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Production of orange juice concentrate using conventional and microwave

vacuum evaporation: Thermal degradation kinetics of bioactive compounds
and color values

Article in Journal of Food Processing and Preservation · September 2021

DOI: 10.1111/jfpp.15902

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Received: 3 April 2021 | Revised: 6 August 2021 | Accepted: 20 August 2021

DOI: 10.1111/jfpp.15902

ORIGINAL ARTICLE

Production of orange juice concentrate using conventional and

microwave vacuum evaporation: Thermal degradation kinetics
of bioactive compounds and color values

Hamza Bozkir1 | Yeliz Tekgül2

1
Food Processing Department, Pamukova
Vocational School, Sakarya University of Abstract
Applied Sciences, Sakarya, Turkey This study aimed to concentrate orange juice using the microwave vacuum evapora-
2
Food Processing Department, Kösk
tion (MVE) and the rotary evaporation (RE) at different absolute pressures (20, 31,
Vocational School, Aydın Adnan Menderes
University, Aydin, Turkey and 47 kPa) and investigate the effects of two different concentration techniques on
Correspondence the degradation kinetics of vitamin C, total phenolic content (TPC), total carotenoid
Hamza Bozkir, Food Processing Department, content (TCC), and color values. The MVE significantly raised the evaporation rate
Pamukova Vocational School, Sakarya
University of Applied Sciences, Sakarya, compared to the RE (p < .05). It was determined that the MVE and the RE at 80℃
Turkey. required concentration-­time 21 and 42 min, respectively. Total soluble solid changes
Email: [email protected]
during the MVE and the RE processes were fitted to six different empirical models
with an R 2 range between 0.915 and 0.998. The results showed that degradation rate
constants for vitamin C, TPC, and TCC of orange juices concentrated using the RE
were higher significantly than the MVE (p < .05). It was determined that the degra-
dation rate constants of the L*, a*, b*, and ΔE orange juices concentrated using MVE
were lower than the RE (p < .05).
Novelty impact statement
1. Orange juices were concentrated using MVE and RE.
2. The MVE significantly increased the evaporation rate compared to the RE.
3. The MVE protected bioactive compounds (values vitamin C, TPC, and TCC) and
color values (L*, a*, b*, and ∆E) in comparison with the RE.

1 | I NTRO D U C TI O N low energy efficiency, and high temperature. These processes re-
duce bioactive components such as phenolics, antioxidants, carot-
Orange juice (Citrus sinensis L.) is a popular beverage consumed enoids, vitamins, and alter the color of the fruit juices and cause
daily in most countries (Paravisini & Peterson, 2019). The orange the undesirable formation of hydroxymethylfurfural (HMF) and
juice contains significant bioactive compounds such as vitamin C, furan (Aguiar et al., 2012; Demirdöven & Baysal, 2015; Katariya
carotenoids, phenolics, antioxidant substances, and dietary fiber et al., 2020; Wahia et al., 2020).
(Giuffrè et al., 2017; Paravisini & Peterson, 2019). The orange juices Novel concentration techniques, which eliminate the negativities
are generally produced by concentrate processing in the fruit and created by the concentrated production processes currently used in
vegetable juices industry. The orange juices are concentrated using the fruit juice industry, have gained importance in recent years. In
thermal evaporation to decrease the operating costs of packaging, this context, microwave vacuum evaporation (MVE) comes to the
transportation, and storage, then the products become microbiolog- fore that enables energy and mass transfer in a shorter time com-
ically, chemically, and biochemically stable (Bozkir & Baysal, 2017). pared to the thermal concentration technique (Assawarachan &
However, the conventional evaporation processes have long times, Noomhorm, 2011; Fazaeli, Hojjatpanah, et al., 2013).

J Food Process Preserv. 2021;00:e15902. wileyonlinelibrary.com/journal/jfpp © 2021 Wiley Periodicals LLC. | 1 of 12

