Method Optimization Study on Isolation of Volatile Compounds by Headspace Solid-Phase Microextraction (HS-SPME) from Custard Apple (Annona squamosa L.) Pulp.

Abstract
Aroma is an important quality parameter, which can help in delaying degradative processes and hence understanding the volatile compounds that are part of an aroma is extremely important. Thus, the aim of this study was to isolate the volatile compounds present in custard apple (Annona squamosa L.) pulp by solid-phase microextraction (SPME) technique using 3 different fibers (DVB/CAR/PDMS, PDMS and PDMS/DVB). An experimental design was set up to evaluate the best extraction conditions wherein the variables were extraction temperature (minimum 28°C, maximum 62°C), ionic strength (minimum 0, maximum 30.0%) and sample concentration (min 1, max 99.0%). The separation of volatiles was achieved in chromatographic columns of different polarity (polar and non-polar) while identification of volatile compounds was performed by high resolution gas chromatography system coupled with mass spectrometry. The results obtained using 3 different fibers revealed the isolation of 71 compounds with fiber DVB/CAR/PDMS, while only 30 and 21 compounds were isolated using fibers PDMS/DVB and PDMS, respectively. The major classes of compounds identified were terpenes, esters, alcohols and aldehydes. Optimum conditions for obtaining higher number of volatiles for non-polar column were 45°C for extraction temperature, 15% of sodium chloride and 50% of pulp amount which resulted in isolation of a maximum of 78 peaks.

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