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PubMed2002

The influence of liquid binder on the liquid mobility and preparation of spherical granules by the process of extrusion/spheronization.

The influence of the type of liquid on the movement of water and the performance of the preparation of pellets by the process of extrusion/spheronization has been studied. Liquid movement was assessed by a pressure membrane technique and by extrusion, while the pellet properties were assessed in the terms of their median size, size range (interquartile range), roundness (by a two-dimensional shape factor) and porosity. The model formulations studied were microcrystalline cellulose (MCC) and mixtures of MCC and barium sulphate at 20, 50 and 80% levels. The liquids were water, a 25% solution of glycerol in water and an anionic surfactant (sodium lauryl sulphate) below its c.m.c. and two concentrations (0.01 and 0.0001%) of a non-ionic surfactant (Pluronic PF68). The presence of the different liquids changed the ease and extent with which the liquid could be removed (drying) and reabsorbed (wetting), resulting in lower levels of saturation with the glycerol solution and considerably increased levels of saturation with the surfactants. Changes in liquid movement during extrusion, were influenced more by the level of liquid and the rate of extrusion, than by its composition. The level of liquid was also an important factor in terms of the force necessary to extrude the different formulations. For a given level of liquid, the glycerol solution tended to increase extrusion force, while the surfactant solutions tended to decrease the extrusion force. The liquid levels, particulate composition and rate of extrusion were important in terms of pellet size, size range, roundness and porosity. The low level of liquid involved produced elongated pellets. The wet formulations produced larger, agglomerated pellets with a wide particle size range and a higher porosity. The lowest porosity pellets were prepared from mixtures with no or a low barium sulphate content while the highest levels of porosity were found with equal parts MCC and barium sulphate. In general, for equivalent liquid contents, pellets made with the glycerol solution were more porous than those prepared with water while the opposite was true for pellets made with surfactants. Although the different liquids influenced water movements, they did not prevent the formation of high quality pellets by the process of extrusion/spheronization.

Algorithms↗
PubMed1998

Near-surface disposal of concentrated NORM wastes.

Naturally occurring radioactive material (NORM) in concentrated forms arises in nature and in industry where natural radioisotopes become mobile and then accumulate at particular sites. In industry this often occurs in an acidic environment, where precipitates containing radionuclides plate out onto pipe walls, filters, tank linings, etc. As the radionuclides are selectively deposited, they build up and there is a multiplying effect in terms of the radioactivity concentration. Conditions often tend to favour the build-up of radium, particularly when barium is present and can cause the co-precipitation of radium compounds. As radium is highly radiotoxic, the handling and disposal of such material requires careful management. The state of Western Australia currently has the only low level waste repository in Australia, located at Mt Walton East. To date this repository has been used predominantly to dispose of packaged radioactive waste containing artificial radioisotopes, but there is an increasing demand for the repository to accept bulk concentrated NORM wastes from mining and related industries. Already steelwork from a dismantled phosphoric acid plant and other items contaminated with NORM have been disposed of. The Mt Walton East repository is now proposed as the disposal site for 6000 tonnes per annum of gangue residue from the processing of monazite. The residue contains thorium and a small amount of radium. This paper looks at the technical and related considerations of these disposal operations.

Environmental Exposure↗
PubMed2005

Effects of divalent cations on drug encapsulation efficiency of deacylated gellan gum.

