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Article

Selected Soluble Dietary Fibres as Replacers of Octenyl Succinic Anhydride (OSA) Starch in Spray-Drying Production of Linseed Oil Powders Applied to Apple Juice

by
Dorota Ogrodowska
1,
Małgorzata Tańska
1,*,
Paweł Banaszczyk
2,
Sylwester Czaplicki
1,
Beata Piłat
1 and
Iwona Konopka
1
1
Faculty of Food Sciences, University of Warmia and Mazury in Olsztyn, Pl. Cieszyński 1, 10-726 Olsztyn, Poland
2
Engineering Department, Process Equipment and Food Biotechnology, Faculty of Food Sciences, University of Warmia and Mazury in Olsztyn, Oczapowskiego 7, 10-719 Olsztyn, Poland
*
Author to whom correspondence should be addressed.
Appl. Sci. 2024, 14(17), 7611; https://doi.org/10.3390/app14177611
Submission received: 19 July 2024 / Revised: 23 August 2024 / Accepted: 25 August 2024 / Published: 28 August 2024
(This article belongs to the Special Issue Effects of Processing on Food Composition, Nutritional Value and Sensory Quality: 2nd Edition)
Browse Figures
Versions Notes

Abstract

:
The aim of the study was to compare two kinds of soluble dietary fibres in a mixture with OSA-starch as wall components of linseed oil capsules. Comparison was made based on emulsion (droplet size, polydispersity index, and viscosity) and powder properties (outer structure, colour, surface oil content, and encapsulation efficiency). Additionally, linseed oil powders were applied to the food model (apple juice) and the colour, physical stability, and volatile compound profile of fortified juice were determined. Although the obtained linseed oil emulsions with different compositions of polysaccharide components showed some variation in droplet size, polydisperse index and viscosity, their encapsulation efficiency by spray-drying was very high (>98%). The powders produced had a similar structure and low surface oil content, and their 2% addition to apple juice did not change its stability and only slightly decreased its colour lightness and yellowness. However, greater differences in the volatile compounds of obtained juices were observed. Overall, the added powders reduced the volatility of aroma compounds typical of apple juice but introduced propanal and hexanal, especially the powders with the highest OSA-starch share.

