LWT - Food Science and Technology 154 (2022) 112625

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LWT
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Effects of different thermal treatment temperatures on volatile flavour

compounds of water-boiled salted duck after packaging
Qiusheng Xie a, Baocai Xu b, Ying Xu a, Zhong Yao a, Benwei Zhu a, Xinfu Li a, Yun Sun a, *
a
College of Food Science and Light Industry, Nanjing Tech University, Nanjing, 211816, China
b
School of Food and Biological Engineering, Hefei University of Technology, Hefei, 230009, China

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

Keywords: The aim of this study was to assess the effects of different thermal treatment temperatures on volatile com­
Water-boiled salted duck pounds, lipid oxidation, and the Maillard reaction in water-boiled salted duck. A total of 38 flavour compounds
Thermal treatment were detected, mainly including aldehydes, ketones, alcohols, esters, and furans. The contents of aldehydes,
GC-IMS
ketones, and furans in duck were significantly increased, while the contents of some alcohols and esters were
Lipid oxidation
Maillard reaction
decreased after high-temperature, high-pressure sterilisation (121 ◦ C, 20 min). Low-temperature heat treatment
(85 ◦ C, 50 min; 95 ◦ C, 40 min) had relatively little effect on the flavour of water-boiled salted duck. Thermal
treatment significantly promoted the oxidative decomposition of unsaturated fatty acids. Monounsaturated fatty
acids may play a key role in the formation of aldehydes and ketones. The Maillard browning was low, and the
increase therein remained small after thermal treatment. The study showed that low-temperature heat treatment
could better control changes in flavour.

1. Introduction
Water-boiled salted duck is a traditional Chinese low-temperature
meat product, famous for its tender texture, delicious taste, and
unique flavour. Volatile flavour indices are one of the more important
indicators used to evaluate the quality of cooked duck meat. Liu, Xu, and
Zhou (2007) investigated the changes in volatile compounds in
water-boiled salted duck during processing and found that the compo­
sition and amounts of volatile compounds were affected by treatment
processes such as dry-curing, brining, and boiling.
Researchers believe that flavour precursors mainly include amino
acids, peptides, sugars, and lipids (Khan, Jo, & Tariq, 2015; Mottram &
Edwards, 1983), and processing causes complex chemical reactions
between flavour precursors to produce rich volatile aroma substances.
Some authors suggest that lipid oxidation, Maillard reaction-Strecker
degradation, Maillard reaction products and lipid oxidation reaction,
and thermal degradation of thiamine and microbial metabolism are the
main pathways for the formation of volatile flavour compounds in meat
(Flores, 2018). The most important pathways in the formation of volatile
flavour compounds in meat are lipid oxidation and Maillard reaction.
Lipid oxidation mainly entails oxidation of lipid acyl chains. Liu, Xu,
Ouyang, and Zhou (2006) believed that the main volatile compounds
imparting duck meat flavour come from fatty acid degradation. Lipid
oxidation can produce lipid-derived compounds such as aldehydes, ke­
tones, acids, hydrocarbons, lactones, and furans. Kim, Cadwallader,
Kido, and Watanabe (2013) found that 1-octene-3-one, hexanal, octanal,
nonanal, (Z)-4-heptanal, (Z)-2-nonenal, etc. Are common lipid oxidation
volatiles found in meat products. Maillard reaction, or the carbonyl
ammonium reaction, is one of the most important ways of heating food
to produce flavour. Whitfield (1992) found that volatile compounds in
meat products are related to Maillard reaction, and heterocyclic com­
pounds containing nitrogen, oxygen, and sulphur with long chain alkyl
substituents may be synthesised by Maillard reaction products and al­
dehydes degraded by lipids. Jayasena, Ahn, Nam, and Jo (2019)
believed that the flavour of cooked chicken is thermally derived through
Maillard reaction, lipid degradation and the interaction between these
two reactions, and thermal treatment has an important effect on the
flavour of cooked chicken.
In the commercial processing of water-boiled salted duck, some
microorganisms remain in-situ (Liu, Wang, Du, Zhu, & Xu, 2010) and
re-infection during packaging will have harmful effects on the colour,
flavour, and food safety of meat products. Therefore, thermal treatment
is widely applied after packaging to ensure food safety and prolong the
shelf-life of water-boiled salted duck. Thermal treatment generally

* Corresponding author.
E-mail address: yunsunny012@163.com (Y. Sun).

