Effects of hydrocolloids on acorn starch physical

Starch/Stärke 2016, 68, 1–11

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DOI 10.1002/star.201500304

RESEARCH ARTICLE

Effects of hydrocolloids on acorn starch physical properties Mohammed Saleh 1, Radwan Ajo 2, Khalid Al-Ismail 1 and George Ondier 3 1

Department of Nutrition and Food Technology, The University of Jordan, Amman, Jordan Department of Applied Science, Al-Huson University College, Al-Balqa Applied University, Jordan 3 Taylor Laboratories, Inc., Houston, TX, USA 2

The effect of hydrocolloids (arabic gum, carrageenan, carboxymethyl cellulose, and xanthan gum) on the physical properties of acorn starch was investigated. First order mixture response surface model was used and the effects of 1% hydrocolloids on acorn starch water holding capacity, starch solution viscosity, gel strength, freeze–thaw stability, and pasting properties were evaluated. Contributions of each hydrocolloid on determining acorn starch functionality were also calculated. Hydrocolloid combinations significantly (p < 0.05) decrease acorn starch water holding capacity held at 23.3°C from 213.6% of 100% starch to less than 208.3% with minor exceptions. The increase in holding temperature, however, increased water holding capacity (WHC) irrespective of the hydrocolloids set used. The flow behavior indices of treatments ranged from 0.43 to 0.99 and were significantly (p < 0.05) greater than that of pure acorn starch (i.e., 0.66) for most treatments. The consistency coefficient of treatments were significantly (p < 0.05) greater than that of the control and were best fit for the shear-thickening model. Significant (p < 0.05) improvement in gel strength and decrease in freeze–thaw stability of treatments compared to the control was also reported. The pasting properties of treatments increased with the use of hydrocolloids, thus showing the significant role of hydrocolloids in dictating the pasting characteristics of the acorn–hydrocolloids interaction.

Received: November 8, 2015 Revised: January 4, 2016 Accepted: January 13, 2016

Keywords: Acorn starch / Hydrocolloids / Physical properties

1

Introduction

The use of oak (Quercus calliprinos, commonly referred to as acorn) milled flour; acorn for human consumption has increased due to its unique nutritional value. Acorn contains more than 55% of starch, 2.75–8.44% proteins, 0.7–7.4% fat, and significant amounts of minerals such as calcium, phosphorus, potassium, and niacin [1, 2]. Acorn also contains flavonoids and polyphenols such as tannins [1]. Flavanoids and polyphenols from acorn have recently been

Correspondence: Mohammed Saleh, Department of Nutrition and Food Technology, The University of Jordan, 11942 Amman, Jordan E-mail: [email protected] Fax: þ962 6 5300806 Abbreviations: ANOVA, analysis of variance; CMC, carboxymethyl cellulose; LSD, least significant differences; m, consistency coefficients; n, flow behavior index; Pasting T, pasting temperature; RVA, rapid viscosity analyzer; WHC, water holding capacity

ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

linked to cancer prevention [3–7]. Rakic et al. [8] showed that ethanolic extracts from thermally treated acorn can minimize lipids deposition, thereby limiting obese weight gain and the development of diabetic complications. Saffarzadeh et al. [9], reported a more nutritious amino acid composition in acorn protein than in pecans. Acorns have been a part of the European, North American, and Asians diets as coffee substitutes as well as additives to porridge dough, astringent and antidiarrhoeal agent, bread cake, and dark bread [2, 8, 10]. Food products rich in hydrocolloids would the potential of playing a significant role in the food industry, especially in the design and process of systems such as pumps, pipes, and heat exchangers [11]. For instance, hydrocolloids reportedly aid in imparting viscosity and thickness to aqueous solutions and dispersions; they have also been tested as fat replacers in many food applications [12]. The concentration to which hydrocolloids are used in product formulations depends on the type that is ideal for the target sensory properties as well as the acceptability of food

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products by consumers [13]. The ability of hydrocolloids to improve food thickenings, and modify texture, rheological, and functional properties are of great interests [14]. Several authors reported the effects of hydrocolloids on the rheological characteristics of food [15]. Several authors discussed the interaction between starch and hydrocolloids. Alam et al. [16], for instance, discussed the effects of different hydrocolloids on the gelatinization behavior of hard wheat flour. The authors reported significant effects of various hydrocolloids (i.e., guar, xanthan, arabic, and carboxymethyl cellulose) on starch gelatinization, pasting, and freeze–thaw properties of wheat flour. Shi and BeMiller [17] also reported a significant influence of food gums on viscosities of corn starch suspensions during pasting. Eidam et al., [18] reported the ability of regulating maize starch gels functionality by the addition of selective hydrocolloids. Moreover, guar gum, alginates, carrageenans, and xanthan gum are widely utilized as stabilizers in the food industry [19–21]. The additions of such hydrocolloids are believed to alter starches structural and rheological characteristics; thus modifying starch–hydrocolloids suitability for specific food applications [22]. Although acorn is used in many countries; limited information is currently available regarding acorn functional properties. In addition, effects of hydrocolloids on the physical properties of acorn starch have not yet been investigated. Therefore, this study was undertaken to evaluate the effects of hydrocolloids on the physical properties of acorn starch; in order to select the most adequate starch–hydrocolloids combinations for a specific food application. Results from this study are expected to explain the acorn-starch–hydrocolloids interactions and how they relate to functional properties.