1. Introduction

Linseed (Linum usitatissimum L.), also called flaxseed, is a source of valuable vegetable oil rich in α-linolenic fatty acid (ALA). This fatty acid is the precursor to long-chain n-3 polyunsaturated fatty acids (n-3 PUFAs) such as eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA). In some varieties of linseed, the ALA share can reach up to 60% [1]. Chia seed oil (Salvia hispanica L.) has an even greater share of this fatty acid [2], but the global production and consumption of linseed oil are still greater than that of chia oil [3,4]. In this context, linseed oil is the best plant source of n-3 fatty acids. Furthermore, the oil is also rich in several antioxidants like tocopherols (mainly γ-tocopherol), phytosterols (mainly β-sitosterol, following campesterol, cycloartenol, Δ5-avenasterol, 2,4-methylenecycloartenol, and stigmasterol), carotenoids (mainly β-carotene), phenols (mainly vanillin, p-hydroxybenzoic and vanillic acid, following caffeic, coumaric, chlorogenic, and ferulic acids, catechin, kaempferol, epicatechin, quercetin-3-rutinoside) [5,6]. Official information on the page of the National Institutes of Health [7] evidence that the consumption of high linseed oil supplements exerted a promising effect in the treatment or prevention of cardiovascular disease and positively affected infant health and development. This organisation also summarised other studies that suggest a possible role in the treatment or prevention of Alzheimer’s disease, dementia, cognitive function, age-related macular degeneration, dry eye disease, and rheumatoid arthritis, but more studies in these fields are needed [7]. The next study summarises other possible pro-healthy roles in depression, inflammation, and osteoporosis [5]. Linseed oil consumption also exhibits immunoregulatory and antibacterial effects [8,9]. Unfortunately, ALA is easily oxidised according to the principles of the free radical theory or photosensitizing oxidation. Oxidised ALA decomposes into various components, which have an unpleasant taste and smell and may be harmful to health [10]. One of the possible methods of protecting this valuable fatty acid is encapsulation and the production of edible powders [11]. Sray-drying is the most common method of oil encapsulation. It allows the emulsion to be transformed into a powder, while not changing its valuable properties. An important aspect of spray-drying is the “evaporative cooling effect”. Almost all of the heat supplied to the drying chamber by the drying gas stream is used up in the evaporation process. In a short time, the latent heat of the evaporating water is removed from the dried particles. Due to the large surface area of the droplets, the water evaporates almost immediately, and the droplets are transformed into particles. Drying is a well-established method of preserving liquid foods, because it significantly limits the growth of microorganisms and enzymatic degradation reactions [11,12].
Edible powders made by spray-drying are composed of core material (lipids, vitamins, phenolic compounds, etc.) and a wall matrix surrounding the core. Wall matrix is typically built by various starch preparations, proteins, non-starch polysaccharides (e.g., cellulose, glucans, pectins, gums, chitin, and mucilages), or their mixtures. Proper choice of wall components is crucial for encapsulation efficiency as well as for microcapsule size and stability [13]. Solubility, viscosity, emulsifying properties, thermal stability, and mechanical properties of wall materials affect microcapsule size and encapsulation efficiency [14].
Starches or maltodextrin modified by the use of octenyl succinic anhydride (OSA-starches) are often used as stabilisers and emulsifiers in the food industry, including encapsulation processes [15]. Type/biological origin of starch and processing conditions (e.g., use of acid vs. α- or β-amylase hydrolysis, mechanical, hydrothermal, or ultrasound treatment) are key factors that affect emulsion and powder final properties [16]. In general, the use of low molecular weight OSA-starch tends to provide high encapsulation efficiency and capacity, while for high molecular weight results, the opposite is true (more data in [15]). To date, OSA-starches have been used, for example, to encapsulate avocado oil [17] and fish oil [18], and the obtained powders had good oxidative stability.
Although maltodextrin and OSA-starch are popular wall matrix ingredients, there is still a need to look for reduced-calorie wall materials. Such materials can be prebiotics like Nutriose® and inulin. Nutriose® is a soluble fibre obtained from non-GMO raw materials (wheat, corn, or pea), produced by Roquette company [19]. In this preparation, the distribution of α-D 1,4-, 1,6-, 1,2-, and 1,3-glycosidic bonds is 41%, 32%, 13%, and 14%, respectively [20]. Only 15% of Nutriose® is enzymatically digested in the small intestine and provides 1.7 kcal/g [20]. The molecular weight of Nutriose® varies from 3500 to 6000 Da [21,22]. In contrast, inulin is extracted primarily from the chicory root, but it is also found in garlic, onion, Jerusalem artichoke, and other plants [23]. It is a fructan consisting of fructosyl units linked by β-D (2,1) glycosidic bonds with a fully proven prebiotic function [24]. The molecular weight of inulin varies from 500 to 13,000 Da [25]. Energy supply by inulin is 1.5 kcal/g [26].
The aim of the study is to compare the effects of soluble dietary fibre Nutriose® (SDF N) and soluble dietary fibre inulin (SDF I) used in a mixture with OSA-starch on the properties of linseed oil emulsion and the powder obtained from it by spray-drying. Additionally, a real food model (apple juice) with the resulting linseed oil powders for colour, aroma, and oxidative and physical stability was tested. Apple juice was selected as a model since colour and stability changes can be easily observed because of its optical clarity [27]. Furthermore, it is the most-produced fruit juice in the world [28].

2. Materials and Methods

2.1. Materials and Chemicals

Cold-pressed linseed oil was purchased from J.A.W. Łącz Przetwórstwo Roślin Oleistych-Nasiennictwo sp. z o.o. (Świecie nad Osą, Poland). Nutriose® (soluble maize fibre) and octenyl succinic anhydride starch (OSA-starch, waxy maize basis) were purchased from Roquette (Lestrem, France). Inulin from chicory root was purchased from Simpatiko sp. z o.o. (Łuże, Poland). Organic apple naturally cloudy direct juice was purchased from Jacoby Fruchtsäfte GmbH (Auggen, Germany).
Analytical grade n-hexane was purchased from Sigma-Aldrich (Poznań, Poland).

2.2. Emulsions Preparation and Spray-Drying

Emulsions (2 L) containing 70% distilled water (temperature of 20 °C), 10% cold-pressed linseed oil, and various amounts (5, 10, or 15%) of wall materials such as soluble dietary fibres such as Nutriose® (SDF N) and inulin (SDF I) SDF I, and OSA-starch were formed at a temperature of 30 °C for 20 min using Thermomix (Vorwerk Elektrowerke GmbH & Co. KG., Wuppertal, Germany) and then homogenized using a M110P Microfluidizer® Processor (Microfluidics International Corporation, Westwood, MA, USA) at 150 MPa. Six emulsions were prepared, and their formulations are presented in Table 1.
Immediately after preparation, the emulsions were subjected to spray-drying using a pilot plant spray dryer (A/S Nitro Atomizer, Copenhagen, Denmark). An inlet air temperature in the range of 123–129 °C and an outlet temperature in the range of 72–78 °C were applied in the drying process. The feed flow rate was set at 77 mL/min and controlled during the process.

