Analytical Method Development to Determine Residual Solvents in Esomeprazole by Gas Chromatography (GC/FID) with Head Space

Ojas Joshi, Parag Gide
2017 10, Issue:1 Citation: Ojas Joshi et al. Ijppr.Human   unpublished
Residual solvents in pharmaceuticals are termed as organic Volatile Impurities. These are the chemicals that are used in the manufacture of drug substance or excipients or use in the preparation of final formulation. Analysis of organic volatile impurities is of key importance for Active Pharmaceutical Ingredients (API). Most of the available methods use liquid chromatography which could be expensive and time consuming. Hence, an analytical method for the quantification of residual solvents in
more » ... sidual solvents in Esomeprazole was established using a headspace gas chromatography (HSGC) coupled with a flame ionization detector (FID). Methanol, Acetone, Isopropyl alcohol, Methylene dichloride, Toluene as residual solvents were determined in Esomeprazole. Analysis was performed by headspace GC/FID method on Agilent GC 7820A system. Nitrogen was used as a carrier gas with constant flow rate of 4.2 mL/min and the separation of residual solvents was achieved on DB-624 column. The thermostat temperature was 105ºC for 30 minutes for each vial and after the equilibration, the vials were pressurized and injected on GC column. The % RSD for six injections obtained in acceptance criteria. The percentage recovery ranges obtained from 92.49 and 106.69%. The correlation coefficient R2 obtained greater than 0.99. The method parameters were validated included specificity, limit of detection and quantification, accuracy, linearity, precision, and robustness. A new, simple, specific, accurate and precise method was validated according to the International Conference on Harmonization (ICH) guidelines.