Measurement: Food 6 (2022) 100030

Contents lists available at ScienceDirect

Measurement: Food
journal homepage: www.elsevier.com/locate/meafoo

Influence of drying techniques on sensory profile and chlorogenic acid

content of instant coffee powders
Shweta M. Deotale, Sayantani Dutta, J.A. Moses, C. Anandharamakrishnan∗
Computational Modeling and Nanoscale Processing Unit, National Institute of Food Technology, Entrepreneurship and Management - Thanjavur, Ministry of Food
Processing Industries, Govt. of India, Thanjavur 613005, Tamil Nadu, India

a r t i c l e i n f o a b s t r a c t

Keywords: To ascertain the best technique for retention of sensory properties and chlorogenic acid (CGA) in instant coffee, the
Coffee present study involved several drying techniques such as spray drying, freeze drying, spray freeze drying (SFD),
Chlorogenic acid conductive hydro drying, and compared the effect with a commercial sample. From the analysis of all coffee
Spray-freeze drying
samples, both by sensory analysis (based on fuzzy logic) and by descriptive analysis (for foaming characteristics),
Fuzzy logic
SFD coffee was preferred. This fact was further corroborated by electronic nose-based aroma analysis of coffee.
E-nose
Chromatographic analysis (HPLC) revealed maximum (85%) retention of CGA in SFD (52.35±0.61 mg CGA/g of
coffee powder). Overall, SFD emerged as the most preferred technique for the preparation of instant coffee.

1. Introduction as its foaming stability [4]. Thus, with more CGA retained in the dried
coffee powder, the foaming properties of the coffee beverage will be
Instant coffee powder is a common form of coffee powder (dried) improved [5]. Besides foaming and aroma, CGA confers salutary bene-
used globally for the preparation of coffee (beverage). To prepare in- fits such as antioxidant effects [6], positive neurocognitive effects [7],
stant coffee powder, drying of the natural coffee extract is required. and it helps in prevention of type-2-diabetes mellitus [8]. Therefore,
Hence, common drying techniques such as spray drying (SD), freeze it is necessary to retain the CGA content in the instant coffee for sen-
drying (FD), spray freeze drying (SFD), and conductive hydro drying sory as well as therapeutic benefits. Earlier, studies reported the ef-
(CHD) have been employed in the present work for instant coffee pow- fect of roasting on CGA content in coffee [9,10]; however, retention
der preparation. Evaluation of aroma of the coffee powders is important of CGA through drying techniques is still unknown to the best of our
in assessing the retention of the signature aroma in the beverage; hence, knowledge.
the work presented herein includes electronic nose (e-nose) analysis of The objectives of the present study were therefore, identification of
instant coffee powders produced by the drying techniques. Sensory eval- the best drying technique for retention of aroma profile and CGA content
uation of the instant coffee powders is also essential, after all coffee in instant coffee by hedonic sensory evaluation (assisted by fuzzy logic)
should be sensorically appealing. Therefore, hedonic sensory analysis of of dried coffee samples, e-nose analysis of aroma, analysis of foaming
beverages from these instant coffee powders was conducted; as well as behavior in the coffee samples by descriptive sensory evaluation and
sensory validation of foaming in those beverages was conducted by de- quantification of CGA content in dried coffee powders.
scriptive sensory analysis. To avoid sensory bias, owing to dependency
on human perception and preconceived notions, in the present study 2. Materials and methods
fuzzy logic has been applied on the hedonic sensory data to achieve
a numerical quality index. It is a dependable method that has earlier 2.1. Materials
been successfully applied on hedonic sensory data of many other food
products [1,2]. For this work, a sample of medium roasted Arabica coffee beans was
Chlorogenic acid (CGA) content is considered important for ascer- kindly donated by CCL Industries, Hyderabad, India. The commercial
taining the coffee bean quality, since it contributes to the signature freeze dried instant soluble coffee powder (CS) was purchased from a
aroma of coffee [3]. CGA also facilitates the formation of self-assembly local market in Thanjavur, Tamil Nadu, India. CGA standard (≥ 95%
of surface active components of coffee by reducing the surface hy- purity) and DPPH (2, 2-diphenyl-1-picrylhydrazyl) were procured from
drophobicity; hence, it enhances the foaming capacity of coffee as well Merck, India.

