Development and validation of a liquid chromatographic method for determination of lacidipine residues on surfaces in the manufacture of pharmaceuticals.

ABSTRACT

A high-performance liquid chromatographic (HPLC) method for the assay of lacidipine residues in swabs collected from various surfaces involved in drug manufacture is described. The swabbing procedure using two cotton swabs was validated applying a wipe test. An RP-HPLC method, developed to determine low quantities of the drug in the presence of its main impurities, was also validated. To remove drug residues from stainless steel and glass surfaces, the first cotton swab must be soaked preferably in acetonitrile whereas, on vinyl surfaces better results are obtained using methanol. The HPLC method selected involves a C12 column, at 40 degrees C, a mixture of acetonitrile-0.05 M ammonium acetate (8812, v/v) as a mobile phase and UV detection at 282 nm. Recoveries obtained are strongly dependent on the type of surface tested, being higher on stainless steel. The surface material has also different influence on the drug stability. The method was validated over a range of 0.5-100 microg/400 cm2 and had a detection limit of 0.1 microg/400 cm2.