Home Effects of chitosan and Tween 80 addition on the properties of nanofiber mat through the electrospinning
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Effects of chitosan and Tween 80 addition on the properties of nanofiber mat through the electrospinning

  • Chalongwut Boonpratum , Patcharin Naemchanthara , Pichet Limsuwan and Kittisakchai Naemchanthara EMAIL logo
Published/Copyright: February 25, 2022
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e-Polymers
From the journal e-Polymers Volume 22 Issue 1

Abstract

Chitosan (CS) with excellent biomedical properties was mixed with polyvinyl alcohol (PVA) to be used as the spinning solution. The spinning solutions with various concentrations of CS:PVA from 10:90% to 50:50% (v/v) were investigated. Tween 80 (T80) was added in the spinning solutions of CS and PVA. The nanofiber mats with and without T80 addition obtained from the spinning solutions by electrospinning technique were investigated and addressed. The results showed that the viscosity of the CS and PVA spinning solutions increased with increasing the CS concentration, whereas the viscosity decreased after T80 addition. The nanofiber mats with 10–30% CS concentrations were prepared successfully as a smooth surface and high dense nanofiber mat. The average diameter of the nanofiber decreased with increasing the CS concentration. The increase in the CS concentration of the nanofiber mat can increase the mechanical and antibacterial properties, whereas the wettability and drug release property were decreased. Moreover, the nanofiber mats with T80 addition had higher mechanical property and wettability than the nanofiber mats without T80 addition. Finally, the T80 addition can enhance hydrophilicity and promote the drug release property of the nanofiber mat.

Graphical abstract

Keywords: nanofiber; chitosan; Tween 80; antibacterial activity; drug release

1 Introduction

Nowadays, nanofiber is one of the nanomaterials, which has a high specific surface area and porosity that is widely used in various applications such as sensing (1,2), filtration (3,4,5), and biomedicine (6,7). The nanofiber material has a high surface area used as an accelerator for wound healing in medical treatment (8). Moreover, the nanofiber material with specific properties is additional functionalized nanofiber and broadens the number of biomedical applications. The specific properties include wound healing, infection controlling after surgery, exudate absorption, and antibacterial property. These specific properties not only depend on the type of raw materials but also can be obtained from the specific process as an electrospinning technique (9,10,11,12). Polyvinyl alcohol (PVA), a synthetic polymer, is an outstanding material to produce the nanofiber by electrospinning technique. The PVA can be easily spun to the continuous nanofiber and the nanofiber mat without droplets formation during the electrospinning process. In addition, the PVA can be prepared as solution by dissolving in deionized water for the spinning process. Moreover, the PVA has a high water content along with high elasticity that can provide cell adhesion and its tensile strength, which is similar to the human articular cartilage. Therefore, the PVA is the appropriate material to produce the nanofiber mat for biomedical applications. Although the PVA has some good properties including the biocompatibility and biodegradability (13,14), it also lacks bioactivity for wound healing and tissue growth inducement (15). Nevertheless, chitosan (CS) as a natural polymer has the bioactive property that can induce tissue growth. The biodegradability, nontoxicity, and antibacterial activity are also excellent properties of the CS (16,17,18). Furthermore, the CS has hyaluronic acid inducement as skin substitutes that can aid the wound healing rapidly (19,20,21). However, in the electrospinning process, the CS solution with high viscosity can induce the droplet formation on the nanofiber mat. The droplet formation relates to the strong hydrogen bonding, preventing the CS polymeric chains movement, and the repulsive force formation in the CS backbone that obstruct the continuous fiber forming during electrospinning (22). The combination of these outstanding properties to produce the CS and PVA material includes the bioactive, biocompatible, and biodegradable properties. The CS and PVA material with the excellent properties could accelerate wound healing and reduce the treatment time after surgery of patients. This leads to the reduction of the treatment duration and frequency to see the doctor at a hospital. Especially during the COVID-19 pandemic situation, this also encourages the increase in social distancing and decreases the infection of patients. However, the production of the nanofiber with nanosize and continuous fiber from the CS and PVA material by electrospinning is also difficult and challenging for researchers. Moreover, the addition of a surfactant in the spinning solution could be an alternative way to enhance the possibility of continuous nanofiber production. Tween 80 (T80), polyoxyethylene sorbitan monooleate, is one of the nonionic surfactants used in the food and pharmaceutical industries. The T80 has advantages including reasonable cost, biodegradability, nontoxicity, and friendly with the environment (23,24). Thus, T80 is selected as the surfactant to produce the continuous nanofiber from the CS and PVA.

In this study, the CS and PVA to be used as the spinning solutions were prepared and characterized. The nanofiber mats were prepared from the CS and PVA spinning solutions by electrospinning technique. The T80 was chosen and added to the CS and PVA spinning solutions and the nanofiber mats. The effect of T80 addition in spinning solutions and the nanofiber mats was observed and compared with another nanofiber mat. The morphology and characteristic of the nanofiber mats were investigated and compared. The mechanical properties and wettability of the nanofiber mats with and without T80 addition were reported. In addition, the essential properties for biomedical application such as antibacterial activity and drug release behavior of the nanofiber mats with and without T80 addition were evaluated and addressed.

2 Materials and methods

2.1 Preparation of the spinning solution and nanofiber mat

The PVA solution was prepared by dissolving 10 g of PVA powder (molecular weight, 80–90 kDa; degree of hydrolysis, 86.6–89.0 mol%; Union Chemical 1986 Co., Ltd, Thailand) in 100 mL of distilled water. The CS solution was prepared by dissolving 5 g of CS powder (degree of deacetylation >90%; molecular weight, 500–700 kDa; Burnwachr Bio-Lin Co., Ltd, Thailand) in 100 mL of 2% acetic acid solution (purity >95%, Union Chemical 1986 Co., Ltd, Thailand). The spinning solution had two solution sample groups including the spinning solutions with and without T80 addition. The CS and PVA solutions were mixed at the range of 10–50% (v/v) CS solution without T80 addition. The obtained samples were denoted as CS10, CS20, CS30, CS40, and CS50. Similarly, the mixed solution of CS and PVA were added with 5% (v/v) of T80 (density of 1.072 g·mL−1 and viscosity of 315 mPa·s at 30°C, Hong Huat Co., Ltd, Thailand). The samples were denoted as CST10, CST20, CST30, CST40, and CST50. The conductivity of all spinning solutions was measured by a conductivity meter (WTW inoLab Cond 720, Germany) at a temperature of 25°C, and the conductivity values are shown in Table 1. The rheological properties of all spinning solutions were analyzed by a rheometer (Physica MCR-150, Germany) with a cone plate diameter of 50 mm and a parallel plates gap of 0.05 mm. The shear stress versus shear rate was recorded from 0.01 to 100 s−1 and fitted by the power law model to obtain the apparent viscosity of the spinning solution according to Eq. 1.

