EDIBLE NANOFIBER WITH OLIVE OIL ADDITIVE, SUITABLE FOR APPLICATION TO FOODS.

Abstract

The invention relates to the production of nanofibers obtained by electrospinning using a combination of edible and biocompatible polymer materials (polyvinyl alcohol and chitosan) and the addition of cold-pressed olive oil with antimicrobial properties, as well as the production of these nanofibers.

Description

1 TARIFF EDIBLE NANOFIBER WITH OLIVE OIL ADDITIVE, SUITABLE FOR APPLICATION TO FOODS. TECHNICAL FIELD The invention relates to polymer materials (polyvinyl alcohol and 5) that are edible and biocompatible. (chitosan) used together with cold-pressed olive oil, which has antimicrobial properties. Nanofibers obtained by electrospinning method as a result of addition and these nanofibers It is related to production. PREVIOUS TECHNIQUE 10 Edible film coatings are applied to the surfaces of foods using various methods. They can be obtained from plant and animal sources. Properties of edible films. among them are; reducing moisture loss, being biodegradable, and having a good appearance, exhibiting barrier properties against oxygen and physical stress, and having economic and toxicological implications. It can be considered safe from this perspective. 15 Because they are produced from natural and biologically recyclable materials materials that do not cause environmental pollution and contribute to the protection of the environment They are also known as antimicrobial and antioxidant agents for foods. They form a carrier medium for [products]. Therefore, frozen, fresh and processed [products] In food, to extend shelf life, prevent spoilage, and preserve sensory characteristics. 20 For this purpose, the use of edible films is increasing through modification. Edible nanofibers create a semi-permeable gas and water barrier between food and the environment. They also prevent bacterial contamination, extend the shelf life of food, and protect the food. They protect against mechanical damage and light. They are biodegradable. They improve the properties of packaged food. They reduce moisture loss and improve nutrition. They increase its value. It acts as a carrier for antimicrobial and antioxidant substances in food. By applying it to the surface, the rate of diffusion of protective substances from the surface to the interior is increased. They can also be used for control purposes. Edible films and coatings control oxygen, carbon dioxide, and lipid transfer. 30 By keeping it under control, it improves the mechanical properties of the food system, as well as taste and aroma. reducing the loss of substances, antioxidants, antimicrobial substances and By retaining pigments within the product, it improves food quality and shelf life. Food edible films and coatings that form a non-sticky and non-oily surface 2 It also provides mechanical protection by reducing food crushing and breakage, thus It contributes to the integrity of the food. The first known use of edible films in food coatings dates back to the 12th century. It is a coating made from wax in China and applied to citrus fruits. The coatings... The first coating applications in the food industry were candied apples, chocolate-coated candies, and 5 It consists of Kashar cheeses coated with edible wax. Applications are made with this. It has not been limited to that; in some meat products, edible collagen is used instead of animal intestine. Cases have started to be used. Edible film coatings for meat and meat products; for fresh or frozen meats. reducing moisture loss during storage, 10 in plastic containers fresh red meat or chicken sold has its water trapped, lipids reducing rancidity due to oxidation, preventing pathogenic microorganisms from entering the meat. to prevent it from entering the interior from the surface and to eliminate unwanted bad taste and odor. It ensures the prevention of the formation of its components. To minimize quality losses in food and spoilage reactions 15 Edible films are important for preventing moisture, oxygen, carbon dioxide, and... They can also form a barrier to the diffusion of flavoring components. Furthermore... properties of components found in foods such as antioxidants and antimicrobial substances They are also effective in contributing to the sensory characteristics and nutritional value of food. They can increase it. 20 Olive oil contains monounsaturated fatty acids such as oleic acid and linoleic acid. It differs from other oils in that it contains polyunsaturated fatty acids. This shows that olive oils contain phenolic organic compounds. It includes anti-inflammatory, antiproliferative, antioxidant and antimicrobial properties. Why does it happen? 