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At least 703 records · Page 39Linked to original sources
PubMed2001

Vibrational spectroscopy of dimethylchlorooctadecylsilane covalently bonded to ultrathin silica films immobilized on Ag surfaces.

FTIR and Raman spectroscopies have been used to characterize the structure and conformational order of dimethylchlorooctadecylsilane (DOS) covalently bonded to ultrathin silica films supported on Ag substrates. Ultrathin silica films of ca. 30 A thickness prepared from sol-gel methods are immobilized on Ag surfaces modified with a self-assembled monolayer of (3-mercaptopropyl)trimethoxysilane (3MPT). This layered structure provides a unique opportunity for acquiring complementary spectral data from both FTIR and Raman spectroscopies, which are useful in elucidating alkylsilane conformation pertaining to stationary phases for reversed-phase liquid chromatography (RPLC). Characterization of octadecyltrichlorosilane (OTS) layers on thin silica films of ca. 800 A thickness on 3MPT-modified Ag surfaces has been reported previously. Differences between the ultrathin silica films used in this study and the thin silica films used in this previous study are considered. The results from both FTIR and Raman spectroscopy presented here suggest that bonded DOS alkyl chains are in a disordered, liquid-like state with close to monolayer surface coverage.

Journal Article↗
PubMed2005

Effects of silica on the bioactivity of calcium phosphate composites in vitro.

In the present study, silica-calcium phosphate composites (SiO(2)-CaP composites) were developed by mixing the starting materials (SiO(2) and CaHPO(4)) in different ratios with the addition of 0.1% w/v NaOH solution. The phase composition of the SiO(2)-CaP composites was determined by XRD and FTIR. After thermal treatment at 350 degrees C/1 h and at 1000 degrees C/3.5 h; all SiO(2)-CaP composites composed of beta-quartz, alpha-cristobalite and beta-Ca2P2O7. The presence of calcium phosphate enhanced the transformation of beta-quartz into alpha-cristobalite at 1000 degrees C. SEM observation indicated favorable attachment and spreading of neonatal rat calvaria osteoblasts onto the surface of silica-rich SiO(2)-CaP composites. After attachment, these cells produced significantly higher amount of protein and expressed higher AP activity than cells attached to silica-poor samples. Results of the study suggested that the silica-based composites are more bioactive than calcium phosphate-based composites. Silica promoted the expression of osteoblast phenotype by both solution-mediated effect and direct interaction with the surface of the substrate.

Alkaline Phosphatase↗
PubMed1984

Effect of silica and volcanic ash on the content of lung alveolar and tissue phospholipids.

Silica or volcanic ash (VA) was administered to rats via intratracheal instillation and the changes in extracellular (i.e., lavage fluid) and tissue phospholipids, as well as various biochemical parameters, were monitored over a 6-month period. VA produced relatively minor (up to 2.8-fold) increases in lung tissue or lavage fluid phospholipids that were maximal at 1 month postinstillation. These increases were quantitatively similar to the increases in protein and DNA content of lung tissue and lavage fluid induced by VA and, thus, may be attributable to hypercellularity and accumulation of cellular breakdown products in the alveolar lumen. Instillation of silica produced a much greater (up to 11-fold) increase than VA in total phospholipid over time, primarily due to a 14-fold increase in phosphatidylcholine (PC). The accumulation of PC was more pronounced in the lavage fluid during the first month following silica instillation, but thereafter progressed more rapidly in the lung tissue. The relatively small increases (1.3- to 3.5-fold) in other phospholipids induced by silica appeared to be nonspecific, since they did not differ greatly from the increases in lung weight, DNA, and protein. Collectively, these results indicate that intratracheal instillation of silica induces selective accumulation of lung PC, implying enhanced synthesis and secretion of pulmonary surfactant from alveolar epithelial Type II cells into the lumen.

Air Pollutants↗
PubMed1985

Effects of prolonged inhalation of silica and olivine dusts on immune functions in the mouse.