(1) η = k γ ̇ n − 1

where η is the apparent viscosity (Pa·s), k is the consistency index (Pa·s), γ ̇ is the shear rate (s−1), and n is the flow behavior index.

Table 1

Conditions and conductivity of all samples

Sample Conditions of sample (% (v/v)) Conductivity (µS·cm−1)
CS PVA T80
CS10 10 90 No 24.90
CS20 20 80 No 33.70
CS30 30 70 No 46.20
CS40 40 60 No 57.50
CS50 50 50 No 68.60
CST10 10 90 Yes 22.40
CST20 20 80 Yes 20.20
CST30 30 70 Yes 41.10
CST40 40 60 Yes 49.40
CST50 50 50 Yes 60.60

For the nanofiber mat preparation, the spinning solution was spun by the horizontal electrospinning technique, which included a syringe equipped with a metal needle (diameter = 0.8 mm), a high voltage power supply, and a square aluminum collector (10 cm × 10 cm). The spinning solution was contained in a syringe and spun under parameters as follows: the high voltage was 15 kV, the flow rate was 1 mL‧h−1, the tip-to-collector distance was 15 cm, the temperature was 25 ± 2°C, and the relative humidity was 45 ± 5%. The nanofiber mat was collected on the collector after spinning for 90 min. The details of all samples in various conditions are summarized in Table 1.

2.2 Characterization and tensile testing of the nanofiber mat

The functional groups of the nanofiber mats were investigated to confirm the chemical compositions by Fourier-transform infrared spectrometer (FTIR, Perkin Elmer spectrum two, USA). The FTIR was carried out in the range of 4,000–400 cm−1 at a resolution of 4 cm−1 with 16 scans in the transmittance mode. Then, the surface and cross-sectional morphology of the nanofiber mats were monitored by a digital camera (Sony ILCE-6400, Japan) and a field emission scanning electron microscope (FESEM, FEI Quanta 450, USA). The average diameter of the nanofibers was determined from FESEM image using the ImageJ program. The roughness property of the nanofiber mats was analyzed by an atomic force microscope (AFM, Park NX10, South Korea) with a scan size of 10 µm × 10 µm and calculated using the Park Systems XEI program. The mechanical properties of the nanofiber mats were tested by a texture analyzer (TA.XT Plus Stable Micro System, UK) based on the ASTM D882 standard. The wettability of the nanofiber mats was investigated using a contact angle analyzer (KINO SL 150E, USA).

2.3 Antibacterial and drug release studies of the nanofiber mat

For antibacterial study, the antibacterial activity against the Gram-positive bacteria Staphylococcus aureus (ATCC 25923, Department of Microbiology, Faculty of Science, King Mongkut’s University of Technology Thonburi, Thailand) of the nanofiber mats with and without T80 addition was evaluated. The nanofiber mats were cut into a circular shape with a diameter of 10 mm and placed onto nutrient agar plates that contained bacterial suspensions of 0.1 mL with a density of 1 × 106 CFU·mL−1. All plates were incubated in the incubator at 37°C for 24 h to record the inhibition zone. Afterward, the antibacterial activity was measured in the inhibition zone by a digital Vernier caliper (Mitutoyo Absolute Digimatic, Japan). For the drug release study, the nanofiber mats with and without T80 addition were soaked in 10% (w/v) povidone iodine solution (PI, Mundipharma, Co., Ltd, Thailand) for 15 min and dried at room temperature for 3 h. Then, the nanofiber mats contained PI were immersed in 100 mL of the phosphate buffered saline solution (PBS, pH 7.4, Merck, Co., Germany). The PI release study was maintained at an approximately temperature of 37°C throughout the experiment. The 5 mL of PI release was withdrawn and replaced with the same volume of fresh PBS solution at 2, 4, 6, 8, 10, 15, 20, 30, 40, 50, 60, and 90 min. Next, the collected PI release with various release times were analyzed, and the absorbance value of PI peak at 292 nm was measured by a UV-visible spectrophotometer (BioMate 160, USA). The cumulative PI release percentage was calculated from the absorbance value using the calibration curve. Furthermore, the nanofiber mats weight were measured before and after the PI release study for determining the initial PI loaded, the cumulative PI release, and the PI remaining on the nanofiber mats.

