Desarrollo y validación de un método analítico para la deterninación de disolventes residuales por Espacio de Cabeza Estático-Cromatografía Gaseosa Capilar en policosanol

Authors

  • Bárbara Luna Saucedo Luna Saucedo Centro Nacional de Investigaciones Científicas
  • Luis Gonzalez Bueno Centro Nacional de Investigaciones Científicas
  • Esperanza Rodríguez Centro Nacional de Investigaciones Científicas
  • Tamara Bello Centro Nacional de Investigaciones Científicas
  • Bárbara Acosta Centro Nacional de Investigaciones Científicas
  • Javier Mosquera Sierra Centro Nacional de Investigaciones Científicas
  • Lisbet Benavides Centro Nacional de Investigaciones Científicas
  • Odila Quintana Centro Nacional de Investigaciones Científicas

Abstract

In the process of policosanol obtainment the solvents n-hexane and acetone are used and they are eliminated later on in the corresponding drying stages. The objective of this work was to develop and to validate an analytical method that allowed the determination of residuals of solvents in policosanol lots using the technique of HeadSpace Static - Gas Chromatography Capillary. The parameters of operation of the gas chromatograph it as well as those of the analysis for headspace, were optimized: balance temperature among the phases: 30 ºC; temperature of the transfer line: 150 ºC; temperature of the commutation valve: 120 ºC; time of balance among the phases: 10 min; time of injection: 2 s and flow of haulage gas (argon): 5 mL/min. The validation criteria were the following: linearity, proportionality, accuracy, sensibility and precision in repeatability and reproducibility conditions and the limits of detection. In all cases acceptance criteria were the same as the Catalan Section of Standards of Good Manufacture and Control of Quality (Validation of Analytical Methods). In the linearity study the coefficients of variation of the response response factors were lower than 5 % and acceptable values for the variance of the total experimental error and the deviation of standard of the slope, which denotes a good linearity. In the proportionality it was proven that the system doesnt present any bias.

Published

2022-05-25

How to Cite

Luna Saucedo, B. L. S., Gonzalez Bueno, L. ., Rodríguez, E. ., Bello, T. ., Acosta, B. ., Mosquera Sierra, J. ., Benavides, L. ., & Quintana, O. . (2022). Desarrollo y validación de un método analítico para la deterninación de disolventes residuales por Espacio de Cabeza Estático-Cromatografía Gaseosa Capilar en policosanol. NATIONAL CENTER FOR SCIENTIFIC RESEARCH (CENIC) CHEMICAL SCIENCES JOURNAL, 36(3), 143-147. Retrieved from https://revista.cnic.cu/index.php/RevQuim/article/view/1539

Issue

Section

Research articles