CLEANING VALIDATION FOR ESTIMATION OF ACTIVE INGREDIENTS’ RESIDUES OF VICAZID UNCOATED TABLETS (PYRANTEL 100 MG/MEBENDAZOLE 150 MG) ON SURFACES OF PHARMACEUTICAL MANUFACTURING EQUIPMENT USING SWAB SAMPLING AND HPLC METHOD

摘要

Objective: The validation of HPLC methods for residual estimation of pyrantel and mebendazole in swab samples from equipment surfaces after manufacturing of Vicazid uncoated tablets and the demonstration of the efficiency of the cleaning procedure. Methods: For pyrantel residues: Column-Luna Silica 250×4.6 mm, 5 μm; Mobile phase-a mixture of acetonitrile, acetic acid, diethyl amine and water (92.8:3:1.2:3); The flow rate-1.0 ml/min; The detector wavelength-288 nm; The injection volume-20 μl. For mebendazole residues: Column-Luna C18(2) 150×4.6 mm, 5 μm; Mobile phase-a mixture of methanol and 0.05 M monobasic potassium phosphate solution (60:40) pH 5.5; The flow rate-1.5 ml/min; The detector wavelength-247 nm; The injection volume-15 μl. Results: The calibration curve is linear (the correlation coefficient>0.999) over a concentration range 0.04-80μg/ml (pyrantel pamoate) and 0.005-50μg/ml (mebendazole); The limit of detection and limit of quantitation-0.04 (pyrantel pamoate)/0.005 (mebendazole) and 0.08 (pyrantel pamoate)/0.0125μg/ml (mebendazole), respectively; The mean recovery is>90 %; No interference from swab solution was observed and samples were stable for 24?h. The determined amounts (varying 0.02–9.74 μg pyrantel residues and 0.09–61.19 μg mebendazole) are well below the calculated limit of contamination. Conclusion: The HPLC methods with appropriate swab wipe procedure were validated and the obtained results confirm that the cleaning procedures used are able to remove residues of both active ingredients from equipment surfaces. Keywords : Residual estimation, Swab sampling, Cleaning validation, HPLC