∗
Corresponding author.
E-mail addresses: moses.ja@iifpt.edu.in (J.A. Moses), anandharamakrishnan@iifpt.edu.in (C. Anandharamakrishnan).

https://doi.org/10.1016/j.meafoo.2022.100030
Received 11 January 2022; Received in revised form 17 March 2022; Accepted 18 March 2022
2772-2759/© 2022 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/)
S.M. Deotale, S. Dutta, J.A. Moses et al. Measurement: Food 6 (2022) 100030

2.2. Drying of coffee extract through different techniques VOCs increase the conductivities of the sensors, and the corresponding
changes in voltages are recorded.
Coffee extract was prepared by brewing (10 min) 40 g of ground In the present study, process parameters such as granularity and
coffee bean powder (CB) in 1 L water. The infusion was subsequently batch size of coffee powder, heating time, headspace generation time,
filtered using Whatman No. 1 filter paper. This extract was concentrated sampling, and purging time were optimized from preliminary trials. Dif-
in accordance with Deotale et al. to obtain coffee extract (CE) [5]. ferent batches of CB were used to calibrate the e-nose and the param-
CE was used to produce instant coffee powder using different drying eters were optimized based on the maximum response of the sensors.
techniques according to the methods detailed in our earlier study [11]. From the findings of preliminary trials, 10 g of each coffee powder (dp =
Briefly, SD coffee powder was obtained using a laboratory-scale spray 0.50 ± 0.02 mm) was placed in a sample holder (100 mL) and heated
dryer (JISL, Mumbai) with a feed flow rate at 5 mL/min, with the flow by a miniature halogen lamp (50 W) for 450 s at 50±2 °C. For the pro-
being maintained by a peristaltic pump (PP-500 Master, Parisa Technol- duction of adequate concentration of VOCs, 30 s was provided for the
ogy, Mumbai, India). The inlet and outlet air temperatures were 120 °C headspace generation, followed by sampling, which was kept constant
and 55 °C, respectively, and the airflow was maintained at 1.1 m3 /min. at 50 s. Post sensing, purging of fresh air (5 mL/s flow rate) for 300 s
CE was freeze dried in a laboratory-scale freeze dryer (Lyophilizer LYO enabled the sensors to return to their baseline values.
10 T, Borg Scientific, Chennai, India) at −40 °C shelf temperature un- From the data obtained for CB, four sensors were selected that pro-
der a vacuum of 0.01 bar. For SFD of CE, a fabricated spray freezing vided maximum responses (∆R) i.e., the amount of change in the signals
rig was used [12]. The feed was sprayed with the help of compressed of the particular sensor from its base value, due to the VOCs generated
air (588.39 kPa) through a twin fluid nozzle atomizer at 6 mL/min into from a particular sample. From the results obtained for these four sen-
liquid nitrogen. The frozen fine coffee particles thus obtained were then sors, a PCA plot was plotted to differentiate the aroma profiles of all the
freeze dried in the conditions mentioned above. The initial moisture coffee samples.
content of concentrated coffee extract was 27.05 ± 3.14% (wet basis).
There was no significant difference in the moisture content of all the cof- 2.5. Sensory analysis of coffee beverage by fuzzy logic
fee powders. The values were found in the range of 6.66 – 6.90%. The
water activity of SD, FD, and SFD ranged from 0.35 to 0.41, detailed in For sensory analysis, coffee beverages were prepared from each of
our earlier investigation [11]. the dried coffee powders (SD, FD, SFD, CHD), along with CS. Filter coffee
For CHD, a layer of CE (∼1.0 mm thickness) was spread on a food- was prepared from CB, and other coffee powders were used to prepare
grade polyester (PET) film (ARYAPETV®- A 250, Ganapathy Industries, instant coffee (espresso), according to the method stated by Stokes et al
Bangalore) having 100 μm thickness. The set up was placed on a cir- [15]. All the beverages were served to the panelists’ at 70 °C that was
culating water reservoir (1 m X 0.5 m X 0.3 m) [13]. The water tem- maintained by a thermostatically controlled container.
perature was maintained at 50±5 °C during drying. All the dried coffee
powder samples were stored in desiccators kept at ambient temperature 2.5.1. Sensory evaluation
(20±2 °C) in laminated bags for 1–2 days until further use for analysis. Sensory evaluation for all the coffee beverages was conducted by a
