Ultrasonics Sonochemistry 100 (2023) 106636

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Ultrasonics Sonochemistry
journal homepage: www.elsevier.com/locate/ultson

Combined ultrasound and low temperature pretreatment improve the

content of anthocyanins, phenols and volatile substance of Merlot red wine
Qi Xie a, Yurou Tang a, Xueyan Wu a, Qingyan Luo a, Wentong Zhang a, Hanyang Liu a,
Yulin Fang a, c, Xiaofeng Yue b, *, Yanlun Ju a, c, *
a
College of Enology, Northwest A & F University, Yangling 712100, Shaanxi, China
b
College of Food Science and Engineering, Northwest A & F University, Yangling 712100, Shaanxi, China
c
Heyang Viti-viniculture Station, Northwest A & F University, Yangling 712100, Shaanxi, China

A R T I C L E I N F O A B S T R A C T

Keywords: Ultrasound combined with low temperature treatment is a new food processing technology. In this study, low
Ultrasound temperature, three ultrasound power levels, and their combinations were adopted in the must before fermen­
Low temperature tation to study their effects on Merlot red wine. The results showed that ultrasound combined with low tem­
Anthocyanins
perature pretreatment increased the total and monomer contents of anthocyanins and phenols, affected the color
Phenols
of the wine, and significantly increased its antioxidant capacity. In particular, 240 W of ultrasound combined
Volatile
Fermentation with low temperature pretreatment reduced the bad odors (caprylic acid, benzaldehyde, and 1-ethanol content)
and improved the flower and fruit aroma (1-octanol and phenethyl acetate), as well as the aftertaste, thus
improving the quality of the wine. Ultrasound combined with low temperature pretreatment positively affected
the quality of Merlot red wine.

1. Introduction
Ultrasound is an advanced non-thermal food-processing technology
as an alternative to, or an adjuvant method for, conventional processing
techniques [1]. The mechanism of ultrasound extraction of bioactive
compounds is the union of multiple physical mechanisms (fragmenta­
tion, erosion, sonocapillary effect, sonoporation, local shear stress, and
detexturation) [2]. Ultrasound affects food processing by provideing
promoting or damage effects on enzyme activities at the molecular level
[3]. Ultrasound processing, whether used alone or in combination with
other methods, improves food quality significantly, and thus is consid­
ered beneficial [4]. In recent years, ultrasound technology has been
applied to the processing of food by-products, including fruits [5],
vegetables [6], and juices [7]. Gambacorta et al., [8] demonstrated that
ultrasound in winemaking increased the extraction of polyphenols from
grapes and improved the sensory characteristics and health benefits of
wine due to a higher content of nutraceuticals. Natrella et al., [9]
applied an ultrasound treatment during the vinification of three
different red grape cultivars with the aim of assessing the impact on the
volatile profile of the wines. A clear separation was observed between
the control and ultrasound-treated wines for all three cultivars, with
ethyl decanoate, ethyl isopentyl succinate, and butyric acid having the
highest discriminant coefficients. Lukić et al., [10] found that high
power ultrasound modified phenolic and volatile composition, with
greater effect in white wines with lower concentration of antioxidants.
Similarly, Aragón-García et al., [11] proposed that application of ul­
trasound during the pre-fermentative maceration process favors the
release and extraction of volatile compounds in greater amounts.
Low temperature pretreatment is now used in various fields of food
processing. Low temperature pretreatment is defined as lowering the
temperature of foodstuffs reduces microbiological and biochemical
spoilage by decreasing microbial growth rates and enzymatic activity
[12]. Fruits, vegetables and other foods are processed at temperatures
above freezing but below room temperature, around 0 − 5℃. The
application of pretreatment at low temperature before fermentation is
one of the most applied and investigated practices [13]. The vinification
technique with low temperature pretreatment—referred to as pre-
fermentative cold maceration—is used to enhance anthocyanin diffu­
sion from the skins to the must, increasing pigment extraction. Casassa
et al., [14] found that a short period of low temperature pretreatment
before fermentation did not affect the basic physicochemical indexes,
volatile compounds, or improve the aroma of Merlot wine, but

* Corresponding authors.
E-mail addresses: yuexiaofeng@nwsuaf.edu.cn (X. Yue), juyanlun2016@nwsuaf.edu.cn (Y. Ju).

