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Journal of Food Engineering 54 (2002) 167174 www.elsevier.

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Stabilization of emulsions by OSA starches


S. Tesch
a

a,*

, Ch. Gerhards b, H. Schubert

Institute of Food Process Engineering, University of Karlsruhe, Kaiserstr. 12, D-76137 Karlsruhe, Germany b Zurich University of Applied Sciences at Wadenswil, P.O. Box 335, CH-8820 Wadenswil, Switzerland Received 22 August 2001; accepted 15 October 2001

Abstract In continuous mechanical emulsication, droplets of a coarse premix are rst deformed and disrupted. Secondly, the newly formed interface has to be stabilized. Emulsions are thermodynamically unstable, as droplets tend to coalesce. To avoid coalescence of droplets, dierent eects have to be taken into account. The objective of this paper is to investigate the possibility of producing nely dispersed emulsions by using OSA starches as additive. Experiments were carried out using two commercially available OSA starches that dier mainly in viscosity of their aqueous solutions. In the experiments, the dispersed phase content, starch concentration as well as pH value and the inuence of dissolved salts of dierent ion strength have been investigated. By droplet size analysis directly after production of oil-in-water emulsions the emulsifying properties of such starches were determined. Measurements of interfacial tension prove that OSA starches are surface active substances. It was shown by emulsication experiments that the stabilization of droplets by OSA starches is very ecient. The emulsication results achieved with OSA starches have been found to be independent from the type of starch and the starch concentration above the lower limit of starch needed for stabilization. The emulsication results are independent of pH value and ion valence. Therefore it can be concluded that steric hindrance is the main stabilizing mechanism of OSA starches. As proteins stabilize emulsion droplets mainly by electrostatic repulsive forces, the emulsication result depends strongly on pH, which leads to poor emulsication at pH values near the iso-electric point. The results of the work presented here suggest that whey proteins can be substituted by OSA starches with a specic advantage at low pH values near the iso-electric point of the protein. 2002 Published by Elsevier Science Ltd.
Keywords: Emulsions; OSA starches; Stability; Whey protein

1. Introduction The emulsication process includes two steps. First, deformation and disruption of droplets, and secondly, stabilization of the newly formed interfaces. The quality of an emulsion depends on the droplet size of the dispersed phase. Usually, the aim of emulsication is to produce as small droplets as possible. Emulsions have to be stable for a certain period of time, i.e., droplet size must not increase during storage. Emulsions are thermodynamically unstable, as droplets tend to coalesce. Thus, during the continuous mechanical emulsication process, there is the possibility of coalescence immediately after droplet disruption. To stabilize the disruption result, i.e., to improve the emulsions short term stability, the coalescence frequency has to be controlled (Tesch & Schubert, 2001). Regarding avoidance of coCorresponding author. E-mail addresses: sabine.tesch@lvt.uni-karlsruhe.de (S. Tesch), c.gerhards@hswzfh.ch (C. Gerhards). 0260-8774/02/$ - see front matter 2002 Published by Elsevier Science Ltd. PII: S 0 2 6 0 - 8 7 7 4 ( 0 1 ) 0 0 2 0 6 - 0
*

alescence of droplets, dierent eects have to be taken into account. Hydrodynamic stabilization by slowing down the drainage of the liquid between two colliding droplets is one of these eects. Furthermore, steric hindrance or electrostatic repulsion are stabilizing mechanisms caused by surfactants adsorbed at the interface of the droplets. Starches have always been essential to human nutrition. They provide a major part of the overall caloric intake worldwide. Besides their nutritional value starches have been used for their functional properties such as thickening in soups and sauces (Murphy, 2000). By chemical modication of starches, process and storage stability of starch containing foods may be increased. Furthermore, it is possible to add hydrophobic side chains to the originally mere hydrophilic starch molecule. By this means starch may adsorb to the interface of water and oil, thus stabilizing an emulsion. Such emulsifying starch is octenyl-succinate starch, so-called OSA starch. It is made by esterication of starch and anhydrous octenylsuccinic acid under alkaline

