Development and validation of a high-performance liquid chromatographic method for analysis of nimesulide residues on manufacturing equipment surfaces

Abstract

In the pharmaceutical industry it is important to remove drug residues from the equipment and areas used. Cleaning procedures must be validated, so special attention must be devoted to the methods used for analysis of trace amounts of drugs. To monitor a cleaning procedure, a high-performance liquid chromatographic method for analysis of nimesulide residues in swab samples has been developed and validated. The swabbing procedure was optimized to achieve suitable recovery of nimesulide from stainless steel. Mean recovery was >80% when two swabs were used. The precision of the results, reported as the relative standard deviation (RSD), was <2.00%. The method was validated over the concentration range 0.30-50.00 μg mL -1 . Small amounts of the drug residues were analysed by HPLC with an ODS column (250 mm × 4.6 mm, 5-μm particles), at 20°C, with 65:35:3:0.13 (v/v/v/w) methanol-water-phosphate buffer (pH 3; 0.05 M)-sodium heptane sulfonate as mobile phase at a flow rate of 0.8 mL min -1 . Nimesulide was detected at 235 nm. This procedure enabled simple, sensitive, and convenient HPLC analysis of nimesulide residues on stainless steel. © 2009 Akadémiai Kiadó, Budapest.