25 The hydroxytyrosol and oleuropein in olive oils have high antioxidant properties. their capacities and metal chelation and free radical scavenging activities It is known. Olive oil has antioxidant, anti-inflammatory and antibacterial effects. It was stated. In addition, vitamins A, E, K, and essential minerals (calcium, 30 potassium, iron, etc.) and amino acids, unsaturated fatty acids, and micronutrients. It is recommended for use in daily diets because of the substances it contains. It is a food product. Studies on animal models have shown that olive oil... 3 It is believed that the squalene it contains reduces colon, lung, and skin tumors. Studies have been conducted. For food products, the time from producer to consumer is important, and this time The food must not spoil during transit. The food must be protected from oxygen, water vapor, from harmful ultraviolet (UV) rays, microorganisms, and chemical compounds. It is necessary to select a suitable packaging material that will protect the mixtures from harmful effects. Biodegradable films and coating materials are less harmful to the environment than plastic. Environmentally friendly packaging materials are preferred. Polysaccharides are polymeric structures, like proteins and fats. These materials are non-toxic. and 10 that are non-allergenic, biodegradable and highly biocompatible. are materials. In the current state of the art, the edible food packaging that is the subject of our invention the material contains a binary polymer mixture and olive oil together No studies have been found. The most important component is its antimicrobial properties. It is olive oil that produces it. 15 THE PURPOSE OF THE INVENTION The main purpose of our invention is to directly add olive oil to the polymer mixture, The extraction step is eliminated. Thus, the extraction is done first. Not doing so provides a cost advantage. 20 From a medical perspective, the use of oleic acid in the Mediterranean region has implications for coronary artery disease. It is known to be beneficial for various diseases. Furthermore, olive oil consumption can help with LDL / HD cholesterol levels. It improves the fat profile of cardiovascular risk by reducing the ratio. Olive oil, insulin resistance, lipid levels, DNA oxidation, and thrombotic processes in our bodies It positively affects the factors and blood pressure. Third stage in nanofiber production 25 The component is olive oil obtained from olives produced in Aydıncık district of Mersin province. It is known to consist of fatty acids and phenolic compounds. The composition of olive oil. Gas Chromatography (GC-FID)-Flame is used to verify this information, although it is already known. The ratios and types of fatty acids are determined using an Ionization Detector system. Attempts have been made to shed light on this. 30 Considering the methods applied under the known state of the art, both This reveals the originality of our study and the antimicrobial results we have obtained. Compared to others, it has shown activity against a large number of microorganisms. 4 It has been observed. Data obtained by comparing with the known state of the art, A comparison is made using the table below. Job title: Voltage (kV) Distance (cm) Flow rate Antimicrobial Activity (zone diameter) Reference Chitosan / PEO / marigold (2%) 18-20 15 0.1- 0.3 mL S. Aureus, E. Coli 22.0 ± 0.4 (mm), 20.9 ± 1.1 (mm) Kharat et al., 2021 Chitosan / gelatin / St. John's wort (1%, 5%) Spinning-free (Casting Method) S. Aureus / B. Cereus / E. Coli / S.Tyhpi (inhibition diameters) 21-14 years old) Lightening & Little, 2020 PVA / CS (0.5-1; 6-7) Enzyme study 13-16 16-20 0.2-0.6 - Nur Kutlu, 2017 10% PVA / 5% Ozone oil 30 15 5 mL - Falconer et al., 2022 Polyamide 6 / chitosan 34 15 0.5 - Virtue & Starboard, 2013 PEO / CS / PLC / olive oil 15-25 7.5-20 0.6-1 - E. Coli, S. Aureus, Zarghami et al., 2015 PVA / CS / zy (%1,%2) 20-25 18 0.5 - B. subtilis, S. aureus, E. faecalis, E. coli, K.pneumoniae, P. aeruginosa, C. albicans, A. niger, Our invention LIST OF FIGURES Figure 1. SEM image of the nanofibers that are the subject of the invention. Figure 2. Infrared spectrum graph of the nanofibers