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Gum Arabic, known for its natural, biodegradable, and non-toxic attributes, holds significant promise in encapsulation. Despite the limited capacity of its natural form to create particles or fibers, this study aimed to produce nanocapsules through co-axial electrospraying, employing a solution of Gum Arabic/poly(vinyl alcohol) for the shell and Irgasan for the core. Additionally, process and solution parameters during co-axial electrospraying have been optimized. Solvent concentrations, total feed rates of shell/core solutions, needle tip to collector distance, electric field, and needle diameter have been studied in detail as a part of this optimization. Their effects on nanocapsule formation were observed through SEM images for morphological analyses and TEM images for observing capsule wall formation. The study thoroughly examines the properties of the resulting nanocapsules, reporting successful acquisition in the nano size range and monodispersity. This highlights the co-axial electrospraying method’s potential for the nanoencapsulation of Gum Arabic and Irgasan.
The Nonwovens Institute, North Carolina State University, Raleigh, NC, USA
Serap Gamze Serdar*
Department of Textile Engineering, Gaziantep University, Gaziantep, Turkey
Hatice Ibili
Department of Textile Engineering, Gaziantep University, Gaziantep, Turkey
Bilgen Çeliktürk Kapar
Department of Textile Engineering, Gaziantep University, Gaziantep, Turkey
*Address all correspondence to: sgserdar@gantep.edu.tr
1. Introduction
Gum Arabic (GA) has been widely utilized for its certain advantages such as wide availability, cost-effectiveness, and biocompatibility; furthermore, it offers exceptional encapsulation properties such as high efficiency, controlled release, and protection against compound degradation. The most common type is derived from Acacia senegal—Senegal trees [1]. GA is typically characterized as neutral or mildly acidic and primarily constitutes a branched complex polysaccharide structure, enriched with mineral combinations of potassium, magnesium, and calcium salts [2].
Currently, GA finds extensive application across the food and pharmaceutical sectors, especially in food processing to enhance texture and consistency. GA can be employed in lower-calorie candies [3], serving as a coating agent [4, 5], pigment stabilizer [3, 6], emulsifier [3, 7], and texture enhancer [7] in various products such as candies, jellies, soups, and dessert mixes [1]. GA serves multiple roles in cosmetics, including stabilizing lotions and protective creams by enhancing viscosity and providing a smooth texture. It also acts as an adhesive in blushers and a foam stabilizer in liquid soaps. Furthermore, GA functions as a dispersant in paints ensuring uniform distribution of pigments and active ingredients. Within the textile sector, it serves as a thickening agent in printing pastes for dyeing cellulose fabrics [3]. Microcapsules are obtained by encapsulating very small liquid droplets, solid particles, or gases with a continuous film or polymer material [1]. Common encapsulation methods include spray drying [8, 9], electro-spraying [10], and coacervation [11].
There are numerous studies on microencapsulation, with GA being commonly used in most of them [12]. GA is typically used as an auxiliary material or viscosity enhancer in the electrospraying process [13]. In the study conducted by Stinjman et al. [14] a total of 17 natural polymers were divided into three groups to examine their electrospinning capabilities: polysaccharides obtained from microorganisms, polysaccharides obtained from algae, and polysaccharides obtained from plant cells and plant exudates. GA was included in the third group, and a 50% concentration was prepared and subjected to the electrospinning process. During the process, droplets were observed at the needle tip, but electrospinning could not be achieved. In another study, researchers aimed to explore the impact of combining synthetic and natural biopolymers with GA on the encapsulation of probiotics. The utilization of GA enhanced the viability of cells within the electrosprayed capsules [15]. GA was also used as a nanocomposite scaffold and demonstrated promising potential [16]. It contains low protein content in its structure, is one of the most important hydrocolloids with a high solubility in water, and solutions can be prepared up to concentrations of 50–55%. This property of GA stems from its highly branched and complex structure [17].
