Cleaning method validation for estimation of dipyridamole residue on surface of the drug product manufacturing equipment using the swab sampling and by using high performance liquid chromatographic technique.

INTRODUCTION: The cleaning validation is the procedure use to ensure the cleaning process to eliminate the residues of the drug substance after drug product manufactured in the equipment surface. A simple, sensitive, robust, accurate HPLC method was developed for the quantitative estimation of dipyridamole in the swab samples from drug product manufacturing of the Dipyridamole modified release capsules equipment surface after manufacturing.
METHODS: The method was developed by using Hypersil BDS C18 (150 mm x 4.6 mm, 5 µm) column with mobile phase containing mixture of buffer (Potassium dihydrogen phosphate buffer, pH 7.0 ± 0.05) and methanol in the ration of 30: 70 v/v, flow rate 1.5 mL/min, column temperature 45°C and injection volume as 5µL.
RESULTS: The method was validated, the specificity study was conducted to prove that, there was no interference from blank and swab blank at the retention time of dipyridamole. The limit of detection and limit of quantification limit was established by using the series of linearity solutions and found 0.041 µg/mL and 0.124 µg/mL respectively. The method precision at limit of quantification level 8.6 % RSD, Method precision 0.2 % RSD and ruggedness study results were found 0.3 % RSD. The method was accurate from the concentration of 0.13 µg/mL to 21.80 µg/mL, the recovery results were meeting the acceptance criteria. The linearity of the method was found from 0.12 µg/mL to 20.14 µg/mL and found (r2) value is 0.997. The robustness study for the flow rate, wave length, column temperature, Buffer pH and Mobile phase ratio variations were conducted, and all the system suitability parameters were meeting.
DISCUSSION AND CONCLUSION: The method validation was performed as per the regulatory requirements and guidelines. The validation parameters were meeting the acceptance criteria and proposed method can be applied for the intended swab routine analysis.