https://doi.org/10.1016/j.ultsonch.2023.106636
Received 10 August 2023; Received in revised form 22 September 2023; Accepted 6 October 2023
Available online 7 October 2023
1350-4177/© 2023 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
Q. Xie et al.
effectively reduced the astringency and pain perception in the generated
wine. Studies have shown that, during pre-fermentative cold maceration
of Merlot red wine, an increase in total polyphenol index, anthocyanins,
and tannins of around 10 % takes place, and this increment is main­
tained until the end of the alcoholic fermentation [15]. Yan et al., (2018)
used a low temperature technique combined with ultrasound to treat
raw sweet white wine and obtained a more microbially stable and higher
quality sweet white wine. There are currently no reports on the com­
bined use of ultrasound and low temperature pretreatment in dry wine.
Phenolic compounds are the most abundant fraction of the nonvol­
atile compounds of red wine and have a large contribution to color,
astringency, and bitterness [16]. Moderate amounts of polyphenols in
wine are associated with anti-inflammatory activity, endothelial func­
tion, and flow-mediated dilation, and thus are beneficial to human
health [17]. Anthocyanins are a type of polyphenol derivative, and the
copigmentation of anthocyanins is beneficial to the stability of wine
color [18]. Wine aroma is a complex mixture of volatile substances that
are a crucial determinant of wine quality [19]. The composition and
content of volatile compounds lead to a variety of aromas and create
differences between wines.
Therefore, a combination of ultrasound and low temperature pre­
treatment might be a promising method for improving the winemaking
process and the quality of wine. With the development of modern food
technology, consumer demands for food safety and green approaches
have greatly increased. Compared with chemical methods, a physical
method is more in line with the requirements of green food. This study
aims to fill a knowledge gap in the combined effects of ultrasound and
low temperature pretreatment on a red dry wine, which can provide a
new direction for the development of wine production technology.
2. Materials and methods
2.1. Wine samples and vinification process
Grapes (Vitis vinifera L. cultivars Merlot) were collected from a
commercial vineyard located at Yangling, Shaanxi, China (39◦ 54′ N,
116◦ 23′ E) and the sugar content was 191.84 g•L-1. A small container
brewing method was used, referring to Jiang et al. [20]. The grapes were
sorted by hand, then crushed and destemmed. Pectinase (Lallzyme EX,
Lallemand, France) was added at 30 mg•L-1 and SO2 was sulfited at 50
mg•L-1. About 4 L (80 % of fermenter) musts were homogeneously
distributed in eight 5-L glass fermenters that were cleaned and dried in
advance, and were pretreated using one of the following methods: 1) no
ultrasound treatment and low temperature pretreatment (CK); 2) 120 W
ultrasound treatment (120U); 3) 240 W ultrasound treatment (240U); 4)
400 W ultrasound treatment (400U); 5) no ultrasound treatment but low
temperature pretreatment (LT); 6) 120 W ultrasound treatment and low
temperature pretreatment (LT + 120U); 7) 240 W ultrasound treatment
and low temperature pretreatment (LT + 240U); or 8) 400 W ultrasound
treatment and low temperature pretreatment (LT + 400U). The ultra­
sonic device is ultrasonic bath (KQ-400DE, Kun Shan Ultrasonic In­
struments Co., Ltd, China). The internal temperature of the ultrasonic
device was controlled to be constant at room temperature (25℃ ± 1℃)
by continuous injection of cold water and discharge of hot water. The
ultrasound treatment time was 30 min and the low temperature pre­
treatment was at 4 ◦ C for 12 h.
The pretreated musts were inoculated with yeast (Saccharomyces
cerevisiae RC212, Lallenmand, Denmark) that had been activated by
grape juice at 0.5 g•L-1 in terms of dry weight. The fermentation tem­
perature was 21 ◦ C ± 2 ◦ C. During alcoholic fermentation, we moni­
tored the temperature, specific gravity, and sugar degree each day. The
wine was racked and decanted after 2 d of fermentation. When the
specific gravity became constant, the wines were racked and 60 mg•L-1
of SO2 was added to complete the fermentation. All analyses were per­
formed after cold-stabilization for 60 d [21] at 0 ◦ C ± 2 ◦ C and matu­
ration for 60 d in bottles at 20 ◦ C.
2
Ultrasonics Sonochemistry 100 (2023) 106636
2.2. Chemicals
Methanol, ethyl acetate, acetic acid, and acetonitrile (HPLC grade)
were obtained from Sigma (Shanghai, China). Folin–Ciocalteu, 6-hy­
droxy-2,5,7,8-tetramethylchroman-2-carboxylic acid, and 2,2-
diphenyl-1-picrylhydrazyl (analytical grade) were obtained from
Fisher (Suwanee, GA, USA). The standards (citric acid, tartric acid, malic
acid, amber acid, lactic acid, acetic acid, delphinidin 3-O-glucoside,
cyanidin 3-O-glucoside, petunidin 3-O-glucoside, peonidin 3-O-gluco­
side, malavidin 3-O-glucoside, peonidin 3-O-(6-O-acetyl)-glucoside,
malavidin 3-O-(6-O-acetyl)-glucoside, trans-peonidin 3-O-(6-O-p-cou­
maryl)-glucoside, trans-malvidin 3-O-(6-O-p-coumaryl)-glucoside,
gallic acid, protocatechuic acid, catechin, gentianic acid, caffeic acid,