https://doi.org/10.1016/j.lwt.2021.112625
Received 17 July 2021; Received in revised form 9 September 2021; Accepted 12 October 2021
Available online 14 October 2021
0023-6438/© 2021 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Q. Xie et al.
includes high-temperature sterilisation, for example at 121 ◦ C, and
low-temperature heat treatment, such as pasteurisation. 85 ◦ C is the
commonly used Pasteurisation temperature, which is regarded as the
key method of meat preservation (Lyng, Clemente, & McKenna, 2019).
And the 85 ◦ C thermal treatment is one of the sterilisation processes
commonly used by water-boiled salted duck manufacturers. Commercial
sterilisation can prolong the shelf life of meat products, but the steri­
lisation temperature has an impact on the nutrients, texture and flavour
of meat products. Although some water-boiled salted ducks on the
market have a long shelf life, but the sensory quality of the products has
changed. (Chen, 2008; Liu et al., 2010). Wang et al. (2020) reported that
heat treatment at 95 ◦ C can be developed as one potential thermal
treatment temperature for Dezhou-braised chicken due to its positive
effects on maintaining fresh odour and texture together with its
extending the shelf life while also protecting food safety.
As far as we know, few researchers have studied the effect of heat
treatment after packaging on the volatile flavour of water-boiled salted
duck. Therefore, in this study, the volatile flavour compounds of water-
boiled salted duck treated with different heat treatment temperatures
(85 ◦ C, 95 ◦ C, and 121 ◦ C) were analyzed and the lipid oxidation, free
fatty acids, and Maillard reaction related to the formation of volatile
compounds were investigated.
2. Materials and methods
2.1. Materials
A total of 12 duck legs were required for the experiment. The duck
legs used to make water-boiled salted duck were purchased from the
same local supermarket, and cold chain transportation was used
throughout. After the samples arrived at the laboratory, the raw duck
legs were stored at − 18 ◦ C. All the chemicals used in this study were of
analytical grade or chromatographic grade.
2.2. Sample production and thermal treatment
The main process points of water-boiled salted duck include pre-
treatment, salting (marinating with 8% by weight of duck legs for 4
h), marinating (soaking in brine for 3 h), and boiling (95 ◦ C, 45 min).
After cooking, cool the water-boiled salted duck to room temperature,
and then vacuum packaging (to 0.06 MPa). After vacuum packaging, the
samples were divided into four groups, the first group was the control
check, and no thermal treatment was applied thereto; the thermal
treatment temperature applied to the second group was 85 ◦ C, 50 min;
the third group was treated at 95 ◦ C, 40 min; the fourth group at 121 ◦ C,
20 min. All treated samples were rapidly cooled with cold water and
stored at − 18 ◦ C until analysis.
2.3. E-nose
The E-nose system (FOX4000, France) was used to investigate the
odour characteristics of the muscle tissue of water-boiled salted ducks.
The E-nose system was equipped with data processing software (Alpha
soft) and 18 metal sensors. Each sensor corresponded to a specific sen­
sitive substance.
After cutting the muscle part of duck meat into minced meat, 3 g
duck meat was accurately weighed in the headspace bottle dedicated to
such testing. The analysis parameters of E-nose included: head space
heating temperature 70 ◦ C, heating time 200 s, delay acquisition time
600 s, data acquisition time 120 s, acquisition cycle 1.0 s; the carrier gas
was high-purity air at a flow rate of 150 mL/min, using an injection
volume of 500 μL at an injection rate of 500 μL/s.
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LWT 154 (2022) 112625
2.4. Headspace gas chromatography-ion mobility spectrometer (HS-GC-
IMS)
A gas chromatography-ion mobility spectrometer ((GC-IMS), Fla­
vourspec, G.A.S. Instrument, Germany) was used to detect volatile
compounds in water-boiled salted duck legs. The instrument was
equipped with an automatic headspace sampling system and a gas
phase-ion mobility spectrometry system. The muscle of duck leg was
minced, 2 g sample was weighed and placed in 20 mL headspace bottle,
incubated at 60 ◦ C and 500 rpm for 15 min. After incubation, the system
automatically injected 500 μL of headspace sample into the injection
needle (at 65 ◦ C). The sample was automatically injected into the gas
chromatograph by the injection needle and separated by the mxt-5
capillary column (15 m × 0.53 mm). The column temperature was
kept at 60 ◦ C with high-purity nitrogen used as the carrier gas at a flow
rate of 2 mL/min in the first 2 min of the program, and then increased to
100 mL/min after 2 min (Duan, Dong, Sun, Dong, & Gao, 2021). The
total operation time was 20 min. After chromatographic separation, the
compounds were fed into a drift tube at 45 ◦ C. High-purity nitrogen was
used as the drift gas to detect ion migration at a rate of 150 mL/min.The
retention index (RI) of volatile organic compounds (VOCs) was calcu­
lated with reference to n-ketone C4–C9 (Sinopharm Chemical Reagent
Beijing Co., Ltd, Beijing, China). VOCs were identified in the GC–IMS
library by comparing the RI and drift time. The intensities of VOCs were
based on the peak volume of the selected signal peak by Gallery Plot
analysis.
2.5. Thiobarbituric acid reactive substance (TBARS)
We weighed 5 g of minced duck meat and added 50 mL of 7.5%
trichloroacetic acid (containing 0.1% EDTA), the shaking table was run
at 130 rpm for 30 min: the minced duck meat was then filtered using
double-layer filter paper, 5 mL of filter solution was transferred into a
centrifuge tube, and 5 mL (at 0.02 mol/L) of 2-thiobarbituric acid so­
lution added. The specimens were kept in a covered water bath at 80 ◦ C
for 40 min, cooled to room temperature, 2 mL chloroform was added and
the specimens were shaken, which was allowed to stratify, then the
supernatant was taken for colorimetric analysis at wavelengths of 532
nm and 600 nm (Xia et al., 2021). TBARs were calculated according to
the formula:
(A532 − A600 ) × V × VV21 × 72.06 × 100
TBARs (mg/100g) =
155000 × m
A532, A600 - The absorbance measured at 532 nm and 600 nm
wavelengths respectively.
V - total amount of reaction solution (mL), V1 - The amount of
malondialdehyde extraction solution in the reaction solution (mL), V2 -
total amount of extraction solution (mL), 155000 - Molar extinction
coefficient (L/(mol•cm)),
72.06 - Molecular weight of malondialdehyde,
m - the mass of the sample (g).
2.6. Free fatty acids
Taking 20 g leg muscle sample, added 60 mL chloroform methanol
(2:1, v/v), homogenised at 100 rpm for 30 min, allowing the specimens
to then stand for 1 h, filtered the slurry and then added 10 mL normal
saline (7.3 g/L NaCl, 0.5 g/L). After centrifugation at 3000 rpm for 15
min, the lower liquid was retained. The organic solvent was evaporated
to dryness by rotary steamer in water bath at 44 ◦ C to obtain light-yellow
pure fat. 20 mg lipid was then weighed and 1 mL chloroform was added
to dissolve the lipid. First, the dissolved lipid chloroform mixed solution
was transferred to the activated aminopropyl silica gel column, and then
2 mL chloroform isopropanol solution (2:1, v/v) was added to elute the
column, and the eluent was discarded. 3 mL Acetic acid-ether solution
Q. Xie et al.
(1:49, w/w) was added to elute free fatty acids, and collected the eluate
(Monin, Hortos, Diaz, Rock, & Garcia-Regueiro, 2003). The solvent in
the sample was dried by nitrogen-blowing, 2 mL of 14% boron tri­
fluoride methanol (w/w) solution and 0.5 mL of 2,2-dimethoxypropane
were added for methyl esterification, and the temperature was kept at
60 ◦ C for 30 min. After cooling, 1 mL distilled water and 1 mL n-hexane
were added to the mixture. After standing to allow stratification, the
upper organic layer was collected. 1 mL of 0.5 mg/mL methyl hepta­
decanoate was added as an internal standard. Nitrogen was used to
blow-dry the solvent. Finally, 1 mL n-hexane was added to fix the vol­
ume for gas chromatographic analysis.
The gas chromatograph (Agilent 7890b) was equipped with an SP-
2560 capillary column (100 m × 0.25 mm × 0.20 μm). High-purity
Fig. 1. E-nose analysis. A: The radar fingerprint of duck samples treated with different thermal treatment temperatures; B: Principal component analysis of char­
acteristic flavour of duck samples after thermal treatment.
3
LWT 154 (2022) 112625
nitrogen was used as the carrier gas, the injection volume was 1 μL at
a flow rate of 1 mL/min, the split ratio was 25:1, the injection port
temperature was 200 ◦ C, and the FID detector temperature was 300 ◦ C.
The temperature was changed thus: the initial column temperature was
kept at 100 ◦ C for 1 min, then increased at 10 ◦ C/min to 180 ◦ C for 5
min, then increased at 1 ◦ C/min to 200 ◦ C for 5 min, and then increased
at 10 ◦ C/min to 230 ◦ C for 16 min.
Qualitative analysis was performed by comparing the peak retention
time of mixed standard samples of 37 different fatty acids; according to
the peak area of the internal standard (0.4 mg/mL methyl heptadeca­
noate), the free fatty acid was quantitatively analyzed.
Q. Xie et al. LWT 154 (2022) 112625

