A novel method to delaminate nitrate-intercalated MgAl layered double hydroxides in water and application in heavy metals removal from waste water.

Nitrate-intercalated MgAl layered double hydroxide (LDH) was successfully delaminated in water by a facile and effective method upon reflux at 120 °C for 24 h followed by sonication at 40 °C for 5 h. This process is environmentally friendly since water is the only solvent used. The delaminated nanosheets were characterized by microscopic, spectroscopic, and particle size analyses. The delamination process successfully produced octahedron-shaped single-layer nanosheets 50-150 nm in size. X-ray photoelectron spectroscopy (XPS) data confirmed that the surface elements and their chemical status are consistent with the basic layer of MgAl LDH. The delaminated nanosheets displayed higher adsorption capacity for removing heavy metals from waste water than the original powdered LDH. After treating the waste water, a sharp and intense peak in the X-ray powder diffraction (XRD) pattern of the precipitate confirms the restacking of the LDH nanosheets.

Kinetics of intercalation of fluorescent probes in magnesium-aluminium layered double hydroxide within a multiscale reaction-diffusion framework.

We report the synthesis of magnesium-aluminium layered double hydroxide (LDH) using a reaction-diffusion framework (RDF) that exploits the multiscale coupling of molecular diffusion with chemical reactions, nucleation and growth of crystals. In an RDF, the hydroxide anions are allowed to diffuse into an organic gel matrix containing the salt mixture needed for the precipitation of the LDH. The chemical structure and composition of the synthesized magnesium-aluminium LDHs are determined using powder X-ray diffraction (PXRD), thermo-gravimetric analysis, differential scanning calorimetry, solid-state nuclear magnetic resonance (SSNMR), Fourier transform infrared and energy dispersive X-ray spectroscopy. This novel technique also allows the investigation of the mechanism of intercalation of some fluorescent probes, such as the neutral three-dimensional rhodamine B (RhB) and the negatively charged two-dimensional 8-hydroxypyrene-1,3,6-trisulfonic acid (HPTS), using in situ steady-state fluorescence spectroscopy. The incorporation of these organic dyes inside the interlayer region of the LDH is confirmed via fluorescence microscopy, solid-state lifetime, SSNMR and PXRD. The activation energies of intercalation of the corresponding molecules (RhB and HPTS) are computed and exhibit dependence on the geometry of the involved probe (two or three dimensions), the charge of the fluorescent molecule (anionic, cationic or neutral) and the cationic ratio of the corresponding LDH.This article is part of the themed issue 'Multiscale modelling at the physics-chemistry-biology interface'.

Impact of size, secondary structure, and counterions on the binding of small ribonucleic acids to layered double hydroxide nanoparticles.

Use of ribonucleic acid (RNA) interference to regulate protein expression has become an important research topic and gene therapy tool, and therefore, finding suitable vehicles for delivery of small RNAs into cells is of crucial importance. Layered double metal hydroxides such as hydrotalcite (HT) have shown great promise as nonviral vectors for transport of deoxyribose nucleic acid (DNA), proteins, and drugs into cells, but the adsorption of RNAs to these materials has been little explored. In this study, the binding of small RNAs with different lengths and levels of secondary structure to HT nanoparticles has been analyzed and compared to results obtained with small DNAs in concurrent experiments. Initial experiments established the spectrophotometric properties of HT in aqueous solutions and determined that HT particles could be readily sedimented with near 100% efficiencies. Use of RNA+HT cosedimentation experiments as well as electrophoretic mobility shift assays demonstrated strong adsorption of RNA 25mers to HT, with twofold greater binding of single-stranded RNAs relative to double-stranded molecules. Strong affinities were also observed with ssRNA and dsRNA 54mers and with more complex transfer RNA molecules. Competition binding and RNA displacement experiments indicated that RNA-HT associations were strong and were only modestly affected by the presence of high concentrations of inorganic anions.

Almagate interference in breath test results for the diagnosis of Helicobacter pylori infection.

