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At least 757 records · Page 42Linked to original sources
PubMed2007

High-precision determination of 18O/16O ratios of silver phosphate by EA-pyrolysis-IRMS continuous flow technique.

A high-precision, and rapid on-line method for oxygen isotope analysis of silver phosphate is presented. The technique uses high-temperature elemental analyzer (EA)-pyrolysis interfaced in continuous flow (CF) mode to an isotopic ratio mass spectrometer (IRMS). Calibration curves were generated by synthesizing silver phosphate with a 13 per thousand spread in delta(18)O values. Calibration materials were obtained by reacting dissolved potassium dihydrogen phosphate (KH(2)PO(4)) with water samples of various oxygen isotope compositions at 373 K. Validity of the method was tested by comparing the on-line results with those obtained by classical off-line sample preparation and dual inlet isotope measurement. In addition, silver phosphate precipitates were prepared from a collection of biogenic apatites with known delta(18)O values ranging from 12.8 to 29.9 per thousand (V-SMOW). Reproducibility of +/- 0.2 per thousand was obtained by the EA-Py-CF-IRMS method for sample sizes in the range 400-500 microg. Both natural and synthetic samples are remarkably well correlated with conventional (18)O/(16)O determinations. Silver phosphate is a very stable material and easy to degas and, thus, could be considered as a good candidate to become a reference material for the determination of (18)O/(16)O ratios of phosphate by high-temperature pyrolysis.

Animals↗
PubMed1993

Calcitonin induces a decreased Na+ conductance in identified neurons of Aplysia.

The ionic mechanism of the effect of extracellularly ejected calcitonin (CT) on the membrane of identified neurons R9 and R10 of Aplysia was investigated with voltage-clamp, micropressure ejection, and ion substitution techniques. Micropressure-ejected CT caused a marked hyperpolarization in the unclamped neuron. Heat-inactivated CT was without effect. Clamping the same neuron at its resting potential level (-60 mV) and re-ejecting CT with the same dose produced a slow outward current (Io(CT), 30-40 sec in duration, 4-6 nA in amplitude) associated with a decrease in input membrane conductance. Io(CT) was decreased by depolarization and increased by hyperpolarization. The extrapolated reversal potential of Io(CT) was approximately +10 mV. Io(CT) was sensitive to changes in the external Na+ concentration but not to changes in K+, Ca2+, and Cl- concentrations. Micropressure-ejected forskolin produced a slow outward current, which, like the current to CT, was associated with a decrease in input membrane conductance, and was sensitive to changes in the external Na+ concentration. Io(CT) was prolonged by bath-applied isobutylmethylxanthine (IBMX) but was not affected by 1-oleoyl-2-acetylglycerol (OAG) and calphostin C. Neither superfusion of the neuron with nordihydroguaiaretic acid (NDGA) nor superfusion with indomethacin caused any changes in Io(CT). These results suggest that extracellular CT can induce a slow outward current associated with a decrease in Na+ conductance, mediated by a receptor-controlled increase in intracellular cyclic adenosine 3',5'-monophosphate.

1-Methyl-3-isobutylxanthine↗
PubMed1987

[Supplementary methods for the determination of the Gram reaction of anaerobic pathogens].

Anaerobic microorganisms (364 gram-negatives and 154 gram-positives) were investigated with respect to their behaviour against aqueous solutions of potassium hydroxide as well as their sensitivity to polymyxin and vancomycin by means of the disk diffusion test. Whereas the gram-negative anaerobes showed a good correlation (97.5%) with a positive KOH test, only 88.3% of the gram-positive microorganisms exhibited a negative KOH reaction. Therefore, in cases of ambiguous gram-negative staining results, the KOH test alone cannot give sufficient informations about the exact gram reaction. It was shown, however, that together with the determination of resistance to polymyxin and vancomycin, this uncertainty remains only for microorganisms showing a positive KOH reaction, polymyxin resistance, and vancomycin sensitivity. Therefore, in combination with the polymyxin and vancomycin disk diffusion test, the KOH test is recommended as an additional means to determine the gram reaction of anaerobes.

Bacteria, Anaerobic↗
PubMed1997

Optimization of catalase biosynthesis in submerged cultures of Aspergillus niger mutant.