These samples, along with CE and CS were subjected to LC-MS analysis group of 20 semi-trained panelists (six men and fourteen women in the
for screening of compounds. age group of 21–40 years). The panelists were chosen based on their
interest in sensory evaluation, who voluntarily participated in the as-
sessment, and had familiarity with coffee. Panelists were served coffee
2.3. LC-MS analysis of coffee bean
samples (20 mL) in glasses in a well-ventilated room under white light,
between 10 am and 12 noon [16]. The samples were blind coded dur-
LC-MS analysis was carried out to identify the compounds present
ing serving and served randomly to the panelists. Drinking water was
in CB, CE, CS and dried coffee powders, according to the method pre-
provided to rinse their palate between consecutive samples.
viously reported [3,5]. Briefly, 1 g of coffee powder was subjected to √
The panelists were asked to give tick mark ( ) for the appropriate
extraction in 70% methanol in an incubator shaker (SZ-044A, Sub-Zero,
score in the five-point sensory scale (‘not satisfactory’, ‘fair’, ‘medium’,
India) operating at 150 rpm, at room temperature for 60 min. Subse-
‘good’ and ‘excellent’) based on their preference for each of the qual-
quently, the extract was centrifuged for 10 min at 3000 rpm followed
ity attribute (aroma, color, taste, after taste and overall appearance) of
by membrane filtration (0.45 𝜇m). The excess methanol was evaporated
each sample. They were requested to score first for the ‘aroma’ of the
by purging a gentle nitrogen stream. The extract thus obtained was used
coffee samples. Further, the relative importance (NI: not important, SI:
for LC-MS analysis (Model: LCMS 8040, Triple Quadrupole, Shimadzu
somewhat important, I: important, HI: highly important, EI: extremely
Corporation, Kyoto, Japan).
important) of the quality attributes of coffee (for all coffee beverage
The instrumental parameters employed were: ionization by electro-
and not for a particular sample) was also requested to the panelists to
spray ionization (ESI) (negative); ion spray voltage +4.5 kV / −3.5 kV;
ascertain the importance of a particular quality attribute.
CDL temperature 250 ºC; block temperature 400 ºC; detector voltage
1.3 kV; nebulizer gas flow rate 1.5 L/min; drying gas flow rate 15 L/min;
2.5.2. Fuzzy logic analysis for sensory scores
scan mode was single ion monitoring (SIM). Identification of the com-
Linguistic variables such as ‘not satisfactory’, ‘fair’, ‘good’ are used
pounds was performed according to literature reports [6,7].
in fuzzy system to define relationships between independent variables
(e.g. color, aroma, and flavor) and dependent variables (acceptance and
2.4. Analysis of aroma profile by e-nose rejection), numerically, on the hedonic data. Defuzzification of the fuzzi-
fied score generates a numeric value for the entire sensory analysis that
The aroma profile of all the dried coffee powders (SD, FD, SFD, CHD) can be used as an index for direct interpretation of quality [2].
was compared with that of CB and CS with the help of an e-nose sys- The responses given by panelists were used to obtain the relation-
tem (ENOVISION, C-DAC, Kolkata, India). The operational protocol de- ship between each quality attribute and its relative importance. This
scribed by Dutta and co-workers [14] was followed. The e-nose system relationship was established using fuzzy logic, in accordance with the
contains an array of 8 metal oxide gas sensors (non-specific) that re- process described by Debjani [17]. Based on membership distribution
spond to a wide range of volatile organic compounds (VOCs). The sam- pattern (Fig. 1A), ‘triplets’ (Ts ) were generated from the responses of
ples are heated by the instrument for a brief period to generate VOCs the sensory panel (total number of tick marks) that denotes the triangu-
that are detected by the sensors. These VOCs are exposed to the array of lar fuzzy number of the same (Table 1). Basically, one triplet (i.e. 0 0
sensors with the help of a mini air compressor. At the sensor surface, the 25, 25 25 25 etc.) is a set of three numbers that denote the triangular

2
S.M. Deotale, S. Dutta, J.A. Moses et al. Measurement: Food 6 (2022) 100030

Fig. 1. Schematic representation of fuzzy logic, (A) triangular membership function distribution pattern of five point sensory scale, (B) overall sensory score as ∆ABC
when (a+c)≤100 (modified from [17]).

