Rapid verification of identity and content of drug formulations using mid-infrared spectroscopy.

A general method for the rapid verification of both identity and content of complete solid drug formulations has been devised. Infrared spectra for the samples were recorded using the diffuse reflectance technique, and specially written software was employed to identify the type of formulation and level of active ingredient. This software was devised to ensure reliable use when applied by those with minimal operator skills. Three differing drug tablet formulations containing simvastatin, enalapril maleate and lovastatin, as well as a capsule formulation containing finastride were studied. Adequate precision was obtained to reliably verify drug dosage levels. Near-infrared (NIR) and mid-infrared (MIR) spectrometers were evaluated for use with the method. The MIR instrument allowed sufficient resolution and spectral/structural selectivity to reliably verify correctness of either of two near derivative drugs necessarily present in the same clinical study. Drug tablet and capsule dosage levels tested ranged from 0.2 to 40 mg of drug. Approximately 1% (w/w) of the drug in the formulation was the minimum amount determined. Parameters affecting method ruggedness in routine use were optimized. Experimental addition of an extraneous material to a simvastatin formulation was easily detected and flagged by the routine test procedure. Subsequent data retrieval and searching against spectral libraries was used to demonstrate identification of the additive.