The effect of some medium components, viscous substances and metabolic inhibitors, on catalase production by mutant Aspergillus niger has been studied in shake culture. Altering the composition of the basal medium, particularly substituting NaNO3 for KNO3, and peptone for yeast extract brought an increase in extra- and intracellular catalase activity by 1.5- and 3-fold, respectively. The addition of 2.0-6.0 mg sodium alginate or pectin/ml as viscous additive to the medium, containing glucose as carbon source, increased the medium viscosity and catalase production in shake culture by about 2.8- to 3.0-fold. The highest yield of extracellular catalase activity of A. niger was obtained in the presence of sodium orthovanadate and Triton X-100, which improved the activity of this enzyme by about 1.5-2.2-fold. A significant increase in intracellular catalase activity was observed in the presence of hematin, Tween 80 and sodium orthovanadate (1.7-, 1.6- and 1.4-fold respectively). The time course of growth and enzyme production by A. niger in the optimized medium is also reported.

Alginates↗
PubMed1981

Effect of combined nitrogen sources on heterotrophic growth of a blue-green alga Westiellopsis prolifica.

The autotrophic and photoheterotrophic growth of light pre-treated and dark pre-treated strains of Westiellopsis prolifica was decreased in the presence of NH4+, NO3-- and urea in the culture medium. On dark incubation, after pre-treatment with light as well as in the dark, the alga showed better growth response to all the combined nitrogen sources. However, only the light pre-treated strain of the organism utilized the exogenous nitrogen sources appreciably for its dark heterotrophic growth.

Ammonium Chloride↗
PubMed1994

Estimation of material properties in the equine metacarpus with use of quantitative computed tomography.

The purpose of this study was to investigate the relationships between data obtained from quantitative computed tomography and mechanical properties in the equine metacarpus, as measured in vitro in bone specimens. Three hundred and fifty-five bone specimens from the metacarpi of 10 horses were machined into right cylinders aligned with the long axis of the bone. A computed tomographic scan of the specimens, along with a Cann-Genant K2HPO4 calibration standard, was obtained. The specimens then were compressed to failure, and the elastic modulus, yield stress, yield strain, strain energy density at yield, ultimate stress, ultimate strain, and strain energy density at ultimate failure were calculated. The specimens were dried and ashed. Quantitative computed tomography-derived K2HPO4 equivalent density proved to be an excellent estimator (r2 > 0.9) of elastic modulus, yield stress, ultimate stress, wet density, dry density, and ash density; a moderately good estimator (0.4 < r2 < 0.9) of strain energy density at yield and at ultimate failure; and a poor estimator (r2 < 0.2) of yield strain and ultimate strain. It was concluded that the relationships between quantitative computed tomography data and mechanical properties of the equine metacarpus were strong enough to justify the use of these data in automated finite element modeling.

Animals↗
PubMed2002

The effect of salts on the micellization temperature of aqueous poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide) solutions and the dissolution rate and water diffusion coefficient in their corresponding gels.

Studies were performed to examine the effect of ionic salts on phase transitions, dissolution rates, and diffusion coefficients of water in gels of poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide) with polymer concentrations ranging from 22 to 32% w/w and salt concentrations ranging from 0 to 1.5% w/w. Salts tested include Na(3)PO(4), Na(2)SO(4), Na(2)HPO(4), NaH(2)PO(4), NaCH(3)CO(2), NaCl, and KI. Micellization transition temperatures were obtained using differential scanning calorimetry. The dissolution rates were obtained by measurement of the surface erosion rates, and diffusion coefficients were obtained by using a method to analyze the intrusion of water into the aqueous gels. It was found that salts had no effect on the dissolution rate of the polymer gels into deionized water. However, when the salt concentration in the aqueous dissolution media was adjusted to match the concentration in the gels, the dissolution rate of the polymer gel decreased with increasing salt concentration. The salts also had a profound effect on the critical micellization temperature (CMT) and the diffusion coefficient of water within the gel. The diffusion coefficient and CMT decreased in the presence of salts. The magnitude of these effects was comparable to their placement on the Hofmeister, or lyotropic series for salts. The effects of polymer and salt concentrations on the CMT were quantified, and a single correlation was proposed to predict the micellization temperatures for a wide range of salt and polymer concentrations.

Diffusion↗
PubMed2004

The stability of 2-acetoxy-4-trifluoromethylbenzoic acid (Triflusal) in micellar pseudophase.

