INTRODUCTION:

Cinnamomum camphora, commonly known as the camphor tree, is a member of the Lauraceae family. In some types of trees, the camphor content in the leaf oil can reach approximately 74 %, while in other types, borneol is the main component. Aside from camphor and borneol, there are also other compounds such as 1,8-cineole, and ÿ-terpineol found in the essential oil of camphor tree leaves. The group of oxyterpene compounds such as borneol dominates the essential oil content in young camphor tree leaves. Due to the hydrophobic nature of the oil, it can be used in topical preparations loaded into nanofiber as a matrix^1-2.

Nanofiber can be formed from various polymers such as polyacrylonitrile (PAN), polyvinyl pyrrolidone, polyvinyl alcohol, gelatin, collagen, chitosan, and carboxymethylcellulose using the electrospinning method. The unique properties of nanofiber include a large surface area, small pore size, and the ability to be formed into three- dimensional structures³. In addition, nanofiber can also be applied as a wound dressing³ and transdermal drug carrier⁵. The fiber has a diameter ranging from 100 – 500nm⁶. In this study, PAN polymer was used due to the stable jet formation, better fiber uniformity, more rigid molecular structure as well as hydrophobic nature that can help to enhance the permeation of lipophilic agent⁶. It also has good adhesion to the skin surface and creates an occlusive effect that increases drug absorption. The nanofiber was produced using electrospinning method, a simple, versatile, and useful technique for producing nano-sized fibers with very long and uniform diameters. In general, nanofiber produced from electrospinning is influenced by several parameters. These include solution parameters namely viscosity, conductivity, and surface tension of the polymer solution, as well as process parameters comprising flow rate, tension, and needle. Collector distance and environmental parameters also include temperature and humidity. Therefore, this study aimed to examine the effect of process parameters on nanofiber with the active ingredient camphor and characterization.

MATERIALS AND METHODS:

Materials:

The materials used in the nanofiber optimization and characterization process are N,N-Dimethylformamide (DMF) (Sigma Aldrich, Singapore), distilled water, polyacrylonitrile (Merck), Cinnamomum camphora oil.

Methods of preparation of PAN/C.camphora oil solution:

Figure 1 shows the experimental process of PAN/ C.camphora oil nanofiber. The main ingredients used in this study include C.camphora oil as active agent, PAN as polymer, and N, N-Dimethylformamide (DMF) as representing solvent. The polymer solution was prepared by dissolving PAN in DMF at 8 % by weight (P8). This was followed by stirring using a magnetic stirrer for 30 minutes until a homogeneous and clear solution was obtained. The C.camphora oil solution was prepared by dissolving in DMF at 10% by weight (C10). The C10 was added into P8 at 4% (P2), 6% (P3), 8% (P4), and 10 % (P5). The PAN/C.camphora solution was stirred without heating for about 3 minutes until a clear solution was obtained.

Figure 1: PAN/C.camphora oil solution preparation

Observations during the electrospinning process were carried out by the camera and showed on the monitor. The voltage used was 7 kV with a flow rate of 2µL min^-1, while the distance between the needle and collector was 10cm. The electrospinning process was carried out at room temperature, lasting for 3minutes on glass slides and 150min on aluminum foil⁶.

Electrospinning Setup:

PAN/C.camphora nanofibrous mats were produced by an electrospinning system (Nachriebe 601) as shown in Figure 1. The PAN/C.camphora solution was poured into a 10-mL syringe (inner diameter of 0.8 mm; 21 G) and pumped out with a flow rate of 2 µL min^-1. A positive voltage of 7 kV from a high voltage power supply was applied to the syringe with the needle tip being separated for 10 cm from a grounded collector. Specifically, the grounded collector was a rotary drum collector with a diameter of 5.5 cm and a length of 12 cm. The rotary drum collector was wrapped using aluminum foil as a collector to the PAN/C.camphora oil fibers⁴.

Characterizations of Nanofibrous Mat:

The physical and chemical characteristics of the fabricated PAN/C.camphora oil nanofibrous mats were evaluated, including fiber morphology, packing density, functional groups analysis, thermal properties, wettability, and mechanical strength.

Morphology was investigated by using a scanning electron microscope (SEM) (Hitachi tipe SU3500®). To calculate the nanofibrous mat packing density, the thickness, basis weight, and solid density must first be calculated. The thickness was measured by a thickness gauge (Mitutoyo®), while the basis weight, defined as mass per unit area⁷, was measured by cutting the mats into 10×10 cm² pieces. The pieces were then weighed by a digital mass scale (Fujitsu, FSR-A320).

Fourier transform infrared (FTIR) spectrometer (Shimadzu IRSpirit A224161 QATR-S®), examined the functional groups in the PAN/C.camphora oil, PAN, and C.camphora nanofibrous mats by scanning from 500 to 3500 cm^-1. A contact-angle measurement apparatus (Nachriebe 320) evaluated the wettability. The material surface wettability is divided into four categories based on the water contact angle (WCA) namely (i) super hydrophilic for WCA=0^o, (ii) hydrophilic for 0^o<WCA<90^o, (iii) hydrophobic for 90^o<WCA<120^o, (iv) ultra- hydrophobic for 120^o<WCA<150^o, and (v) superhydrophobic for WCA>150^o [20]. The mechanical strength of the PAN/C.camphora oil nanofibrous mats was measured by a tensile strength test apparatus (Zwick Roell DIN EN ISO 527-1®).

