Charged Silanol Groups Research Articles

Synthesis and Crystallization Mechanism for SAPO-34 Zeolite Derived from Magadiite.

In this work, we explored the hydrothermal synthesize and crystallization process of SAPO-34 zeolites from two-dimensional layered silicate magadiite by using tetraethylammonium hydroxide (TEAOH) as a templating agent. Comprehensive characterization was conducted by XRD, SEM, FTIR, Raman, and BET. Time-resolved PXRD analysis revealed that SAPO-34 zeolite exhibited a steep growth curve when the crystallization time was 30 h, and the crystallinity reached 98.65 % at 48 h. Specifically, the disruption of the magadiite layer exposed charged silanol groups on the surface, fostering an affinity for AlO4 and PO4 species, thereby initiating the nucleation process. Under the guidance of TEAOH, these nucleation sites transformed into SAPO-34 nuclei, gradually advancing towards crystallization. FTIR and Raman analyses affirmed the presence of 6Rs, followed by D6R and 4Rs SBUs, along with the characteristic CHA structure. Combined with 29Si NMR established that disaggregated silicate minerals served as zeolite synthesis "seeds", enhancing nucleation sites and overall crystallization efficiency.

Characterization of β-lactoglobulin adsorption on silica membrane pore surfaces and its impact on membrane emulsification processes

Protein adsorption plays a key role in membrane fouling in liquid processing, but the specific underlying molecular mechanisms of β-lactoglobulin adsorption on ceramic silica surfaces in premix membrane emulsification have not been investigated yet.In this study, we aimed to elucidate the β-lactoglobulin adsorption and its effect on the premix membrane emulsification of β-lactoglobulin-stabilized oil-in-water emulsions. In particular, the conformation, molecular interactions, layer thickness, surface energy of the adsorbed β-lactoglobulin and resulting droplet size distribution are investigated in relation to the solvent properties (aggregation state of β-lactoglobulin) and the treatment of the silica surface (hydrophilization).The β-lactoglobulin adsorption is driven by attractive electrostatic interactions between positively charged amino acid residues, i.e., lysin and negatively charged silanol groups, and is stabilized by hydrophobic interactions. The strong negative charges of the treated silica surfaces result in a high apparent layer thickness of β-lactoglobulin. Although the conformation of the adsorbed β-lactoglobulin layer varies with membrane treatment and the solvent properties, the β-lactoglobulin adsorption offsets the effect of hydrophilization of the membrane so that the surface energies after β-lactoglobulin adsorption are comparable. The resulting droplet size distribution of oil-in-water emulsions produced by premix membrane emulsification are similar for treated and untreated silica surfaces.

Does Adsorption of Cd, Cu and Pb on Polymeric Silicic Acid Occur Under Acidic Conditions?

Contamination with Cd, Cu and Pb is a major environmental issue. Cations of those metals may adsorb on negatively charged surfaces of polymeric silicic acid (pSi), altering their environmental fate. Aiming to elucidate the underlying mechanisms and the extent of adsorption, we conducted batch adsorption experiments at pH 4 to 6 and concentrations that excluded precipitation of solid phases. Zeta-potential measurements were conducted to monitor surface charge changes. In addition, isothermal titration calorimetry (ITC) was used to derive thermodynamic parameters of the interaction between the metals and pSi. Surprisingly, neither did batch-adsorption experiments reveal any metal adsorption on pSi after 24 h reaction time, nor did ITC experiments show any evidence for chemical adsorption of the metals, as no heat was released or absorbed during the experiments. However, zeta-potential measurements indicated weak electrostatic interactions between the negatively charged silanol groups and the metals. These electrostatic interactions may be the initial step of metal incorporation into the matrix of polymerizing silicic acid, which were spectroscopically proven in long-term experiments.