epicatechin, p-coumaric acid, rutin, trans-ferulic acid, rhizoside,
resveratrol, quercetin, and kaempferol) used in this study were of HPLC
grade and obtained from Sigma (Shanghai, China).
2.3. Detection of basic physicochemical indices of wine samples
The detection of the ethanol, pH, volatile acid, and titratable acid of
the wine samples was conducted according to International Vine and
Wine Organization [22]. The total phenolic content (TPC) was deter­
mined using the Folin-Ciocalteu assay reference to Jara-Palacios et al.,
[23]. The total anthocyanin content (TAC) was determined using pH-
differential spectrophotometry based on the method of Cliff, King, and
Schlosser [24] with some modifications. The total flavonoid content
(TFC) was determined using aluminum chloride colorimetry [25]. Total
flavan-3-ol (TFOC) was determined using spectrophotometric determi­
nation [26].
2.4. Color intensity of the wine samples
The a* (green/red), b* (blue/yellow), and c* (saturation) values and
h◦ (hue angle) were obtained directly by analyzing the color of wine
samples with a wine color analyzer (W100, Hanon Advanced Technol­
ogy Group Co., Ltd, China). An equal amount of liquor was added to a
standard wine glass and photographed in the same small studio to obtain
a true image of the color of the wine sample.
2.5. HPLC analyses of the wine samples
2.5.1. Sugar
The sugar analysis was based on published reports (Ju et al., 2018).
The wine samples were filtered with a 0.45-μm filter membrane and
then injected into a 1.5-mL bottle with a sterile syringe. A high perfor­
mance liquid chromatography (HPLC) system (Agilent 1100, Agilent
Technologies Co. Ltd., USA) was used for the determination of sugar.
Chromatographic conditions were as follows: a ZORBAXSB-C18 (4.6
mm × 250 mm, 5 μm) was used as the column; the mobile phase was
acetonitrile–water (7525, V/V); the flow rate was 1.0 mL/min; the
column temperature was 40 ◦ C; difference detection was used; the
sample size was 10 μL; and the analysis time was 20 min. The curve was
drawn with standards and compared with the standard curve to obtain
the results.
2.5.2. Organic acid
The organic acid analysis was based on that of a previously published
report [27]. The wine samples were filtered with 0.45-μm filter mem­
branes and then injected into 1.5-mL bottles with sterile syringes. An
HPLC system (Agilent 1100, Agilent Technologies Co. Ltd., USA) was
used for the determination of organic acid. The chromatographic con­
ditions were as follows: a Hypersil GOLDa Q (250 mm × 4.6 mm, 5 μm)
was used as the column; the mobile phase was 0.01 mol/L dipotassium
phosphate solution (pH 2.2); the flow rate was 0.5 mL/min; the column
temperature was 25 ◦ C; the sample size was 10 μL; the wavelength was
210 nm; and the analysis time was 30 min. The curve was drawn with
Q. Xie et al.
standards, and the quantitative calculations were carried out according
to the curve of standard samples.
2.5.3. Anthocyanins
Anthocyanin identification was performed following a modification
of the method described by Yue et al., [28]. After filtering through a
0.22-μm filter, the anthocyanin content was analyzed by an HPLC sys­
tem (LC-20AT, Shimadzu Co., Ltd., Japan) fitted with a C18 column (4.6
× 250 mm, 4 μm, SynergiTM 4-µm Hydro-RP 80A, Phenomenex, USA).
Formic acid–water-acetonitrile (1:32:4, v/v/v) was used as solvent A,
and formic acid–water-acetonitrile (1:16:20, v/v/v) was used as solvent
B. The solvent gradient elution was as follows: 0.00–15.00 min, 0–10 %
B; 15.00–30.00 min, 10–20 % B; 30.00–45.00 min, 20–35 % B;
45.00–46.00 min, 35–100 % B; and 50.00–51.00 min, 100–0 % B. The
standard product was dimethoxylin-3-O-glucoside. The standard was
used to establish a calibration curve, and the relative concentration of
each monomeric anthocyanin was expressed as the equivalent of
dimethoxylin-3-O-glucoside.
2.5.4. Phenolic substances
The extraction of phenolic substances in wine samples was according
to reports [29] with some modifications. HPLC was used for the phenolic
substance content determination. Samples were filtered through a 0.22-
μm filter, in an LC-20AT (Shimadzu Co., Ltd., Japan). Formic acid–water
(1:99, v/v) was used as solvent A, and acetonitrile (HPLC grade) was
used as solvent B. The solvent gradient elution was as follows:
0.00–5.00 min, 3–10 % B; 5.00–15.00 min, 10–15 % B; 15.00–33.00
min, 15–26 % B; 33.00–40.00 min, 26–45 % B; and 40.00–50.00 min,
45–3 % B. Mixed standards of five concentration levels were prepared
and standard curves were drawn. The identification and quantification
of phenolic substances were undertaken according to the calibration
curve of the respective standard.
2.6. Analyses of the volatile compounds of wine samples
Volatile compounds were analyzed by a gas chromatography-mass
spectrometry system (GC–MS) (ThermoFinnigan, USA) using a pub­
lished methodology [30] with some modifications. The GC conditions
were: a DB-WAX column (30 m × 0.25 mm, 0.25 µm) was used; helium
(He) was the carrier gas; the flow rate was 1 mL/min; the column
temperature was maintained at 40 ◦ C for 3 min, then increased to 160 ◦ C
at 4 ◦ C/min, and then to 230 ◦ C at 7 ◦ C/min for 8 min; and the tem­