3 Results and discussion

3.1 Rheological properties of the spinning solution

To produce the nanofiber by electrospinning, the spinning solution viscosity is the key factor in the solution spinnability and morphology of the as-received nanofiber. The viscosity of the spinning solution depends on various parameters such as type, concentration, shear rate, and others. Thus, the investigation of the spinning solution viscosity is significant in nanofiber production. The apparent viscosity of the spinning solutions in various conditions as a function of the shear rate is shown in Figure 1. The PVA solution had the lowest viscosity, whereas the CS solution had the highest viscosity (Figure 1a). Because the PVA has low molecular weight than the CS. However, this means that the PVA has a low number of entanglement chains in the spinning solution. Then, the CS solution was added to the PVA solution from 10% to 50% (v/v) of CS (see solid lines of CS10, CS20, CS30, CS40, and CS50 samples in Figure 1b). The results showed that the CS10 solution had the lowest viscosity, whereas the CS50 solution had the highest viscosity. The apparent viscosity of the spinning solutions increased with increasing the CS concentration. This apparent viscosity increase can be explained by the increase of molecular weight resulting in the more entanglement chains in the PVA and CS spinning solution. The CS effect on the improvement of the hydrogen bonding between the CS and PVA solutions after the CS was added to the spinning solution. The improvement of hydrogen bonding results from the increase of the intrachain hydrophobic bonds in CS. Moreover, the intermolecular interactions between the CS and PVA molecules in the spinning solution are also improved through a hydrogen bond. From the results, it can be implied that the CS50 solution has higher entanglement chains and intrachain hydrophobic bonds as compared with other spinning solutions. However, the apparent viscosity versus the shear rate curves of the PVA solution are shown in Figure 1a. The lowest apparent viscosity was observed from the PVA solution. The trend line slightly decreased and became stable at a shear rate of approximately 7 s−1 until reaching the final shear rate. In typical PVA solution, the shear-thinning trend to be the exponential line. In this case, the PVA solution has a low concentration (10% (w/v)); hence, its behavior shows slightly the exponential trend line. After CS addition, the relationship between the apparent viscosity and shear rate increased and clearly showed the exponential trend line. The spinning solution showed a higher viscosity at a low shear rate, then it decreased with increasing shear rate. This phenomenon is well known as shear-thinning behavior and can be described that the coiled polymer chain at a low shear rate has high resistance against flow resulting in high viscosity. When the shear rate was increased, the aggregation of the coiled polymer was broken and uncoiled aligning with the direction of the external shear force that generated from the cone plate during testing and showing the lower viscosity. After T80 addition, the effect of T80 addition is shown in Figure 1b (dashed lines). The relationship between the apparent viscosity and shear rate of the CST10, CST20, CST30, CST40, and CST50 solutions still showed similarly exponential trend line, but it decreased as compared with the spinning solution without T80 addition, respectively. This is due to the relaxation of entanglement between the CS and PVA polymer chains in the spinning solution. The T80 as a surfactant dispersed in the form of single-molecule or micelle, interrupting the hydrogen bond interaction between the CS and PVA polymers. The T80 molecule has a head with hydrophilic property and a tail with hydrophobic property. When the molecules of T80 move randomly in the spinning solution, the hydrophobic tail convolves and covers the CS and PVA molecular chains resulting in the decreasing viscosity. Furthermore, the rheological behavior of the spinning solutions was fitted by the power law model in Eq. 1, and the relative parameters are shown in Table 2. The consistency index (k) and the flow behavior index (n) of the spinning solutions were well fitted by the power law model (R 2 > 0.99). The lowest k value was observed in the PVA solution, whereas the highest value was observed in the CS solution. Similarly, the k values of CS10, CS20, CS30, CS40, and CS50 solutions increased with increasing the CS concentration. It means that the k value depends on the viscosity of non-Newtonian fluids. The n value of the PVA solution was 0.95 that represents a shear-thinning behavior slightly, whereas that of the CS solution was 0.51 that represents a shear-thinning behavior strongly (25). The n values of CS10, CS20, CS30, CS40, and CS50 solutions decreased with increasing the CS concentration, which means that the n value significantly depends on the concentration of the CS. After T80 addition, the k values of CST10, CST20, CST30, CST40, and CST50 solutions decreased as compared with those of CS10, CS20, CS30, CS40, and CS50 solutions, respectively. This clearly showed that the effect of T80 addition on the k value decrease relates to the viscosity of the spinning solutions. Moreover, the increase of T80 also affected the n value due to the decrease of the shear-thinning behavior degree.

Figure 1 Relationship between apparent viscosity and shear rate of: (a) CS and PVA solutions and (b) spinning solutions in various conditions with and without T80 addition.
Figure 1

Relationship between apparent viscosity and shear rate of: (a) CS and PVA solutions and (b) spinning solutions in various conditions with and without T80 addition.

Table 2

Rheological parameters from the power law model of all samples in various conditions with and without T80 addition

Sample k (Pa·s) n R 2
PVA 1.10 0.95 ± 0.004 0.997
CS 45.02 0.51 ± 0.005 0.994
CS10 2.79 0.78 ± 0.002 0.999
CS20 5.32 0.75 ± 0.010 0.994
CS30 7.70 0.72 ± 0.007 0.997
CS40 9.71 0.69 ± 0.002 0.998
CS50 16.81 0.65 ± 0.006 0.997
CST10 1.98 0.80 ± 0.010 0.995
CST20 3.83 0.76 ± 0.004 0.992
CST30 5.73 0.74 ± 0.001 0.999
CST40 7.98 0.71 ± 0.002 0.999
CST50 13.17 0.68 ± 0.003 0.999

3.2 Chemical functional group of the nanofiber mat

The FTIR spectra of the PVA nanofiber mat, CS powder, T80 powder, and the CS and PVA nanofiber mats in various conditions with and without T80 addition are shown in Figure 2. The spectra of PVA nanofiber mat showed seven transmission peaks that consist of the broad peaks at 3,364–3,242 cm−1 assigned to O–H stretching vibration, weak peak at 2,939 cm−1 assigned to C–H stretching vibration, a strong peak at 1,640 cm−1 assigned to C═O stretching vibration and four small peaks at 1,430 cm−1 attributed to C–O–H bending vibration, 1,378 cm−1 attributed to H–C–H bending vibration and 1,269, 1,090, and 1,028 cm−1 attributed to C–O stretching vibration (13,26–28). The appearance of the C═O stretching vibration is the acetate group. This is due to the PVA production of raw PVA powder that showed the acetate group remaining. Although the CS powder showed that the characteristic peaks are similar to that of PVA solution, a special peak at 1,550 cm−1 was found in the CS solution, which is attributed to N–H bending vibration (amide II) of the amino group in the organic compound (29). The spectra of T80 powder showed four functional groups of the C–H, C═O, C–O, and C–C. The C–H functional group had three vibrations consisting of the peaks at 2,925, 2,869, and 950 cm−1 assigned to C–H stretching vibration, 1,460 and 1,348 cm−1 assigned to C–H scissoring vibration, and 720 cm−1 assigned to C–H rocking vibration. The C═O functional group of the peak 1,734 cm−1 was assigned to C═O stretching vibration. The C–O functional group had four vibrations consisting of the peaks at 1,300, 1,240, 1,090, and 1,028 cm−1 assigned to C–O stretching vibration. The C–C functional group at a peak of 850 cm−1 was assigned to C–C stretching vibration (23,30). After electrospinning, the FTIR was used to confirm the chemical functional groups of the nanofiber mats. The spectra of the CS10 nanofiber mat (solid lines) showed the characteristic peaks of the CS and PVA. However, the peak at 1,550 cm−1 according to N–H bending vibration of the CS10 nanofiber mat was observed unclear due to its low CS concentration and shading effect from the strong peak at 1,640 cm−1 of C═O stretching vibration. The spectra of the CS20, CS30, CS40, and CS50 nanofiber mats also showed the characteristic peaks of CS and PVA. Considering the peak at 1,550 cm−1, this peak was clearly observed when the CS concentration in the nanofiber mat was increased. After T80 addition (dashed lines), the spectra peak of the CST10, CST20, CST30, CST40, and CST50 nanofiber mats showed some peaks that are similar to that of nanofiber mats without T80. However, the T80 characteristic peaks at 2,925 and 1,090 cm−1 assigned to C–H stretching and C–O stretching vibration were found in the nanofiber mats with T80 addition.