2.3. Food Model Preparation

The food model was apple juice with a 2% addition of spray-dried linseed oil powders. Model juice was prepared by mixing 200 mL of the commercial apple juice with 4 g of the spray-dried powders in a 200 mL bottle and pasteurized at a temperature of 90 ± 1 °C for 60 s in a water bath with stirring. The fortified juice was then cooled to room temperature and tested immediately.

2.4. Characterization of Emulsions

2.4.1. Droplet Size Distribution, Mean Particle Diameter (Z-Average) and Polydispersity Index (PDI) Analyses

Droplet size distribution of the fresh and reconstituted emulsion was determined by dynamic light scattering using the Malvern Zetasizer Nano ZS90 (Malvern Instruments Ltd., Worcestershire, UK), and then the mean particle diameter (Z-average) and polydispersity index (PDI) were calculated. Additionally, the powders were dissolved in water, thanks to which the initial composition of the emulsion was obtained (reconstituted emulsion) (Table 1). All tests were performed in triplicate at a temperature of 25 °C, and the results were shown as the mean ± standard deviation (SD).

2.4.2. Emulsion Viscosity Analysis

The emulsion viscosity was determined using a Brookfield RV DV–II+ Pro Extra (Ametek Brookfield, Middleboro, MA, USA). The measurement was performed in triplicate in parallel plate geometry at a temperature of 25 ± 1 °C. The apparent viscosity measured by the Brookfield viscosimeter, which works as any strain-controlled rheometer—since it applies angular velocity (reported in rotation-per-minute units, RPM) and measures torque (reported in percentage of the maximum torque specific for the given type of the instrument) [29].

2.5. Characterization of Powders

2.5.1. Surface Oil Content Analysis

Surface oil content was analysed by its extraction from powders with n-hexane added at a ratio of 1:10 (w/v) and shaken for 2 min at a temperature of 20 ± 2 °C. The solvent was then filtered, and the collected solid residue was rinsed three more times with 20 mL of n-hexane. The collected filtrates were evaporated using a rotary evaporator (Büchi Labortechnik AG, Flawil, Switzerland). Then residue was weighted, and the surface oil content was calculated as a percentage of the powder.

2.5.2. Encapsulation Efficiency Analysis

The encapsulation efficiency (EE) of emulsion was calculated by dividing the amount of encapsulated oil (determined as the difference between the total and surface oil content) by the total oil content of the powder and then multiplying by 100%. The total oil content was the theoretical amount of oil in the anhydrous fraction of the prepared emulsion.

2.5.3. Powder Morphology Analysis

Powder morphology was analysed using scanning electron microscopy (SEM). SEM Quanta 200 (FEI Company, Hillsboro, OR, USA) was used for the analysis. Powder was attached to the microscope state using two-sided adhesive tape, mounted on SEM tubs, and coated with palladium in a sputter coater. Then the powder surface was analysed at an accelerating voltage of 30 kV and ×400 magnifications.

2.6. Characterization of Juices

2.6.1. Colour Analysis

The colour of juices was measured using digital image analysis (DIA), which consisted of a computer with a monitor, a digital camera (DXM-1200, Nikon Inc., Melville, NY, USA), a light set (colour temperature about 5400 K, Kaiser Fototechnik GmbH and Co., KG, Buchen, Germany), and LUCIA G v. 4.8 software (Laboratory Imaging, Praha, Czech Republic). The parameters of the CIEL*a*b* colour model were determined for each juice sample (20 mL in a 50-mL beaker) at a temperature of 20 ± 1 °C [30]. The L* value represents lightness (from black to white for values in the range from 0 to 100, respectively), the a* value represents the green or red colour (negative or positive values, respectively), and the b* value represents the blue or yellow colour (negative or positive values, respectively). Additionally, the chroma (C*, the degree of colour saturation) was calculated with the following formula: C* = √(a*² + b*²), and the total colour difference (ΔE) comparing fortified samples to control sample was calculated with the following formula: ΔE = √(ΔL*² + Δa*² + Δb*²).

2.6.2. Physical Stability Analysis

The physical stability of fresh and stored (1, 2, and 6 days) juices was determined using the Turbiscan Classic 2 (Formulaction Co., Toulouse, France) by measuring the backscattering of light (ΔRW). The profile of changes in the backscattering coefficient (RW) over time was analysed, and the slope coefficient of the curve was calculated.