GA is water-soluble (except below pH 3.0), exhibits compatibility with solids, and demonstrates low viscosity in Newtonian fluid foods at below 40% concentrations [17]. Because of being water soluble, GA treated products have low washing stability which makes these products disposable. While insoluble in fats and many organic solvents, GA can dissolve in aqueous ethanol solutions. Additionally, it has limited solubility in glycerol, ethylene glycol, acetate esters, and acetate-alcohol mixtures [17]. GA has been widely utilized in encapsulating due to its numerous benefits, including its widespread availability, affordability, non-toxic nature, and encapsulation properties such as high efficiency, controlled release. Despite its advantages, the biodegradability of GA may vary based on processing conditions and cross-linking agents used. Combining GA with other polymers is suggested to enhance the mechanical properties of microcapsules [1]. Several studies have been conducted on GA utilization for different purposes. Recent studies such as those by Zaeim et al. [10] and Koh et al. [18] reported on the significance, optimization potential, and positive impact of GA on the stability and viability of microencapsulated probiotics.
Polyvinyl alcohol (PVA) stands as a significant polymer, holding pivotal importance within the biodegradable counterparts PVA, a synthetic polymer, is non-toxic and biodegradable, possessing superb compatibility and film-forming capabilities [19]. It is commonly employed as a stabilizing agent in the fabrication of nanoparticles, facilitating the production of small, homogeneous particles [20]. In a study, nanocapsules were synthesized using the emulsion diffusion technique, wherein PVA served as a stabilizer in conjunction with polylactic acid (PLA) in the external phase and plasmid DNA in the internal phase [19]. Ganti et al. [21] employed PVA as a cryoprotectant material during the manufacture of nanocapsules. Similarly, in the study conducted by Yadav et al. [22] nanocapsules were prepared via the salting-out method, with PVA utilized once again as a stabilizing agent.
Biodegradable polymers widely utilized in various applications, Irgasan is one of the potent agents known for its broad-spectrum effectiveness. It is a non-ionic, broad-spectrum antimicrobial agent known as Triclosan, demonstrates rapid and lasting antibacterial efficacy, and is extensively utilized across various personal care products such as toothpaste, deodorant, soaps, detergents, dish washing liquid, cosmetics [23, 24, 25]. Subsequently, Irgasan has been used for skincare applications and oral care products. Irgasan serves to inhibit bacterial growth on various plastic items used in households, bathroom accessories, flooring materials, and toys [24, 25]. Several studies have reported on Irgasan utilization for antibacterial applications such as coating plasma-modified polyethylene [26] and active antibacterial medical-grade polyvinyl chloride for medical purposes [23], using in drug delivery applications for increasing the efficiency [27].
The objective of this study was to produce GA/PVA-based nanocapsules using the coaxial electrospraying technique, with GA/PVA solution serving as the shell and Irgasan (triclosan) solution as the core. The investigation centered on analyzing the impact of process parameters such as flow rate, needle size, working distance, and voltage on the formation of nanocapsules. Additionally, the effects of solvent concentration of Irgasan core solution on nanocapsule formation were explored. The properties of the nanocapsules were assessed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM).
Irgasan (72,779 ≥ 97%), GA, and ethanol (CAS No:64-17-5) were all purchased from Sigma Aldrich.
25/75 v/v% GA/distilled water solutions were prepared at 50°C. Poly(vinyl alcohol) (PVA) solutions were prepared weight/volume concentration (wt/vol%) as 2 wt/vol% at 40–80°C. For electrospraying, 1:1 GA/PVA solution was prepared.
Irgasan solutions were prepared weight/volume concentration (wt/vol%) with ethanol solvent. Three different solvent concentration (25%, 50%, and 100% ethanol) were prepared using distilled water. Irgasan solution was prepared at 1 wt/vol% concentration.
2.2 Methods
GA/PVA solution is fed from the outer needle tip while Irgasan solution is fed from inner needle tip through dual syringe pumps via micro pumps (New Era NE-1000X). The coaxial needle tip is connected to the high DC voltage (Gamma High Voltage Series ES100P). The samples were collected on an aluminum foil covering the grounded plate. In each experiment, GA/PVA and Irgasan solutions at each mixing ratio were subjected to a 30-minute electrospraying process. Electrospraying parameters are presented in Table 1. Temperature and humidity were measured as 20–28°C and 20–25%, respectively.
Investigated material and process parameters (temp. 20–28°C, hum. 20–25%, time 30 min).
Increment.