The new platelet antiaggregant Triflusal or 2-acetoxy-4-trifluoromethylbenzoic acid presents a structural analogy to acetylsalicylic acid (ASA). Alkaline hydrolysis of triflusal was studied in the presence and absence of cationic micelles of N-cetyl-N-ethyl-N,N-dimethylammonium bromide (CDEABr) at different KOH concentrations and different temperatures (25, 30, and 37 degrees C) using a spectrophotometric method. The influence of potassium bromide concentration upon alkaline hydrolysis at 25 degrees C is also discussed. At constant [KOH] pseudofirst-rate constant (k(obs)) decreased with increasing [CDEABr] at concentrations greater than the CMC and also decreased with increasing [KBr] at constant [KOH] and [CDEABr]. To explain the effect of cationic micelles of CDEABr upon alkaline hydrolysis, the pseudophase ion exchange model was used. The values of the micellar properties such as the critical micelle concentration, the degree of micellar ionization and the neutralized fraction of the head group obtained by conductivity measurements were determined previously.

Algorithms↗
PubMed2004

Highly accurate nephelometric titrimetry.

A method that accurately indicates the end-point of precipitation reactions by the measurement of the relative intensity of the scattered light in the titrate is presented. A new nephelometric titrator with an internal nephelometric sensor has been devised. The work of the titrator including the sensor and change in the turbidity of the titrate and intensity of the scattered light are described. The accuracy of the nephelometric titrimetry is discussed theoretically. The titration of NaCl with AgNO(3) serves as a model. A relative error as well as deviation is within 0.2% under the experimental conditions. The applicability of the titrimetry in pharmaceutical analyses, for example, phenytoin sodium and procaine hydrochloride, is generally illustrated.

Chemistry, Pharmaceutical↗
PubMed2004

Effects of potassium bromide disk formation on the infrared spectra of dried model proteins.

The most common method of sample preparation for Fourier transform infrared spectroscopic analysis of proteins in the solid state is compression after mixing with potassium bromide (KBr). Recently, questions have arisen as to whether proteins are conformationally altered by this process. In this study, the amide I Fourier transform infrared spectra of two model proteins, lysozyme and alpha-chymotrypsinogen, were measured before and after compression in KBr, and the effects of moisture exposure and the ratio of KBr to protein were examined. Contrary to earlier reports, compaction of the KBr/protein mixtures did not foster aggregation, and only minor apparent structural alterations were observed.

Bromides↗
PubMed2001

Lyophilization-induced protein denaturation in phosphate buffer systems: monomeric and tetrameric beta-galactosidase.

During freezing in phosphate buffers, selective precipitation of a less soluble buffer component and subsequent pH shifts may induce protein denaturation. Previous reports indicate significantly more inactivation and secondary structural perturbation of monomeric and tetrameric beta-galactosidase (beta-gal) during freeze-thawing in sodium phosphate (NaP) buffer as compared with potassium phosphate (KP) buffer. This observation was attributed to the significant pH shifts (from 7.0 to as low as 3.8) observed during freezing in the NaP buffer (1). In the current study, we investigated the impact of the additional stress of dehydration after freezing on the recovery of active protein on reconstitution and the retention of the native structure in the dried state. Freeze-drying monomeric and tetrameric beta-gal in either NaP or KP buffer resulted in significant secondary structural perturbations, which were greatest for the NaP samples. However, similar recoveries of active monomeric protein were observed after freeze-thawing and freeze-drying, indicating that most dehydration-induced unfolding was reversible on reconstitution of the freeze-dried protein. In contrast, the tetrameric protein was more susceptible to dehydration-induced denaturation as seen by the greater loss in activity after reconstitution of the freeze-dried samples relative to that measured after freeze-thawing. To ensure optimal protein stability during freeze-drying, the protein must be protected from both freezing and dehydration stresses. Although poly(ethylene glycol) and dextran are preferentially excluded solutes and should confer protection during freezing, they were unable to prevent lyophilization-induced denaturation. In addition, Tween did not foster maintenance of native protein during freeze-drying. However, sucrose, which hydrogen bonds to dried protein in the place of lost water, greatly reduced freezing- and drying-induced denaturation, as observed by the high retention of native protein in the dried state as well as the complete recovery of active beta-gal on reconstitution. These results indicate that addition of an effective stabilizer, such as sucrose, may minimize protein denaturation during freeze-drying in phosphate buffers, even if there are large-scale changes in solution pH during freezing.

