a r t i c l e i n f o a b s t r a c t
Article history: The aim of the present study was to investigate the effect of different drying conditions on the char-
Received 22 March 2017 acterization of pectin extracted from sugar beet pulp pectin. Sugar beet pulp pectin produced by hot air-
Received in revised form drying (40, 50, 60 C), vacuum-drying (40, 50, 60 C), freeze-drying, spray-drying (160, 190, 220 C) were
17 April 2017
evaluated for their apparent viscosity, activation energy, chemical structure, degree of esterification and
Accepted 18 April 2017
Available online 21 April 2017
emulsifying properties. The results indicated that the drying conditions affected the apparent viscosity
and activation energy of all pectin samples. FTIR (Fourier transform infrared spectroscopy) spectral
analysis showed no major structural differences in sugar beet pectin produced by various drying con-
Keywords:
Sugar beet pulp pectin
ditions. The zeta-potential and conductivity for different dried samples were from 47.9 to 55.6 mV
Drying condition and 0.0079 to 0.0095 mS/cm, respectively. Drying conditions had significant effects on the emulsifying
Rheological property properties of the sugar beet pulp pectin emulsions.
Emulsifying property © 2017 Elsevier Ltd. All rights reserved.
1. Introduction et al., 2015). SBP has high pectin content on dry basis and pectin
extracted from SBP exhibits superior emulsifying properties than
Pectin, extracted from cell wall material using chemical or from other sources (Ma et al., 2013). Sugar beet pulp pectin (SBPP)
enzymatic methods under different conditions, is an anionic poly- possess better surface-active and emulsifying properties mainly
saccharide. Pectin has been widely used as food additives: as gelling because of a higher amount of protein. The enzymatic modification
agent in jams and jellies; as fillers or stabilizer in confections, dairy decrease of the protein content from 1.56% to 0.13% without
products, fruit preparations, bakery fillings, icings and frostings in significantly other composition change decreased the emulsifying
food industry (Kalapathy and Proctor, 2001; Li et al., 2012). Pectin is activity and stabilizing ability (Funami et al., 2007). The SBPP
the most complex macromolecules found in nature that consists of contains ample amount of soluble dietary fiber which is crucial in
a backbone in which of a-D-(1e4)-galacturonanregions are inter- functional and health foods and contains galacturonic acid, rham-
rupted by ramified rhamnogalacturonanregions, highly substituted nose, arabinose and galactose as main sugar constituents (Lv et al.,
by neutral sugar-rich side chains (Constenla et al., 2002; Westereng 2013).
et al., 2008). Commercial pectin is mainly extracted from citrus Pectin extracted from sugar beet pulp can be obtained at high
peel, apple pomace and sugar beet pulp, especially from the former temperature in the present of acid on a laboratory and factory scale
two (Li et al., 2012). (Levigne et al., 2002; Yapo et al., 2007). Recently, the character-
As a by-product of the sugar-refining industry, sugar beet (Beta ization of pectin under different extraction methods and conditions
vulgaris) pulp (SBP) is generally used for feed formulation, with few were studied (Ma et al., 2013; Westereng et al., 2008; Yapo et al.,
commercial value. Meanwhile the process often generates an 2007). Drying process plays an important role in the extraction
environmental problem. Therefore, multiple attempts have been procedure of natural plant gums, pectin included (Amid and
used to utilized to make the best use of these byproducts (Chen Mirhosseini, 2012). Different drying conditions have been applied
in the related studies about pectin by previous researchers. Several
techniques have been employed for the drying of pectin including
* Corresponding author. hot air-dying (HD), vacuum-drying (VD), freeze-drying (FD), spray-
E-mail address: wlj@cau.edu.cn (L.-j. Wang).
http://dx.doi.org/10.1016/j.jfoodeng.2017.04.022
0260-8774/© 2017 Elsevier Ltd. All rights reserved.
2 X. Huang et al. / Journal of Food Engineering 211 (2017) 1e6
drying (SD), and many others (Chen et al., 2015; Kontogiorgos et al., squeezed in a nylon cloth to remove the ethanol. Then the SBPPwas
2012; Koubala et al., 2008; Kratchanova et al., 2004; Yapo et al., washed three times with ethanol (analytical pure). After purifica-
2007). tion, the wet pectin was dried by different drying conditions.
