TR201608065A2

TR201608065A2 - ANTIMICROBIAL MIXTURE WITH HYDROGEN PEROXIDE

Info

Publication number: TR201608065A2
Application number: TR2016/08065A
Authority: TR
Inventors: Tezcan Erdem; Kemal Avci Murat
Original assignee: Tezcan Erdem; Kemal Avci Murat
Priority date: 2016-07-04
Filing date: 2016-07-04
Publication date: 2016-09-21

Abstract

Buluş, hidrojen peroksit içerikli olan ve antimikrobiyal özellik gösteren kimyasal bileşimlerin üretim yöntemi ile ilgilidir. Özellikle medikal endüstride, dezenfeksiyon amacıyla kullanılabilecek ve çok etkili antimikrobiyal özellik gösteren ve stabil olan kimyasal karışımların üretim yöntemini içerir.The invention relates to the production method of chemical compounds containing hydrogen peroxide and showing antimicrobial properties. It includes the production method of chemical mixtures that can be used for disinfection purposes, especially in the medical industry, and have very effective antimicrobial properties and are stable.

Description

TARIFNAME HIDROJEN PEROKSIT IÇERIKLI ANTIMIKROBIYAL KARISIM Bulus, hidrojen peroksit içerikli olan ve antimikrobiyal özellik gösteren kimyasal bilesimlerin üretim yöntemleri ile ilgilidir. DESCRIPTION ANTIMICROBIAL MIX WITH HYDROGEN PEROXIDE The invention is a chemical that contains hydrogen peroxide and has antimicrobial properties. relates to the production methods of the compositions.

Günümüzde antimikrobiyal ajanlar olarak azot içeren katyonik kimyasallar oldukça genis kullanima sahiptirler. Benzalkonyum klorür, setrimit gibi kuaterrier amonyum tuzlari bunlara birer örnektir. Bu kimyasallar en basit ifadeyle, sahip olduklari katyonik gruplarin, mikroorganizmalarin hücre yüzeylerindeki negatif uçlara baglanmasiyla onlari inhibe edip öldürürler. Katyonik azot içeren kimyasallar, çok düsük dozlarda bile, planktonik haldeki mikroorganizmalarin negatif hücre yüzeylerine baglanabilmekte ve onlari öldürebilmektedirler. Örnegin, piyasada bile planktonik haldeki birçok mikroorganizmaya karsi etkilidir. Bu tür kimyasallardaki sorun, mikroorganizmalarinin negatif yüzey yüklerinin her zaman ulasilabilir olmamasidir. Mikroorganizmalar genelde sulu çözeltiler içerisinde planktonik halde bulunup negatif hücre yüzeyini açiga çikarirlarken, Spor olusumu ve zemin gibi yüzeylere tutunduklarinda biyofilm olusumu gibi durumlarda negatif hücre yüzeyi açikta degildir. Bu nedenle azot içeren katyonik kimyasallar tavsiye edilen dozlarda sadece planktonik haldeki mikroorganizmalari öldürürlerken, spor ve biyofilm halindeki mikroorganizmalara karsi etkisizlerdir. Bu nedenle, azot içeren katyonik kiinyasallar yüksek düzey dezenfeksiyondan ziyade basit dezenfeksiyon islemlerinde kullanilirlar, Hidrojen peroksit, H202 formülüne sahip olan ve su ile her oranda karisabilen bir kimyasaldir. Oksidatif özelliginden dolayi antimikrobiyal etki gösterir. %10 ve üzeri derisimlerdeki hidrojen peroksitin oksidatif özelligi ve ona bagli olarak da antimikrobiyal özelligi çok yüksektir. Bu nedenle %10 ve üzeri derisimlerdeki hidrojen peroksit, “yüksek düzey dezenfeksiyon” için tercih edilen bir kimyasaldir. Today, nitrogen-containing cationic chemicals are widely used as antimicrobial agents. they have wide usage. Quaternary ammonium such as benzalkonium chloride, cetrimite salts are examples. In the simplest terms, these chemicals have cationic groups are attached to the negative terminals on the cell surfaces of microorganisms. By binding, they inhibit and kill them. Chemicals containing cationic nitrogen Even at low doses, microorganisms in planktonic state can become negative cells. They can attach to their surfaces and kill them. For example, in the market It is effective against many microorganisms, even in planktonic form. This kind The problem with chemicals is that the negative surface charges of microorganisms are always is not accessible. Microorganisms are usually found in aqueous solutions. While they are in a planktonic state and reveal the negative cell surface, Spore formation and negative in cases such as biofilm formation when they cling to surfaces such as floors. cell surface is not exposed. Therefore, nitrogen-containing cationic chemicals are recommended. While they kill only planktonic microorganisms at the doses given, spores and They are ineffective against microorganisms in the form of biofilms. Therefore, the nitrogen-containing cationic chemicals are simple disinfection rather than high-level disinfection are used in their Hydrogen peroxide is a compound that has the formula H2O2 and can be mixed with water in any ratio. is chemical. It shows antimicrobial effect due to its oxidative property. 10% and above The oxidative properties of hydrogen peroxide in concentrations and, accordingly, It has very high antimicrobial properties. Therefore, in 10% and above skins hydrogen peroxide is the chemical of choice for “high-level disinfection”.

