Element Determination in Pharmaceuticals Using Direct Solid Analysis- Electrothermal Vaporization Inductively Coupled Plasma Optical Emission Spectrometry

A solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry (ETV-ICP OES) method for determination of As, Cd, Cr, Cu, Mn, Mo, Ni, Pb, Pd, Pt, Rh, Ru and V in pharmaceuticals is proposed. Tricyclic pharmaceuticals were directly analyzed due to their difficult decomposition with acids. Pyrolysis and vaporization temperature, sample mass, and reaction gas (Freon) flow rate were evaluated. The effect of organic and inorganic compounds was evaluated for matrix matching. The limits of detection ranged from 0.04 µg g−1 (Cu) to 107 µg g−1 (As) and the relative standard deviation was lower than 10%. The investigated elements were not detected in the analyzed samples with the exception of Cr in cyclobenzaprine hydrochloride. Since there was no certified reference materials available for metals and metalloids in pharmaceuticals, the accuracy of the method was evaluated by an independent technique and by analyte recovery. Inductively coupled plasma mass spectrometry was employed for analyte determination after sample decomposition by microwave induced combustion. The agreement of the results found by both techniques was better than 87% and analyte recoveries ranged from 91 to 103%.