Impurities in pharmaceutical compounds are defined as any compounds in a pharmaceutical substance other than water, which have a chemical structure that differs from the original drug substance. Impurities were classified into three categories classified organic impurities, inorganic impurities and residual solvents (RS). Residual solvents are produced during manufacturing process of the raw material or the formulation process of the pharmaceutical dosage form. Therefore, Determination of residual solvents in dosage forms is important. In this context, Rosuvastatin and Atorvastatin are long-acting synthetic compounds that are not free of residual solvents especially propanol-2 that belongs to the third category according to the International Conference on Harmonization ICH. In this study, a new headspace gas chromatographic method with mass spectrometer HS-GC-FID was developed to determine the residues of propanol-2 in raw materials and their locally marketed dosage forms. The method was validated according to ICH and all results were acceptable with a limit of detection (LOD) of 3.7 ppm. Limit of quantification LOQ was 11.1 ppm. The percentage recovery values were 98.59% for propanol-2. When RSD% values were set for peak areas, the result was 4.0195%, and the RSD values for retention times were below 2% in all samples.
Correlation factor R2 for propanol-2 was found to be 0.9988. The method could detect other solvents by comparing their retention times with retention time of single standards. In addition to retention time, NIST 17 Mass spectral library used to confirm and interpretation of the results obtained. The total run time is 16 minutes. Propanol-2 was found in the samples of rosuvastatin and atorvastatin and 10 mg film coated tablets of these substances with acceptable concentrations. The method was able to detect the presence of other solvent residues (Toluene, Acetone, Formic Acid, Cyclohexane, Tetra Butyl Methyl ether).
Homs University Journal.
2018.