2.6.3. Juice Volatile Compounds Analysis

A juice sample (5 mL) was placed into a 20 mL headspace screw top vial, incubated at 80 °C for 20 min, and shaken at 500 rpm. The analysis of volatile compounds in 2.5 mL of the headspace was performed using an Agilent model 8890 series (Agilent Technologies, Santa Clara, CA, USA) gas chromatograph in combination with an MPS Robotic autosampler (GERSTEL GmbH & Co.KG, Mülheim an der Ruhr, Germany) and an Agilent 7000D QQQ mass detector (Agilent Technologies, Santa Clara, CA, USA). The compounds were separated using a Zebron ZB-624plus column (30 m × 0.25 mm × 1.4 μm) purchased from Phenomenex Inc. (Torrance, CA, USA). The following temperature program was applied during the analysis: 40 °C, followed by holding for 5 min; 11 °C/min up to 80 °C; and 22 °C /min up to 250 °C, followed by holding for 2 min. The temperature for the injection port was 200 °C, the ion source was 230 °C, the quadrupole was 150 °C, and the interface was 230 °C. Mass spectra were obtained in the electron impact at 70 eV in a scan range from m/z 10 to 200. The detected compounds were identified by comparing their mass spectra with the NIST20L MS library.

2.7. Statistical Analysis

The statistical analysis of the data was performed using Statistica 13.1 software (StatSoft, TIBCO, Palo Alto, CA, USA). The results were analysed statistically using a one-way ANOVA with a Tukey test, and statistically significant differences were considered if the p-value was below 0.05.

3. Results and Discussion

3.1. Physical Properties of Prepared Linseed Oil Emulsions

Emulsions (size < 200 nm) solve the problem of the solubility of hydrophobic materials and enable their use in aqueous food systems with improved bioavailability and targeted delivery [31]. In many applications, the dry emulsion (the powder produced from the emulsion after drying) should be able to reconstitute the primary emulsion after rehydration [32]. Therefore, the particle size distributions in fresh emulsions (E) and those reconstituted from the obtained powder in water (ER) were compared. The results are shown in Figure 1, while their compositions were presented in Material and Methods. As a result of the comparative analysis, it was shown that emulsions reconstituted from powder have a slightly different microstructure than fresh emulsions. Although all samples were monodispersed, none of the emulsion samples reconstituted from powder were able to fully reproduce the particle size distribution profile of the original emulsion. In the case of samples Nos. 1, 2, and 4, the particle size distribution of the reconstituted emulsion was wider than that of the original emulsion.
The polydispersity index (PDI) for samples Nos. 1, 2 and 4 had values of 0.11, 0.12, and 0.14 for E and 0.19, 0.21, and 0.19 for ER, respectively, with the average particle size (Z-average) being 175.02 nm, 167.70 nm, and 170.34 nm for E and 199.24 nm, 199.68 nm, and 204.59 nm for ER (Table 2). In the case of emulsion samples Nos. 5 and 6 (containing 10% and 15% SDF I), changes in the structure caused by drying and redispersion were not as visible as in the previous ones. The PDI values for samples Nos. 5 and 6 were 0.14 and 0.13 for E and 0.18 and 0.17 for ER, respectively, with an average particle size (Z-average) of 177.38 nm and 197.31 nm for E, and 195.02 nm and 223.19 nm for ER. The best reproduction of the particle size distribution profile for the emulsion reconstituted from powder relative to the original emulsion was obtained in the case of sample No. 3 (coating: 15% SDF N + 5% OSA-starch). The value of the PDI was 0.10 for E and 0.12 for ER, while the average particle size was 166.60 nm for E and 174.28 nm for ER. The PDI in the emulsions is the standard deviation of the particle diameter distribution divided by the mean particle diameter and is related to several factors, such as the homogenizing process, the use of emulsifiers, and the concentration and properties of the wall material. When values are close to 1, this indicates heterogeneity, whereas values less than 0.5 indicate more uniformity and homogeneity of particle dispersion [33]. According to Jan et al. [34], a mean particle size of <200 nm and a PDI < 0.5 are usually preferred for the emulsion. Only in samples Nos. 4 and 6 for the reconstituted emulsions values above 200 nm were obtained. The obtained results are consistent with those reported by El-Messery et al. [35]. In their study, high-pressure homogenization at 172.3 MPa (in our study 150 MPa) led to the formation of an emulsion with nano-size droplets, whose diameter varied from 154 to 162 nm. Also, Sharif et al. [31] using a microfluidizer at 100 MPa pressure obtained an emulsion with droplets in the range of 100-558 nm, and the particle size increased with the increase in starch concentration. On the other hand, Domian et al. [32] reported that an increase in water hardness resulted in a significant increase in the size of the smaller particles, especially in the emulsion reconstituted from spray-dried powders with a lower content of the oil phase.
Dynamic shear rheometers, such as the Brookfield rotational rheometer, are popular devices for simple measurements of the viscosity of emulsions at a single speed. This type of viscometer uses shear deformation force and measures viscosity based on the torque required to rotate a spindle immersed in the fluid, which increases proportionally to the viscosity of the sample [36]. Factors influencing the value of this parameter in an oil-in-water (o/w) emulsion system include chemical composition, density, particle size of the dispersed phase, temperature, shear rate, and shear stress [37]. In our study, emulsions Nos. 1 and 4 with the highest content of OSA-starch were characterised by the highest viscosity of 269.51 and 242.20 mPa·s, respectively (Table 2). According to Agama-Acevedo and Bello-Perez [38], OSA-starch is an emulsifier that causes an increase in viscosity and physical stability. Powders with the highest content of SDF N and SDF I (samples Nos. 3 and 6) had the lowest viscosity of 58.67 and 42.80, respectively. Our research is consistent with that presented by Carneiro et al. [39] verified that a mixture of maltodextrin and Capsul TA® (n-octenyl succinic anhydride (OSAN)—modified starches derived from tapioca starch) has shown higher viscosity in comparison to those produced with WPC and Hi-Cap (derived from waxy maize). El-Messery et al. [35] reported that increasing total solids concentrations (by increasing the amount of oil in the emulsion) resulted in an increase in the viscosity of the emulsion, but in our study, this parameter was clearly influenced by the coating components.