Table 1
Sum of the number of panelists having varying preferences for the particular quality attribute of coffee samples along with the fuzzified and defuzzified
scores for coffee samples.

Sample Quality attributes NS F M G E Triplets for sensory scores Overall fuzzified score Defuzzified score

CB Aroma 1 5 9 4 1 48.75 23.75 23.75 58.87 41.62 32.83 55.94

Color 1 2 9 8 0 55.00 23.75 25.00
Taste 0 1 3 16 0 68.75 25.00 25.00
After taste 1 1 6 11 1 62.50 23.75 23.75
Overall appearance 1 2 6 11 0 58.75 23.75 25.00
SD Aroma 3 8 5 4 0 37.50 21.25 25.00 42.89 33.38 29.85 41.71
Color 3 2 5 9 1 53.75 21.25 23.75
Taste 3 7 3 5 2 45.00 21.25 22.50
After taste 6 7 3 4 0 31.25 17.50 25.00
Overall appearance 3 6 4 5 2 46.25 21.25 22.50
FD Aroma 2 7 8 3 0 40.00 22.50 25.00 49.01 38.65 32.07 46.82
Color 0 4 6 10 0 57.50 25.00 25.00
Taste 1 3 10 6 0 51.25 23.75 25.00
After taste 1 6 10 3 0 43.75 23.75 25.00
Overall appearance 0 4 10 6 0 52.50 25.00 25.00
SFD Aroma 0 3 4 5 8 72.50 25.00 15.00 71.69 46.00 25.45 64.84
Color 0 2 2 6 10 80.00 25.00 12.50
Taste 0 3 4 6 7 71.25 25.00 16.25
After taste 1 3 4 4 8 68.75 23.75 15.00
Overall appearance 1 3 5 4 7 66.25 23.75 16.25
CHD Aroma 4 7 6 2 1 36.25 20.00 23.75 38.28 30.21 29.33 37.99
Color 2 6 2 8 2 52.50 22.50 22.50
Taste 5 4 5 5 1 41.25 18.75 23.75
After taste 7 6 4 2 1 30.00 16.25 23.75
Overall appearance 7 5 4 4 0 31.25 16.25 25.00
CS Aroma 0 6 6 6 2 55.00 25.00 22.50 48.21 36.98 30.75 46.14
Color 2 2 7 7 2 56.25 22.50 22.50
Taste 1 8 4 6 1 47.50 23.75 23.75
After taste 2 6 6 6 0 45.00 22.50 25.00
Overall appearance 5 5 5 5 0 37.50 18.75 25.00

CB: roasted coffee bean; SD: spray dried coffee sample; FD: freeze dried coffee sample; SFD: spray freeze dried coffee sample; CHD: conductive hydro
dried coffee sample; CS: commercial sample; NS: not satisfactory; F: fair; M: medium; G: good; E: excellent.

membership function distribution pattern of sensory scores [2]. The first for each quality attribute was calculated from the corresponding Ts and
number of triplet denotes the coordinate of the abscissa where the value TI of each sample using the triplet multiplication rule and the extended
of the membership function is ‘1′, the other two values are termed as the product rule [17] (Table 1). The triplets obtained from the sum of the
left and right spreads, respectively, and their membership functions are overall sensory score denote the overall fuzzified score. These triplets
‘0′ [18]. Similarly, the triplets for the relative importance of each quality (a,b,c) represent a ∆ABC (Fig. 1B). For the value of (a + c) ≤ 100, the
attribute (TI ) were also calculated (Table 2). The overall sensory score ∆ABC lies within the sensory scale interval [0, 100]; for this case, the

3
S.M. Deotale, S. Dutta, J.A. Moses et al. Measurement: Food 6 (2022) 100030

Table 3
Details of descriptors and corresponding scores for descriptive analysis of coffee
foam.

Descriptor Category Score

Initial foam Abundant 3

Rank
(foam formed immediately after pouring the (foam fills the glass

IV

III
V
II
coffee into the glass) and persists)

I
Normal 2
Defuzzified score (foam fills the glass but
disappears)
Poor 1
(foam does not fill the
0.196
0.182
0.207
0.172
0.193
glass)
Foam area Total 3
(proportion of coffee surface area covered Partial 2
Triplets of relative weightage (Trel )

by bubbles) None 1
0.02695
0.03892
0.01497
0.03593
0.02695

Foam collar Total 3

(bubble lace formed around the coffee Partial 2
surface, following the glass circumference) None 1
Global impression Very good 4
0.05988
0.05988
0.05988
0.05988
0.05988

(overall foam quality) Good 3

Acceptable 2
Bad 1
0.20659
0.18862
0.22156
0.17964
0.20359

defuzzified score (ya ) can be calculated from Eq. (1) [2].