2.7. Degree of Maillard reaction 50 min), and A3 (95 ◦ C, 40 min) three groups of samples were more
closely distributed, and the characteristic flavour composition was
We weighed 3 g samples and homogenised them with 10 mL of pre- similar; however, the samples of group A4 (121 ◦ C, 20 min) were
cooled deionised water. Then 10 mL of pre-cooled 20% (v/v) TCA so­ distributed in the fourth quadrant and far away from the other three
lution was mixed with the homogenate. The mixture was centrifuged at groups, indicating that the volatile flavour of the samples changed
4 ◦ C for 10 min at 7000 rpm, and the supernatant was filtered using filter significantly.
paper. The browning intensity was determined by measuring the
absorbance at a wavelength of 420 nm of the extract (Geng et al., 2019). 3.2. Determination of volatile compounds by HS-GC-IMS
The content of Maillard intermediates was determined by measuring the
absorbance at 294 nm. The fluorescence intensity was measured at GC-IMS was used to explore the flavour of the muscle tissue of water-
excitation and emission wavelengths of 370 nm and 440 nm. boiled salted duck after thermal treatment, and the two-dimensional
spectra of the volatile compounds therein were obtained (Fig. 2A).
2.8. Statistical analysis The colour point distribution contours of the four groups of samples in
Fig. 2A were similar, and the types of volatile compounds of the water-
All the data were processed using SPSS 23.0 software, and the data boiled salted ducks treated at different temperatures were similar.
presented in the form of mean ± standard deviation. SPSS 23.0 software Taking group A1 (ck) as the model, the variations of flavour compounds
was used to conduct one-way ANOVA tests and Waller-Duncan homo­ were evaluated by differential analysis (Fig. 2B); with the increase in
geneity tests to determine the significance of differences between sam­ thermal treatment temperature, the content of some compounds with
ples (P < 0.05). PCA analysis was performed with Simca-p 13.0 relative DT of 0–1.0 decreased; the content of some compounds with
software. SPSS 23.0 and Origin 2019b were used for correlation analysis relative DT of 1.0–1.8 increased. After the packaged water-boiled salted
and visualisation of any differences between samples. ducks were thermal treated, compared with the 85 ◦ C treatment group,
some signal response values in the 95 ◦ C treatment group were slightly
higher, but the change was smaller than that of the 121 ◦ C treatment
3. Results and discussion
group. The flavour compounds of water-boiled salted duck treated at
121 ◦ C for 20 min underwent the most significant change. This phe­
3.1. Analysis of E-nose data
nomenon indicated that the temperature of thermal treatment after
packaging of meat products has an impact on the flavour of the product.
It can be seen from the radar fingerprint (Fig. 1A) that the charac­
The medium and low temperature conditions below 100 ◦ C may be more
teristic flavour of water-boiled salted duck changed after thermal
conducive to ensuring the stability of the product’s flavour. The Gallery
treatment. The main volatile compounds in water-boiled salted duck
Plot plug-in was used to generate the fingerprint (Fig. 2C) of the volatile
were detected by P30/2, P40/2, P30/1, PA/2, T70/2, and T30/1 sen­
compounds of the water-boiled salted duck. Each column in the figure
sors. The difference of volatile compounds among different products was
represented a monomer or dimer of a substance. It can be seen from the
mainly concentrated in sensors P30/2, PA/2, T70/2, and T30/1. Ac­
figure that 38 volatile compounds (including monomers and dimers)
cording to Table 1, the main compounds of water-boiled salted duck
were identified in water-boiled salted duck samples (19 aldehydes, 5
flavour included hydrocarbons, ammonia, hydrogen sulphide, fluorines,
ketones, 8 alcohols, 5 esters, and 1 furan, (Table 2).
ketones, and other polar compounds, while thermal treatment resulted
The main volatile compounds in water-boiled salted duck were al­
in significant changes in hydrocarbons, benzene, ammonia, ketones, and
dehydes, and a total of 19 aldehydes (including dimers) were detected.
other polar compounds in duck flavour.
Aldehydes are the main products of lipid oxidation and amino acid
The further to analyse the difference of flavour characteristics of
degradation (Wu & Wang, 2019) and because the odour threshold of
salted duck samples after thermal treatment, the response value signals
aldehydes is low, aldehydes are considered as important compounds of
of duck samples were analyzed by PCA (Fig. 1B); the total contributions
characteristic flavour of duck meat and other meat products. It is
of the first principal component PC1 and the second principal compo­
generally believed that straight-chain aldehydes come from the oxida­
nent PC2 reached 85.2% (65.5% and 19.7%, respectively), which could
tive degradation of unsaturated fatty acids (Zeng, Xia, Jiang, Xu, & Fan,
reflect the overall information pertaining to the sample. According to
2017). After thermal treatment of water-boiled salted duck, the content
the distribution of sample points, it can be seen that A1 (ck), A2 (85 ◦ C,
of straight-chain aldehydes tended to increase, especially at 121 ◦ C
where the accumulation of volatile aldehydes was the highest. Hexanal
Table 1
dominated among those aldehydes present. At low concentration,
The E-nose sensor and its corresponding sensitive substance types.
hexanal imparts a grassy flavour, while at high concentrations, it will
Number Sensor Types of sensitive substances produce an oily rancidity (Duan et al., 2021). Pentanal, heptanal,
name
octanal, and nonanal are respectively described as imparting almond
1 LY2/LG Chlorine, fluorine, nitrous compounds, sulfides flavour, meat flavour, flower flavour, and wax flavour (Chmiel et al.,
2 LY2/G Ammonia, amine compounds, carbon and oxygen
2020) and these are derived from the oxidation of oleic acid. The
compounds
3 LY2/AA Ethanol, acetone, ammonia amounts of branched chain aldehydes, including 2-methylbutyralde­
4 LY2/GH Ammonia, amine compounds hyde and 3-methylbutyraldehyde, also increased significantly (P <
5 LY2/gCT1 hydrogen sulfide 0.05) after sterilisation. Branched chain aldehydes were mainly pro­
6 LY2/gCT Propane, butane duced by oxidative deamination and decarboxylation of amino acids
7 T30/1 Polar compounds, hydrogen chloride
8 P10/1 Nonpolar, hydrocarbon, ammonia, chlorine
(especially valine, isoleucine, and leucine) (Bruna, Fernandez, Hierro,
9 P10/2 Nonpolar, Methane, ethane Ordonez, & De la Hoz, 2000) through the Strecker degradation pathway
10 P40/1 Chlorine, fluorine (Liu et al., 2020). 2-Methylbutyraldehyde and 3-methylbutyraldehyde
11 T70/2 Toluene, xylene, carbon monoxide impart cheese and nutty flavours, respectively, and were mainly pro­
12 PA/2 Ethanol, ammonia, amine compounds
duced by leucine amino acid and isoleucine as formed by Strecker
13 P30/1 Hydrocarbons, ammonia, ethanol
14 P40/2 Chlorine, hydrogen sulfide, fluoride degradation pathway and biosynthesis pathway (Ding et al., 2020).
15 P30/2 Hydrogen sulfide, ketone Benzaldehyde was the only aromatic aldehyde detected in water-boiled
16 T40/2 Chlorine salted duck samples, with almond and nut flavour arising therefrom; this
17 T40/1 Fluorine was generated by Strecker degradation of phenylalanine or a linolenic
18 TA/2 Ethanol
acid oxidation pathway (Duan et al., 2021; Ding et al., 2020). The

