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J Chromatogr A

Title:		"Solid-phase microextraction-gas chromatography and ultra-high performance liquid chromatography applied to the characterization of lemon wax, a waste product from citrus industry"
Author(s):		Costa R; Albergamo A; Arrigo S; Gentile F; Dugo G;
Address:		"Dipartimento di Scienze Biomediche, Odontoiatriche e delle Immagini Morfologiche e Funzionali (BIOMORF), Universita di Messina, Viale Annunziata, 98168 Messina, Italy. Electronic address: costar@unime.it. Dipartimento di Scienze Biomediche, Odontoiatriche e delle Immagini Morfologiche e Funzionali (BIOMORF), Universita di Messina, Viale Annunziata, 98168 Messina, Italy; Science4Life s.r.l., a spin-off of the University of Messina, Polo Annunziata, ex Facolta di Medicina Veterinaria, Messina, Italy. Consiglio per la Ricerca in agricoltura e l'analisi dell'Economia Agraria - Olivicultura, Frutticultura Agrumicultura (CREA-OFA), Corso Savoia 190, 95024 Acireale, Italy"
Journal Title:		J Chromatogr A
Year:		2019
Volume:		20190625
Issue:
Page Number:		262 - 268
DOI:		10.1016/j.chroma.2019.06.049
ISSN/ISBN:		1873-3778 (Electronic) 0021-9673 (Linking)
Abstract:		"A novel application of SPME-GC and UHPLC is presented for the elucidation of an unexplored citrus by-product, namely lemon wax. In view of the current environmental protection strategies, directed toward reuse and/or recovery of waste products, this study aimed to evaluate a possible utilization of a discarded fraction from citrus fruits processing. Headspace SPME coupled with GC-MS and GC-FID allowed determining a residual amount (162.25 mg?ª+kg(-1)) of lemon volatiles, by means of accurate calibration of 38 terpenoids through linear regression analysis (R(2)?ª+=?ª+0.99). SPME method development, was supported by statistical analysis, consisting of experimental design and multisample comparison, where parameters such as type of coating, temperature and time of fiber exposure, were manipulated towards optimization. The optimized method was validated, showing limits of quantification (LOQ) and of detection (LOD) in the ranges 0.24 - 2.65 ng?ª+g(-1) and 0.11 - 0.87 ng?ª+g(-1), respectively; recoveries ranged from 84.9% to 111.5%. After optimization and validation, the UHPLC-PDA method revealed the presence in lemon wax samples of six coumarins, the most abundant being bergamottin (964?ª+mg?ª+kg(-1)), followed, in decreasing amount, by citropten, 8-geranyloxypsoralen, biacangelicin, oxypeucedanin, 5-geranyloxy-7-methoxycoumarin; each analyte was calibrated by external standard methodology. Sensitivity (LOD, 31 - 112 ng?ª+g(-1); LOQ, 102-370 ng?na?ª+g(-1)), accuracy (recovery, 81-94%), and precision (Retention time RSD, 0.03 - 0.09%; peak area RSD, 1.03-2.92%), were also measured"
Keywords:		"Calibration Chromatography, High Pressure Liquid/*methods Citrus/*chemistry Gas Chromatography-Mass Spectrometry/*methods Industrial Waste/*analysis Multivariate Analysis Reproducibility of Results Solid Phase Microextraction/*methods Volatile Organic Com;"
Notes:		"MedlineCosta, Rosaria Albergamo, Ambrogina Arrigo, Sara Gentile, Fausto Dugo, Giacomo eng Netherlands 2019/07/02 J Chromatogr A. 2019 Oct 11; 1603:262-268. doi: 10.1016/j.chroma.2019.06.049. Epub 2019 Jun 25"