Nanoscale zerovalent Iron-incorporated kaolinite for hemostatic and antibacterial applications

Nanoscale zero-valent iron (nZVI) was converted into iron oxide and used as an active component in hemostasis, but have to avoid inefficient nano agglomerates and tissue thermal damage. Herein, a nZVI-kaolinite composite was fabricated with kaolinite as the support material through the sodium borohydride reduction method, and its multiple hemostatic mechanisms and broad-spectrum antibacterial activity were studied. Incorporated kaolinite improves the dispersed state in an appropriate spacing against the exothermic oxidation reaction in advance, reducing exothermic side effects within a tissue-tolerable allowance. Regarding the hemostatic properties of nZVI-incorporated kaolinite, the blood coagulation index was 4.10% to 7.30%, and the hemolysis rate in vitro was less than 5%. The hemostatic mechanism originates from negatively charged silanol groups on the kaolinite surface and the iron oxide nanoparticles oxidized from nZVI. In addition, broad-spectrum antibacterial activities were obtained in vitro due to the synergistic effect of nZVI particles and kaolinite, including physical adsorption, exothermic effects, and the generation of reactive oxygen species. This work offered a feasible idea for using nZVI to treat infectious wounds.

Mutual Effects of pH and Competing Cations on the Mobility of Metoprolol in Saturated Quartz Sand: Parameter Estimation and Mobility Prediction Using Retardation Modeling

Predicting the fate of organic compounds in the aquatic environment remains a challenge due to the complexity of natural systems and diverse interactions with surfaces. In this study, the transport behavior of the β-blocker metoprolol (MTP) was studied in water-saturated columns filled with quartz sand (pH 3–11; [NaCl] of 1, 10, and 100 mmol L–1). A significant dependence of MTP retardation on pH and [NaCl] was observed ranging from a 10-fold retardation at pH 6 and 1 mmol L–1 NaCl to virtually none at pH 11. A retardation model was implicated considering (1) the speciation of MTP, (2) the surface reactions of MTPH+, and Na+ with charged surface silanol groups SiO– of quartz, and (3) the protolysis reaction between SiO– and SiOH. Modeling was performed using the complete dataset of 43 retardation values at once (R2 = 0.998). Exemplary predictions were performed for three aquifer settings to illustrate general trends in mobility. This comprehensive approach is an important basis for environmental fate prediction of organic contaminants in the future.

Synthesis and characterization of nanoparticulate niobium- and zinc-doped bioglass-ceramic/chitosan hybrids for dental applications

Dental caries and periodontal disease are responsible for the most frequent set of chronic diseases in humans, for which no perfectly regenerative solutions are available yet. As a result, materials combining an intrinsic antibacterial activity with tissue regeneration properties for minimally invasive dental therapies are in high demand. Here we report on the fabrication and characterization of a novel nanocomposite material for such dental applications. The material is composed of narrowly disperse Na2O–CaO–P2O5–SiO2 bioglass-ceramic nanoparticles, 30–70 nm in diameter, doped with antibacterial and osteogenic zinc and niobium ions, and hybridized with chitosan. These systems were characterized for their particle size, morphology, atomic and phase composition, and glass-ceramic/polymer interface with the use of transmission electron microscopy, energy-dispersive X-ray analysis, X-ray diffraction and Fourier transform infrared spectroscopy. After annealing at 680 °C, amorphous silica in the bioglass-ceramic coexisted with silicalite-1 and combeite, the average crystallite size of which was 20–40 nm. In spite of the significantly better incorporation of zinc than of niobium inside the glass-ceramic network, zinc did not affect the particle size and shape distribution, while niobium lowered the average particle size. Chitosan increased the hydration capacity of the bioglass-ceramic and it formed a continuous interface around the bioglass-ceramic nanoparticles, devoid of micropores. This intimacy of the interface was confirmed by the downshift of the critical Si–O(–Si) vibration modes in the bioglass-ceramic upon hybridization with chitosan. The addition of zinc ions hampered the partial recrystallization during annealing by interfering with the Si–O network restructuring, in direct proportion with its concentration. Niobium ions produced a similar structure-breaking effect, which was evidenced, as in the case of zinc, by upshifting the antisymmetric Si–O–Si stretch of the bridging oxygen and increasing the full-width at half maxima for all the major Si–O(–Si) vibration modes. The effective electrostatic attraction between the aminated hydrocarbon chains of chitosan and the negatively charged silanol groups of silica may extend to the interaction with dentin collagen fibrils decalcified due to caries, making the material of potential interest for adhesive fillers of cariogenic lesions in teeth. Both the undoped and the doped bioactive glass-ceramics interacted favorably with odontoblast-like cells, accentuating their potential for further research for applications in minimally invasive reparative dentistry.

