and 1.29-19.3 µg/ml for impurity-IV. The limit of quantification (LOQ) and limit of detection (LOD) were established as 0.07 and 0.02 µg/ml, 0.14 and 0.05 µg/ml, 0.59 and 0.19 µg/ml, 1.06 and 0.35 µg/ml for impurities I-IV respectively. The percent relative standard deviation (%RSD) of the replicate analysis for impurities I-IV, was within the acceptance criteria (0.4, 0.2, 0.3, and 0.1% respectively) that proved the precision of the method. The accuracy of the method was studied from 50%-150% of test concentration and the results ranged from 100.3% to 109.4%. The container-closure compatibility study revealed that the solution stored in the glass container system did not generate any additional peaks in the chromatogram.


Conclusion: Hence, the developed method can be employed by quality testing laboratories to quantify impurities in fluticasone propionate nasal spray. The study also suggests that glass containers could serve as a compatible system for the storage of fluticasone propionate nasal solution.

Keywords: Fluticasone propionate, UPLC, Nasal spray, Impurities, Method validation

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References

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RAO, M. R. P., R. K. THOTA, M. SENTHI, P. MOGADATI, and S. ARUTLA. “A MASS COMPATIBLE UPLC METHOD FOR THE QUANTIFICATION OF IMPURITIES IN FLUTICASONE PROPIONATE NASAL SPRAY”. International Journal of Pharmacy and Pharmaceutical Sciences, Vol. 12, no. 11, Nov. 2020, pp. 80-87, doi:10.22159/ijpps.2020v12i11.38750.
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