perature of the connecting rod was set to 230 ◦ C. The MS conditions
were: full scan, ranging from 33 to 450 amu, once per second; electron
bombardment was the ion source; the ion source temperature was
230 ◦ C; the electron energy was 70 eV; the filament current was 0.2 mA;
and the detector voltage was 350 V. Volatile compound identification
was conducted according to the NIST 14 mass spectrum library and
retention indices of the authentic standards. The internal standard was
4-methyl-2-amyl alcohol (1.0 g/L). The calibration curve of volatile
compounds was established by using the area ratio and concentration
ratio of the target compound and internal standard. The volatile com­
pounds were quantitatively analyzed using calibration curves.
2.7. Analysis of the antioxidant capacity of wine samples
The antioxidant activity of wine samples was determined using the
methods of 1,1′-diphenyl-2-picryl-hydrazyl radical (DPPH) and ferric-
reducing antioxidant power (FRAP). The DPPH method referred to
previous methods [31]. Three replicates of each sample were prepared.
Briefly, 0.1 mL of a wine sample was added to 3.9 mL of the DPPH
mother liquor (25 mg•L-1 of a DPPH formic acid solution) and mixed
evenly, and the light absorption value was determined at 517 nm after
20 min of a light-shielded reaction. The same volume of a 15 % ethanol
solution was used to replace the wine samples as the control. The DPPH
value was expressed as DPPH (%) = [(Ablank – Asample)/Ablank] × 100 %
3
Ultrasonics Sonochemistry 100 (2023) 106636
[32].
The FRAP method referred to previous methods [33] with some
modifications. Briefly, 1 mL of a wine sample was reacted with 5 mL of
tripyridyltriazine (TPTZ) in a bath of 37 ◦ C for 10 min, and then the
absorbance was measured at 593 nm. The results were expressed as
FeSO4 equivalence (μmol•L-1).
2.8. Sensory evaluation of the wine samples
The American Wine Society (AWS) wine tasting list was used with
slight adjustments to organize a sensory tasting panel of eighteen people
(eight men and eight women). Prior to the tests, the panelists were
informed about the procedures, samples, and treatments, and written
consent was obtained. In particular, the tasting group was intensively
trained for taste and smell using the standard taste and aroma substances
of wine. The eight wine samples were blind tasted and scored for degree
of clarification, color, aroma balance, aroma intensity, taste balance,
flavor intensity, and aftertaste persistence, and the full score of each
parameter was 5 points. The parameter ratings were then averaged.
2.9. Statistical analysis
The experimental data were analyzed by Microsoft Office 2016
software and SPSS Statistics 22.0 software (Duncan test). The signifi­
cance level of all test results was α = 0.05. GraphPad Prism 9 software
was used to draw line charts and bar charts. After the calculation of the
volatile substance normalization, Origin software was used to draw the
heat map and perform principal component analysis (PCA).
3. Results and discussion
3.1. Fermentation process
The changes in temperature, specific gravity, and sugar degree of the
wine samples were monitored during fermentation, and the results are
shown in Fig. 1. The overall temperature fluctuation trend was consis­
tent, which impacted fermentation kinetics [34], and was primarily
dependent on the fermentation process rather than the pretreatment.
Due to the different pretreatments, the initial proportion of each group
was different. Specific gravity is mainly related to the concentration of
the extract in the liquid. It was clearly observed that after the highest
power ultrasound treatment and low temperature pretreatment, the
extract in grape juice had the highest specific gravity. When no ultra­
sound treatment was performed, the difference in specific gravity be­
tween samples was 1.85 % whether or not low temperature
pretreatment was performed. When low temperature pretreatment was
not performed, the maximum power ultrasound treatment decreased the
specific gravity. With the highest power ultrasound pretreatment, the
specific gravity of the low temperature pretreatment samples was 5.41
% higher than that without low temperature pretreatment. In conclu­
sion, the combined ultrasound and low temperature pretreatment
increased the concentration of extracts in the pre-fermentation liquid.
After fermentation, the proportion in the LT + U400 group decreased the
fastest but reached an equilibrium value 24 h later than the other
groups. The law of sugar degree value is similar to that of specific
gravity, and the same LT + U400 group had the fastest decrease in the
sugar degree. It should be noted that small fluctuations in the specific
gravity and sugar degree curves may be due to sampling errors caused by
an uneven distribution of liquor during fermentation.
3.2. Physicochemical characteristics
The physicochemical characteristics of wine, including pH, ethanol,
volatile acid, titratable acid, citric acid, tartaric acid, malic acid, amber
acid, lactic acid, TPC, TAC, TFC, and TFOC were measured in each
sample, and the results are shown in Table 1. There was almost no
Q. Xie et al. Ultrasonics Sonochemistry 100 (2023) 106636