Buffers↗
PubMed1983

Moisture sorption kinetics for water-soluble substances. II: Experimental verification of heat transport control.

The rates of water sorption as a function of relative humidity for water-soluble substances exhibiting deliquescence have been measured in an atmosphere of pure water vapor. The substances studied included a series of alkali halides, choline halides, and sugars. The results were compared with a theoretical model, previously described, which relates the rate of water uptake to the transport of heat produced during the process away from the surface. Taking into account the heat of water vapor condensation, heat of solution, and heat of hydration, when hydration occurs, the model allows excellent a priori prediction of water uptake rates as a function of relative humidity.

Absorption↗
PubMed1984

Simultaneous determination of nitrate and nitrite in toothpastes by high-performance liquid chromatography.

A stability-indicating analytical method is described for the simultaneous determination of nitrate, and if present, its reductive degradation product, nitrite, in toothpastes. Nitrate and nitrite were extracted from the toothpaste using distilled water and separated from other water-soluble excipients by two RP-8 columns (250 mm X 4 mm i.d.) using a mobile phase containing 0.2% (w/v) sodium acetate and 2.5% (v/v) glacial acetic acid in distilled water. A UV detector set at 313 nm was used for quantitation. The method was applied to commercial toothpastes containing 5% potassium nitrate and yielded an average recovery of 100.1% with a relative standard deviation of 1.43%. Average recovery of nitrate and nitrite from spiked samples were 100.6% and 96.4%, respectively. The minimum detectable concentration for nitrite was 50 micrograms/g of toothpaste.

Chromatography, High Pressure Liquid↗
PubMed1985

Moisture sorption kinetics for water-soluble substances. IV: Studies with mixtures of solids.

This paper extends earlier work from this laboratory concerning the sorption kinetics of water vapor on deliquescent water-soluble substances to mixtures of these solids. A theoretical model, based on heat transport control, excellently predicted a priori the rate of water uptake by a variety of binary mixtures of alkali halides and sugars. The rates for mixtures containing highly water-soluble quaternary ammonium salts, as either one or both of the components, were less successfully predicted as the combined water solubilities of the two components increased. It is concluded that water-soluble deliquescent substances, normally encountered in pharmaceutical dosage forms, rapidly form saturated aqueous solutions in the aqueous film formed as water vapor uptake proceeds, and that the water uptake rate can be predicted a priori from known and experimentally determinable parameters using the heat transport model.

Adsorption↗
PubMed1985

Kinetics of phosphoramide mustard hydrolysis in aqueous solution.

Hydrolysis of phosphoramide mustard was investigated using HPLC, 31P NMR, and GC-MS with specific deuterium labels. The hydrolysis of phosphoramide mustard in sodium phosphate buffers was found to follow apparent first-order kinetics. The rate of hydrolysis was temperature and pH dependent, being slower under acidic conditions. The hydrolysis was not catalyzed by hydroxyl ion, and its pH dependence appeared to be the result of a change in the mechanism of hydrolysis at different pH values. At a pH value approximately above the pKa of the phosphoramide mustard nitrogen, the major hydrolytic pathway of phosphoramide mustard was via the formation of the aziridinium ion, followed by nucleophilic attack. At pH values below its pKa, cleavage of the P-N bond predominated. At pH 7.4, the formation of an aziridinium ion was followed by a rapid hydrolysis to yield the monohydroxy and, subsequently, the dihydroxy products. The hydrolysis at this pH was adequately described by consecutive first-order kinetics. Seven species in the hydrolytic mixture have been identified as intact phosphoramide mustard, N-(2-chloroethyl)-N-(2-hydroxyethyl)phosphorodiamidic acid, N,N-bis-(2-hydroxyethyl)phosphorodiamidic acid, phosphoramidic acid, phosphoric acid, N,N-bis-(2-chloroethyl)amine, and N-(2-chloroethyl)-N-(2-hydroxyethyl)amine by GC-MS with the aid of deuterium labels. Phosphoramide mustard was found to be stabilized by chloride ion. The stabilization was linearly related to the chloride ion concentration, and the mechanism was found to be via the formation of phosphoramide mustard from the aziridinium and chloride ions. Phosphoramide mustard was significantly more stable in human plasma and in 5% human serum albumin as compared to aqueous buffers, an observation that may be important in vivo.