Figure 2 FTIR spectra of the PVA nanofiber mat, CS powder, T80 powder, and the nanofiber mats prepared in various conditions with (dashed lines) and without (solid lines) T80 addition.
Figure 2

FTIR spectra of the PVA nanofiber mat, CS powder, T80 powder, and the nanofiber mats prepared in various conditions with (dashed lines) and without (solid lines) T80 addition.

3.3 Morphology and roughness of the nanofiber mat

The nanofiber mats of various conditions with and without T80 addition are shown in Figure 3. The CS10, CS20, and CS30 nanofiber mats showed a smooth surface and high dense fiber. The CS40 nanofiber mat showed dense fiber at the center of mat enclosed by slight fibers and small size of bubbles, whereas the CS50 showed high agglomeration of droplet dispersing over the surface of the nanofiber mat because the high viscosity of the spinning solution led to the formation of the droplets at the tip of syringe and the jet to collector. Then, the droplets dried and became bubble appearing on the nanofiber mat. After T80 addition, the CST10, CST20, and CST30 nanofiber mats also showed a smooth surface and high dense fiber. The CST40 nanofiber mat clearly showed a smooth surface and low dense fiber, whereas the CST50 nanofiber mat showed a high agglomeration of droplets. Considering the effect of T80 addition, the CST10, CST20, and CST30 nanofiber mats are not significantly affected by the nanofiber spinning process. The effect of T80 addition can be clearly observed in the CST40 nanofiber mat. The CST40 has a higher dense fiber than that of the CS40 nanofiber mat. However, the CST50 has more droplets that spread orientation randomly on the nanofiber mat as compared with the CS50 nanofiber mat. It means that the effect of T80 addition strongly depends on the initial viscosity of the spinning solution. Nevertheless, the T80 addition in the CST40 and CST50 of the spinning solution cannot reduce enough viscosity to produce the suitable nanofiber mat (Figures 1 and 3 and Table 2). Moreover, the damaged nanofiber mats of CS40, CS50, CST40, and CST50 cannot be collected and removed from an aluminum collector. Thus, the nanofiber mats spinning from CS concentration in the range of 10–30% (v/v) with and without T80 addition were used for characterization on the morphology, mechanical property, wettability, antibacterial activity, and drug release property investigation to apply in biomedical applications.

Figure 3 Photographs of the nanofiber mats prepared in various conditions with and without T80 addition.
Figure 3

Photographs of the nanofiber mats prepared in various conditions with and without T80 addition.

The surface morphology of nanofiber mats was investigated by using FESEM, and the fiber diameter and the size distribution were measured by ImageJ program, and the results are shown in Figure 4a. The CS10 nanofiber mat showed that the nanofiber had good uniformity, continuous fiber, and a circular cross-sectional structure. Similarly, the CS20 and CS30 nanofiber mats also showed the obtained nanofiber with continuous fiber and the same structure, but the size and uniformity of the nanofiber were decreased. Considering the fiber diameter, the average diameter of the CS10, CS20, and CS30 nanofiber mats were 306 ± 35, 180 ± 51, and 160 ± 84 nm, respectively. This result showed that the average diameter decreased with increasing the CS concentration. It means that the increasing CS concentration as a cationic polymer in the spinning solution leads to a higher charge density on the surface of ejected nanofiber. The overall tension in the nanofiber forming depends on the self-repulsion of the excess charges on the spinning solution surface under the electrical field. When the charge density increases, the diameter of ejected nanofiber becomes smaller. This phenomenon was confirmed with the conductivity of the spinning solutions as shown in Table 1. After T80 addition, the CST10 nanofiber mat showed the continuous nanofiber with a circular cross-sectional structure and higher diameter than that of the CS10 nanofiber. Similarly, the CST20 and CST30 nanofiber mats also showed continuous nanofiber with good uniformity and a circular cross-sectional structure. The average diameter of CST10, CST20, and CST30 nanofibers were 350 ± 74, 181 ± 29, and 178 ± 50 nm, respectively. The increasing average diameter of the nanofiber results from the T80 molecules in the spinning solution. Normally, the T80 was blended homogeneously in the CS and PVA spinning solution. The comolecules of the CS and PVA were convolved and covered by the hydrophobic tail of the T80 molecule (31). This affects the decrease in the viscosity of the CS and PVA spinning solutions. Meanwhile, the T80 addition also affects the decrease in the conductivity in terms of the excess charges and charge density of the CS and PVA spinning solutions (Table 1). It can be concluded that all the CST samples have a higher diameter than those of CS samples (without T80 addition). In addition, the uniformity of the nanofiber mats with and without T80 addition was investigated through the thickness value and the cross-sectional images, as shown in Figure 4b. The result showed that the thickness of the CS10, CS20, and CS30 nanofiber mats decreased with increasing the CS concentration because the average diameter decreased (see at the top of Figure 4b). Meanwhile, the thickness of the CST10, CST20, and CST30 nanofiber mats also decreased. It means that the T80 addition is not significantly affected the nanofiber mat thickness. Additionally, the cross-sectional image showed the high number of nanofibers at high CS concentration as compared with a low CS concentration of the nanofiber mat (see at the bottom of Figure 4b). These results confirmed that the T80 addition can increase the uniformity of the nanofiber mat with the increasing number of nanofiber and decreasing the size distribution of nanofiber (Figure 4). Furthermore, the topology of the nanofiber mats was observed by AFM in noncontact mode, as shown in Figure 5. The average diameter of the nanofiber tended to decrease with increasing the CS concentration. The uniformity of the nanofiber mats increased after T80 addition that relates to the decrease of root mean square (RMS) roughness as shown in Table 3. It means that the topology results correlate well with FESEM images.

