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In an attempt to improve bifunctional chelate labelling of Mab, we investigated the use of a polyamino acid backbone for multiple DTPA substitutions. Poly-L-lysine (PL) (3.8 Kd, n = 25) was partially acetylated with MADTPA to yield 11 moles of DPTA per mole of PL. The average numbers of DTPA on PL were directly quantified with MADTPA-C-14. The remaining epsilon amino groups on PL-DTPA (I) were measured with TNBS reagent. A selective maleimide derivatization of (I) with S-SMPB yielded (II), which contains 2.3 moles of maleimide groups per mole of (I). The sulfhydryl activation of Mab-TP41.2F(ab')2 with 2-Iminothiolane hydrochloride produced (III), containing 1.3 moles of sulfhydryl groups per mole of Mab. Compounds (II) and (III) were combined to form a single thioether-spaced chain linkage of Mab-PL-DTPA (IV), which was subsequently chelated with 111In to yield (V), which was the compound of interest. Indium-111-PL-DTPA (VI) and 111In-DTPA-MabTP41.2F(ab')2 (VII) also were prepared for control studies. Direct cell binding assay revealed the mean immunoreactivity of (V) to be 79.4% and that of (VII) to be 39.5%. In a biodistribution study on melanoma tumor-bearing athymic mice at 4, 24, and 48 hr postinjection, the tumor/blood and tumor/liver ratios at 48 hr were 11.6 and 1.2 for (V), compared to 3.7 and 0.13, respectively, with (VII). Thus, the PL configuration for radiolabeled antibodies seems to result in decreased hepatic accumulation and retained tumor activity. The findings suggest that further studies of this new compound are warranted.
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PMID:Reduced hepatic accumulation of radiolabeled monoclonal antibodies with indium-111-thioether-poly-L-lysine-DTPA-monoclonal antibody-TP41.2F(ab')2. 155 42

The thermotropic behavior of multilamellar liposomes prepared from mixtures of sulfatide and dipalmitoylphosphatidylcholine has been studied by DTA calorimetry. The cooperative unit size and the enthalpy change of the main transition decrease concomitant with the increase of the sulfatide-phospholipid mole ratio. The origin of these effects and their dependence on the sulfatide content suggest that the in-plane distribution of sulfatide and the physical state of the lipid bilayer are affected by the sulfatide-phospholipid mole ratio.
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PMID:Thermotropic behavior of dipalmitoylphosphatidylcholine-sulfatide liposomes. 689 86

Crystallization kinetics studies for six experimental glass formulations in the system Na2O-CaO-SiO2-P2O5 synthesized by wet chemistry were conducted by means of differential thermal analysis. These glasses had CaO/P2O5 and SiO2/ (CaO + Na2O) ratios ranging from 8.74-3.38 and 0.92-3.03, respectively. Samples of each glass (n = 30 were heated from 23 to 1250 degrees C under N2 atmosphere at heating rates ranging from 10 to 50 degrees C/min. Glass-ceramics were obtained after heat treating the initial glasses at temperatures determined from their DTA exotherms. The activation energy of crystallization for each glass composition was calculated from an expression-relating log-heating rate and the reciprocal of the exothermic peak temperature. The compositions of the six glasses were significantly different (p = 0.05). The activation energy of crystallization (Q) values ranged from 196 to 782 kJ/mole. A correlation was obtained between Q and CaO/P2O5 and between Q and the Young's modulus (P < 0.001). Two of the six glasses exhibited bulk crystallization. X-ray diffraction studies showed that four of the six glasses exhibited different proportions of crystalline phases following heat treatment. These phases were wollastonite (CaSiO3), Na2CaSi3O9, combeite [Na4Ca3SI6O16(OH)2], and some unidentifiable phases. Two of the six bioceramic materials had a mixture of unknown crystalline phases.
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PMID:Crystallization of experimental bioactive glass compositions. 886 80

