Development and validation of a UPLC method for the determination of duloxetine hydrochloride residues on pharmaceutical manufacturing equipment surfaces

Abstract

Background: In pharmaceutical industries, it is very important to remove drug residues from the equipment and areas used. The cleaning procedure must be validated, so special attention must be devoted to the methods used for analysis of trace amounts of drugs. A rapid, sensitive, and specific reverse phase ultra-performance liquid chromatographic (UPLC) method was developed for the quantitative determination of duloxetine in cleaning validation swab samples. Material and Methods: The method was validated using an Acquity UPLC™ HSS T3 (100×2.1mm2) 1.8pm column with a isocratic mobile phase containing a mixture of 0.01M potassium dihydrogen orthophosphate, pH adjusted to 3.0 with orthophosphoric acid and acetonitrile (60:40v/v). The flow rate of the mobile phase was 0.4ml/min with a column temperature of 40°C and detection wavelength at 230nm. Cotton swabs, moisten with extraction solution (90% methanol and 10% water), were used to remove any residue of drug from stainless steel, glass and silica surfaces, and give recoveries >80% at four concentration levels. Results: The precision of the results, reported as the relative standard deviation, were below 1.5%. The calibration curve was linear over a concentration range from 0.02 to 5.0μg/ml with a correlation coefficient of 0.999. The detection limit and quantitation limit were 0.006 and 0.02μg/ml, respectively. The method was validated over a concentration range of 0.05–5.0μg/ml. Conclusion: The developed method was validated with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness.