Changes in the physicochemical and volatile profiles during the winemaking of Marselan in the Eastern Foot of Helan Mountain, China

Lei Fang; Ningli Qi; Yajun Li; Tinghui Chen; Xiao Gong; Lei Fang; Ningli Qi; Yajun Li; Tinghui Chen; Xiao Gong

doi:10.48130/fia-0024-0039

Figures (6) Tables (2)

Figure 1.
2D-topographic plots of volatile organic compounds in Marselan wine at different fermentation stages.
Figure 2.
Fingerprints of volatile organic compounds in Marselan wine at different fermentation stages.
Figure 3.
PCA based on the signal intensity obtained with different fermentation stages of Marselan wine.
Figure 4.
Scores plot of OPLS-DA model of volatile components in Marselan wine at different fermentation stages.
Figure 5.
Permutation test of OPLS-DA model of volatile components in Marselan wine at different fermentation stages (n = 200).
Figure 6.
VIP plot of OPLS-DA model of volatile components in Marselan wine at different fermentation stages.

No.	Compounds	Formula	RI^*	Rt [sec]^**	Dt [RIPrel]^***	Identification approach	Concentration (μg/mL) (n = 4)
No.	Compounds	Formula	RI^*	Rt [sec]^**	Dt [RIPrel]^***	Identification approach	Stage 1	Stage 2	Stage 3	Stage 4
Aldehydes
5	Furfural	C₅H₄O₂	1513.1	941.943	1.08702	RI, DT, IS	89.10 ± 4.05^c	69.98 ± 3.22^c	352.16 ± 39.06^b	706.30 ± 58.22^a
6	Furfural dimer	C₅H₄O₂	1516.6	948.77	1.33299	RI, DT, IS	22.08 ± 0.69^b	18.68 ± 2.59^c	23.73 ± 2.69^b	53.39 ± 9.42^a
12	(E)-2-hexenal	C₆H₁₀O	1223.1	426.758	1.18076	RI, DT, IS	158.17 ± 7.26^a	47.57 ± 2.51^b	39.00 ± 2.06^c	43.52 ± 4.63^bc
17	(E)-2-pentenal	C₅H₈O	1129.2	333.392	1.1074	RI, DT, IS	23.00 ± 4.56^a	16.42 ± 1.69^c	18.82 ± 0.27^b	18.81 ± 0.55^b
19	Heptanal	C₇H₁₄O	1194.2	390.299	1.33002	RI, DT, IS	17.28 ± 2.25^a	10.22 ± 0.59^c	14.50 ± 8.84^b	9.11 ± 1.06^c
22	Hexanal	C₆H₁₂O	1094.6	304.324	1.25538	RI, DT, IS	803.11 ± 7.47^c	1631.34 ± 19.63^a	1511.11 ± 26.91^b	1526.53 ± 8.12^b
23	Hexanal dimer	C₆H₁₂O	1093.9	303.915	1.56442	RI, DT, IS	588.85 ± 7.96^a	93.75 ± 4.67^b	92.93 ± 3.13^b	95.49 ± 2.50^b
29	3-Methylbutanal	C₅H₁₀O	914.1	226.776	1.40351	RI, DT, IS	227.86 ± 6.39^a	33.32 ± 2.59^b	22.36 ± 1.18^c	21.94 ± 1.73^c
33	Dimethyl sulfide	C₂H₆S	797.1	193.431	0.95905	RI, DT, IS	120.07 ± 4.40^c	87.a02 ± 3.82^d	246.81 ± 5.62^b	257.18 ± 3.04^a
49	2-Methylpropanal	C₄H₈O	828.3	202.324	1.28294	RI, DT, IS	150.49 ± 7.13^a	27.08 ± 1.48^b	19.36 ± 1.10^c	19.69 ± 0.92^c
Ketones
45	3-Hydroxy-2-butanone	C₄H₈O₂	1293.5	515.501	1.20934	RI, DT, IS	33.20 ± 3.83^c	97.93 ± 8.72^b	163.20 ± 21.62^a	143.51 ± 21.48^a
46	Acetone	C₃H₆O	836.4	204.638	1.11191	RI, DT, IS	185.75 ± 8.16^c	320.43 ± 12.32^b	430.74 ± 3.98^a	446.58 ± 10.41^a
Organic acid
3	Acetic acid	C₂H₄O₂	1527.2	969.252	1.05013	RI, DT, IS	674.66 ± 46.30^d	3602.39 ± 30.87^c	4536.02 ± 138.86^a	4092.30 ± 40.33^b
