Elaboración y propuesta de validación de un método analítico para la determinación de límites de etilenglicol y dietilenglicol en sorbitol solución 70% por cromatografía de gases en la industria farmacéutica Anglopharma S.A.

Abstract

The purpose of this work is to describe the implementation and validation proposal of a methodology for the determination of ethylene glycol and diethylene glycol limits in a 70% sorbitol solution. A validation protocol was developed proposing a methodology by gas chromatography with flame ionization detector (FID), where a mixture of hydrogen, nitrogen and makeup gas (35:40:350) was used as carrier gas. The temperature ramp starts at 70 ºC, with a ramp at a rate of 50 ºC/min until 260 ºC was reached. A 0.32 mm x 30 m fused silica capillary column with a 1.8 µm film of G46 (624) phase was used. The column flow rate was set at 3.0 mL/min, the injector and detector temperatures were set at 300 ºC. The implemented methodology was established taking as a reference the monograph cited in the American pharmacopoeia USP 43-NF 38 for the evaluation of the diethylene glycol limit evaluation of the limit of diethylene glycol (DEG) and ethylene glycol (EG) in sorbitol solution. solution. Given the clarification that, being a limit analysis, according to the regulatory body in Colombia (INVIMA) the specificity and detection limit parameters must be analyzed, however, this protocol establishes the performance parameters and other tests to be evaluated for the development of the validation proposal. As main acceptance criteria and parameters were evaluated: system suitability, accuracy, specificity and robustness. Of which, the robustness did not comply with the established parameters, nor was it possible to determine the inter the determination of the intermediate precision and linearity of the method, due to factors such as the determination of the intermediate precision and linearity of the method, due to factors such as equipment availability, lack of time, space and supplies, space and supplies. The specificity study showed that there was no interference in the determination of (EG) and (DE). (EG) and (DEG) determination once the samples were subjected to stress conditions. stress conditions. High recovery percentages were obtained in the accuracy study (99.8 to 100.4%) for ethylene glycol, and (99.7 to 100.1%) for diethylene glycol. for diethylene glycol.