Figure 4 FESEM images of: (a) surface morphology and (b) thickness (top) and cross-sectional morphology (bottom) of the nanofiber mats with and without T80 addition.
Figure 4

FESEM images of: (a) surface morphology and (b) thickness (top) and cross-sectional morphology (bottom) of the nanofiber mats with and without T80 addition.

Figure 5 AFM images of the nanofiber mats with and without T80 addition.
Figure 5

AFM images of the nanofiber mats with and without T80 addition.

Table 3

RMS roughness and mechanical properties of the nanofiber mats with and without T80 addition

Sample RMS roughness (µm) Elastic modulus (MPa) Tensile strength (MPa) Strain at break (%)
CS10 0.539 14 2 66
CS20 0.365 27 4 54
CS30 0.295 54 6 38
CST10 0.561 24 3 77
CST20 0.319 54 5 60
CST30 0.180 87 6 44

3.4 Mechanical properties of the nanofiber mat

The tensile test was carried out to evaluate the effect of the CS and T80 addition on the nanofiber mat properties. The mechanical properties such as elastic modulus, tensile strength, and strain at break of the nanofiber mats with and without T80 addition are shown in Table 3 and Figure 6. The elastic modulus and tensile strength of the nanofiber mats increased with increasing the CS concentration, but the strain at break decreased because the PVA has low molecular weight with high elasticity, whereas the CS has high molecular weight with a low elasticity. Therefore, the CS polymer shows more entanglement itself and high mechanical properties. When the CS was added to PVA, these nanofiber mats have been improved on the elastic modulus and tensile strength but lost the elasticity and the strain at break percentage. This improvement results from the intermolecular hydrogen bonds between hydroxyl and amino groups originated from CS and hydroxyl groups originated from PVA. In addition, the increase in the CS concentration leads to the decrease in nanofiber diameter, so the mechanical properties of the nanofiber mat with a small size nanofiber are also improved. Similarly, the elastic modulus and the tensile strength of the CST10, CST20, and CST30 nanofiber mats increased with increasing the CS concentration, whereas the strain at break decreased. After T80 addition, the mechanical properties: the elastic modulus, the tensile strength, and the strain at break were improved. As the T80 serves as a bridge combining different polymer phases and improving the miscibility of the blend polymer in the nanofiber mat (32,33).

Figure 6 Stress–strain curves of the nanofiber mats with and without T80 addition.
Figure 6

Stress–strain curves of the nanofiber mats with and without T80 addition.

3.5 Wettability of the nanofiber mat

Wettability is an important characteristic property of material for biomedical applications. The wettability of the nanofiber mats with and without T80 addition was monitored by the water contact angle, as shown in Figure 7. The water contact angle of the CS10, CS20, and CS30 nanofiber mats were 64 ± 2°, 69 ± 2°, and 75 ± 2°, respectively. The result showed that the water contact angle increased with increasing the CS concentration. This is due to the structure of the CS molecule with both cationic amino-groups and hydrophobic acetyl groups in the nanofiber mat that increase the hydrophobic behavior leading to the increase of contact angle (34). After T80 addition, the water contact angle of the CST10, CST20, and CST30 nanofiber mats were 25 ± 1°, 28 ± 2°, and 34 ± 1°, respectively. The result showed that the water contact angle also increased with increasing the CS concentration, but its water contact angle dramatically decreased as compared with the nanofiber mats without T80 addition. Because of the increase of hydrophilicity, the interaction between the water droplets and the surface of nanofiber mat is increased. The common backbone structure of T80 is a sorbitan ring with three ethylene oxide polymers attached to three different hydroxyl positions and an ethylene oxide attached to the fatty acid moieties through an ester linkage that is the tail with hydrophobicity, whereas the multiheaded structure of ethylene oxide is the hydrophilicity. When the hydrophobic tail of the T80 molecule convolved and covered, the comolecules of the CS and PVA resulting in the hydrophilic head of T80 molecule is on the outside of the nanofiber surface. The hydroxyl group attracted with the hydrophilic heads can easily interact with the water molecule of the water droplet through the hydrogen bond (24,35,36). Thus, the T80 addition as a surfactant clearly affects the hydrophilic property improvement of the nanofiber mat.

Figure 7 Water contact angles of the nanofiber mats with and without T80 addition.
Figure 7

Water contact angles of the nanofiber mats with and without T80 addition.

3.6 Antibacterial study of the nanofiber mat

The antibacterial activity of the nanofiber mats with and without T80 addition was investigated by the disc diffusion method against the S. aureus, as shown in Figure 8. The average diameter of inhibition zone of the CS10, CS20, and CS30 nanofiber mats were 13.90 ± 1.05, 18.55 ± 2.62, and 22.82 ± 2.83 mm, respectively. The increase of the inhibition zone showed the antibacterial activity of the CS. This result showed that the inhibition zone increased with increasing the CS concentration. This can be explained based on the electrostatic interaction. The electrostatic force occurs between the positive charges from amino groups of CS and the negative charges on the microbial surface of the S. aureus. This electrostatic force promotes the change in the permeability of the cell wall that provokes the internal osmotic imbalance. This electrostatic force causes the hydrolysis of the peptidoglycans in the cell wall and leads to the leakage of the intracellular electrolytes such as K+ and the low molecular weight proteinaceous constituents like proteins, nucleic acids, glucose, and lactate dehydrogenase. This electrostatic interaction results in the microorganism growth inhibition and death. Moreover, the CS network structure can form a thin film and cover the cell wall of bacteria. The CS thin film can block the transportation of essential solutes into the cell leading to the microorganism death (37). This antibacterial effect was clearly shown with the increasing CS concentration of the nanofiber mat. After T80 addition, the average diameter of inhibition zone of CST10, CST20, and CST30 nanofiber mats were 14.17 ± 1.66, 19.97 ± 1.86, and 24.33 ± 0.71 mm, respectively. Similarly, the inhibition zone of the nanofiber mats with T80 addition also increased with increasing the CS concentration. However, the inhibition zone of nanofiber mats with T80 addition slightly increased as compared with the nanofiber mats without T80 addition. It means that the T80 addition has no significant effect on the antibacterial property of the nanofiber mat.