subject to the invention. DETAILED DESCRIPTION OF THE INVENTION 10 Our invention involves the combination of PVA / CS / olive oil materials in specified ratios. Edible film with nanofiber structure obtained by mixing and electrospinning. It is related to. In the production of the invention, firstly, polyvinyl alcohol (PVA), which is a support polymer, is dissolved in water. The solution was prepared homogeneously and then mixed with 1.5% chitosan solution for 15 minutes. The solution was mixed. The PVA / chitosan ratio was kept constant at 70:30 by weight. The solution is formed by adding olive oil at rates of 1% and 2% to the prepared solution. Electrospinning studies were conducted on the solutions. Preparation of a PVA / CS solution containing 1% olive oil. The PVA / CS ratio is kept constant at 70:30 by weight, and 1% is added to it. Olive oil was added. To prepare a 1% olive oil solution, 45ᵒC 24.75 grams of PVA / CS solution (70:30) in a heater with magnetic stirrer at [temperature] for 30 minutes. by stirring to raise the temperature of the solution and dissolve the olive oil 5 It was heated. Then, 1% olive oil was added to the PVA / CS solution at 45ᵒC. (0.25 g) was added and the solution mixture was stirred for 3 hours until complete dissolution was achieved. After the solution has a homogeneous appearance, it should be stirred for 20 hours at room temperature. The PVA / CS / olive oil solution was obtained after the mixing process. It has been left to rest. 10 Preparation of a PVA / CS solution containing 2% olive oil. The PVA / CS ratio is kept constant at 70:30 by weight, while adding 2%... Olive oil was added. To prepare a 2% olive oil solution, 45ᵒC 19.6 grams of PVA / CS solution (70:30) in a heater with magnetic stirrer at 15°C for 30 minutes. by stirring to raise the temperature of the solution and dissolve the olive oil. It was heated. Then, 2% olive oil was added to the PVA / CS solution at 45ᵒC. (0.4 g) was added and the solution mixture was stirred for 3 hours until complete dissolution was achieved. After the solution has a homogeneous appearance, it should be stirred for 20 hours at room temperature. This has been achieved. After the mixing process, the PVA / CS / olive oil solution is 20. It has been left to rest. Nanofibers were prepared by optimizing the following parameters. Solution mixture Distance (cm) Voltage (kV) Pump rate (mL / hr) PVA 14 16 0.5 PVA / CS (70:70) 14 17 0.5 PVA / CS / 1% olive oil 18 25 0.5 PVA / CS / 2% olive oil 18 25 0.5 6 Chromatographic (GC-FID) Analysis of Olive Oil Components Olive oil, fatty acids, and various organic materials are used in the production of nanofibers. It consists of compounds. The fatty acids found in the structure of olive oil The combination is determined by chromatographic devices and is predominantly gaseous. A chromatography (GC-FID)-Flame Ionization Detector system is used. This 5 In the analysis, the fatty acids found in the structure of olive oil were detected in an alcoholic medium using a KOH solution. The analysis is carried out using the method of converting it into methyl ester. The most abundant component in olive oil is Oleic Acid Methyl Ester (63.581%). It is located. After oleic acid methyl ester, there is palmitic acid methyl ester (%). It contains linoleic acid methyl ester (16,433%) and linoleic acid methyl ester (12,692%). 10 SEM image of the obtained nanofibers magnified 20,000 times (Figure 1). Upon examination, it was observed that the addition of olive oil slightly darkened the color of the nanofibers. It has been observed that the nanofibers are uniform and homogeneous. Their dimensions are as shown in Figure 1. It is approximately 200 nm. The increase in the amount of phenolic organic compounds with the addition of olive oil is 15 As a result of its formation and the presence of hydroxyl groups (OH) in its structure, Infrared The intensity of the peaks in the spectrum has increased (Figure 2). At the same time, the OH group has increased. This has resulted in a wide range and a broad peak. Antibacterial and antifungal activity results of nanofibers Minimum Inhibitory The concentration (MIC) is defined in the National Clinical Laboratory Standards Committee as 20 Broth was determined in 96-well microplates using the microdilution method. It has been done. The nanofibers tested were compatible with three Gram-positive, three Gram-negative, and two fungal species. Minimum inhibitory