Immunologic responses were determined in Balb/c mice following intermittent silica or olivine inhalations for 150, 300, or 570 days. Animals dust-exposed for 570 days were tested immediately postexposure, while those exposed for 150 or 300 days were tested immediately or were rested for 30 or 150 days as a measure of possible recovery from effects of the dust inhalations. Silica inhalation suppressed the number of specific plaque-forming cells (PFC) in the spleen produced in response to aerosolized Escherichia coli bacteria. When tested after 570 days, silica inhalation also reduced the ability of alveolar macrophages to phagocytize Staphylococcus aureus in vitro. Olivine inhalation also suppressed splenic PFCs and alveolar macrophage phagocytosis, but to a lesser degree than silica. In animals tested after 570 days of dust exposure, it was determined that the ability to lyse allogeneic tumor cells in vitro was impaired by olivine slightly more than by silica, while antibody-dependent cell-mediated cytotoxic and mitogenic responses by splenic lymphocytes were unchanged by inhalation of either dust. The effects of increased exposure periods, and of recovery periods after exposure, were confounded by age-related immunologic changes which were present after the longer exposures.

Aerosols↗
PubMed1986

Preparation and evaluation of inorganic anion-exchange sorbents not based on silica.

The use of alternate macroporous (greater than 200 A) inorganic support materials in the preparation of pellicular anion-exchange packings was explored. Alumina, magnesia, titania, and a zirconia-coated silica were chosen for comparison with silica. The stationary phase attached to the support surfaces was an adsorbed polyethyleneimine, crosslinked with 1,4-butanediol diglycidyl ether. Packing materials were characterized by static elemental analyses, chromatographic retention, static loading capacity and pH stability. Titania, alumina, and zirconyl-clad silica packings were found to be substantially more stable under alkaline conditions than silica-based materials. The data show that the stationary phase was successfully bonded in all cases and functioned in anion-exchange chromatography. When the surface area and pore diameter of these alternate materials is equivalent to silica, there is little difference in chromatographic properties.

Animals↗
PubMed1995

Purification of monoclonal antibodies on dextran-coated silica support grafted by thiophilic ligand.

Coated silica beads are promising supports for high-performance liquid chromatography (HPLC) of proteins; they combine the excellent mechanical properties of silica with minimal non-specific interactions with proteins in solution due to the presence of hydrophilic dextran polymers adsorbed at the silica surface. So, dextran-coated porous silica beads can be grafted with beta-mercaptoethanol by using divinylsulfone as coupling reagent to obtain new thiophilic supports usable in HPLC. The affinity of monoclonal IgG subclasses from mouse ascitic fluids for the active phases can be analysed. These dextran-coated silica supports grafted with thiophilic ligands allow a one-step purification of these antibodies. Moreover, the chromatographic separation of two subclasses, immunoglobulin G1 (IgG1) and IgG3, is observed and can be correlated to the high resolution of these new HPLC thiophilic supports.

Animals↗
PubMed1995

Preparation of cDNA-silica using reverse transcriptase and its DNA sequence determination.

A new method for producing macroporous silica (suitable for high-performance liquid chromatography) with covalently attached DNA is presented. The method uses (dT)18-silica as a primer, annealed to a poly(A)-RNA template, which is then transcribed using reverse transcriptase. The RNA template is eluted and single-stranded cDNA-silica is recovered. The cDNA-silica can be sequenced using the dideoxy method. These methods provide a facile method for producing cDNA-silica of demonstrable authenticity and provide a unique approach to DNA and RNA sequencing.

Base Sequence↗
PubMed1996

Characterisation of silica-based heparin-affinity adsorbents through column chromatography of plasma fractions containing thrombin.