https://doi.org/10.1111/jfpp.15902
2 of 12 | BOZKIR and TEKGÜL

The microwave heating technique creates volumetric heating in The initial total soluble solids of orange juices were determined
the foodstuff, thereby significantly shortening the heating time. The as 12 ± 0.05 °Brix and concentrated to 42 ± 0.10 °Brix.
microwave vacuum concentration technique considerably reduces
process time by transferring fast mass and energy at low tempera-
tures. This concentration technique develops more water vapor 2.2 | Microwave vacuum evaporation
separation, efficient use of power, and qualities of the products
(Assawarachan & Noomhorm, 2008, 2011). The MVE techniques The features of the vacuum unit of the system are two magne-
have been successfully practiced in concentrated apple juice, black trons (2.450 MHz), temperature control and indicator, vacuum
mulberry juice, grape, pineapple juice, pomegranate juice, raspberry control and indicator, working power: 250–­1 ,000 W, and vacuum
juices, and black carrot juices (Assawarachan & Noomhorm, 2008, pressure: 0–­
101.325 kPa. The system's temperature measure-
2011; Bozkir & Baysal, 2017; Dinçer et al., 2019; Fazaeli, Hojjatpanah, ments were carried out with a fiber optic infrared sensor (optris
et al., 2013; Fazaeli, Yousefi, et al., 2013; Hojjatpanah et al., 2011; 161 CTLT 15:1). The measured temperature values were recorded
Yousefi et al., 2012, 2013). The previous results have shown that the on the computer with the software of the optical fiber infra-
MVE had lower processing time and high-­energy efficiency and con- red sensor. Four hundred fifty milliters orange juice placed in a
served quality characteristics of products such as total phenolic con- 1,000 ml glass flask was concentrated by the MVE under absolute
tent (TPC) and total phenolic and anthocyanin contents, antioxidant, 20, 31, and 47 kPa pressures (60, 70, and 80℃) and 688 W power
antioxidant activity, and color values compared to the conventional (Figure 1).
evaporation technique (Assawarachan & Noomhorm, 2008, 2011;
Bozkir & Baysal, 2017; Hojjatpanah et al., 2011; Yousefi et al., 2013).
The scope of the literature has determined that MVE techniques 2.3 | Rotary evaporation
better to protect the quality characteristics of fruit juices and reduce
the processing time. To the best of our knowledge, there is no study RE was carried out using a laboratory type Heidolph (Heidolph,
comparing orange juices concentrated using MVE and rotary evapora- Hei-­VAP Value, Germany). The T-­t ype thermocouple was placed to
tion (RE) at different temperatures. Consequently, this study aimed to measure 1 cm from the bottom of the balloon in the rotary evapo-
concentrate orange juices using MVE and RE techniques at different ab- rator. Besides, data were obtained by connecting temperature re-
solute pressures (20, 31, and 47 kPa) and analyze the degradation kinet- corder, vacuum control, and digital vacuum meters. 450 ml orange
ics of vitamin C, total carotenoid content (TCC), TPC, and color values. juice placed in a 1,000 ml glass flask was concentrated by the RE
under absolute 20, 31, and 47 kPa pressures (60, 70, and 80℃) and
50 rpm rotation speed.
2 | M ATE R I A L S A N D M E TH O DS

2.1 | Materials 2.4 | Mathematical modeling

Oranges (C. sinensis) of Valencia varieties were supplied from The evaporation rate is defined as the number of molecules, which
Zumdieck Canned and Frozen Food Company (Manisa, Turkey). For pass from the juice to the vapor phase per unit of time according to
orange juice production, the oranges, which have been subjected to Equation (1) (Bozkir & Baysal, 2017):
washing and peeling, have been extracted with Moulinex (JU5000)
fruit extractor. Pulp ratios were adjusted by passing through Δx
Evaporation rate = , (1)
Δt
1 × 1 mm sieves to decrease the pulp ratios of orange juice below
10%. Then, freshly squeezed orange juices were pasteurized at where x is the loss of weight orange juice (gH2O), and t is evaporation
90 ± 1℃ for 2 min and then stored at −25℃. time (min).

Magnetrons F I G U R E 1 Schematic diagram of the

microwave vacuum evaporation system

Vacuum heating
Vacuum pump chamber

Condenser unit
Microprocessor

Power
BOZKIR and TEKGÜL | 3 of 12

The mathematical models, which could characterize the changes 2.7 | Total phenolic content
between total soluble solids and times, were used during concentra-
tion processings. The mathematical models are presented in Table 1. Total carotenoid content was estimated using the Folin-­C iocalteu
The compatibility of these mathematical models with experi- method (Franke et al., 2004) 1 ml of orange juice, 5 ml of phenol
mental total soluble solids curves was detected by non-­linear regres- reagent (10%), and 10 ml of saturated NaHCO3 were added, and
sion analysis using the SPSS package program (SPSS Inc., Chicago, IL, distilled water 100 ml was completed. The solutions were incu-
USA). The coefficient of determination (R 2), the chi-­square (χ2), and bated in the dark for 2 hr. The solutions were measured at 760 nm
root mean square error (RMSE) were the parameters for detecting using a Varian Cary 50 Scan (Austria) spectrophotometer. The re-
model acceptability, which were calculated according to Bozkir and sults were expressed as mg of gallic acid equivalents (GAE) per
Baysal (2017): liter.
( )2
∑ ΔBexp, i − ΔBpred, i
x2 = , (2)
N − np
2.8 | Vitamin C
√
1 ∑N ( (3) Vitamin C was determined according to the method of Hışıl (2007).
)2
RMSE = ΔBexp, i − ΔBpred, i ,
N i=1
Ten milliliters orange juice was mixed with 90 ml oxalic acid (0.4%,
w/v) and filtered. 1 ml of the sample extract was mixed with 9 ml
where ∆Bpred,i and ∆Bexp,i are predicted and experimental alteration 2,6-­dichlorophenolindophenol then the absorptions were immedi-
total soluble solids values of with observation, N is the number of prac- ately measured at 518 nm.
tical, and np is the number of constant in the model.
The evaporation times of concentrated orange juice were de-
tected from 12 ± 0.05 °Brix to 42 ± 0.10 °Brix for two different 2.9 | Color
concentration techniques.
Orange juice concentrates diluted to 12 °Brix values prior to per- Lightness (L*), redness (a*), and yellowness (b*) values were deter-
forming the quality analysis. mined using a colorimeter (CR-­10; Konica Minolta, Japan). The total
color difference (ΔE) was calculated according to Equation (4):

2.5 | Total soluble solids

√
(4)
( )2 ( )2 ( ∗ 2
)
ΔE = L∗ − L∗ref + a∗ − a∗ref + b∗ − bref ,

The total soluble matter contents (°Brix) of orange juices were de- where L∗ref, a∗ref, bref
∗
were the reading of fresh orange juice; and L*, a*,
tected using a digital refractometer at 20℃ (HANNA, USA). and b* were the reading at any time during the concentration.