The surface morphology of electrosprayed GA/PVA nanocapsules is examined using a scanning electron microscope (SEM) (JEOL JSM-6390). The SEM images were captured at magnifications ranging from 1000 to 10,000 at an acceleration voltage of 5–20 kV. Transmission electron microscope (TEM) (JEOL JEM 100C) was used for high-resolution imaging to determine nanocapsule formation. Nanocapsules produced by electrospraying were collected onto copper grids placed on the upper surface of the foil during application. Samples on these grids were characterized using TEM.
3.1 Effects of total flow rate on nanocapsulation formation
Flow rates of solutions frequently serve as critical parameters for regulating the formation of structures through the electrospray method [28]. Coaxial electrospraying was conducted at different total flow rates, including 5 μl min−1, 10 μl min−1, 20 μl min−1, and 40 μl min−1. Electrospraying process was conducted at fixed applied voltage and distance as presented in Table 1. The ratio of needle tip area of the core and the shell was calculated as 55/45%. This ratio was used to arrange the flow rates of the core and the shell. According to this arrangement, the flow rates of the core and the shell are given in Table 2.
Total flow rate
5 μl min−1
10 μl min−1
20 μl min−1
40 μl min−1
Core flow rate
2.75 μl min−1
5.5 μl min−1
11 μl min−1
22 μl min−1
Shell flow rate
2.25 μl min−1
4.5 μl min−1
9 μl min−1
18 μl min−1
Table 2.
Flow rate ratios of core and shell solutions.
The pictures of the samples are presented in Figure 1. Dripping was observed in all samples across all flow rates. Upon comparing the effects of flow rate, an increase in the flow rate of the shell solution corresponded to an increase in dripping. Particularly, at total flow rates of 20 and 40 μl min−1, dripping was much more intense.
Figure 1.
Images of samples.
SEM images were captured to observe the formation of nanocapsule (Figure 2). Electrospraying was observed at all flow rates. However, at flow rates of 5 μl min−1 and 10 μl min−1, film formation occurred, obscuring the nanocapsules underneath. At flow rates of 20 μl min−1 and 40 μl min−1, film formation also occurred, but the capsules were more clearly visible. A monodisperse distribution was observed at 20 μl min−1 and 40 μl min−1, indicating successful encapsulation on a nanoscale, with no fibril formation.
Figure 2.
SEM images of samples electrosprayed at different total flow rate.
Due to issues with dripping and film formation, the coaxial electrospraying setup was isolated, and the electrospraying process was repeated using the same total flow rates. In the isolated setup, in all samples (at all flow rates), dripping was observed. However, this dripping was less than previous samples.
Isolated environment provided electrospray with much less dripping. In the isolated setup, dripping was observed in all samples at all flow rates, though to a lesser extent compared to previous samples. The isolated environment resulted in significantly reduced dripping during the electrospray process (Figure 3).
Figure 3.
Images of samples in isolated environment.
SEM images confirmed the formation of nanospheres with a monodisperse distribution, and no fibril formation was observed, indicating successful encapsulation on a nanoscale (Figure 4). The quantity of nanocapsules increased with the rising flow rate, while the particle size enlarged between 5 and 10 μL min−1. Several studies reported that higher flow rates produced larger particles [29, 30, 31, 32]. Increased flow rates led to the ejection of more solution, leading to the formation of larger particles, whereas lower rates produced small, highly charged droplets, resulting in small particles through Coulomb fission [31]. At higher flow rates, the particle size remained similar. Based on the SEM analysis, a total flow rate of 20 μL min−1 was chosen considering the quantity and morphology of the nanocapsules.
Figure 4.
SEM images of samples electrosprayed at different total flow rate in isolated environment.
3.2 Effects of solvent concentration
The effects of solvent concentration on electrospray were investigated. 25/75% water/ethanol, 50/50 water/ethanol, and 100% ethanol solvents were used to solve Irgasan. Electrospraying was observed in all solvent concentration. SEM images were captured to ensure nanocapsule formation through electrospraying (Figure 5).
Figure 5.
SEM images of samples electrosprayed at different solvent concentration.
