ABSTRACT:
Residual solvents are one of the different impurities to be controlled in active pharmaceutical ingredients APIs and pharmaceutical products. The purpose of this research is to determine the residual solvents present in some statins. A selective Gas chromatography) with headspace and Mass Spectrometer detectors (HS-GC-MS) has been developed and validated according to. different aspect of validation has been achieved to prove the method reliability, according to ICH guideline The methods has been found to be simple, sensitive, rugged, reliable and reproducible for the quantitation of n-hexane and ethanol widely used during synthesizing of raw materials (atorvastatin and rosuvastatin) or formulating into dosage form. The limit of detection was calculated to be 2.53 ppm and 1.63 ppm per sample for ethanol and n-hexane, respectively. Limit of quantification was 7.59 ppm ethanol, LOQ= 4.89 ppm for n-Hexane. Correlation factor was 0.999 for both ethanol and n-hexane. The percentage recovery was calculated and the value was 99.29 % and 96.01% for ethanol and n- hexane, respectively. The total run is 16 minutes. In addition to retention time, NIST 17 Mass spectral library used to confirm and interpretation of the results obtained. N-hexane (class 2) and ethanol (class 3) found to be at high rejected levels in some atorvastatin and rosuvastatin raw materials and some brands of film coated tablets (10 mg). The method could detect other solvents (toluene, acetone, formic acid, cyclohexane) presented in APIs and their film coated tablets but it hasn’t been validated for these solvents.