Constenla et al. (2002) evaluated the effect of different air
temperature on apple pectin characteristics. They reported that the 2.3. Drying of pectin
degree of esterification and molecular weight depended on the air
temperature. Amid and Mirhosseini (2012) investigated the influ- In present study, four different drying methods (HD, VD, FD, SD)
ence of different purification and drying methods on rheological were used to dry the pectin precipitates. Samples produced by
properties and viscoelastic behavior of durian seed gum. The study different drying conditions were milled and exposed to potassium
indicated that all drying methods diminished the elastic and acetate saturated solution at 25 C for more than one week until no
viscous modulus, which the freeze-drying and oven-drying had the significant change of weight (0.001 g) was observed. The moisture
highest and the lowest viscous modulus. The effects of drying content of the SBPP samples was 5.8% on wet basis (w.b.)which
methods on the rheological and functional properties of flaxseed determined using a moisture analyzer (HB 43-S, Mettler-Toledo,
gum were studied. The results showed that drying methods Switzerland). Then the samples were sealed and stored at 4 C for
decreased the apparent viscosity and increased the activation en- the following analysis.
ergy slightly. Meanwhile different drying methods influenced zeta
potential, foaming and emulsion properties of flaxseed gum. Re- 2.3.1. Hot air drying
sults showed that researchers could select appropriate drying The purified wet pectin was dispersed in water in a glass plate
method and condition depending on characterization needed (direct 30 cm, 5 mm thick) and then dried in a hot air oven (model
(Wang et al., 2010b; Wang et al., 2009). 101-3, Shanghai Luda Experimental Instrument Co., Shanghai,
The purpose of this study was to explore the influence of China) at 40,50,60 C for 8 h, respectively. The hot air-drying was
different drying conditions on the rheological and emulsifying according to the previous researchers with slightly modification
properties of sugar beet pulp pectin. In the present study, four (Koubala et al., 2008; Kratchanova et al., 2004).
different drying techniques (i.e., HD (40, 50, 60 C), VD (40, 50,
60 C), FD, SD (160, 190, 220 C))were chosen to study the char- 2.3.2. Vacuum drying
acterization of dried SBPP. To the best of our knowledge, there is no The vacuum drying was carried out using a DZ-3 vacuum drier
similar published report investigating the effect of drying condi- (Tianjin Taisite Instrument Co., Tianjin, China). The purified wet
tions on the rheological and emulsifying behavior of sugar beet pectin was dispersed in water in a glass plate and the temperature
pulp pectin. was set at 40, 50, 60 C for 8 h, respectively. The vacuum pressure
was maintained at 0.1 MPa (14.5 psi). The vacuum drying
2. Material and methods method was based on previous researchers (Wang et al., 2009; Yapo
et al., 2007).
2.1. Materials
2.3.3. Freeze drying
SBP was supplied by COFCO Tunhe Co., Ltd. (Xinjiang, China), The purified pectin was dispersed in water and pre-frozen
with moisture content of 4.6%. This sugar beet pulp was dried and at 30 C for 2 h prior to freeze drying. Then the sample was
pulverized into powder to go through 60-mesh sieve using a high- freeze-dried in a LGJ-18S freeze dryer (Beijing Songyuan Huaxing
speed multifunction grinder (Bingdu Electrical Appliances Co., Ltd., Technology Develop Co., Beijing, China) for 8 h with the tempera-
Shanghai, China). The dried raw materials were then packed in ture ranged from 30 C to 20 C. The freeze dryer was equipped
plastic bags and stored in room temperature until the extraction with a temperature controller, which controlled the temperature to
process. All chemical reagents, including ethanol, hydrochloric acid increase steadily.
(HCl), ammonia solution (NH3$H2O), etc., used in this experiments
were analytical grade and purchased from Lanyi reagent company 2.3.4. Spray drying
(Beijing, China). The deionized water was performed in all the The purified pectin was diluted indeionized water according to
experiments. the previous researches. The extracted pectin solution was spray
dried using a bench-top spray drier (GPW120-II, Shandong Tianli
2.2. Pectin extraction Drying Equipment Inc., China). The inlet temperature and the
exhaust aspiration lever were set at 160, 190, 220 C and 95%,
Sugar beet pulp pectin, extracted from dry beet pulp material respectively. The outlet temperature was performed at 85e90 C.
using an acidified medium, was subjected to purification through The flow rate of the air was maintained at 0.1 m3/h. The feed rate
alcohol precipitation. Pectin extracted by traditional heating was 4 mL/min throughout the experiments. The dried pectin was
method according to our research previously was followed with collected at the bottom of the cyclone.