3.2. Physical Properties of Linseed Oil Powders

3.2.1. Encapsulation Efficiency and Surface Oil Content

The surface oil content ranged from 0.41% (sample No. 1) to 0.57% (sample No. 6) (Table 3), and these values are very low compared to those obtained in our previous studies, where we used polysaccharide microcapsule coatings [11,40]. On the other hand, these values are similar to those presented by Domian et al. [32]. In their study, surface oil content ranged from 0.14 to 2.27% for powders with OSA-starch and linseed oil. This shows that not only the high-pressure homogenization process has an impact on the surface oil content but also on the coating ingredients used. The ability to capture bioactive ingredients is defined as encapsulation efficiency, which can be expressed as a ratio of encapsulating substances trapped in the total amount of initially encapsulated substances added to the emulsion. Encapsulation efficiency (EE) was at a high level in the range of 98.27–98.76% (Table 3). El-Messery et al. [35], using similar homogenization pressure (~170 MPa) and obtaining similar emulsion particle size (~160 nm), obtained a much lower EE range of between 62.2 and 78.8%. Jan et al. [34] reported that the average EE of the optimised emulsion formulation was found to be 91%. In a study conducted by Karim et al. [41], encapsulated delphinidin-3-O-sambubioside had good EE ranging from ~88 to 97%. The authors also found that higher concentrations of SDF N exerted the highest EE, but in our study, this relationship has not been confirmed. Similar to research conducted by Carneiro et al. [39], the results obtained for EE could not be related to the emulsion droplet size or viscosity. The insignificant differentiation between EE results can be explained by the differences between the polymer matrices formed by each one of the wall materials used, which have different retention properties and film-forming properties.

3.2.2. Powder Morphology

Scanning electron microscopy (SEM) images of the powders obtained from emulsions showed that particle shapes and surface regularities were quite similar regardless of SDF I or SDF N presence (Figure 2). The particles had a generally highly porous structure and varied sizes. Some differences can be observed in samples with the lowest OSA-starch concentration (samples Nos. 3 and 6), where particle deformation appears to be lower. Furthermore, the powders containing SDF N (samples Nos. 1–3) were characterised by a higher number of fine particles than those with SDF I (samples Nos. 4–6). This morphological characterization of oil powders differs significantly from that presented for powders composed of linseed oil, maltodextrin, milk protein, and guar gum, where a regular and globular particle shape is observed [39]. Globular particle shapes were also presented by Sotelo-Bautista et al. [42], encapsulating an emulsion containing avocado oil and a mixture of OSA-starch and maltodextrin as wall materials. In turn, Granados-Vallejo et al. [43] reported that polysaccharide spray-dried powders (e.g., OSA-starch) are characterised by spherical particles of several sizes with outer surfaces free of pores, but more dents are observed on their surface. Also, He et al. [44] encapsulated conjugated linoleic acid with OSA-starch and obtained microcapsules whose surface morphology was lacking in cracks. They explained this phenomenon by the strong viscoelastic properties of the wall material during expansion at the final stage of spray drying. Such properties of wall material to prevent capsule breakage can probably be linked to the low surface fat content of the powders, and thus the high encapsulation efficiency of the linseed oil (Table 3). The cited authors also observed wrinkles on the surface of most microcapsules, which is consistent with our study.