RESULT:

Nanofiber produced in this experiment was milky white in color. The resulting nanofiber was made from 8% PAN solution (P8) mixed with C.champora solution and then spun by the electrospinning method for ± 3 hours with a process parameter of 7 kV voltage, 2 mL/min flow rate, and 10 cm needle-to-collector distance. Figure 2 shows the stages of C.champora oil nanofiber production. P8 was prepared by mixing PAN powder and DMF followed by stirring using a magnetic stirrer until the PAN powder dissolved completely and the solution became homogeneous. Initially, the pure PAN solution was clear, then the C.champora solution was added. A mixture of 8% PAN solution and C.champora solution produced a milky white mixed solution. Spinning through the electrospinning method produced milky white nanofiber. PAN solution with C.champora solution was mixed in various ratios including 100:0 (P1); 96:4 (P2); 94:6 (P3); 92:8 (P4); 90:10 (P5).

Table 1: Viscocity Precursor Liquid Nanofiber

Sample	Ratio (8% PAN: 10% *C.champora*)	Average diameter (nm)	Coefficient variation (CV)	Viscocity (cP)
P1	100: 0	473 ± 66.00	0.1	19.38
P2	96: 4	380 ± 109.79	0.3	15.85
P3	94: 6	342 ± 4.36	0.01	13.25
P4	92: 8	326 ± 109.79	0.34	11.52
P5	90: 10	328 ± 109.81	0.33	7.98

Nanofiber P2-P5 have the nanometer orde, as seen from the results of nanofiber morphology measurements, the average diameter of nanofiber P1 is 473 ± 66.00 nm, while the average diameter of nanofiber P1, P2, P3, P4 is 380 ± 109.79 nm, 342 ± 4.36 nm, 326 ± 109.79 nm, and 328 ± 109.81 nm, respectively. The difference in standard deviation values is related to the resulting diameter size. Table 1 shows that the CV values for P1, P2, and P3, are <0.3.

The CV values for P4 and P5 are >0.3. A good nanofiber CV value is <0.3, which means it has a uniform diameter size. Meanwhile, nanofiber P4 and P5 are not uniform, as seen from the CV value>0.3, which is influenced by viscosity. From the data, it can be seen that the viscosity of the solution is too low, thus making the polymer jet less stable and the fiber size is not uniform and causing the nanofiber diameter to be smaller and non- uniform. Increasing the concentration of C.camphora can make the viscosity of the essential oil base solution and decreasing the concentration of the nanofiber polymer to be low so that it tends to form droplets that cause the formation of beads. Beads in nanofibers are droplets that form small clumps due to the failure of the electrospinning process of the essential oil solution and the polymer to turn into fine fibers during the electrospinning process.

Figure 3: SEM and fiber diameter distribution of nanofiber PAN/C.champora

FTIR spectroscopy:

Characterization was carried out on several samples including PAN-C.champoraoil nanofiber, PAN (P8) nanofiber, PAN-C.camphora (P3) in ratio 94:6 with DMF solution. Figure 4 shows the chemical bonds contained in the nanofiber sample. The spectrum band shows transmission at specific wavelengths belonging to the O–H; N- H functional group (3000 - 3500 cm^-1), the C-H group (2800-3000 cm^-1), and C=O (1600- 1800 cm^-1)⁶.

Figure 4: FTIR spectrum of nanofibers

The FTIR nanofiber results include absorption bands at 3000-3500 cm-1 indicating O-H and N-H bonds. The absorption band of 2800-3000 cm-1 indicates (C-H) bonds. The absorption band of 2200-2300 cm-1 indicates the nitrile group (C≡N). The absorption band at 1600-1800 cm-1 indicates the (C=C) or (C=N) bond. The absorption band of 1700-1750 indicates the presence of a (C=O) group which is a carbonyl group. The absorption band at 1000-1500 cm-1 is a fingerprint containing various bending and stretching modes. The PAN (P1) spectrum profile (black line) is depicted, the absorption band at 2240 cm-1 indicates the presence of (C≡N) which is the nitrile group of PAN. The absorption band around 2900 cm⁻¹ is the (C-H) group. The absorption band at 1450-1460 cm⁻¹ includes the (CH2) group. The spectrum profile of nanofiber containing C.champora (red line), in the absorption band around 1740 cm⁻¹ indicates the presence of a (C=O) group which is a carbonyl group. The absorption band at 2850-2960 cm⁻¹ includes the (CH2) and (CH3) groups. The absorption band of 1350-1450 cm⁻¹ indicates the presence of (CH2) and (CH3) groups. Identification of the spectrum of nanofiber containing a combination of PAN-C.champora, P3 (blue line), shows an overlap of both PAN and C.champora compounds. The nitrile peak of PAN and the carbonyl peak of C.champora are seen in the combined (C-H) absorption band area. The intensity variation indicates a molecular interaction between PAN and C.champora. This FTIR analysis shows that in P3, the incorporation of C.champora and PAN has been successful into the nanofiber structure.