slightly modification (Lv et al., 2013). The sample (50 g)was mixed
with deionized water(1000 mL) in a 3000 mL beaker and then the 2.4. FTIR analysis and degree of esterification
pH of these suspensions was adjusted to 1.2 with 12 mol/L HCl. The
suspended samples were heated to 90 Cusing a temperature Fourier transform infrared spectroscopy (FTIR) spectra were
controlled water bath and extraction was carried out with contin- tested in the range 4000 to 650 cm1 with 32 scans at a resolution of
uous stirring at 200 rpm for 3 h by a digital mechanical agitator 4 cm1using a Varian 600-IR FTIR spectrometer (Varian, Palo Alto,
(RW 20; IKA, Staufen, Germany). After the reaction was completed, CA, USA). The degree of esterification (DE) of pectin was determined
the resulting slurries were cooled down to 40 C, and then the pH according to the method described by Mesbahi et al. (2005).
was adjusted to 4.5 with 25 g/100 g NH3$H2O and filtered using a
Buchner funnel under vacuum condition. The filtrate was collected 2.5. Rheological characterization
and stored in a refrigerator at 4 C for subsequent purification.
One volume of crude pectin was precipitated using two volumes Samples were dissolved indeionized water using a magnetic
of 95 mL/100 mL ethanol for 1 h at an ambient temperature, then stirrer for 1 h at ambient temperature. The concentration was
X. Huang et al. / Journal of Food Engineering 211 (2017) 1e6 3
2.5.1. Apparent viscosity where Ø is oil volume fraction of the dispersed phase and c is the
The apparent viscosity of the samples was determined using concentration of pectin in emulsion.
AR2000 exrheometer (TA Instruments Ltd., New Castle, DE, USA).
The temperature was controlled using a water bath connected to 2.6.2. Zeta potential and conductivity
the Peltier system. Flow curves over the shear rate (1-100s1) were Zeta-potential of SBPP emulsions weremeasured by dynamic
measured at 25 C using an aluminum plate geometry (40 mm light scattering using Malvern Zetasizer NanoZS (Malvern In-
diameter, 1 mm gap). Each sample was tested in triplicate. The struments, Worcestershire, UK). Emulsions were diluted to a final
apparent viscosity and steady shear rate measurement were fitted oil droplet concentration of 0.053 g/L withpH-adjusted deionized
to the Hershel-Bukley models (Eq. (1)) (Wang et al., 2011): water to avoid multiple scattering effects. Then the emulsions were
injected into the clear disposable zeta cell. Refractive index of 1.45
s ¼ s0 þ k$gn (1) and 1.33were used for the oil droplet and the solvent, respectively.
All the tests were measured at 25 C with equilibration time of
where s is the shear stress (Pa), s0is the yield stress (Pa), k is the 120s. The conductivity of solutions was also measured at the same
consistency index (Pa$sn), gis shear rate (s1), n is the flow behavior time (Wang et al., 2010a). The zeta-potential and conductivity of
index. the emulsion droplets were measured based on the measuring
technique combined electrophoresis method with laser Doppler
velocimetry method and according to the direction and rate of the
2.5.2. Activation energy measurement
droplets in the applied electric field. Determinations were per-
The apparent viscosity was determined over temperatures
formed at least in triplicate.
range from 10 to 50 Cusing a strain controlled rheometer
(AR2000ex; TA Instruments Ltd., New Castle, DE, USA) at a constant
2.7. Statistical analysis
shear rate of 10 s1 with an aluminum plate geometry (40 mm
diameter, 1 mm gap). The influence of temperature on the apparent
All experiments were performed at least in triplicate. The FTIR
viscosity at a constant shear rate (10 s1) of 20 g/LSBPP solution can
data was disposed using the OPUS 7.2 software (Bruker, Billerica,
be calculated using the Arrhenius equation Eq. (2) (Wang et al.,
MA, USA). The rheological data was obtained from Rheology
2009):
Advantage Data Analysis V5.7.0 (TA Instruments Ltd., New Castle,
ha ¼ h∞ expðEa =RTÞ (2) DE, USA). The zeta-potential and conductivity data were obtained
from Zetasizer Software 7.01 (Malvern Instruments, Worcester-
where ha is the apparent viscosity at a specific shear rate, h∞ is the shire, UK). The data was evaluated by Duncan’s multiple compari-
frequency factor, Ea is the activation energy (kJ/mol), R is the gas son test (p < 0.05) using the statistical software SPSS 20.0 (SPSS Inc.,
constant (8.3145 J/mol K), and T is the absolute temperature (K). Chicago, IL, US).
2:303$A$V
T¼ (3)
I
Table 1
Degree of esterification (DE) and activation energy (Ea) of sugar beet pulp pectin produced by different drying conditions.
Results are presented as mean values ± standard deviation of triplicate tests.Different letters superscripted on the results were significantly different at p < 0.05.
functional groups in pectin and those spectral regions are used to ones. As can be concluded, low methoxyl pectins were obtained in
recognize different types of pectin (Pappas et al., 2004; Synytsya, this research and drying conditions had an effect on DE values.
