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Optimization of Experimental Parameters and Chemometrics Approach to Identify Potential Volatile Markers in Seven Cucumis melo Varieties Using HS–SPME–GC–MS

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Volatile compounds produce the aroma of fruits such as melons (Cucumis melo) and therefore play a key role in fruit quality. Here, we optimized experimental parameters to evaluate the effect of blending time, extraction temperature and time, different fibers, sample weight, different columns, and salt on the volatile composition of melons was performed using headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC–MS). In general practice, samples are queued up for GC–MS analysis at room temperature (25 °C) for 12–24 h; during this time, the volatile concentrations in samples may vary. To address this, we examined the effect of storage at 4 and 25 °C for 0, 12, 24, 48, and 72 h on samples with and without salt added. Overall, the addition of salt to the sample enhanced the volatile concentration in the headspace and helped preserve the sample at 4 and 25 °C without any significant changes up to 72 h. Our results showed that blending the sample for 1 min, the addition of 1 mL 30% NaCl in a 1 g sample, followed by the adsorption of volatiles with 50/30 µm divinylbenzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) coated 2-cm SPME fiber, and extraction at 80 °C for 30 min were optimal for the detection of melon volatile organic compounds (VOCs). These optimized conditions were employed for the analysis of VOCs from seven melon varieties. Principal component analysis (PCA), partial least squares-discriminant analysis (PLS-DA), and variable importance on projection (VIP) analyses were performed to identify markers responsible for melon variety discrimination. A total of twenty volatile compounds with VIP > 1.4 are considered as potential markers for the separation of melon varities studied. The combination of HS–SPME–GC–MS and chemometric classification offers a valuable tool for the identification of type-specific volatile markers in melons.

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The authors are thankful to Dr. John L. Jifon (Texas A&M AgriLife Research and Extension Center, Weslaco, TX) for growing and providing the melon varieties for this study.


This study was supported by the USDA-NIFA-SCRI-2017–51181-26834 through the National Center of Excellence for Melons at the Vegetable and Fruit Improvement Center of Texas A&M University.

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Correspondence to Bhimanagouda S. Patil.

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Metrani, R., Jayaprakasha, G.K. & Patil, B.S. Optimization of Experimental Parameters and Chemometrics Approach to Identify Potential Volatile Markers in Seven Cucumis melo Varieties Using HS–SPME–GC–MS. Food Anal. Methods 15, 607–624 (2022).

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