4
Q. Xie et al. LWT 154 (2022) 112625

Fig. 2. GC-IMS analysis. A: Two-dimensional spectrogram of volatile compounds. The vertical red line represents the reactive ion peak (RIP) normalized to the drift
time (DT). Each point on the graph represents a volatile compound. The color of the dot represents the concentration of the substance, white represents low con­
centration, and red represents high concentration; B: Differential spectrogram of volatile compounds. The color of the dot represents the concentration of the
substance, white indicates the same concentration, blue indicates low concentration, and red indicates high concentration; C: Fingerprint of volatile compounds. Four
different thermal treatments: A1 (ck), A2 (85 ◦ C, 50 min), A3 (95 ◦ C, 40 min), A4 (121 ◦ C, 20 min). (For interpretation of the references to colour in this figure
legend, the reader is referred to the Web version of this article.)

5
Q. Xie et al.
Fig. 3. Correlation analysis of volatile compounds and free fatty acids in water-boiled salted duck: (red indicates positive correlation, green shows negative cor­
relation, and the deeper the colour, the greater the absolute value of correlation, the stronger the correlation between them. The asterisk indicates a significant
difference: *P < 0.05, **P < 0.01). (For interpretation of the references to colour in this figure legend, the reader is referred to the Web version of this article.)
content of unsaturated aldehydes was lower than that of saturated al­
dehydes, but the overall increasing trend was similar. The sources of
unsaturated aldehydes and straight-chain aldehydes were homologous.
It was generally believed that they were mainly derived from the
decomposition of peroxide formed by the oxidation of unsaturated fatty
acids (Liu et al., 2020). Chang, Wu, Zhang, Jin, and Wang (2020) found
that unsaturated aldehydes were related to changes in the content of
linoleic acid.
The main ketones detected in water-boiled salted duck were 2-buta­
none, 2-pentanone, and 2-heptanone. The characteristic flavour of these
ketones is usually described as imparting a creamy flavour and a cheese
flavour. Ketones in meat products usually come from the automatic
oxidation of lipids (Arief, Afiyah, Wulandari, & Budiman, 2016), and
may also be formed via the lipid decomposition pathway during
fermentation. After thermal treatment, the contents of 2-butanone,
2-pentanone, and 2-heptanone in duck showed an overall upward
trend, but there was no significant difference between 85 ◦ C group and
95 ◦ C group (P > 0.05), and the 121 ◦ C group had the highest ketone
content. It was noteworthy that ketones, as carbonyl compounds, may
react with amino acids, peptides, proteins, and other substances,
resulting in a reduction in the content thereof (Duan et al., 2021). This
may be the reason why the content of 2-heptanone in water-boiled salted
duck in specimens in group A4 (121 ◦ C, 20 min) after high-temperature
sterilisation did not increase significantly compared with other groups
(P > 0.05).
Alcohols are also considered as important flavour compounds in
cooked duck meat (He et al., 2020), especially aliphatic alcohols that
6
LWT 154 (2022) 112625
make a significant contribution to flavour formation in meat products
(Cai et al., 2020). The lipid oxidation pathway will lead to the formation
of linear alcohols, which is the reason for the increase in the content of
pentanol and hexanol. Branched-chain alcohols generally come from the
decomposition of branched aldehydes, and in this experiment, the
content of branched-chain alcohols was low, and changes therein were
negligible. Ethanol was the dominant alcohol detected in water-boiled
salted duck, which may come from adding a certain amount of rice
wine during the re-brining process. Hexanol and 1-octen-3-ol were the
most important alcohols in the formation of characteristic flavour of
salted duck. Hexanol is related to the oxidative degradation of oleic acid.
1-octen-3-ol is produced by lipase-catalysed reaction and oxidative
decomposition of unsaturated polyunsaturated fatty acids (such as
arachidonic acid). The content of both substances increased significantly
after thermal treatment (P < 0.05). It was particularly important to note
that it is one of the factors deemed to produce a peculiar smell due to the
low threshold of 1-octen-3-ol (Iglesias et al., 2009).
Esters are common in fermented foods, such as soy sauce, rice wine
and ham, mainly including ethyl ester and acetate (Gao, Xia, Li, & Liu,
2019). Some ethyl esters in water-boiled salted duck may come from the
rice wine added in the production process. Their low odour threshold
allows these esters to impart the characteristic odour of fruit and flowers
(Liu et al., 2019). The esters in meat products are formed by esterifi­
cation of carboxylic acid and alcohol. Table 2 displays that the content of
ethyl formate tended to be stable throughout, ethyl acetate and propyl
acetate decreased significantly (P < 0.05), which indicated that the
degree of esterification was mild. 2-pentylfuran imparted a potato
Q. Xie et al. LWT 154 (2022) 112625