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Materials and methods

2.1 Materials Xanthan gum (FCCIV/USP) was purchased from TNN Development Ltd. Dalian/P. R. China, sodium carboxymethylcellulose (CMC) (FVH6-4) was obtained from Denizli Chemical Industry and Trade Co. Denizli/Turkey, k-carrageenan (INS no. 407) was procured from Agarmex, S.A. DE C.V. Ensenada (k-carrageenan was designated as carrageenan for simplicity throughout this study), Mexico and Sudanese arabic gum (Pre-Hydrated1 Gum Arabic FT Powder) was acquired from TIC Gums, Inc., White Marsh, MD, USA. Acorn starch was produced using representative composites of hand harvested oak (Q. calliprinos) from local area in northern Jordan. Right after harvesting, oak was washed using tape water, soaked for 24 h before washing again and then water blanched at 95°C for 6 min. Blanched oak was sun dried for 72 h, peeled and acorn flour was then ground into flour and sifted to pass through a US 100-mesh (i.e., 149 m). ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim


Acorn starch was produced using sodium hydroxide alkaline solution according to the method described by Sosulski et al. [23] with minor modification of soaking durations. In summary, acorn flour was defatted by soaking in hexane (1:10 w/v) for 24 h after which hexane was drained. Defatted acorn flour was soaked in a 0.2N sodium hydroxide solution (1:10 ratio w/v) for 2 h at 25°C with continues stirring. The soaked sample was then wet-milled in an Osterizer blender for 3 min (i.e., speed setting at 6) and filtered twice though US standard test sieves number 100 and then 400, respectively. The slurry was then centrifuged at 4000 rpm for 30 min at 4°C in a 5810R centrifuge (Eppendorf, Germany); the supernatant was discarded. The sediment was washed five times with 0.2N sodium hydroxide (1:10 flour to sodium hydroxide) and the slurry was then centrifuged again at 4000 rpm for 30 min. The dark tailings layer atop the starch sediment was carefully scraped away and discarded. The sediment was washed three times using distilled water, centrifuged at 4000 rpm for 30 min and again the dark tailings layer atop the starch was carefully scraped away and discarded. After washing and centrifugation, the resulting sediment was suspended in distilled water and adjusted to pH of 7.0 (pH meter no. 40675/0001: HANNA Instrument, UK) with 0.1N hydrochloric acid (HCl) before a final centrifugation at 4000 rpm for 30 min. The resulting starch was then air dried for 48 h at 40°C to a moisture content of 12% before grinding and sifting through US standard sieve number 100. 2.2 Acorn starch chemical composition AACC methods 44-15.02, 30-25.01, 46-13.0, and 08-01.01 were used for moisture, total lipid, proteins, and ash contents determination of acorn starch [24]. Carbohydrates were calculated by difference method. Amylose of acorn starch was determined according to the procedure outlined by the manufacturer for the Megazyme amylose/amylopectin assay kit. Percent amylose was directly calculated following the specific Megazyme equation. Produced acorn starch had 8.54% moisture, 0.21% lipids, 0.77% proteins, 2.73% ash, and 29.2% (wet bases) amylose contents. 2.3 Design of the experiment A three factors mixture response surface design was used as described by Scheffe [25] was used to conduct the experiment where four hydrocolloids (carrageenan, xanthan gum, arabic gum, CMC) were considered as the main factors. Three hydrocolloids of five different combinations and four different sets hydrocolloids (i.e., 20 treatments) were used to perform this study. The three hydrocolloids evaluated in each set were (x1), (x2), and (x3) (Table 1). The proportion for each hydrocolloid used in the model was calculated for each


Effects of hydrocolloids on acorn starch physical . . .

Starch/Stärke 2016, 68, 1–11 Table 1. Mixture response surface model of hydrocolloids used in this studya)

Hydrocolloid’s fraction Treatments

X1 (%)

X2 (%)

X3 (%)

66% X1, 17% X2, 17% X3 50% X1, 50% X2, 0% X3 33% X1, 34% X2, 33% X3 17% X1, 66% X2, 17% X3 0% X1, 50% X2, 50% X3

66.0 50.0 33.0 17.0 0.0

17.0 50.0 34.0 66.0 50.0

17.0 0.0 33.0 17.0 50.0

a) Fractions represent percentage of a total of 1.0 g of three hydrocolloids used in each treatment. X1, X2, and X3 represent the hydrocolloids used for a treatment.

treatment combination where the sum of each component proportion was equal to one. X i ¼ x1 þ x2 þ x3 ¼ 1 Full factorial combinations of each of the three hydrocolloid’s sets were used in this study. In this design, the number of points (n) necessary to run a mixture experiment is: n ¼ 2q 1 where q is equal to the number of components being studied (3). JMP version 10.0 (SAS Institute, Cary, NC) was used to build the model parameters. Table 1 also presents the percentages of each variable used in the model. Fractions represented percentages of a total of 1.0 g of hydrocolloids used in each treatment. A 1% (w/w) hydrocolloids: acorn starch was used to form each treatment. 100% acorn starch was also used as a control sample (i.e., no hydrocolloids) and was included in the study to compare treatments. Combinations of hydrocolloids included in the mixture response surface model were: Set a ¼ CMC (X1), arabic gum (X2), and carrageenan (X3). Set b ¼ CMC (X1), arabic gum (X2), and xanthan gum (X3). Set c ¼ CMC (X1), carrageenan (X2), and xanthan gum (X3). Set d ¼ arabic gum (X1), carrageenan (X2), and xanthan gum (X3). For treatment formulation, a total of 1% (w/w) hydrocolloids were used to replace acorn starch. A control sample of no replacements (i.e., 100% acorn starch) was also included in the sample set. Treatments were mixed thoroughly using a household kitchen aid mixer (Model KSM150PSER, USA) at speed 4 for 5 min before performing the experiment. 2.4 Water holding capacity (WHC) Water holding capacity (%) of each treatment was determined by the method described by Abu-Salem and AbouArab [26] with modifications of the centrifuge speed and the holding temperatures. In brief, 5 g of each treatment was dispersed in distilled water after which the dispersions was ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