3.3. Physical Properties of Juice with Linseed Oil Powders

3.3.1. Colour

The results of the colour measurements of the model juices are shown in Table 4. The colour of pure juice (J, without additives) showed the highest lightness (L* = 95.15 ± 0.4) and yellowness (b* = 10.09 ± 1.23), and the lowest greenness (a* = −2.10 ± 0.15). The colour of the juice samples with added powders differed significantly from the control sample (p ≤ 0.05). Regardless of the powder wall composition, only minor differences were observed in the colour parameters of the fortified juices, which are also visible in the photo (Figure 3). The average values were as follows: L* ranged from 88.13 to 89.78, a* ranged from −3.27 to −2.75, and b* ranged from 6.96 to 8.69. Juices with powders containing equal amounts of OSA-starch and SDF I or SDF N (samples Nos. 2 and 5) were the most distinct in colour compared to the control sample, as confirmed by ΔE values greater than 7. In contrast, the highest concentration of SDF I and the lowest concentration of OSA-starch (sample No. 6) resulted in the smallest changes in colour, although the total difference of 5.78 still indicated perceptible colour differences to an observer. The chroma of apple juice (C* = 10.09) was also decreased by the addition of powders, with the highest change noted (a decrease of more than 26%) in the case of the SDF I and OSA-starch proportion 1:1 in powder formulation (sample No. 5). In a study conducted by Yousefi et al. [45], colour variation was higher in samples with encapsulated probiotics compared to that in free bacteria. This could be associated with the existence of colourless xanthan–chitosan microcapsules in the yellow background of the apple juice, which led to a decrease in colour. As shown in Figure 3, the addition of capsules reduced the transparency of juice. Zhang et al. [46] presented the same observations for apple juice fortified with DHA/EPA emulsion.

3.3.2. Physical Stability

Figure 4 shows changes in backscattering of light (ΔRW), and backscattering coefficients (RW) for juices fortified in powders. The measuring vessel of the apparatus was each time filled with the same volume of liquid to a height of 65 mm, understood as a concave meniscus. In this way, it was possible to observe the appearance of a separate phase, which in drinks manifests itself as a “ring” visible at the boundary of the liquid and air if the beverage is stored in transparent packaging, e.g., a bottle. The variability of the RW coefficient value for all juice samples fortified with encapsulated linseed oil reconstituted from powder after 6 days of storage does not exceed 3.1%. The instability of emulsion results migration of particles leading to creaming or sedimentation [32]. The phenomenon of sedimentation was observed in each sample, but in sample no 4, it was least visible. In samples Nos. 1, 2, 5, and 3/6 at a height of 61 to 65 mm, the recorded RW values most strongly reveal the separation of a separate phase. Zhang et al. [46] also obtained stable apple juice with the addition of powders and explained this by the fact that the ultra-fine droplets of the emulsion dramatically reduce the gravity, and Brownian motion is sufficient to overcome the gravity and thus make it difficult to negatively affect the fruit juice during storage. Our results show that samples were quite stable against separation during storage, and it is possible to incorporate powders into food and beverages.

3.4. Volatile Compounds of Apple Juice with Linseed Oil Powders

The volatile compounds of apple juices are presented in Figure 5. Three groups of compounds were detected in pure juice: esters (ethyl acetate, butyl acetate, 2-methylbutyl acetate, and hexyl acetate), alcohols (ethanol, 2-methyl-1-butanol, and 1-nonanol), and aldehyde (hexanal). An even higher number of volatile compounds in apple juices produced from four varieties of apples planted in China was previously presented [47], but in the cited study, the salting-out effect was applied. Juices fortified with 2% of prepared linseed oil powders showed a significant change in relation to pure juice. In all variants, increased hexanal content (Figure 6) was noted, and additionally, propanal appeared. The highest propanal content was noted in juices with capsules of the highest OSA-starch share (samples No. 1 and 4) and gradually diminished. We tried to find scientific sources that would indicate potential production paths for propanal, but we were unsuccessful. Propanal seems to be a relatively easy chemical to produce, as it was found among a few compounds in prototypical interstellar clouds [48]. In contrast, hexanal was determined to be a marker of undergoing oxidation and degradation product of linoleic acid [49]. Hexanal content in fortified apple juices was the highest in variants with the highest OSA-starch share (samples Nos. 1 and 4) and gradually decreased with a diminishing share of OSA-starch in the capsule wall. Furthermore, it was noted that the volatile compound profile was also influenced by the highest concentration of SDF I (sample No. 5). Compared to other samples with this wall component (sample Nos. 4 and 6), it contained more volatile compounds, except for hexanal and propanal. Degradation of SDF I can probably be the result of low pH in the juice and high temperature during pasteurisation, as suggested by studies of the chemical stability of inulin solutions under various pH and temperature conditions conducted by Glibowski and Bukowska [50].
The content of volatiles typical for apple juice was diminished in the headspace of fortified juice samples. It is probably a result of the enhanced viscosity of fortified juices. The volatility of individual compounds depends on the viscosity of the liquid. Increasing the viscosity of apple juice tends to decrease some aspects of flavour intensity by the descriptive panel [51].