Different heparin-silicas, synthesised in this laboratory via directional end-point attachment of heparin (H) onto various amino-derivatised silicas, have been evaluated in packed-bed and expanded-bed column chromatographic experiments using crude preparations of the therapeutic protein, thrombin (T). Adsorbent capacities, determined through batch adsorption experiments, were verified by employing frontal analysis in packed-bed systems. The performance of these adsorbents was also investigated in terms of thrombin purification factors and recoveries. The potential of the heparin-silicas was further examined in the expanded-bed column chromatographic mode using a scaled-up procedure. With heparin-Fractosil 1000 adsorbents, capacities of around 100,000 U thrombin/ml adsorbent could be achieved. Heparin-Fractosil 1000 adsorbents of intermediate heparin content (around 4 mg heparin/ml sorbent) displayed binding stoichiometries similar to that of the commercial heparin-Sepharose (2.6-2.7 mol T/mol H). Furthermore, binding stoichiometries were largely unaffected by increasing the heparin content on the heparin-Fractosil 1000 adsorbents from 0.8 to 4.6 mg of heparin/ml of sorbent. This result suggests that optimal binding site accessibilities for the thrombin-heparin interaction occurs at lower ligand density values. The binding capacity values determined from frontal analysis were confirmed by the recovery data, thus indicating minimal irreversible adsorption. Specific activities of ca. 2100 U/mg were obtained for thrombin when affinity-purified on these heparin-LiChroprep Si60 or heparin-Fractosil 1000 adsorbents. These values were higher than the maximum achievable purity obtained through alternative, multi-step chromatographic purification procedures reported by other investigators. These results indicated that the packed-bed performances with these silica-based adsorbents were superior to currently available commercial soft gel adsorbents, with the more dense heparin-silicas exhibiting very good potential for use in expanded-bed applications.

Adsorption↗
PubMed1989

Kinetics of pulmonary surfactant phosphatidylcholine metabolism in the lungs of silica-treated rats.

Exposure of rats to silica by intratracheal injection increased the intra- and extracellular compartments of pulmonary surfactant phospholipid. These changes were dose and time dependent, but both pools were not affected equally. Seven days after the instillation of 10 mg of silica, the intracellular pool increased 13.3-fold, from 1.49 +/- 0.30 to 19.86 +/- 0.77 mg of surfactant phospholipid per pair of lungs, and the extracellular pool increased 7.4-fold, from 1.87 +/- 0.79 to 13.79 +/- 0.72 mg of surfactant phospholipid per pair of lungs. To investigate the physiologic processes responsible for these massive accumulations of surfactant. [14C]choline was injected into the tail veins of control and silica-treated rats and the specific activity of surfactant phospholipids within the intracellular and extracellular pools was determined at various times between 0 and 26 hr after injection. All of the processes measured were increased in response to silica exposure, but not to the same extent. At 1 hr, incorporation of [14C]choline into the intracellular surfactant pool was increased 12.6-fold above controls, from 4.8 +/- 1.1 x 10(3) to 60.6 +/- 26.6 x 10(3) dpm. The flux of [14C]choline-labeled phospholipid from the intracellular to the extracellular pool was increased 7.3-fold, from 102 +/- 10 to 749 +/- 39 micrograms/hr in silica-treated animals, but its disappearance from the extracellular pool was increased only 5.0-fold, from 87 +/- 8 to 434 +/- 21 micrograms/hr. The half-life of [14C]choline-labeled phospholipids in the intracellular pool of surfactant was increased from 10.1 +/- 1.0 to 18.3 +/- 5.3 hr and that in the extracellular surfactant pool from 14.8 +/- 1.4 to 21.9 +/- 4.9 hr. Expansion of the intra- and extracellular pools of surfactant phospholipids may be explained on the basis of a metabolic imbalance in which the intracellular production of surfactant is increased above its secretion rate into the extracellular compartment, and the secretion rate is elevated above the rate at which surfactant phospholipids are cleared from the alveoli.

Animals↗
PubMed1982

Protection against experimental allergic neuritis with silica quartz dust.

