Solid-state CPMAS NMR Research Articles

Drug release profile of phenytoin-loaded starch-based biomaterials incorporating hierarchical microparticles with photothermal effects

This study aimed to synthesize phenytoin (PHT)-loaded water chestnut starch-based biomaterials and evaluate their drug release kinetics for use in transdermal drug delivery systems for antiepileptic therapy. Hierarchical microparticles (HMPs) extracted from human hair were also used to improve the PHT release efficiency. The physicochemical characteristics of PHT, HMPs, and the prepared biomaterials were evaluated by physical properties, antimicrobial activities, FE-SEM, FT-IR, XRD, 1H NMR, and 13C CPMAS solid-state NMR. The photothermal effect and the PHT release profile were confirmed through 808 nm NIR laser irradiation. After 30 min of the laser exposure, the temperature of the HMP-added biomaterials increased by 1.50–1.59 times compared to that of without the HMPs. PHT release in buffers and artificial skin test under NIR laser irradiation enhanced by 1.20–1.85 times owing to the photothermal effect. The release kinetics in pH buffer and artificial skin were determined using the Fickian diffusion and Korsmeyer-Peppas models. Additionally, to verify the transdermal penetration of PHT, drug-release simulations were conducted using rhodamine B in agar blocks and pig ears. The results implied that the photothermal effect of the HMPs enhanced the penetration of the drug.

Ionothermal Carbonization of Sugarcane Bagasse in 1-Alkyl-3-methylimidazolium Ionic Liquids: Insights into the Role of the Chloroferrate Anion.

We report the ionothermal carbonization (ITC) of lignocellulosic biomass in imidazolium tetrachloroferrate ionic liquids (ILs) as an advantageous approach for the preparation of nanostructured carbonaceous materials, namely, ionochars. In a previous study, we investigated the role of the imidazolium cation and demonstrated the possibility of controlling both the textural and morphological properties of ionochars by cation engineering. Although essential for providing intermediate Lewis acidity and relatively high thermal stability, the role of the chloroferrate anion is still open to debate. Herein, we investigated the ITC of sugarcane bagasse and its main component, cellulose, in 1-alkyl-3-methylimidazolium ILs with different chloroferrate anions. We identified anionic speciation and its impact on the properties of the IL by Raman spectroscopy, thermogravimetric analysis, and differential scanning calorimetry. The obtained ionochars were characterized by gas physisorption, electron microscopy, Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, and 13C solid-state CP-MAS NMR spectroscopy. We show that the anionic species have a predominant impact on the textural and morphological properties of the ionochars.

Tailoring pore size of mesoporous silica and organosilica using biodegradable pentablock copolymer templates via EISA process

In this work, we have designed unique poly(lactic acid-co-glycolic acid)-b-poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide)-b-poly(lactic acid-co-glycolic acid) pentablock copolymers using Pluronic F68 and F108 triblock copolymers as macroinitiators. The poly(lactic acid-co-glycolic acid) (PLGA) blocks were attached as glycolide and lactide monomers at the both ends of each F68 and F108 triblock copolymer. The molecular weights and the block fractions were confirmed by gel permeation chromatography (GPC) and proton nuclear magnetic resonance (1H NMR) for the four kinds of pentablock copolymers. Using these pentablock copolymers as templates, we synthesized mesoporous ethane-silicas as well as silicas by the evaporation-induced self-assembly (EISA) method. 1,2-bis(triethoxysily)ethane (BTEE) were used as an organosilica precursor. The mesoporous ethane-silica samples were characterized using synchrotron small angle X-ray scattering (SAXS), nitrogen sorption experiments, transmission electron microscopy (TEM), and solid-state 29Si CP-MAS NMR. Based on the experimental results, it was confirmed that the porosity and pore diameter can be varied with the PLGA weight fraction of the pentablock copolymer. It is due to the PLGA block in polymer forming the hydrophobic domain in micelles, which leads to the formation of increased pore size over 20 nm without any additive pore expander. In addition, it seems that as the organosilica precursor increases, the association number of block copolymers forming one micelle decreases, resulting in a decrease in pore size. In summary, the polymer template plays a vital part in tuning the structure of the mesoporous ethane-silica samples. Thus, the development of synthetic method of mesoporous organosilica materials using polymer templates with different topology is still challenging and can endow the unique structure and property for mesoporous organosilica for future applications.