Sum of number of panelists for the relative importance of quality attributes of coffee samples and ranking of the parameters.

11.25
16.25

15.00
11.25

1
6.25

𝑦𝑎 = (3 𝑎 − 𝑏 + 𝑐 ) (1)
Triplets for scores (Ts )

3
25.00
25.00
25.00
25.00
25.00

Defuzzified scores were calculated for each coffee sample along with
quality attributes and ranking was given for the same based on these
values.
NI: Not important, SI: somewhat important, I: important, HI: highly important, EI: extremely important.
86.25
78.75
92.50
75.00
85.00

2.6. Descriptive sensory analysis for foaming properties of coffee powders

EI (100 25 0)

Foaming properties of all the coffee samples were tested by descrip-

tive analysis. The same sensory panel, as stated earlier, was employed
11

15

11
7

and the same protocol was followed for this analysis also, with different
HI (75 25 25)

descriptors (initial foam, foam area, foam collar, global impression) for
foam. Each descriptor had three categories, except for global impres-
sion which had four categories, comprising of the separate scores for
each category (Table 3) [19]. Similar to the sensory analysis, all pan-
√
7
9
4
4
6

elists were asked to give tick marks ( ) for the suitable category of each
I (50 25 25)

descriptor. The average score for each category was calculated and the
PCA plot was generated to differentiate the samples based on the foam-
ing properties.
2
4
1
8
3
SI (25 25 25)

2.7. Estimation of CGA content of coffee powders

High performance liquid chromatography (HPLC, i-Series Plus, C18

0
0
0
0
0

column, Shimadzu, Maryland, United States) was used to estimate CGA

NI (0 0 25)

content in CE, CS, and all the dried coffee samples obtained from differ-
ent drying techniques. 100 mg of each coffee powder was mixed with
5 mL of 70% methanol and vortexed (2 min). Thereafter, the solution
0
0
0
0
0

was centrifuged at 3000 g for 15 min, and the supernatant was filtered
through a syringe filter (PTFE, 0.2 𝜇m). The final solution obtained was
Overall appearance
Quality attribute

subjected to HPLC analysis. During analysis, the compound was eluted

in a solvent gradient consisting of 70% methanol, with 1 mL/min flow
After taste

rate. The quantification was carried out with the help of a standard curve
Table 2

Aroma
Color
Taste

of pure CGA, which was read at a wavelength of 315 nm (UV detector).

CGA has several isomers, and among the isomers, 5-O-caffeoylquinic
acid (5-CQA) is the most abundant in coffee beans [20]. In the present
study however, the total CGA content was considered for quantification,
instead of a particular isomer, to determine the quality of the instant
coffee (since detection of isomer was beyond the scope of the present
objectives).

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S.M. Deotale, S. Dutta, J.A. Moses et al. Measurement: Food 6 (2022) 100030

Table 4
Comparison of peak area (%) of compounds obtained from phytochemical screening of different coffee powders and roasted coffee bean.

Sl. Compound Peak area (%)