4. Conclusions

The presented study showed that both soluble fibres, (SDF N) and inulin (SDF I), used in a mixture with OSA-starch, influenced the properties of emulsion and obtained powder. Emulsions reconstituted from powders had a slightly different microstructure than fresh samples, with the best particle size distribution profile of the reconstituted emulsion compared to the original emulsion occurring in the case of the sample containing 15% SDF N and 5% OSA-starch. SEM images showed that powders containing SDF N had a higher number of fine particles than those containing SDF I. However, the composition of the coating materials had no significant effect on the surface oil content, which remained extremely low. Juices with powders containing the same amounts of OSA-starch and SDF I or SDF N, were characterized by the most distinct colour compared to the control sample. The highest concentration of SDF I and the lowest concentration of OSA-starch resulted in the smallest changes in colour, however the colour change was still visible to the observer. The fortified juices were stable during storage, but greater differences were observed in the content of volatile components of the obtained juices. The added powders reduced the volatility of aroma compounds typical of apple juice but introduced propanal and hexanal, especially the powders with the highest OSA-starch share. The comparison of SDF N and SDF I showed that the impact of both of these preparations on the properties and functionality of linseed oil capsules in apple juice was practically the same. These results show that it is possible to add nanocapsules of omega-3-rich oils to apple juice to increase its nutritional value, but pilot-scale studies are needed.

Author Contributions

Conceptualization, D.O. and M.T.; methodology, D.O., M.T., S.C. and P.B.; formal analysis, D.O., M.T., P.B., S.C. and B.P.; investigation, D.O., M.T., P.B., S.C. and I.K.; resources, D.O.; data curation, D.O., M.T., S.C. and I.K.; writing—original draft preparation, D.O., M.T., S.C. and I.K.; writing—review and editing, D.O., M.T., S.C. and I.K.; visualization, M.T., P.B. and S.C.; supervision, I.K.; project administration, D.O.; funding acquisition, M.T. and I.K. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

The raw data supporting the conclusions of this article will be made available by the authors on request.

Acknowledgments

The authors would like to thank Waldemar Brandt for technical assistance during the spray drying process and SEM images of obtained powders.

Conflicts of Interest

The authors declare no conflicts of interest.