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allowed to stand for 1 h at 25, 35, 45, and 55°C before centrifuging (Eppendorf, 5810R, Hamburg, Germany) at 3800 rpm for 30 min at 4°C. Sediments weights were recorded and WHC (%) was calculated using the following equation. WCHð%Þ ¼ ðSediment weight=dry solids weightÞ 100% ð1Þ 2.5 Rheological measurements A mixture of 5.0 g of each treatment and 95 mL distilled water was prepared for rheological property measurements. Homogenized treatments (i.e., using (120), Igenieurbuero CAT, Stufen, Germany) were held at 23.2°C for 1 h before rheological measurement. Apparent viscosity was measured during shearing in a range of 6–60 s1 using a rotational viscometer (SNB-AI Digital Viscometer, Shandong China). Samples were kept constant in a holding cup during rheological measurements. Treatments consistency coefficient (m) and flow behavior index (n) was evaluated using Herschel–Bulkley model (Eq. 2). t ¼ to þ m g_ n

ð2Þ

where t is the shear stress (mPa), to is the yield stress (mPa), m is the consistency coefficient (mPa sn), g_ is the shear rate (s1), and n is the flow behavior index (dimensionless). Herschel–Bulkley model was used to describe the rheological behavior of treatments functional properties. The flow behavior index (n) was used to characterize Newtonian and non-Newtonian fluid behaviors. 2.6 Gel strength Gel strength of all treatments was measured using 15 g acorn starch–hydrocolloids mixtures and 100 mL distilled water. Samples were heated at 95°C in a shaking water bath for 30 min after which the hot starch pastes were poured into cylindrical molds with a diameter of 10 mm diameter and height of 20 mm height. The formed starch gels were covered and cooled at room temperature for 1 h before storage at 4°C for 24 h. Starch gels were placed at room temperature for 1 h before measurement of gel strength. Gel strength was measured using a texture analyzer (Mecmesin Ltd., West Sussex, RH1306Z, UK). For the measurement, a cylindrical probe with a 5 mm diameter was used to penetrate the gel at a test speed of 0.5 mm/s to a distance of 10 mm. Force required to penetrate a distance of 10 mm was recorded and expressed as the gel strength (N) of treatments. Five measurements were performed for each treatment. 2.7 Freeze–thaw stability The aqueous dispersions of treatments (5 g treatment/100 g distilled water) were heated at 95°C in a shaking water bath


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for 30 min then cooled to room temperature (23.2°C) in an iced water bath. All pastes were weighed (approximately 20 g) into centrifuge tubes, subjected to freeze–thaw cycles at 22°C for 24 h followed by thawing at 30°C for 2.0 h and then centrifuged at 3800 rpm for 30 min. Separated supernatants were then weighed and the degree of syneresis was expressed as the percentage of freeze stability of samples. Three freeze– thaw cycles were performed and results were expressed as the average of three measurements for each cycle. 2.8 Pasting measurements Treatments pasting viscosities including peak viscosity, trough, setback viscosity, breakdown viscosity, final viscosity, and pasting temperature were evaluated and recorded with a Rapid Viscosity Analyzer (RVA-4, Foss North America, EdenPrairie, MN, USA) according to the AACC approved method 76-21 (AACC 2000). In summary, 3 g of treatments were mixed with 25 mL of distilled water; the slurry was then mixed at 50°C for 1 min at 160 rpm then heated from 50 to 95°C at a heating rate of 12°C/min. The hot paste was then held at 95°C for 2.5 min and then cooled down to 50°C at a cooling rate of 12°C/min and RVA data were processed using Thermocline version 1.2 software (Newport Scientific, Inc., Warriewood, Australia). All samples were measured in triplicate.

R2 ¼ 0:99

Analysis of variance (ANOVA) was carried out on physical treatments data using JMP version 10.0 (SAS Institute). A level of 5% probability between treatments was calculated based on the least significant differences (LSD). A mixture response surface model was fitted using three sets of hydrocolloids as the model factors. The model search was started with the special cubic equation (Eq. 1): Y ¼ b1 x1 þ b2 x2 þ b3 x3 þ b12 x1 x2 þ b13 x1 x3 þ b23 x2 x3 ð3Þ where Y is the predicted response, b’s are the parameter estimates models prediction model parameters, x1, x2, x3, x1x2, x1x3, and x2x3 are the linear terms of the hydrocolloids used and the cross product terms, respectively. The model chosen was based on its significance (p < 0.05), the insignificance of the lack of fit and the highest R2 according to Cornell [27].