Hidrojen peroksit çözeltileri %107dan daha zayif olduklarinda ise mikroorganizmalara karsi etkileri Ciddi olarak düser. Bu nedenle, genelde agirlikça dezenfeksiyon amaciyla kullanildiklarinda en fazla 5 kat sulandirildiginda tatmin edici neticeler verebilmektedir. Bundan dolayi, daha fazla sulandirilmak isteniliyorsa azot içeren katyonik kimyasallarla birlikte olacak sekilde formülize edilmelidirler. When hydrogen peroxide solutions are weaker than 107%, Effects against microorganisms Severely reduced. Therefore, it is generally Satisfaction when diluted up to 5 times when used for disinfection. can give conclusive results. Therefore, if it is desired to be diluted further They must be formulated together with nitrogen-containing cationic chemicals.

Fakat, %10 ve üzeri derisimlerdeki hidrojen peroksit çözeltileri çok aktif olduklari için hizli bir sekilde bozulup oksijen gazi açiga çikarirlar. Bu durum ise ürün siselerinin basinçtan sismesine, hatta patlamasina neden olabilmektedir. Ayrica, hidrojen peroksit çözeltileri oldukça reaktif olduklarindan, azot içeren katyonik kimyasallarla da tepkimeye girip onlari bozmaktadirlar. Bu durum, hidrojen peroksit çözeltilerinin azot içeren katyonik kimyasallar ile birlikte formülize edilmesinin önünde büyük bir engeldir. However, hydrogen peroxide solutions in 10% and above concentrations are very active. They decompose quickly to release oxygen gas. In this case, the product It can cause the bottles to swell or even explode due to pressure. Moreover, Since hydrogen peroxide solutions are highly reactive, nitrogen-containing cationic they also react with chemicals and spoil them. This is hydrogen peroxide formulation of solutions with nitrogen-containing cationic chemicals. is a big obstacle.

Günümüzde hidrojen peroksit sulu çözeltilerinin stabilizasyonu için nano gümüs, gümüs ve kalay tuzlari ve fosfonatlar gibi çesitli kimyasallar (stabilizanlar) mevcut olsa da, bu stabilizanlar hidrojen peroksitten baska aktif içermeyen çözeltilerde iyi sonuç vermektedir. Örnegin, dietilentriamin penta(metilen fosfonik asit] isimli stabilizan, sadece hidrojen peroksit ve sudan olusan çözeltileri gayet basarili bir sekilde stabil ederken, ortamda ilave olarak benzalkonyum klorür varliginda onunla etkilesim yapmakta ve bu durum son ürünün stabilizasyonunu ve antiiriikrobiyal etkisini azaltmaktadir. Today, nano silver for the stabilization of hydrogen peroxide aqueous solutions, various chemicals (stabilizers) such as silver and tin salts and phosphonates are present However, these stabilizers work well in solutions containing no actives other than hydrogen peroxide. gives results. For example, diethylenetriamine penta(methylene phosphonic acid] stabilizer, solutions consisting only of hydrogen peroxide and water can be used very successfully. while it is stable in shape, in the presence of additional benzalkonium chloride in the environment with it. interacts and this causes the stabilization of the final product and its antimicrobial lessens its effect.

Nano gümüs, hem hidrojen peroksit stabilizasyonu etkisi olmasi, hem de antimikrobiyal özelliginin olmasi nedeniyle özel bir öneme sahiptir, Ayrica, dezenfeksiyon sonucu ortamda kalan gümüs nanoparçaciklari, gümüs tuzlarinin aksine oldukça stabildir. Nano gümüsün uygulamadan sonra stabil olmasi, dezenfeksiyon sonrasi ortamin antimikrobiyal kalmasini saglar. Mevcut tekniklerle nano gümüs üretimi, gümüs nitrat gibi gümüs tuzlari içeren sulu çözeltilerin elektrolitik yöntemle veya askorbik asit kullanimi gibi kimyasal yöntemle islenmesiyle gerçeklestirilir. Nano silver has both a hydrogen peroxide stabilization effect and It has a special importance due to its antimicrobial properties. silver nanoparticles remaining in the environment as a result of disinfection, silver salts On the contrary, it is quite stable. Stability of nano silver after application, It ensures that the environment remains antimicrobial after disinfection. with existing techniques nanosilver production is the production of aqueous solutions containing silver salts such as silver nitrate. electrolytic method or chemical method such as the use of ascorbic acid carried out by processing.

