Desarrollo y validación de una metodología análitica por cromatografía gaseosa para la determinación de alcoholes totales en cera de abejas

Abstract

A gas-chrornatographic analytical method using filled column and argon as carrier gas, was developed and validated for deterrnining the total ali­phatic alcohols content from beeswax. The method was based on the extraction with 1,2-dichloroethane of the insaponified material from beeswax, at a tem­perature of 85 ºC. The product obtained was analysed by gas chromatography, using 1-eicosanol as interna! Standard and N-methyl,N-trimethylsyliltri­fluoroacetamide (MSTFA) as derivatizing reagent. A good linearity was found over a range from 80 to 120 % of nominal mass, according to the values of the correlation coefficient (0.992 3), the relative standard deviation of the response factors (1.43 %), and the Y intercept for p = 0.05. The repeatability and repro­ducibility val u es, 1.46 and 2.07 % respectively, gave the precision. The accuracy of the method (as recovei-y) R = 100.4 %, was checked to 100 % value with the Student t test. In the ruggedness study were evaluated the influence of small operational changes on: the quantitative determination, the resolution between C and C₃₀, and the relative retention time of C₃₀. It was shown that the resolution between C₂₈ and C₃₀ alcohols was affected when the final temperature ofthe oven was changed. The method can be used as a suitable procedure for routine measurements of the total alcohol content in beeswax.