4	Acetic acid dimer	C₂H₄O₂	1527.2	969.252	1.15554	RI, DT, IS	45.25 ± 3.89^c	312.16 ± 19.39^b	625.79 ± 78.12^a	538.35 ± 56.38^a
Alcohols
8	1-Hexanol	C₆H₁₄O	1365.1	653.825	1.32772	RI, DT, IS	1647.65 ± 28.94^a	886.33 ± 32.96^b	740.73 ± 44.25^c	730.80 ± 21.58^c
9	1-Hexanol dimer	C₆H₁₄O	1365.8	655.191	1.64044	RI, DT, IS	378.42 ± 20.44^a	332.65 ± 25.76^a	215.78 ± 21.04^b	200.14 ± 28.34^b
13	3-Methyl-1-butanol	C₅H₁₂O	1213.3	414.364	1.24294	RI, DT, IS	691.86 ± 9.95^c	870.41 ± 22.63^b	912.80 ± 23.94^a	939.49 ± 12.44^a
14	3-Methyl-1-butanol dimer	C₅H₁₂O	1213.3	414.364	1.49166	RI, DT, IS	439.90 ± 29.40^c	8572.27 ± 60.56^b	9083.14 ± 193.19^a	9152.25 ± 137.80^a
15	1-Butanol	C₄H₁₀O	1147.2	348.949	1.18073	RI, DT, IS	157.33 ± 9.44^b	198.92 ± 3.92^a	152.78 ± 10.85^b	156.02 ± 9.80^b
16	1-Butanol dimer	C₄H₁₀O	1146.8	348.54	1.38109	RI, DT, IS	24.14 ± 2.15^c	274.75 ± 12.60^a	183.02 ± 17.72^b	176.80 ± 19.80^b
24	1-Propanol	C₃H₈O	1040.9	274.803	1.11042	RI, DT, IS	173.73 ± 4.75^a	55.84 ± 2.16^c	80.80 ± 4.99^b	83.57 ± 2.34^b
25	1-Propanol dimer	C₃H₈O	1040.4	274.554	1.24784	RI, DT, IS	58.20 ± 1.30^b	541.37 ± 11.94^a	541.33 ± 15.57^a	538.84 ± 9.74^a
28	Ethanol	C₂H₆O	930.6	231.504	1.11901	RI, DT, IS	5337.84 ± 84.16^c	11324.05 ± 66.18^a	9910.20 ± 100.76^b	9936.10 ± 101.24^b
34	Methanol	CH₄O	903.6	223.79	0.98374	RI, DT, IS	662.08 ± 13.87^a	76.94 ± 2.15^b	61.92 ± 1.96^c	62.89 ± 0.81^c
37	2-Methyl-1-propanol	C₄H₁₀O	1098.5	306.889	1.35839	RI, DT, IS	306.91 ± 4.09^c	3478.35 ± 25.95^a	3308.79 ± 61.75^b	3313.85 ± 60.88^b
48	1-Pentanol	C₅H₁₂O	1257.6	470.317	1.25222	RI, DT, IS	26.13 ± 2.52^c	116.50 ± 3.71^ab	112.37 ± 6.26^b	124.17 ± 7.04^a
Esters
1	Methyl salicylate	C₈H₈O₃	1859.6	1616.201	1.20489	RI, DT, IS	615.00 ± 66.68^a	485.08 ± 31.30^b	470.14 ± 23.02^b	429.12 ± 33.74^b
7	Butyl hexanoate	C₁₀H₂₀O₂	1403.0	727.561	1.47354	RI, DT, IS	95.83 ± 17.04^a	62.87 ± 3.62^a	92.59 ± 11.88^b	82.13 ± 3.61^c
10	Hexyl acetate	C₈H₁₆O₂	1298.6	524.366	1.40405	RI, DT, IS	44.72 ± 8.21^a	33.18 ± 2.17^d	41.50 ± 4.38^c	40.89 ± 4.33^b
11	Propyl hexanoate	C₉H₁₈O₂	1280.9	499.577	1.39274	RI, DT, IS	34.65 ± 3.90^d	70.43 ± 5.95^a	43.97 ± 4.39^b	40.12 ± 4.05^c
18	Ethyl hexanoate	C₈H₁₆O₂	1237.4	444.749	1.80014	RI, DT, IS	55.55 ± 5.62^c	1606.16 ± 25.63^a	787.24 ± 16.95^b	788.91 ± 28.50^b
20	Isoamyl acetate	C₇H₁₄O₂	1127.8	332.164	1.30514	RI, DT, IS	164.22 ± 1.00^d	243.69 ± 8.37^c	343.51 ± 13.98^b	365.46 ± 1.60^a
21	Isoamyl acetate dimer	C₇H₁₄O₂	1126.8	331.345	1.75038	RI, DT, IS	53.61 ± 4.79^d	4072.20 ± 11.94^a	2416.70 ± 49.84^b	2360.46 ± 43.29^c
26	Isobutyl acetate	C₆H₁₂O₂	1020.5	263.605	1.23281	RI, DT, IS	101.65 ± 1.81^a	15.52 ± 0.67^c	44.87 ± 3.21^b	45.96 ± 1.41^b
27	Isobutyl acetate dimer	C₆H₁₂O₂	1019.6	263.107	1.61607	RI, DT, IS	34.60 ± 1.05^d	540.84 ± 5.64^a	265.54 ± 8.31^c	287.06 ± 3.66^b