Elektrolitik yöntemde; üretilebilen nano gümüs miktarinin oldukça sinirli olmasi, bu üretim için gerekli ekipmanin çok pahalli olmasi ve sürecin oldukça yavas olmasi gibi dezavantajlar mevcuttur. Bu nedenle elektrolitik yöntemle nano gümüs üretiminin endüstriyel ölçekte kullanimi oldukça sinirlidir. Kimyasal yöntemde, gümüs tuzlarinin sulu çözeltisinin, askorbik asit gibi kimyasallar kullanilarak redüksiyonu gerçeklestirilir. Bu yöntem, çok daha konsantre nano gümüs üretimini oldukça basit ekipmanlarla hizli ve ucuz olarak gerçeklestirmeye olanak saglar. Fakat sürecin hizli olmasi partikül boyutunun kontrolünü zorlastirir ve sulu çözelti içerisinde olusan metalik gümüs bir araya gelerek çökme egiliminde olur. Bu nedenle, kimyasal yöntemle nano gümüs sentezinde, nano gümüs parçaciklarini kaplayarak stabil edici baska kimyasallar da ortama eklenir. Bu kimyasallar arasinda SBS ve karboksimetil selüloz gibi birçok seçenek mevcuttur. Nano gümüs üretiminde mevcut olan bu seçeneklerin çogu, hidrojen peroksitin tek basina bulundugu sulu çözeltileri stabil etmekte gayet basarili iken, ortamda katyonik azot bilesikleri mevcutken onlarla etkilesime girip etkilerini kaybederler. Bu nedenle, hem hidrojen peroksit hem de azot içeren katyonik bilesiklerin bulundugu çözeltiler basarili bir sekilde stabil edilememektedir. In the electrolytic method; Since the amount of nano silver that can be produced is quite limited, this the equipment required for production is very expensive and the process is quite slow There are disadvantages such as For this reason, nano silver with electrolytic method The use of its production on an industrial scale is quite limited. In the chemical method, of the aqueous solution of silver salts using chemicals such as ascorbic acid. reduction is performed. This method allows the production of much more concentrated nano silver. It allows to perform it quickly and cheaply with very simple equipment. But the rapidity of the process makes it difficult to control the particle size and the aqueous solution The metallic silver formed in it tends to come together and collapse. This Therefore, nano silver particles are used in nano silver synthesis by chemical method. Other chemicals that stabilize it by coating are also added to the medium. Among these chemicals Many options are available, such as SBS and carboxymethyl cellulose. nano silver Many of these options available in the production of hydrogen peroxide alone While it is very successful in stabilizing the aqueous solutions it is in, cationic nitrogen in the environment While their compounds are present, they interact with them and lose their effect. Therefore, both solutions containing both hydrogen peroxide and nitrogen-containing cationic compounds cannot be successfully stabilized.

Bu bulus ile, hem azot içeren katyonik bilesen hem de hidrojen peroksit kimyasallarinin ikisini birden içeren antimikrobiyal karisimlarin üretilmesi ve stabil kalmasi mümkün kilinmistir. Bunun için 2 asamali sentez yöntemi gelistirilmistir. With this invention, both the nitrogen-containing cationic component and hydrogen peroxide production of antimicrobial mixtures containing both possible to remain. For this, a two-stage synthesis method has been developed.

Ilk asaina Sekil l”de gösterilen arap zamki ile kaplanmis nano gümüs stok çözeltisi sentezi”dir. Bu asama en temel halinde; - Arap zamkinin suda çözündürülmesi (101), - olusan karisima askorbik asit eklenip çözündürülmesi (102), - olusan karsima gümüs tuzunun karistirilmasi (103), - karisima pH ayarlayici eklenerek, nano gümüs sentezi için gerekli pH degerinin saglanmasi (104) - nano gümüs içeren çözeltinin karistirilmasi (105), - nano gümüs içeren karisima pH ayarlayici eklenerek istenilen pH degerinin saglanmasi (106) Ikinci asama ise “Sekil 2: Hidrojen peroksit içerikli antimikrobiyal karisim üretimi,”dir. Bu asama en temel halinde ; - hidrojen peroksit çözeltisine, istenilen miktarda “arap zamki ile kaplanmis nano gümüs stok çözeltisi” (100) karistirilmasi (201), - olusan karisima azot içeren katyonik bilesen eklenip karistirilmasi (202), - Olusan karisima kalay tuzunun karistirilmasi (203), - olusan karisima sivi bilesen karistirilmasi (204), - karisimin pH ayarlayici ile istenilen pH degerine ayarlanmasi (205), - karisimin partiküllerden arindirilmasi (206). The first step is the nano silver stock solution coated with gum arabic, shown in Figure 1 synthesis”. This phase is in its most basic form; - Dissolving gum arabic in water (101), - adding ascorbic acid to the resulting mixture and dissolving it (102), - mixing the silver salt to the resulting mixture (103), - By adding a pH adjuster to the mixture, the pH value required for nano silver synthesis providing (104) - mixing the solution containing nano silver (105), - The desired pH value can be adjusted by adding a pH adjuster to the mixture containing nano silver. providing (106) The second stage is “Figure 2: Antimicrobial mixture containing hydrogen peroxide. production”. This phase is in its most basic form; - into the hydrogen peroxide solution, nano gum coated with the desired amount of "gum arabic" silver stock solution” (100) mixing (201), - adding nitrogen-containing cationic component to the resulting mixture and mixing (202), - Mixing the tin salt in the resulting mixture (203), - mixing the liquid component of the resulting mixture (204), - adjusting the mixture to the desired pH value with a pH adjuster (205), - removal of particles from the mixture (206).

Sekil 1”de ilk asama olan arap zamki ile kaplanmis nano gümüs stok çözeltisi sentezinin islem adimlari gösterilmistir (100). Öncelikle istenilen miktar arap zamki suda çözündürülür (101). Sonrasinda, olusan karisima askorbik asit eklenip çözündürülür (102). Daha sonra, olusan karsima gümüs tuzu karistirilir (103). Sonra, pH ayarlayici eklenerek, nano gümüs sentezi için gerekli pH degeri saglanir (104). Nano silver stock solution coated with gum arabic, which is the first step in Figure 1 The processing steps of the synthesis are shown (100). First, the desired amount of gum arabic dissolved in water (101). Afterwards, ascorbic acid is added to the resulting mixture. is dissolved (102). Then, silver salt is mixed with the resulting mixture (103). Then, By adding a pH adjuster, the pH value required for nano silver synthesis is provided (104).