Fig. 1. Effects of ultrasonic combined with low temperature pretreatment on fermentation process of Merlot wine. (A): Temperature, (B): Specific gravity, (C): Sugar
degree, CK: No-low temperature pretreatment, U120: 120 W ultrasound treatment, U240: 240 W ultrasound treatment, U400: 400 W ultrasonic treatment, LT: low
temperature pretreatment, LT + U120: low temperature pretreatment and 120 W ultrasound treatment, LT + U240: low temperature pretreatment and 240 W
ultrasound treatment, LT + U400; low temperature pretreatment and 400 W ultrasound treatment.

Table 1
Effects of ultrasound combined with low temperature pretreatment on basic physicochemical indexes of Merlot wine.
Ultrasonic power

No-low temperature pretreatment Low temperature pretreatment

0W 120 W 240 W 400 W 0W 120 W 240 W 400 W

pH 3.55± 3.53± 3.58± 3.57± 3.52± 3.59± 3.59± 3.56±

0.02 cd 0.00de 0.01ab 0.01bc 0.00e 0.00a 0.01ab 0.01c
Ethanol / %vol 10.67± 10.45± 10.44± 10.46± 10.73± 10.48± 10.56± 10.06±
0.06a 0.04ab 0.01ab 0.01ab 0.04a 0.23ab 0.42a 0.01b
Volatile acid / g⋅L-1 0.34± 0.34± 0.42± 0.31± 0.34± 0.33± 0.33± 0.34±
0.02bc 0.01bc 0.00a 0.01c 0.01bc 0.00bc 0.02bc 0.01b
Titrable acid / g⋅L-1 5.08± 5.49± 5.30± 5.40± 5.39± 5.11± 5.12± 5.39±
0.05c 0.01a 0.04b 0.04ab 0.03ab 0.05c 0.07c 0.01b
Citric acid / g⋅L-1 0.78± 0.77± 0.77± 0.75± 0.80± 0.80± 0.80± 0.79±
0.02a 0.03a 0.04a 0.01a 0.00a 0.00a 0.00a 0.01a
Tartric acid / g⋅L-1 1.12± 1.11± 1.12± 1.10± 1.13± 1.12± 1.11± 1.11±
0.03a 0.01a 0.03a 0.00a 0.02a 0.00a 0.02a 0.02a
Malic acid / g⋅L-1 2.27± 2.20± 2.27± 2.20± 2.27± 2.20± 2.20± 2.20±
0.11a 0.00a 0.11a 0.00a 0.11a 0.00a 0.00a 0.00a
Amber acid / g⋅L-1 3.32± 3.28± 3.35± 3.41± 3.29± 3.22± 3.22± 3.27±
0.01a 0.18a 0.08a 0.00a 0.01a 0.10a 0.12a 0.02a
Lactic acid / g⋅L-1 3.03± 3.00± 3.10± 3.17± 3.03± 2.90± 2.91± 2.99±
0.00a 0.25a 0.10a 0.00a 0.00a 0.09a 0.11a 0.06a
Total phenol content / mg⋅L-1 98.41± 90.71± 128.69± 119.19± 100.46± 82.76± 86.09± 152.55±
3.47d 3.95e 1.18b 2.35c 0.77d 1.33f 1.94ef 1.18a
Total anthocyanins content 56.11± 48.91± 50.67± 55.37± 57.72± 54.34± 65.21± 68.30±
/ mg⋅L-1 1.16b 1.57d 1.30 cd 1.62b 3.14b 1.45bc 3.60a 1.25a
Total flavonoids content 607.85± 493.62± 437.46± 793.23± 785.92± 751.69± 746.69± 554.77±
/ mg⋅L-1 12.30b 5.77 cd 1.92d 40.77a 29.62a 37.69a 10.38a 44.62bc
Total flavan-3-ol content 15.94± 13.46± 17.42± 18.31± 9.40± 15.16± 13.07± 16.62±
/ mg⋅L-1 0.21 cd 0.26e 0.02ab 1.47a 0.29f 1.45d 0.17e 1.28bc

Note: Different letters in the row indicate significant differences (Duncan test, P ≤ 0.05) among treatments.

4
Q. Xie et al. Ultrasonics Sonochemistry 100 (2023) 106636

difference in pH or the content of various acids among the groups, and
the values were all within the range prescribed by OIV [22], thus
meeting the standard. The ethanol contents of the non-ultrasound
treatment groups were higher than that of the ultrasound treatment
groups, regardless of whether low temperature pretreatment was per­
formed, which was consistent with previously reported experimental
results [35]. The 400 W ultrasound and low temperature pretreatment
significantly reduced the alcohol content. The pre-fermentation sugar
concentration in the LT + 300 W group was higher than that in the other
groups, but the post-fermentation ethanol was significantly lower than
that in the control group, possibly because more sugars were converted
to other byproducts, such as glycerol [36] and higher alcohols [37]. The
TPC of LT + U400 was significantly higher than that of the other groups,
and the TPC of the group treated with the highest ultrasound power was
higher than that of the corresponding control group with or without low
temperature pretreatment. The TAC of the LT + U400 and LT + U400
groups was significantly higher than that of the other groups. Under the
same temperature pretreatment conditions, TAC regularly decreased
and then increased with an increase in ultrasound frequency. TFC and
TFOC showed a similar pattern, with group U400 having the highest
levels, and were significantly higher than the control group. Because the
TFC of the LT + U400 group was lower than that of the LT group and the
flavanols were thought to be chiefly responsible for astringency in wines
[38], high power ultrasound may counteract the astringent feeling
caused by low temperature pretreatment. A significant interaction was
observed between pretreatment and TPC, TAC, TFC, and TFOC. Tang
et al., (2016) conducted ultrasound treatment on wine during fermen­
tation, and the results of the physicochemical characteristics obtained
were similar to those in this experiment.
3.3. Anthocyanin profile
Anthocyanins are the main pigments of red grapes primarily
responsible for the color of red wines [39], and therefore play a major
role in consumer preference and appreciation [40]. Fig. 2 shows the
effect of ultrasound combined with low temperature pretreatment on
the anthocyanin content of Merlot wines, expressed as the means (mg⋅L-
1
) of the three analytical replicates. Nine anthocyanin compounds were
identified and quantified: Dp-3-O-Glu, Cy-3-O-Glu, Pt-3-O-Glu, Pn-3-O-
Glu, Mv-3-O-Glu, Pn-3-acetylglc, Mv-3-acetylglc, Pn-3-p-coumglc trans,

Fig. 2. Effects of ultrasonic combined with low temperature pretreatment on anthocyanin of Merlot wine. (A): Delphinidin 3-O-glucoside, (B): Cyanidin 3-O-gluco­
side, (C): Petunidin 3-O-glucoside, (D): Peonidin 3-O-glucoside, (E): Malavidin 3-O-glucoside, (F): Malavidin 3-O-(6-O-acetyl)-glucoside, (G): Peonidin 3-O-(6-O-
acetyl)-glucoside, (H): Trans-Peonidin 3-O-(6-O-p-coumaryl)-glucoside and (I): Trans-Malvidin 3-O-(6-O-p-coumaryl)-glucoside. Values presented are means ± SD
(n = 3). Different letters indicate significant differences among treatments using Duncan test (p ≤ 0.05). CK: No-low temperature pretreatment, U120: 120 W ul­
trasound treatment, U240: 240 W ultrasound treatment, U400: 400 W ultrasonic treatment, LT: low temperature pretreatment, LT + U120: low temperature pre­
treatment and 120 W ultrasound treatment, LT + U240: low temperature pretreatment and 240 W ultrasound treatment, LT + U400; low temperature pretreatment
and 400 W ultrasound treatment.

