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PubMed2004

In-gel precipitation of enzymatically released phosphate.

The phosphate precipitation reaction using ammonium molybdate and triethylamine under low pH has been applied to gel-based assays for detecting phosphate-releasing enzymes. The sensitivity of the assay is 10 pmol Pi/mm2 of 1.5-mm-thick gel. The assay is applicable to enzymes with a wide range of optimal pH, from acid (pH 4.5) to alkaline phosphatase (pH 9.7), and to enzymes that use acid-labile substrates such as apyrase and glutamine synthetase. Using a negative staining approach, maltose phosphorylase, a phosphate-consuming enzyme, can also be detected. The assay was used to detect glutamine synthetase isoforms, separated by nondenaturing polyacrylamide gel electrophoresis from crude maize extracts. For downstream applications such as staining gels for proteins, the gels with precipitate should be incubated in 10 mM dithiothreitol or beta-mercaptoethanol until the precipitate is dissolved and then thoroughly washed in water. In comparison to calcium phosphate precipitation or the phosphomolybdate-malachite green method, this method is more sensitive. It is a very simple, rapid, versatile, reproducible, and inexpensive method that could be a useful tool in enzymological studies.

Chemical Precipitation↗
PubMed2005

Theoretical analysis of calcium phosphate precipitation in simulated body fluid.

The driving force and nucleation rate of calcium phosphate (Ca-P) precipitation in simulated body fluid (SBF) were analyzed based on the classical crystallization theory. SBF supersaturation with respect to hydroxyapatite (HA), octacalcium phosphate (OCP) and dicalcium phosphate (DCPD) was carefully calculated, considering all the association/dissociation reactions of related ion groups in SBF. The nucleation rates of Ca-P were calculated based on a kinetics model of heterogeneous nucleation. The analysis indicates that the nucleation rate of OCP is substantially higher than that of HA, while HA is most thermodynamically stable in SBF. The difference in nucleation rates between HA and OCP reduces with increasing pH in SBF. The HA nucleation rate is comparable with that of OCP when the pH value approaches 10. DCPD precipitation is thermodynamically impossible in normal SBF, unless calcium and phosphate ion concentrations of SBF increase. In such case, DCPD precipitation is the most likely because of its highest nucleation rates among Ca-P phases. We examined the influences of different SBF recipes, interfacial energies, contact angle and molecular volumes, and found that the parameter variations do not have significant impacts on analysis results. The effects of carbonate incorporation and calcium deficiency in HA were also estimated with available data. Generally, such apatite precipitations are more kinetically favorable than HA.

Biocompatible Materials↗
PubMed2006

Hospitalization due to acute heart failure. Role of the precipitating factors.

BACKGROUND AND AIMS: Many precipitating factors for decompensation of a chronic, stable heart failure (HF) have been described. OBJECTIVES: To evaluate the precipitating factors associated with HF decompensation among 293 patients admitted to a teaching hospital because of acute HF. RESULTS: 173 women and 120 men were included, and mean age was 76.7 years. In 221 patients (75%) there was some evidence of a factor that was potentially accountable for the decompensation of HF; a combination of two or more factors could be elicited in 100 patients. Except for a worse prior functional status, no differences were found between patients with and without identified precipitating factors. CONCLUSIONS: Precipitating factors may be identified in most patients suffering an acute episode of decompensation of HF. The majority of these factors appear to be preventable, and should thus be avoidable with a better, more comprehensive control of the HF patient.

Adult↗
PubMed2005

Ibuprofen-loaded nanoparticles prepared by a co-precipitation method and their release properties.

A co-precipitation method was established to fabricate nano-scale core-shell particles, by which poor water-soluble drugs can be effectively dispersed with rather good stability during storage. Exemplified with formation of ibuprofen (Ib) nanoparticles stabilized by DEAE dextran (Ddex), the process includes precipitation of Ib in a supersaturated solution and deposition of Ddex onto the precipitated Ib particles through electrostatic interaction. Characterized by transmission electron microscopy (TEM), atomic force microscopy (AFM), dynamic light scattering (DLS) and zeta potential, the core-shell structure of the particles formed at pH 6.0 with a Ddex/Ib weight ratio of 5:1 was identified with Ib being the core and Ddex being the shell. As a comparison, particles formed at other pH values and other Ddex/Ib ratios were also studied. Along with increase of the Ddex/Ib ratio or pH value of the final aqueous solution, the particle size was decreased, demonstrating that the particle sizes could be readily tuned by variation of the fabrication parameters. At conditions that the Ib concentration was lower than its supersaturated value, for example at higher pH value, instead of co-precipitation mechanism, forces such as electrostatic complexation dominate the formation of Ddex-Ib particles. Moreover, drug entrapment was mainly dependent on the Ib solubility regardless of the ratio between Ddex and Ib, while the drug content was decreased as a function of Ddex/Ib ratio. In vitro release studies showed that the loaded Ib could be again released in a burst manner during the initial stage, followed with a slow rate. The final released amount of Ib showed a positive correlation with the bulk pH value, e.g. approximately 60, 80 and 90% of the loaded Ib were released in pH 1.0, 5.8 and 7.4 buffered solutions after incubation for 40 h, respectively.