Böyle bir ortamda, askorbik asit, gümüs tuzunu indirgeyerek onu metalik gümüs haline çevirir. Metalik gümüs ise ortamdaki arap zamki ile kaplanip stabil hale gelir. In such an environment, ascorbic acid reduces the silver salt to make it metallic silver. turns it into. Metallic silver, on the other hand, is coated with gum arabic and becomes stable.

Sistem belirlenen süre karistirildiktan (105) sonra tekrar pH ayarlamasi (106) yapilarak, arap zamki ile kaplanmis nano gümüs stok çözeltisi sentezinin tamamlanmasi saglanir (100). pH adjustment (106) after the system has been stirred for the specified time (105) synthesis of nano silver stock solution coated with gum arabic. completion is ensured (100).

Sekil 2”de ikinci asama olan hidrojen peroksit içerikli antimikrobiyal karisim üretiminin islem adimlari gösterilmistir (200). Bu islem adimlari sentezin ikinci asamasidir. Bunun için, ilk asamada üretilen “arap zamki ile kaplanmis nano gümüs stok çözeltisi” (100), istenilen miktarda hidrojen peroksit çözeltisi ile karistirilir (201]. Daha sonra, olusan karisima azot içeren katyonik bilesen eklenip karistirilir (202). Sonra, olusan karisima kalay tuzu karistirilir (203). Olusan karisima sivi bilesen eklenip karistirildiktan (204) sonra karisimin pH degeri, pH ayarlayici bir kimyasalin eklenmesi ile ayarlanir (205). Son olarak ise, üretilen karisim partiküllerinden arindirilir (206). Antimicrobial mixture containing hydrogen peroxide, which is the second stage in Figure 2 The processing steps of the production are shown (200). These process steps are the second step of the synthesis. is the phase. For this purpose, "nano silver coated with gum arabic" produced in the first stage “stock solution” (100) is mixed with the desired amount of hydrogen peroxide solution. (201]. Next, the nitrogen-containing cationic component is added to the resulting mixture and mixed. (202). Then, the resulting mixture is mixed with tin salt (203). The resulting mixture of liquid After adding the component and mixing (204), the pH value of the mixture is adjusted to a pH-adjusting adjusted by the addition of the chemical (205). Finally, the mixture produced It is purified from particles (206).

Sentezin ilk asamasi olan “arap zamki ile kaplanmis nano gümüs stok çözeltisi tercihen 10-50 gram, daha tercihen 40-60 gram araliginda olmalidir. Kullanilan tercihen 0,8-1,2 gram araliginda olmalidir. Gümüs nitrat, gümüs klorür, gümüs hidroksit, gümüs oksit ve gümüs sitrat kimyasallarindan en az biri sentezde kullanilan gümüs kaynagi olarak kullanilmalidir (103). Gümüs iyonu derisimi ise olmalidir(103). Böylece, gümüs iyonunu indirgeyecek miktarda askorbik asit, ve indirgenen gümüsü kaplayabilecek miktarda arap zamki ortamda bulunacaktir. The first step of the synthesis, the "Gum arabic nano silver stock solution" preferably in the range of 10-50 grams, more preferably 40-60 grams. Used preferably between 0.8-1.2 grams. silver nitrate, silver chloride, silver At least one of the chemicals hydroxide, silver oxide and silver citrate is in the synthesis. used silver should be used as a source (103). If the silver ion skin should be(103). Thus, an amount of ascorbic acid to reduce the silver ion, and gum arabic in sufficient quantity to cover the reduced silver will be present in the environment.

Gümüs nano partikülü sentezi sirasinda pH araligi 0,5-14 araliginda tutulabilir. Fakat pH degeri 3-9, daha tercihen ise 4-8 araliginda olmalidir (104). Reaksiyon pH degeri ayarlandiktan sonra sistem karistirilir (105). Bu asamada, reaksiyonu eksi on derece (-10 OC) ile arti yüz elli derece (+150 °Cl sicaklik araliginda gerçeklestirmek mümkündür. Düsük sicaklikta reaksiyon süresinin çok uzayip, yüksek sicakliklarda ise üründe bozulmalar olup üretim sürecinin zorlastigi için, ideal sicaklik degeri oda sicakligidir. Sistemin ayarlanan pH ve sicaklik degerinde karistirilmasi (105) zamki ile kaplanmis nano gümüs stok çözeltisi sentezinin (100) son asamasi olan pH ayarlanmasi (106) sirasinda pH degeri 1-14 arasina ayarlanabilir. Fakat, çözeltinin stabil olmasi için pH degeri tercihen 4-9, daha tercihen 6-8 arasinda olmalidir (106). During the synthesis of silver nanoparticles, the pH range can be kept in the range of 0.5-14. But The pH value should be in the range of 3-9, more preferably 4-8 (104). Reaction pH value Once set, the system is mixed (105). At this stage, his reaction is minus ten degrees. (-10 OC) to plus one hundred and fifty degrees (+150 °Cl) possible. At low temperature, the reaction time is very long, at high temperatures on the other hand, the ideal temperature value should be in the room, since there is deterioration in the product and the production process becomes difficult. is the temperature. Mixing the system at the adjusted pH and temperature (105) pH, the final step of the synthesis (100) of nano silver stock solution coated with gum During the adjustment (106), the pH value can be adjusted between 1-14. However, the solution To be stable, the pH value should preferably be between 4-9, more preferably between 6-8 (106).