Rare earth binary complex Eu(NNA)3 (NNA, alpha-naphthylacetic acid), ternary complex Eu(NNA)3.phen (phen, 1,10-phenanthroline) and a series of dinuclear complexes with different mole ratios of Eu3+ to Gd3+ were synthesized. Many advanced approaches, such as element analysis, FTIR spectra, TG and DTA analysis, were used to determine the composition and structure of binary and ternary complex. Moreover, their fluorescence properties were studied by fluorescent spectra and lifetimes. The fluorescence spectra and decay curves of dinuclear complexes indicated that the fluorescence emission intensity was enhanced and the fluorescence lifetime was prolonged by Gd3+. The dinuclear complexes show the best properties when the mole ratio of Eu3+ to Gd3+ is 6:4. A new parameter Y, which was used to evaluate the effect of Gd3+, was introduced. In addition, the relationship of Y value and mole fraction of Gd3+ was analyzed by mathematical software. The results showed that Y value decreased by single exponential mode when the content of Gd3+ decreased.
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PMID:Synthesis and fluorescence properties of rare earth (Eu3+ and Gd3+) complexes with alpha-naphthylacetic acid and 1,10-phenanthroline. 1630 32

Cryogenic transmission electron microscopy (cryoTEM) was used to study the structures formed in mixtures of sodium dodecylsulfate (SDS) and dodecyltrimethylammonium bromide (DTAB) in dilute aqueous solutions with 0-300 mM NaBr. The DTAB mole fraction, X, was in the range 0.2-0.4, limited at 25 degrees C by precipitation of solid DTA-DS at X=0.38 without salt to X=0.25 at 300 mM NaBr. At a total surfactant concentration of 100 mM the samples separated into two liquid phases (the bottom phase birefringent) within a narrow (+/-0.01 mole fraction units) composition range. At the mid-point X varied from 0.32 without salt to 0.22 at 300 mM NaBr. Elemental analysis of C, S, O, and N in the separated phases of a sample with 100 mM NaBr and X=0.26 showed the top phase to contain almost only SDS at a low concentration, 14 mM, and the bottom phase 175 mM total surfactant, with X=0.27. Elemental analysis on samples without added salt gave erratic results, indicating problems in the physical separation of the phases. The cryoTEM survey of the separated phases revealed similar problems. Without salt both phases showed similar structures, whereas the top phase in the sample with added salt was void of structures larger than small micelles. The cryoTEM survey revealed a variety of structures being simultaneously present in most samples. A general trend with increasing X was an evolution from globular micelles, over disks, bands, branched bands transforming into sparse webs, perforated bilayer structures, and finally smooth bilayers. Increasing salt and total surfactant concentrations resulted in the emergence of structures with smaller mean curvature at lower X. Perforated bilayers were found in samples with 100 mM or less of added salt, and usually persisted to DTAB contents where precipitates appeared. The porous bilayers seemed to derive from sparse webs of band-like structures, and the hole size decreased with increasing X and salt concentration. Two types of recurrent structures were noticed: blastula aggregates, seemingly an intermediate structure transforming crumpled bilayers into vesicles of similar size (diameter 400-500 A), observed over a broad range of conditions, and at 100 mM total surfactant concentration and 50 mM added salt or more a type of regular disks with a diameter of 180+/-30 A.
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PMID:Stomatosomes, blastula vesicles and bilayer disks: morphological richness of structures formed in dilute aqueous mixtures of a cationic and an anionic surfactant. 1905 97

(Solid + liquid) phase equilibria (SLE) for the binary systems, ionic liquid (IL) 1-butyl-3-methylimidazolium thiocyanate [BMIM][SCN] with an alcohol (1-octanol, 1-nonanol, 1-decanol, 1-undecanol, or 1-dodecanol) or water, and (liquid + liquid) phase equilibria (LLE) for the binary systems of [BMIM][SCN] with an alkane (n-hexane, n-heptane, n-octane, n-nonane, or n-decane), benzene, an alkylbenzenes (toluene or ethylbenzene), tetrahydrofuran (THF), cycloalkanes (cyclohexane or cycloheptane), or ethers (di-n-propyl ether, di-n-butyl ether, di-n-pentyl ether, n-butylmethyl ether, tert-butylmethyl ether (MTBE), or tert-butylethyl ether (ETBE)) have been determined at ambient pressure. A dynamic method was used over a broad range of mole fractions and temperatures from 250 to 430 K. In the case of systems IL + alkane, cycloalkane, or ether, the mutual immiscibility with an upper critical solution temperature (UCST) was detected, and in the systems of IL + benzene, alkylbenzene, or THF, the mutual immiscibility with a lower critical solution temperature (LCST) was observed. UV-vis spectroscopy was used to determine the very small compositions of the IL in the n-hexane (about 2 x 10(-5) IL mole fraction), benzene (about 2 x 10(-3) IL mole fraction), cyclohexane (about 2 x 10(-5) IL mole fraction), and THF (about 1.2 x 10(-2) IL mole fraction). For the binary systems containing alcohol, it was noticed that with increasing chain length of an alcohol, the solubility decreases. The basic thermal properties of the pure IL, that is, the glass-transition temperature as well as the heat capacity at the glass-transition temperature, have been measured using a differential scanning microcalorimetry technique (DSC). Decomposition of the IL was detected by the simultaneous TG/DTA experiments. Well-known UNIQUAC, Wilson, and NRTL equations have been used to correlate the experimental SLE data sets for alcohols and water. For the systems containing immiscibility gaps {IL + alkane, benzene, alkylbenzene, cycloalkane, tetrahydrofuran, or ether}, the parameters of the LLE correlation have been derived using the NRTL equation.
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PMID:Phase equilibria study of the binary systems (1-butyl-3-methylimidazolium thiocyanate ionic liquid + organic solvent or water). 1940 27