Results and discussion

3.1 Water holding capacity Table 2 presents changes in water holding capacity of acorn starch treatments (i.e., added various combinations of ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

WCH ð%Þ ðarabic=carrageen=xanthanÞ ¼ 0:009x1 þ1:4x2 þ4:7x3 þ0:06x1 x2 þ 0:033x1 x3

2.9 Statistical analysis

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hydrocolloids) after holding at 25, 35, 45, and 55°C for 1 h. A significant (p < 0.05) increase in WHC with the increase in holding temperature for almost all treatments was reported. Results were attributed to the effect hydrocolloids in facilitating maximum water absorption with temperature exposure [28]. WHC is an essential functional properties of starch (i.e., particularly pore size) and protein (i.e., hydrophilic nature). The increased WHC of the combination acorn and hydrocolloids would improve the texture and quality of acorn. Shadi et al. [29] reported WHC of acorn subjected to various treatments to be superior to maize flour (149.0 4) and wheat (63.8 2.1). WHC of various acorn treatments ranged from 162.0% for CMC0:arabic50:carrageen50 at 25°C to 305.3% for arabic0:carrageen50:xanthan50 at 55°C compared with 213.3 and 243.8% for pure acorn starch held at 25 and 45°C, respectively. The contribution of various sets of hydrocolloids combinations (i.e., set a ¼ carboxymethyl cellulose: arabic gum: carrageen, set b ¼ CMC: arabic gum: xanthan gum, set c ¼ CMC: carrageen: xanthan gum, and set d ¼ arabic gum: carrageen: xanthan gum) to WHC after being held at 45°C was further evaluated using mixture response surface model regression equations (Eq. 4a–d, respectively). A similar trend was noticed when holding treatments at 25, 35, and 55°C.

ð4aÞ WCH ð%Þ ðCMC=arabic=carrageenÞ ¼ 1:7x1 þ1:7x2 þ 1:9x3 þ 0:011x1 x2 þ 0:014x1 x3 R2 ¼ 0:85 ð4bÞ WCH ð%Þ ðCMC=arabic=xanthanÞ ¼ 1:7x1 þ2:1x2 þ1:8x3 þ0:0017x1 x2 þ 0:003x1 x3 R2 ¼ 0:75 ð4cÞ WHC ð%Þ ðCMC=carrageen=xanthanÞ ¼ 1:5x1 þ0:3x2 þ5:8x3 þ 0:048x1 x2 0:021x1 x3 R2 ¼ 0:99 ð4dÞ Results show that changes in water holding capacity were caused by the hydrocolloids in acorn starch treatment. The models indicated a significant influence of the linear terms on the WHC of acorn treatments. Furthermore, the equations suggested that xanthan had the greatest influence in increasing WHC with model parameter estimates of 4.7, 1.8, and 5.8 of various treatments. Model parameters for


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Table 2. Water holding capacity (WHC %) of acorn starch combined with ratios of hydrocolloidsa)

Holding temperature Hydrocolloid sets/treatments

23.3°C

35°C

45°C

55°C

Arabic66.6:carrageen16.6:xanthan16.6 Arabic50:carrageen50:xanthan0 Arabic33.3:carrageen33.3:xanthan33.3 Arabic16.6:carrageen66.6:xanthan16.6 Arabic0:carrageen50:xanthan50 Acorn starch

182.6 173.4 210.4 195.4 202.6 213.6

0.4bc 0.3c 5.6a 8.3ab 2.4ab 3.2a

221.8 179.4 300.9 214.2 200.4 209.9

2.6b 0.8f 0.9a 2.0c 1.2e 0.5d

203.7 209.4 303.0 242.6 302.4 243.8

4.8c 4.8c 7.7a 3.7b 0.5a 3.3b

216.2 183.3 275.7 260.0 305.3 233.6

0.6e 0.3f 1.3b 2.5c 0.2a 3.2d

CMC66.6:arabic16.6:carrageen16.6 CMC50:arabic50:carrageen0 CMC33.3:arabic33.3:carrageen33.3 CMC16.6:arabic66.6:carrageen16.6 CMC0:arabic50:carrageen50 Acorn starch

166.7 173.4 163.2 179.3 162.0 213.6

0.1c 0.3bc 1.3c 1.4b 4.5c 3.2a

192.5 176.1 176.8 173.7 175.7 209.9

6.5b 5.4c 8.3c 0.1c 3.0c 0.5a

199.8 196.8 202.2 188.2 177.6 243.8

0.1bc 4.7c 0.6b 2.9d 2.7d 3.3a

229.2 216.5 213.8 226.0 219.2 233.6

2.3a 2.1bc 2.2b 2.8a 1.3c 3.2a

CMC0:arabic50:xanthan50 CMC66.6:arabic16.6:xanthan16.6 CMC50:arabic50:xanthan0 CMC33.3:arabic33.3:xanthan33.3 CMC16.6:arabic66.6:xanthan16.6

176.4 173.4 180.1 185.1 189.3

1.3bc 0.3c 1.3bc 0.5bc 4.2b

174.1 176.1 180.1 178.9 179.6

5.3b 5.4b 1.3b 5.0b 0.8b

177.9 196.8 185.5 201.1 195.3

7.6e 1.7c 0.1d 2.8b 1.2c

231.1 216.5 211.4 208.9 204.3

2.6a 1.1a 0.1a 2.7a 4.9a

Acorn starch CMC66.6:carrageen16.6:xanthan16.6 CMC50:carrageen50:xanthan0 CMC33.3:carrageen33.3:xanthan33.3 CMC16.6:carrageen66.6:xanthan16.6 CMC0:carrageen50:xanthan50 Acorn starch

