A MASS COMPATIBLE UPLC METHOD FOR THE QUANTIFICATION OF IMPURITIES IN FLUTICASONE PROPIONATE NASAL SPRAY
The objectives of the present study were to develop and validate a sensitive, selective, accurate and reproducible, mass compatible UPLC method to quantify the impurities in fluticasone nasal spray, and to establish a suitable container-closure system for the formulation.
A gradient separation method was optimized with a flow rate of 0.5 mL/min, detector wavelength-240 nm, run time-25 min and 0.1% TFA in water as solvent A and Methanol as solvent B.
The developed method was linear over the range of 0.07-1.10 ppm for impurity-I, 0.16-2.47 ppm for impurity-II, 0.67-10.0 ppm for impurity-III, and 1.29-19.3 ppm for impurity-IV. The limit of quantification (LOQ) and limit of detection (LOD) were established as 0.07 and 0.02 ppm, 0.14 and 0.05 ppm, 0.59 and 0.19 ppm, 1.06 and 0.35 ppm for impurities I-IV respectively. The percent relative standard deviation (%RSD) of the replicate analysis for impurities I-IV, was well 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 the test concentration and the results ranged from 100.3% to 109.4%. The container-closure compatibility study revealed that the solution stored in glass container system did not generate any additional peaks in the chromatogram.
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 storage of fluticasone propionate nasal solution.
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