Amphiphilic titania Janus nanoparticles containing ionic groups prepared in oil-water Pickering emulsion.

Titania nanoparticles with a diameter of 8 nm underwent an anisotropic modification using apolar 6-bromohexylphosphonic acid and cationic polar N,N,N-trimethyl-6-phosphonohexan-1-aminium bromide. The Janus modification was achieved through a straightforward one-step Pickering emulsion approach using toluene-water mixtures. The resulting Janus particles were compared with isotropically and statistically modified titania particles, where either a single coupling agent is attached to the surface or both coupling agents are assembled over the surface randomly, respectively. The covalent binding of the phosphonic acids to the titania surface was confirmed by FTIR and 31P solid-state CP-MAS NMR analyses. The grafting density was assessed using TGA, elemental analysis, and ICP-MS, revealing grafting densities of 0.1 mmol g-1 to 0.5 mmol g-1 for the cationic coupling agent and 1.2 mmol g-1 to 1.5 mmol g-1 for the apolar coupling agent, respectively. ζ-Potential titration measurements of both pristine and modified particles revealed isoelectric points at pH 4.5 to 9.3, depending on the type of modification. The ability of the particles to stabilize Pickering emulsions was tested under various conditions, with statistically and Janus-modified particles demonstrating a significant increase in stabilization compared to their isotropically modified counterparts. Furthermore, Janus particles were deposited onto glass substrates by a simple layer-by-layer approach. Through the self-assembly of these Janus particles, the glass substrate's properties could be tailored from hydrophilic to hydrophobic to hydrophilic, depending on the dipping cycle.

17-β-Estradiol-β-Cyclodextrin Complex as Solid: Synthesis, Structural and Physicochemical Characterization.

17-β-estradiol (EST) is the most potent form of naturally occurring estrogens; therefore, it has found a wide pharmaceutical application. The major problem associated with the use of EST is its very low water solubility, resulting in poor oral bioavailability. To overcome this drawback, a complexation with cyclodextrins (CD) has been suggested as a solution. In this work, the host-guest inclusion complex between the ß-CD and EST has been prepared using four different methods. The obtained samples have been deeply characterized using 13C CP MAS solid state NMR, PXRD, FT-IR, TGA, DSC, and SEM. Using SCXRD, the crystal structure of the complex has been determined, being to the best of our knowledge the first solved crystal structure of an estrogen/CD complex. The periodic DFT calculations of NMR properties using GIPAW were found to be particularly helpful in the analysis of disorder in the solid state and interpretation of experimental NMR results. This work highlights the importance of a combined ssNMR/SCXRD approach to studying the structure of the inclusion complexes formed by cyclodextrins.

Copper(II)-Incorporated Porphyrin-Based Porous Organic Polymer for a Nonenzymatic Electrochemical Glucose Sensor.

To date, the fabrication of multifunctional nanoplatforms based on a porous organic polymer for electrochemical sensing of biorelevant molecules has received considerable attention in the search for a more active, robust, and sensitive electrocatalyst. Here, in this report, we have developed a new porous organic polymer based on porphyrin (TEG-POR) from a polycondensation reaction between a triethylene glycol-linked dialdehyde and pyrrole. The Cu(II) complex of the polymer Cu-TEG-POR shows high sensitivity and a low detection limit for glucose electro-oxidation in an alkaline medium. The characterization of the as-synthesized polymer was done by thermogravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, and 13C CP-MAS solid-state NMR. The N2 adsorption/desorption isotherm was carried out at 77 K to analyze the porous property. TEG-POR and Cu-TEG-POR both show excellent thermal stability. The Cu-TEG-POR-modified GC electrode shows a low detection limit (LOD) value of 0.9 μM and a wide linear range (0.001-1.3 mM) with a sensitivity of 415.8 μA mM-1 cm-2 toward electrochemical glucose sensing. The interference of the modified electrode from ascorbic acid, dopamine, NaCl, uric acid, fructose, sucrose, and cysteine was insignificant. Cu-TEG-POR exhibits acceptable recovery for blood glucose detection (97.25-104%), suggesting its scope in the future for selective and sensitive nonenzymatic glucose detection in human blood.

In situ preparation of compounds using silanized mPEG inspired by talc-like structures.