BACKGROUND: Infection by Helicobacter pylori is common and affects both genders at any age. The 13C-urea breath test is a widely used test for the diagnosis of this infection. However, multiple drugs used for the treatment of Helicobacter pylori infection symptoms have interactions with this breath test that generate false negative results. This observational study was to assess the potential interaction between almagate and the breath test. METHODS: Thirty subjects on almagate therapy who underwent a breath test were included. If the result was negative, almagate was withdrawn for a month and the breath test was then repeated. RESULTS: In general, 51.9 % of assessed subjects had a negative result after the first test, and 100 % of these also had a negative result after the second test. CONCLUSIONS: It was concluded that the use of almagate does not interfere in breath test results. These results provide a drug therapy option for the treatment of symptoms associated with Helicobacter pylori infection during the diagnostic process.

In situ pH management for microbial culture in shake flasks and its application to increase plasmid yield.

Shake flasks are widely used to culture microorganisms, but they do not allow for pH control without additional infrastructure. In the presence of a carbon source like glucose, culture pH typically decreases due to overflow metabolism and can limit the growth of microorganisms in shake flasks. In this study, we demonstrate the use of magnesium hydroxide-loaded pH managing hydrogels (m-pHmH) for in situ base release to counter the decrease in culture pH in shake flasks using Escherichia coli as a model organism, in both complex and mineral salts medium. Base release from m-pHmH is shown to increase with decreasing pH (22-fold increase in release rate from pH 8 to 5), thus providing feedback from culture pH. The addition of m-pHmH resulted in better pH maintenance and higher biomass yields of E. coli K12 in media containing glucose as a carbon source. The use of m-pHmH with additional buffer resulted in pH being maintained above 6.9 while pH decreases below 5 without m-pHmH. We demonstrate one application of such in situ pH management to increase the volumetric plasmid yield from E. coli in shake flask culture. In situ glucose release through a hydrogel to mimic fed-batch culture along with the addition of m-pHmH resulted in a 395 % increase in volumetric plasmid yield to 38 µg/ml in shake flask culture.

Boron sorption from aqueous solution by hydrotalcite and its preliminary application in geothermal water deboronation.

Hydrotalcite and its calcination product were used to treat pure water spiked with various concentrations of boron and geothermal water containing boron as a major undesirable element. The kinetics process of boron sorption by uncalcined hydrotalcite is controlled by the diffusion of boron from bulk solution to sorbent-solution boundary film and its exchange with interlayer chloride of hydrotalcite, whereas the removal rate of boron by calcined hydrotalcite rests with the restoration process of its layered structure. The results of isotherm sorption experiments reveal that calcined hydrotalcite generally has much stronger ability to lower solution boron concentration than uncalcined hydrotalcite. The combination of adsorption of boron on the residue of MgO-Al2O3 solid solution and intercalation of boron into the reconstructed hydrotalcite structure due to "structural memory effect" is the basic mechanism based on which the greater boron removal by calcined hydrotalcite was achieved. As 15 geothermal water samples were used to test the deboronation ability of calcined hydrotalcite at 65 °C, much lower boron removal efficiencies were observed. The competitive sorption of the other anions in geothermal water, such as HCO3-, SO4(2-), and F-, is the reason why calcined hydrotalcite could not remove boron from geothermal water as effectively as from pure boron solution. However, boron removal percents ranging from 89.3 to 99.0% could be obtained if 50 times of sorbent were added to the geothermal water samples. Calcined hydrotalcite is a good candidate for deboronation of geothermal water.

First identification of O,S-diethyl Thiocarbonate in Indian Cress absolute and odor evaluation of its synthesized homologues by GC-sniffing.

Indian cress (Tropaeolum majus L.) absolute was studied by GC-olfactometry (VIDEO-Sniff method) in order to identify odor-active aroma compounds. Because of its fruity-sulfury odor note, a compound that has never been identified in plant extracts before stood out: O,S-diethyl thiocarbonate, present at 0.1% (percentage of the total GC/FID area) in the extract. GCxGC-TOFMS allowed for a clean mass spectrum to be obtained, and isolation by preparative GC followed by NMR studies allowed its identification. Here, we report on the first detection of O,S-diethyl thiocarbonate in Indian cress absolute by GC-olfactometry/VIDEO-Sniff and on its isolation and identification. The synthesis and odor evaluation of its homologues are presented.