Thiamin Determination in Food: A Chromatographic Challenge (P13-038-19)

ObjectivesThiamin plays an essential role during several metabolic reactions. Thiamin deficiency is a problem in developing countries, where a varied diet is lacking and people mainly rely on rice, which contains insufficient levels of thiamin, for their energy supply.A cost-effective strategy to fight this deficiency is the improvement of the nutritional quality of staple crops via biofortification.Although several methods for the determination of thiamin have been published, no method exists which allows a combined determination of thiamin, its phosphate derivatives and precursors. MethodsLC-MS/MS was used to determine the low-level and labile thiamin vitamers. Volatile buffers are required for MS/MS detection, excluding commonly used phosphate buffers. Furthermore, determination of thiamin mono (TMP)- and diphosphate (TPP) is highly challenging due to their strong polar and ionogenic character, whereby regular C18 columns lack retention. HILIC columns are recommended for these types of compounds, however, the solubility of the phosphate derivatives is incompatible with the required organic injection solvent. Therefore, we tested numerous columns and mobile phases, in order to determine all five compounds in one chromatographic run from a single biological sample. ResultsWith the Gemini® C18 column (Phenomenex) we were able to separate all compounds of interest. However, TMP and TPP could only be detected under basic conditions (≥pH 8.8), which resulted in secondary interactions between the charged silanol groups and the quaternary thiamin. We therefore transferred our method to a Gemini® NX C18 column, which offers a higher robustness at high pH and minimizes peak tailing since silanol groups are shielded. Finally, in an 8 minute run, we could achieve acceptable separation of all thiamin vitamers and precursors, with sufficient sensitivity for their determination in ≤200 mg of wild-type unpolished rice and Arabidopsis samples. ConclusionsAn LC-MS/MS method was successfully developed for the combined determination of all thiamin vitamers and precursors. Application of this method will allow to guide the effectiveness of biofortification strategies in order to fight thiamine deficiency in developing countries. Funding SourcesThe research was supported by the Research Foundation – Flanders. Supporting Tables, Images and/or Graphs▪

Development and application of SBA‐15 assisted electromembrane extraction followed by corona discharge ion mobility spectrometry for the determination of Thiabendazole in fruit juice samples

A new sample preparation method based on SBA-15 assisted electromembrane extraction coupled with corona discharge ion mobility spectrometer was developed for the determination of Thiabendazole as a model basic pesticide in fruit juice samples. The addition of SBA-15 in the supported liquid membrane in electromembrane extraction system not only can lead to enhancement of the effective surface area, but also introducing the negatively charged silanol groups into supported liquid membrane might improve migration of positively charged analytes toward the supported liquid membrane and finally into the acceptor solution. To investigate the effect of the presence of SBA-15 in the supported liquid membrane on the extraction efficiency, a comparative study was carried out between the conventional electromembrane extraction and SBA-15/electromembrane extraction methods. Under the optimized conditions, SBA-15/electromembrane extraction method showed higher extraction efficiencies in comparison with conventional electromembrane extraction method. SBA-15/electromembrane extraction method exhibited a low limit of detection (0.9ng/mL), high preconcentration factor (167) and high recovery (83%). Finally, the applicability of SBA-15/electromembrane extraction method was studied by the extraction and determination of Thiabendazole as a model basic pesticide in fruit juice samples.