Composite materials show improved properties compared to pristine materials, in particular when the filler is dispersed homogeneously in the matrix. For polymer-clay composites, different strategies exist to improve clay mineral dispersion in the polymer matrix. In this study, an innovative approach is suggested which consists of forming a talc-like structure directly in a polymer matrix using a silanized polymer as the silicon source. Poly(ethylene glycol) methyl ether of different average molar masses (Mn = 350, 500, 750, 1900 g mol-1) were functionalized with (3-isocyanatopropyl)triethoxysilane and added to the ethanolic solutions of magnesium nitrate. 1H-29Si CPMAS solid state NMR experiments revealed partial condensation of silane compounds, and FTIR analysis confirmed the presence of both Si-O and Mg-O bonds, but an additional proof of the Si-O-Mg bond is needed to prove the formation of such a structure.

Tuning the Cu/SiO2 wettability features for bio-derived platform molecules valorization

A simple organosilane-grafting protocol has been used for the preparation of a copper heterogeneous catalyst with tunable wettability properties. A series of Cu/SiO2 trietoxyoctylsilane-modified systems with gradually reduced alcoholphilicity has been used in the hydrogenation of the platform molecule γ-valerolactone into 1,4-pentandiol, a valuable biobased monomer. The surface modification obtained with the proposed procedure allows to significantly increase the selectivity (99%) of the process and therefore the yield (80%) in the desired diol. Several characterization techniques (static contact angle, ATR, CP-MAS solid state NMR, pyridine and ammonia adsorption) put in light the modification of the surface while preserving the hydrogenation activity of the metallic phase. The results obtained show the opportunity given by this simple catalytic system in combining the activity of the copper phase and the modified polarity of the surface.

Ambiguous structure determination from powder data: four different structural models of 4,11-di-fluoro-quinacridone with similar X-ray powder patterns, fit to the PDF, SSNMR and DFT-D.

Four different structural models, which all fit the same X-ray powder pattern, were obtained in the structure determination of 4,11-di-fluoro-quinacridone (C20H10N2O2F2) from unindexed X-ray powder data by a global fit. The models differ in their lattice parameters, space groups, Z, Z', molecular packing and hydrogen bond patterns. The molecules form a criss-cross pattern in models A and B, a layer structure built from chains in model C and a criss-cross arrangement of dimers in model D. Nevertheless, all models give a good Rietveld fit to the experimental powder pattern with acceptable R-values. All molecular geometries are reliable, except for model D, which is slightly distorted. All structures are crystallochemically plausible, concerning density, hydrogen bonds, intermolecular distances etc. All models passed the checkCIF test without major problems; only in model A a missed symmetry was detected. All structures could have probably been published, although 3 of the 4 structures were wrong. The investigation, which of the four structures is actually the correct one, was challenging. Six methods were used: (1) Rietveld refinements, (2) fit of the crystal structures to the pair distribution function (PDF) including the refinement of lattice parameters and atomic coordinates, (3) evaluation of the colour, (4) lattice-energy minimizations with force fields, (5) lattice-energy minimizations by two dispersion-corrected density functional theory methods, and (6) multinuclear CPMAS solid-state NMR spectroscopy (1H, 13C, 19F) including the comparison of calculated and experimental chemical shifts. All in all, model B (perhaps with some disorder) can probably be considered to be the correct one. This work shows that a structure determination from limited-quality powder data may result in totally different structural models, which all may be correct or wrong, even if they are chemically sensible and give a good Rietveld refinement. Additionally, the work is an excellent example that the refinement of an organic crystal structure can be successfully performed by a fit to the PDF, and the combination of computed and experimental solid-state NMR chemical shifts can provide further information for the selection of the most reliable structure among several possibilities.