Liquid-liquid phase equilibria (LLE) of binary mixtures containing a room-temperature ionic liquid N-hexylisoquinolinium thiocyanate, [HiQuin][SCN] with an aliphatic hydrocarbon (n-hexane, n-heptane), aromatic hydrocarbon (benzene, toluene, ethylbenzene, n-propylbenzene), cyclohexane, thiophene, water, and 1-alcohol (1-ethanol, 1-butanol, 1-hexanol, 1-octanol, 1-decanol) have been determined using a dynamic method from room temperature to the boiling-point of the solvent at ambient pressure. N-hexylisoquinolinium thiocyanate, [HiQuin][SCN] has been synthesized from N-hexyl-isoquinolinium bromide as a substrate. Specific basic characterization of the new compound including NMR spectra, elementary analysis, and water content have been done. The density and viscosity of pure ionic liquid were determined over a wide temperature range from 298.15 to 348.15 K. The mutual immiscibility with an upper critical solution temperature (UCST) for the binary systems {IL + aliphatic hydrocarbon, cyclohexane, or water} was detected. In the systems of {IL + aromatic hydrocarbon or thiophene} an immiscibility gap with a lower critical solution temperature (LCST) was observed. Complete miscibility in the liquid phase, over a whole range of ionic liquid mole fraction, was observed for the binary mixtures containing IL and an 1-alcohol. For the tested binary systems with immiscibility gap {IL + aliphatic hydrocarbon, aromatic hydrocarbon, cyclohexane, thiophene, or water}, the parameters of the LLE correlation have been derived using the NRTL equation. The basic thermal properties of the pure IL, that is, the glass-transition temperature as well as the heat capacity at the glass-transition temperature, have been measured using a differential scanning microcalorimetry technique (DSC). Decomposition of the IL was detected by simultaneous thermogravimetric/differential thermal analysis (TG/DTA) experiments.
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PMID:Phase equilibria study of the binary systems (N-hexylisoquinolinium thiocyanate ionic liquid + organic solvent or water). 2242 76

LaCrO3 was prepared by using the polymeric precursor method for use as a receptor material and its NOx sensing characteristics were investigated. Nano-LaCrO3 powders were synthesized at the optimum compositions of the mole ratio of [La-, Cr-source]:[EG]:[AcAc] = [a, a]:[160 a]:[8 a] with 1 wt% polyvinylpyrrolidone (PVP) using ethylene glycol (EG) as a solvent, acetyl acetone (AcAc) as a chelating agent, and PVP as a polymer additive. The thermal decomposition behavior, crystal structure, morphology, and particle sizes of nano powders were characterized by a thermal analysis (TG-DTA), X-ray diffraction (XRD), a field emission scanning electron microscopy (FE-SEM), and a particle size analyzer, respectively LaCrO3 powders were mainly orthorhombic in structure and the primary particle size was 30 nm according to the XRD results. All solid-state compact impedancemetric-type sensor devices composed of Li1.5Al0.5Ti1.5(PO4)3 (LATP) as a transducer and a perovskite-type LaCrO3 nano powder as a receptor, have been investigated for their ability to detect NOx (NO and NO2) in the range of 1-250 ppm at 400 degrees C. The sensor device showed high gas sensitivities at NO gas, but relatively low gas sensitivities for NO2 gas.
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PMID:Fabrication of nano-LaCrO3 receptor by polymeric precursor method and its impedancemetric NOx sensing properties. 2262 9