Hydrothermal treatment of MSWI bottom ash forming acid-resistant material.

To recycle municipal solid waste incinerator (MSWI) bottom ash, synthesis of hydrothermal minerals from bottom ash was performed to stabilize heavy metals. MSWI bottom ash was mixed with SiO(2), Al(OH)(3), and Mg(OH)(2) so its chemical composition was similar to that of hydrothermal clay minerals. These solid specimens were mixed with water at a liquid/solid ratio of 5. The reaction temperature was 200 degrees C, and reactions were performed for 24-240h. Generation of kaolinite/smectite mixed-layer clay mineral was found in the samples after the reaction of the mixture of bottom ash, SiO(2), and Mg(OH)(2). Calcium silicate hydrate minerals such as tobermorite and xonotlite were also generated. X-ray powder diffraction suggested the presence of amorphous materials. Leaching tests at various pHs revealed that the concentration of heavy metals in the leachates from MSWI bottom ash hydrothermally treated with SiO(2) and Mg(OH)(2) was lower than that in leachates from non-treated bottom ash, especially under acid conditions. Hydrothermal treatment with modification of chemical composition may have potential for the recycling of MSWI bottom ash.

Dust exposure in indoor climbing halls.

The use of hydrated magnesium carbonate hydroxide (magnesia alba) for drying the hands is a strong source for particulate matter in indoor climbing halls. Particle mass concentrations (PM10, PM2.5 and PM1) were measured with an optical particle counter in 9 indoor climbing halls and in 5 sports halls. Mean values for PM10 in indoor climbing halls are generally on the order of 200-500 microg m(-3). For periods of high activity, which last for several hours, PM10 values between 1000 and 4000 microg m(-3) were observed. PM(2.5) is on the order of 30-100 microg m(-3) and reaches values up to 500 microg m(-3), if many users are present. In sports halls, the mass concentrations are usually much lower (PM10 < 100 microg m(-3), PM2.5 < or = 20 microg m(-3)). However, for apparatus gymnastics (a sport in which magnesia alba is also used) similar dust concentrations as for indoor climbing were observed. The size distribution and the total particle number concentration (3.7 nm-10 microm electrical mobility diameter) were determined in one climbing hall by an electrical aerosol spectrometer. The highest number concentrations were between 8000 and 12 000 cm(-3), indicating that the use of magnesia alba is no strong source for ultrafine particles. Scanning electron microscopy and energy-dispersive X-ray microanalysis revealed that virtually all particles are hydrated magnesium carbonate hydroxide. In-situ experiments in an environmental scanning electron microscope showed that the particles do not dissolve at relative humidities up to 100%. Thus, it is concluded that solid particles of magnesia alba are airborne and have the potential to deposit in the human respiratory tract. The particle mass concentrations in indoor climbing halls are much higher than those reported for schools and reach, in many cases, levels which are observed for industrial occupations. The observed dust concentrations are below the current occupational exposure limits in Germany of 3 and 10 mg m(-3) for respirable and inhalable dust. However, the dust concentrations exceed the German guide lines for work places without use of hazardous substances. In addition, minimizing dust concentrations to technologically feasible values is required by the current German legislation. Therefore, substantial reduction of the dust concentration is required.

Quantitative determination of alginic acid in pharmaceutical formulations using capillary electrophoresis.

A capillary electrophoresis (CE) method has been developed and validated for the quantitative determination of alginic acid, which is used as a rafting agent in complex antacid formulations. The method involves a preliminary separation of the alginic acid from the formulation by washing the sample matrix with methanol, diluted HCl and water. This is followed by electrophoresis within a fused silica capillary using borate/boric acid buffer as the electrolyte, and the quantification is performed by a UV detector monitoring at 200 nm, where the intrinsic absorption of alginic acid is measured. An assay precision of better than 3% was achieved in intra- and interday determinations. No interference was found from the matrix of the antacid formulations.