5
Q. Xie et al.
and Mv-3-p-coumglc trans. Mv-3-O-Glu (30.59–41.31 mg⋅L-1) was the
most abundant species of the various monomeric anthocyanins and Dp-
3-O-Glu (0.25–0.41 mg⋅L-1) was the least abundant, which was consis­
tent with levels previously measured in Merlot wines. As shown in Fig. 3,
all anthocyanin compounds were found at significantly higher levels in
wine samples pretreated with 400 W ultrasound and low temperature.
All anthocyanin compounds were found to be increased with an increase
of ultrasound power with low temperature pretreatment. The results
indicated that ultrasound combined with low temperature pretreatment
effectively increased the content of each monomeric anthocyanin.
Interestingly, we did not find that low temperature pretreatment
improved the content of anthocyanins in wine as previously reported
[41], as neither the content of total anthocyanins nor of monomeric
anthocyanins increased by low temperature pretreatment alone.
3.4. Chromatic characteristics
As shown in Table 2, significant changes of a*, b*, c*, h*, and ΔE
were observed in wine samples pretreated by ultrasound combined with
low temperature. The a*, c*, and ΔE levels of the wine samples pre­
treated with low temperature alone were observed to be significantly
higher than those of the other groups. The wine samples pretreated with
400 W ultrasound alone were found to have the significantly highest b*,
and samples pretreated with 400 W and low temperature were found to
have the significantly highest h*. A larger a* value indicates a redder
color and a larger b* value indicates a yellower color. With ultrasound
treatment, the higher the power, the redder the wine sample. Ultrasound
treatment changed the color of the wine to yellow without low tem­
perature pretreatment but changed the color of the wine sample to blue
with low temperature pretreatment.
3.5. Phenolic acid profile
Phenolic acids play an important role in controlling oxidation [42].
Phenolic compounds in wine samples pretreated by ultrasound com­
bined with low temperature are listed in Table 3, expressed as the means
(mg⋅L-1) of three analytical replicates. A total of 14 phenolic acid com­
pounds were determined in the samples. The content of different
phenolic acids also differed according to the pretreatment. The highest
substance content was found in ultrasound combined with low
Fig. 3. Effects of ultrasonic combined with low temperature pretreatment on antioxidant capacity of Merlot wine. (A): ferric reducing antioxidant power (FRAP), (B):
1,1-diphenyl-2-picrylhydrazyl (DPPH). CK: No-low temperature pretreatment, U120: 120 W ultrasound treatment, U240: 240 W ultrasound treatment, U400: 400 W
ultrasonic treatment, LT: low temperature pretreatment, LT + U120: low temperature pretreatment and 120 W ultrasound treatment, LT + U240: low temperature
pretreatment and 240 W ultrasound treatment, LT + U400; low temperature pretreatment and 400 W ultrasound treatment.
6
Ultrasonics Sonochemistry 100 (2023) 106636
temperature pretreated samples (except for protocatechuic acid, gen­
tianic acid, quercetin, and kaempferol). Gallic acid, epicatechin, rutin,
and resveratrol contents of wine samples pretreated by ultrasound
combined with low temperature were positively correlated with the
ultrasound power, while the content of caffeic acid was negatively
correlated. The total amount of phenolic acid in the wine samples with
ultrasound treatment was higher than that in the corresponding control
group. In conclusion, ultrasound combined with low temperature pre­
treatment significantly increased the content of most phenolic acids and
the total phenolic content.
3.6. Antioxidant activities
Antioxidant activity and total phenolic content are highly correlated
[43]. In this study, it was found that ultrasound combined with low
temperature pretreatment affected the content of anthocyanins and
phenolic acids in wine samples. Therefore, two methods (FRAP and
DPPH) were further used to determine the antioxidant capacity of the
wine samples, and the results are shown in Fig. 3. The highest values of
FRAP appeared in the wine samples of the LT + U400 group (3.73 ±
0.05 U⋅mL− 1), but the highest values of DPPH appeared in the LT +
U240 group (50.23 ± 5.39 %), and both were also significantly higher
than those of the CK group (3.17 ± 0.03 U⋅mL− 1 and 22.23 ± 2.69 %,
respectively). The values of FRAP showed that only ultrasound at the
highest power (400 W) significantly increased the antioxidant capacity
of the wine samples, but the values of DPPH showed that the antioxidant
capacity of the wine samples was improved with any power of ultra­
sound treatment. The DPPH results showed that low temperature pre­
treatment improved the antioxidant capacity of the wine samples
(except for 120 W ultrasound), and the effect was notable at medium
and high ultrasound power, while FRAP results did not show this effect.
The results of both methods showed that ultrasound combined with low
temperature pretreatment contributed to improving the antioxidant
activity of the wine samples, which was consistent with the effect on the
content of anthocyanins and phenolic acids.
3.7. Volatile components
The volatile compounds were qualitatively and quantitatively
analyzed by GC–MS. To more intuitively reflect the differences of
Q. Xie et al. Ultrasonics Sonochemistry 100 (2023) 106636

Table 2
Effects of ultrasound combined with low temperature pretreatment on the chromatic characteristics of Merlot wine.
Ultrasonic power Apparent appearance a* b* c* h* ΔE

