Optimization of the Extraction of the Volatile Fraction from Honey Samples by SPME-GC-MS, Experimental Design, and Multivariate Target Functions

Abstract

Head space (HS) solid phase microextraction (SPME) followed by gas chromatography with mass spectrometry detection (GC-MS) is the most widespread technique to study the volatile profile of honey samples. In this paper, the experimental SPME conditions were optimized by a multivariate strategy. Both sensitivity and repeatability were optimized by experimental design techniques considering three factors: extraction temperature (from 50 ∘ C to 70 ∘ C), time of exposition of the fiber (from 20 min to 60 min), and amount of salt added (from 0 to 27.50%). Each experiment was evaluated by Principal Component Analysis (PCA) that allows to take into consideration all the analytes at the same time, preserving the information about their different characteristics. Optimal extraction conditions were identified independently for signal intensity (extraction temperature: 70 ∘ C; extraction time: 60 min; salt percentage: 27.50% w/w) and repeatability (extraction temperature: 50 ∘ C; extraction time: 60 min; salt percentage: 27.50% w/w) and a final global compromise (extraction temperature: 70 ∘ C; extraction time: 60 min; salt percentage: 27.50% w/w) was also reached. Considerations about the choice of the best internal standards were also drawn. The whole optimized procedure was than applied to the analysis of a multiflower honey sample and more than 100 compounds were identified.

Quantification of Volatile Compounds in Wines by HS-SPME-GC/MS: Critical Issues and Use of Multivariate Statistics in Method Optimization

“…Carrillo et al [38] employed a full factorial design (2 4 ) to establish the relative influence of four factors (type of fiber, temperature, pre-incubation time and sodium chloride addition) and their interactions on the chromatographic responses of extracted compounds in order to develop a method for the determination of oak-derived volatile compounds in wine. Robotti et al [39] used an experimental design for the optimization of the SPME procedure according to both the maximum signal intensity and repeatability. In a study on Maresco sparkling wine volatiles, Tufariello et al [21] focused on the equilibration of parameters and extraction times through a full two-factor three-level design with the purpose of optimizing the overall time of analysis and eventually finding an interaction factor between the two parameters affecting the analytical response.…”

Volatiles Analysis of Honey by Gas Chromatography-Mass Spectrometry (GC-MS) : Comparison of SPME Volatiles Extraction Methods

“…Without the addition of salt, volatile and less polar compounds can be extracted with SPME from honey samples. In SPME, the amount of sample used during extraction is very important to provide the highest signal intensity while avoiding saturation effects occurring on the fiber (Robotti et al, 2017). An average number of peaks representing volatiles profiles of without salt addition of chestnut honey, acacia and jujube extracted by the SPME followed by GC-MS analysis were 91, 66 and 124, respectively.…”

Carbonized Aramid Fiber as the Adsorbent for In-Tube Solid-Phase Microextraction to Detect Estrogens in Water Samples

“…Solid-phase microextraction (SPME) was firstly introduced by Arthur and Pawliszyn in the early 1990s [10]. SPME is a simple and convenient sample preparation technique that has enabled automation, miniaturization, and high-throughput performance [11][12][13][14][15][16][17][18]. In-tube SPME is a novel SPME technique that is easy to operate, solvent free, and cost effective [19][20][21][22].…”