213.6 208.3 178.3 189.7 229.5 202.6 213.6

3.2a 6.2b 0.5e 2.6d 2.4a 2.1c 3.2b

209.9 216.7 179.4 239.1 169.3 200.4 209.9

0.5a 4.8b 8.1d 0.0a 2.9d 2.6c 0.5b

243.8 234.1 209.4 284.5 189.5 302.4 243.8

3.3a 1.7c 4.8d 0.2b 1.9e 0.5a 3.3c

233.6 204.0 183.3 273.1 245.7 305.3 233.6

3.2a 1.0e 0.3f 1.9b 6.3c 0.1a 3.2d

set a, CMC/arabic/carrageen; set b, CMC/arabic/xanthan; set c, CMC/carrageen/xanthan; and set d, arabic/carrageen/xanthan. After holding at 25, 35, 45, and 55°C for 1 h. a) For the same set of hydrocolloids used and holding temperature; water holding capacity (%) of hydrocolloids (i.e., same column) having different letter(s) are significantly (p < 0.05) different according to the least square difference (LSD). The number underneath hydrocolloid indicated the percentage of a total of 1.0 g of hydrocolloids used in each treatment. CMC, carboxymethyl cellulose.

arabic gums, CMC and carrageenan ranged from 0.009 to 2.1, 0.3 to 1.9, and from 1.5 to 1.7, respectively. WHC has for a long time been strongly correlated with the swelling power of starch molecules, which is dependent on the crystallinity of the starch and hydrogen bonding [30]. Rojas et al. [31] and Teacante and Doublier [32] observed an increased starch swelling with the addition of hydrocolloids. Starch swelling is responsible for the unique characteristics such as pasting viscosity and eating quality of food products made from flour [33, 34]. 3.2 Rheological measurements Viscosity data were fitted to the Herschel–Bulkley model using Eq. 2. Flow behavior index (n) and consistency coefficients (m) of acorn starch treatments are presented in Table 3. The ANOVA results showed significant differences in flow behavior index and consistency coefficient for all the samples (Table 3). For all treatments, the flow behavior index, ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

n, varied from 0.43 for (CMC66.6:arabic16.6:carrageen16.6) to 0.99 for (arabic33.3:carrageen33.3:xanthan33.3). Consistency coefficient of acorn treatments, m, ranged from 0.03 to 0.17 mPa sn for (CMC66.6:carrageen16.6:xanthan16.6). Additionally, acorn starch had lower flow behavior index and consistency coefficient compared to the hydrocolloids treatments, with few exceptions. Flow behavior index and consistency coefficient of acorn starch were n ¼ 0.66 and m ¼ 0.01 mPa sn, respectively. Starch dispersions are described as a composite materials consisting of swollen amylopectin granules dispersed in a continuous amylose biopolymer matrix [35, 36]. A close look at the values of flow behavior index, n, show acorn starch and acorn starch treatments exhibiting a shear thinning behavior. During shearing, thinning of materials is caused by the changes in the physical orientation of molecules as well as to the direction of flow and breaking of hydrogen bonding between amylose– amylopectin–water structures [37].


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Table 3. Flow behavior index (n), consistency coefficient (m), and gel strength of acorn starch combined with ratios of hydrocolloidsa)

n

Hydrocolloid sets/treatments

m (mPa sn)

Gel strength (N)


0.74 0.66 0.99 0.94 0.67 0.66

0.012c 0.004d 0.025a 0.008b 0.008d 0.006d

0.06 0.07 0.05 0.10 0.07 0.01

0.002c 0.000b 0.003d 0.001a 0.002b 0.000e

0.42 0.25 0.18 0.40 0.18 0.22

0.005a 0.006c 0.007e 0.007b 0.005e 0.006d


0.43 0.53 0.66 0.53 0.68 0.66

0.002c 0.006b 0.013a 0.047b 0.025a 0.006a

0.05 0.03 0.03 0.03 0.07 0.01

0.001b 0.001c 0.000c 0.006c 0.002a 0.000d

0.31 0.26 0.37 0.45 0.39 0.22

0.086c 0.019d 0.007b 0.008a 0.009b 0.006e

CMC0:arabic50:xanthan50 CMC66.6:arabic16.6:xanthan16.6 CMC50:arabic50:xanthan0 CMC33.3:arabic33.3:xanthan33.3 CMC16.6:arabic66.6:xanthan16.6 Acorn starch

0.89 0.53 0.85 0.65 0.96 0.66

0.017b 0.006e 0.011c 0.007d 0.021a 0.006d

0.03 0.03 0.05 0.06 0.05 0.01

0.002c 0.001c 0.003b 0.001a 0.004b 0.000d

0.35 0.26 0.25 0.38 0.78 0.22

0.005c 0.019d 0.007d 0.006b 0.022a 0.006e

CMC66.6:carrageen16.6:xanthan16.6 CMC50:carrageen50:xanthan0 CMC33.3:carrageen33.3:xanthan33.3 CMC16.6:carrageen66.6:xanthan16.6 CMC0:carrageen50:xanthan50 Acorn starch

0.50 0.66 0.77 0.68 0.67 0.66

0.001d 0.004c 0.010a 0.010b 0.008bc 0.006c

0.17 0.07 0.12 0.14 0.07 0.01

0.009a 0.000d 0.005c 0.006b 0.001d 0.000e

0.18 0.25 0.22 0.40 0.16 0.22

0.001d 0.006b 0.002c 0.013a 0.005e 0.006c

set a, CMC/arabic/carrageen; set b, CMC/arabic/xanthan; set c, CMC/carrageen/xanthan; and set d, arabic/carrageen/xanthan. a) For the same set of hydrocolloids used, flow behavior index (n), consistency coefficient (m) and gel strength (N) standard deviation of hydrocolloids (i.e., same column) having different letter(s) are significantly (p < 0.05) different according to the LSD. The number underneath hydrocolloid indicated the percentage of a total of 1.0 g of hydrocolloids used in each treatment. CMC, carboxymethyl cellulose.