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conditions (Trubiano, 1986). This modication has been FDA approved for the use in food. OSA starches have also been approved as food additive in the EU (E 1450). By use of various starch base (native starch, acid uidities, dextrin) the desired functional properties, namely viscosity and solubility, are determined. Most useful are cold-water soluble OSA starches, as the heating step for the gelatinization otherwise necessary may be omitted. OSA starches have been used successfully for many years for encapsulation and for beverage emulsions. It is a special advantage that these starches are almost colourless and tasteless in solution. When used in encapsulation processes valuable ingredients are most favourably protected against oxidation. In the production of beverage emulsions the high consistency of quality is remarkable, quite opposite to a complete natural ingredient like Gum Arabic. Using OSA starches in culinary products like low fat spreads provide some advantages; e.g., starches are cholesterol free unlike egg yolk. Because starches increase the viscosity of the continuous phase, a cost reduction for the nal product is possible because emulsifying starches may act as a combination of surfactant and stabilizer. It is the objective of the present study to investigate the stabilizing properties of OSA starches in the production of emulsions. Experiments were carried out using two commercially available OSA starches that dier mainly in viscosity of their aqueous solutions. In the experiments, the dispersed phase content, starch concentration as well as pH value and the inuence of dissolved salts of dierent ion strength have been investigated. By droplet size analysis directly after production of oil-in-water emulsions the emulsifying properties of such starches were determined. Storage stability

of such emulsions are part of further studies to be carried out.

2. Materials and methods Commercial vegetable oil and de-ionized water were used for preparation of oil-in-water emulsions. Materials are given in Table 1. Starches were put at the authors disposal for free by National Starch and Chemical GmbH, Hamburg, Germany. Purity Gum 539-E and Purity Gum 2000 are OSA starches developed for emulsication purposes. Instant Clearjel-E is a pregelatinized modied starch for thickening purposes. Starches were completely dissolved in the water phase prior to emulsication. A high-pressure homogenizer (APV Gaulin GmbH, beck, Germany) with a standard valve was used for Lu preparation of emulsions. Pressure was varied from 50 to 250 bar. Two samples were taken at each homogenizing pressure corresponding to a specic energy density: energy density EV J=m3 is calculated by Eq. (1) (Karbstein, 1994): _ P DpV Dp 1 _ _ V V with P is the power intake of the emulsion (W), Dp the _ is the volumetric homogenization pressure (bar), and V ow (m3 =s). One sample of the original emulsion containing the starch was used for measuring rheological properties. In the other sample tube a solution of 5 wt% of the fast stabilizing surfactant sodium-dodecyl-sulfate (SDS) in water was supplied. Mixing the emulsion sample with the SDS-solution freezes the droplet size distribution EV

Table 1 Materials Vegetable oil (rape seed) (Lesieur, Mannheim, Germany) Purity Gum 2000 (National Starch and Chemical GmbH, Hamburg, Germany) q 0:92 g=cm3 g 60 mPa s g 3:3 mPa s (5 wt% in water) pH 4 (5 wt% in water) Cold water soluble OSA starch (E 1450) g 360 mPa s (5 wt% in water) pH 5 (5 wt% in water) Cold water soluble OSA starch (E 1450) g 422 mPa s (5 wt% in water) pH 5 (5 wt% in water) Cold water soluble modied starch (E 1422) ~ 28 838 g=mol M Fast stabilising, water soluble anionic surfactant, not approved for food use ~ 1308 g=mol M Fast stabilising, water soluble non-ionic surfactant (E 433) Spray-dried whey protein mainly consisting of a-lactalbumine and b-lactoglobuline

Purity Gum 539-E (National Starch and Chemical GmbH, Hamburg, Germany)

Instant Clearjel-E (National Starch and Chemical GmbH, Hamburg, Germany)

sseldorf, Germany) SDS (Sodium-dodecyl-sulfate, Texapon K 1296, Henkel KGaA, Du

nau Illertissen GmbH, IllerTween 80 (Polyethylene-(20)-Sorbitan-Monooleate, Gru tissen, Germany) Lacprodan-60 (Arla Foods Ingredients, Denmark)