2.6 | Total carotenoid content 2.10 | Degradation kinetics

Total carotenoid content was determined according to the method Degradation kinetics of Vitamin C, TPC, TCC values of orange juices
of Lee (2001). For this purpose, 15 ml of orange juice was homog- concentrated by the MVE, and the RE were defined according to the
enized with 30 ml of extraction solvent (hexane/acetone/ethanol; first-­order kinetic model (Equation 5) (Dhuique-­Mayer et al., 2007;
50/25/25, v/v/v) and then centrifuged (4,000 rpm, 5℃, 10 min). Johnson et al., 1995). Similarly, the degradation kinetics of L*, a*, b*
Afterward, the absorptions were measured at 450 nm using a Varian values were calculated using the first-­order kinetic model, while ΔE
Cary 50 Scan (Austria) spectrophotometer. The results were ex- values were computed the zero-­order kinetic model (Equation 6)
pressed as β-­carotene equivalents per mg of the liter. (Ahmed et al., 2002; Kardile et al., 2019):

TA B L E 1 Mathematical models used for concentration of orange juice

Model names Model References

Lewis B − B 0 = exp(−kt) Assawarachan and Noomhorm (2008)

Henderson and Pabis B − B 0 = a.exp(−kt) Assawarachan and Noomhorm (2011)
Modified Henderson and Pabis B − B 0 = a.exp(−kt) + b.exp(−g.t) + c.exp(−ht) Goula et al. (2014)
Logarithmic B − B 0 = a.exp(−kt) + c Assawarachan and Noomhorm (2011)
Two-­term B − B 0 = a.exp(−kt) + b.exp(−k1t) Bozkir (2020)
Wang and Singh B − B 0 = 1 + at + bt2 Yaldiz et al. (2001)

Note: B and B 0 are total soluble solids of at any time and initial (°Brix), t is evaporation time (min), and a, b, c, g, h, k, and k1 are model constants.
4 of 12 | BOZKIR and TEKGÜL

C = C0 exp ( ± kt) , (5) 70, and 80℃ were 4.593, 7.116, and 8.817 gH2O/min, respectively
(Table 2). It was detected that the evaporation rates increased with
C = C0 ± kt, (6) increasing temperature (absolute pressure) in the two concentration
techniques. There was a statistical difference between the evapora-
where C is the number of bioactive substances during the con- tion rates of orange juices concentrated using the MVE and the RE
centration process at time t, C0 is the amount of bioactive substance at 60, 70, and 80℃ (p < .05). It was determined that the evapora-
initial, k is a kinetic rate constant, and t is the concentration–­time. tion rates of the MVE were higher than the RE at 60, 70, and 80℃.
Half-­life values (t1/2) of bioactive substances were computed Similarly, Assawarachan and Noomhorm (2008) reported that the
using the following Equation (7): evaporation rate of the MVE (185 W and 80 kPa) used for concen-
trating pineapple juices was higher than the RE (80 kPa). In another
ln2 (7) study conducted by the same researchers, it was reported that the
t1∕2 = .
k
evaporation rate of the MVE was higher than microwave and ro-
The relationship between the reaction rate constant and the tary evaporators (Assawarachan & Noomhorm, 2010). Bozkir and
temperature was calculated by the Arrhenius equation given below: Baysal (2017) detected that the evaporation rate (14.51 gH2O/min)
of apple juice concentrated using the MVE was higher than the RE
(4.33 gH2O/min). In another study, Assawarachan and Noomhorm
( )
Ea
k = ka exp − , (8)
RT (2012) detected that the evaporation rate of concentrated pineap-
ple juices using the MVE was observed to be more two times faster
where k, ka, Ea, R, and T were the kinetic rate constant at temperature than the RE. It was determined that the evaporation rate of concen-
T (K), the frequency factor, the activation energy (kJ/mol), the univer- trated black mulberry juices using the MVE significantly raised the
sal gas constant (8.314 J/mol·K), and the evaporation temperature (K), drying rate compared to the RE (Fazaeli, Hojjatpanah, et al., 2013).
respectively (Ahmed et al., 2002; Johnson et al., 1995). Yousefi et al. (2012) reported that pomegranate juice concentrated
using the MVE significantly increased the evaporation rate (0.007–­
0.014 min−1) in comparison with the RE (0.006–­0.009 min−1) at 7.3,
2.11 | Statistical analysis 38.5, and 100 kPa.
The changes in total soluble solids during the RE and the MVE
The results were statistically analyzed by analyzing variance processes are presented in Figure 2. The required concentration
(ANOVA) using the software SPSS 20 (SPSS Inc., Chicago, IL, USA). times of concentrated orange juice were 38, 33.5, and 21 min at 60,
The differences between the treatments were evaluated with inde- 70, and 80℃ for the MVD, while the concentration times were 80,
pendent samples T-­test and Duncan test at p < .05. The concentra- 52, and 42 min for the RE, respectively. Likewise, Assawarachan and
tion experiments were repeated three times, and all measurements Noomhorm (2012) determined the time required for concentration
were triplicated. to the MVE and the RE as 37.5 and 88.5 min, respectively. Bozkir and
Baysal (2017) decided that the concentration–­time (27 min) of apple
juice concentrated using the MVE was lower than the RE (90 min).
3 | R E S U LT S A N D D I S CU S S I O N The times required to produce pineapple juices concentrated using
the microwave vacuum, microwave, and rotary evaporators were 23,
3.1 | Concentration kinetics and evaporation rate 38, and 50 min, respectively (Assawarachan & Noomhorm, 2010).
Moreover, it was reported that pineapple juice, pomegranate juice,
The initial total soluble solids of orange juices were detected as raspberry juice, black mulberry juice, grape juice, and black carrot
12 ± 0.05 °Brix and concentrated to 42 ± 0.10 °Brix. The evapora- juice concentrated using the MVE decreased the concentration-­time
tion rates of the MVE at 60, 70, and 80℃ were 9.765, 11.063, and significantly compared to the RE (Assawarachan & Noomhorm, 2011;
17.660 gH2O/min, respectively. The RE's evaporation rates at 60, Dinçer et al., 2019; Fazaeli, Hojjatpanah, et al., 2013; Fazaeli, Yousefi,