Bare and Effective Charge of Mesoporous Silica Particles.

We develop and combine a novel numerical model, within the Poisson-Boltzmann framework, with classical experimental titration techniques for mesoporous silica particles to study the charging behavior as both pH and the amount of monovalent salt are varied. One key finding is that these particles can be considered to have an effectively or apparent electroneutral inner core with an effectively charged rim. As a consequence, the total apparent charge of the particle is several orders of magnitude smaller than that of the bare silica charge, which accounts only for the charged silanol groups of the mesoporous silica particles and which has its major contribution from the interior. Hence, the interior dictates the mesoporous silicas' bare charge while the rim its effective charge. We furthermore report density, charge, and accumulated charge profiles across the particle's interface.

Calcium Silicate Improved Bioactivity and Mechanical Properties of Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) Scaffolds.

The poor bioactivity and mechanical properties have restricted its biomedical application, although poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) had good biocompatibility and biodegradability. In this study, calcium silicate (CS) was incorporated into PHBV for improving its bioactivity and mechanical properties, and the porous PHBV/CS composite scaffolds were fabricated via selective laser sintering (SLS). Simulated body fluid (SBF) immersion tests indicated the composite scaffolds had good apatite-forming ability, which could be mainly attributed to the electrostatic attraction of negatively charged silanol groups derived from CS degradation to positively charged calcium ions in SBF. Moreover, the compressive properties of the composite scaffolds increased at first, and then decreased with increasing the CS content, which was ascribed to the fact that CS of a proper content could homogeneously disperse in PHBV matrix, while excessive CS would form continuous phase. The compressive strength and modulus of composite scaffolds with optimal CS content of 10 wt % were 3.55 MPa and 36.54 MPa, respectively, which were increased by 41.43% and 28.61%, respectively, as compared with PHBV scaffolds. Additionally, 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay indicated MG63 cells had a higher proliferation rate on PHBV/CS composite scaffolds than that on PHBV. Alkaline phosphatase (ALP) staining assay demonstrated the incorporation of CS significantly promoted osteogenic differentiation of MG63 cells on the scaffolds. These results suggest that the PHBV/CS composite scaffolds have the potential in serving as a substitute in bone tissue engineering.

In Situ Surface Assembly Derived Ultralow Refractive Index MgF2–SiO2 Hybrid Film for Tri‐Layer Broadband Antireflective Coating

For the broadband antireflective (AR) coating working in specific wavelengths, the precise control over refractive index and film thickness of each layer is critical to guarantee the peak position locating at the targeted wavelengths. In this paper, a simple sol–gel procedure without post‐treatment is used to prepare MgF2–SiO2 hybrid coating with tunable refractive index for the fabrication of tri‐layer tri‐wavelength broadband AR coating. The MgF2–SiO2 coating with ultralow refractive index of 1.12 is realized through in situ surface assembly of negatively charged silanol groups on vesicle‐like MgF2 particles to obtain porous crosslinking structure. The electrostatic attraction between the negatively charged silanol groups and positively charged MgF2 colloidal particles plays a key role. Furthermore, the MgF2–SiO2 coating with a wide range of refractive index between 1.20 and 1.44 is achieved by adjusting the addition amount of acid‐catalyzed silica sol into the vesicle‐like MgF2 sol. According to the theoretical design, a tri‐layer broadband AR coating with refractive index model of 1.12/1.26/1.36 is prepared, which can enhance the transmittance of quartz substrate to near 100% simultaneously at 351, 527, and 1053 nm.

