izotermalna titracijskamikrokalorimetrija(itc)
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1 P / µw t / min Polielektroliti u otopini i na površini Prema IUPAC-u: Polielektroliti - makromolekule kod koje je prisutan znatan udjel konstitucijskih(gradivnih) jedinica koje sadrže ionske i/ili lako ionizirajuće skupine. suprotno nabijeni polielektroliti u otopini izotermalna titracijska mikrokalorimetrija Na + PSS M w = 7 g mol -1 izotermalna titracijskamikrokalorimetrija(itc) G. E. Boyd, D. P. Wilson, G. S Manning, J. Phys. Chem. 8 (1976) 88 mikrokalorimetrijskatitracija vodene otopine G. Vesnaver, Z. Kranjc, C. Pohar, J. Škerjanc, J. Phys. Chem. 91 (1987) 3845 Na + PSS vodenom otopinom CsNO 3 mikrokalorimetrijska titracija vodene otopine Na + PSS - vodenim otopinama različitih soli H / µj Li H / µj Li Na n (M + ) / n m n (M + ) / n m H / µj Li H / µj Li Na Na K n (M + ) / n m Rb K n (M + ) / n m 1
2 n (M + ) / n m n(m + ) / n m mikrokalorimetrijska titracija vodene otopine Na + PSS - vodenim otopinama različitih soli H / µj 3 2 Li 1 4 a Rb 1-1 Na K potenciometrijska titracija Li Cs -2-3 Rb Cs H /mj Na K Rb Cs Me 4 N Et 4 N hydr H/ kj mol 1 kompleksiranje polielektrolita (polikationa i polianiona) u otopini Nastajanje polielektrolitnih kompleksa elektrostatske interakcije polielektrolitni kompleksi (polyelectrolyte complexes) topljivi kompleksi izdvajanje faze (phase separation) istraživali Voorn, Bungeberg de Jong i Michaels u Colloid Science, H. R. Kruyt, Ed. (Elsevier Publishing Company, Amsterdam, 1949) vol. II, pp Polielektroliti u otopini Nastajanje polielektrolitnih kompleksa uz otpuštanje kationa i aniona koji se homogeno raspoređuju u otopini Miješanje suprotno nabijenih homopolimera, utjecaj količinskog udjela jedne komponente I c topljivi kompleksi topljivi kompleksi izdvajanje faze f + 1 Suvišak pozitivnog naboja - topljivi kompleksi Nastajanje netopljivih agregata količinski udjel PAA Suvišak negativnog naboja - topljivi kompleksi 2
3 .95.9 M n AMA = 2 g/mol (13 monomera) M n PAA = 11 g/mol (158 monomera) bistra otopina Fizikalne kemije kompleksnih micela (Complex Micelles) miješanje blok-kopolimera različitih naboja polyion complex micelles c(nacl)/mol / l.85 razdvajanje faza A. Harada and K. Kataoka, Science, 283 (1999) 65. A. Harada and K. Kataoka, Macromolecules, 28 (1995) c(polimer)/g/l Diblok-kopolimer Neutralna, hidrofilna kruna P-AMA-(GMA) Poli(di-metil-Amino-etil-MetAkrilat)-(kopoli(Gliceril-MetAkrilat)) Nenabijeni, hidrofilni blok Kationski blok C CH 2 C O n O C CH 2 C O O m CH 2 HC-OH CH 2 HC-OH N H 2C-OH Različiti omjeri duljine blokova (M w,total = konst.) Neutralna hidrofobna jezgra Anionski homopolimer complex coacervation core micelles ph, ionska jakost, omjer mješanja, duljina blokova, itd... PAA PoliAcrylic Acid CH CH 2 C OH O Različite molekulske mase PMA Poly Methacrylic Acid C CH 2 C O OH Različite molekulske mase Smjesa homopolielektrolita i suprotno nabijenog diblok-kopolimera, utjecaj omjera miješanja 7 6 Utjecaj odnosa duljine blokova diblok-kopolimera Mutna otopina, makroskopsko razdvajanje faza Bistra otopina, stabilne micele Bistra otopina, nema interakcija 5 Size (nm) Suvišak pozitivnog naboja, topljivi kompleksi Izoelektrična smjesa Množinski udjel PAA Suvišak negativnog naboja, topljivi kompleksi 1 PAA M w mm NaNO Množinski udjel GMA u diblok-kopolimeru 3
4 36 34 Množinski udjel PAA/AMA,877 5 mm NaNO 3 Mw PAA 1361 P-AMA-GMA 1:3 Janusove micele R (nm) Izoelektrična točka ph iep = 5.8 Scattering Intensity (a.u.) miješanje blok-kopolimera različitih naboja polyion complex micelles amfifilni diblok (triblok) kopolimeri Janusove micele ph ( - ) Janus Janusove micele hidrofobna PS polukruna (hemicorona) hidrofilna PMMA polukruna (hemicorona) rimski bog ulaza i vrata, početka i kraja R. Erhardt et al, Macromolecules, 34 (21) 169. R. Erhardt et al, J. Am. Chem. Soc., 125 (23) 326. Janusove micele cross-linking prekursor: polistiren-blok-polibutadien-blok-poli(metil metakrilat) (SBM) triblok kopolimer sintetiziran sekvencijalnom anionskom polimerizacijom cross-linking metoda - reaktant S 2 Cl 2 4