NLT 0W 22.24± 7.23± 23.38± 0.31± 29.59±

0.02 g 0.03e 0.03 g 0.01c 0.04d

120 W 24.45± 7.50± 25.61± 0.30± 31.72±

0.04d 0.06d 0.16d 0.01c 0.01c

240 W 25.03± 7.61± 26.16± 0.30± 32.50±

0.04b 0.06c 0.06b 0.01c 0.01b

400 W 24.73± 8.16± 25.97± 0.32± 32.73±

0.07c 0.02a 0.02c 0.00b 0.01ab

LT 0W 25.23± 7.71± 26.51± 0.30± 33.27±

0.15a 0.02b 0.04a 0.00c 0.04a

120 W 19.93± 6.97± 21.19± 0.34± 26.37±

0.06 h 0.01 g 0.06 h 0.00a 0.06e

240 W 22.90± 7.14± 24.00± 0.30± 30.18±

0.04f 0.02f 0.03f 0.00c 0.30d

400 W 23.82± 5.53± 24.49± 0.23± 29.54±

0.02e 0.02 h 0.04e 0.00d 0.80d

Note: Different letters in the row indicate significant differences (Duncan test, P ≤ 0.05) among treatments. NLT: No low temperature pretreatment: NT: Low tem­
perature pretreatment.

volatile components in different wine samples, the content of the vola­
tile components was normalized and then drawn into a heat map. The
results are shown in Fig. 4A. Sixty volatile components were measured in
the wine samples, including 37 alcohols, four fatty acids, 21 esters, two
terpenes, and six carbonyl compounds. Higher alcohols have been
related to pungent, caramel, and fruity odors [44], and esters affect the
fruity aroma of wine [45]. In general, ultrasound combined with low
temperature pretreatment increased the content of most alcohols and
esters in the volatile components of the wine samples. Particularly when
the ultrasound power was 240 W, the contents of most volatile com­
ponents reached a maximum, indicating that the pretreatment improved
the caramel and fruity odors of the wine. 1-Octanol and phenethyl ac­
etate produce intense citrus and pleasant floral aromas, respectively
[46], contributing positively to the wine aroma. Low temperature pre­
treatment increased the content of these two compounds and thus
improved the aroma of the wine, but there were losses after combining

7
Q. Xie et al. Ultrasonics Sonochemistry 100 (2023) 106636

Table 3
Effects of ultrasound combined with low temperature pretreatment on phenolic acid substances of Merlot wine (mg⋅L-1).
Ultrasonic power

No-low temperature pretreatment Low temperature pretreatment

0W 120 W 240 W 400 W 0W 120 W 240 W 400 W

Gallic acid 9.38± 8.78± 11.05± 10.78± 9.43± 7.30± 12.94± 14.93±
3.41bc 0.69bc 1.56abc 1.23abc 4.15abc 0.49c 1.29ab 0.34a
Protocatechuic acid 9.98± 14.90± 6.39± 8.56± 6.61± 4.76± 4.51± 11.27±
1.45ab 0.23a 2.05b 1.43ab 3.16b 0.08b 0.03b 7.40ab
Catechin 3.30± 2.84± nd 1.85± 4.22± 4.50± 3.93± 2.54±
0.02ab 0.35ab 0.61b 2.08a 0.31a 0.29a 0.20ab
Gentianic acid 213.97± 196.14± 374.06± 370.53± 260.59± 302.51± 271.45± 312.55±
16.63d 4.02d 39.63a 6.42a 8.29c 3.51bc 9.12bc 22.98b
Caffeic acid 6.19± 6.89± 9.96± 8.84± 9.02± 9.17± 9.77± 8.42±
3.20a 1.88a 0.70a 0.25a 1.01a 1.44a 0.66a 0.20a
Epicatechin 11.22± 12.31± 11.97± 11.10± 11.28± 13.74± 13.70± 18.55±
0.32d 0.16 cd 0.77d 0.18d 0.17d 0.13b 1.09bc 0.81a
P-coumaric acid 9.44± 9.10± 9.30± 9.32± 9.30± 9.33± 9.74± 9.40±
0.39ab 0.01b 0.04ab 0.00ab 0.10ab 0.19ab 0.17a 0.31ab
Rutin 15.03± 12.30± 12.77± 12.03± 14.19± 14.81± 16.20± 17.43±
2.71ab 0.81b 1.02b 0.56b 0.02ab 1.44ab 1.50a 0.36a
Trans-ferulic acid 8.02± 5.86± 7.48± 7.58± 8.52± 7.42± 9.50± 6.84±
1.85ab 1.47b 1.00ab 0.00ab 1.49ab 1.12ab 1.38a 0.17ab
Rhizoside 3.38± 1.93± 1.59± 1.15± 1.10± 2.55± 3.93± 2.95±
0.22ab 0.76bcd 1.00 cd 0.62d 1.00d 0.55abcd 0.48a 0.34abc
Resveratrol 6.47± 6.50± 6.55± 6.55± 6.64± 6.67± 6.68± 6.90±
0.01d 0.02 cd 0.02c 0.00 cd 0.02b 0.03b 0.03b 0.08a
Quercetin 2.53± 3.05± 2.44± 2.39± 2.48± 2.46± 2.49± 2.37±
0.05b 0.12a 0.08bc 0.01bc 0.07bc 0.04bc 0.02bc 0.04c
Kaempferol 1.83± 1.84± 1.96± 2.47± 2.03± 2.01± 2.00± 2.07±
0.02d 0.01d 0.00c 0.00a 0.06bc 0.04bc 0.02c 0.03b
Gallic acid 9.38± 8.78± 11.05± 10.78± 9.43± 7.30± 12.94± 14.93±
3.41bc 0.69bc 1.56abc 1.23abc 4.15abc 0.49c 1.29ab 0.34a
Total 300.74 282.43 454.75 453.15 345.43 387.24 366.85 416.22

Note: Different letters in the row indicate significant differences (Duncan test, P ≤ 0.05) among treatments. “nd” indicates that the substance was not detected.