TA B L E 2 The evaporation rates

Vacuum microwave
for orange juices under different
Rotary evaporation evaporation
Absolute pressure concentration techniques
(kPa) Temperature (℃) Evaporation rate (gH2O/min)

21 60 4.593 ± 0.177c,B 9.765 ± 0.469c,A

31 70 7.116 ± 0.166b,B 11.063 ± 0.510 b,A
a,B
47 80 8.817 ± 0.403 17.660 ± 0.793a,A

Note: Different subscripts (a to c) symbolize significant differences within columns (p < .05).
Different subscripts (A to B) symbolize significant differences within lines (p < .05).
BOZKIR and TEKGÜL | 5 of 12

F I G U R E 2 The changes in total soluble solids during the evaporation processes (a) MVE 60℃, MVE 70℃, MVE 80℃, (b) RE
60℃, RE 70℃, RE 80℃

et al., 2013; Hojjatpanah et al., 2011; Yousefi et al., 2012). The or- Page model was the best fitting model for pineapple juice concentra-
ange juice's initial temperature was measured as 4℃ in the MVE and tion by the MVE. It was detected that the first-­order kinetic model
the RE systems. The temperatures of orange juice concentrate under was the most suitable model for pomegranate and black mulberry
absolute 20, 31, and 47 kPa pressures were 64.7, 74.6, and 84.5℃, juices concentrated using the MVE and the RE (Fazaeli, Yousefi,
respectively (Figure 3). et al., 2013; Yousefi et al., 2012). Goula et al. (2014) declared that
The regression coefficient (R 2), root means square error (RMSE), the logarithmic model gave better results in the pomegranate juice
2
and chi-­square (χ ) values have adequate prediction ability. It was concentrated using the RE. Sabanci and Icier (2017) reported that
detected that R 2 values (0.915–­
0.998) were higher than 0.90 in the Midilli model was the most suitable model for sour cherry juice
all the mathematical models. As shown in Table 3, the highest R 2, concentrated by ohmic heating-­assisted vacuum evaporation.
the lowest RMSE, and the lowest χ2 values were acquired from the
Logarithmic, the Logarithmic, and the Wang and Singh models for the
RE 60, 70, and 80℃, respectively. The Logarithmic, the Logarithmic, 3.2 | Degradation kinetics of vitamin C, TPC,
and the Wang and Singh were the best-­chosen models for concen- and TCCs
trated orange juice using the MVE at 60, 70, and 80℃ with the high-
est R 2 values (0.995–­0.998) and the lowest RMSE (0.3852–­0.7414) The initial vitamin C content of the fresh orange juice was de-
and χ2 values (0.1979–­0.8245). However, there are a limited number tected as 80.42 ± 2.21 mg/100 ml. The degradation rate constants
of studies in the literature model the concentration of fruit juices. for vitamin C of the RE at 60, 70, and 80℃ were 0.609, 0.954, and
Assawarachan and Noomhorm (2011) reported that the modified 1.336 hr−1. The degradation rate constants of the MVE at 60, 70, and
6 of 12 | BOZKIR and TEKGÜL

FIGURE 3 The changes in temperature of orange juice during the concentration processes

