High-performance liquid chromatographic determination of isepamicin in plasma, urine and dialysate

A high-performance liquid chromatographic method for the measurement of isepamicin, a new aminoglycoside, in plasma, urine and dialysate is reported. The assay utilizes a simple extraction of isepamicin in plasma using commercially available Cyano solid-phase cartridges and dilution of urine and dialysate samples. The separation is performed on a Hypersil C18 column (15 cm X 4.6 mm I.D., 5 microns particle size) and utilizes a mobile phase consisting of 10% methanol and 90% buffer solution containing 0.01 M sodium hexanesulfonate, 0.1 M sodium sulfate and 17 mM acetic acid. The flow-rate is 1.1 ml/min. Dibekacin is used as the internal standard. Isepamicin is derivatized post-column with o-phthalaldehyde for spectrofluorometric detection. The method can also be used for the measurement of other aminoglycosides, i.e. tobramycin, kanamycin, netilmicin and gentamicin. The assay is fast, accurate and has a quantitation limit of 100 ng/ml isepamicin in plasma and 50 ng/ml in urine and dialysate.     

A direct injection high-throughput liquid chromatography tandem mass spectrometry method for the determination of a new orally active alphavbeta3 antagonist in human urine and dialysate

A generic high-throughput liquid chromatography (HTLC) tandem mass spectrometry (MS/MS) assay for the determination of compound I in human urine and dialysate (hemodialysis) was developed and validated. By using the HTLC on-line extraction technique, sample pretreatment was not necessary. The sample was directly injected onto a narrow bore large particle size extraction column (50 x 1.0 mm, 60 microm) where the sample matrix was rapidly washed away using a high flow rate (5 mL/min) aqueous mobile phase while analytes were retained. The analytes were subsequently eluted from the extraction column onto an analytical column using an organic-enriched mobile phase prior to mass spectrometric detection. The analytes were then eluted from the analytical column to the mass spectrometer for the determination. The linear dynamic range was 2.0-6000 ng/mL for the urine assay and 0.1-300 ng/mL for the dialysate assay. Intraday accuracy and precision were evaluated by analyzing five replicates of calibration standards at all concentrations used to construct the standard curve. For the urine assay, the precision (RSD%, n=5) ranged from 1.9 to 8.0% and the accuracy ranged from 87.8 to 105.2% of nominal value. For the dialysate assay, the precision (RSD%, n=5) ranged from 1.1 to 10.0% and the accuracy from 94.5 to 105.2% of nominal value. In-source fragmentation of the acyl glucuronide metabolite (compound III) did not interfere with the determination of parent compound I. The developed HTLC/MS/MS methodology was specific for compound I in the presence of compound III. Column life-time is increased and sample analysis time is decreased over traditional reversed-phase methods when direct injection assays for urine and dialysate are coupled with the technology of HTLC.     

Rotating Biological Contactor Reactor with Biofilm Promoting Mats for Treatment of Benzene and Xylene Containing Wastewater

A novel rotating biological contactor (RBC) bioreactor immobilized with microorganisms was designed to remove volatile organic compounds (VOC), such as benzene and xylene from emissions, and its performance was investigated. Gas-phase VOCs stripped by air injection were 98?% removed in the RBC when the superficial air flow rate was 375?ml/h (1,193 and 1,226?mg/l of benzene and xylene, respectively). The maximum removal rate was observed to be 1,007 and 1,872?mg/m³/day for benzene and xylene, respectively. The concentration profile of benzene and xylene along the RBC was dependent on the air flow rate and the degree of microbial adaptation. Air flow rate and residence time were found to be the most important operational parameters for the RBC reactor. By manipulating these operational parameters, the removal efficiency and capacity of the bioreactor could be enhanced. The kinetic constant K _s demonstrated a linear relationship that indicated the maximum removal of benzene and xylene in RBC reactor. The phylogenic profile shows the presence of bacterium like Pseudomonas sp., Bacillus sp., and Enterococcus sp., which belonged to the phylum Firmicutes, and Proteobacteria that were responsible for the 98?% organic removal in the RBC.     