The objective of this research was to evaluate the effects of various divalent cations on the encapsulation efficiency of gellan gum and to probe the underlying mechanisms responsible for drug-loading efficiency. Spherical beads containing azathioprine were prepared from deacetylated gellan gum by ionotropic gelation method. One molar solution of various divalent chlorides (MgCl(2), BaCl(2), CaCl(2), CuCl(2) and ZnCl(2)) and two additional concentrations of CaCl(2) (2.5 M and 5.0 M) were used as ionotropic media. Drug solubility was also determined in these ionotropic media and statistically evaluated using ANOVA. Solubility in various divalent chloride solutions (1.0 M) suggests that azathioprine forms complex with Ca(2+), Zn(2+) and Cu(2+), while there might be a formation of poorly water-soluble chelates with Mg(2+) and Ba(2+) as solubility in these media were less than in deionized water. The encapsulation efficiency of gellan gum was much higher in the presence of transition elements (Cu(2+) and Zn(2+)) when compared to alkaline earth metal ions (Ca(2+), Mg(2+) and Ba(2+)). Higher concentrations of Ca(2+) decreased the encapsulation efficiency of gellan gum in a nearly proportional manner. The correlation between encapsulation efficiency and pH of the ionotropic media was negative and significant (r=-0.9574, p<0.05), although the solubility of azathioprine seems to be independent of the pH of the ionotropic medium. Overall, the results suggest that drug encapsulation efficiency of deacetylated gellan gum is largely affected by the concentration and nature of various divalent cations (e.g. atomic number, valency or electro-positivity, co-ordination property, etc.) and pH of the ionotropic medium.

Antimetabolites↗
PubMed2002

Nonselective currents and channels in plasma membranes of protoplasts from coats of developing seeds of bean.

In developing bean (Phaseolus vulgaris) seeds, phloem-imported nutrients move in the symplast from sieve elements to the ground parenchyma cells where they are transported across the plasma membrane into the seed apoplast. To study the mechanisms underlying this transport, channel currents in ground parenchyma protoplasts were characterized using patch clamp. A fast-activating outward current was found in all protoplasts, whereas a slowly activating outward current was observed in approximately 25% of protoplasts. The two currents had low selectivity for univalent cations, but the slow current was more selective for K(+) over Cl(-) (P(K):P(Cl) = 3.6-4.2) than the fast current (P(K):P(Cl) = 1.8-2.5) and also displayed Ca(2+) selectivity. The slow current was blocked by Ba(2+), whereas both currents were blocked by Gd(3+) and La(3+). Efflux of K(+) from seed coat halves was inhibited 25% by Gd(3+) and La(3+) but was stimulated by Ba(2+) and Cs(+), suggesting that only the fast current may be a component in the pathway for K(+) release. An "instantaneous" inward current observed in all protoplasts exhibited similar pharmacology and permeability for univalent cations to the fast outward current. In outside-out patches, two classes of depolarization-activated cation-selective channels were observed: one slowly activating of low conductance (determined from nonstationary noise to be 2.4 pS) and another with conductances 10-fold higher. Both channels occurred at high density. The higher conductance channel in 10 mM KCl had P(K):P(Cl) = 2.8. Such nonselective channels in the seed coat ground parenchyma cell could function to allow some of the efflux of phloem-imported univalent ions into the seed apoplast.

Barium↗
PubMed1992

Isolation, identification and pharmacological studies on three toxic metabolites from a mushroom, Hebeloma spoliatum.

Three metabolites, tentatively named HS-A, -B and -C, were isolated from a mushroom, Hebeloma spoliatum, as the fatal toxic principles to mice. HS-A was identified as 3-acetyl-2-(3'-hydroxy-3'-methyl)glutarylcrustulinol, which has been isolated from Hebeloma crustuliniforme and H. sinapizans as a cytotoxic principle. HS-B and -C were deduced to be 3,21-diacetyl-2-(3'-hydroxy-3'-methyl)glutarylcrustulinol and 3-acetyl-2-(3'-hydroxy-3'-methyl)glutarylanhydrocrustulinol, respectively, from their chemical and spectral data. Intraperitoneal administration of HS-A, -B and -C at a dose of 100 mg/kg caused death after paralysis of the limbs in mice. The compounds caused relaxation of mouse small intestine contracted by acetylcholine chloride or barium chloride treatment in vitro. They appear to exhibit a papaverine-like relaxation effect.

Animals↗
PubMed1990

Characterization of interactions of methylmercury with Ca2+ channels in synaptosomes and pheochromocytoma cells: radiotracer flux and binding studies.