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immediately after the production of the emulsion by hindering subsequent coalescence. Before particle size analysis the emulsion was centrifuged for 30 min at 1700 g in a high-speed centrifuge (DuPont de Nemours, USA; rotor SS 34) to separate the starch particles from the emulsion. The supernatant was collected and dispersed in water prior to measurement. It was shown that the sample preparation did not change the original droplet size distribution. The droplet size distribution was measured using a laser light scattering system (Malvern Mastersizer X, Malvern Instruments, Germany), allowing the detection of droplets with a minimum diameter of 0.1 lm. Parameters derived from this distribution were calculated by the original software of the instrument. The mean droplet diameter was expressed as the mean Sauter diameter, d3; 2 , which is the diameter of a spherical droplet having the same area per unit volume, SV m1 , as the total collection of droplets in the emulsion Z xmax 6 d3; 2 xq2 x dx 2 SV xmin where x is the droplet diameter (m), q2 x is the surface frequency distribution of droplet diameters m1 . To determine rheological properties of the emulsion, a controlled stress rheometer (CSL-100 Rheometer, sseldorf, Germany) was used at 25 C. Carri-Med, Du Emulsions of low viscosity were measured using a double-gap cylinder, for high-viscous samples a cone/ plate system was used. The aqueous solutions of the starches investigated are shear thinning. Viscosity indicated is given at a constant shear rate of 100 s1 .

Dynamic interfacial tension of starch solutions was measured using a droplet volume tensiometer (Lauda nigshofen, Germany). Dr. R. Wobser GmbH, Lauda-Ko This method allows measurements of dynamic interfacial tension even for solutions of high viscosity as Purity Gum 539-E at 1 wt%. Results were compared with those of common surfactants (e.g., Tween 80 and Lacprodan60), using the bursting membrane method (Anbarci & Armbruster, 1987). This method could not be used for starch systems due to their viscosity.

3. Results 3.1. Dynamic interfacial tension of OSA-starches Dynamic interfacial tension of aqueous starch solutions and solutions of commonly used surfactants, is plotted in Fig. 1. The interfacial tension of Tween 80 decreases to about 8 mN=m within less than 5 s. Tween 80 is considered a fast stabilizing system which is approved for food application. The decrease in interfacial tension of Lacprodan-60 is much slower than for Tween 80; after 100 s a value of 18 mN=m is observed. Lacprodan-60 is a spray dried whey protein consisting mainly of a-lactalbumine and b-lactoglobuline. Due to the higher molar mass and the defolding of proteins taking place during adsorption, its kinetic is rather slow. Interfacial tension of aqueous solutions of Purity Gum 539-E decreases slightly within about 7 s from 27 to 26 mN=m, using Purity Gum 2000 a nal value of 22 mN=m is achieved. If the concentration of Purity

30 interfacial tension / (mN/m)

20

vegetable oil demineralized water modified starches: droplet volume tensiometer Lacprodan-60, Tween 80: bursting membrane method cPurity Gum 539-E = 1 wt.-% cPurity Gum 2000 = 5 wt.-%

10

cPurity Gum 2000 = 1 wt.-% cTween 80 = 5 g/l cLacprodan-60 = 5 g/l

0 10-2

10-1

100

101 102 time t / s

103

104

Fig. 1. Dynamic interfacial tension of the OSA starches Purity Gum 539-E and Purity Gum 2000 (droplet volume tensiometer) in comparison to the dynamic interfacial tension of the surfactant Tween 80 and the whey protein Lacprodan-60 (bursting membrane method).

