Optimization of SPME-Arrow-GC/MS Method for Determination of Free and Bound Volatile Organic Compounds from Grape Skins

Abstract

(1) Background: Solid phase microextraction (SPME)-Arrow is a new extraction technology recently employed in the analysis of volatiles in food materials. Grape volatile organic compounds (VOC) have a crucial role in the winemaking industry due to their sensory characteristics of wine.; (2) Methods: Box–Behnken experimental design and response surface methodology were used to optimise SPME-Arrow conditions (extraction temperature, incubation time, exposure time, desorption time). Analyzed VOCs were free VOCs directly from grape skins and bound VOCs released from grape skins by acid hydrolysis.; (3) Results: The most significant factors were extraction temperature and exposure time for both free and bound VOCs. For both factors, an increase in their values positively affected the extraction efficiency for almost all classes of VOCs. For free VOCs, the optimum extraction conditions are: extraction temperature 60 °C, incubation time 20 min, exposure time 49 min, and desorption time 7 min, while for the bound VOCs are: extraction temperature 60 °C, incubation time 20 min, exposure time 60 min, desorption time 7 min.; (4) Conclusions: Application of the optimized method provides a powerful tool in the analysis of major classes of volatile organic compounds from grape skins, which can be applied to a large number of samples.

Improved Analytical Method for Determination of Furan and Its Derivatives in Commercial Foods by HS-SPME Arrow Combined with Gas Chromatography–Tandem Mass Spectrometry

“…13,14 However, the traditional SPME fiber has several drawbacks of extracting a lesser number of volatile compounds, limited mechanical robustness, poor physical durability, and low reproducibility. 24 More recently, a new prototype SPME Arrow technique is emerging as a promising extraction method, which combines the advantages of both SPME and SBSE techniques, resulting in high sensitivity and reliability in determining furan compounds in food. 13,14,24 More importantly, the HS-SPME Arrow method uses a large amount of sorbent to enhance the sensitivity and offers less fragility than the traditional SPME fibers.…”

“…In the last few years, various headspace techniques such as dynamic HS (DHS), SPME, and stir-bar sorptive extraction (SBSE) microextraction have been widely used in conjugation with gas chromatography . Among these HS methods, SPME is the most widely used for extraction of volatile compounds as it offers a fully automated approach at a lower cost. , However, the traditional SPME fiber has several drawbacks of extracting a lesser number of volatile compounds, limited mechanical robustness, poor physical durability, and low reproducibility . More recently, a new prototype SPME Arrow technique is emerging as a promising extraction method, which combines the advantages of both SPME and SBSE techniques, resulting in high sensitivity and reliability in determining furan compounds in food. ,, More importantly, the HS-SPME Arrow method uses a large amount of sorbent to enhance the sensitivity and offers less fragility than the traditional SPME fibers. , Therefore, by employing HS-SPME Arrow extraction with CAR/PDMS cellulose in this study with optimized extraction conditions of sample weight at 1–5 g, saturated sodium chloride volume at 5–9 mL, stirring speed at 250 rpm, equilibration time at 10–15 min, and extraction temperature at 30 °C, furan and its 10 derivatives could be analyzed by GC–MS/MS within 10 min.…”

“…Among these HS methods, SPME is the most widely used for extraction of volatile compounds as it offers a fully automated approach at a lower cost. , However, the traditional SPME fiber has several drawbacks of extracting a lesser number of volatile compounds, limited mechanical robustness, poor physical durability, and low reproducibility . More recently, a new prototype SPME Arrow technique is emerging as a promising extraction method, which combines the advantages of both SPME and SBSE techniques, resulting in high sensitivity and reliability in determining furan compounds in food. ,, More importantly, the HS-SPME Arrow method uses a large amount of sorbent to enhance the sensitivity and offers less fragility than the traditional SPME fibers. , Therefore, by employing HS-SPME Arrow extraction with CAR/PDMS cellulose in this study with optimized extraction conditions of sample weight at 1–5 g, saturated sodium chloride volume at 5–9 mL, stirring speed at 250 rpm, equilibration time at 10–15 min, and extraction temperature at 30 °C, furan and its 10 derivatives could be analyzed by GC–MS/MS within 10 min.…”

Croatian Native Grapevine Varieties’ VOCs Responses upon Plasmopara viticola Inoculation

“…During the early stages of infection, the susceptible cultivar undergoes the following changes: at 24 hpi, the zoospores germinate and the germ tube penetrates the substomatal cavity; at 48 hpi, the P. viticola hyphae are observed in the intercellular spaces; at 96 hpi, the sporangiophores begin to develop from the stomata [ 37 ]. A novel SPME-Arrow GC/MS technique proved to be efficient for this kind of analysis by processing a large number of samples and providing a whole range of VOCs [ 30 ].…”

“…The research was performed using Solid Phase Microextraction (SPME)–Arrow Gas Chromatography–Mass Spectrometry (GC–MS). Similar methods have been used previously [ 8 , 11 , 14 , 15 ], but this one has proven to be particularly effective for the detection of VOCs [ 30 ]. Defining the differences between the metabolomic profiles of susceptible and resistant grapevines and detecting the resistance–related metabolites could broaden and introduce new concepts in plant protection strategies.…”