Two structural types of dithiocarbamato-chlorido complexes of mercury(II): Preparation, supramolecular self-assembly, solid-state 13C and 15N NMR characterisation and thermal behaviour of pseudo-polymeric compounds of [Hg2(S2CNBu2)2Cl2] and [Hg4(S2CNiBu2)6][Hg2Cl6

Two new crystalline dithiocarbamato-chlorido complexes of mercury(II), [Hg2{S2CN(C4H9)2}2Cl2] (1) and [Hg4{S2CN(iso-C4H9)2}6][Hg2Cl6] (2), have been prepared and chemically identified by solution (1H, 13C) NMR and solid-state (13C, 15N) CP-MAS NMR and FT-IR spectroscopy. The crystal, molecular and supramolecular structures of these compounds were established using single-crystal X-ray diffraction (XRD) analysis. The obtained complexes reveal two principally different types of structural organisation. In the structure of the former neutral complex, there are two isomeric doubly-bridged binuclear molecules [Hg2(S2CNBu2)2Cl2] (‘A’ and ‘B’), whereas the latter compound comprises two ionic structural moieties: the tetranuclear cation [Hg4(S2CNiBu2)6]2+ and the binuclear anion [Hg2Cl6]2−. In both ionic units, pairs of iBu2Dtc or chloride ligands, which perform a bridging structural function, combine with neighbouring mercury atoms. In turn, intermolecular/interionic secondary interactions Hg···S/Hg···Cl are involved in the formation of supramolecular structures of complexes 1/2, yielding pseudo-polymeric chains of (···‘A’···‘B’···)n/(···[Hg4(S2CNiBu2)6]···[Hg2Cl6]···)n, which exhibit alternation of isomeric molecules of 1/ionic moieties of 2 along their lengths. Despite the significant structural difference between the above complexes, we established, using simultaneous thermal analysis (STA), that both exhibit very similar thermal behaviour. Moreover, during the thermal transformations of both compounds 1 and 2, the same two substances are generated: HgCl2 and HgS.

Interactions Between Amyloid-β (1-42) and Hydroxyapatite-Cholesterol Spherules Associated with Age-Related Macular Degeneration.

Drusen deposition on sub-retinal pigment epithelium is the causal factor for age-related macular degeneration for the old-aged individuals. These deposits contain hydroxyapatite-cholesterol spherules on which several proteins and lipids accumulate to cover the retina and choroid, causing blurred vision and blindness. Amyloid-β, the known culprit in Alzheimer's disease, is one among the few major proteins known to occur in these deposits. In the present article, we report preliminary analyses of interactions between amyloid-β and hydroxyapatite-cholesterol composites using Thioflavin-T binding kinetics, solid-state NMR and transmission electron microscopy (TEM). Thioflavin-T fluorescence kinetics shows that amyloid-β (1-42) aggregates only under certain conditions of concentration of cholesterol in the hydroxyapatite-cholesterol composites prepared by two different methods. These results were confirmed by 1D 13C CPMAS solid-state NMR. TEM imaging revealed that there is an exposure of the cholesterol surface in the composites prepared by sonication method. These imaging experiments explain the dependence of aggregation kinetics on the exposure and availability of cholesterol surface in the composites to a certain extent.

A novel silver(I) di-iso-butyldithiocarbamate: Unusually complicated 1-D polymeric structure, multiple ligand-supported Ag–Ag interactions and its capability to bind gold(III). Preparation, structural organisation and (13C, 15N) CP-MAS NMR of [Ag6(S2CNiBu2)6]n and [Au(S2CNiBu2)2][AgCl2

We have synthesised three new complexes of [Ag6{S2CN(iso-C4H9)2}6]n (1), [Au{S2CN(iso-C4H9)2}2][AgCl2] (2) and [Au{S2CN(iso-C4H9)2}2][Ag0.69Au0.31Cl2] (3), chemically identified these compounds using solution (1H, 13C) and solid-state (13C, 15N) CP-MAS NMR and FT-IR spectroscopy, and structurally characterised them by single-crystal X-ray diffraction analysis. There are six structurally inequivalent silver(I) centres in the former compound, whose unusually complicated, monodimensional polymeric structure is generally stabilised by six unequal iBuDtc ligands acting as bridges, along with numerous ligand-supported Ag–Ag interactions. Studying the capability of the precipitated AgiBuDtc to bind gold(III) from a [AuCl4]–/5.15 M NaCl solution, the double pseudo-polymeric heterometallic dithiocarbamato-chlorido complexes 2 and 3 were successfully obtained as individual fixation modes of gold to the solid phase. In the self-assembly of a bidimensional supramolecular structure of the latter two compounds, numerous interionic secondary bonds (Au···S, Ag···S and S···Cl), the anagostic HC···Ag interactions and the Cl···HC hydrogen bonds play a key role. To study the thermal behaviour of crystalline compounds 1 and 2, we additionally used simultaneous thermal analysis (STA). During the thermolysis of 1/2, the formation of Ag2S/AgCl,Au0 was supported, respectively, by energy dispersive X-ray (EDX) spectroscopy, while the dispersity and morphology of residual substances were studied using scanning electron microscopy.