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Gum 2000 is enlarged to 5 wt%, a lower nal value of c is obtained than for a concentration of 1 wt%. Hence, a further decrease of the interfacial tension of Purity Gum 539-E can be expected at higher concentrations, yet could not be measured due to high viscosity of a 5 wt% solution. These results show that the kinetics of the dynamic interfacial tension of starches is similar to those of proteins and stabilization of interfaces due to adsorbed starch molecules is rather slow. During emulsication, the mean residence time in the apparatus is lower than 4 s (which is the limit of the measuring range of the droplet volume tensiometer). Adsorption of proteins and starches onto newly formed interfaces takes more time than available in the dispersing zone of the apparatus, hence, the inuence of stabilization of interfaces within the homogenizer due to adsorbed molecules of slow emulsiers is negligible. During the subsequent residence time after the actual emulsication step, molecules adsorb to the newly formed interface, thus stabilizing the emulsion. 3.2. Investigation of the stabilizing mechanism of OSA starches For a rst orientation about the starches ability of stabilizing emulsions, experiments with Purity Gum 539-E and Purity Gum 2000 were carried out in comparison with the fast stabilizing anionic surfactant SDS (Fig. 2). Using both types of starches, mean droplet diameters of about 1 lm are obtained, as small as those obtained with SDS. The results of the starches do not dier signicantly from the technical, low molecular weight surfactant SDS. Although SDS is not approved for food emulsions it serves as a benchmark due to its

fast stabilization by electrostatic repulsive forces. After some time, however, creaming is observed in emulsions stabilized with SDS. Emulsions prepared using the starch systems, do not cream because of a higher viscosity of the continuous phase and possibly colloidal solved starch molecules forming a network in the continuous phase. These results show that OSA starches are indeed suitable to produce stable emulsions of small droplet sizes. In Fig. 3 results for Purity Gum 2000 are shown, with the oil content varied. Results for Purity Gum 539-E are alike (not shown). At constant energy density (i.e., homogenization pressure), mean droplet size raises with increasing the oil content. At u 80% the emulsion breaks, if EV > 5 106 J=m3 . The increase of droplet size with higher oil content at constant EV is explained by the enhancing collision frequency and thus, coalescence frequency. In the range of 130%, however, emulsication results are hardly inuenced by the oil content, as coalescence frequency is low (Karbstein, 1994). To investigate the inuence of the type of starch on the emulsication result, experiments were carried out using dierent starches at constant viscosity of the aqueous phase. Viscosity of the aqueous solution of Purity Gum 2000 was increased by adding Instant Clearjel-E, which is not modied by hydrophobic side chains. Also emulsions containing solely Instant Clearjel-E were produced for comparison. The results are shown in Fig. 4. At low energy density, emulsions produced with Instant Clearjel-E have larger mean droplet diameters than those containing Purity Gum 539-E or Purity Gum 2000 mixed with Instant Clearjel-E. Taking the standard deviations into account, this dierence is not to be regarded as signicant. At higher energy

10 Sauter diameter d3,2 / m high-pressure homogenizer oil content = 30 Vol.-% = 5 wt.-% cdissolved= SDS 1 Purity Gum 2000

Purity Gum 539-E

0.1 1 06

1 07 energy density Ev / (J/m3)

1 08

Fig. 2. Sauter diameter in dependence on energy density: OSA starches in comparison to the technical surfactant SDS u 30%. High-pressure homogenizer.

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10 Sauter diameter d3,2 / m emulsions break high-pressure homogenizer cPurity Gum 2000 = 5 wt.-% c = 3.3 mPas oil content / vol.-% 1 1 30 80

0.1 1 06

1 07 energy density Ev / (J/m3)

1 08

Fig. 3. Inuence of the oil content on the Sauter diameter of emulsions stabilized by Purity Gum 2000. High-pressure homogenizer.

densities, there is no inuence of the type of starch used. Emulsions with similar droplet size distributions are produced independent of the composition of the continuous phase. Surprisingly, even droplet sizes of emulsions made with Instant Clearjel-E, only, were small immediately after production. It is known, however, that without the use of surfactants these emulsions tend to break. Emulsions using OSA starches are stable for a prolonged time. In Fig. 5, results for producing emulsions containing Purity Gum 539-E in dierent concentrations are shown. The viscosity of the continuous phase is 360 mPa s for a concentration of 5 wt% and 2.2 mPa s for 0.08 wt%. The concentration of 0.08 wt% was chosen to provide a viscosity similar to the viscosity of aqueous solutions of 5 wt% Purity Gum 2000. Diminishing the concentration
10 Sauter diameter d3,2 / m