Effect of hydrotalcite-like compounds on the aqueous solubility of some poorly water-soluble drugs.

A new approach of improving drug dissolution properties is described. This method exploits the property of a carrier owing to the hydrotalcite-type anionic clays (HTlc). HTlc is an inorganic layered solid that lodges anionic compounds among its layers. As HTlc dissolves at acidic pH values (pH < 4), the anions intercalated among the layers are promptly released in the medium. In this article some nonsteroidal antiinflammatory drugs were chosen as models of poorly water-soluble drugs. They were intercalated in HTlc and solubility measurements in acidic medium were performed. A remarkable improvement of drug solubility was observed especially in the case of indomethacin.

Molecular assembly in synthesised hydrotalcites of formula Cu(x)Zn(6 - x)Al2(OH)16(CO3) x 4H2O--a vibrational spectroscopic study.

Infrared and Raman spectroscopy have been used to characterise synthetic hydrotalcites of formula Cu(x)Zn(6 - x)Al2(OH)16(CO3) x 4H2O. The spectra have been used to assess the molecular assembly of the cations in the hydrotalcite structure. The spectra may be conveniently subdivided into spectral features based (a) upon the carbonate anion (b) the hydroxyl units (c) water units. The Raman spectra of the hydroxyl-stretching region enable bands to be assigned to the CuOH, ZnOH and AlOH units. It is proposed that in the hydrotalcites with minimal cationic replacement that the cations are arranged in a regular array. For the Cu(x)Zn(6 - x)Al2(OH)16(CO3) x 4H2O hydrotalcites, spectroscopic evidence suggests that 'islands' of cations are formed in the structure. In a similar fashion, the bands assigned to the interlayer water suggest that the water molecules are also in a regular well-structured arrangement. Bands are assigned to the hydroxyl stretching vibrations of water. Three types of water are identified (a) water hydrogen bonded to the interlayer carbonate ion (b) water hydrogen bonded to the hydrotalcite hydroxyl surface and (c) interlamellar water. It is proposed that the water is highly structured in the hydrotalcite as it is hydrogen bonded to both the carbonate anion and the hydroxyl surface.

A RP-LC method with evaporative light scattering detection for the assay of simethicone in pharmaceutical formulations.

A reversed-phase liquid chromatographic method has been developed and validated for the determination of the polydimethylsiloxane (PDMS) component of Simethicone, which is used as an anti-foaming agent in pharmaceutical formulations. The method involves acidification to neutralise antacid components of the formulation, then a single extraction of the PDMS with dichloromethane. This is followed by separation with a reversed-phase column using an acetonitrile-chloroform solvent gradient, and quantification by an evaporative light scattering detector. An assay precision of 3% was achieved in intraday and interday determinations. No interference was found from the aluminium and magnesium hydroxide components of antacid formulations.

[Phosphate ion-exchange with hydrotalcite-like compound in the presence of trypsin].

A Cl(-)-intercalated hydrotalcite-like compound (HTAL) is a promising material as a better phosphate adsorbent for further clinical use than the currently marketed aluminum hydroxide gels. In the preceding study, we found that Cl- ions in the interlayer of HTAL can be exchanged with phosphate ions equivalently. In the present study, we have investigated the adsorption of porcine pancreas trypsin on HTAL and the influence of trypsin adsorption on the phosphate/Cl- ion-exchange properties of HTAL. The isotherm for trypsin adsorption at 310K and pH 8.4 showed the curve of BDDT V type and gave an adsorption capacity of 88.6 mg/g for trypsin. The zeta-potential analysis of HTAL suggested that the trypsin adsorption on HTAL at pH 8.4 was restrained by the electrostatic repulsion between HTAL surface and trypsin with positive charge. XRD and nitrogen adsorption studies showed that trypsin was adsorbed on the external surface of HTAL by occupying the area (ca. 22 nm2) per trypsin molecule. The phosphate/Cl- ion-exchange reaction with HTAL was not affected by the presence of trypsin; the phosphate ion-exchange capacity reached 73.6 mg P/g from the solution containing 3200 mg trypsin/dm3. On the other hand, the trypsin adsorption was significantly depressed by the loading of phosphate ions. The XRD analysis of the phosphate-loaded HTAL revealed that the layered structure of hydrotalcite holds after the phosphate ion-exchange, but shows a slight increase of the interlayer distance from 0.3 nm to 0.5 nm by the intercalation of phosphate ions.

