Development and Validation of Stability-Indicating Impurity Profiling Method for Azelastine Hydrochloride and...

Azelastine HCl (AZ) and fluticasone propionate (FL) nasal spray drug product is commonly used in the treatment of allergic rhinitis worldwide. To date, the impurity profiling of this product has not been reported.

The present study aimed to develop and validate a novel RP-HPLC stability-indicating analytical method for the estimation of impurities from AZ and FL nasal spray drug product.

A mixture of octane sulfonic acid sodium salt and trifluroacetic acid is used as a mobile phase A. Acetonitrile is used as a mobile phase B. Good separation was achieved on Baker bond phenyl hexyl, 250 × 4.6, 5 µm column at 1 mL/min flow rate in gradient elution mode. The chromatograms were monitored at 239 nm.

The LOD and LOQ were found to be 0.006 and 0.019 µg/mL for AZ and 0.010 and 0.030 µg/mL for FL, respectively. The correlation coefficient for all the known impurities and principal analytes was 0.999 from LOQ level to 150% of standard concentration. The recovery for all the known impurities was found to be between 90 and 110%. In the stress study, 15% degradation was observed in basic conditions and 8.7% in acidic conditions. No significant degradation was observed in thermal and oxidative conditions.

An impurity profiling method for AZ and FL combination nasal spray product was successfully developed, validated, and demonstrated to be accurate, precise, specific, robust, and stability-indicating. The method can be routinely used for impurity testing of commercial batches in QC laboratories in the pharmaceutical industry.

No impurity study has been reported for this combination product until now.