Chemical Precipitation↗
PubMed2006

A 96-well single-pot protein precipitation, liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the determination of muraglitazar, a novel diabetes drug, in human plasma.

A 96-well single-pot protein precipitation, liquid chromatography/tandem mass spectrometry (LC/MS/MS) method has been developed and validated for the determination of muraglitazar, a PPAR alpha/gamma dual agonist, in human plasma. The internal standard, a chemical analogue, was dissolved in acetonitrile containing 0.1% formic acid. The solvent system was also served as a protein precipitation reagent. Human plasma samples (0.1 mL) and the internal standard solution (0.3 mL) were added to a 96-well plate. The plate was vortexed for 1 min and centrifuged for 5 min. Then the supernatant layers were directly injected into the LC/MS/MS system. The chromatographic separation was achieved isocratically on a Phenomenox C18(2) Luna column (2 mm x 50 mm, 5 microm). The mobile phase contained 20/80 (v/v) of water and acetonitrile containing 0.1% formic acid. Detection was by positive ion electrospray tandem mass spectrometry on a Sciex API 3000. The standard curve, which ranged from 1 to 1000 ng/mL, was fitted to a 1/x weighted quadratic regression model. This single-pot approach effectively eliminated three time consuming sample preparation steps: sample transfer, dry-down, and reconstitution before the injection, while it preserved all the benefits of the traditional protein precipitation. By properly adjusting the autosampler needle offset level, only the supernatant was injected, without disturbing the precipitated proteins in the bottom. As a result, the quality of chromatography and column life were not compromised. After more than 600 injections, there was only slightly increase of column back-pressure. The validation results demonstrated that this method was rugged and provide satisfactory precision and accuracy. The method has been successfully applied to analyze human plasma samples in support of a first-in-man study. This method has also been validated in monkey and mouse plasma for the determination of muraglitazar.

Animals↗
PubMed2004

Recycling of Ni(II)-citrate complexes using precipitation in alkaline solutions.

When the excess of Ni(II) ions as compared to citrate concentration is used both Ni(II) ions and citrate can be precipitated in alkaline solutions. The ratio between Ni(II) and citrate in the precipitate and completeness of citrate precipitation depends on the ratio between the Ni(II) and citrate concentrations in the initial solution and its pH. The data of chemical analysis, potentiometric titration, FT-IR as well as visible spectrophotometric investigations suggest that Ni(II) in the insoluble compound is bound with three -COO- groups and -OH group of the citrate. The insoluble compound also contains SO4(2-) and hydroxides. The treatment of this precipitate with H2SO4 enables to recover a soluble Ni(II)-citrate complex, which can be reused in practice, and to remove the excess of Ni(II) in the form of insoluble Ni(OH)2.

Alkalies↗
PubMed2005

Examination of the jarosite-alunite precipitate addition in the raw meal for the production of sulfoaluminate cement clinker.

The aim of the present research work was to investigate the possibility of adding a jarosite-alunite chemical precipitate, a waste product of a new hydrometallurgical process developed to treat economically low-grade nickel oxides ores, in the raw meal for the production of sulfoaluminate cement clinker. For that reason, two samples of raw meals were prepared, one contained 20% gypsum, as a reference sample ((SAC)Ref) and another with 11.31% jarosite-alunite precipitate ((SAC)J/A). Both raw meals were sintered at 1300 degrees C. The results of chemical and mineralogical analyses as well as the microscopic examination showed that the use of the jarosite-alunite precipitate did not affect the mineralogical characteristics of the so produced sulfoaluminate cement clinker and there was confirmed the formation of the sulfoaluminate phase (C4A3S), the most typical phase of this cement type. Furthermore, both clinkers were tested by determining the grindability, setting time, compressive strength and expansibility. The hydration products were examined by XRD analysis at 2, 7, 28 and 90 days. The results of the physico-mechanical tests showed that the addition of jarosite-alunite precipitate did not negatively affect the quality of the produced cement.

Aluminum Compounds↗
PubMed2006

Precipitation of heavy metals in produced water: influence on contaminant transport and toxicity.