[Drug interactions during storage of mixtures of the antacid group. III. Effect of relative humidity on structural changes in mixtures aluminum hydroxide gel and magnesium hydroxide in the solid phase]. / Badanie oddzialywan zachodzacych podczas przechowywania mieszanin z grupy antacida.III. WpLyw wilgotnosci wzglednej na zmiany struktury mieszanin zelu wodorotlenku glinowego i magnezowego w fazie staLej.

Mixtures of A1(OH)3 gel and Mg(OH)2 were stored for 14 months in the solid phase in chambers with relative air humidity of 35%, 55%, 76% and 92%. IR spectra of the stored mixtures were measured. In mixtures stored at relative air humidity of 35% there were found no changes in IR spectra, while the mixtures stored at relative air humidity of 92% proved to exhibit IR spectra characteristic for hydrotalcite.

Bile salt binding properties of commonly used gastrointestinal drugs: maalox, carafate, and questran.

We have validated a method to measure bile salt binding by Maalox (aluminum hydroxide and magnesium hydroxide), Carafate (sucralfate), and Questran (cholestyramine) in vitro. The method used in this study involves a correction for adherent water volume and thus provides a correct measure of bile salt binding. With this approach, we described the binding properties of Maalox, Carafate, and Questran. The bile salt binding capacities of Carafate and Maalox are limited and do not have physiological or pharmacological significance. On the other hand, we found that Questran has substantial bile salt binding capacity. At the recommended dosage, Questran could deplete the total bile salt pool. We also found that Carafate, although not used as an antacid, has buffering capacity (maintaining a pH of solution in the range 4.2-4.8) which might contribute to its effectiveness as an ulcer treatment drug.

Studies of neutralizing properties of antacid preparations. Part 3: Constant pH neutralization of hydrochloric acid by hydrotalcite.

The neutralization reaction of hydrochloric acid by powdered hydrotalcite (HT) was studied by pH-stat method in the range of pH from 3.0 to 4.8. The neutralization process was examined by monitoring the appearance of aluminium and magnesium ions in the reaction medium, by determination of the chloride concentration in solution and by IR analysis of partially neutralized HT. The mechanism of acid neutralization of HT is discussed.

Preparation, characterization, and controlled release from coprecipitates of fluorescein and magnesium hydroxide.

Magnesium hydroxide was precipitated as a lyophobic sol in the presence of various concentrations of fluorescein sodium (3'6'-dihydroxyspiro[isobenzofuran-1(3H),9'-[9H]xanthen++ +]-3-one, disodium salt) ranging in molar equivalents between 0.1 and 2 times that of the hydroxide. Coprecipitates were washed and dried, and release of the dye and magnesium was determined (pH 7.4, 37 degrees C) from rotating disks. Release rates varied depending upon fluorescein content. The rate of dye release was retarded by less than or equal to 10(4) times that of fluorescein sodium alone, implying the existence of some form of solid association between the components of the coprecipitates. The presence of the dye in certain concentrations reduced magnesium hydroxide dissolution rates by a factor of three. Fluorescein dissolution rates, when expressed as percent release, passed through a minimum (coincident with the dye-induced reduction in Mg(OH)2 dissolution). Adsorption experiments revealed evidence for multiaffinity binding of fluorescein at the surface of freshly precipitated Mg(OH)2. Magnesium, fluorescein, and water contents of the coprecipitates were characterized by atomic absorption and UV spectroscopy and by thermogravimetric analysis. Fluorescein content increased in direct proportion to its initial concentration in solution. Controlled, but variable release of this easily assayed dye is possible by employing precipitates with different fluorescein contents.