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. 2022 Aug 4;27(15):4955.
doi: 10.3390/molecules27154955.

Chemical Approach to the Optimization of Conditions Using HS-SPME/GC-MS for Characterization of Volatile Compounds in Eugenia brasiliensis Fruit

Ana Luiza Coeli Cruz Ramos  1 , Laiza Andrade Nogueira  2 , Mauro Ramalho Silva  3 , Ana Carolina do Carmo Mazzinghy  2 , Ana Paula Xavier Mariano  1 , Tássia Nunes de Albuquerque Rodrigues  1 , Ana Cardoso Clemente Filha Ferreira de Paula  4 , Angelita Cristine de Melo  2 , Rodinei Augusti  5 , Raquel Linhares Bello de Araújo  1 , Inayara Cristina Alves Lacerda  1 , Júlio Onésio Ferreira Melo  2
Affiliations

Chemical Approach to the Optimization of Conditions Using HS-SPME/GC-MS for Characterization of Volatile Compounds in Eugenia brasiliensis Fruit

Ana Luiza Coeli Cruz Ramos et al. Molecules. .

Abstract

Grumixama (Eugenia brasiliensis Lam.) is a native fruit of the Brazilian Atlantic Forest, belonging to the Myrtaceae family, which designatesthe most significant number of species with food potential. It stands out due to its phytochemical characteristics because of the presence of polyphenols and volatile organic compounds. Volatile compounds are substances released by foods that give off an aroma and influence flavor. Solid-phase microextraction is a technique that allows for low-cost, fast, and solvent-free extraction, has an affinity for numerous analytes, and is easily coupled to gas chromatography. The objectives of this work were to evaluate the efficiency of different fibers of SPME (solid-phase microextraction) in the extraction of volatile organic compounds from grumixama pulp; optimize a method for extraction time, temperature, and sample weight; and to determine the characteristic volatile profile of this fruit. For the extraction of volatile compounds, three fibers of different polarities were used: polar polyacrylate (PA) fibers, divinylbenzene/carboxyne/polydimethylsiloxane (DVB/CAR/PDMS) semipolar fibers, and polydimethylsiloxane/divinylbenzene (PDMS/DVB). Fourteen volatile organic compounds (VOCs) were identified by DVB/CAR/PDMS, six by PA, and seven by PDMS/DVB through solid-phase microextraction in the headspace mode (SPME-HS). Considering the total number of compounds identified, regardless of the fiber used, and the optimization of the method, Eugenia brasiliensis presented sesquiterpene fractions (85.7%, 83.3%, and 85.7% of total VOCs) higher than the monoterpene fractions (14.3%, 16.7%, and 14.3%) for DVB/CAR/PDMS, PA, and PDMS/DVB, respectively in its composition. In addition, it was possible to verify that the fiber DVB/CAR/PDMS presented a better efficiency due to the larger chromatographic area observed when the grumixama pulp was subjected to conditions of 75 °C, 2.0 g, and an adsorption time of 20 min.

Keywords: SPME fibers; grumixama; sesquiterpene; volatile organic compounds.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
Chromatogram generated for grumixama fruits.
Figure 2
Figure 2
Effects of parameters: sample weight, extraction time, and extraction temperature on the extraction of volatiles using different fibers for HS-SPME-(a) DVB/CAR/PDMS, (b) PA, and (c) PDMS/DVB.
Figure 3
Figure 3
Three-dimensional response surface (RSM) graphs of the parameters time, extraction temperature, and sample weight in the extraction of volatile compounds using different fibers for HS-SPME: (a) DVB/CAR/PDMS extraction temperature vs. sample weight, (b) DVB/CAR/PDMS extraction time vs. sample weight, (c) DVB/CAR/PDMS extraction time vs. extraction temperature, (d) PA extraction temperature vs. sample weight, (e) PA extraction time vs. sample weight, (f) PA extraction time vs. extraction temperature, (g) DVB/PDMS extraction temperature vs. sample weight, (h) DVB/PDMS extraction time vs. sample weight, and (i) DVB/PDMS extraction time vs. extraction temperature.
Figure 3
Figure 3
Three-dimensional response surface (RSM) graphs of the parameters time, extraction temperature, and sample weight in the extraction of volatile compounds using different fibers for HS-SPME: (a) DVB/CAR/PDMS extraction temperature vs. sample weight, (b) DVB/CAR/PDMS extraction time vs. sample weight, (c) DVB/CAR/PDMS extraction time vs. extraction temperature, (d) PA extraction temperature vs. sample weight, (e) PA extraction time vs. sample weight, (f) PA extraction time vs. extraction temperature, (g) DVB/PDMS extraction temperature vs. sample weight, (h) DVB/PDMS extraction time vs. sample weight, and (i) DVB/PDMS extraction time vs. extraction temperature.
Figure 3
Figure 3
Three-dimensional response surface (RSM) graphs of the parameters time, extraction temperature, and sample weight in the extraction of volatile compounds using different fibers for HS-SPME: (a) DVB/CAR/PDMS extraction temperature vs. sample weight, (b) DVB/CAR/PDMS extraction time vs. sample weight, (c) DVB/CAR/PDMS extraction time vs. extraction temperature, (d) PA extraction temperature vs. sample weight, (e) PA extraction time vs. sample weight, (f) PA extraction time vs. extraction temperature, (g) DVB/PDMS extraction temperature vs. sample weight, (h) DVB/PDMS extraction time vs. sample weight, and (i) DVB/PDMS extraction time vs. extraction temperature.
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