Figure 8 Photographs of inhibition zone against S. aureus of the nanofiber mats with and without T80 addition.
Figure 8

Photographs of inhibition zone against S. aureus of the nanofiber mats with and without T80 addition.

3.7 Drug (PI) release study of the nanofiber mat

The nanofiber mats with and without T80 addition were evaluated on the PI release property. The PI release behavior of the nanofiber mats in PBS solution with a total release time of 90 min is shown in Figure 9a. The cumulative PI release percentage was calculated from the absorbance value using the calibration curve. The PI release behavior of the CS10, CS20, and CS30 showed that 70% of PI loaded nanofiber mats were rapidly released within 15 min and then gradually released until the end of the release time. The PI release behavior of the nanofiber mat has two regions consisting of the region I as a rapid release and the region II as a gradual release. At the region I, the absorbed PI molecules on the nanofiber mat surface rapidly diffuse into the PBS solution that is the dissolution-controlled mechanism. At the region II, the remaining PI molecules in nanofiber matrix are gradually diffused into the PBS solution that is the diffusion-controlled mechanism (38,39). However, the PI release behavior decreased with increasing the CS concentration because of the enhancement of hydrophobicity. In the same way, the hydrophilicity of the nanofiber mat was increased from PVA molecule that promotes the penetration of the aqueous medium to the nanofiber matrix leading to the PI release improvement (28). Nevertheless, the PI release behavior in the region II showed a decrease in the cumulative PI release percentage due to the PI degradation. Because the PI solution (yellowish-brown in color) contains I− (iodide ions), I3 − (triiodide ions), and I5 − (pentaiodide ions), these ions can interact with any other active ions via an oxidation reaction. In this case, many active ions in PBS solution as Na+, K+, and H+ can interact with iodine ions. This oxidation reaction leads to iodine eliminating (light yellowish-brown in color) correlating with the decreasing of cumulative PI release percentage. After T80 addition, the PI release behavior of the CST10, CST20, and CST30 showed that 57% of PI loaded nanofiber mats were rapidly released within 8 min (region I) and then gradually released until the end of release time (region II). Similarly, the PI release behavior of the nanofiber mats with T80 addition decreased with increasing the CS concentration. However, the result clearly showed that T80 addition can enhance the drug release property of the nanofiber mat. To clarify, the PI release percentage of the nanofiber mats with and without T80 addition was fitted by the Korsmeyer–Peppas model as given by Eq. 2 (40):

(2) M t M ∞ × 100 = K t m

Figure 9 (a) Cumulative PI release profile and (b) release rate of the nanofiber mats with and without T80 addition.
Figure 9

(a) Cumulative PI release profile and (b) release rate of the nanofiber mats with and without T80 addition.

The parameters of release kinetics were obtained from the log–log plot of cumulative PI release percentage M t M ∞ × 100 and release time (t). The fraction of M t M ∞ was determined from the cumulative amount of PI release at any time t divided by the cumulative amount of PI release at the end time of the measurement. The obtained slope of this plot is equal to the release exponent (m) that demonstrates the PI release mechanism of the nanofiber mat as Fickian diffusion (m ≤ 0.5). The release rate (K) can be calculated from the vertical-axis intercept of the plot that shows the PI release ability of the nanofiber mat, as shown in Figure 9b. All parameters of PI release kinetics are summarized in Table 4. The result showed that the PI release behavior of the nanofiber mats with and without T80 addition was well fitted by the Korsmeyer–Peppas model (R 2 > 0.99). The K values of the nanofiber mats with and without T80 addition decreased with increasing the CS concentration because the hydrophilic property was decreased. Moreover, the K values of the nanofiber mats with T80 addition increased approximately two times as compared with the nanofiber mats without T80 addition because the hydrophilic property of the nanofiber mat was improved (Figure 9 and Table 4).

Table 4

Drug (PI) release parameters of the nanofiber mats with and without T80 addition obtained from the Korsmeyer–Peppas model

Sample K m R 2
CS10 18.51 0.44 0.995
CS20 17.47 0.46 0.994
CS30 16.32 0.48 0.996
CST10 35.14 0.27 0.999
CST20 33.88 0.29 0.996
CST30 32.14 0.30 0.993

To clarify the effect of hydrophilicity of the nanofiber mats in PI release study, the initial PI loaded on the nanofiber mats was calculated, and the results are shown in Figure 10a. The results of the CS10, CS20, and CS30 nanofiber mats showed that the initial PI loaded on the nanofiber mat decreased with increasing the CS concentration. This result is due to the decreasing hydrophilicity of the nanofiber mats after CS addition. After T80 addition, the CST10, CST20, and CST30 nanofiber mats showed that the initial PI loaded is higher when compared with the nanofiber mats without T80 addition. This confirmed that the hydrophilicity of the nanofiber mat increased by T80 addition. Nevertheless, the hydrophilicity of the nanofiber mats may result in the PI release property as well as the PI remaining on the nanofiber mat. From Figure 8a, the percentage of the cumulative PI release from the nanofiber mats is the residual PI in PBS solution. Due to the PI degradation that can occur throughout the PI release study, the total percentage of PI release in this study is considered. The total percentage of PI release consists of the cumulative PI release and the PI degradation in PBS solution. The percentage of the cumulative PI release and the PI degradation in PBS solution and the PI remaining on the nanofiber mats with and without T80 addition are shown in Figure 10b. The results showed that the PI remaining of the CS10, CS20, and CS30 nanofiber mats increased with increasing the CS concentration. This result is due to the hydrophilicity of the nanofiber mat and related to the cumulative PI release and initial PI loaded results. After T80 addition, the PI remaining of the CST10, CST20, and CST30 nanofiber mats is lower than that of the nanofiber mats without T80 addition. This is due to the increasing hydrophilicity of the nanofiber mat by T80 addition, which agrees with the previous discussion. In addition, the PI degradation percentage of the CS10, CS20, and CS30 nanofiber mats were approximately 20 with a 0.21 ± 0.01 min−1 of the average PI degradation rate, whereas the PI degradation percentage of the CST10, CST20, and CST30 nanofiber mats after T80 addition were approximately 40 with a 0.43 ± 0.01 min−1 of the average PI degradation rate. When considering only the effect of nanofiber structure on the mechanical and PI release properties of the nanofiber mats, the nanofiber mats obtained in this study are normal fiber structure with solid cylindrical shape (41). The results showed that this structure has good mechanical and PI release properties (see Figures 4, 6, and 9). Moreover, the T80 addition in nanofiber mats has no significant effect on the nanofiber structure.