The nanocapsules displayed a spherical shape with uniform distribution and no fibril formation across all solvent concentrations. The solvent evaporation in electrospraying plays a key role for achieving particles that are monodispersed and uniform in size [33]. At 25/75% water/ethanol and 100% ethanol solvent concentrations, the size of nanocapsules was reduced; however, the number of nanocapsules was decreased too. Employing 100% ethanol solvent resulted in the presence of nanocapsules of various sizes. At 50/50% water/ethanol solvent, nanocapsules were slightly larger, yet displayed the most uniform distribution, with the highest number observed. Therefore, subsequent applications were conducted using a 50/50% water/ethanol solvent.
3.3 Effects of working distance
The effect of distance between the needle and the collector on electrospraying was investigated. Electrospraying was conducted at four different distances as 5 cm, 10 cm, 15 cm, and 20 cm to determine the optimum distance between the needle and the collector. 50/50% water/ethanol solvent was used. The total flow rate was set to 20 μl min−1. SEM images of electrosprayed surfaces were captured to ensure nanocapsule formation (Figure 6). Nanocapsules were in form of sphere and had monodisperse distribution without fibril formation. Encapsulation is achieved on a nanoscale.
Figure 6.
SEM images of samples electrosprayed at various distance.
SEM images in Figure 6 revealed that with increasing distance, the distribution of capsules became more uniform. At a distance of 5 cm, a wide size distribution was observed. At short distances, the solvent did not fully evaporate before reaching the collector, leading to an increase in particle size [34, 35]. The size has also decreased proportionally, but the capsules at a distance of 20 cm are so small that they cannot even be observed with SEM images properly. Also at 20 cm, the number of nanocapsules was reduced. Although increasing the distance allows for longer evaporation time and enhances cone-jet stability, it also results in a decrease in the electric field [29]. Determining the optimal distance is crucial for electrospraying. Figure 6 shows that nanocapsules formed at a distance of 15 cm exhibited uniform distribution and smaller diameter compared to those at 5 and 10 cm. This is because as the distance increases, drying occurs more effectively. Also at 15 cm, the number of nanocapsules was higher compared to those at 20 cm. Therefore, the distance of 15 cm was selected for optimum process parameter.
3.4 Effects of electric field
The effect of electric field on electrospray process was investigated. At this stage, electrospray was conducted at four different voltages as 5 kV, 10 kV, 15 kV, and 20 kV. Other process parameters were set as 20 μl min−1 total flow rate, 15 cm distance, 50/50% water/ethanol solvent. SEM images of electrosprayed surfaces were captured to ensure nanocapsule formation (Figure 7). Electrospraying was not achieved at all voltages. At 5 kV voltage, only dripping occurred. However, electrospraying was occurred at 10 kV, 15 kV, and 20 kV. Nanocapsules were in form of sphere and had monodisperse distribution without fibril formation. Encapsulation is achieved on a nanoscale.
Figure 7.
SEM images of samples electrosprayed at various voltage.
Voltage was known as a fundamental parameter for electrospraying process [33]. Lowering the voltage could result in a reduced electrical field, potentially leading to the formation of non-spherical droplets. The uniform shape was related to higher voltage [32, 33]. According to the SEM images, nanocapsules formed at a voltage of 10 kV were smallest in diameter. At higher voltage the diameter of nanocapsules was getting larger. At 20 kV voltage, the number of the nanocapsules was reduced significantly. Therefore, a voltage of 10 kV is selected as the optimum voltage.
3.5 Effects of flow rate
The effect of flow rate of shell and core solutions on electrospraying was investigated. Total flow rate was kept constant at 20 μl min−1. Coaxial electrospraying of GA/PVA as shell and 1% Irgasan solution as core was conducted at four different core/shell solution flow rate as 25/75% (5–15 μl min−1) core/shell, 50/50% (10–10 μl min−1) core/shell, 75/25% (15–5 μl min−1) core/shell, and 55/45% (11–9 μl min−1) core/shell.
SEM and TEM images of electrosprayed surfaces were captured to ensure nanocapsule formation (Figures 8 and 9).
Figure 8.
SEM images of samples electrosprayed at various flow rate.
Figure 9.
TEM images of samples electrosprayed at 5–15 and 11–9 μL min−1 core/shell ratio flow rate.