no. name m/z
CE SD FD SFD CHD CS

1 Acetaldehyde 44 0.070 1.890 0 2.068 4.966 2.687

2 Acetic acid 66 0.682 4.080 0 4.465 10.721 5.801
3 Pyridine 79 9.380 28.040 0 0.733 6.509 39.874
4 2, 3 Butanedione 86 0.240 0 14.673 0.078 0 0
5 2,3 Pentanedione 100 14.371 0 4.941 8.860 0.219 0
6 2 Ethyl pyrazine 108 0.105 1.941 2.446 2.124 5.101 2.760
7 Maltol 126 0.238 6.862 0 7.511 0 9.757
8 Trigonelline 138 1.343 0.681 0.826 0.746 1.791 0.969
9 2, 4, 6-triethyl pyridine 163 1.978 0 14.682 8.703 0 0
10 3-decenoic acid 170 2.029 0 8.357 0.754 0 0
11 4-cyclohexylphenol 176 3.036 0 0.823 0.614 0.180 0
12 Caffeic acid 180 4.471 22.516 13.333 24.644 59.167 32.012
13 Caffeine 194 4.419 1.403 8.385 1.536 3.688 1.995
14 Chlorogenic acid 354 0.826 0.689 4.075 0.754 1.810 0.979
15 2,6-pyridinedicarboxylic acid, 2-(2-methoxyethyl) heptyl propyl ester 365 16.764 29.664 17.792 32.467 0 0
16 3-O-Feruloylquinic acid 367 8.952 0.804 0.056 0.884 2.123 1.148
17 DL-Valine, N-methyl-N-decyloxycarbonyl-dodecyl ester 483 16.871 0 0.406 0.746 0 0
18 3,4-Di-O-caffeoylquinic acid 543 13.438 1.416 8.373 1.549 3.721 2.013
19 Cafestol arachidate 610 0.775 0 0.823 0.754 0 0

CE: extract obtained from roasted coffee bean; SD: spray dried coffee sample; FD: freeze dried coffee sample; SFD: spray freeze dried coffee sample;
CHD: conductive hydro dried coffee sample; CS: commercial sample.

2.8. Statistical analysis sensor 7 (TGS2611), and sensor 8 (TGS2600) were selected for PCA anal-
ysis of the odor profiles of coffee samples (Fig. 3A). Clearly, in the PCA
Estimation of aroma profiles of coffee powders by e-nose, and CGA plot, coffee powders obtained from SD and CHD formed a separate clus-
contents of coffee samples by HPLC were conducted in triplicate and ter that was distant from that of the CB and other instant coffee pow-
the data are represented with standard deviation (SD). XLSTAT (version ders (Fig. 3B). The discrimination index of 98.46% indicated a distinct
2014.5.03, AddinsoftTM , N.Y., US) software was used to obtain PCA plots separation of the coffee samples’ odor profiles. In fact, the aroma pro-
of sensory data. file of CB was quite different from SD, SFD, and even CS. Previously,
a few researchers have reported segregating up to 7 varieties of coffee
3. Results and discussion with e-nose (Pico-1, Brescia, Italy) [23], mixed samples of coffee [24],
and few even have differentiated samples of instant freeze-dried coffee
3.1. LC-MS analysis of coffee powder with e-nose technology [25]. The current finding suggests that indeed
the aroma profiles of FD and SFD instant coffee were close, and it was
From the LC-MS analysis of CB, around 20 components were iden- possible to discriminate them from the rest.
tified, such as caffeine (m/z ratio 194.1), CGA (m/z ratio 354.3), and
its derivatives such as 3-O-feruloylquinic acid (m/z 368.33), 3, 4 di- 3.3. Sensory evaluation (hedonic) and fuzzy logic
O-caffeoyl quinic acid (m/z 544), and caffeic acid (m/z 180), and es-
ters such as 2,6-pyridinedicarboxylic acid, 2-(2-methoxyethyl) heptyl The hierarchical importance of the quality attributes obtained from
propyl ester and DL-valine, N-methyl-N-decyloxycarbonyl-dodecyl ester the sensory panel was taste>aroma>overall appearance>color>after
at their respective peaks (labeled in Fig. 2). These finds agreed with lit- taste (Table 2). Based on the judgment of the sensory panel, ‘taste’ re-
erature, where other authors have reported the presence of compounds ceived the highest defuzzified score (0.207), and was found to be the
such as caffeoyl-dimethoxycinnamoylquinic acids, chlorogenic acids, most important quality parameter for coffee. This finding was in accor-
diferuloylquinic acids, dimethoxycinnamoylquinic acids, and feruloyl- dance with Lazim and Suriani, where panelists expressed that among
dimethoxycinnamoylquinic acids in Arabica coffee [3,6,7,21]. It was re- the quality parameters, ‘taste’ is ‘most important’ when they conducted
ported that these phytochemicals are responsible for the development a fuzzy logic-based analysis of quality attributes for different coffee sam-
of astringency, flavor, and antioxidant activity of coffee [2]. ples [26].
The phytochemical screening by LC-MS of all dried coffee powders From the defuzzified scores of all the coffee samples, it was clear that
showed the presence of specific compounds such as CGA, caffeine, caf- coffee prepared with SFD (64.84) showed the highest score followed by
feic acid, and derivatives of CGA with different intensities. Comparison CB, FD, CS, SD, and CHD (Table 1). From the fuzzy logic approach of
of LC-MS profiles of these powders with that of CB exhibits the effect of sensory analysis the ranking of coffee beverages based on the sensory
drying on bioactive components in coffee; maximum retention of bioac- panel was found to be SFD> CB > FD > CS > SD > CHD. Therefore, the
tives was observed in the sequence of SFD>FD>CS>CHD>SD (Table 4). sensory profile of SFD was most preferred by the sensory panel; whereas,
Reportedly, during the SD process, majority of volatile compounds that CHD was the least liked. Also, combining the findings of CGA content
are responsible for sensory notes were found to be degraded [17]; in and e-nose, SFD emerges as the most appropriate drying technique for
the current study also the LC-MS spectrum of SD showed only a few instant coffee.
compounds. It has been observed that caffeine content changes during Fuzzy logic-based inferences for the preference of coffee have been
roasting due to heat processing [22]; similar trend has also been ob- conducted in the past with success. While Lazim and Suriani identified
served in the present work. the Indoc coffee as the ‘best’ among three different coffee samples (Nesc,
Indoc and Incom) [26], Kumar and Badgujar have used this approach
3.2. Differentiation of odor profiles of coffee powders by e-nose to find out the best combination of instant coffee powder and brown
seaweed (Sargassum wightii) among many sample mixes [27]. However,
For CB, based on the maximum signal response (∆R) obtained from there is no literature report on dried coffee extract to directly correlate
different sensors, four sensors, sensor 1 (TGS832), sensor 3 (TGS823), the present findings.