Sentezin ikinci asamasi olan “hidrojen peroksit içerikli antimikrobiyal karisim üretimi” (200) kisminda, sentez için kullanilan hidrojen peroksit derisimi agirlikça Son karisim içerisindeki hidrojen peroksitin agirlikça orani ise %0,1-%49, tercihen klorhekzidin tuzlari, polihegzametilen biguanid, didesil dimetil amonyum klorür, setrimonyum tuzlari ve setrimit kimyaSallarindan en az birisi azot içeren katyonik bilesen olarak karisima eklenmelidir (202]. Azot içeren katyonik bilesenin son fonnülasyondaki agirlikça orani ise %0,01-%50, tercihen %1-% 25, daha tercihen sodyum stannat, kalay klorür, kalay dioksit ve kalay karbonat kimyasallarindan en az birinden seçilmelidir. Kullanilan kalay tozunun son formülasyondaki agirlikça orani Karisima eklenen “sivi bilesen” (204) olarak ise tercihen deiyonize su olmak üzere, distile su, musluk suyu, izotonik sodyum klorür çözeltisi, sitrat tampon çözeltisi, fosfat tampon çözeltisi, dimetil sülfoksit, dimetil formamid, izopropil miristat, etil alkol, metil alkol, izopropil alkol, propilen glikol, dipropilen glikol ve polietilen glikol sivi bilesenlerinden en az birisi kullanilmalidir. Sentez sirasinda sisteme eklenen “hidrojen peroksit çözeltisi”, “azot içeren katyonik bilesen”, “kalay tuzu” ve dogrudan sisteme karistirilabilecegi gibi, yukarida bahsedilen herhangi bir “sivi bilesen” içerisinde karistirildiktan sonra da sisteme karistirilabilir. Forrnülasyonun pH degeri, 1-12 araliginda ayarlanabilir (205). Fakat, ürünün stabilizasyonu ve antimikrobiyal etkisinin korunmasi için pH degeri tercihen 1-8; daha tercihen 4-6 araliginda ayarlanmalidir (205). Sitrik asit, asetik asit, hidroklorik asit, hidroflorik asit, nitrik asit, sülfürik asit, sodyum hidroksit, potasyum hidroksit, sezyum hidroksit ve rubidyum hidroksit kimyasallarindan en az birisi, hem ilk asamada hem de ikinci asamada kullanilan pH ayarlayici olarak seçilebilir. Islem sonunda olusan Iiltreden geçirme, santrifüjleme, dinlendirme yöntemlerinden en az bir tanesi seçilebilir. Partiküllerin uzaklastirilmasi islemine nano gümüsten dolayi olusan partiküller dahil edilmeyebilirler. Böylece, ortamda kalan nano gümüs partikülleri hem antimikrobiyal karisimin stabilizasyonunu arttirirken, hem de dezenfeksiyon sonrasinda ortamda kalarak aseptik sartlarin devamini saglar. Bulus konusu üretim yönteminde “islem sirasi” önemli olmadigi için islem sirasi degistirilebilir. The second step of the synthesis, the “antimicrobial mixture containing hydrogen peroxide Production of hydrogen peroxide used for synthesis in section (200) is calculated by weight. The ratio of hydrogen peroxide in the final mixture by weight is 0.1%-49%, preferably chlorhexidine salts, polyhexamethylene biguanide, didecyl dimethyl ammonium chloride, cetrimonium salts and at least one of the cetrimide chemicals cationic containing nitrogen It should be added to the mixture as a component (202]. The last of the nitrogen-containing cationic component the weight ratio in the formulation is 0.01%-50%, preferably 1%-25%, more preferably sodium stannate, stannous chloride, tin dioxide and tin carbonate chemicals one must be chosen. The weight ratio of tin powder used in the final formulation As the “liquid component” (204) added to the mixture, preferably deionized water, distilled water, tap water, isotonic sodium chloride solution, citrate buffer solution, phosphate buffer solution, dimethyl sulfoxide, dimethyl formamide, isopropyl myristate, ethyl alcohol, methyl alcohol, isopropyl alcohol, propylene glycol, dipropylene glycol and polyethylene At least one of the glycol liquid components should be used. system during synthesis. "hydrogen peroxide solution", "nitrogen-containing cationic component", "tin salt" and As it can be mixed directly into the system, any “liquid” mentioned above It can also be mixed into the system after being mixed in the “component”. formulation The pH value can be adjusted within the range of 1-12 (205). However, product stabilization and pH value preferably 1-8 in order to preserve its antimicrobial effect; more preferably 4-6 should be set in the range (205). citric acid, acetic acid, hydrochloric acid, hydrofluoric acid, nitric acid, sulfuric acid, sodium hydroxide, potassium hydroxide, cesium hydroxide and at least one of the rubidium hydroxide chemicals, both in the first stage and in the second It can be selected as the pH adjuster used in the step. If you are at the end of the transaction At least one of the methods of filtering, centrifugation, and resting can be selected. Formed due to nano silver in the process of removing particles particles may not be included. Thus, the nano silver particles remaining in the environment while increasing the stabilization of the antimicrobial mixture and disinfection then it stays in the environment and ensures the continuation of aseptic conditions. Inventive production Since the “processing order” is not important in the method, the processing order can be changed.