A three-dimensional covalent organic framework with turn-on luminescence for molecular decoding of volatile organic compounds

A rare example of fluorescence sensing was realized by 3D covalent organic framework (3D-LCOF) as molecular decoder for VOCs identification based on turn-on luminescence. 3D-LCOF was synthesized via [T4 + C4] imine condensation of TFBM and PyTTA. The structure of 3D-LCOF was confirmed by FT-IR, 13C CP-MAS solid state NMR and Powder X-ray diffraction. Structural simulation revealed that 3D-LCOF had three-dimensional pts topological structure with quadrilateral pores. 3D-LCOF present high BET surface area of 875 m2 g−1 with an average pore size of ∼0.85 nm. Due to the conjugated skeleton and unique porous structure, 3D-LCOF can accurately distinguish and locate more than twenty kinds of VOCs, including aromatic, alcohol-based and other industrial common VOCs. Furthermore, 3D-LCOF was also very efficient for the ultra-low detection of nitro pesticides at ppm levels (0.056 ppm for NA, 0.15 ppm for DCN). This study sheds lights on the design of porous framework sensor and expand the utilization of COF materials.

Structural insight into the photoinduced E→Z isomerisation of cinnamate embedded in ZnAl and MgAl layered double hydroxides

Hybrid E-cinnamate- and Z-cinnamate-intercalated layered double hydroxides (Mg2Al- E- or Z-Cin LDH and Zn2Al- E- or Z-Cin LDH) were prepared by the co-precipitation method, and structurally characterised by powder X-ray diffractometry, UV–Vis, FT-IR and 13C CP MAS solid-state NMR spectroscopies to gain further insights on the arrangement of the organic anions in the interlamellar domain. UV light irradiation induced E–Z isomerisation reaction was subsequently attempted in the solid state and in methanolic suspension. Although reaction was observed in the solid state; however, E–Z isomerisation mainly occurred in the slurry phase. The fact that there was no isomerisation when E-Cin was solely adsorbed on the surfaces of pristine LDHs highlights that the reaction took place in the interlayer region. Similar behaviour was observed for the two LDH compositions proving that the LDH structures acted as nanoreactors confining the photoinduced isomerisation.

Manipulation on microstructure of MFI membranes by binary structure directing agents

Abstract The good quality pure-silica MFI zeolite membrane with hydrophobic surface was fabricated by the addition of TBABr in “TEOS-TPAOH-H2O” synthesis solution. The effects of TBABr on PV performance and the microstructure of MFI membranes were explored by pervaporation, single-component gas permeation, water contact angle, scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS) and 13C solid state CP MAS NMR. It was found that small amounts of TBABr could accelerate the growth and contribute to compact membranes with high bulk Si/Al ratio and good hydrophobic surface, hence resulting in better pervaporation performance. Excessive amounts of TBABr would interfere the crystallization and result in lower pervaporation performance. For example, when the TBABr/Si ratio increased to 0.01 from 0 with the TPAOH/Si ratio of 0.09, the membrane separation factor was increased from 35 to 59 with the flux of 1.85 kg m−2 h−1 for 5 wt% of ethanol/water mixtures at 60 °C.

C-N cross coupling: Novel approach towards effective aryl secondary amines modification on nanodiamond surface

Present work elaborates utilization of CN cross coupling reaction for the first time on a nanoscale level. An array of aryl halides carrying nitro, trifluoro, azido or aryl groups were coupled effectively with amine modified nanodiamond particles (ND-NH2) leading to the formation of secondary aromatic amine functionalized nanodiamond. Successful fabrication of organic groups on to the nanodiamond surface was established initially using FT-IR (Fourier transform infrared spectroscopy), then confirmed by 13C CP-MAS solid state NMR spectroscopy and elemental analysis. X-ray diffractometer (XRD) and Transmission electron microscopy (TEM) findings disclose that the surface modification do not alter the crystalline structure of nanodiamond. Furthermore, thermal stabilities and effective surface loadings for the functionalized NDs were investigated by thermogravimetric analysis. X-ray photoelectron spectroscopy (XPS) analysis exhibited the true perspective regarding elemental composition of functionalized NDs and corroborated the grafting indicating good yield of the reaction. In addition, attachment of hydrophobic groups augmented their dispersion in organic solvents with reduction in aggregation.