80℃ were 0.382, 0.658, and 0.806 hr−1, respectively (Table 4). The and 0.320 hr−1, respectively. It was detected that the k values sig-
differences between the rate constants of orange juices concen- nificantly increased with raising the temperature in the RE (p < .05),
trated using the RE and the MVE were statistically significant under whereas the k values of the MVE significantly decreased (p < .05).
absolute 20, 31, and 47 kPa pressures (p < .05). Lima et al. (1999) It was determined that the MVE preserved the TPCs compared to
used ohmic heating and traditional heating for the pasteurization of the RE. This is thought to be due to shortening the evaporation time
orange juices. They observed that vitamin C's degradation rate dur- of MVE or releasing some phenolic compounds bound in the juices.
ing ohmic heating and conventional heating increased in tempera- Similarly, Saikia et al. (2016) used microwave heating and traditional
ture values from 65 to 90℃. The activation energies of the vitamin C heating for pineapple and watermelon juices' pasteurization. They
for the RE and the MVE were determined as 38.487 (R 2 = 0.996) and detected that microwave heating preserved and increased its TPCs
36.708 (R 2 = 0.965) kJ/mol. Johnson et al. (1995) determined that compared to conventional heating. It was determined that k values
the activation energy for vitamin C of the orange juice concentrate of the MVE were lower than the RE at 60, 70, and 80℃. Likewise,
varied between 97.48 and 120 kJ/mol. It was detected that the half-­ Bozkir and Baysal (2017) reported that the difference between apple
life time (t1/2) of vitamin C of orange juice decreased because vita- juice's TPC concentrated using the MVE and the RE were statistically
min C was highly affected by concentration temperature. Vitamin C significant (p < .05). Similarly, Hojjatpanah et al. (2011) determined a
could be degraded by factors such as oxygen presence, temperature, statistically significant difference between the TPC of concentrated
and light. This degradation mechanism has increased even more in black mulberry juice using the MVE compared to the RE. They re-
the presence of high temperatures and oxygen (Gregory, 1996). ported that the reaction rate constants for the TPC of the MVE were
Consequently, it was determined that the vitamin C degradation of lower than the RE. In another study, it was determined that there
the RE was more than the MVE. Likewise, Vieira et al. (2000) de- was a difference between the reaction rate constants for total phe-
clared that anaerobic conditions reduced ascorbic acid degradation nolic substances, total anthocyanin, and antioxidant contents of the
by half or one-­third in cupuaçu juice (Figure 4). two raspberry juices concentrated with the MVE and the RE (Yousefi
The initial TPCs of fresh orange juices were 698.00 ± 16.90 mg et al., 2013). The activation energies of the TPC for the RE, and the
gallic acid equivalent (GAE)/L. Ramful et al. (2011) reported that cit- MVE were detected as 52.854 (R 2 = 0.941) and 24.792 (R 2 = 0.965)
rus juices' TPC varied between 406 and 1694 mg GAE/L. It was de- kJ/mol, respectively. The half-­life time for the TPC of orange juice
tected that the TPCs of the orange juice samples used in the study concentrated using the RE was 1.628 hr at 60℃, but it was reduced
were compatible with the values found in previous studies. The to 0.555 hr at 80℃. However, it was detected that the half-­life time
degradation rate constants for TPCs of concentrated orange juice for the TPC of orange juice concentrated using the MVE increased
using the RE at 60, 70, and 80℃ were 0.426, 0.936, and 1.429 hr−1, from 1.306 to 2.165 hr (Figure 5).
respectively. The reaction rate constants for the TPC of orange juice In this study, the initial TCCs in fresh orange juices were detected
concentrated using the MVE at 60, 70, and 80℃ were 0.531, 0.376, as 12.57 ± 0.05 mg/L. It was reported that the total carotenoid of
BOZKIR and TEKGÜL | 7 of 12

TA B L E 3 Statistical results obtained from different mathematical models for concentrating orange juices

Rotary evaporator Vacuum microwave evaporator

Models Parameter 60℃ 70℃ 80℃ 60℃ 70℃ 80℃

Lewis k −0.043 −0.068 −0.083 −0.089 −0.104 −0.165

X2 1.6382 10.2173 7.8653 1.7028 3.7355 2.9014
RMSE 3.0191 2.9900 2.5965 1.2303 1.8222 1.5333
R2 0.974 0.915 0.940 0.984 0.963 0.974
Henderson and Pabis k −0.039 −0.052 −0.066 −0.104 −0.086 −0.143
a 1.391 2.132 1.963 0.583 1.709 1.541
2
X 2.3248 5.0521 4.2392 0.8512 1.6138 1.6884
RMSE 1.3447 1.9466 1.7401 0.8136 1.1204 1.1153
2
R 0.980 0.959 0.969 0.994 0.983 0.985
Modified Henderson k −0.014 −0.052 −0.066 −0.104 −0.086 −0.143
and Pabis a −15.733 0.697 0.655 0.258 0.479 0.483
g −0.021 −0.052 −0.066 −0.104 −0.086 −0.143
b 8.702 0.711 0.654 0.215 0.709 0.527
h −0.021 −0.052 −0.066 −0.104 −0.086 −0.143
c 6.304 0.724 0.655 0.111 0.521 0.531
X2 3.5946 15.1564 21.1769 1.8548 3.7656 4.9753
RMSE 1.0946 1.9466 1.7393 0.7863 1.1204 1.1153
R2 0.995 0.959 0.969 0.994 0.983 0.985
Logarithmic k −0.028 −0.031 −0.041 −0.096 −0.060 −0.105
a 3.683 8.13 6.797 0.82 4.663 3.834
c −4.534 −9.21 −7.80 −0.905 −5.168 −4.362
X2 0.8168 1.9837 1.5756 0.8245 0.2531 0.4187
RMSE 0.7379 1.1135 0.9489 0.7414 0.4108 0.5116
R2 0.994 0.987 0.992 0.995 0.998 0.997
Two term k −0.039 −0.052 −0.066 −0.104 −0.086 −0.143
a 0.736 1.066 0.982 0.215 0.787 0.785
k1 −0.039 −0.052 −0.066 −0.104 −0.086 −0.143
b 0.655 0.1066 0.982 0.368 0.922 0.756
X2 3.2547 7.5782 7.0590 1.1137 2.2594 2.4877
RMSE 1.3447 1.9466 1.7393 0.7866 1.1204 1.1153
R2 0.980 0.959 0.969 0.994 0.983 0.985
Wang and Singh a −0.095 −0.014 −0.055 −0.425 −0.094 −0.269
b 0.006 0.011 0.018 0.03 0.028 0.079
2
X 1.1836 1.7257 0.8056 2.1852 0.2595 0.1979
RMSE 0.9595 1.3377 0.7586 1.3037 0.4492 0.3852
2
R 0.997 0.990 0.994 0.983 0.997 0.997