with ultrasound, although the levels were still higher than those of the
control group. Ultrasound treatment increased the content of caprylic
acid, which imparts a rancid feeling to red wine [46], but low temper­
ature pretreatment offset this effect. Combined treatment reduced
benzaldehyde and 1-ethanol content to reduce the green and bitter
almond taste [47]. Fig. 4B and 4C show the PCA data. Multivariate data
analysis revealed the effects of combined treatment on the volatile
components of the wine. The first two principal components accounted
for 65.4 % (PC1 and PC2 were 47.5 % and 17.9 %, respectively). The
distance between the LT and the CK groups on the load diagram was far,
indicating that their volatile components were different, which was
consistent with the results shown in the heat map (Fig. 5A). Combined
with the score chart, it was found that the differences between the two
groups were mainly in 1-octanol and octanoic acid. LT + 120U was also
located far away from the other groups, which was primarily reflected
by ethyl acetate levels. The difference between the experimental and CK
groups in PC1 was mainly due to various esters. In conclusion, the
combined treatment was beneficial to the formation of a pleasant aroma
and greatly reduced undesirable aromas.
3.8. Sensory analysis
Fig. 5 shows the results of the sensory evaluation of 18 panelists on
eight wine samples. There were no differences in the degree of clarifi­
cation between the wines from different pretreatments, and all scored
between 4.3 and 4.5 points. Low temperature pretreatment improved
the wine aroma significantly, which increased the aroma intensity, and
also increased the balance degree, but ultrasound treatment interfered
with these improvements. In terms of taste, the wines with low tem­
perature pretreatment did not perform well, except combined with 120
W ultrasound treatment. The wine samples treated with 400 W ultra­
sound had the highest aftertaste persistence scores, and the red wines
that were not treated with low temperature had higher overall aftertaste
scores. Ultrasound treatment of wine samples offset the negative effects
of low temperature on the aftertaste. As such, ultrasound combined with
low temperature treatment improved the aftertaste performance of red
wine and offset part of the influence of low temperature on aroma and
taste.
4. Conclusions
This study investigated the effects of combined ultrasound and low
temperature pretreatment on the quality of dry red wine. The results
showed that the effect of combined ultrasound and low temperature
pretreatment on the fermentation process was mainly to increase the
initial specific gravity and sugar concentration of the must. Combined
pretreatment significantly increased the content of anthocyanins and
phenolic acids while increasing the TPC, TAC, and TFC, which further
affected the color of the wine and significantly improved the antioxi­
dants. Furthermore, combined treatment affected the composition of
volatile substances, thus affecting the aroma of the wine and reducing
the generation of undesirable odors. Low temperature pretreatment
improved the fruit and flower aroma of the wine, and combined ultra­
sound pretreatment offset the green taste induced by low temperature.
In the sensory aspect, combined pretreatment contributed to improving
the quality of the aftertaste. Pretreatment with 240 W ultrasound
combined with low temperature increased the content of anthocyanins
and phenols in wine and improved the aroma, thus demonstrating
excellent application prospects.
CRediT authorship contribution statement
Qi Xie: Writing – original draft, Visualization, Formal analysis.
Yurou Tang: Investigation, Data curation. Xueyan Wu: Investigation,
Data curation. Qingyan Luo: Investigation, Data curation. Wentong
Zhang: Investigation, Data curation. Hanyang Liu: Investigation, Data

8
Q. Xie et al. Ultrasonics Sonochemistry 100 (2023) 106636

Fig. 4. Effects of ultrasonic combined with low temperature pretreatment on volatile substances of Merlot wine. (A): Aroma substance heat map, (B): scores plot of
PCA results for the reference samples of different treatment group. (C): loadings plot of PCA results for the reference samples of different treatment group. CK: No-low
temperature pretreatment, U120: 120 W ultrasound treatment, U240: 240 W ultrasound treatment, U400: 400 W ultrasonic treatment, LT: low temperature pre­
treatment, LT + U120: low temperature pretreatment and 120 W ultrasound treatment, LT + U240: low temperature pretreatment and 240 W ultrasound treatment,
LT + U400; low temperature pretreatment and 400 W ultrasound treatment.

curation. Yulin Fang: Writing – review & editing. Xiaofeng Yue:

Conceptualization, Resources. Yanlun Ju: Supervision.

Declaration of Competing Interest

The authors declare that they have no known competing financial

interests or personal relationships that could have appeared to influence
the work reported in this paper.

Acknowledgments

This study was supported by the Science and Technology Develop­

Fig. 5. Effects of ultrasonic combined with low temperature pretreatment on
sense of Merlot wine. CK: No-low temperature pretreatment, U120: 120 W ul­
trasound treatment, U240: 240 W ultrasound treatment, U400: 400 W ultra­
sonic treatment, LT: low temperature pretreatment, LT + U120: low
temperature pretreatment and 120 W ultrasound treatment, LT + U240: low
temperature pretreatment and 240 W ultrasound treatment, LT + U400; low
temperature pretreatment and 400 W ultrasound treatment.
ment Plan Project of Shaanxi Province (2023-YBNY-163, 2023KXJ-008,
2023-ZDLNY-23); Huailai County Science and Technology Support Plan
Project (2021C-14); College Students’ Innovative Entrepreneurial
Training Plan Program (202310712181); Shaanxi Provincial Innovation
Capability Support Plan (2020TD-047); Xianyang Qinchuangyuan Sci­
ence and Technology Innovation Project (L2022-QCYZX-NY-008).
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