New chitin derivatives and their Schottky diodes: Synthesis and characterization

First, chitin was reacted with 4,5-dichlorophthalic acid and diphenic acid, and thus two new chitin derivatives (C45DA and CDA) were synthesized. Then, C45DA and CDA were characterized by various spectroscopies and techniques (FTIR, 13C CP-MAS solid-state NMR, XRPD, SEM, and TGA/DTA). Besides, some electrical properties of C45DA were measured. After the characterization process, the Schottky diodes of C45DA and CDA were made. It was determined that these diodes showed photodiode characteristics at the same time. Later on, both electrical properties ( ϕb, n, and Rs) and photoelectrical properties ( I Illumination/ I Dark, I SC, and V OC) of these diodes were determined.

Schottky Diodes Based on the New Chitin Derivatives

New chitin derivatives were synthesized by the reactions of chitin with o-acetylsalicyloyl chloride and phthaloyl chloride and their structure was characterized by FTIR and 13C CP-MAS solid-state NMR spectroscopy and X-ray powder diffraction technique. Also, the thermal and surface properties of the chitin derivatives were investigated by thermogravimetric analysis and a scanning electron microscope. In addition, some electrical properties of the polymers were determined using Hall effect technique. Then, the Schottky diodes were fabricated by the formation of interlayers of chitin derivatives between Au metal and n-Si semiconductor, and the electrical and photoelectrical properties of the diodes were determined.

Synthesis of high silica zeolites using a combination of pyrrolidine and tetramethylammonium as template

High silica ZSM-39 (MTN structure), ZSM-35 (FER structure) and ZSM-5(MFI structure) zeolites were successfully synthesized using pyrrolidine and tetramethylammonium as structure directing agents (SDAs), in absence of alkaline cation and fluoride medium. The effect of the relative amount of tetramethylammonium and pyrrolidine, and Si/Al molar ratio on the crystalline phases was investigated. All structures could be synthesized using pyrrolidine as solely SDA. On the other hand, when a mixed template system being used, the crystallization was accelerated by a factor of 2 times, TMA+ would then play a generally beneficial but structurally non-specific role in the crystallization spicily for FER and MFI zeolites. The obtained products were characterized by XRD, 13C solid-state CP MAS NMR, TGA and SEM techniques. The XRD patterns confirmed the formation of pure zeolites with high crystallinity.13C CP MAS NMR spectroscopy confirmed the incorporation of pyrrolidine and tetramethylammonium in the structure of Al-ZSM-5 and Al-ZSM-35 zeolites. These two kinds of SDAs played a cooperative role in the crystallization of these zeolites. The role of pyrrolidine was to provide the initial nucleation and tetramethylammonium to provide both space-filling and basicity capacities.

Biofunctionalization of Nano Channels by Direct In-Pore Solid-Phase Peptide Synthesis.

Diatom biosilica are highly complex inorganic/organic hybrid materials. To get deeper insights on their structure at a molecular level, model systems that mimic the complex natural compounds were synthesized and characterized. A simple and efficient peptide immobilization strategy was developed, which uses a well-ordered porous silica material as a support and commercially available Fmoc-amino acids, similar to the known solid-phase peptide synthesis. As an example, Fmoc-glycine and Fmoc-phenylalanine are immobilized on the silica support. The success of functionalization was investigated by 13 C CP MAS and 29 Si CP MAS solid-state NMR. Thermogravimetric analysis (TGA) and elemental analysis (EA) were performed to quantify the functionalization. Changes of the specific surface area, pore volume, and pore diameters in all modification steps were studied by Brunauer-Emmett-Teller based nitrogen adsorption-desorption measurements (BET). The combination of the analytical methods provided high grafting densities of 2.1±0.2 molecules/nm2 on the surface. Furthermore, they allowed for monitoring chemical changes on the pore surface and changes of the pore properties of the material during the different functionalization steps. This universal approach is suitable for the selective synthesis of pores with tunable surface-peptide functionalization, with applications to the synthesis of a big variety of silica-peptide model systems, which in the future may lead to a deeper understanding of complex biological systems.