Table 2
The evolution of volatile compounds in water-boiled salted duck after secondary sterilisation.
No. Compound MW RI RT (s) DT (a.u.) Volumn (a.u)

A1 A2 A3 A4

1 Butanal 72.1 564.4 125.529 1.28899 290.58 ± 169.69b 358.51 ± 88.68b 321.65 ± 50.76b 698.26 ± 77.60a
2 Pentanal-M 86.1 702.8 165.756 1.18185 1129.06 ± 10.70b 1144.23 ± 20.40 ab 1148.53 ± 21.74 ab 1176.44 ± 19.45a
3 Pentanal-D 86.1 698.3 163.917 1.42973 3962.51 ± 330.02a 4131.07 ± 143.54a 4042.09 ± 27.26a 4061.59 ± 150.19a
4 Hexanal-M 100.2 797.4 206.493 1.25535 1310.00 ± 31.83a 1168.35 ± 43.54b 1193.37 ± 47.49b 1182.07 ± 2.81b
5 Hexanal-D 100.2 797 206.302 1.57369 7871.32 ± 477.82b 8505.83 ± 39.17b 8497.33 ± 80.30b 8585.22 ± 49.05a
6 Heptanal-M 114.2 905.8 266.379 1.3289 1348.13 ± 84.36a 1322.35 ± 35.67a 1382.74 ± 33.28a 1359.72 ± 23.89a
7 Heptanal-D 114.2 905.3 265.998 1.70499 978.60 ± 223.07b 1180.13 ± 37.06 ab 1259.97 ± 50.24a 1256.03 ± 107.75a
8 Octanal-M 128.2 1010 363.638 1.40265 1252.13 ± 218.55b 1618.46 ± 111.75a 1588.29 ± 144.45a 1665.93 ± 33.01a
9 Octanal-D 128.2 1008.4 361.024 1.83021 312.50 ± 110.50b 565.31 ± 68.78a 531.60 ± 110.67a 610.41 ± 91.45a
10 Nonanal-M 142.2 1098.9 512.197 1.47489 1260.31 ± 196.52b 1647.46 ± 198.81 ab 1698.57 ± 220.74a 1942.99 ± 213.38a
11 Nonanal-D 142.2 1098.9 512.197 1.95125 89.46 ± 19.6b 129.44 ± 30.2 ab 140.92 ± 32.20 ab 186.77 ± 50.12a
12 2-Methylbutyraldehyde-M 86.1 670.8 154.933 1.16005 999.03 ± 50.27b 1148.00 ± 53.28a 1250.57 ± 21.45a 1267.66 ± 96.52a
13 3-Methylbutyraldehyde-D 86.1 651.8 149.682 1.17395 854.38 ± 35.93b 1050.04 ± 89.30b 1050.16 ± 40.82b 1117.68 ± 78.83a
14 (E)-2-Pentenal 84.1 753.4 186.849 1.1068 43.89 ± 4.44b 50.99 ± 6.94b 49.75 ± 4.93b 66.64 ± 7.86a
15 (E)-2-Hexenal 98.1 853.8 235.482 1.18505 61.11 ± 7.32b 59.16 ± 6.40b 56.02 ± 2.15b 83.39 ± 10.24a
16 (E)-2-Heptenal 112.2 959.3 310.488 1.25818 166.56 ± 21.84b 205.53 ± 23.77 ab 203.26 ± 14.16 ab 248.36 ± 36.47a
17 (E)-2-Octenal 126.2 1052 433.779 1.33823 143.29 ± 24.21c 184.98 ± 18.90b 168.99 ± 4.00bc 261.94 ± 25.88a
18 Benzaldehyde-M 106.1 965.7 315.715 1.15276 692.61 ± 196.47b 800.94 ± 52.52 ab 791.45 ± 78.86 ab 1003.30 ± 66.16a
19 Benzaldehyde-D 106.1 965.7 315.715 1.47684 199.60 ± 99.60b 270.00 ± 35.51b 250.07 ± 51.67b 411.74 ± 57.62a
20 2-Butanone 72.1 592.9 133.405 1.25116 4764.66 ± 809.15b 5462.98 ± 339.34b 5607.44 ± 341.07b 7366.18 ± 329.50a
21 2-Pentanone-M 86.1 686.6 159.307 1.12354 82.61 ± 3.01b 66.02 ± 2.27c 84.33 ± 5.86b 101.62 ± 8.69a
22 2-Pentanone-D 86.1 693.7 161.967 1.63736 400.68 ± 10.41c 427.55 ± 27.76bc 517.85 ± 22.28 ab 613.15 ± 89.41a
23 2-Heptanone-M 114.2 896.7 258.941 1.2616 523.28 ± 103.97b 725.51 ± 6.25a 734.96 ± 50.91a 756.16 ± 17.21a
24 2-Heptanone-D 114.2 895.4 257.797 1.63736 130.14 ± 53.06b 319.23 ± 65.79a 294.96 ± 71.71a 301.87 ± 31.08a
25 Ethanol 46.1 464.1 97.777 1.04941 2972.67 ± 265.87a 2943.44 ± 15.62a 2259.86 ± 45.63b 2189.67 ± 24.48b
26 2-Propanol 60.1 495.4 106.445 1.09127 419.29 ± 45.24a 388.60 ± 31.81a 432.04 ± 16.29a 424.45 ± 29.28a
27 1-Pentanol-M 88.1 770.8 194.096 1.2527 968.39 ± 48.64b 1116.71 ± 23.84a 1104.63 ± 9.89a 1091.78 ± 20.25a
28 1-Pentanol-D 88.1 768.9 193.333 1.5087 415.50 ± 64.11b 786.91 ± 63.48a 686.80 ± 39.44a 686.23 ± 64.62a
29 1-Hexanol 102.2 877.2 247.498 1.32433 69.32 ± 1.22b 113.49 ± 17.66a 94.16 ± 7.35a 105.36 ± 14.62a
30 3-Methyl-1-butanol 88.1 737 180.022 1.24229 144.27 ± 23.45a 117.72 ± 5.44 ab 126.67 ± 24.59 ab 97.73 ± 2.43b
31 2-Methyl-1-butanol 88.1 737.6 180.283 1.22859 31.50 ± 3.61a 25.46 ± 0.58a 31.19 ± 2.29a 28.62 ± 4.30a
32 1-Octen-3-ol 128.2 992.1 337.498 1.16642 593.30 ± 103.65b 937.91 ± 46.38a 832.00 ± 86.53a 840.91 ± 54.80a
33 Ethyl formate 74.1 499.2 107.494 1.07253 551.11 ± 228.46a 607.98 ± 97.50a 349.85 ± 19.27a 388.19 ± 103.83a
34 Ethyl acetate -M 88.1 625.2 142.331 1.09982 350.63 ± 21.10a 310.58 ± 25.02b 261.72 ± 13.78c 204.28 ± 16.19d
35 Ethyl acetate -D 88.1 619.5 140.756 1.34304 801.62 ± 85.65a 718.84 ± 23.16a 550.73 ± 46.86b 341.75 ± 30.82c
36 Propyl acetate -M 102.1 718.8 172.449 1.16191 167.81 ± 9.34a 152.62 ± 6.45 ab 160.75 ± 6.30 ab 144.16 ± 11.37b
37 Propyl acetate -D 102.1 710.4 168.937 1.48095 59.91 ± 15.87c 104.79 ± 13.35b 184.03 ± 1.72a 134.49 ± 23.52b
38 2-Pentylfuran 138.2 1000.6 347.954 1.25818 193.89 ± 68.78b 229.45 ± 28.66 ab 194.12 ± 25.82b 313.79 ± 50.00a