of Purity Gum 539-E to 0.08 wt% does not aect the emulsication result for EV < 1 107 J=m3 . It should be noticed that such a low concentration is sucient for stabilizing the emulsion: At 0.08 wt%, the viscosity of the continuous phase is hardly increased. Thus, the probability of coalescence is not decreased due to a lengthened drainage time with increasing viscosity of the continuous phase. The stabilization is therefore not governed by hydrodynamic eects. The stabilization can be attributed to steric stabilization of the oil droplets by starch colloids, which are either attached to the interface or dispersed in the region between two colliding droplets. At energy densities higher than 1 107 J=m3 the emulsion breaks: There is not enough starch provided in the system to stabilize the smaller droplets, i.e., the larger interfacial area.

high-pressure homogenizer oil content = 30 vol.-% c = 360 mPa s cP. G. 2000 = 5.0 wt.-% cInst. C.l-E = 4.84 wt.-% cInst. C.-E = 4.9 wt-% cP. G. 539-E = 5 wt.-%

0.1 1 06

1 07 energy density Ev / (J/m3)

1 08

Fig. 4. Inuence of the type of starch used as additive on the Sauter diameter gc const, u 30. High-pressure homogenizer.

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10 Sauter diameter d3,2 / m high-pressure homogenizer oil content = 30 vol.-%

1 emulsions break

cP. G. 539-E = 5 wt-% c = 360 mPas cP. G. 539-E = 0.08 wt-% c = 2.2 mPas

0.1 1 06

1 07 energy density Ev / (J/m3)

1 08

Fig. 5. Inuence of the starch concentration on the Sauter diameter gc const, u 30. High-pressure homogenizer.

In order to further elucidate if droplets are sterically stabilized by suspended starch particles or by colloidal solved starch molecules, the following experiment was carried out: After producing an emulsion of u 30% containing 5 wt% Purity Gum 539-E at EV 5 106 J=m3 , the suspended particles were separated by centrifugation. The emulsions were observed microscopically before and after centrifugation; no changes in emulsion structure and droplet size were found. This implies that suspended starch particles are not mainly responsible for stabilization. The results presented above indicate that OSA starches stabilize droplets sterically by attachment of colloidal solved starch molecules to the interface.

If droplets are stabilized by steric hindrance, electrostatic forces should not have any inuence on droplet size. In order to investigate the stabilization mechanism of OSA starches, experiments were carried out at various pH and with addition of dierent ions. Ionic strength was kept constant to realize a constant Debyelength. In Fig. 6 results are given, demonstrating the inuence of pH on Purity Gum 539-E; results for Purity Gum 2000 are alike (not shown). As expected, the emulsication result is independent from pH within the range of pH investigated. For elucidating the inuence of ion valence on starch molecules, experiments using NaCl and CaCl2 were carried out at constant ion strength and pH 5 (Fig. 7). As could also be expected,

10 Sauter diameter d3,2 / m

high-pressure homogenizer cPurity Gum 539-E = 5 wt.-% oil content = 30 vol.-% cion = const. = 10 -3 mol/l H + , Cl-, Na + , OH-

1 pH 3 5 7

0.1 1 06

1 07 energy density Ev / (J/m3)

1 08

Fig. 6. Inuence of pH on the Sauter diameter at constant ion-concentration cion 103 mol=l. Purity Gum 539-E u 30. High-pressure homogenizer.

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10 Sauter diameter d3,2 / m

high-pressure homogenizer cstarch = 5 wt.-% oil content = 30 vol.-% ionic strength Iion = const. pH = 5

1 PG 2000 NaCl CaCl2 PG 539-E NaCl CaCl2

0.1 1 06

1 07 energy density Ev / (J/m3)

1 08

Fig. 7. Inuence of ion valence (salts: NaCl; CaCl2 ) on the Sauter diameter at constant ionic strength. High-pressure homogenizer.