Recently, we reported a unique and nearly ubiquitous phenomenon of inducing simple and complex coacervation in solutions of a broad variety of individual and mixed amphiphiles and over a wide range of concentrations and mole fractions. This paper describes a novel type of biphasic separation in aqueous solutions of mixed cationic-anionic (catanionic) surfactants induced by hexafluoroisopropanol (HFIP). The test cases included mixtures of cetyltrimethylammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) (surfactants with different carbon chain lengths) as well as dodecyltrimethylammonium bromide (DTAB) with SDS (surfactants with the same carbon chain lengths). The CTAB-SDS-HFIP coacervate systems can be produced at many different mole ratios of surfactant, but DTAB-SDS-HFIP formed only coacervates at equimolar (1:1) mole ratios of DTAB and SDS. The phase-transition behavior of both systems was studied over a wide range of surfactant and HFIP concentrations at the stoichiometric (1:1) mole ratio of cationic/anionic surfactants. The chemical compositions of each of the two phases (aqueous-rich and coacervate phases) were studied with regard to the concentrations of HFIP, water, and individual surfactants. It is revealed that the surfactant-rich phase (coacervate phase) contains a large percentage of fluoroalcohol relative to the aqueous phase and is enriched in both surfactants but contains a small percentage of water. Surprisingly, the concentration of water in the coacervate phase increases as the total HFIP concentration is increased while the concentration of HFIP in the coacervate phase remains relatively constant, which means a larger amount of water associated with HFIP molecules is extracted into the coacervate phase, which results in the growth of the phase. The volume of the coacervate phase increases with an increase in surfactant concentration and total HFIP %. The coacervate phase is highly enriched in the two amphiphilic ions (DTA(+) and DS(-)) whereas the two counterions (Br(-) and Na(+)) primarily reside in the aqueous-rich phase. The results suggest the formation of a catanionic complex in the coacervate phase through ion pairing with a concomitant release of the surfactant counterions (Na(+) and Br(-)) into the aqueous-rich phase. Finally, the fluorocarbon alcohol systems are contrasted with the effects of aliphatic alcohols in the mixed catanionic surfactant systems. Isopropanol does not have the same interactions as HFIP with respect to solubilization, aggregation, and phase separation of the oppositely charged surfactants.
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PMID:Perfluorinated Alcohols Induce Complex Coacervation in Mixed Surfactants. 2688 98

Some novel transition metal [Cu (II), Ni (II) and Co (II)] complexes of nalidixic acid hydrazone have been prepared and characterized by employing spectro-analytical techniques viz: elemental analysis, 1H-NMR, Mass, UV-Vis, IR, TGA-DTA, SEM-EDX, ESR and Spectrophotometry studies. The HyperChem 7.5 software was used for geometry optimization of title compound in its molecular and ionic forms. Quantum mechanical parameters, contour maps of highest occupied molecular orbitals (HOMO) and lowest unoccupied molecular orbitals (LUMO) and corresponding binding energy values were computed using semi empirical single point PM3 method. The stoichiometric equilibrium studies of metal complexes carried out spectrophotometrically using Job's continuous variation and mole ratio methods inferred formation of 1:2 (ML2) metal complexes in respective systems. The title compound and its metal complexes screened for antibacterial and antifungal properties, exemplified improved activity in metal complexes. The studies of nuclease activity for the cleavage of CT- DNA and MTT assay for in vitro cytotoxic properties involving metal complexes exhibited high activity. In addition, the DNA binding properties of Cu (II), Ni (II) and Co (II) complexes investigated by electronic absorption and fluorescence measurements revealed their good binding ability and commended agreement of Kb values obtained from both the techniques. Molecular docking studies were also performed to find the binding affinity of synthesized compounds with DNA (PDB ID: 1N37) and "Thymidine phosphorylase from E.coli" (PDB ID: 4EAF) protein targets.
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PMID:Spectro Analytical, Computational and In Vitro Biological Studies of Novel Substituted Quinolone Hydrazone and it's Metal Complexes. 2916 79


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