Values represent the mean ± SD (n = 3). a, b, c means in the same row without common letters are significantly different at P < 0.05. Four different thermal treatments:
A1 (ck), A2 (85 ◦ C, 50 min), A3 (95 ◦ C, 40 min), and A4 (121 ◦ C, 20 min). MW: molecular weight; RI: retention index; RT: retention time; DT: drift time; volume (a.u.):
peak volume.

aroma and was the only furan derivative detected in water-boiled salted
duck. It is often considered to be the oxidation product of ω-6 poly­
unsaturated fatty acids. However, due to its low content and high odour
threshold (Zhao, Shen, Guo, Wu, & Dai, 2016), so it was considered that
2-pentylfuran was unlikely to play a significant role in formation of
flavour in water-boiled salted duck in this experiment.
3.3. Changes of TBARs in water-boiled salted duck
Lipid oxidation plays a vital role in the flavour formation of meat
products (Xia et al., 2021). It can be seen from Fig. 4A that, compared to
specimens in control group A1 (ck), the TBARs value of the water-boiled
salted duck under the thermal treatment conditions of A2 (85 ◦ C, 50
min) and A3 (95 ◦ C, 40 min) showed a significant increasing trend (P <
0.05), and the TBARs value of the 95 ◦ C group was higher than that of
the 85 ◦ C group, indicating that the thermal treatment process signifi­
cantly increased the degree of lipid oxidation (P < 0.05). However, it
was found that, under the conditions applied to specimens in group A4
(121 ◦ C, 20 min), the TBARs value in the duck muscle tissue had
decreased significantly (P < 0.05). The value of TBARs in group A4
decreased, showing that lipid peroxide malondialdehyde (MDA) had
been lost or participated in other biochemical reactions as a substrate.
Roldan, Antequera, Armenteros, and Ruiz (2014) had shown that un­
saturated aldehydes, binary aldehydes, and other active carbonyl com­
pounds produced by fat oxidation can participate in the advanced stage
of the Maillard reaction, and MDA readily reacts with amino compounds
such as protein, phospholipids, and amino acids in meat products, thus
resulting in the loss of MDA and other carbonyl compounds that can
react with TBA, thus reducing the TBARs value: the higher the reaction
temperature, the faster the rate of reaction of MDA with amino com­
pounds. High temperature may promote the formation of aldehydes
with two to four carbons in meat products, and further oxidation to form
organic alcohols and carboxylic acids (Zhang, Jin, Wang, & Zhang,
2011), which may be another reason for the decrease in the TBARs
value. Water-boiled salted ducks lost a large amount of juice under
high-temperature, high-pressure sterilisation, which may also cause loss
of water-soluble carbonyl compounds such as malondialdehyde.
3.4. Analysis of FFA
Free fatty acids are mostly derived from the hydrolysis of tri­
glycerides and phospholipids and are involved in the second part of the
pathway of lipid oxidation to form flavour compounds (Xia et al., 2021).
Free fatty acids are oxidised to generate a large amount of hydroper­
oxides, which combine a variety of decomposition pathways to generate
various volatile compounds and flavour precursors (Huang, Li, Huang,
Li, & Sun, 2014). It can be seen from Table 3 that a total of 18 free fatty
acids were detected in the water-boiled salted duck, including 10 satu­
rated fatty acids, 3 monounsaturated fatty acids and 5 polyunsaturated
fatty acids. The fatty acids in water-boiled salted duck were mainly