Lewis rats sensitized against peripheral nervous system antigens can be protected against experimental allergic neuritis (EAN) by the intraperitoneal injection of silica quartz dust. Two doses of 200 mg silica given 8 and 11 days post-inoculation (dpi) protected against the development of both clinical and pathological disease. A single dose of 200 mg silica 8 dpi gave significant protection against clinical disease but all animals developed pathological signs. A single injection of 200 mg silica 11 dpi, after the onset of early signs, protected against further progression of disease. The protection was long lasting. Given the known toxic effects of silica for macrophages, these results would support the conclusion that macrophages function during the effector stage in the clinical and pathological expression of EAN in the Lewis rat.

Animals↗
PubMed1996

Effect of silica treatment on resistance to Babesia rodhaini infection in immunized mice.

The effect of silica treatment on the course of Babesia rodhaini infection was investigated in ICR mice pretreated with either a mixture of B. rodhaini parasitized red blood cell hemolysation-sonication (S) antigen and Propionibacterium acnes bacterin or P. acnes bacterin alone and not subjected to immunization. In the normal mice (non-immunized), the mean survival time was decreased by approximately 1 day when 5 mg per mouse of silica were intraperitoneally inoculated at 5 h before infection. In immunization with S antigen and P. acnes bacterin, all mice survived regardless of the dose of silica (15-25 mg per mouse) treatment. In contrast, in immunization with P. acnes bacterin alone, 3/10, 4/10 and 1/10 mice died of B. rodhaini, when inoculated with 15 mg per mouse, 20 mg per mouse and 25 mg per mouse of silica treatment 5 h before infection, respectively. These results suggest that peritoneal macrophages (M luminal diameter of), especially when activated non-specifically by P. acnes bacterin, play an important role in inhibiting multiplication of organisms at the early stage of infection and the mice immunized with S antigen were ready to quickly acquire an enhanced solid specific protection even if the function of M luminal diameter of was damaged by a high dose of silica treatment.

Animals↗
PubMed2006

Fluorescent silica nanospheres for digital counting bioassay of the breast cancer marker HER2/neu [correction of HER2/nue].

This paper describes the use of fluorescent silica nanospheres as luminescent signal amplifiers in biological assays based on digital counting of individual particles instead of measuring averaged fluorescence intensity. We recently described a simple method to prepare highly fluorescent mono-dispersed silica nanospheres that avoids microemulsion formulations and the use of surfactants. Modification of the Stöber method was used successfully to prepare fluorescent silica spheres with the inorganic dye dichlorotris(1,10-phenanathroline)ruthenium (II) hydrate encapsulated during the condensation of tetraethylorthosilicate in ethanol and dye aqueous mixtures. Modifications in the ammonia and water content in the reaction mixture resulted in mono-dispersed silica spheres of 65, 440 and 800 nm in diameter. The dye-encapsulating particles emit intense red luminescence when excited at 460 nm. We observed an increased photostability and longer fluorescence lifetime in our particles that we attributed to increased protection of the encapsulated dye molecules from molecular oxygen. The newly prepared fluorescent silica particles were easily modified using trialkoxysilane reagents for covalent conjugation of anti-HER2/neu. We demonstrated the utility of the fluorescent nanospheres to detect the cancer marker HER2/neu in a glass slide based assay. The assay was shown to be simple but highly sensitive with a limit of detection approaching 1 ng/mL and a linear range between 1 ng/mL and 10 microg/mL of HER2/neu.

Binding, Competitive↗
PubMed2004

Development of standard operation procedures for the manufacture of n-octadecyl bonded silicas as packing material in certified reference columns for reversed-phase liquid chromatography.