Bulus konusu yöntemin, medikal endüstri basta olmak üzere sanayiye birçok uygulanma biçimi mevcuttur. Üretilen forrnülasyonlar hem stabil olmakta, hem de antimikrobiyal özellikleri olan hidrojen peroksit, azot içeren katyonik bilesen ve nano gümüs kiiriyasallarinin tümünü içermektedirler. Böylece, bulus konusu yöntemle üretilen formülasyonlar, tüm bu antimikrobiyal kimyasallarin kümülatif etkilerine Sahip olurlar. Ayrica bulus konusu metotla, azot içeren katyonik bilesen olarak benzalkonyum tuzlari veya setrimit seçilmesi durumunda yer-yüzey dezenfektani; klorhekzidin tuzlari seçilmesi durumunda el ve cilt antiseptigi; biguanid seçilmesi durumunda ise havuz dezenfektani gibi ürünleri stabil halde üretmek mümkündür. The method of the invention has been applied to many industries, especially the medical industry. application form is available. The formulations produced are both stable and hydrogen peroxide with antimicrobial properties, cationic component containing nitrogen and They contain all of the nano silver materials. Thus, the subject of the invention The formulations produced by this method show the cumulative effect of all these antimicrobial chemicals. have their effects. In addition, with the method of the invention, the nitrogen-containing cationic component If benzalkonium salts or cetrimite are selected as the ground-surface disinfectant; hand and skin antiseptic if chlorhexidine salts are chosen; If biguanide is selected, products such as pool disinfectant can be stabilized. possible to produce.

Asagida, bulusun daha iyi anlasilabilmesi için bir sentez yöntemi, sentezlenen formülün stabilizasyon derecesi, kullanim alani ve antimikrobiyal özelligi verilmistir. Below is a synthesis method for a better understanding of the invention. The degree of stabilization, usage area and antimicrobial properties of the formula are given.

Bulus, verilen örnekle sinirli degildir. The invention is not limited to the example given.

Arap zamki ile kaplanmis nano gümüs stok Çözeltisi sentezi 25g deiyonize suyun içerisinde 0,25g arap zamki eklenip karistirilmaya baslanir. Synthesis of nano silver stock solution coated with gum arabic Add 0.25g gum arabic in 25g deionized water and start mixing.

Arap zamki çözündükten sonra bu çözeltiye, 50mMilik gümüs nitrat stok çözeltisinden lml eklenip karistirilir. Daha sonra yavas yavas 50mMilik askorbik asit stok çözeltisinden 5ml eklenir. pH degeri kendiliginden 3,64 olarak ölçülmüstür. 0,5M`lik NaOH çözeltisi eklemek suretiyle pH degeri 4,00°a yükseltilir ve sistem 3 saat karistirilir. Sonrasinda sistem hacmi deiyonize su ile 45ml`ye çikartilir. After dissolving the gum arabic, add 50mM silver nitrate stock to this solution. lml of the solution is added and mixed. Then slowly 50mM ascorbic acid 5ml of the stock solution is added. The pH value was automatically measured as 3.64. By adding 0.5M NaOH solution, the pH value is increased to 4.00° and the system 3 the hour is mixed. Afterwards, the system volume is increased to 45 ml with deionized water.

Ardindan, 0,5Milik NaOH çözeltisi eklemek suretiyle pH degeri 7,00”a yükseltilip, hacim de deiyonize su ile 50ml”ye çikartilir. Böylece, “arap zamki ile kaplanmis nano gümüs stok çözeltisi” sentezlemek için lmM gümüs, 5mM askorbik asit ve 5mg/ml arap zamki kullanilmis olur. Then, the pH value is increased to 7.00 by adding 0.5 Milik NaOH solution, The volume is increased to 50 ml with deionized water. Thus, “coated with gum arabic To synthesize “nano silver stock solution”, lmM silver, 5mM ascorbic acid and 5mg/ml gum arabic is used.