citrus juices varied between 6.4 and 31.8 mg/L (Bozkir et al., 2015; and the MVE was 17.29%–­20.43% and 6.68%–­9.91%, respectively.
Gama & de Sylos, 2007). The reaction rate constants for the TCC A study by Lessin et al. (1997) determined that there was a 36% loss
of orange juice concentrated using the RE at 60, 70, and 80℃ were in carotenoids (α-­carotene, β-­carotene, and β-­cryptoxanthin) of or-
0.514, 0.743, and 1.073 hr−1, respectively. The degradation rate ange juice due to the effect of heat treatment. Gama and de Sylos
constants for TCC of orange juice concentrated using the MVE at (2007) reported that the degradation for TCCs of orange juice con-
−1
60, 70, and 80℃ were detected 0.407, 0.582, and 0.803 hr , re- centrated was 17.15%. In another study, it was reported that there
spectively. It was found that the k values significantly raised with was significant degradation of carotenoids (α-­carotene, β-­carotene,
increasing temperature in the RE and the MVE techniques (p < .05). β-­apo-­8-­carotenal, α-­cryptoxanthin, β-­cryptoxanthin, xanthophyll,
The degradation for TCCs of orange juice concentrated using the RE, and zeaxanthin) and TCC of orange juice because of the effect of
 8 of 12 | BOZKIR and TEKGÜL

(R2 = 0.943)

(R2 = 0.998)
(R2 = 0.965)
Ea (kJ/mol)

33.221
36.708

24.792
t1/2 (hr)

1.306
0.860

0.863
1.233
1.842
1.053
1.815

1.703
2.165
Vacuum microwave evaporation

0.658 ± 0.006b,B

b,B

0.803 ± 0.003a,B
0.376 ± 0.028b,B
0.531 ± 0.012a,A

c,B

c,B
c,B

a,B
0.382 ± 0.002

0.320 ± 0.005
0.407 ± 0.005
0.582 ± 0.005
0.806 ± 0.007
k (hr−1)

0.990

0.920

0.963
0.991
0.958

0.973

0.973
0.913
0.976
The degradation kinetic parameters of bioactive components of orange juices concentrated under concentration processes

R2

(R2 = 0.999)
(R = 0.996)

(R = 0.941)
Ea (kJ/mol)

38.487

52.854

35.927
2

2
t1/2 (hr)

0.646
1.347
1.628

0.555
1.138
0.727

0.932
0.740
0.519

F I G U R E 4 The degradation kinetics of vitamin C of orange

b,A

b,A
c,A
c,A

a,A
a,A
0.954 ± 0.011b,A

1.073 ± 0.011a,A
0.426 ± 0.014 c,B

juices during the concentration processes (a) RE 60℃, RE 70℃,

0.514 ± 0.006
0.609 ± 0.002

0.743 ± 0.005
0.936 ± 0.034
1.249 ± 0.031
1.336 ± 0.015

RE 80℃, (b) MVE 60℃, MVE 70℃, MVE 80℃

Rotary evaporation

k (hr−1)

Note: Different subscripts (a to c) symbolize significant differences within columns (p < .05).

heat treatment (Bozkir et al., 2015). It was detected that the activa-
tion energy for the TCC of the MVE (33.221 kJ/mol, R 2 = 0.998) was
Different subscripts (A to B) symbolize significant differences within lines (p < .05).
0.999
0.993

0.993
0.998

0.998
0.998
0.985
0.996

lower than the RE (35.927 kJ/mol, R 2 = 0.999). It was determined

0.974
R2

that the half-­life time (t1/2) for the TCC of orange juice decreased
because the TCC was positively affected by processing temperature
(Figure 6).

