Assessment of MEKC suitability for residue drug monitoring on pharmaceutical manufacturing equipment.

The suitability of micellar electrokinetic chromatography for the simultaneous trace determination of several compounds (sulfamethoxazole, trimethoprim, sulfanilic acid, sulfanilamide, 3,4,5-trimethoxybenzoic acid and nonoxynol-9) was assessed. The mixture was separated within 14min at an applied voltage of 22kV by using 30mM phosphate electrolyte, containing 10mM SDS, adjusted to pH 7.8. Under optimized separation conditions acceptable levels of linearity, precision and accuracy were obtained for all compounds. The method could be used as part of a cleaning validation study when assaying trace levels of co-trimoxazole drug, some of its decomposition products and detergent in the swab samples collected from pharmaceutical manufacturing equipment, after cleaning.

A validated HPLC method for determining residues of a dual active ingredient anti-malarial drug on manufacturing equipment surfaces.

Analytical method validation, determining the recovery rate from the equipment surface and the stability of a potential contaminant are important steps of a cleaning validation process. A rapid, sensitive and reproducible reversed-phase high-performance liquid chromatographic method was developed for the determination of pyrimethamine (PYR) and sulfadoxine (SUL) in cleaning validation swab samples. The active compounds can be selectively quantified in a sample matrix containing detergent and swab material as low as 0.12 microg/ml. The swabbing procedure used on stainless steel coupons was validated and the stability of PYR and SUL in the swab samples was assessed. The calculated limit of contamination values for PYR (4.99 microg/cm2) and SUL (19.14 microg/cm2) were not exceeded during four consecutive equipment cleaning trials. This confirms that the desired level of cleanliness is achieved with the current cleaning procedures, which are consequently validated.