5 Janusove micele Janusove micele karakterizacija: Transmission Electron Microscopy (TEM) Multi-Angle Laser Light Scattering Gel Permeation Cromatography (MALLS-GPC) Confocal Fluorescence Correlation Spectroscopy (FCS) na svaku PB jezgru vezano 13 ± 5 lanaca radijus procijenjen na 11,4 ±,8 nm Janusove micele nastajanje supermicela u otopini tvore superstrukture orijentirane prema površini priprava raznih supramolekularnih objekata iznad kritične agregacijske koncentracije (,3 g/l) nastaju u vodenoj otopini (uz NaCl) sferne superstrukture ( supermicele ) od oko 3 PS-PMAA micela radijusa 4-6 nm. primjena nosači lijekova (drug carriers) ugradnja hidrofobnih anti-tumorskih lijekova u jezgru i njihova dostava do tumora Block copolymer micelles for gene therapy Transfection of plasmid DNA using diblock copolymer. DNA is released inside the cytosol and appears in the nucleus to express a desired protein. Forster and M. Konrad, J. Mater. Chem., 23 5
6 Janus beads polimeri na površini; adsorpcija polimera parcijalna hidrofobna modifikacija staklenih sfernih čestica C. Casagrande and M. Veyssié, C. R. Acad. Sci (Paris) II 36 (1988) višesloj (multilayer)? nastaju naizmjeničnom adsorpcijom polikationa i polianiona na čvrstu površinu najčešća metoda naizmjenično uranjanje u otopinu polielektrolita intenzivno istraživan posljednjih petnaestak godina (preko 1 radova godišnje) istražuju se uglavnom jaki polielektroliti polikationi i polianioni; ponašanje na površini adsorpcija polielektrolita na kovinskim oksidima izmjenično dodavanje pozitivno i negativno nabijenih polielektrolita nastajanje višesloja na površini metalnog oksida izrastanje višesloja je karakterizirano porastom adsorbirane mase metoda praćenja reflektometrija polyelectrolyte multilayers 6
7 otvorena pitanja eksperimentalne metode: ponašanje slabih polielektrolita mehanizam nastajanja višeslojeva polielektrolitni višeslojevisu ravnotežne strukture? eksponencijalni vs. linearni rast Elipsometrija Optička reflektometrija Quartz crystal microbalance(qcm) Optical vaweguide lightmode spectroscopy Surface plasmon resonance spectroscopy Neutron reflectometry FTIR-IR, AFM, itd, itd... optička reflektometrija P-AMA Poli(di-metil-Amino-etil-MetAkrilat) C CH 2 C O n O CH 2 CH 2 Mw= 2 kg/mol Ms= 157 g/mol N PAA Poli Akrilna kiselina (Acid) CH CH 2 C O OH Mw= 12.5 kg/mol Ms= 72 g/mol polielektrolitni višeslojevi (Polyelectrolyte Multilayers) mm 3,5 3,.6 2,5 2, 1,5 polikation polianion.4 1,,5.2 AMA, -,
8 mm.8 2 mm PAA.2 AMA mm.8 2 mm PAA AMA mm 4 2 mm PAA
9 mm mm 2 mm 5 mm 2 mm c s L L S L c cr AFM mjerenja usporedba između uzoraka pripremljenih pri mm i 5 mm contact mode AFM G f + 1 c g mm 2 5 mm
10 otvorena pitanja ponašanje slabih polielektrolita mehanizam nastajanja višeslojeva polielektrolitni višeslojevisu ravnotežne strukture? eksponencijalni vs. linearni rast eksponencijalni vs. linearni rast eksponencijalni vs. linearni rast linearni rast 8 eksponencijalni rast eksponencijalni vs. linearni rast eksponencijalni vs. linearni rast Faktori koji utječu na tip rasta: eksponencijalni kemijska priroda polielektrolitnog para vrsta dodanog elektrolita linearni ionska jakost 2 1 temperatura metoda priprave 1
11 year adsorpcija BSA na prethodno formirani polielektrolitni višesloj polielektrolitne četke (Polyelectrolyte Brushes) BSA 2. BSA PSS PAH 1. PAH PSS PAH PAH t /s t /s g/L,5g/L,75g/L BSA PAH.5 PSS PAH t/s Biomedicine andpharmaceuticalindustry Surface modification(thickness, charge, etc ) Drug delivery polyelectrolyte multilayers- applications Formation of stimuli responsive systems(e.g. mechanical, temperature, ph) Surfaces with antibacterial properties Zeta potential (mv) adhesion of bacteria on polyelectrolyte multilayers 3, 2, 1,, , -2, Number of layers number of documents number of publication per year: antimicrobial properties of polyelectrolyte multilayers PAH/PSS multilayer adhesion of bacteria Pseudomonas aeruginosa on PAH/PSSmultilayer (SEM). (A) five layers with positive terminating layer (PAH) (B) six layers with negative terminating layer (PSS) adhesion of bacteria onprotein-terminating polyelectrolyte multilayers Fraction of the multilayer surface covered with P. aeruginosa PAH as terminating PSS as layer (5 layers) terminating layer (6 layers) 2.4 % ± 4.8 % 9. % ± 3.1 % Lysozyme as BSA as Glucanase as terminating terminating terminating layer (5 layers) layer (5 layers) layer (5 layers) Contact angle 63.2 ± ± ± 9.4 Roughness/µm.12 ±..72 ±..18 ±.6 z-potential/mv 2.1 ± ± ±.4 Contact angle 48.9 ± ± 5. Roughness.17 µm ±.4 µm.19 µm ±.6 µm 11
12 adhesion of bacteria on protein-terminating polyelectrolyte multilayers adhesion of bacteria on protein-terminating polyelectrolyte multilayers lysozyme BSA Two types of bacteria: Pseudomonas aeruginosa - left Escherichia Coli - right glucanase šuplje sfere 12
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