3.3 | Degradation kinetics of color values

Temperature

The L*, a*, and b* values of fresh orange juice were determined as
61.14 ± 0.20, 7.30 ± 0.80, and 55.72 ± 0.24, respectively. It was
(℃)

detected that the reaction rate constants for L* changed between

60
70
80
60
70
80
60
70
80

0.026 and 0.049 hr−1 for the RE, and the values varied between
0.019 and 0.032 hr−1 for the MVE. The differences between the re-
Total carotenoid content (mg/L)
Total phenolic content (mg/L)

action rate constants of orange juices concentrated using the MVE

and the RE were statistically significant at 60, 70, and 80℃ (p < .05).
Bozkir and Baysal (2017) reported that the L* value of apple juice
concentrated using the MVE was higher than the RE. Assawarachan
and Noomhorm (2012) detected that the L*/L0 (0.984 ± 0.002) of
(mg/100 ml)
Parameters

Vitamin C
TA B L E 4

concentrated pineapple juices using the MVE was found to be higher

than the RE (L*/L0 (0.952 ± 0.001)). In another study, it was reported
that first-­order kinetic coefficients (k × 10−2) for L* color values
BOZKIR and TEKGÜL | 9 of 12

F I G U R E 5 The degradation kinetics of total phenolic content of

orange juices during the concentration processes (a) RE 60℃, F I G U R E 6 The degradation kinetics of total carotenoid content
RE 70℃, RE 80℃, (b) MVE 60℃, MVE 70℃, MVE 80℃ of orange juices during the concentration processes (a) RE 60℃,
RE 70℃, RE 80℃, (b) MVE 60℃, MVE 70℃, MVE 80℃

of vacuum microwave, microwave, and rotary evaporators were

0.033 ± 0.01, 0.141 ± 0.03, and 0.064 ± 0.01 min−1, respectively and 1.958 min−1, respectively (Assawarachan & Noomhorm, 2010).
(Assawarachan & Noomhorm, 2010). The first-­degree kinetic coef- In another study, the pineapple juice's degradation rate con-
ficient (k × 10−3) of the pineapple juice's L* color values concentrated stants a* values concentrated using the MVE was determined as
using the MVE was determined as 0.041 ± 0.01 min−1, whereas it 6.67 ± 0.63 min−1, whereas it was detected as 15.37 ± 0.72 min−1 in
−1
was detected as 0.054 ± 0.01 min in the RE (Assawarachan & the RE (Assawarachan & Noomhorm, 2008). Moreover, it was deter-
Noomhorm, 2008). Furthermore, it was reported that the MVE mined that the MVE preserved the a* values of concentrated black
preserved the L* values of concentrated black mulberry juice and mulberry juice and concentrated pomegranate juice compared to the
concentrated pomegranate juice in comparison with the RE (Fazaeli, RE (Fazaeli, Yousefi, et al., 2013; Yousefi et al., 2012) (Table 5).
Yousefi, et al., 2013; Yousefi et al., 2012). There were statistically significant differences between the deg-
The degradation rate constants for a* value of orange juice con- radation rate constants of orange juices concentrated using the MVE
centrated using the RE at 60, 70, and 80℃ were 0.195, 0.307, and and the RE (p < .05). Similarly, Bozkir and Baysal (2017) determined
−1
0.362 hr . The reaction rate constants for a* value of orange juice a significant difference between the b* value of apple juice con-
concentrated using the MVE at 60, 70, and 80℃ were 0.172, 0.221, centrated using the MVE and the RE. It was reported that the MVE
and 0.331 hr−1. There were statistically significant differences be- preserved the b* values of concentrated black mulberry juice, con-
tween the degradation rate constants of orange juices concentrated centrated pineapple juice, and concentrated pomegranate juice in
using the MVE and the RE (p < .05). Bozkir and Baysal (2017) re- comparison with the RE (Assawarachan & Noomhorm, 2008, 2010,
ported that the a* value of apple juice concentrated using the MVE 2012; Fazaeli, Yousefi, et al., 2013; Yousefi et al., 2012).
was higher than the RE. Assawarachan and Noomhorm (2012) de- The rate constants for total color difference (ΔE) of orange juice
tected that the a*/a 0 (0.942 ± 0.001) of concentrated pineapple concentrated using the MVE at 60, 70, and 80℃ were 2.701, 3.497,
juices using the MVE was higher than the RE (a*/a 0 (0.848 ± 0.015)). and 4.423 hr−1, respectively. The degradation constants for ΔE of
In another study conducted by the same researchers, it was reported orange juice concentrated using the RE at 60, 70, and 80℃ were
that the degradation rate constants for a* color values of vacuum 2.926, 4.158, and 5.494 hr−1, respectively. The least change in the ΔE
microwave, microwave, and rotary evaporators were 0.724, 3.771, was found in orange juices concentrated using the MVE compared
 10 of 12 | BOZKIR and TEKGÜL

to the RE. Likewise, Bozkir and Baysal (2017) reported that the ΔE
value of apple juice concentrated using the MVE was lower than the

(R2 = 0.993)

(R2 = 0.999)
(R2 = 0.966)
RE. Assawarachan and Noomhorm (2012) determined that the ΔE

(R2 = 0.976)
Ea (kJ/mol)
value (0.676 ± 0.004) of concentrated pineapple juices using the