Produced water undergoes changes in its physical chemistry including precipitation of heavy metals after being discharged and mixed with ambient seawater. Potential impacts of the precipitation of heavy metals on their transport and toxicity were studied using samples from offshore oil production sites on the Scotian Shelf off eastern Canada. Concentrations of aluminum, cadmium, chromium, cobalt, copper, iron, lead, manganese, nickel and zinc were measured in total, particulate and dissolved fractions together with Microtox tests for assessment of toxicity. Heavy metals in produced water were transformed from dissolved to particulate phase in a period of hours under oxygenated conditions, and aggregated to larger particles that settle rapidly (>100 m/day) over a few days. In addition, there was production of buoyant particles comprised of heavy metal precipitates sequestered onto oil droplets that were transported to the surface. The particulate fraction was generally more toxic than the dissolved fraction. This was evident at the mixing interface between produced water and seawater where elevated particulate and toxicity levels were observed. Laboratory studies suggest an increase in the toxicity of discharged produced water over time. Time-series experiments showed a sustained toxic response for more than a week following the oxidation of freshly discharged produced water that initially elicited little or no toxic response in the Microtox test. Chemical processes identified in this study, namely precipitation of heavy metals and consequent settling and rising fluxes of particles, will influence the toxicity, the fate and the transport of potential contaminants in the produced water. Therefore, these processes need to be considered in assessment of the environmental impact associated with offshore oil and gas operations.

Chemical Precipitation↗
PubMed2004

Ethanol or/and captopril-induced precipitation and secondary conformational changes of human serum albumin.

We determined the secondary structure of solid-state native human serum albumin (HSA) and its precipitates induced by ethanol, captopril, or a captopril/ethanol mixture. A transmission Fourier transform infrared (FT-IR) microspectroscopy equipped with a thermal analyzer was used. The secondary structural composition of solid-state native HSA was 54% alpha-helices (1655 cm(-1)), 22% beta-turns (1679 cm(-1)), and 23% beta-sheets (1633 cm(-1)). After ethanol treatment, a new peak was observed at 1690 cm(-1), and the peak at 1633 cm(-1) was more apparent in the HSA precipitates. The corresponding compositions consisted of 59% alpha-helices, 17% beta-turns, and 24% beta-sheets. After treatment with captopril with or without ethanol, the percentage of alpha-helices and beta-turns decreased in both HSA precipitates, but the percentage of beta-sheets increased. The temperature-dependent structural transformation from alpha-helices/random coils to beta-sheets for the solid-state HSA samples occurred at markedly different onset temperatures. The onset temperature for native HSA was 85 degrees C, and that for HSA precipitates obtained from ethanol, captopril, or captopril/ethanol was 100, 48 or 57 degrees C, respectively. The thermal-induced structural transformation from alpha-helices/random coils to beta-sheets implies a partial unfolding structure in these HSA samples.

Captopril↗
PubMed2005

Self-perception of factors that precipitate or inhibit seizures in juvenile myoclonic epilepsy.

PURPOSE: To assess self-perception of factors that precipitate or inhibit seizures in patients with juvenile myoclonic epilepsy (JME). PATIENTS AND METHODS: Thirty-six males and 39 females with JME and mean age of 25.8+/-8.7 years were analysed. All patients completed a standardized questionnaire to assess for the presence or absence of precipitant or inhibitory factors for their seizures in a face-to-face interview. These data were statistically analysed through logistic and linear regression models and Phi coefficient. RESULTS: Ninety-two percent of the patients identified at least one precipitating factor (PF). In order of frequency the following PFs were recorded: stress (83%), sleep deprivation (77%), specific thoughts/mental concentration (23%), performance of hand activities and complex finger movements (20%), flashing lights and playing games (15%), speaking out in public (11%) and alcohol intake (11%), reading (7%), calculating and writing (5%), playing musical instruments (4%), drawing (3%), and specific types of music (1%). Menstrual cycle was the third most important PF in the women (33%). Although PFs were easily recognized, 77% of the patients stated that they were unable to avoid the occurrence of the seizures. CONCLUSIONS: Structured questionnaire is useful in stimulating patients to self-report seizure precipitants. Patients with higher education and uncontrolled seizures identified them more easily. The presence of a significant number of uncommon PFs, such as mental and motor hand tasks, considered uncommon for other epileptic syndromes, suggests that the role of these factors may be under-recognized in JME.

Adolescent↗
PubMed2006

Phosphate and potassium recovery from source separated urine through struvite precipitation.