Hidroien peroksit içerikli antimikrobival karisimin üretimi 28,9g deiyonize suya, agirlikça %50ilik hidrojen peroksit sulu çözeltisinden 50 gram eklenip manyetik olarak karistirmaya baslanilir. Karistirrna islemi devam ederken, agirlikça %507lik benzalkonyum klorür sulu çözeltisinden 20 gram, agirlikça %1 °lik sodyum stannat sulu çözeltisinden 1 gram ve yukarida sentezi yapilan “arap zamki ile kaplanmis nano gümüs stok çözeltisi"nden 0,1 gram eklenir. 1 saat Oda sicakliginda karistirildiktan sonra formülasyon filtre kagidindan geçirilerek süzülür. peroksit, lOg benzalkonyum klorür ve 0,1g sodyum stannat kimyasallarina ilaveten; mM askorbik asit, 5 mg/ml arap zamki ve 1 mM gümüs nitrat kullanilarak üretilen Karsilastirmali Örnek 1 Bulus konusu formülasyonla karsilastirmak için yapilan bu örnek sentezde, “arap zamki ile kaplanmis nano gümüs stok çözeltisi” ve kalay tuzu kullanilmamistir. ,0g deiyonize suya, agirlikça %50'lik hidrojen peroksit sulu çözeltisinden 50 gram eklenip manyetik olarak karistirmaya baslanilir. Karistirma islemi devam ederken, agirlikça %50”lik benzalkonyum klorür sulu çözeltisinden 20 gram eklenir. 1 saat oda sicakliginda karistirildiktan sonra formülasyon filtre kâgidindan geçirilerek süzülür. Böylece, IOOg formülasyon içerisinde 659 deiyonize su, 259 hidrojen peroksit ve lOg benzalkonyum klorür bulunur. Production of antimicrobial mixture containing hydroene peroxide 50 grams of hydrogen peroxide aqueous solution of 50% by weight into 28.9g of deionized water added and magnetically mixed. While the Karistrna process continues, 20 grams of 507% by weight benzalkonium chloride aqueous solution, 1% by weight Gum arabic synthesized from sodium stannate aqueous solution 1 gram and above 0.1 grams of nano silver stock solution coated with After mixing at temperature, the formulation is filtered by passing through filter paper. in addition to chemicals peroxide, 10g benzalkonium chloride and 0,1g sodium stannate; Produced using mM ascorbic acid, 5 mg/ml gum arabic and 1 mM silver nitrate Comparative Example 1 In this exemplary synthesis made to compare with the formulation of the invention, Nano silver stock solution coated with gum and tin salt were not used. 50 grams of a 50% by weight hydrogen peroxide aqueous solution to 0,0g deionized water added and magnetically mixed. While the mixing process continues, Add 20 grams of 50% by weight benzalkonium chloride aqueous solution. 1 hour After mixing at room temperature, the formulation is passed through filter paper. is filtered. Thus, 659 deionized water, 259 hydrogen in 100g formulation. peroxide and 10g of benzalkonium chloride.

Stabilite Testleri Bulus konusu yöntemle üretilen “Örnek 1” ve bilinen yöntemlerle üretilen gerçeklestirildi. Bunun için, her iki formülasyondan l0°ar gram, ayri ayri 15ml”lik tüplere konulup agzi kapatildi. Daha sonra her iki örnek de 54 °C sicaklikta 14 gün bekletilmek suretiyle hizlandirilmis yaslandirma testine tabi tutuldu. Yaslandirma sonucunda her ikisinin de hidrojen peroksit oranlari ölçülüp, hidrojen peroksitteki bozulma oranlari hesaplandi. Sonuçlar Tablo l°de verilmistir. Stability Tests "Example 1" produced by the method of the invention and produced by known methods carried out. For this, 10 grams of both formulations and 15 ml separately It was put into the tubes and the mouth was closed. Then, both samples were stored at 54 °C for 14 days. was subjected to accelerated aging test. Aging As a result, the hydrogen peroxide ratios of both were measured and the hydrogen peroxide deterioration rates were calculated. The results are given in Table 1.

Tablo 1: Bulus konusu yöntemle üretilen ”Örnek 1” ve bilinen yöntemlerle üretilen N umune Ismi Peroksit Orani (0/0) Peroksit Orani (%) Kayip Hizlandirilmis stabilite testlerini geçmek için, formülasyonun 54 0C sicaklikta 14 gün bekletilmesi sonucu aktif madde miktarindaki kaybin en fazla %10 olmasi gerekmektedir. Tablo 1`den de görüldügü gibi bulus konusu yöntemle üretilen ”Ömek 1” %3,41”lik (Table 1: ”Example 1” produced by the method of the invention and produced by known methods N sample name Peroxide Ratio (0/0) Peroxide Ratio (%) Loss To pass the accelerated stability tests, the formulation must be maintained at 54 0C for 14 days. maximum 10% loss in the amount of active substance as a result of waiting required. As can be seen from Table 1, produced by the method of the invention, ”Example 1” 3,41% (