7
Q. Xie et al.
Fig. 4. A: Changes of TBARs in water-boiled salted duck after thermal treatment (mg/100 g); B: Browning intensity; C: Maillard intermediate content; D: Fluo­
rescence intensity. B, C, D can reflect the three stages in the Maillard reaction process in water-boiled salted duck leg muscle tissue. a, b, c means in the different samples
without common letters are significantly different at P < 0.05.
saturated fatty acids, accounting for 61% of the total fatty acids
(Table 3). Palmitic acid (C16:0) and stearic acid (C18:0) accounted for
the largest proportion of free fatty acids; Hunter, Zhang, and
Kris-Etherton (2010) suggested that moderate intake of stearic acid may
influence the prevention of cardiovascular disease. While short chain
fatty acids (C < 6) such as butyric acid itself had typical flavour char­
acteristics (Chen et al., 2021).
It can be seen from Table 3 that the composition abundance of free
fatty acids of water-boiled salted duck changed after thermal treatment.
In general, the contents of saturated fatty acids and unsaturated fatty
acids all exhibited a fluctuating downward trend, indicating that ther­
mal treatment promoted the oxidative loss of free fatty acids from duck
leg muscle. The content of monounsaturated fatty acids in 85 ◦ C group
and 95 ◦ C group was significantly lower than that in the control group
(P < 0.05), but there was no significant change between the two groups,
indicating that thermal treatment has a stronger tendency to oxidative
decomposition for monounsaturated fatty acids in water-boiled salted
ducks. Oleic acid can be oxidised and decomposed when heated to above
80 ◦ C under atmospheric pressure, producing a rancid aroma, which
may be the main reason for the significant decrease in monounsaturated
fatty acid content. It should be noted that the saturated fatty acids,
8
LWT 154 (2022) 112625
monounsaturated fatty acids, and polyunsaturated fatty acids in water-
boiled salted duck were significantly decreased (P < 0.01) under con­
ditions involving sterilisation at 121 ◦ C for 20 min, which indicated that
high temperature could significantly promote the oxidative decompo­
sition of free fatty acids. There was no double-bond structure in satu­
rated fatty acids, and the physical and chemical properties should be
relatively stable, but after autoclaving at 121 ◦ C for 20 min, the content
of palmitic acid (C16:0) and stearic acid (C18:0) also decreased signif­
icantly (P < 0.05).
Free fatty acids are the main precursors of volatile compounds in
meat. In this experiment, the correlation between volatile compounds
and free fatty acids in water-boiled salted duck was assessed, and the
data were visualised (Fig. 3). It was found that aldehydes and ketones
were positively correlated with short-chain saturated fatty acids and
some medium-chain saturated fatty acids (P < 0.05), and negatively
correlated with long-chain saturated fatty acids, monounsaturated fatty
acids, and some polyunsaturated fatty acids (P < 0.05). Aldehydes and
ketones are the main products of fatty acid degradation (Ba et al., 2019),
which are mainly formed by the oxidative decomposition of unsaturated
fatty acids such as oleic acid, linoleic acid, and arachidonic acid. In this
experiment, the correlation distribution of aldehydes and ketones at
Q. Xie et al. LWT 154 (2022) 112625

Table 3 potentially related unsaturated fatty acid of 1-octen-3-ol was γ-linolenic