The increase in viscosity with the addition of hydrocolloids was described by Shi and Bemiller [19] who demonstrated that during heating, added gums tend to lodge in the amylose continuous phase of starch dispersions resulting in a decrease in volume of this phase, which leads to drastic increase in gum concentration, thereby producing viscous solution. Moreover, the magnitudes of change in flow behavior index (n) and consistency coefficient (m) for acorn starch treatments mixtures were significantly greater than those for the control due to synergistic interaction between acorn starch and hydrocolloids [38]. Choi and Yoo [38] evaluated the effects of k-carrageenan, Aarabic, gellan, locust bean, xanthan, guar, pectin, and alginate gums, on the flow behavior and yield stress of sweet potato starch; they reported a synergistic effect on the elastic properties of starch–gum mixtures. The authors suggested that this effect could result in improved products quality and a reduction in production cost of starch gum mixtures. Similar findings were reported by Choi and Yoo [39] and Liu and Eskin [40]. Acorn starch treatments viscoelastic behavior was believed to be a function of chemical composition, water ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

availability, as well as temperature. Free water, for instance, was reported to play a role in determining viscoelastic properties of starch because starches are usually not soluble in cold water; the higher the resistance the lower water availability [41, 42]. The results of this study also showed that acorn starch treatments exhibited Newtonian behavior, i.e., having a flow behavior index value, n, approaching 1. The interaction observed between the hydrocolloids and acorn starch and the influence on rheological properties was probably associated with hydrocolloids hydration capacity and thickening properties [43]. Similar findings were observed by Changala et al. [44] who reported an increase in flow behavior index and a decrease in consistency coefficient with lower water holding capacity for both native and fermented black gram flour dispersions. 3.3 Gel strength Gel strength results of acorn-starch–hydrocolloids in water treatments are presented in Table 3. The strengths of the formed treatments gels were significantly (p < 0.05) greater www.starch-journal.com



than that of pure acorn starch indicating that the gels formed with inclusion of hydrocolloids were harder than those made with the pure starch. For all treatments sets, penetration force ranged from 0.16 N for (arabic0:carrageen50:xanthan50) to 0.78 N for (CMC16.6:arabic66.6:xanthan16.6). Similar findings were observed by Wasserman et al. [45] who reported an increase in gel strength of wheat starch when adding various types of gums. The increase in gel strength was attributed to the increased effect of hydrocolloids concentration in the formed gel resulting in immobilized water molecules. The addition of hydrocolloids to pure starch also believed to increase formation of hydrogen bonds formations [46]. The effects of hydrocolloids on acorn gel strength were further evaluated using the mixture response surface model regression equations (Eq. 5a–d, respectively). Results indicated significant interactions between hydrocolloids and starch, which affected gel strength. For instance, when CMC, arabic gum, and xanthan were used (Eq. 5c), CMC positively impacted acorn starch gel strength having a parameter coefficient of 1.12 while CMC xanthan interaction negatively impacted gel strength having a negative parameter coefficient of 3.37. Similar trends were reported for arabic gum and carrageen with both having parameter coefficients of 0.87 and 0.97, respectively, and a negative interaction parameter coefficient of 2.66 (Eq. 5a). Gel Strength ðarabic=carrageen=xanthanÞ ¼ 0:87x1 þ 0:97x2 0:66x3 2:66x1 x2 þ 0:81x1 x3 R2 ¼ 0:99 ð5aÞ Gel Strength ðCMC=arabic=carrageenÞ ¼ 0:21x1 þ 0:67x2 þ 0:11x3 0:72x1 x2 þ 1:03x1 x3 R2 ¼ 0:76 ð5bÞ Gel Strength ðCMC=arabic=xanthanÞ ¼ 1:12x1 þ 0:61x2 0:95x3 2:41x1 x2 3:37x1 x3 R2 ¼ 0:99 ð5cÞ Gel Strength ðCMC=carrageen=xanthanÞ ¼ 0:27x1 þ 0:65x2 0:34x3 þ 0:25x1 x2 þ 1:60x1 x3 R ¼ 0:99

7

CMC66.6:carrageen16.6:xanthan16.6 during the third freezing cycle. Syneresis (%) for most of the acorn-starch–hydrocolloids treatments were significantly (p < 0.05) lower than that of the acorn starch (i.e., control) sample during all freeze–thaw cycles. This finding indicates that the freeze–thaw stability of acorn starch treatments improved by using hydrocolloids, which indicates a significant acorn-starch–hydrocolloids interaction. Superior freeze–thaw stability was observed after the incorporation of CMC16.6:arabic66.6:carrageen16.6 having a syneresis of 1.8% during the first cycle and for CMC33.3: carrageen33.3:xanthan33.3 having a syneresis of 8.2% during the third freezing cycle. CMC66.6:carrageen16.6:xanthan16.6 had the worst freeze–thaw stability with a syneresis of 21.4% after three freezing–thawing cycles. Acorn starch had a syneresis of 12.1, 12.6, and 18.1% during freeze cycles 1, 2, and 3, respectively. Results show the ability of hydrocolloids to provide stability in food applications. Yamazaki et al. [47] who reported that incorporating polysaccharide from leaves of Corchorus olitorius L. into the corn starch gel at 0.7% was effective in reducing the syneresis of the starch gel after five freeze–thaw cycles. Pongsawatmanit and Srijunthongsiri [48] also reported an improved stability of tapioca starch using xanthan gums. Ahmad and Williams [49] also reported a significant increase in freeze–thaw stability of sago starch gels with the addition of galactomannans. The ability of each hydrocolloid to reduce syneresis during the third freezing–thawing cycles are presented in equations Eq. 6a–d, respectively. Xanthan gum was more effective in reducing syneresis than other hydrocolloids having the lowest confident parameters while CMC had the greatest effect in increasing syneresis. For instance, xanthan gum had a coefficient of 3.5, 8.6, and 5.6 when using arabic: carrageen:xanthan, CMC:arabic:xanthan and CMC:carrageen:xanthan, hydrocolloid sets, respectively compared to 26.0, 12.6, and 53.2 for CMC. Similar trends were reported for all freeze–thawing cycles. Syneresis ð%Þ ðarabic=carrageen=xanthanÞ ¼ 17:8x1 þ 21:6x2 þ 3:5x3 35:5x1 x2 þ 15:9x1 x3 R2 ¼ 0:78 ð6aÞ