SEM images have shown that electrospraying was achieved with no fibrillation at all flow rate ratios (Figure 8). A distinctive core/shell structure was observed at all flow rates. The lower shell solution flow rate resulted in the failure of the shell material to cover the core material, whereas higher shell solution flow rates facilitated capsule formation [36]. Xie et al. studied on encapsulation of protein inside PLGA (poly(DL-lactide-co-glycolide)) microparticles by coaxial electrospray and found that when the flow rate of the shell solution was significantly higher than that of the core solution, the distribution of droplet diameters tended to be more uniform [32]. Yet, the most uniform distribution was achieved at the flow rate 11–9 μL min−1 core/shell ratio in this study. At 15–5 and 5–15 μL min−1 core/shell ratios, the size of the nanocapsules was seen smaller in diameter. However, TEM images of electrosprayed surfaces proved that at the 11–9 μL min−1 core/shell ratio, this flow rate gave the best morphology (Figure 9). Therefore, the optimum flow rate was determined as 11 μL min−1 for 1% Irgasan core and 9 μL min−1 for GA/PVA shell. In TEM images, the inner and outer phases of the formed capsules can be clearly observed (Figure 9).
3.6 Effects of needle size
The needle size may influence the electrospraying process, particle size and distribution [35]. The effect of needle size on electrospraying was investigated. Four different needle size combinations for core/shell construction were used for coaxial electrospraying. By this way, flow rate ratios of core/shell solutions were changed, and its effect on electrospraying and nanocapsule formation were investigated. 21, 24, and 26 G needle utilization implied a decrease in core flow rate.
SEM images of coaxial electrosprayed surfaces were captured to ensure nanocapsule formation (Figure 10). Electrospraying was achieved with all needle size combinations. Nanocapsules were in form of sphere with no fibril formation.
Figure 10.
SEM images of samples electrosprayed with various needle sizes.
Some studies found no significant relation between the needle size and particle size [37, 38]. Larger particles may be produced by utilizing larger needle due to higher flow rate [26]. The effect of the needle size was found more significant especially at lower flow rates [28]. At the constant flow rate, with 21–24 G and 21–26 G needle combinations, smaller core needle caused decrease in the size of the nanocapsules compared to that of 21–22 G needle combination. Also, the number of the nanocapsules was higher (Figure 10). 21–26 G needle combination resulted to form larger and less nanocapsules. TEM images of coaxial electrosprayed surfaces were captured to ensure nanocapsule formation (Figure 11). In TEM images, the inner and outer phases of the formed capsules can be clearly observed. With 22–26 G needle combination, the nanocapsules were formed at more uniform distribution.
Figure 11.
TEM images of samples electrosprayed with 21–26 G needle size combination.
This study investigated the formation of nanocapsules through the coaxial electrospraying method employing GA/PVA solutions for the shell and Irgasan solution for the core. The effects of ethanol solvent concentration, flow rate and total flow rate, needle size, working distance, and electric field were analyzed to see compatibility these parameters on the electrospraying process. Following the electrospraying process, SEM and TEM images were utilized to discuss the size, morphology, and distribution of produced particles. Our findings revealed that the solvent concentration influenced the nanocapsule size and the distribution. At 50/50% water/ethanol solvent, nanocapsules were displayed the most uniform distribution, with the highest number observed. Furthermore, working distance and electric field play crucial roles in determining nanocapsule size and morphology. The electrostatic field affected the balance between coulombic forces and flight time, resulting in smaller particles at higher values up to a threshold point. Our findings also indicate that electrospraying distance has similar working mechanism and optimum working distance was found as 15 cm. The other significant outcome of our study was lower flow rate of the shell solution led to inadequate coverage of the core material by the shell material. As a result of this study, desired nanocapsules comprising GA/PVA shell and Irgasan core were achieved. Optimum electrospraying parameters and concentration rates were found to be key for achieving a well-formed shell-core structure from GA and Irgasan. These findings suggest that the electrospraying process of the GA/PVA-Irgasan nanocapsules can be a valuable reference for future encapsulation applications.
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Written By
Mehmet Dasdemir, Serap Gamze Serdar, Hatice Ibili and Bilgen Çeliktürk Kapar
Submitted: 12 April 2024Reviewed: 23 April 2024Published: 01 July 2024
Open access peer-reviewed chapter - ONLINE FIRST