Phosphate can be recovered as struvite or apatite in fluidised bed reactors. Urine has a much higher phosphate concentration than sludge reject water, allowing simpler (and less expensive) process for precipitation of phosphates. A stirred tank reactor with a special compartment for liquid solid separation was used to precipitate struvite from urine. Magnesium ammonium phosphate as well as potassium magnesium phosphate are two forms of struvite that were successfully precipitated. Liquid/solid separation was very effective, but the compaction of struvite was rather poor in the case of potassium struvite. Crystals did not form clusters and maintained the typical orthorhombic structure. Ammonium struvite had slightly lower effluent phosphate concentrations, but an average of 95% of influent phosphate was removed regardless of ammonium or potassium struvite precipitation. Fluid mechanics is believed to be important and should inform further work.

Chemical Precipitation↗
PubMed2003

Studies of urinary cystine precipitation in vitro: ontogeny of cystine nephrolithiasis and identification of meso-2,3-dimercaptosuccinic acid as a potential therapy for cystinuria.

Children with fully recessive (Type I/I) cystinuria have a high risk of stone formation in the first decade of life. To assess the tendency for cystine to precipitate in individual urine samples, we developed an in vitro assay in which radiolabelled cystine (4mM) was dissolved in urine at 37 degrees C after alkalization to pH 10. Samples were then brought to pH 5, cooled, and centrifuged. The % decrease in supernatant cpm was used as a measure of cystine precipitation (CP). CP varied widely among normal children (74%+/-34) whereas variability of repeated determinations on a single adult individual was modest (64%+/-3.3). The assay was used to compare various potential therapies for cystinuria. Precipitation of exogenous cystine from normal urine was strongly inhibited by addition of D-penicillamine (CP: 8%+/-3) or dimercaptosuccinic acid (DMSA) (CP: 5%+/-1), at urinary concentrations attained by standard oral doses of each drug. Mercaptopropionylglycine (MPG) was moderately effective (CP: 43%+/-9), whereas captopril was a weak inhibitor (CP: 63%+/-12). Precipitation of endogenous cystine (2191 micromol/L) from a cystinuric patient showed that DMSA and D-penicillamine were again highly effective compared to the other agents. In addition DMSA and penicillamine added to the same patient's urine reduced the free cystine by 50% (as measured by automated amino acid analyzer) whereas MPG and captopril had no effect. In conclusion, DMSA is comparable to D-penicillamine as an in vitro inhibitor.

Adolescent↗
PubMed1990

Diagnostic of precipitant for biomacromolecule crystallization by quasi-elastic light-scattering.

The translational diffusion coefficient D25,w of hen egg-white lysozyme and concanavalin A from the jack bean is measured in various precipitating agent solutions as a function of salt and protein concentration using quasi-elastic light-scattering. With some precipitants, in undersaturated protein solutions, a protein or salt concentration dependence of the diffusion coefficient of the scatters is observed. It can be correlated with the inability of the protein to crystallize in this precipitant once the solution is supersaturated. These variations of D25,w are interpreted in terms of non-specific interactions and/or aggregation that prevent the protein from making appropriate contacts to form a crystal. With other precipitants known to lead to crystallization, no significant variation of the diffusion coefficient with increasing concentration was observed, indicating that under such conditions up to saturation the proteins remain essentially monodisperse. Application of this technique to find crystallization conditions of other proteins is discussed.

Ammonium Sulfate↗
PubMed2001

Conditions influencing the precipitation of magnesium ammonium phosphate.

Struvite precipitation in wastewater treatment works has caused substantial operational problems since the early 1960s. Struvite, magnesium ammonium phosphate hexahydrate (MgNH4PO4 6H2O), is a white inorganic crystalline mineral that precipitates in places with increased turbulence such as pumps, aerators and pipe bends. Batch experiments were conducted to examine the influence of a number of physical and chemical parameters on struvite crystallisation. This was undertaken by dosing a medium of de-ionised water with varying concentrations of Mg2+, NH4+ and PO4(3-) ions. Preliminary experiments found that struvite could be precipitated out of solution at pH 10 and increasing the ion concentration stoichiometrically could increase crystal yield. Increasing the NH4+ concentration increased purity of the precipitate. As reaction time was increased from 1 to 180 min, crystal size was found to increase from 0.1 to 3mm.

Chemical Precipitation↗
PubMed2003

Optimization of metal sulphide precipitation in fluidized-bed treatment of acidic wastewater.