2

ð5dÞ 3.4 Freeze–thaw stability Three freezing-thawing cycles of acorn starch combined with ratios of hydrocolloids results are presented in Table 4. The percentage syneresis (%) of the control and acorn starch treatments values ranged from 1.8% for CMC16.6:arabic66.6: carrageen16.6 during the first freezing cycle to 21.4% for ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Syneresis ð%Þ ðCMC=arabic=carrageenÞ ¼ 26:0x1 þ 11:3x2 þ 5:5x3 37:0x1 x2 þ 7:5x1 x3 R2 ¼ 0:87 ð6bÞ Syneresis ð%Þ ðCMC=arabic=xanthanÞ ¼ 12:6x1 þ 16:0x2 þ 8:6x3 20:0x1 x2 11:3x1 x3 R2 ¼ 0:76 ð6cÞ


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M. Saleh et al.


Table 4. Freeze–thaw stability of acorn starch combined with ratios of hydrocolloidsa)

Syneresis (g/100 g) Hydrocolloid sets/treatments

Cycle 1

Cycle 2

Cycle 3


9.0 7.8 8.9 10.9 9.2 12.1

0.21cd 0.26d 0.68cd 0.57b 0.74c 0.27a

12.0 9.0 11.3 13.6 11.5 12.6

0.19b 0.36d 0.23c 0.86a 1.31c 0.14b

13.8 10.8 12.1 14.3 12.5 18.1

0.04bc 0.18e 0.64de 0.88b 0.64cd 0.25a


12.6 4.4 7.2 1.8 3.0 12.1

0.33a 0.12c 0.9b 0.48e 0.4d 0.27a

13.8 8.6 9.2 5.5 5.8 12.6

0.27a 0.09c 0.26c 0.33d 0.18d 0.14b

16.6 9.3 10.9 8.8 8.4 18.1

0.91b 0.28d 0.56c 0.06d 0.07d 0.25a


6.9 4.4 4.1 7.8 8.3 12.1

0.25c 0.12d 0.46d 0.46bc 0.87b 0.27a

8.4 8.6 8.4 9.6 10.8 12.6

0.33d 0.09d 0.06d 0.32c 0.54b 0.14a

9.6 9.3 9.5 11.8 12.3 18.1

0.35c 0.28c 0.25c 0.11b 0.12b 0.25a


16.7 7.8 6.0 5.9 9.2 12.1

0.14a 0.26c 1.0 d 0.62d 0.74c 0.27b

19.5 9.0 7.3 8.5 11.5 12.6

0.04a 0.36c 0.86c 0.20c 1.31b 0.14b

21.4 10.8 8.2 9.7 12.5 18.1

0.42a 0.18d 0.55e 0.02d 0.64c 0.25b

set a, CMC/arabic/carrageen, set b, CMC/arabic/xanthan; set c, CMC/carrageen/xanthan; and set d, arabic/carrageen/xanthan. a) For the same set of hydrocolloids used, freeze–thaw stability standard deviation for each cycle of hydrocolloids (same column) having different letter(s) are significantly (p < 0.05) different according to the LSD. The number underneath hydrocolloid indicated the percentage of a total of 1.0 g of hydrocolloids used in each treatment. CMC, carboxymethyl cellulose.

Syneresis ð%Þ ðCMC=carrageen=xanthanÞ ¼ 53:2x1 þ19:5x2 þ 5:6x3 102:3x1 x2 58:4x1 x3 R2 ¼ 0:70 ð6dÞ Retrogradation rate is reportedly to be influenced by factors such as amylose-amylopectin, molecular size, temperature, pH, and hydrocolloids [50]. 3.5 Pasting properties Pasting properties (i.e., peak, trough, breakdown, final, and setback (cP), and pasting temperature (Pasting T.) °C) of acorn–hydrocolloids ratio results are presented in Table 5. Peak, trough, breakdown, final, and setback viscosities ranged from 282.5 to 676.0 cP, 250.5 to 631.0 cP, 24.5 to 40.0 cP, 513.0 to 1313.0 cP, and from 251.5 to 682.0 cP, respectively. Results indicated a significant increase in pasting viscosities of starch as a result of hydrocolloids ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

addition regardless of type and ratio of hydrocolloids added. Results of the pasting properties of acorn–hydrocolloids treatments are generally in line with the WHC results. The swelling (i.e., increase in peak viscosity) of the starch granules are expected to increase with the use of various hydrocolloids concentration [38]. However, various hydrocolloids used affected pasting properties of acorn starch in different ways. For instance, arabic and xanthan gums attributed negatively to the formation of peak viscosity having models coefficients of 72.1 and 15.9 (i.e., using arabic:xanthan:carrageenan variables). Carrageenan on the other hand had a model coefficient of 29.5. The use of CMC as one of the hydrocolloids, however, positively impacted pasting viscosities (Eq. 7a). Similar trends were reported for setback, breakdown, and final viscosities (Eq. 7b–d, respectively). Results were attributed mainly to the variation in molecular structure of hydrocolloids and/or ionic charges of both starches and hydrocolloids [19, 33].


