GC-MS 84.22% % Aroma components analysis in blackcurrant fruit and fruit wine by GC-MS

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2014 33 3 265 141 GC-MS 1 1 * 2 2 1. 730070 2. 100029 - HS-SPME - GC-MS 1399 50 84.22% 2- -3- -2-4- -1-48 92.65% 3- -1- - - TS207.3 doi 10.3969/j.issn.0254-5071.2014.03.034 A 0254-50712014 03-0141-06 Aroma components analysis in blackcurrant fruit and fruit wine by GC-MS JIA Qingqing 1, SHAO Weiping 1 *, XIN Xiulan 2, CHEN Liang 2 (1.College of Food Science and Engineering, Gansu Agricultural University, Lanzhou 730070, China; 2.College of Bioengineering, Beijing Polytechnic, Beijing 100029, China) Abstract: Aromatic composition and content in blackcurrant fruit and blackcurrant fruit wine fermented with fruit wine yeast 1399 were identified by HS-SPME and GC-MS. The change of aroma components in black currant fruit and the fruit wine was compared. 50 components were identified in the black currant fruit, accounting for 84.22% of the peak area. The main aroma components in fruit were 2-methyl-3-butene-2-alcohol, 4-methyl-1- amyl alcohol, ethyl caprylate, ethyl caprate, amylene normal, n-octanal, nonanal, hexanal, pentanal and so on. 48 components were identified in fruit wine, accounting for 92.65% of the peak area. The main aroma compounds in fruit wine were benzene ethanol, 3-methyl-1-butanol, ethyl acetate, ethyl caprylate, ethyl caproate, ethyl caprate, phenethyl acetate, benzeneacetaldehyde, and so on. Key words: blackcurrant fruit; HS-SPME; GC-MS; aroma components Ribes nigrum L. [1] 1 [2] 1.1 [3] 1399 3 000U/g [4] 1.2 - headspace solid phase micro-extraction HZ200LB SPX-250 TM3H HS-SPME - gas chromatographymass spectrometrygc-ms PHS-3C 2014-01-06 201103037 PHR201107151 - - PXM2013_014306_000113 PXM2013_014306_000056 1988- * 1969-

142 2014 Vol.33 No.3 Serial No.265 China Brewing Analysis and Examination AR2140-40 5min 5 /min 250 1min 7890A 5975 250 He99.999% 1.0mL/min Agilent 50/30μM DVB/CAR/ 1399 1399 2.1 0.55% 1 GC-MS 45 2h SO 2 1 GC-MS 40mg/L NIST08.L ph3.3 20 Bx 3 5% 28 8d 20 22d 1.3.2 25mL 50mL 0.3g/mL NaCl 40 40min 5min 5g 5g NaCl [6] 1.3.3 - GC-MS - [7] DB-5MS30m 0.25mm 0.25μm 250 MS 150 240 PDMS electron ionization EI 35~625m/z 1.3 70ev [5] 1.3.1 national institute of standards and technology NIST 08.L - 50 3 1min 5 /min 280 10min 2 1 GC-MS Fig. 1 GC-MS total ion current chromatograms of aroma components in blackcurrant fruit 1 GC-MS Table 1 GC-MS analysis results of aroma components in black currant fruit /% 1 ethanol 2.50 2 2- -3- -2-2-methyl-3-butene-2-ol 7.25 3 1-1-pentanol 2.02 4 4- -1-4-methyl-1-pentanol 5.58 5 4-4-methyl-1-1-methylethyl - 3-cyclohexen-1-ol 1.79 6 1- -4-1- -1- - -2-7 2 6- -1 4-8 E -2-1-methyl-4-1-acetoxy-1-methylethyl -cyclohex-2-enol 0.22 2 6-bis1 1-dimethylethyl - 1 4-benzenediol 0.47 E -2-heptenal 1.07 9 octanal 1.33 10-2- E -2-octenal 0.61 11 12 13 3 5- -4- nonanal decanal 3 5-di-tert-butyl-4-hydroxybenzaldehyde 3.86 0.47 0.38