Figure 10 (a) Relative of the initial PI loaded of all nanofiber mats and (b) cumulative PI release, PI degradation and PI remaining of all nanofiber mats.
Figure 10

(a) Relative of the initial PI loaded of all nanofiber mats and (b) cumulative PI release, PI degradation and PI remaining of all nanofiber mats.

Finally, all of the results can confirm that the T80 addition not only enhances the hydrophilic property of the nanofiber mat but also promote the drug release property and possess the possibility in biomedical applications.

4 Conclusion

In this research, the nanofiber mats with and without T80 addition were prepared from the spinning solution at the range of 10–50% (v/v) CS solution by electrospinning technique. The result showed that the spinning solutions with the CS concentration at 10–50% (v/v) had an increase in apparent viscosity when the CS concentration was increased. However, only at 10–30% (v/v) CS concentrations of the spinning solution can be used to prepare nanofiber mats for biomedical application. Then, the nanofiber mats were investigated on the characteristics and morphology, mechanical property, wettability, antibacterial, and drug (PI) release properties. The results showed that the increase of the CS concentration in the nanofiber mat could reduce the nanofiber diameter and enhance the mechanical and antibacterial properties, whereas the wettability and drug release properties were diminished. Next, the effect of T80 addition in the spinning solution was investigated. The nanofiber mat with T80 addition can increase the uniformity leading to the increase of mechanical properties. Its wettability and drug release property were also enhanced. Moreover, the T80 addition not only promotes hydrophilicity that improves the drug release property but also maintains the antibacterial property of the nanofiber mat.

Acknowledgments

The authors would like to express thanks to the research professional development project under the Science Achievement Scholarship of Thailand (SAST) for the financial support and sincere thanks to the Faculty of Liberal Arts and Science, Kasetsart University, Kamphaeng Saen Campus, Thailand, for experimental support.

  1. Funding information: The research professional development project under the SAST provided some financial support to Chalongwut Boonpratum, PhD Student, in this study.

  2. Author contributions: Chalongwut Boonpratum: writing – original draft, methodology, and formal analysis; Patcharin Naemchanthara: writing – review and editing and formal analysis; Pichet Limsuwan: supervision and resources; and Kittisakchai Naemchanthara: writing – review and editing, project administration, and resources.

  3. Conflict of interest: Authors state no conflict of interest.

  4. Data availability statement: The raw/processed data required to reproduce these findings cannot be shared at this time as the data also form part of an ongoing study.

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Received: 2021-10-12
Revised: 2022-01-11
Accepted: 2022-01-11
Published Online: 2022-02-25