Sulphate-reducing biofilm and suspension processes were studied for treatment of synthetic wastewater containing sulphate, zinc and iron. With lactate supplemented wastewater with 170-230mg/l Zn and 58mg/l Fe, the following precipitation rates were obtained: 250 and 350mg/l d for Zn in fluidized-bed (FBR) and upflow anaerobic sludge blanket reactors, respectively, and 80mg/l d for Fe in both reactors with hydraulic retention time of 16h. The effluent Zn and Fe concentrations remained at less than 0.1 mg/l. The alkalinity produced in lactate oxidation increased the initial pH of 2.5-3, resulting in effluent pH of 7.5-8.5. The highest sulphate reduction rate was over 2000 mg/l d. In terms of sulphate reduction, hydrogen sulphide production and effluent alkalinity, the start-up of the FBR with the 10% fluidization rate was superior to the FBRs with 20-30% fluidization rates. With increased loading rates, high recycling rate became an advantage. After process failure caused by intentional overloading, the sulphate reduction partially recovered within 2 weeks. Metal precipitates in the reactors were predominantly FeS2, ZnS and FeS. The metal mass balance was as follows: 73-86% of Zn and Fe accumulated into the reactors and water level adjustors, 14-23% of the metals were washed out as precipitates and 0.05-0.15% remained as soluble metals. Biomass yield in the sulphate-reducing processes was 0.039-0.054g dry biomass (VS or VSS) per g of lactate oxidized or 0.035-0.074g dry biomass per g of sulphate reduced. The results of this work demonstrate that the lactate supplemented sulphate-reducing processes precipitated the metals as sulphides and neutralized the acidity of the synthetic wastewater.

Biofilms↗
PubMed2003

Control of the sulfide (S2-) concentration for optimal zinc removal by sulfide precipitation in a continuously stirred tank reactor.

Precipitation of Zn2+ with S2- was studied at room temperature in a continuously stirred tank reactor of 0.5l to which solutions of ZnSO4 (800-5800 mgl(-1) Zn2+) and Na2S were supplied. The pH was controlled at 6.5 and S2- concentration in the reactor was controlled at set point values ranging from 3.2x10(-19) to 3.2x10(-4) mgl(-1), making use of an ion-selective S2- electrode. In steady state, the mean particle size of the ZnS precipitate decreased linearly from 22 to 1 microm for S2- levels dropping from 3.2x10(-4) to 3.2x10(-18) mgl(-1). At 3.2x10(-11) mgl(-1) of S2-, the supplies of ZnSO4 and Na2S solutions were stoichiometric for ZnS precipitation. At this S2- level, removal of dissolved zinc was optimal with effluent zinc concentration <0.03 mgl(-1) while ZnS particles formed with a mean geometric diameter of about 10 microm. Below 3.2x10(-11) mgl(-1) of S2- insufficient sulfide was added for complete zinc precipitation. At S2- levels higher than 3.2x10(-11) mgl(-1) the effluent zinc concentration increased due to the formation of soluble zinc sulfide complexes as confirmed by chemical equilibrium model calculations.

Chemical Precipitation↗
PubMed1985

Morphology of pseudophakic precipitates on intraocular lenses removed from human patients.

Cellular precipitates on the surface of 52 intraocular lenses removed from human patients for various reasons from one week to five years following implantation were studied with cytologic techniques and scanning electron microscopy. A variety of cellular responses were characterized: mononuclear precipitates composed of lymphocytes and macrophages, multinucleated giant cells, and a fibroblastic proliferation. Polymorphonuclear leukocytes were encountered less frequently. Acellular membranous precipitates were also observed. Cellular response was related to clinical history to correlate temporal and possible etiopathogenic factors in the formulation of these precipitates and their possible relationship to implant failure.

Chemical Precipitation↗
PubMed2001

A piezoelectric quartz crystal impedance study on Cu(2+)-induced precipitation of bovine serum albumin in aqueous solution.

Piezoelectric quartz crystal impedance (QCI) technique was used for monitoring the Cu(2+)-induced precipitation of bovine serum albumin onto the gold electrode. The critical precipitate concentration of Cu(2+) reflected by the significant decrease in the resonant frequency was estimated to be 9.98 x 10(-5) mol x l(-1), and the saturated adherence of the precipitate on the electrode occurred when the Cu(2+) concentration was greater than 9.79x10(-3) mol x l(-1). The frequency shift in air was about 85.5% of that in liquid, and the Deltaf(0)/DeltaR(1) ratio found in solution was 82.67 Hz Omega(-1), suggesting that the frequency response was predominated by the mass change due to precipitate adherence to the electrode surface. The response of the resonant frequency was analyzed using an equation Deltaf=a(0) + a(1) e(-t/tau(1)) + a(2) e(-t/tau(2)). The relationship between the total a(0) values and the Cu(2+) concentration was discussed.

Animals↗