Multivariate optimization of dual-sorbent dynamic headspace extraction of volatiles in wine analysis

摘要

The main critical point of newly developed miniaturized sample preparation techniques is a limited extraction capacity. Dynamic headspace extraction offers increased volume of sorbent which is commonly used in environmental analysis. Application of two sorbents (Carbopack B/Carbopack X and Tenax (R) TA) at different extraction temperatures allows enhancing a range of volatile organic compounds available for analysis. Such approach was applied in our research for quantification of volatile organic compounds in botrytized wines with gas chromatography. The central composite design was included to analysis simultaneous effects of incubation time, incubation temperature, purge volume and purge flow. In attempt to properly assess results, the data evaluation involved Pareto charts, surface response methodology and principal component analysis. Multivariate experimental design revealed statistical significance of purge volume and quadratic terms of incubation time and temperature, for response of volatiles. The quantification method with 0.2-2.0 mu g/L LOD and 0.5-5.0 mu g/L LOQ values, was developed under simultaneously optimized experimental conditions such as a 54 degrees C incubation temperature, a 20.18 min incubation time, a 344.3 mL purge volume and a 16.0 mL/min purge flow. The increased levels of linalool oxide, ethyl phenylacetate, gamma-hexalactone and alpha-terpineol were observed in the samples, that correlated with botrytized wine technology.