the valence of ions does not aect the emulsication result within the range investigated. Also at pH 3 and pH 7 no inuence of the ion valence was detected (not shown). All results conrm that steric hindrance is the main stabilization mechanism in emulsions containing OSA starches. 3.3. Comparison of emulsication results of OSA starches and commonly used surfactants Previous work investigated emulsication with Tween 80 and Lacprodan-60 at dierent pH values in a highpressure homogenizer, using a Microuidizer to prepare sel & Schubert, 1999). In order to the emulsions (Bro compare the results obtained using starches with those

of Tween 80 and Lacprodan-60, Sauter diameters of the emulsions are plotted against energy density for pH 3, 5 and 7 in Fig. 8. The emulsication result obtained using the whey protein Lacprodan-60 (grey symbols) is strongly inuenced by pH. In the range of the iso-electric point of Lacprodan-60, which is at pH 4.3 (Karbstein, 1994), the eective charge of protein molecules is neutral, i.e., there is no electrostatic repulsive force acting between the droplets. Thus, stabilization by Lacprodan-60 at pH 5 is rather poor. Using the anionic, low molecular weight surfactant Tween 80 (open symbols), there is no inuence of pH on droplet size, because the charge of Tween 80 molecules is not aected by pH. The same result is achieved using Purity Gum 539-E (black

100 Sauter diameter d 3,2 / m high-pressure homogenizer oil content = 30 vol.-% cPurity Gum 539-E = 50 g/l 10 pH 3 5 7

cTween 80 = 43 g/l 1 pH 3 5 7

cLacprodan-60 = 17,2 g/l pH 3 5 7

0.1 1 06

1 07 1 08 energy density EV / (J/m3)

1 09

Fig. 8. Inuence of pH on the Sauter diameter of emulsions stabilized the OSA starch Purity Gum 539-E in comparison to the results obtained with the surfactant Tween 80 or the whey protein Lacprodan-60 u 30.

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symbols); there is no inuence of pH on the emulsication result. The Sauter diameters of the emulsions prepared with starch are in the range of the smallest droplets obtained with Lacprodan-60. By increasing the energy density from 5 106 to 2 107 J=m3 , mean droplet diameters of emulsions prepared with starch as well as with Tween 80 are both decreased by a factor of 4. In the case of Tween 80, coalescence immediately after droplet disruption is negligible to a high extent. Also the use of Purity Gum 539-E provides a sucient short term stability. It can be concluded that whey proteins can be replaced by OSA starches in culinary products with the advantage of obtaining good emulsication stability independent of pH value. Test of storage stability, however, was not in the scope of the present investigation and is part of further studies.

sive for stabilization. It was shown that emulsication results are independent of pH value and ion valence. Therefore it can be concluded that steric hindrance is the main stabilizing mechanism of OSA starches. As proteins stabilize emulsion droplets mainly by electrostatic repulsive forces, the emulsication result depends strongly on pH, which leads to poor emulsication at pH values near the iso-electric point. Because electrostatic repulsive forces do not govern the stabilization of emulsions prepared with starches, the experiments suggest that whey proteins can be substituted by OSA starches with a specic advantage at low pH values near the iso-electric point of the protein.

Acknowledgements This research project was supported by the FEI (Forschungskreis der Ern ahrungsindustrie e.V., Bonn), the AiF and the Ministry of Economics and Technology. Project No. 11393 N.

4. Summary and conclusions This paper presents the stabilization of emulsions by OSA starches. Measurements of interfacial tension prove that OSA starches are surface active substances, their dynamic surface tension being comparable to that of whey protein like Lacprodan-60. OSA starches are able to adsorb at interfaces, thus stabilizing droplets against coalescence. It was shown by emulsication experiments that the stabilization of droplets by OSA starches is very ecient: Using Purity Gum 2000 and Purity Gum 539-E, stable emulsions of Sauter diameters of 1 lm were prepared, which is in the range of results obtained by the technical surfactant SDS used as reference. The emulsication results achieved with OSA starches have been found to be independent from the type of starch and the starch concentration above the lower limit of starch needed for stabilization. The results of Purity Gum 539-E show that this limit can be as low as 0.08 wt%. The viscosity of a aqueous solution of 0.08 wt% Purity Gum539-E is very low (2.2 mPa s), thus, increased viscosity of the continuous phase is not deci-

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