2003). The FTIR spectra showed that there were no major struc-
tural differences in pectin produced by different drying methods. 3.2. Rheological characterization
The board around 2400 cm1 was due to adsorbed moisture in the
pectin samples. 3.2.1. Apparent viscosity
Bands between 1600 and 1800 cm1 are typically associated Drying processes greatly influence the viscosity and rheological
with identifying different types of pectin and the absorption bands properties of gum (Jaya and Durance, 2009). The present study also
at 1630e1650 and 1740-1750 cm1 are indicative of free and indicated that the viscosity of SBPP was affected by drying condi-
esterified carboxyl groups, respectively (Monsoor, 2005). It was tions. The flow behavior of the solutions of SBPP dried by different
observed that the carboxyl bands existed at 1649 and 1746 cm1 in methods and conditions is shown in Fig. 2(aec). The viscosity of the
the pectin spectra in this study. FTIR structure analysis indicated pectin dispersions decreases with shear rate increase which indi-
that drying methods had no detrimental effect on the structure of cating pseudoplastic (shear-thinning) flow behavior. Cui (2005)
SBPP from FTIR analysis which was consistent with the influence of reported that the viscosity of gum dispersions decreased due to
drying methods on the soy hull pectin and grewia polysaccharide decreasing number of chain entanglements at high shear rates with
gum (Monsoor, 2005; Nep and Conway, 2011). the increase of shear rate. In Fig. 2(a), temperature seems no impact
The Degree of esterification (DE) of pectin was from 38.6 to on the viscosity of samples dried by HD method with the presence
40.8% (Table 1) which was similar to the results of pectin extracted of oxygen and same drying time. The apparent viscosity of samples
from sugar beet pulp using traditional acid method (Ma et al., dried by VD method decreases with temperature increase from 40
2013). In the HD method, the DE values decreased with the tem- to 60 C in Fig. 2(b). Comparing with samples dried by HD, tem-
perature increase. The increase in temperature may destroy the perature has influence on the viscosity of samples in vacuum
methyl esterified carboxyl groups of the pectin side chains. The environment. Samples dried at high temperature using spray dry-
vacuum environment in VD method and the instantaneous drying ing (160, 190, 220 C) and at freezing temperature using freeze
process at high temperature in SD method made no obvious dif- drying has obvious difference in apparent viscosity; and SD190
ference on DE values. The HD 40 C sample had the highest DE Cand FD sample showed the highest and the least viscosity,
value. The DE values of SD samples were higher than the SD and FD respectively (Fig. 2(c)). Combined with the process of different
Fig. 2. Effect of drying conditions on the apparent viscosity of 20 g/L sugar beet pulp pectin solutions. (a) hot air-drying (HD), (b) vacuum-drying (VD), (c) freeze-drying (FD) and
spray-drying (SD).
X. Huang et al. / Journal of Food Engineering 211 (2017) 1e6 5
Table 3
Zeta potential and conductivity for sugar beet pulp pectin emulsions produced by
different drying conditions.HD, hot air-drying; VD, vacuum-drying; FD, freeze-
drying; SD, spray-drying.
properties (Leroux et al., 2003). The VD 50 C and the HD 40 C navel orange peel assisted by ultra-high pressure, microwave or traditional
heating: a comparison. Carbohydr. Polym. 88 (2), 441e448.
samples had the lowest and highest zeta-potential, respectively.
Jaya, S., Durance, T.D., 2009. Compressive characteristics of cellular solids produced
The temperature in SD method had little effect on zeta-potential using vacuum-microwave, freeze, vacuum and hot air dehydration methods.
values and the FD sample exhibited good emulsion stability. The J. Porous Mater. 16 (1), 47e58.
zeta-potential values were related to the DE ones. It could be Kalapathy, U., Proctor, A., 2001. Effect of acid extraction and alcohol precipitation
conditions on the yield and purity of soy hull pectin. Food Chem. 73 (4),
inferred that the high degree of esterification decreases the abso- 393e396.
lute value of zeta-potential. Khalil, M., Mohamed Jan, B., 2012. Herschel-Bulkley rheological parameters of a
The conductivity of emulsion can indicate the change of the novel environmentally friendly lightweight biopolymer drilling fluid from
xanthan gum and starch. J. Appl. Polym. Sci. 124 (1), 595e606.
emulsion stability over time. The low conductivity reflects a slow Kontogiorgos, V., Margelou, I., Georgiadis, N., Ritzoulis, C., 2012. Rheological char-
molecular mobility, this will retard the emulsion phase separation acterization of okra pectins. Food Hydrocoll. 29 (2), 356e362.