The development of standard operation procedures for the manufacture of a n-octadecyl bonded spherical silica packing from partially condensed tetraethoxysilane as silica source is described. The synthesis comprises five intermediate products and six synthesis steps which were examined according to their reproducibility and robustness. The results led to the optimisation of the manufacturing process for a n-octadecyl bonded silica. Correlations were drawn between the dynamic viscosity of the poly(ethoxy)siloxane (PES), the synthesis parameters, the resulting pore structural properties and particle size distribution of the silicas. Validated procedures were developed to manufacture spherical porous ultra-pure silicas with a specific surface area of 350 m2 g(-1) +/- 5% R.S.D., a specific pore volume of 1.0 ml (-1) +/- 3.7% R.S.D., an average pore diameter of 12.0 nm +/- 0.5% R.S.D. and an average particle diameter of 5 microm. Results are presented on trial batches and the final master batch which were both used as packing materials in reversed-phase liquid chromatography (RP-LC) columns. The latter columns were certified and accepted as an HPLC column as reference material (BCR-722) by the European Commission, Institute for Reference Materials and Measurements (IRMM), Geel, Belgium.

Chromatography, Liquid↗
PubMed2004

Physical origin of peak tailing on C18-bonded silica in reversed-phase liquid chromatography.

Single component isotherm data of caffeine and phenol were acquired on two different stationary phases for RPLC, using a methanol/water solution (25%, v/v, methanol) as the mobile phase. The columns were the non-endcapped Waters Resolve-C18, and the Waters XTerra MS C18. Both columns exhibit similar C18 -chain densities (2.45 and 2.50 micromol/m2) and differ essentially by the nature of the underivatized solid support (a conventional, highly polar silica made from water glass, hence containing metal impurities, versus a silica-methylsilane hybrid surface with a lower density of less acidic free silanols). Thirty-two adsorption data points were acquired by FA, for caffeine, between 10(-3) and 24 g/l, a dynamic range of 24,000. Twenty-eigth adsorption data points were acquired for phenol, from 0.025 to 75 g/l, a dynamic range of 3000. The expectation-maximization procedure was used to derive the affinity energy distribution (AED) from the raw FA data points, assuming a local Langmuir isotherm. For caffeine, the AEDs converge to a bimodal and a quadrimodal distribution on XTerra MS-C18 and Resolve-C18, respectively. The values of the saturation capacity (q(s,1) approximately equal to 0.80 mol/l and q(s,2) approximately equal to 0.10 mol/l) and the adsorption constant (b1 approximately equal to 3.11/mol and b2 approximately equal to 29.1 l/mol) measured on the two columns for the lowest two energy modes 1 and 2, are comparable. These data are consistent with those previously measured on an endcapped Kromasil-C18 in a 30/70 (v/v), methanol/water solution (q(s,1) = 0.9 mol/l and q(s,2) = 0.10 mol/l, b1 = 2.4 l/mol and b2 = 16.1 l/mol). The presence of two higher energy modes on the Waters Resolve-C18 column (q(s,3) approximately equal to 0.013 mol/l and q(s,4) approximately equal to 2.6 10(-4) mol/l, b3 approximately equal to 252 l/mol and b4 = 13,200 l/mol) and the strong peak tailing of caffeine are explained by the existence of adsorption sites buried inside the C18-bonded layer. It is demonstrated that strong interactions between caffeine and the water protected bare silica surface cannot explain these high-energy sites because the retention of caffeine on an underivatized Resolve silica column is almost zero. Possible hydrogen-bond interactions between caffeine and the non-protected isolated silanol groups remaining after synthesis amidst the C18-chain network cannot explain these high energy interactions because, then, the smaller phenol molecule should exhibit similarly strong interactions with these isolated silanols on the same Resolve-C18 column and, yet, the consequences of such interactions are not observed. These sites are more consistent with the heterogeneity of the local structure of the C18-bonded layer. Regarding the adsorption of phenol, no matter whether the column is endcapped or not, its molecular interactions with the bare silica were negligible. For both columns, the best adsorption isotherm was the Bilangmuir model (with q(s,1) approximately equal to 2 and q(s,2) approximately equal to 0.67 mol/l, b1 0.61 and b2 approximately equal to 10.3 l/mol). These parameters are consistent with those measured previously on an endcapped Kromasil-C18 column under the same conditions (q(s,1) = 1.5 and q(s,2) = 0.71 mol/l, b1 = 1.4 l/mol and b2 = 11.3 l/mol). As for caffeine, the high-energy sites are definitely located within the C18-bonded layer, not on the bare surface of the adsorbent.