5
S.M. Deotale, S. Dutta, J.A. Moses et al. Measurement: Food 6 (2022) 100030

Fig. 2. LC-MS profile of extract obtained from roasted

coffee bean (CE).

3.4. Descriptive analysis of coffee foam the sensory acceptability of foam of SFD was similar to that of CS, but
the foam of SD and CHD was not comparable with that of CS.
The descriptive sensory analyses of coffee foams revealed that the The biplot also reflects the variables (i.e. foam characteristics) as
panelists liked the ‘global impression’, ‘initial foam’, and ‘foam area’ of vectors, and from the length of the vectors foam collar was found to
SFD and CS, followed by that in sample CB (Table 5). Foam collar was be the characteristic with the highest variability represented by F1 and
most acceptable for CS, with limited acceptability for CB and FD. CHD F2. Among the vectors, initial foam was highly correlated with global
was provided the least preference for the tested attributes. Low accep- impression since these two vectors formed very small angle; and foam
tance for the said parameters was also observable for SD and FD. From collar was not correlated with global impression owing to the formation
the PCA biplot, the first (F1) and second (F2) components (PCs) explain of 90° angle between them. However, there was no negative correlation
96.51 and 2.88% variability in the data, i.e. together 99.39% of the total among the variables. Although descriptive analysis provided a some-
diversity (Fig. 4). Foam characteristics that contributed most to the vari- what mixed response, based on data, SFD coffee emerged as the most
ability in F1 were foam area, initial foam and global impression (Eigen preferred sample (and the drying technique) for instant coffee.
vectors were 0.5083, 0.5028 and 0.5015, respectively), whereas, in F2,
foam collar (Eigen vector 0.8555) was found to be the characteristic 3.5. CGA content in coffee
that contributed largely to the variability. The biplot clearly shows the
position of CS and SFD in a separate cluster which is close to CB and FD The experimental trials revealed that the roasted coffee beans con-
(Fig. 4). Considering CS as the reference sample, the data denotes that tained 61.82 ± 0.64 mg CGA/g coffee powder. The CGA content in

6
S.M. Deotale, S. Dutta, J.A. Moses et al. Measurement: Food 6 (2022) 100030

Fig. 3. Electronic nose analysis of coffee samples. (A)

Selection of e-nose sensors based on e-nose response
for roasted coffee bean, (B) PCA plot to differentiate
the aroma profiles of all coffee powders. CB: roasted
coffee bean; SD: spray dried coffee sample; FD: freeze
dried coffee sample; SFD: spray freeze dried coffee
sample; CHD: conductive hydro dried coffee sample;
CS: commercial sample.