30	Ethyl acetate dimer	C₄H₈O₂	885.2	218.564	1.33587	RI, DT, IS	1020.75 ± 6.86^d	5432.71 ± 6.55^a	5052.99 ± 9.65^b	5084.47 ± 7.30^c
31	Ethyl acetate	C₄H₈O₂	878.3	216.574	1.09754	RI, DT, IS	215.65 ± 3.58^a	38.29 ± 2.37^c	71.59 ± 2.99^b	69.32 ± 2.85^b
32	Ethyl formate	C₃H₆O₂	838.1	205.127	1.19738	RI, DT, IS	175.48 ± 3.79^d	1603.20 ± 13.72^a	1472.10 ± 5.95^c	1509.08 ± 13.26^b
35	Ethyl octanoate	C₁₀H₂₀O₂	1467.0	852.127	1.47312	RI, DT, IS	198.86 ± 36.71^b	1853.06 ± 17.60^a	1555.51 ± 24.21^a	1478.05 ± 33.63^a
36	Ethyl octanoate dimer	C₁₀H₂₀O₂	1467.0	852.127	2.03169	RI, DT, IS	135.50 ± 13.02^d	503.63 ± 15.86^a	342.89 ± 11.62^b	297.28 ± 14.40^c
38	Ethyl butanoate	C₆H₁₂O₂	1042.1	275.479	1.5664	RI, DT, IS	21.29 ± 2.68^c	1384.67 ± 8.97^a	1236.52 ± 20.21^b	1228.09 ± 5.09^b
39	Ethyl 3-methylbutanoate	C₇H₁₄O₂	1066.3	288.754	1.26081	RI, DT, IS	9.70 ± 1.85^d	200.29 ± 4.21^a	146.87 ± 8.70^b	127.13 ± 12.54^c
40	Propyl acetate	C₅H₁₀O₂	984.7	246.908	1.48651	RI, DT, IS	4.57 ± 1.07c	128.63 ± 4.28a	87.75 ± 3.26b	88.49 ± 1.99b
41	Ethyl propanoate	C₅H₁₀O₂	962.1	240.47	1.46051	RI, DT, IS	10.11 ± 0.34^d	107.08 ± 3.50^a	149.60 ± 5.39^c	167.15 ± 12.90^b
42	Ethyl isobutyrate	C₆H₁₂O₂	971.7	243.229	1.56687	RI, DT, IS	18.29 ± 2.61^d	55.22 ± 1.07^c	98.81 ± 4.67^b	104.71 ± 4.73^a
43	Ethyl lactate	C₅H₁₀O₃	1352.2	628.782	1.14736	RI, DT, IS	31.81 ± 2.91^c	158.03 ± 2.80^b	548.14 ± 74.21^a	527.01 ± 39.06^a
44	Ethyl lactate dimer	C₅H₁₀O₃	1351.9	628.056	1.53618	RI, DT, IS	44.55 ± 2.03^c	47.56 ± 4.02^c	412.23 ± 50.96^a	185.87 ± 31.25^b
47	Ethyl heptanoate	C₉H₁₈O₂	1339.7	604.482	1.40822	RI, DT, IS	39.55 ± 6.37^a	38.52 ± 2.47^a	28.44 ± 1.52^c	30.77 ± 2.79^b
Unknown
1						RI, DT, IS	15.53 ± 0.18	35.69 ± 0.80	12.70 ± 0.80	10.57 ± 0.86
2						RI, DT, IS	36.71 ± 1.51	120.41 ± 3.44	198.12 ± 6.01	201.19 ± 3.70
3						RI, DT, IS	44.35 ± 0.88	514.12 ± 4.28	224.78 ± 6.56	228.32 ± 4.62
4						RI, DT, IS	857.64 ± 8.63	33.22 ± 1.99	35.05 ± 5.99	35.17 ± 3.97
* Represents the retention index calculated using n-ketones C4−C9 as external standard on MAX-WAX column. Represents the retention time in the capillary GC column. * Represents the migration time in the drift tube.

Table 1.

GC-IMS integration parameters of volatile compounds in Marselan wine at different fermentation stages.

Winemaking stage	TFC (mg CE/L)	TPC (mg GAE/L)	FRAP (mM FeSO₄/mL)	ABTs (mM Trolox/L)
Stage 1	315.71 ± 0.00^d	1,083.93 ± 7.79^d	34.82^c	38.92 ± 2.12^c
Stage 2	1,490.00 ± 7.51^c	3,225.51 ± 53.27^c	77.32^b	52.17 ± 0.95^b
Stage 3	1,510.00 ± 8.88^a	3,307.143 ± 41.76^b	77.56^b	53.04 ± 0.76^b
Stage 4	1,498.57 ± 6.34^b	3,370.92 ± 38.29^a	85.07^a	57.46 ± 2.55^a
Means in the same column with different letters are significantly different (p < 0.05).

Table 2.

Antioxidant activity, total polyphenols, and flavonoids content of Marselan wine at different fermentation stages.