Bromides↗
PubMed1990

Determination of iloprost in 5% dextrose in water solution by reversed-phase high performance liquid chromatography.

A high-performance liquid chromatographic (HPLC) method utilizing absorbance detection was developed for the rapid and precise determination of the stable prostacyclin analogue iloprost in 5% dextrose in water solution (D5W). Samples were prepared for chromatographic analysis by extracting the drug into chloroform, evaporating the solvent, and solubilizing the residue in methanol. The resulting solutions were chromatographed on a Shandon ODS Hypersil column using 0.02 M potassium phosphate (pH 3.0), methanol, and acetonitrile (456:144:400, v/v) at a flow rate of 1.8 mL/min. 2-Naphthoic acid was employed as an internal standard. The detector response at 207 nm was linear (correlation coefficient greater than 0.9998) for concentrations of iloprost from 10 ng on-column, the lower limit of quantitation, up to 7 micrograms on-column. The precision of the method was approximately 5% based on peak area, with a recovery of iloprost from D5W of 87%. Liquid-liquid extraction was found to be superior to solid-phase sorbent extraction as a sample preparation method due to incompatibility of dextrose with the sorbent bed.

Chemical Phenomena↗
PubMed1994

Deformation kinetics of potassium bromide crystals predict tablet stress relaxation.

A model relating the interparticulate contact stress within a tablet matrix with the compaction stress was developed previously to permit the nonlinear deformation kinetic analysis of the viscoelastic behavior of pharmaceutical tablets with the known properties of the tablet constituents. The present research was undertaken to determine whether the inverse operation (i.e., using tablet stress relaxation to determine single crystal properties) was possible. The stress relaxation of potassium bromide (KBr) compacts was evaluated as a function of temperature and relative density, and an attempt was made to calculate the deformation kinetic parameters. The stress relaxation of KBr did not fit the model under ambient conditions for two reasons: (1) KBr has two slip systems with approximately the same shear stress at room temperature; and (2) KBr strain-hardens. When these complications were taken into consideration, the stress relaxation behavior could be explained. Therefore, whereas single crystal tests are capable of yielding parameters that can be used to predict compact behavior, the inverse process of quantifying fundamental material parameters from compact behavior is problematic due to the difficulty of determining, a priori, all the processes that operate simultaneously.

Bromides↗
PubMed1995

Variables that affect the mechanism of drug release from osmotic pumps coated with acrylate/methacrylate copolymer latexes.

The feasibility of using modified Eudragit acrylic latexes as microporous coatings for osmotic devices was investigated. Potassium chloride tablets were coated with mixtures of Eudragit RS30D and RL30D acrylic latexes that also contained a plasticizer (triethyl citrate or acetyl tributyl citrate) and a pore-forming agent (urea). A 2(5-1) fractional factorial experimental design was employed to determine the effect of five formulation variables (RS30D:RL30D polymer ratio plasticizer type, plasticizer level, urea level, and cure) on the in vitro release rate of KCl in deionized water (di water), lag time, and coat burst strength. The RS30D:RL30D polymer ratio had the greatest effect on the release rate, and both lag time and burst strength were most affected by the urea level. Statistical optimization was performed, and a coat formulation with predicted desirable in vitro performance was prepared and tested. The in vitro release rate (di water), lag time, and coat burst strength agreed well with the prediction. Dissolutions were also performed in phosphate buffered saline (PBS; pH 7.4); several formulations released markedly slower in PBS than in di water. This discrepancy was dependent on the type of plasticizer and the amount of pore former. Only those coat formulations containing acetyl tributyl citrate as the plasticizer and a 100% urea [(g urea/g polymer solids) x 100] level exhibited similar release rates in di water and PBS. The mechanism of release from these devices was primarily osmotic, whereas the release from devices coated with a formulation containing triethyl citrate and 50% urea was not dependent on the osmotic pressure difference. Devices with an osmotic release mechanism behaved similarly in vivo and in vitro.(ABSTRACT TRUNCATED AT 250 WORDS)

Acrylates↗