rate which guarantee the stability of the emulsion system Koubala, B.B., Mbome, L.I., Kansci, G., Tchouanguep Mbiapo, F., Crepeau, M.J.,
Thibault, J.F., Ralet, M.C., 2008. Physicochemical properties of pectins from
(Mirhosseini et al., 2009). The conductivity of emulsions was from ambarella peels (Spondias cytherea) obtained using different extraction con-
0.0079 to 0.0095 mS/cm which indicating that all emulsions had ditions. Food Chem. 106 (3), 1202e1207.
good emulsion stability. and showed significant (p < 0.05) differ- Kratchanova, M., Pavlova, E., Panchev, I., 2004. The effect of microwave heating of
fresh orange peels on the fruit tissue and quality of extracted pectin. Carbohydr.
ence. This observation was consistent with the ones made on the Polym. 56 (2), 181e185.
zeta-potential suggesting that drying conditions made an impact Leroux, J., Langendorff, V., Schick, G., Vaishnav, V., Mazoyer, J., 2003. Emulsion
on the emulsion stability. stabilizing properties of pectin. Food Hydrocoll. 17 (4), 455e462.
Levigne, S., Ralet, M., Thibault, J.O., 2002. Characterisation of pectins extracted from
fresh sugar beet under different conditions using an experimental design.
4. Conclusion Carbohydr. Polym. 49 (2), 145e153.
Li, D., Jia, X., Wei, Z., Liu, Z., 2012. BoxeBehnken experimental design for investi-
The current study showed that the effect of drying conditions gation of microwave-assisted extracted sugar beet pulp pectin. Carbohydr.
Polym. 88 (1), 342e346.
(hot air-drying (40, 50, 60 C), vacuum-drying (40, 50, 60 C), Lv, C., Wang, Y., Wang, L., Li, D., Adhikari, B., 2013. Optimization of production yield
freeze-drying, spray-drying (160, 190, 220 C)) on the character- and functional properties of pectin extracted from sugar beet pulp. Carbohydr.
ization of pectin extracted from sugar beet pulp. The results indi- Polym. 95 (1), 233e240.
Ma, S., Yu, S., Zheng, X., Wang, X., Bao, Q., Guo, X., 2013. Extraction, characterization
cated that all SBPP samples showed pseudo-plastic (shear- and spontaneous emulsifying properties of pectin from sugar beet pulp. Car-
thinning) flow behavior. Drying conditions affected the apparent bohydr. Polym. 98 (1), 750e753.
viscosity and activation energy of all SBPP samples. The FTIR Mesbahi, G., Jamalian, J., Farahnaky, A., 2005. A comparative study on functional
properties of beet and citrus pectins in food systems. Food Hydrocoll. 19 (4),
analysis showed that drying conditions had no effect on the 731e738.
structure of pectin and the degree of esterification ranged from 38.6 Mirhosseini, H., Tan, C.P., Hamid, N.S.A., Yusof, S., Chern, B.H., 2009. Characterization
to 40.8%. The results of emulsifying properties demonstrated that of the influence of main emulsion components on the physicochemical prop-
erties of orange beverage emulsion using response surface methodology. Food
all samples behaved good emulsifying activity and stability. Drying Hydrocoll. 23 (2), 271e280.
conditions made a significant difference on the characterization of Monsoor, M.A., 2005. Effect of drying methods on the functional properties of soy
pectin extracted from sugar beet pulp. hull pectin. Carbohydr. Polym. 61 (3), 362e367.
Nep, E.I., Conway, B.R., 2011. Physicochemical characterization of grewia poly-
saccharide gum: effect of drying method. Carbohydr. Polym. 84 (1), 446e453.
Acknowledgement Pappas, C.S., Malovikova, A., Hromadkova, Z., Tarantilis, P.A., Ebringerova, A.,
Polissiou, M.G., 2004. Determination of the degree of esterification of pectinates
This research was supported by The National Key Research and with decyl and benzyl ester groups by diffuse reflectance infrared Fourier
transform spectroscopy (DRIFTS) and curve-fitting deconvolution method.
Development Program of China (2016YFD0701801) and Common- Carbohydr. Polym. 56 (4), 465e469.
weal Guild Grain Scientific Research Program of China (201513004). Pongsawatmanit, R., Temsiripong, T., Ikeda, S., Nishinari, K., 2006. Influence of
tamarind seed xyloglucan on rheological properties and thermal stability of
tapioca starch. J. Food Eng. 77 (1), 41e50.
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