Multivariate optimization of headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry
José Manuel Muñoz-Redondo1, María José Ruiz-Moreno1, Belén Puertas2
1Department of Food Science and Health, Andalusian Institute of Agricultural and Fisheries Research and Training (IFAPA), Alameda del Obispo, Avda. Menéndez Pidal, SN, 14004, Córdoba, Spain.
Abstract:
A headspace solid-phase microextraction coupled to gas-chromatography and mass spectrometry (HS-SPME-GC-MS) was developed and validated for the determination of 26 terpenes in sparkling wines. The use of a Box-Behnken experimental design, together with the desirability function D, allowed the extraction conditions of the method to be optimized. The optimal extraction conditions were found at a dilution ratio of 2:3, the addition of 3.5 g of NaCl, an extraction temperature of 46 °C and an extraction time of 52 min, using the DVB/CAR/PDMS fibre. Afterwards, the analytical method was successfully validated in terms of linearity, matrix effect, limit of detection and quantification, precision and accuracy. To test the developed method, 35 commercial sparkling wines from different grape varieties, geographical regions and ageing times were analysed and their terpenoid profile was monitored. The use of multivariate statistical tools made it possible to highlight differences in the samples related to the terpene profile. Finally, the most important compounds involved in the discrimination of the samples were identified by means of iterative variable selection procedures.
Related Concept Videos
Gas Chromatography–Mass Spectrometry (GC–MS)
A gas chromatograph consists of a long, narrow capillary column with a polysiloxane coating on the inner wall....
Optimizing Chromatographic Separations
Band broadening refers to spreading solute bands as they travel through the column. This broadening can impact resolution. Plate height (H) represents the length required for one theoretical plate. A lower plate height corresponds to...
Gas Chromatography: Introduction
In GC, a sample is vaporized and mixed with an inert carrier gas (the mobile phase), which transports it through a...
Gas Chromatography: Sample Injection Systems
Two primary injection methods are used...
Supercritical Fluid Chromatography
SFC utilizes a supercritical fluid mobile phase,...
Mass Spectrometry: Complex Analysis
GC–MS is a powerful hyphenated method commonly used in forensics and environmental...