Chromatography, Liquid↗
PubMed2004

Auto-regeneration of anion-trap columns for improved determination of silica by ion chromatography.

The goal of this project was to develop an automated method to regenerate the ATC-3 trap columns that are used on the DX-800 on-line ion chromatography silica systems. The old method of regenerating the ATC-3 trap columns was to physically remove the trap columns from the silica system once every 2 weeks and manual regenerate them. A new automated regeneration method was developed by re-plumbing the silica system to allow 300 mM NaOH to run as the eluent. This regenerates the trap column automatically once every 24 h. The data have shown that regenerating the ATC-3 trap columns once per day improves the R.S.D. values for 250 ng/l silica analysis from 26.0 to 8.7%. The length of useful lifetime for the silica concentrator column was increased by an average of 9 months.

Anions↗
PubMed2004

Surfing silica surfaces superciliously.

The present mini-review summarizes the experience gathered by our group in developing different classes of novel quaternarized heterocyclic compounds able to modulate and reverse the electroendoosmotic flow (EOF) in a most peculiar manner. The first class comprises mono-salt compounds, with the determinant omega-iodoalkyl chains of different lengths (typically C4-C8), able to be adsorbed by silicas, at alkaline pH, and spontaneously alkylate ionised silanols, thus becoming covalently affixed to it. The second class is constituted by di-salt compounds, attached at the termini of an alkyl chain of variable lengths (here too, typically, C4-C8). This second class is unable to bind covalently silica surfaces, although, in thin-layer chromatography, it exhibits an extraordinary affinity for silica beads, contrary to the first one. On the basis of the strikingly different behaviour, structural rules are derived for the minimum requirements for general classes of amines to bind to silica walls and modify EOF. For compounds unable to bind covalently to the wall, the most important structural motif is two quaternary nitrogens spaced apart by a C4 chain: this seems to be the average distance (i.e., 0.8 nm) between two adjacent, ionized silanols for a snug fit. The other structural binding motif is the "hydrophobic decoration", i.e., the ratio of charged groups to alkyl residue in the various amines; amines with high levels of such alkane groups (i.e., with higher hydrophobicity), seem to bind more tenaciously to the wall, probably due to hydrophobic interaction not to the wall but among the amine derivatives themselves, when carpeting the silica.

Silicon Dioxide↗
PubMed2005

Preparation and characterization of a new C18 urea phase based on titanized silica.

A new stationary phase containing embedded urea groups (-NH-C(O)-NH-) was prepared by a procedure based on the synthesis of a trifunctional C18 urea-alkoxysilane, followed by modification of titanized silica and further endcapping to evaluate if the embedded group would minimize the higher retention and tailing for basic compounds seen with C18 titanized silica phases. Infrared, 13C and 29Si spectroscopies were employed to characterize the C18-urea titanized silica phase. Chromatographic evaluations used hydrophobic, polar and basic compounds to verify the effects of the polar urea groups embedded in the C18 urea phase. The chromatographic parameters, especially for the separation of basic compounds, compare favorably with those obtained on a C18 titanized silica stationary phase, prepared by silanization of titanized silica with octadecyltrimethoxysilane.

Calorimetry, Differential Scanning↗
PubMed2005

Preparation of pyrenebutyric acid bonded silica stationary phases for the application to the separation of fullerenes.

A novel immobilization method was proposed for the preparation of pyrenebutyric acid-bonded silica (PYB-silica) stationary phases. The pyrene moiety was grafted to silica gel through spacers of aminoalkyl silanes. The HPLC separation of C60, C70 and higher fullerenes on the new pyrenebutyric acid-bonded silica stationary phases was also studied. Based on the temperature effect, the intermolecular interaction between stationary phases and solutes and the retention mechanism were discussed. The results of column loading capacity test demonstrated the potential for the separation of fullerenes in large amounts on the PYB-silica stationary phases.

Chromatography, High Pressure Liquid↗