Sorption of amitriptyline and amphetamine to mixed-mode solid-phase microextraction in different test conditions

A solid-phase microextraction (SPME) method based on a sampler coating that includes strong cation groups (C18/SCX) is explored as a rapid direct sampling tool to detect and quantify freely dissolved basic drugs. Sampling kinetics, sorption isotherms and competitive effects on extraction yields in mixtures were tested for amphetamine and the relatively large/hydrophobic tricyclic antidepressant amitriptyline. Both compounds are >99% ionized at pH 7.4 but their affinity for the C18/SCX fiber is markedly different with distribution coefficients (Dfw values) of 2.49±0.02 for amphetamine and 4.72±0.10 for amitriptyline. Typical changes in electrolyte homeostasis that may occur in biomedical samples were simulated by altering pH and ionic composition (Na+ and K+ concentrations). These changes were shown to affect C18/SCX sorption affinities of the tested drugs with less than 0.2log units. At relatively low fiber loadings (<10mmol/L coating) and at all tested exposure times, linear sorption isotherms were obtained for both compounds but at aqueous concentrations of the individual drugs corresponding to concentrations in blood that are lethal, sorption isotherms became strongly nonlinear. Competition effects within binary mixtures occurred only if combinations of aqueous concentrations resulted in total fiber loadings that were in the nonlinear range of the SPME sorption isotherm for the individual compounds. We also compared sorption to the (prototype) C18/SCX SPME coating with analogue (biocompatible) C18 coated SPME fibers. C18/SCX fibers show increased sorption affinity for cationic compounds compared to C18 fibers, as tested using amitriptyline, amphetamine and trimethoprim. Surprisingly, sorption affinity of these ionized compounds for the C18 SPME fibers were within 1log unit of the C18/SCX SPME fibers. This shows that the strong cation exchange groups within the C18/SCX coating only has a relatively small contribution to the total sorption affinity of cationic compounds. Also the role of negatively charged silanol groups in both the C18 and C18/SCX coating seems small, as anionic diclofenac species sorbed strongly to the C18 fiber. Ionized organic species seem to be substantially adsorbed to the high surface area of C18 in SPME types using porous silica based coatings.

Aqueous silane modified silica sols: theory and preparation

PurposeThe purpose of this paper is to study methods of reacting the surface of the particles of silica sols with silanes, primarily gamma‐glycidoxypropyltrimethoxysilane (GPTMS) and study some basic properties of the modified sols and the nature and structure of the silane groups attached to the particle surface.Design/methodology/approachThe surface of the silica particles was modified by reacting the silica sols with aqueous solutions of silanes, chiefly GPTMS. The presence and structure of silane groups on the particle surface were established by Si‐NMR and C‐NMR, respectively.FindingsSeveral silanes were studied but silica sols could be readily modified only with GPTMS and glycidoxypropylmethoxydiethoxysilane (GPMDES), most readily if the silanes were pre‐hydrolysed in water. Higher degrees of silylation were preferably done by continuous addition of silane. Lower degrees of modification can be achieved at room temperature by the stepwise addition of the silane solution. The silylation of the silica surface with GPTMS significantly reduces the number of charged surface groups and silanol groups. GPTMS binds covalently to the silica surface and the epoxy ring opens and transforms into a diol. Silica sols modified with GPTMS and GPMDES are stable toward aggregation.Research limitations/implicationsOnly organo‐reactive silanes were studied.Originality/valueThis is the first work to study the modification by silanes of silica aquasols with high concentrations of silica. The silane modification can extend the use of silica to areas of applications previously inaccessible to silica sols.

Synthesis and characterisation of π-conjugated polymer/silica hybrids containing regioregular ionic polythiophenes

Highly regioregular poly{3-[n-(1-methylimidazolium-3-yl)alkyl]thiophene-2,5-diyl bromide} (n = 4, 6, 8) (10–12) has been prepared by reaction of poly[3-(n-bromoalkyl)thiophene-2,5-diyl] (n = 4, 6, 8) (7–9) with 1-methylimidazole. Acid-catalyzed hydrolysis and polycondensation of tetraethoxysilane (TEOS) were carried out in the presence of these polymers. The strong ionic interactions between the imidazolium moieties of the polythiophene and the charged silanol groups enabled the homogeneous dispersion of the polythiophene within silica. The resulting composite materials were characterised by SEM, TEM and tapping mode atomic force microscopy (TM-AFM). The optical and thermal properties were investigated by UV and TGA measurements.

