Journal of Food Science and Biotechnology

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1 Journal of Food Science and Biotechnology 27 No. 6 Vol. Nov : (2008) ,2, 1,2, 1,2, 3 1,2 (1., ; 2., ) : ( HS2SPM E) ( GC2MS) 3 95, 73 ; , 23 3 TIC 2 3 : ;; ;; ; :O : A Determination of Volatile Compounds in Fruit Wine by Headspace Solid Phase Microextraction ( HS2SPME) Follo wed by Gas Chromatography2Mass Spectrometry ( GC2MS) ZHAN G Ying2lu 1,2, FAN Wen2lai 1,2, J IAN G Wen2guang 1,2, XU Yan 3 1,2 (1. Key Laboratory of Industrial Biotechnology, Ministry of Education, Jiangnan University, Wuxi 21422,China ; 2. School of Biotechnology, Jiangnan University, Wuxi , China) Abstract :A rapid and simple met hod was developed for determinatio n of aro ma co mpo nent s of f ruit wine by headspace solid p hase microext ractio n ( HS2SPM E ) co upled to capillary gas chromatograp hy mass spectrometry ( GC2MS). A total of 95 volatiles were detected in t hree f ruit wines, and 73 volatile compounds were identified by GC2MS. Of these, t hese were 46, 52, and 50 volatile compounds identified in plum wine, lichee wine, and medlar wine, respectively. Furthermore, 23 compounds were existed in all fruit wines studied in this manuscript, of which, ethyl octanoate, octanoic acid, and 2phenylethyl alcohol and so on were the main volatile compounds. Key words : headspace solid p hase microextraction ( HS2SPM E) ; f ruit wine ; gas chromatograp hy2 mass spectrometry ( GC2MS) ; plum wine ; lichee wine ; medlar wine,,, 12 % ( ) [ 1 ], [2 ], : : (19682),,,. 3 : (19622),,,,,. edu. cn

2 116 27,1 mg/ L 1 g/ L,1 ng/ L,, ( HS2SPME) :, [3 ],,, [4 ] [2,4,5 ] HS2SPM E ( GC 2 MS) 3,, : ; :; : NaCl :, () ; :Sigma2Aldrich ( ) Agilent 6890 N 5975 ( GC2MS) ; :DB2Wax (30 m 0125 mm 0125 m) ; Gerstel MPS : ml,20 ml, 3 g NaCl, SPM E CAR/ DVB/ PDMS, 5 min,50 30 min GC2MS :250, :50,2 min, 3 / min 230,10 min ; He N IST05a TIC SPME SPM E, PA PDMS PDMS/ CAR CAR/ DVB/ PDMS 4, CAR/ DVB/ PDMS 3, PA,,HS2SPM E ;,,, , 50 20,30,40,60 min, 30 min [ 4 ], 30 % NaCl SPM E : CAR/ DVB/ PDM, min, 30 % NaCl 212 1, GC2MS, N IST05a 1 (a)

3 5 : 117 (b) (c) 1 ( a),( b) ( c) 2 Fig. 1 GC2MS total ionic chromatogram of volatile compounds in ( a) plum wine, ( b) lichee wine, ( c) medlar wine 1 HS2SPME GC2MS Tab. 1 The volatile compounds in three fruit wines were detected by HS2SPME and GC2MS / % RI d acids 1449 acetic acid a,b,c hexanoic acid a,b,c heptanoic acid a,b,c ND ND 2051 octanoic acid a,b,c sorbic acid a,b decanoic acid a,b,c benzenecarboxylic acid a,b,c dodecanoic acid a,b,c ND 2908 hexadecanoic acid a,b,c ND ND alcohols < 900 ethyl alcohol a,b propanol a,b,c methyl212propanol a,b

4 / % RI d butanol a,b,c ND methyl212butanol a,c ND ND methyl212butanol a,b pentanol a,c ND hexanol a,b,c (z)232hexen212ol a,b ND ND (e)232hexen212ol a,b ND ND ethyl212hexanol a,b ND nonanol a, c ND ND octanol a,b,c ND ,32 2,32butanediol a,b,c ND nonanol a,b,c ND ND benzyl alcohol a,b,c phenylethyl alcohol a,b,c esters 892 ethyl acetate a,b,c ethyl butyrate a,b,c ND ethyl 22methylbutyrate a,b,c ND ND ethyl 32methylbutyrate a,b,c methylbutyl acetate a,b,c ND ethyl hexanoate a,b,c hexyl acetate a,b ND ND ethyl heptanoate a,b,c ND ethyl 22hexenoate a,c ND ND ethyl 22hydroxypropanoate a,b ND ethyl octanoate a,b,c ,42 ethyl 2,42hexadienoate a,b ND 1603 butyrolactone a,b,c ND ND 1629 ethyl decanoate a,b,c ethyl benzoate a,b,c diethyl succinate a,b,c ethyl 92decenoate b ND ND ethyl 2phenylacetate a,b,c methyl 22hydroxybenzoate a,b phenylethyl acetate a,b,c ND ethyl benzenepropanoate a,b,c ND ND ethyl cinnamate a,b,c ethyl hexadecanoate a,b,c ND aldehydes and ketones 1073 hexanal a,b,c ND ND 1446 furfural a,b,c benzaldehyde a,b,c ND ND undecanone a,b ND ND benzenes 1245 styrene a,b ND ND terpenes and norisoprenoids