2014 33 3 265 143 /% 14 pentanal 2.44 15 hexanal 1.94 16 2- -3-2-methyl-3-phenyl- propanal 0.23 17 ethyl caproate 1.10 18 ethyl caprylate 1.97 19 L-bornyl acetate 0.79 20 hexyl isobutyrate 0.30 21 ethyl caprate 1.49 22 diisobutyl succinate 0.36 23-1- methyl-butanedioic acid-bis1-methylpropylester 0.25 24 - phthalic acid-isobutyl octadecyl ester 0.12 25 dibutyl phthalate 0.23 26 3- -4-3-methyl-4-nonanone 9.08 27 3- -3 5- -4-28 6 10- -5 9- -2-3-methyl-3 5-cyanoethyl tetrahydro-4-thiopyranone 0.24 6 10-dimethyl-5 9-undecadien-2-one 0.20 29 1S 3S - -4-1S 3S 6R -- -4-carene 0.41 30 3-3-carene 1.19 31 limonene 6.07 32 3- -1-1-ethenyl-3-ethyl-benzene 0.57 33 2 4-34 4- -1-1- - 1-methyl-4-1-methylethenyl -benzene 1.59 4-methyl-1-1-methylethenyl - cyclohexene 0.56 35 benzocycloheptatriene 0.25 36 2 2-37 2 3- -4 4-2 2-bishydroxyphenyl propane 0.30 2 3-epoxy-4 4-dimethylpentane 2.24 38 2- sec-butylamine 5.28 39 selinane 0.76 40 2 6-2 6-bis1 1-dimethylethyl -4-methylphenol; 2.55 41 guanidineacetic acid 0.26 42 N- -1 3-43 E -3- -O- N-methyl-1 3-propanediamine 4.50 E -3-pyridinecarboxaldehyde-O-acetyloxime 3.49 44 2-2-methyl-piperazine 0.71 45 3 5- flamenol 1.04 46 ethyl vinyl ether 1.31 47 [3.2.2]-3-3-azabicyclo[3.2.2]nonane 0.32 48 2 6-49 2 5-50 3-4- - 5- -2-2 - 2 6-di-tert-butyl-p-benzoquinone 1.57 2 5-dibutyl-thiophene 3-4-methoxyphenyl -5-ethyl-2-1 2 4 -oxadiazoline 0.43 0.53 1 50 9 12.33% 3 9.52% 9 84.66% 7 19.83% 6.61% 10 19.22%

144 2014 Vol.33 No.3 Serial No.265 China Brewing Analysis and Examination 11 17.15% 3- -4-9.08% 2- -3- -2-7.25% 6.07% 4- -1-5.58% 2-5.25% N- -1 3-4.5% 3.86% 2.2 2 GC-MS 2 GC-MS 2 NIST 08.L GC-MS Fig. 2 GC-MS total ion current chromatograms of aroma components in black currant wine 2 GC-MS Table 2 GC-MS analysis results of aroma components in black currant wine /% 1 3- -1-3-methyl-1-butanol 1.86 2.+/-. - 3 3 7- -1 6- -3-.+/-. -2-methyl-butanol 1.04 3 7-dimethyl-1 6-octadien-3-ol 0.63 4 phenylethyl alcohol 19.96 5 cis-verbenol 0.34 6 4- -1-1- -3- -1-4-methyl-1-1-methylethyl -3-cyclohexen-1-ol 2.03 7 2-4- -3- -2-8 1- -4-1- -1-2-4-methyl-3-cyclohexene -2-propanol 1.80 1-methyl-4-1-methylethylidene -cyclohexanol 0.89 9 benzeneacetaldehyde 0.49 10 nonanal 0.15 11 [b] -2- benzofuran-2-carboxaldehyde 0.30 12 ethyl acetate 15.15 13 ethyl propionate 1.90 14 propyl isothiocyanate 0.57 15 isoamyl acetate 1.04 16 6-6-heptenoic acid ethyl ester 0.67 17 ethyl caproate 4.53 18 2- ethyl-2-furoate 0.63 19 2-2-ethyl acetoacetate 0.40 20 diethyl succinate 1.56 21 ethyl caprylate 19.03 22 ethyl phenylacetate 0.80 23 phenethyl acetate 3.42 24 methyl caprate 0.37 25 gamma-nonanolactone 0.23 26 2- -3- -2 4 4-2-methyl-propanoicacid-3-hudroxy-2 4 4-trimethylpentyl ester 0.11 27 ethyl caprate 4.22 28 3- octanoic acid-3-methylbutyl ester 0.13 29 ethyl laurate 0.21

2014 33 3 265 145 /% 30 9- ethyl-9-decenoate 0.73 31 tritetracontane 0.25 32 tetradecane 0.10 33 tridecane 0.18 34 methyl-thiirane 0.16 35 allyl fluoride 0.04 36 2- -1-2-methyl-1-allyl benzene 0.08 37 2 4-1-methyl-4-1-methylethenyl -benzene 2.57 38 3-1- 3-1-methylethyl -cyclohexene 0.31 39 [s-r S ]-β-4- -3-40 2 6- -2 6- [s-r* S* ]-β-4- dimethyl-3-cyclohexene-1-ethanol 0.40 6-dimethyl-2 6-octadiene 0.14 41 octanoic acid 1.38 42 2- -4- eugenol 0.29 43 pentamethyl-benzene 0.12 44 1-methyl-2-1-methylethyl -benzene 0.47 45 acetophenone 0.45 46 2-2-methyl-naphthalene 0.25 47 48 N-2-2 4- N-2-phenylethyl -acetamide 2 4-bis1 1-dimethylethyl -phenol 0.07 0.20 2 49 2.3.1 92.98% 8 19.83% 2- -3-28.55% 19 55.7% 3-2- 4- -1-7.25%5.58% 0.94% 10 4.23% 82- -3- -2-4- -1-3.56% 19.96% 28.55% 15.15% 19.03% 4.53% 19.96% 4.22% 3.42% 2 4- [11] 2.57% 4- -1-1- -3- -1-2.03% - 3- -1-1.86% [12] 4-2.3 3- -1-2.3.2 6.61% [8-9] 1.97%1.49% 55.7% 15.15% 19.03%4.22% PAILLARD N N M [10] 78%~ 92% 6%~16% [13] 1.97% 19.03%

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