9



Table 5. Pasting viscosities (peak, trough, breakdown, final, and setback (cP)) and pasting temperature (Pasting T) (°C) of acorn starch combined with ratios of hydrocolloid setsa)

Hydrocolloid sets/treatments

Peak

Trough

Breakdown

Final

Setback

Pasting T


392.5d 300.5e 458.0b 414.5c 676.0a 282.5f

362.5d 270.5e 426.0b 383.0c 631.0a 250.5f

30.0b 30.0b 32.0b 31.5b 45.0a 32.0b

746.0d 548.5e 914.5b 821.5c 1313.0a 513.0e

383.5d 278.0e 488.5b 438.5c 682.0a 262.5e

84.8b 82.5d 84.8b 85.5a 84.0c 80.5e


320.5b 341.0a 337.5a 304.5c 300.5c 282.5d

292.5b 310.0a 306.0a 275.5c 270.5c 250.5d

28.0c 31.0ab 31.5a 29.0bc 30.0abc 32.0a

558.5b 561.5b 604.0a 554.0b 548.5b 513.0c

266.0bcd 251.5d 298.0a 278.5b 278.0bc 262.5cd

84.4c 87.2b 88.5a 83.0d 86.9b 80.5e


430.0c 341.0e 484.0b 384.5d 508.0a 282.5f

403.5c 310.0e 455.0b 360.0d 473.0a 250.5f

26.5cd 31.0b 29.0bc 24.5d 35.0a 32.0ab

654.0c 561.5e 749.0b 612.5d 805.0a 513.0f

250.5c 251.5c 294.0b 252.5c 332.0a 262.5c

85.6ab 87.2a 82.8bc 85.2ab 84.7ab 80.5c


457.0b 292.5c 480.5b 451.0b 676.0a 282.5c

429.0bc 265.5d 455.0b 418.5c 631.0a 250.5d

28.0c 27.0c 25.5c 32.5b 45.0a 32.0b

781.0d 530.5e 917.0b 856.0c 1313.0a 513.0e

352.0d 265.0e 462.0b 437.5c 682.0a 262.5e

85.1b 87.3a 84.8bc 85.2b 84.0c 80.5d

set a, CMC/arabic/carrageen; set b, CMC/arabic/xanthan, set c, CMC/carrageen/xanthan; and set d, arabic/carrageen/xanthan. a) For the same set of hydrocolloids used pasting viscosity (peak, trough, breakdown, final, and setback (cP)) and pasting temperature (°C) for treatments within the same set (same column) having different letter(s) are significantly (p < 0.05) different according to the LSD. The number underneath hydrocolloid indicated the percentage of a total of 1.0 g of hydrocolloids used in each treatment. CMC, carboxymethyl cellulose.

Peak Viscosity ðarabic=xanthan=carrageenanÞ ¼ 72:1x1 15:9x2 þ 29:5x3 þ 1:9x1 x2 þ 0:3x1 x3 R2 ¼ 0:75 ð7aÞ Peak Viscosity ðCMC=arabic=carrageenanÞ ¼ 2:5x1 þ 2:3x2 þ 3:7x3 þ 0:04x1 x2 þ 0:008x1 x3 R2 ¼ 0:93 ð7bÞ Peak Viscosity ðCMC=arabic=xanthanÞ ¼ 3:5x1 þ 2:8x2 þ 7:4x3 þ 0:01x1 x2 þ 0:01x1 x3 R2 ¼ 0:65 ð7cÞ Peak Viscosity ðCMC=carrageenean=xanthanÞ ¼ 6:2x1 þ 5:2x2 þ 8:3x3 0:11x1 x2 0:05x1 x3 R2 ¼ 0:77 ð7dÞ ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

4

Conclusions

This study investigated the effects of hydrocolloids on the physical properties of acorn starch. A mixture response surface model was used and model coefficients were calculated to evaluate the effects of hydrocolloids on acorn starch treatments functionality. Acorn–hydrocolloids interaction played a major role in determining acorn starch end use functionality. Results pointed out to the ability of controlling acorn starch properties through varying the types and proportion of hydrocolloids in a treatment system. For instance, the significant impacts of hydrocolloids of treatments on viscoelastic properties including flow behavior index and consistency coefficient of treatments (showing a shear thinning behavior) can be applied to coating applications. Changes in treatment functionality were attributed to changes in swelling power of starch granules and hydrogen bonding, suggesting significant acorn-starch–hydrocolloids interaction. Furthermore, information provided in this study play an important role in determining the potential use of


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acorn starch to enhance various physicochemical properties thus consumer acceptance/preference of various products. The observed effect of using hydrocolloids presents a practical example on their effects on products functionality. Future sensory evaluations of various acorn-starch–hydrocolloids are expected to provide the ideal processing conditions that influence end use functionality including freeze–thaw stability, and gelling properties. The authors would like to declare no conflict of interest of this work.

5

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