concentration (MIC) values ​​have been determined. Based on the tests conducted... According to PVA / CS / olive oil 2% nanofiber, Gram-positive, Gram-negative and fungus type 25 Higher than all types of PVA / CS / olive oil 1% nanofiber. It has been determined to have antimicrobial activity. PVA / CS / olive oil 2% and PVA / CS / olive oil 1% nanofibers are effective against the Gram-positive Bacillus subtilis. While showing less activity than the antibiotic amoxicillin, both nanofibers (1%) (olive oil and 2% olive oil nanofibers) Gram-negative Pseudomonas 30 It has more activity against aeruginosa than the antibiotic amoxicillin. It has been determined that 1% olive oil and 2% olive oil nanofibers inhibited Gram-positive B. coli. It is effective against S. subtilis, S. aureus, E. faecalis, and the Gram-negative E. coli and K. pneumoniae. It showed less activity than the tetracycline antibiotic. 2% olive oil nanofiber, P. 7 It has higher activity against aeruginosa than the tetracycline antibiotic. It has been observed that 2% olive oil nanofiber also affects the fungus Aspergillus niger. It has been determined to have less activity than the antibiotic ketoconazole. The MIC values ​​(μg / mL) of the tested nanofibers were 5. Nanofibers and standards ABCDEFGH Nanofiber 1 2048 2048 2048 2048 2048 128 - - Nanofiber 2 1024 1024 1024 1024 1024 32 1024 10 Amoxicillin <2 >1024 >1024 >1024 >1024 >1024 - - Tetracycline <2 64 64 <2 64 64 - - Ketoconazole - - - - - - 1 2 A: Bacillus subtilis ATCC 6623; 15 B: Staphylococcus aureus ATCC 25923; C: Enterococcus faecalis ATCC 29212; D: Escherichia coli ATCC 25922; E: Klebsiella pneumoniae ATCC 70060; F: Pseudomonas aeruginosa ATCC 27853; 20 G: Candida albicans ATCC 10231; H: Aspergillus niger ATCC 16404. The texture analysis and mechanical properties of the obtained nanofibers were investigated. Food Properties such as hardness, stickiness, viscosity, and elasticity of materials affect the shelf life of food. This is important for producers in terms of obtaining PVA / CS / olive oil polymer solutions. The nanofibers produced are also food products and are used in food packaging along with the food itself. Its elastic structure is important because it is edible. Texture analysis results show 2%. Nanofibers with added olive oil have a much more elastic and robust structure. It shows. 30 The peroxide content in 1% olive oil is higher than in 2% olive oil. This is due to the high level of active oxygen in the oil. Peroxide is caused by active oxygen. The higher the amount, the lower the degradation level of nanofibers in 1% olive oil, compared to 2%. It appears to contain more nanofibers than olive oil. Foods 8 By examining the peroxide level in its packaging, 2% olive oil nanofiber is more suitable. It can be concluded that it is appropriate. According to the "Regulation on Oils Named After Plants" specified by the Turkish Food Codex. According to this, the maximum limit is 10 meq / kg for refined oils and the maximum limit is 10 meq / kg for cold-pressed oils. It has been stated that there may be milliequivalent active oxygen / kg fat. 5 PVA / CS / zy (1%) Peroxide Number 0.266 - meq / kg - PVA / CS / zy (2%) Peroxide Number 0.191 - meq / kg - 15 25

Claims

9 REQUESTS 1. It is an edible nanofiber characterized by its olive oil content.

2. It is an edible nanofiber composed of PVA (polyvinyl alcohol), chitosan, and olive oil. It is characterized by containing 5 3. A nanofiber that meets any of the above requirements and has the following characteristic: olive oil. It is characterized by having a rate of 1%.

4. The nanofiber is compliant with claim 1 or 2, and its characteristic is that the olive oil content is 2%. It is characteristic.

5. Producing edible nanofibers, the characteristic of which is; 10 - Homogeneous aqueous solution of polyvinyl alcohol (PVA) as a support polymer. prepared in some way - Then, a 1.5% chitosan solution with PVA / chitosan 70:30 by weight. mixing while keeping the ratio constant, - Solutions created by adding olive oil to the prepared solution are 15 It is characterized by steps involving exposure to electrospinning.

6. The additional olive oil mentioned in Claim 5 is characterized by its proportion being 1%. It is characteristic.

7. The additional olive oil mentioned in Claim 5 is characterized by its proportion being 2%. It is characterized by... 20 30

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