| Abstract | Tankoslojna kromatografija (TK) učinkovita je, brza i jednostavna metoda analize metalnih iona koja se može lako primijeniti u analizi uzoraka raznih vrsta materijala. Danas ova metoda ima ogromnu primjenu u analizi povijesnih i suvremenih tekstilnih materijala te se koristi kako bi se identificirale i kvantificirale pojedine komponente u uzorku. U povijesnim uzorcima na oslikanim tekstilima TK metoda primjenjuje se najčešće u analizi voskova, smola, proteina i šećera, odnosno prirodnih veziva koji se često nalaze na povijesnim uzorcima. Za razliku od tih materijala, u suvremenim materijalima će se u premazima moći detektirati širok raspon drugih vrsta materijala koji uzorcima definiraju posebna uporabna svojstva. Takvi su materijali i antimikrobno aktivni biorazgradivi polimeri koji u vanjskom sloju sadrže prisutne nanočestice metala i metalnih oksida.
Biorazgradivi polimeri koji imaju antimikrobna svojstva imaju vrlo široku primjenu u medicini i medicinskim materijalima te se koriste od medicinskih tekstilnih materijala (posteljine i ručnika za bolnice) do potrošnih materijala poput zavoja, gaza, i obloga. Polimeri koji nisu proizvedeni tehnologijom dobivanja vlakana i ispredanjem, već drugim postupcima (poput aditivne tehnologije, odnosno 3D tiska) također mogu biti funkcionalizirani premazima s nanočesticama kako bi dobili antimikrobna svojstva. Ti se materijali stoga mogu koristiti kao kateteri, potrošni materijali, prevlake i vrećice.
U ovom je radu TK metoda primijenjena za analizu 64 različita metalna iona koji mogu biti prisutni u antimikrobnoj prevlaci uzoraka koji su pripremljeni u laboratoriju. Testirana je 31 različita vrsta nepokretnih faza (od celuloze, silikagela, poliamida i aluminijevog oksida), te mnogobrojne pokretne faze koje su činili razni razvijači smjesa anorganskih i organskih otapala (acetonitril, acetil aceton, butanol, trietilamin, etilendiaminotetraoctenakislina, klorovodična kiselina, voda i dr.). Tijekom ispitivanja koristilo se 19 različitih smjesa razvijača.
Optimalni sustav koji su detektirani svi metalni ioni sastojao se od silikagela kao nepokretne faze, dok je pokretnu činio razvijač acetonitril: klorovodična kiselina: voda, volumena od 24 mL u volumnom omjeru 60,00: 19,17: 20,83. Detekcija uzoraka obavljena je pomoću UV kabineta te su prilikom detekcije određeni parametri razdvajanja (RF, Rs i drugi) poznatih standardnih otopina metalnih iona, koji su zatim korišteni u detekciji analita kod nepoznatih uzoraka. Nova je metoda primijenjena u analizi vodenih otopina uzoraka koji su imali sadržaj metalnih iona ispod granica detekcije, te je stoga prije kvantificiranja provedena metoda dodavanja poznatog sadržaja standardnih metala u nepoznate uzorke. Na taj je način detektirano željezo, krom i kobalt u tri različita realna uzorka s vrlo visokom ponovljivošću i točnošću analize. |
| Abstract (english) | Thin layer chromatography (TLC) is an efficient, fast and simple method of metal ion analysis that can be easily applied in the analysis of samples of various types of materials. Today, this method has a huge application in the analysis of historical and contemporary textile materials and is used to identify and quantify individual components in a sample. In historical samples on painted textiles, the TLC method is most often used in the analysis of waxes, resins, proteins and sugars, i.e. natural binders that are often found on historical samples. Unlike those materials, in modern materials it is possible to detect a wide range of other types of materials in coatings, which define special usage properties in the samples. Such materials are for example antimicrobially active biodegradable polymers that contain nanoparticles of metals and metal oxides present in the outer layer.
Biodegradable polymers that have antimicrobial properties have a very wide application in medicine and medical materials and are often used as medical textiles (bedding and hospital towels) or consumables such as bandages, gauze, and wound dressings. Polymers that are not produced by fiber production and spinning technology, but by other processes (such as additive technology or 3D printing) can also be functionalized with nanoparticle coatings to obtain antimicrobial properties. These materials can therefore be used as catheters, consumables, coatings and bags.
In this work, the TLC method was applied to analyze 64 different metal ions in the antimicrobial coating of samples prepared in the laboratory. The stationary phases tested were 31 different preprepared cellulose and silica gel, polyamid and Al2O3, and the mobile phase consisted of various developers containing mixtures of inorganic and organic solvents (such as acetonitrile, acetyl acetone, butanol, triethylamine, ethylenediaminotetraacetic acid, hydrochloric acid, water, etc.). During the experiment, 19 different solvent mixtures were used.
The optimal system that detected all metal ions consisted of silica gel as a stationary phase, while the mobile phase contained a solvent mixture of acetonitrile: hydrochloric acid: water, a volume of 24 mL in a volume ratio of 60.00: 19.17: 20.83. Sample detection was performed using a UV cabinet and during the detection the separation parameters (RF, Rs and others) of known standard solutions of metal ions were determined, which were then used in the detection of analytes in an unknown samples. The new method was applied in the analysis of aqueous solutions of samples that had metal ion content below the detection limits, and therefore, before quantification, a method of adding a known standard metal content to unknown samples was performed. In this way, iron, chromium and cobalt were detected in three different real samples with very high repeatability and accuracy of the analysis. |
| Study programme | Title: Textile Technology and Engineering; specializations in: Clothing Engineering, Textile Design and Management, Industrial Textile Design, Industrial Clothing Design, Textile Chemistry, Materials and Ecology, Textile Chemistry, Materials and Ecology
Course: Textile Chemistry, Materials and Ecology
Study programme type: university
Study level: graduate
Academic / professional title: magistar/magistra inženjer/inženjerka tekstilne tehnologije i inženjerstva (magistar/magistra inženjer/inženjerka tekstilne tehnologije i inženjerstva) |