Figure 5: XRD imaging of nanofibers

Nanofiber P3 was tested using X-ray diffraction (XRD), to determine the crystal form. Each XRD diffraction pattern has a peak. The intensity of the diffraction pattern produced occurs due to X-rays diffracted by the material being tested. XRD testing was carried out using a Rigaku SmartLab tool with general measurement settings, Long-Range Measurement 5-80º, Speed 10º/min, Step 0.01º, and incident slint 0.1º. Figure 5 shows the XRD characterization results of P3 nanofiber with peaks formed at 24.75º and 32.75º. This is due to amorphization during the electrospinning process.

Figure 6: Result of Tensile Strength Test

Mechanical test was carried out to determine the tensile stress of the resulting nanofiber. This test used a tensile testing machine (Zwick Roell DIN EN ISO 527-1). The nanofiber sample was pulled at a constant speed of 1 mm/min which then produced force. Figure 6 shows that the stress obtained from the tensile test results on nanofiber P3 was 0.2237 Mpa.

Table 2: Wettability measurement

Rasio PAN 8% : C10%	Contact angle (^o)
P1	13.61
P2	17.63
P3	17.87
P4	21.51
P5	22.83

Wettability measurement was carried out to determine the properties of variations in the PAN/C.champora nanofiber composite. Table 3 showed test the WCA. It was calculated from the contact angle formed on the surface of the nanofiber with the dripping water. When the contact angle formed is <90°, then the material has hydrophilic properties but when the contact angle formed is >90° the material is hydrophobic. The contact angle test showed variations in the addition of camphor to PAN with variations in the comparison of P2, P3, P4, and P5.

DISCUSSION:

Table 1 and Figure 3 show that P3 had the best fiber diameter as indicated by the lowest SD. This was also showed by the CV P3 value which was <0.3. Meanwhile, in P2, P4, and P5, the shape of the fiber remained lumpy. This was caused by the difference in the value of the viscosity of each solution. When the viscosity of the solution is low, then the solution will be limited because the polymer chain bonds are weakened by the presence of a mixed C.camphora oil. Therefore, during the spinning of the fiber, the solution moving toward the collector was controlled by the cone jet monitor. When the inertial force of the liquid was greater than the viscosity, the resulting fiber tended to have beads. This also affected the difference in CV values on the fiber.

The experiment showed significant differences in fiber characteristics between P1 and P2. Specifically, the fibers in these samples tend to be larger in size, resulting in a more uniform diameter, marked with a CV value of P5 >0.3. P3 also showed uniform fiber mats while P4 was not uniform because the viscosity of the solution was low (11.52 cP), leading to weak polymer chain entanglement. Therefore, during the spinning of the solution towards the collector, the inertial force of the liquid, which tends to form beads, is greater than the viscous force. The fiber will rebuild from the beads after some time of relaxation and then the elongation and thinning of the fiber will continue.

When the PAN solution was released from the needle with a certain voltage, the accelerated movement of positive ions caused the solution to elongate, evaporate the solvent, and experience a liquid-to-solid transition at once⁶. This shows that C.camphora and PAN form intermolecular interactions, specifically hydrogen bonds, as described in the FTIR characterization. The hydroxyl group in C.camphora in DMF liquid is a strong hydrogen bond donor and the nitrile group in PAN is a strong hydrogen bond acceptor. Therefore, a few hydrogen bonds can be formed between both materials inside the nanofiber. The amorphous state of the nanofiber can improve the stability of the dispersed drug. This implies that nanofiber can be used as a drug delivery vehicle^4-7.

Based on the result, the contact between water and nanofiber produced a small angle. The addition of C.camphora concentration to PAN successively, namely 4, 6, 8, and 10 resulted in a contact angle of 13.61, 17.63, 17.87, 21.51, and 22.83º. When the angle formed is between 0 - 90,º then the resulting nanofiber is hydrophilic or has an affinity for water. This also allows nanofiber to be applied in the pharmaceutical world, as a drug carrier.

CONCLUSION:

In conclusion, the addition of C.camphora oil to PAN affected the morphology and diameter of the fiber, which was stable at P3. Furthermore, characterization of chemical compounds carried out using the FTIR method showed that C.camphora oil was successfully encapsulated in nanofiber. The contact angle proved the hydrophilic nature of nanofiber. The XRD results showed that P3 did not form crystal peaks indicating the fiber was amorphous. This suggests that the nanofiber can be used as a drug carrier.

CONFLICT OF INTEREST:

The authors have no conflicts of interest regarding this investigation.

ACKNOWLEDGMENTS:

The authors would like to thank Institut Teknologi Sumatera and ITB for the facilities, scientific and technical supports.

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Received on 15.07.2025 Revised on 06.12.2025

Accepted on 21.02.2026 Published on 01.07.2026

Available online from July 04, 2026

Research J. Pharmacy and Technology. 2026;19(7):3246-3250.

DOI: 10.52711/0974-360X.2026.00462

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