The interaction of methylmercury (MeHg) with neuronal Ca2+ channels in rat forebrain synaptosomes and dihydropyridine (DHP)-sensitive Ca2+ channels in rat pheochromocytoma (PC12) cells was examined using radiotracer flux assays and radioligand binding analyses. In synaptosomes, the influx of 45Ca2+ was used to examine the voltage and state dependence of block of Ca2+ channels by MeHg, as well as the effects of MeHg on apparent inactivation of 45Ca2+ influx. In addition, the differential influx of 45Ca2+, 85Sr2+, and 133Ba2+ was used to examine the effect of MeHg on the ionic selectivity of synaptosomal Ca2+ channels. The ability of MeHg to block 45Ca2+ influx via a DHP-sensitive Ca2+ channel was examined in PC12 cells. Effects of MeHg on binding of [3H]nitrendipine in synaptosomes and 125I-omega-conotoxin GVIA (CgTx) in synaptosomes and PC12 cells were measured. In synaptosomes, MeHg blocked 45Ca2+ influx in a voltage-dependent manner, inasmuch as increasing the extracellular K+ concentration increased the magnitude of block by 100 microM MeHg. When synaptosomes were incubated for 10 sec in either a nondepolarizing or a depolarizing solution before measurement of 1 sec of depolarization-induced 45Ca2+ influx, the potency and efficacy of the block of 45Ca2+ influx by MeHg were similar. Thus, block of Ca2+ channels by MeHg does not appear to be state dependent. To determine the kinetics of apparent inactivation of 45Ca2+ influx, synaptosomes were predepolarized in Ca2(+)-free high [K+] solution, for intervals varying from 1 to 10 sec, before measurement of 1 sec of K(+)-induced 45Ca2+ influx. When compared with control, MeHg (100 microM) altered the rate constant for apparent inactivation and decreased the fraction of 45Ca2+ influx that does not inactivate. Influx of 45Ca2+, 85Sr2+, and 133Ba2+ during 1 sec of depolarization was blocked in a dose-dependent manner by MeHg, with estimated IC50 values of 125, 150, and greater than 150 microM for 45Ca2+, 85Sr2+, and 133Ba2+, respectively. In triple-label experiments, the relative flux of radiolabeled Ca2+:Sr2+:Ba2+ was altered from approximately 6:2:3 to 6:1:3 in the presence of 100 microM MeHg. In undifferentiated and nerve growth factor-differentiated PC12 cells, K(+)-induced 45Ca2+ influx was blocked by the DHP nifedipine, with an approximate IC50 value of 5 nM. MeHg reduced 45Ca2+ influx in PC12 cells with an estimated IC50 value of 50 microM, and 125 microM MeHg reduced uptake by greater than 90%. [3H]Nitrendipine bound to synaptosomes with high affinity in normal and elevated [K+] solutions.(ABSTRACT TRUNCATED AT 400 WORDS)

Adrenal Gland Neoplasms↗
PubMed1997

Synthesis and Characterization of New Alkoxotitanates of Yttrium, Barium, and Copper: Single Crystal X-ray Diffraction Structures of Cl(2)Y{Ti(2)(OPr(i))(9)}, {Ti(OPr(i))(5)}Ba{Ti(2)(OPr(i))(9)}, and ClCu{Ti(2)(OPr(i))(9)}