18.882
26.631

31.819

24.131
MVE was lower than the RE (2.237 ± 0.092). In another study, it
was reported that the zero-­order kinetics coefficients (k × 10−2) for
ΔE values of vacuum microwave, microwave, and rotary evaporators
were 8.365, 25.341, and 14.337 min−1, respectively (Assawarachan
t1/2 (hr)

25.530

15.301
11.505
2.093

0.257
36.870

21.426
4.019

0.157
19.148

0.198
3.141 & Noomhorm, 2010). In another study, the zero-­order kinetics coef-
ficients (k × 10−3) for the ΔE values of the pineapple juice concen-
trated using the MVE was determined as 15.37 ± 0.72 min−1, while
it was detected as 24.01 ± 0.42 min−1 in the RE (Assawarachan &
Vacuum microwave evaporation

0.172 ± 0.004c,B
0.027 ± 0.002b,B

b,B

0.060 ± 0.003a,B
a,B

c,B
0.221 ± 0.016b,B

3.497 ± 0.188b,B
c,B

a,B
a,B

2.701 ± 0.027c,B
Noomhorm, 2008).
0.032 ± 0.002

0.036 ± 0.002
0.045 ± 0.002
0.019 ± 0.001

4.423 ± 0.041
0.331 ± 0.011

According to the results, it was determined that the activation

energies for the L*, a*, b*, and ∆E of the MVE were lower than the
k (hr−1)

RE. It was detected that the half-­life time (t1/2) for the L*, a*, b*, and
∆E of orange juice decreased because the L*, a*, b*, and ∆E were
positively affected by processing temperature. The decreases in
The degradation kinetic parameters of the color values of orange juices concentrated under concentration processes

the half-­life time indicated that the stability of the L*, a*, b*, and ∆E
0.900
0.820
0.865

0.872
0.980

0.940
0.948
0.929

0.907

0.924
0.914

0.951

decreased depending on the temperature. It was determined that

R2

the MVE caused the least change in the color values (L*, a*, b*, and
∆E) examined and calculated compared to the RE. This situation is
thought to be due to the less exposure of orange juices to heat, the
short evaporation time, or the high evaporation rate in the micro-
(R2 = 0.997)

(R = 0.999)
(R = 0.995)

(R = 0.941)

wave vacuum evaporator.

Ea (kJ/mol)

30.430

30.832
25.616
31.112
2

4 | CO N C LU S I O N
Note: Different subscripts (a to c) symbolize significant differences within columns (p < .05).

The orange juices were successfully concentrated by MVE and

t1/2 (hr)

9.888
26.866
18.633
14.233

0.237
2.259
3.558

16.702
1.915

13.103

0.126
0.167

RE under various operational pressures. The MVE significantly in-

creased evaporation rates in comparison with the RE. The MVE de-
Different subscripts (A to B) symbolize significant differences within lines (p < .05).

creased the required concentration–­time of orange juices compared

to the RE. It was detected that the degradation kinetics for vitamin
0.037 ± 0.003b,A

b,A

b,A
a,A

b,A
a,A

0.070 ± 0.002a,A

a,A
c,A

c,A

2.926 ± 0.074c,A
0.195 ± 0.011c,A

C, TPC, and TCC of orange juices concentrated using the MVE was
0.362 ± 0.008

0.053 ± 0.003
0.049 ± 0.003

0.307 ± 0.003
0.026 ± 0.002

0.042 ± 0.002

5.494 ± 0.005
4.158 ± 0.253

lower than the RE. Results showed that the degradations for the L*,
a*, b*, and ∆E of orange juices concentrated using the RE was more
k (hr−1)
Rotary evaporation

than the MVE. Depending on this study it was determined that it is

possible to predict and understand the degradation rates in bioac-
tive compounds and color values that occur in orange juices concen-
trated by using MVE and RE according to zero-­order and first-­order
0.867

0.934
0.902

0.922
0.901
0.901

0.901
0.929

0.915
0.937
0.911

0.952

kinetic models.
R2

C O N FL I C T O F I N T E R E S T
Temperature

The authors have declared no conflicts of interest for this article.

(℃)

AU T H O R C O N T R I B U T I O N S
60
70
80
60
70
80
60
70
80
60
70
80

Hamza Bozkır: Conceptualization; Data curation; Formal analysis;

Investigation; Methodology; Project administration; Supervision;
Writing-­ review & editing. Yeliz Tekgül:
original draft; Writing-­
Parameters
TA B L E 5

Conceptualization; Data curation; Formal analysis; Investigation;

Methodology; Project administration; Supervision; Writing-­original
ΔE
a*

b*
L*

draft; Writing-­review & editing.

BOZKIR and TEKGÜL | 11 of 12

ORCID Fazaeli, M., Yousefi, S., & Emam-­Djomeh, Z. (2013). Investigation on the
effects of microwave and conventional heating methods on the
Hamza Bozkir https://orcid.org/0000-0002-8868-697X
phytochemicals of pomegranate (Punica granatum L.) and black mul-
Yeliz Tekgül https://orcid.org/0000-0001-8173-023X berry juices. Food Research International, 50, 568–­573. https://doi.
org/10.1016/j.foodr​es.2011.03.043
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