Effect of high pH column regeneration on the separation performances in reversed phase chromatography of peptides

Caustic regeneration procedures are often used in chromatographic purification processes of peptides and proteins to remove irreversibly bound impurities from the stationary phase. Silica-based materials are the most commonly used materials in reversed phase chromatography of peptides. Their limited chemical stability at high pH can be, however, problematic when high pH column regeneration (i.e. cleaning in place) is required. The effect of cleaning in place on the surface chemistry of the stationary phase has been investigated using the Tanaka test. It has been shown that the high pH treatment does not significantly affect the hydrophobicity of the material, but it strongly increases its silanol activity. A representative peptide purification process has been used to investigate the impact of cleaning in place on the separation performance. It has been shown that the caustic regeneration increases the peptide retention at high pH (pH 6.5), due to the interactions between the peptide and the negatively charged silanol groups. These unwanted interactions reduce the separation performances by decreasing the selectivity between the late eluting impurities and the main peptide. However, it has been shown that the effect of the silanol groups on the peptide adsorption and on the separation performance can be minimized by carrying out the purification process at low pH (pH ∼ 2). In this case, the silanol groups are protonated and their electrostatic interactions with the positively charged analyte (i.e. peptides) are suppressed. In these conditions, the peptide adsorption and the impurity selectivity is not changing upon high pH column regeneration and the separation performance is not affected.

Novel Vinylpyridine Based Cationic MIP Monoliths for Enantiomer Separation in CEC

Cationic vinylpyridine based molecularly imprinted polymer monoliths were, for the first time, applied to enantiomer separation using capillary electrochromatography. In order to map the synthesis conditions under which superporous monoliths are obtained, capillary columns were prepared by an in situ polymerization technique using varying monomer and porogen compositions. Both electrolyte pH and percentage of the organic modifier acetonitrile were found to affect the electrochromatographic behaviour on such columns. An interesting observation is that the electroosmotic flow changed direction from cathodic at high pH to anodic at low pH of the electrolyte, opening up the opportunity to manipulate the flow. This is attributed to the vinylpyridine based MIP becomes protonated and positively charged at low pH, whereas it is uncharged at high pH where instead negatively charged silanol groups drive the electroosmotic flow. Improved enantiomer resolution, as well as increased retention, was observed when the concentration of acetonitrile in the electrolyte decreased, indicating a significant element of hydrophobic effects in the molecular recognition of the imprinted enantiomer. Enantiomer separation of the non-steroidal anti-inflammatory drug ibuprofen was studied and efficiencies as high as 30,000 plates per meter with an asymmetry factor below 4 were obtained for the last eluting imprinted enantiomer. These values are better than that obtained generally using MIP based chromatography.

Silanization of inner surfaces of nanoelectrospray ionization emitters for reduced analyte adsorption

During the course of nanoelectrospray ionization (nanoESI) of substance P, an unusual type of signal reduction was observed with flow rates <10 nL/min. This reduction in signal appears to be induced by the adsorption of positively charged analytes onto negatively charged free silanol groups on the inner surface of emitters; analytes with higher pI values (such as substance P) exhibit greater tendency for adsorption. Support for this hypothesis is demonstrated by the decrease in signal reduction in the presence of concentrated salts or for emitters whose internal silanols have been covalently silanized. Emitters treated with hexamethyldisilazane or 3-aminopropyltriethoxysilane showed higher analyte signals for substance P than untreated emitters, suggesting a reduction of analyte adsorption onto the inner walls of silanized emitters. The efficacy of reduced peptide adsorption was demonstrated for emitters silanized with 3-aminopropyltriethoxysilane using a simple peptide mixture as well as a more complex peptide mixture (a tryptic digest of horse hemoglobin).

