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

Milenović D. M., Todorović Z. B.

Acta Chromatographica

2009

Vol. 21, no. 4

603--618

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.

Validation of an HPLC method for analysis of nifedipine residues on stainless-steel surfaces in the manufacture of pharmaceuticals

Milenović D. M., Lazić M. L., Veljković V. B., Todorović Z. B.

Acta Chromatographica

2008

Vol. 20, no. 2

183-194

A simple, sensitive, and convenient HPLC method has been developed, validated, and applied to analysis of nifedipine residues on the stainless-steel surfaces of equipment used in drug manufacture. Cotton swabs moistened with methanol were used to remove residues of the drug from the surfaces; recoveries were 82.26, 86.88, and 88.95% for 25, 125, and 250 µg per swab. The precision of the results, as relative standard deviation (RSD), was <5%. The method was validated over the concentration range 3-50 µg mL-1. Small quantities of residues of the drug and its main impurities were determined by HPLC on an ODS column with methanol-water-phosphate buffer (pH 3; 0.05 M)-sodium heptanesulfonate 65:35:3:0.13 (v/v/v/w) as mobile phase at a flow rate of 0.8 mL min-1. Detection was at 235 nm.