The synthesis and characterization of new mixed-metal alkoxides of titanium with yttrium, barium, and copper, achieved via salt elimination and acid-base reactions, is described. The metathesis reactions of KTi(2)(OPr(i))(9) with anhydrous YCl(3) (1:1 and 2:1) and CuCl(2) (1:1) afford chloro-functionalized heterobimetallic alkoxides Cl(2)Y{Ti(2)(OPr(i))(9)} (1), ClY{Ti(2)(OPr(i))(9)}(2) (2), and ClCu{Ti(2)(OPr(i))(9)} (3), respectively, in high yields. The barium-titanium derivatives [Ba{Ti(2)(OPr(i))(10)}](2) (4), {Ti(2)(OPr(i))(9)}Ba{Ti(OPr(i))(5)} (5), and Ba{Ti(2)(OPr(i))(9)}(2) (6) result from the reaction between [Ba(OPr(i))(2)](n) and Ti(OPr(i))(4) in 1:2, 1:3, and 1:4 molar ratios, respectively. All the new derivatives (1-6) have been characterized by elemental analyses, variable-temperature (1)H and (13)C NMR, infrared spectroscopy, cryoscopy, and single crystal X-ray diffraction studies for 1, 3, and 5. The crystallographic study of 1 reveals a mononuclear species where the yttrium atom, coordinated by four alkoxide oxygen atoms of the {Ti(2)(OPr(i))(9)}(-) unit and two chloride ligands, is in a pseudo-octahedral arrangement. The NMR ((1)H and (13)C) and cryoscopic data for 1 indicate that the bioctahedral {Ti(2)(OPr(i))(9)} framework, as observed in the solid state structure, is retained in solution also. The X-ray structure of copper derivative 3 exhibits a triangular heterometallic core CuTi(2)(&mgr;(2)-OPr(i))(3)(&mgr;(3)-OPr(i))(2) with chloride as a terminal ligand on copper. Each titanium bears two terminal OPr(i) groups and displays a distorted octahedral geometry whereas copper has a pseudotrigonal bipyramidal environment. The high-temperature NMR studies for the paramagnetic 3 are in agreement with Curie law behavior; the isotropic shifts indicate that the OPr(i) groups bound directly to the Cu(II) center experience a greater paramagnetic influence in comparison to OPr(i) groups attached to titanium only. Barium titanates reveal an interesting observation of structural and stoichiometry (Ba/Ti) change. The dimeric compound 4 (Ba/Ti, 1:2) reacts with 1 mol of Ti(OPr(i))(4) to offer mononuclear 5 with a Ba/Ti stoichiometry of 1:3; on further addition of 1 mol of Ti(OPr(i))(4), 5 is converted to 6 (Ba/Ti, 1:4). X-ray crystallography performed on 5 shows the molecular structure to be formed by the coordination of monoanionic {Ti(OPr(i))(5)}(-) and {Ti(2)(OPr(i))(9)}(-) units to Ba(2+) in bi- and tetradentate fashion, respectively. The coordination figure of the central atom, barium, corresponds to a trigonal prism distorted toward an octahedron. Crystal data for 1: monoclinic space group Cc, a = 21.618(14) Å, b = 9.878(5) Å, c = 19.949(13) Å, beta = 109.51(4) degrees, V = 4015(4) Å(3), Z = 4. Crystal data for 3: triclinic space group P&onemacr;, a = 10.085(2) Å, b = 10.210(2) Å, c = 21.551(4) Å, alpha = 84.40(3) degrees, beta = 84.03(3) degrees, gamma = 60.86(3) degrees, V = 1924.9(6) Å(3), Z = 2. Crystal data for 5: triclinic space group P&onemacr;, a = 11.850(2)Å, b = 13.888(3) Å, c = 18.716(4) Å, alpha = 86.08(3) degrees, beta = 89.15(3) degrees, gamma = 83.36(3) degrees, V = 3052.3(11) Å(3), Z = 4.

Journal Article↗
PubMed2005

Cluster models and ab initio calculations of (19)F NMR isotropic chemical shifts for inorganic fluorides.