Claims

REQUESTS . The invention is a hydrogen peroxide-containing antimicrobial mixture production method. Dissolving gum arabic in water (101 J, adding ascorbic acid to the resulting mixture and dissolving it (102), mixing the silver salt to the resulting mixture (103), providing the pH value required for nano silver synthesis by adding a pH adjuster to the mixture (104) mixing the solution containing nano silver (105 )I nano silver-containing mixture by adding a pH adjuster to achieve the desired pH value (106], then mixing the desired amount of “nano silver stock solution coated with gum arabic” (100) into the “nano silver stock solution coated with gum arabic” hydrogen peroxide solution (201 i , adding nitrogen-containing cationic component to the resulting mixture and mixing (202), mixing the tin salt (203) into the resulting mixture, mixing the liquid component (204), adjusting the mixture to the desired pH value with a pH adjuster (205), removing the particles from the mixture (206), It is characterized by the fact that it consists of process steps. p feature; is used (101). In Istein 1, “Adding ascorbic acid to the resulting mixture and dissolving it” (102) is the process step and its feature is; 0.1-20 grams, preferably 0.1-1.0 grams, more preferably 0.8-1.2 grams of ascorbic acid per liter. . In claim 1, “mixing the silver salt into the resulting mixture” (103) is the process step and its feature is; said silver salt; silver nitrate, silver chloride, silver hydroxide, silver oxide and silver citrate chemicals. Claim 1”Cleki is the process step of “mixing the silver salt into the resulting mixture” (103) and its feature is; The silver ion concentration in the stock solution (106) obtained as a result of the synthesis (100) of nano silver stock solution coated with gum arabic is 0.1-5 mM, preferably 0.5-1.0 mM, more preferably 0.9-1.1 mM. It is the mixing of silver salt to be in the range (103). The following is the process step of “providing the pH value required for nano silver synthesis by adding a pH adjuster to the mixture” (104) and its feature is; the required pH range is 0.5-14, preferably 3-9, more preferably 4-8. In the prompt, “mixing the solution containing nano silver” (105) is the process step and its feature is; The process is to be carried out at a temperature of minus ten to plus one hundred and fifty degrees, preferably at room temperature. In claim 17, “mixing the solution containing nano silver” (105) is the process step and its feature is; The mixing time is 0.1-24 hours, preferably 05-23 hours, more preferably 0.5-2 hours. In claim 1, it is the process step of “providing the desired pH value by adding a pH adjuster to the mixture containing nano silver” (106) and its feature is; pH value to be adjusted

1-14, preferably 4-9, more preferably 6-8. According to claim 1, it is added to the formulation from a stock solution of nano silver coated with gum arabic, including a hydrogen peroxide-containing antimicrobial mixture production method (201). It is the process step of "Mixing the desired amount of nano silver stock solution (100) coated with gum arabic to the hydrogen peroxide solution in claim 1" (201) and its feature is; 0.1% by weight of the concentration of the said hydrogen peroxide solution - According to claim 1, it is a hydrogen peroxide-containing antimicrobial mixture production method. It is the process step of "Adding and mixing nitrogen-containing cationic component to the resulting mixture" in Claim 1, where the ratio of hydrogen peroxide by weight in the final mixture is (202); said nitrogen-containing cationic component is selected from at least one of benzalkonium salts, chlorhexidine salts, polyhexamethylene biguanide, cetrimonium salts and cetrimide chemicals. It is the process step of “Adding and mixing nitrogen-containing cationic component to the mixture formed” (202) in claim 1, and its feature is; wherein said nitrogen-containing cationic component is 0.01-50%, preferably 1-25%, more preferably 8-12%, by weight in the final formulation. It is the process step of "mixing the tin salt to the resulting mixture" in claim 17, and its feature is; said tin salt is selected from at least one of the chemicals sodium stannate, stannous chloride, tin dioxide and tin carbonate. It is the process step of "mixing the tin salt to the resulting mixture" (203) in claim 1, and its feature is; said tin salt is by weight in the final mixture. It is the process step of “Liquid component mixing to the resulting mixture” (204) in Claim 1 and its feature is; Distilled water, preferably deionized water, tap water, isotonic sodium chloride solution, citrate buffer solution, phosphate buffer solution, dimethyl sulfoxide, dimethyl formamide, isopropyl myristate, ethyl alcohol, methyl alcohol, isopropyl alcohol, propylene glycol, dipropylene glycol and polyethylene selected from at least one of the glycol liquid components. According to claim 1, it is a hydrogen peroxide-containing antimicrobial mixture production method and its feature is; In 100g formulation, 64.8g deionized water, 259 hydrogen peroxide, 109 benzalkonium chloride and 0.19 sodium stannate chemicals are used, in addition to 5mM ascorbic acid, 5mg/ml arabic gum and lmM silver nitrate, produced “nano silver stock solution coated with gum arabic” 0 contains lg. According to claim 1, it is a hydrogen peroxide-containing antimicrobial mixture production method and its feature is; If any of the aforementioned "hydrogen peroxide solution", "nitrogen-containing cationic component", "tin salt" and "nano silver stock solution coated with gum arabic" components are desired, after their mixture is prepared in at least one of the liquid components mentioned in claim 17, the mixture can be mixed. that it can be added. It is the process step of “adjusting the mixture to the desired pH value with a pH adjuster” (205) in claim 1, and its feature is; the adjusted pH value is 1-12, preferably 1-8; more preferably in the range of 4-6. According to claim 1, it is a hydrogen peroxide-containing antimicrobial mixture production method and its feature is; in any mentioned pH adjustment process, at least one of the chemicals citric acid, acetic acid, hydrochloric acid, hydrofluoric acid, nitric acid, sulfuric acid, sodium hydroxide, potassium hydroxide, cesium hydroxide and rubidium hydroxide is selected as the pH adjuster. In claim 1, "removal of particles from the mixture" (206) is the process step and its feature is; Purification of particles is carried out by using at least one of the methods of passing through a filter with a pore size of 0.05-10000 um, centrifugation, and resting. . In claim 1, purification of the mixture from particles (206) is the process step and its feature is; It is the removal of other particles that will form during the synthesis, except for nano silver particles. According to claim 1, it is a hydrogen peroxide-containing antimicrobial mixture production method (200), and its feature is; is that the order of operation can be changed as desired.