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Applsci 14 07611 g001
Figure 1. Fresh (E) and reconstituted emulsion (R) droplet size distribution. Nos. 1–6 according to description in Table 1.
Figure 1. Fresh (E) and reconstituted emulsion (R) droplet size distribution. Nos. 1–6 according to description in Table 1.
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Applsci 14 07611 g002
Figure 2. SEM images of linseed oil powders (mag ×400). Nos. 1–6 according to description in Table 1.
Figure 2. SEM images of linseed oil powders (mag ×400). Nos. 1–6 according to description in Table 1.
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Applsci 14 07611 g003
Figure 3. Pure (sample No. 0) and fortified juices (samples Nos. 1–6). Nos. 1–6 according to description in Table 1.
Figure 3. Pure (sample No. 0) and fortified juices (samples Nos. 1–6). Nos. 1–6 according to description in Table 1.
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Applsci 14 07611 g004
Figure 4. Changes in the backscattering of light (ΔRW), and backscattering coefficient (RW) in the height range of 7–70 mm observed for fortified juices. Nos. 1–6 according to description in Table 1.
Figure 4. Changes in the backscattering of light (ΔRW), and backscattering coefficient (RW) in the height range of 7–70 mm observed for fortified juices. Nos. 1–6 according to description in Table 1.
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Applsci 14 07611 g005
Figure 5. Results of headspace GC-MS analysis of volatile compounds of apple juices. 0—pure juice; 1–6—juices with linseed oil powders as in Table 1. Data are presented in rows as percent change according to pure apple juice separately for each compound. The highest and the lowest values are marked by the most red and green colours, respectively. Colourless cell mean compound was not detected. * For the propanal content samples Nos. 1–6 are categorized according the sample No. 4 with the highest concentration of this compound.
Figure 5. Results of headspace GC-MS analysis of volatile compounds of apple juices. 0—pure juice; 1–6—juices with linseed oil powders as in Table 1. Data are presented in rows as percent change according to pure apple juice separately for each compound. The highest and the lowest values are marked by the most red and green colours, respectively. Colourless cell mean compound was not detected. * For the propanal content samples Nos. 1–6 are categorized according the sample No. 4 with the highest concentration of this compound.
Applsci 14 07611 g005
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Figure 6. Hexanal peak area in pure and fortified juices. a–d—different letters indicate statistically significant differences (p ≤ 0.05). Nos. 1–6 according to description in Table 1.
Figure 6. Hexanal peak area in pure and fortified juices. a–d—different letters indicate statistically significant differences (p ≤ 0.05). Nos. 1–6 according to description in Table 1.
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Table 1. Emulsion composition table (%).
Table 1. Emulsion composition table (%).
SampleWaterLinseed OilSDF NSDF IOSA-Starch
170105-15
2701010-10
3701015-5
47010-515
57010-1010
67010-155
Table 2. Fresh and reconstituted emulsion physical parameters.
Table 2. Fresh and reconstituted emulsion physical parameters.
Mean Particle Diameter [nm]Polydispersity IndexViscosity [mPa·s]
Fresh
1175.02 ± 1.5 c0.12 ± 0.02 b269.51 ± 11.8 f
2167.70± 1.9 a0.11 ± 0.01 a152.97 ± 13.0 d
3166.60 ± 1.7 a0.10 ± 0.01 a58.67 ± 0.8 b
4170.34 ± 1.7 b0.14 ± 0.01 bc242.20 ± 13.2 e
5177.38 ± 2.3 d0.14 ± 0.01 c85.20 ± 1.8 c
6197.31 ± 2.5 e0.13 ± 0.01 bc42.80 ± 1.0 a
Reconstituted
1199.24 ± 2.7 c0.21 ± 0.02 e
2199.68 ± 2.0 c0.19 ± 0.01 cd
3174.28 ± 1.4 a0.12 ± 0.01 a
4204.59 ± 2.1 e0.19 ± 0.01 d
5195.02 ± 1.5 b0.18 ± 0.01 bc
6223.19 ± 1.4 d0.17 ± 0.02 b
a–f—different superscript letters shown in columns (separately for fresh and reconstituted emulsion samples) indicate statistically significant differences (p ≤ 0.05). Nos. 1–6 according to description in Table 1.
Table 3. Surface oil and encapsulation efficiency of linseed oil powders.
Table 3. Surface oil and encapsulation efficiency of linseed oil powders.
SampleSurface Oil [%]Encapsulation Efficiency [%]
10.41 ± 0.03 a98.76 ± 1.8 b
20.42 ± 0.01 a98.73 ± 1.3 b
30.54 ± 0.06 b98.36 ± 1.5 a
40.55 ± 0.03 b98.33 ± 1.0 a
50.44 ± 0.02 a98.67 ± 2.1 b
60.57 ± 0.02 b98.27 ± 2.0 a
a,b—different superscript letters shown in columns indicate statistically significant differences (p ≤ 0.05). Nos. 1–6 according to description in Table 1.
Table 4. Colour parameters of pure and fortified juices.
Table 4. Colour parameters of pure and fortified juices.
Sample No.L*a*b*C*ΔE
Pure95.15 ± 0.4 c−2.10 ± 0.15 d10.09 ± 1.23 c10.31-
188.59 ± 0.6 a−3.22 ± 0.10 a7.94 ± 0.29 ab8.576.99
288.39 ± 0.4 a−3.27 ± 0.05 a7.80 ± 0.58 ab8.467.23
388.36 ± 0.5 a−3.06 ± 0.02 b8.69 ± 0.81 b9.217.00
488.92 ± 0.0 a−3.03 ± 0.00 b8.59 ± 0.00 b9.116.48
588.13 ± 0.8 a−3.09 ± 0.04 b6.96 ± 0.98 ab7.627.75
689.78 ± 1.2 b−2.75 ± 0.11 c8.05 ± 0.92 b8.515.78
a–d—different superscript letters shown in columns indicate statistically significant differences (p ≤ 0.05). Nos. 1–6 according to description in Table 1.
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Ogrodowska, D.; Tańska, M.; Banaszczyk, P.; Czaplicki, S.; Piłat, B.; Konopka, I. Selected Soluble Dietary Fibres as Replacers of Octenyl Succinic Anhydride (OSA) Starch in Spray-Drying Production of Linseed Oil Powders Applied to Apple Juice. Appl. Sci. 2024, 14, 7611. https://doi.org/10.3390/app14177611

AMA Style

Ogrodowska D, Tańska M, Banaszczyk P, Czaplicki S, Piłat B, Konopka I. Selected Soluble Dietary Fibres as Replacers of Octenyl Succinic Anhydride (OSA) Starch in Spray-Drying Production of Linseed Oil Powders Applied to Apple Juice. Applied Sciences. 2024; 14(17):7611. https://doi.org/10.3390/app14177611

Chicago/Turabian Style

Ogrodowska, Dorota, Małgorzata Tańska, Paweł Banaszczyk, Sylwester Czaplicki, Beata Piłat, and Iwona Konopka. 2024. "Selected Soluble Dietary Fibres as Replacers of Octenyl Succinic Anhydride (OSA) Starch in Spray-Drying Production of Linseed Oil Powders Applied to Apple Juice" Applied Sciences 14, no. 17: 7611. https://doi.org/10.3390/app14177611

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