(19)F NMR isotropic chemical shift (delta(iso)) calculations are performed in crystallized compounds using the GIAO method with the B3LYP hybrid functional at DFT level. Clusters centered on the studied fluorine atoms mimic the crystalline structures. The 6-311+G(d) basis set is chosen for the central fluorine atom, and the LanL2DZ basis set for the others. The metal atoms are described by the 3-21G(2d) basis set or, when not available, by the CRENBL basis set with the corresponding ECP, and augmented with 2d polarization functions when existing. First, for high-symmetry systems (MF, MF(2), and MF(3) compounds), a systematization of the cluster building up from coordination spheres is proposed, generalized to fluoroperovskites and fluoroaluminates KAlF(4) and RbAlF(4). When applied to rather low symmetry systems such as barium fluorometalates BaMgF(4), BaZnF(4), and Ba(2)ZnF(6), the definition of the coordination spheres is far from easy. Then, for structures built up from a MF(6) octahedron network, we may define different "starting clusters": [FM(2)F(8)] for the shared fluorine atoms, [FMF(4)] for the unshared ones, and [FBa(4)](7+) for the "free" ones. Analogous "starting clusters" are then tested on compounds from the NaF-AlF(3), BaF(2)-AlF(3), and CaF(2)-AlF(3) binary systems and for alpha-BaCaAlF(7) that are also built up from a MF(6) octahedron network. For each of these corresponding fluorine sites, delta(iso) values are calculated with the "starting clusters" and several larger clusters and compared to the experimental delta(iso) values. For the barium-containing clusters, the RMS deviation is equal to 51 ppm. It is suggested that this result may be related to the poor quality of the barium basis sets for which no polarization functions are available for the moment. In total, chemical shifts were calculated for 122 fluorine sites, in a various range of compounds. For the clusters without barium, the ab initio method leads to a RMS equal to 22 ppm, which is a quite nice result keeping in mind that the (19)F chemical shift range is larger than 200 ppm.

Journal Article↗
PubMed1989

Cytotoxic and neoplastic transforming effects of industrial hexavalent chromium pigments in Syrian hamster embryo cells.

Twenty eight moderately water-soluble to insoluble chromium (VI) compounds, such as zinc and lead chromate, industrial and laboratory synthesized pigments, and the analytical reagents strontium, barium and calcium chromate, were physicochemically characterized and studied for cytotoxicity and morphological transformation in cultured Syrian hamster embryo (SHE) cells. In vivo validation of malignancy of transformed SHE cells was performed. A high physicochemical diversity among the complex chromium pigments was revealed. The solubility of the compounds was greatly increased after incubation in a complete medium and even higher under cell culture conditions. The cytotoxic effects appeared to be due principally to extracellular solubilized chromium because the most solubilized compounds. Zn, Ca and Sr chromates, were equitoxic at about the same Cr concentration treatment and 8-fold more cytotoxic than less soluble compounds such as some Pb chromates and Ba chromate. However, certain physicochemical properties of lead chromate pigments could also influence their cytotoxic activity. All test compounds were, in a dose-dependent manner, efficient in inducing morphological transformation of SHE cells. Many of the Cr pigments, although physicochemically different, were similarly effective in transformation induction. Nevertheless, compounds among Zn and Pb chromates had various transforming potencies. Ba chromate was the least active in inducing transformation. Certain physicochemical properties could mediate the transforming activity but no particular relationship could be established between any one of the physicochemical parameters and the transforming potency. Cloned morphologically-transformed colonies of SHE cells were grown in soft agar medium and showed true neoplastic behaviour by tumour formation in syngeneic animals. These results show that various chromate pigments containing either Zn or Pb, of medium to very low aqueous solubility, induced neoplastic transformation of SHE cells.

Animals↗
PubMed2004

Correlation between 19F environment and isotropic chemical shift in barium and calcium fluoroaluminates.

High-speed MAS (19)F NMR spectra are recorded and reconstructed for 10 compounds from BaF(2)-AlF(3) and CaF(2)-AlF(3) binary systems which leads to the determination of 77 isotropic (19)F chemical shifts in various environments. A first attribution of NMR lines is performed for 8 compounds using a superposition model as initially proposed by B. Bureau et al. The phenomenological parameters of this model are then refined to improve the NMR line assignment. A satisfactory reliability is reached with a root-mean-square (RMS) deviation between calculated and measured values equal to 6 ppm. The refined parameters are then successfully tested on alpha-BaCaAlF(7) whose structure was recently determined. Finally, the isotropic chemical shift ranges are defined for shared, unshared, and "free" fluorine atoms encountered in the investigated binary systems. So, the fluorine surroundings can be deduced from the NMR line positions in compounds whose structure is unknown. Such an approach can also be applied to fluoride glasses.

Journal Article↗