Fig. 4. PCA plot to differentiate the foaming properties of

different coffee samples from the descriptive analysis. CB:
roasted coffee bean; SD: spray dried coffee sample; FD: freeze
dried coffee sample; SFD: spray freeze dried coffee sample;
CHD: conductive hydro dried coffee sample; CS: commercial
sample.

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S.M. Deotale, S. Dutta, J.A. Moses et al. Measurement: Food 6 (2022) 100030

Table 5 descriptive sensory evaluation of foaming properties. Also, the current

Sensory scores of descriptive analysis of foam of different coffee samples. study established SFD as the most suitable method of drying to retain
Sample code Initial foam∗ Foam area∗ Foam collar∗ Global impression∗ almost 85% of CGA in the instant coffee powder. Based on the result ob-
tained, it has been observed that coffee being sensitive in nature should
CB 2.44 2.72 2.66 3.38
be processed at low temperature to avoid losses of functional compo-
SD 1.75 2.28 2.44 2.44
FD 2.22 2.56 2.63 2.88 nents. Moreover, though freeze drying is commercially used technique
SFD 3.00 2.94 2.7 3.53 for coffee drying, with the help of SFD we can reduce the drying time
CHD 1.38 2.00 1.91 2.13 of coffee. Also, conductive hydro drying was found to be not suitable
CS 2.94 2.91 2.84 3.53
for coffee drying in spite of its mildness and economic feasibility. Thus,
∗
Values are average of scores given by 20 panelists. the findings suggest SFD be the most reliable technique for producing
CB: roasted coffee bean; SD: spray dried coffee sample; FD: freeze dried coffee instant soluble coffee, with salutary gains of CGA and consumer prefer-
sample; SFD: spray freeze dried coffee sample; CHD: conductive hydro dried ence.
coffee sample; CS: commercial sample.
Research involving human and/or animal participants

For the type of research that has been conducted, to the best of our
instant coffee powders differed significantly depending on the drying knowledge, no risk assessment is required. Therefore, no ethical clear-
method employed. Among the dried powders, the CGA content was ance is needed.
highest for SFD with 52.35 ± 0.61 mg CGA/g coffee powder, i.e., 85%
retention. FD coffee powder had 49.89 ± 0.24 mg CGA/g coffee powder Declaration of Competing Interest
(81% retention), while CHD coffee powder contained 35.27 ± 0.30 mg
CGA/g coffee powder (61% retention), and SD coffee powder consisted None
of only 8.99 ± 1.59 mg CGA/g coffee powder.
Comparing the data obtained from literature revealed limited simi- CRediT authorship contribution statement
larity with Cropley and co-workers who have reported that the total CGA
content in regular decaffeinated coffee, soluble decaffeinated coffee, and Shweta M. Deotale: Investigation, Writing – original draft.
caffeinated coffee was 224, 521, and 244 mg per 2 g coffee, respectively Sayantani Dutta: Data curation, Formal analysis, Writing – original
[7]. However, the said authors did not specify the coffee variety worked draft. J.A. Moses: Visualization, Writing – review & editing. C. Anand-
with. In another study, Mills et al. have quantified the amount of CGA haramakrishnan: Conceptualization, Writing – review & editing, Su-
in commercially available coffee (beverage) and accounted for it to be pervision.
between 27.33 and 121.25 mg/200 mL brewed coffee. This variation
has been attributed to the processing and roasting conditions of coffee Acknowledgments
beans [28]. Clifford corroborates the idea of progressive destruction and
transformation of CGAs during roasting of coffee seeds that is attributed The authors thank Dr. Nabarun Bhattacharyya and his team at C-
to the decreased CGA content in coffee, post-processing [22,29,30]. DAC, Kolkata, India for providing electronic nose facility for sensory
According to earlier report, CHD is an appropriate method for dry- analysis of coffee samples. The first author would like to acknowledge
ing of fruit and vegetable puree/slices [31], however, from the present Indian Council of Medical Research for providing an ICMR-SRF fellow-
investigation it is proved to be not suitable for drying of coffee extract ship. The second author thanks DST-INSPIRE Faculty Scheme (INSPIRE
owing to the issues of low solubility with suspended solids, poor foaming Faculty program, IFA-17/ENG-238), Govt. of India for funding.
properties and loss of volatiles in the dried coffee sample. The proba-
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