Interactions between Nonpolar Surfaces Coated with the Nonionic Surfactant Hexaoxyethylene Dodecyl Ether C12E6and the Origin of Surface Charges at the Air/Water Interface

The interactions between nonpolar surfaces coated with the nonionic surfactant hexaoxyethylene dodecyl ether C12E6 were investigated using two techniques and three different types of surfaces. As nonpolar surfaces, the air/water interface, silanated negatively charged glass, and thiolated uncharged gold surfaces were chosen. The interactions between the air/water interfaces were measured with a thin film pressure balance in terms of disjoining pressure as a function of film thickness. The interactions between the solid/liquid interfaces were determined using a bimorph surface force apparatus. The influence of the nature of the surface on the interaction forces was investigated at surfactant concentrations below and above the cmc. The adsorption of the nonionic surfactant on the uncharged thiolated surface does not, as expected, lead to any buildup of a surface charge. On the other hand, adsorption of C12E6 on the charged silanated glass and the charged air/water interface results in a lowering of the surface charge density. The reduction of the surface charge density on the silanated glass surfaces is rationalized by changes in the dielectric permittivity around the charged silanol groups. The reason for the surface charge observed at the air/water interface as well as its decrease with increasing surfactant concentration is discussed and a new mechanism for generation of OH- ions at this particular interface is proposed.

Insulin adsorption on coated silica based supports grafted with N-acetylglucosamine by liquid affinity chromatography

Silica beads are coated with dextran carrying a calculated amount of positively charged diethylassminoethyl groups (DEAE) in order to neutralize negative charged silanol groups at the silica surface and in this way to minimize non specific interactions between silica surface and proteins in solution. Dextran-coated silica supports are potentially excellent stationary phases for high-performance liquid chromatography of proteins. These supports combine the advantages of polysaccharide phases with the excellent mechanical characteristics of silica. These supports (silica–dextran–DEAE = SID) are easily functionalized by grafting N-acetylglucosamine (GlcNAc) using conventional coupling methods. The performances of the support bearing GlcNAc are studied by high-performance liquid affinity chromatography (HPLAC) of insulin, the hypoglycemic peptide hormone of the human organism. The study shows that these supports exhibit a reversible and specific affinity towards insulin and allow separations with high purification yields. Moreover, the influence of different physico-chemical parameters (pH, NaCl and insulin concentration) on insulin retention on the support was analysed. This allowed us to optimize the conditions of adsorption and to better understand the interaction mechanisms between insulin and GlcNAc as biospecific ligand.

Adsorptive mechanisms of orthosilicic acid on nano-ball allophane.

Adsorption of orthosilicic acid on two low Si/Al (KyP and KiP) and one high Si/Al (KnP) nano-ball allophane samples was found to be controlled by the species type of the acid. There seemed to be a higher preference for the anion species to the neutral species. Adsorption increased with increasing solution pH with the highest adsorption occurring at initial pH 10. Further increase in pH, however, led to reduced levels in adsorption, particularly in the KnP sample due to repulsion between the negatively charged silanol groups and the anion species of the acid. Adsorption was higher in the low Si/Al samples due to their relatively higher number of aluminol groups per unit mass. The estimated Zero Point of Silicon Adsorption, which was pH dependent, was found to be higher in the KnP sample due to its higher inherent Si content. Adsorption data conformed only to the Freundlich model with the Freundlich parameters increasing with increasing solution pH to a maximum at initial pH 10. Release of Al occurred only at pH 10 and was highly correlated with Si adsorption in the low Si/Al samples suggesting a partial replacement of Al with Si at the pore region.