5 5 : / % RI d 1169 d2 d2limonene a,b,c ND trans2rose oxide a,b ND ND linalool a,b,c ND terpinenol a,b,c ND ND 1721 cadinene a,b ND ND 1714 naphthalene a,b,c ND citronellol a,b ND ND damascenone a,b,c ND methylnaphthalene a,b ND ND Ionone a,b ND ND ionone a,b,c ND nerolidol 2 a,b ND ND phenols 2002 phenol a,b,c isoengenol a,b ND ND ethylphenol a,b ND ND methoxy242vinylphenol a,b,c ND ND ,42 2,42bis(1,12dimethylethyl) phenol b sulfides < 900 dimethyl sulfide a,b ND ND furans furancarboxylic acid ethyl ester b ND ,52 2,52furandicarboxaldehyde a,b ND ND > ( )222 52(hydroxymethyl)222furancarboxaldehyde b ND : d : (22 ) ; a : RI ; b : 94 % ; c : ND : 1,HS2SPM E GC2MS 3 95, 73, ,1 46, , 3 9, 3 (9105 %),,, 21212,1,,, , , % ( ), , 23, 3 10, 32 3,, [6-7 ] 21214

6 [8-9 ] 11 3, 3 6, 7 4, ,,13159 %, [10 ],,, [11 ], 12,, 3 HS2SPM E,,,, 3, 73,23 3, ,42 TIC, , 3, ( References) : [ 1 ]. [ M ]. :,1991. [ 2 ] Wang L, Xu Y, Zhao G, et al. Rapid analysis of flavor volatiles in apple wine using headspace solid2phase microextraction [J ]. Journal of the Institute of Brewing,2004,110 (1) : [ 3 ] Arthur C L, Pawliszyn J. Solid2phase microextraction with thermal2desorption using fused2silica optical fibers[j ]. Ana2 lytical Chemistry,1990,62 (19) : [ 4 ] Fan W L, Qian M C. Headspace solid phase microextraction and gas chromatography2olfactometry dilution analysis of young and aged Chinese Yanghe Daqu liquors [J ]. Journal of Agricultural and Food Chemistry, 2005,53 (20) : [ 5 ],,,, [J ].,2003,22 (1) :1-7. WAN G Li2ping, XU Yan, ZHAO Guang2ao, et al. Rapid determination of aroma component s in apple wine by headspace solid2phase micro extraction ( HS2SPME) [J ]. Journal Wuxi University and Light Industry, 2003, 22 (1) :1-7. (in Chi2 nese) [ 6 ] Fan W L, Qian M C. Characterization of aroma compounds of Chinese Wuliangye and Jiannanchun liquors by aroma extract dilution analysis[j ]. Journal of Agricultural and Food Chemistry,2006,54 (7) : [ 7 ] Fan W L, Qian M C. Identification of aroma compounds in Chinese Yanghe Daqu liquor by normal phase chromatogra2 phy fractionation followed by gas chromatography olfactometry[j ]. Flavour and Fragrance Journal, 2006, 21 (2) : [ 8 ] Pena R M, Barciela J, Herrero C, et al. Optimization of solid2phase microextraction methods for GC2MS determination of terpenes in wine[j ]. Journal of the Science of Food and Agriculture,2005,85 (7) : [ 9 ] Coelho E, Rocha S M, Delgadillo I, et al. Headspace2SPM E applied to varietal volatile components evolution during Vitis vinifera L. cv. Baga ripening[j ]. Analytica Chimica Acta,2006,563 (122) : [ 10 ] Xu Y, Fan W L, Qian M C. Characterization of aroma compounds in apple cider using solvent2assisted flavor evaporation and headspace solid2phase microextraction[j ]. Journal of Agricultural and Food Chemistry, 2007, 55 (8) : [11 ] Cullere L, Escudero A, Cacho J, et al. Gas chromatography2olfactometry and chemical quantitative study of the aroma of six premium quality Spanish aged red wines[j ]. Journal of Agricultural and Food Chemistry, 2004, 52 (6) : ( :)

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