Contents of free fatty acids in water-boiled salted duck (mean ± SD). acid, and it was negatively correlated with linoleic acid and eicosadie­
No. FFA (mg/kg) A1 A2 A3 A4 noic acid, but not to any significant extent. It may be related to duck raw
materials and the processing techniques adopted (Xia et al., 2021).
1 Butyric acid 0.00 ± 0.00 ± 0.00 ± 143.05 ±
(C4:0) 0.00b 0.00b 0.00b 5.91a Generally, the content of ethyl acetate in soy sauce and cooking wine is
2 Hexanoic acid 89.23 ± 57.47 ± 134.36 ± 102.75 ± relatively high (Shi et al., 2020). This experiment suggested that some
(C6:0) 25.76 ab 3.71b 30.27a 24.82 ab esters in water-boiled salted duck flavour, such as ethyl acetate and
3 Octanoic acid 0.00 ± 0.00 ± 0.00 ± 41.34 ± propyl acetate, mainly came from cooking wine added during the pro­
(C8:0) 0.00b 0.00b 0.00b 31.77a
4 Capric acid 66.16 ± 0.00 ± 120.22 ± 118.79 ±
cess. Esters were mainly formed by esterification of carboxylic acid and
(C10:0) 4.57b 0.00c 26.75a 33.89a alcohol, and there was a significantly negative correlation between
5 Undecanoic acid 28.13 ± 0.00 ± 37.66 ± 21.71 ± propyl acetate and monounsaturated fatty acids (P < 0.05), and there
(C11:0) 9.89 ab 0.00c 3.24a 6.11b was no significant difference therein with polyunsaturated fatty acids (P
6 Lauric acid 61.23 ± 58.32 ± 68.84 ± 66.43 ±
> 0.05). This showed that monounsaturated fatty acids exerted a greater
(C12:0) 12.82a 2.69a 6.72a 7.56a
7 Myristic acid 88.81 ± 73.52 ± 82.74 ± 3.34 ± influence on ethyl acetate than polyunsaturated fatty acids. This result
(C14:0) 17.94a 5.12 ab 3.75a 17.25b was similar to previous findings (Xia et al., 2021).
8 Pentadecanoic 47.02 ± 45.91 ± 46.08 ± 41.15 ±
acid (C15:0) 5.79a 2.43a 7.16a 0.68a
3.5. Maillard reaction of water-boiled salted duck
9 Palmitic acid 4572.24 ± 4434.54 ± 4636.17 ± 3177.58
(C16:0) 13.97b 5.18c 5.74a ± 11.56d
10 Palmitoleic acid 335.88 ± 261.12 ± 380.47 ± 209.98 ± The degree of Maillard reaction before and after thermal treatment of
(C16:1) 68.69a 26.81a 158.40a 131.00a water-boiled salted duck was analyzed by measuring the browning in­
11 Stearic acid 2890.07 ± 2796.43 ± 2931.12 ± 2017.36 tensity, Maillard intermediate content, and fluorescence intensity of the
(C18:0) 10.51b 11.43c 2.64a ± 8.50d
sample. Browning intensity was found to be related to the brown com­
12 Elaidic acid 141.24 ± 131.44 ± 78.82 ± 48.25 ±
(C18:1T) 16.25a 19.12a 26.05b 4.55b pound melanoid in the final stage of Maillard reaction (Luo & Fei, 2019),
13 Oleic acid 2855.63 ± 2502.85 ± 2222.56 ± 911.22 ± which directly reflected the colour of the specimens; the Maillard in­
(C18:1) 44.2a 16.90b 8.83c 8.256d termediate content indicated the amount of colourless intermediate
14 Linoleic acid 1329.73 ± 1262.31 ± 1326.77 ± 326.14 ± products (Luo et al., 2019), such as sugars, aldehydes,
(C18:2) 8.99a 7.62b 2.76a 6.63c
15 γ-Linolenic acid 37.87 ± 29.86 ± 35.27 ± 0.00 ±
low-molecular-weight ketones, etc; the fluorescence intensity indicated
(C18:3) 0.97a 0.10c 0.16b 0.00d the fluorescent compounds produced before the formation of pigments
16 Eicosadienoic 38.22 ± 33.29 ± 38.27 ± 0.00 ± (Geng et al., 2019), which can reflect the early process in the Maillard
acid (C20:2) 9.11a 2.75a 1.40a 0.00d reaction.
17 Arachidonic 144.94 ± 173.56 ± 171.65 ± 33.54 ±
It can be seen from Fig. 4B–D that compared with the control group,
acid (C20:4) 1.17b 6.87a 2.58a 3.20c
18 Docosadienoic 100.70 ± 103.91 ± 142.35 ± 166.64 ± the degree of browning in specimens subjected to thermal treatment
acid (C22:2) 47.36a 20.20a 36.73a 40.67a trended upwards, and the browning intensity after sterilisation at 121 ◦ C
19 SFA 7842.89 ± 7466.18 ± 8057.21 ± 5783.51 for 20 min was the highest, indicating that thermal treatment promoted
65.39b 13.11c 9.15a ± 63.11d the Maillard reaction, leading to the increase in the accumulation of
20 MUFA 3332.75 ± 2895.40 ± 2681.85 ± 1169.46
113.40a 29.95b 140.85b ±
melanoid. However, because no sugars were added in the water-boiled
137.15c salted duck production process, the amount of reactive carbonyl
21 PUFA 1651.46 ± 1602.94 ± 1714.30 ± 526.33 ± groups required for the Maillard reaction was low, so that the Maillard
29.26a 31.81b 35.81a 36.02c reaction in the water-boiled salted duck was low and the amount of
22 Total 12827.10 11964.52 12453.36 7479.29
chromogenic substances was low. The amount of Maillard intermediate
± 133.24a ± 51.42c ± 162.70b ±
154.82d products first decreased, then increased. This change may be related to
the formation and consumption of Maillard intermediate products, such
Four different thermal treatments: A1 (ck), A2 (85 ◦ C, 50 min), A3 (95 ◦ C, 40
as sugars, aldehydes and small molecular ketones (Luo et al., 2019). The
min), and A4 (121 ◦ C, 20 min). SFA: saturated fatty acids; MUFA: mono­
Maillard intermediate product concentration fluctuated in the two re­
unsaturated fatty acids; PUFA: polyunsaturated fatty acids. a, b, c means in the
same row without common letters are significantly different at P < 0.05.
actions of formation and consumption. The reasons for this fluctuation
are complex, and may be the result of the combined effects of Strecker
degradation, sugar degradation, and further participation in the
high temperature exhibited a negative correlation. Oleic acid and lino­
carbonyl ammonium reaction (Nooshkam, Varidi, & Bashash, 2019; Luo
leic acid were the key unsaturated fatty acids that affected the formation
et al., 2019). The fluorescent compounds are mainly formed by the
of aldehydes and ketones. Hexanal, nonanal, and octanal (all with a low
recombination of reducing compounds or the degradation of amino
odour threshold), they were generally considered to come from the
compounds by Strecker degradation pathway in the early stage of the
metabolites of oleic acid and linoleic acid. In the experiment, oleic acid,
Maillard reaction. The fluorescence intensity showed a fluctuating up­
linoleic acid, and γ-linolenic acid were negatively correlated with
ward trend, indicating that high temperature may promote protein
hexanal, nonanal, and octanal (P < 0.05), which was consistent with
degradation to low-molecular-weight peptides and amino acids, and
published data; benzaldehyde, as the only aromatic aldehyde detected in
lipid oxidation to form unsaturated aldehydes and other substances, to
water-boiled salted duck, was negatively correlated with palmitic acid,
participate in the Maillard reaction as reaction substances.
oleic acid, linoleic acid, γ-linolenic acid, and eicosadienoic acid (P <
Through three indicators, thermal treatment caused further Maillard
0.05).
reaction in the water-boiled salted duck, although the degree of this
Branched-chain alcohols were positively correlated with unsaturated
change was small.
fatty acids, which may be due to the low concentration of branched-
chain aldehydes in the precursor and low production of branched-
4. Conclusions
chain alcohols; the high temperature caused the loss of branched-
chain alcohols, resulting in a decrease in the content thereof. As a key
The results showed that a total of 38 flavour compounds (including
aromatic compound in duck meat, 1-octen-3-ol was maybe generated by
monomers and dimers) were detected, including aldehydes, ketones,
heating and enzymatic oxidation of n-3, n-6 polyunsaturated fatty acids
alcohols, esters, and furans. The flavour of the water-boiled salted duck
(Liu et al., 2019). The difference in this experiment was that the
after high temperature sterilisation (121 ◦ C, 20 min) deteriorated, and

9
Q. Xie et al.
the content of aldehydes and ketones in the flavour compounds
increased significantly (P < 0.05). Low-temperature thermal treatment
had relatively little effect on the flavour of the samples. The composition
of flavour compounds in 85 ◦ C group and 95 ◦ C group were relatively
similar. Thermal treatment significantly increased the degree of lipid
oxidation in the water-boiled salted duck, but had little effect on Mail­
lard reaction. High-temperature sterilisation significantly promoted the
oxidative decomposition of unsaturated fatty acids to produce a large
number of hydroperoxides, which further generated various volatile
compounds and flavour precursors. Through correlation analysis, it was
speculated that oleic acid and linoleic acid were the key unsaturated
fatty acids influencing the formation of aldehydes and ketones. The
flavour of the samples treated at 85 ◦ C and 95 ◦ C was similar, but
considering that 95 ◦ C had a stronger sterilisation effect on microor­
ganisms (Wang et al., 2020), so it was considered that the 95 ◦ C thermal
treatment was more suitable for the secondary sterilisation of packaged
water-boiled salted ducks. In addition, this conclusion may also apply to
other packaged meat products.
CRediT authorship contribution statement
Qiusheng Xie: Experiment, Investigation, Formal analysis, Writing –
original draft. Baocai Xu: Data curation, Project administration. Ying
Xu: Conceptualization, Methodology. Zhong Yao: Validation. Benwei
Zhu: Software. Xinfu Li: Conceptualization. Yun Sun: Supervision,
Methodology, Project administration.
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.
Acknowledgements
This work was supported by the “13th Five-Year” National Key R&D
Program of China [Grant No. 2016YFD0401501].
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