© 2022 Chalongwut Boonpratum et al., published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/epoly-2022-0029
Keywords for this article
nanofiber; chitosan; Tween 80; antibacterial activity; drug release
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  6. Effect of polyurethane/polyvinyl alcohol coating on mechanical properties of polyester harness cord
  7. Fabrication of flexible conductive silk fibroin/polythiophene membrane and its properties
  8. Development, characterization, and in vitro evaluation of adhesive fibrous mat for mucosal propranolol delivery
  9. Fused deposition modeling of polypropylene-aluminium silicate dihydrate microcomposites
  10. Preparation of highly water-resistant wood adhesives using ECH as a crosslinking agent
  11. Chitosan-based antioxidant films incorporated with root extract of Aralia continentalis Kitagawa for active food packaging applications
  12. Molecular dynamics simulation of nonisothermal crystallization of a single polyethylene chain and short polyethylene chains based on OPLS force field
  13. Synthesis and properties of polyurethane acrylate oligomer based on polycaprolactone diol
  14. Preparation and electroactuation of water-based polyurethane-based polyaniline conductive composites
  15. Rapeseed oil gallate-amide-urethane coating material: Synthesis and evaluation of coating properties
  16. Synthesis and properties of tetrazole-containing polyelectrolytes based on chitosan, starch, and arabinogalactan
  17. Preparation and properties of natural rubber composite with CoFe2O4-immobilized biomass carbon
  18. A lightweight polyurethane-carbon microsphere composite foam for electromagnetic shielding
  19. Effects of chitosan and Tween 80 addition on the properties of nanofiber mat through the electrospinning
  20. Effects of grafting and long-chain branching structures on rheological behavior, crystallization properties, foaming performance, and mechanical properties of polyamide 6
  21. Study on the interfacial interaction between ammonium perchlorate and hydroxyl-terminated polybutadiene in solid propellants by molecular dynamics simulation
  22. Study on the self-assembly of aromatic antimicrobial peptides based on different PAF26 peptide sequences
  23. Effects of high polyamic acid content and curing process on properties of epoxy resins
  24. Experiment and analysis of mechanical properties of carbon fiber composite laminates under impact compression
  25. A machine learning investigation of low-density polylactide batch foams
  26. A comparison study of hyaluronic acid hydrogel exquisite micropatterns with photolithography and light-cured inkjet printing methods
  27. Multifunctional nanoparticles for targeted delivery of apoptin plasmid in cancer treatment
  28. Thermal stability, mechanical, and optical properties of novel RTV silicone rubbers using octa(dimethylethoxysiloxy)-POSS as a cross-linker
  29. Preparation and applications of hydrophilic quaternary ammonium salt type polymeric antistatic agents
  30. Coefficient of thermal expansion and mechanical properties of modified fiber-reinforced boron phenolic composites
  31. Synergistic effects of PEG middle-blocks and talcum on crystallizability and thermomechanical properties of flexible PLLA-b-PEG-b-PLLA bioplastic
  32. A poly(amidoxime)-modified MOF macroporous membrane for high-efficient uranium extraction from seawater
  33. Simultaneously enhance the fire safety and mechanical properties of PLA by incorporating a cyclophosphazene-based flame retardant
  34. Fabrication of two multifunctional phosphorus–nitrogen flame retardants toward improving the fire safety of epoxy resin
  35. The role of natural rubber endogenous proteins in promoting the formation of vulcanization networks
  36. The impact of viscoelastic nanofluids on the oil droplet remobilization in porous media: An experimental approach
  37. A wood-mimetic porous MXene/gelatin hydrogel for electric field/sunlight bi-enhanced uranium adsorption
  38. Fabrication of functional polyester fibers by sputter deposition with stainless steel
  39. Facile synthesis of core–shell structured magnetic Fe3O4@SiO2@Au molecularly imprinted polymers for high effective extraction and determination of 4-methylmethcathinone in human urine samples
  40. Interfacial structure and properties of isotactic polybutene-1/polyethylene blends
  41. Toward long-live ceramic on ceramic hip joints: In vitro investigation of squeaking of coated hip joint with layer-by-layer reinforced PVA coatings
  42. Effect of post-compaction heating on characteristics of microcrystalline cellulose compacts
  43. Polyurethane-based retanning agents with antimicrobial properties
  44. Preparation of polyamide 12 powder for additive manufacturing applications via thermally induced phase separation
  45. Polyvinyl alcohol/gum Arabic hydrogel preparation and cytotoxicity for wound healing improvement
  46. Synthesis and properties of PI composite films using carbon quantum dots as fillers
  47. Effect of phenyltrimethoxysilane coupling agent (A153) on simultaneously improving mechanical, electrical, and processing properties of ultra-high-filled polypropylene composites
  48. High-temperature behavior of silicone rubber composite with boron oxide/calcium silicate
  49. Lipid nanodiscs of poly(styrene-alt-maleic acid) to enhance plant antioxidant extraction
  50. Study on composting and seawater degradation properties of diethylene glycol-modified poly(butylene succinate) copolyesters
  51. A ternary hybrid nucleating agent for isotropic polypropylene: Preparation, characterization, and application
  52. Facile synthesis of a triazine-based porous organic polymer containing thiophene units for effective loading and releasing of temozolomide
  53. Preparation and performance of retention and drainage aid made of cationic spherical polyelectrolyte brushes
  54. Preparation and properties of nano-TiO2-modified photosensitive materials for 3D printing
  55. Mechanical properties and thermal analysis of graphene nanoplatelets reinforced polyimine composites
  56. Preparation and in vitro biocompatibility of PBAT and chitosan composites for novel biodegradable cardiac occluders
  57. Fabrication of biodegradable nanofibers via melt extrusion of immiscible blends
  58. Epoxy/melamine polyphosphate modified silicon carbide composites: Thermal conductivity and flame retardancy analyses
  59. Effect of dispersibility of graphene nanoplatelets on the properties of natural rubber latex composites using sodium dodecyl sulfate
  60. Preparation of PEEK-NH2/graphene network structured nanocomposites with high electrical conductivity
  61. Preparation and evaluation of high-performance modified alkyd resins based on 1,3,5-tris-(2-hydroxyethyl)cyanuric acid and study of their anticorrosive properties for surface coating applications
  62. A novel defect generation model based on two-stage GAN
  63. Thermally conductive h-BN/EHTPB/epoxy composites with enhanced toughness for on-board traction transformers
  64. Conformations and dynamic behaviors of confined wormlike chains in a pressure-driven flow
  65. Mechanical properties of epoxy resin toughened with cornstarch
  66. Optoelectronic investigation and spectroscopic characteristics of polyamide-66 polymer
  67. Novel bridged polysilsesquioxane aerogels with great mechanical properties and hydrophobicity
  68. Zeolitic imidazolate frameworks dispersed in waterborne epoxy resin to improve the anticorrosion performance of the coatings
  69. Fabrication of silver ions aramid fibers and polyethylene composites with excellent antibacterial and mechanical properties
  70. Thermal stability and optical properties of radiation-induced grafting of methyl methacrylate onto low-density polyethylene in a solvent system containing pyridine
  71. Preparation and permeation recognition mechanism of Cr(vi) ion-imprinted composite membranes
  72. Oxidized hyaluronic acid/adipic acid dihydrazide hydrogel as cell microcarriers for tissue regeneration applications
  73. Study of the phase-transition behavior of (AB)3 type star polystyrene-block-poly(n-butylacrylate) copolymers by the combination of rheology and SAXS
  74. A new insight into the reaction mechanism in preparation of poly(phenylene sulfide)
  75. Modified kaolin hydrogel for Cu2+ adsorption
  76. Thyme/garlic essential oils loaded chitosan–alginate nanocomposite: Characterization and antibacterial activities
  77. Thermal and mechanical properties of poly(lactic acid)/poly(butylene adipate-co-terephthalate)/calcium carbonate composite with single continuous morphology
  78. Review Articles
  79. The use of chitosan as a skin-regeneration agent in burns injuries: A review
  80. State of the art of geopolymers: A review
  81. Mechanical, thermal, and tribological characterization of bio-polymeric composites: A comprehensive review
  82. The influence of ionic liquid pretreatment on the physicomechanical properties of polymer biocomposites: A mini-review
  83. Influence of filler material on properties of fiber-reinforced polymer composites: A review
  84. Rapid Communications
  85. Pressure-induced flow processing behind the superior mechanical properties and heat-resistance performance of poly(butylene succinate)
  86. RAFT polymerization-induced self-assembly of semifluorinated liquid-crystalline block copolymers
  87. RAFT polymerization-induced self-assembly of poly(ionic liquids) in ethanol
  88. Topical Issue: Recent advances in smart polymers and their composites: Fundamentals and applications (Guest Editors: Shaohua Jiang and Chunxin Ma)
  89. Fabrication of PANI-modified PVDF nanofibrous yarn for pH sensor
  90. Shape memory polymer/graphene nanocomposites: State-of-the-art
  91. Recent advances in dynamic covalent bond-based shape memory polymers
  92. Construction of esterase-responsive hyperbranched polyprodrug micelles and their antitumor activity in vitro
  93. Regenerable bacterial killing–releasing ultrathin smart hydrogel surfaces modified with zwitterionic polymer brushes
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