Blood flow and oxygen transfer rate of an outside blood flow membrane oxygenator

We evaluated effects of the number of tied hollow fibers of an outside blood flow membrane oxygenator with cross-wound hollow fibers on the blood flow pattern and oxygen transfer rate. The number of tied hollow fibers in a bundle was varied from one to six, and the blood flow pattern was observed by X-ray computed tomography. The oxygen transfer rate and blood pressure drop were measured by in vitro experiments using bovine blood. Uniform blood flow patterns were obtained for each number of tied hollow fibers. A decrease in the number of tied hollow fibers caused more effective contact of blood with the tied hollow fibers and oxygen transfer rate was enhanced, demonstrating that single hollow fiber was the most effective. Empirical equations were obtained based on these results and optimum structure parameters of the membrane oxygenator were determined by simulation analysis. Optimum membrane surface area and axial jacket length of the oxygenator were 3.0 m² and 320 mm, respectively, at a hollow fiber outside diameter of 250 μm.     

Determination of Ammonia/Air Diffusion Coefficient Using Nafion Lined Tube

Abstract

Trace gaseous ammonia in air was removed in a laminar flow Teflon tube lined with Nafion film. The ammonia deposition pattern was obtained by sectioning the Nafion lining, extracting with an aqueous solution, and measuring the concentration with an ammonia gas electrode. Mass transport analysis of the deposition pattern demonstrated that the ammonia was removed from the air stream at a rate controlled by gaseous diffusion. The ammonia/air diffusion coefficient equalled 0.228 ± 0.012 cm² s^?1 at 1 atm 25°C. No dependence on relative humidity was observed over the range 10–92%.     

Dielectric Barrier Discharge for Ammonia Production

The leading after-treatment technology for NOx removal process in Diesel engines for stationary and mobile applications is the selective catalytic reduction of oxides of nitrogen [NOx] by ammonia [NH₃]. A novel non-thermal plasma electrode with a needle array in a dielectric barrier discharge reactor, powered by a high frequency neon transformer, is used for the thermal decomposition of solid urea [(NH₂)CO(NH₂)] to produce ammonia. The thermolysis of urea produces iso-cyanic acid [HNCO] as a byproduct, besides ammonia, which can react with water in the gas phase, thus giving carbon dioxide and more ammonia. The presence of water fed before and/or after the plasma reactor was studied to assess its effect on the amount of produced ammonia. Results clearly showed that water fed to the entrance of the reactor can efficiently promote the reaction of iso-cyanic acid to produce ammonia and this result can be improved when air is used as carrier gas for 115 V of input voltage to a neon transformer and with a gas flow rate of 4 L/min.     

Potentiometric determination of dialysate urea nitrogen

An enzymatically modified ammonium ion-selective electrode has been applied for the determination of urea in spent dialysate. The biosensor has been used in a simple flow-injection analysis (FIA) system. The system enables one to perform over 25 dialysate urea nitrogen (DUN) determinations per hour. The interferences from other components of posthemodialysis fluid were eliminated by simultaneous measurements with non-modified enzymatically ion-selective electrode. It is possible to use both the sensors in a simplified differential potentiometric system. The results of DUN determination using the biosensor/FIA system and a conventional method of urea determination were comparable. The presented analytical system can potentially find wider biomedical application in the monitoring of hemodialysis progress.     

三相流化床电极反应器深度处理制浆废水

应用三相流化床电极反应器(新型电化学反应器)处理制浆废水.研究了曝气量、槽电压、溶液pH值及FeSO4浓度等因素对电解效果的影响.结果表明,该反应器深度处理制浆废水的最佳工艺条件为:槽电压20 V,曝气量为0.3 m3.h-1,FeSO4浓度为1000 mg.L-1,pH值≈2.5,反应时间为90 m in时COD去除率为70.1%.     

An enzyme reactor electrode for urea determinations.

An enzyme reactor electrode system for the determination of urea is described. A buffer is pumped through an enzyme reactor (0.4 ml) containing urease immobilized with glutaraldehyde to glass. The effluent is mixed with sodium hydroxide pumped through a second channel and fed through an ammonia gas electrode. Samples are introduced via a third flow channel and mixed with the buffer. The conversion of urea to ammonia is quantitative for sample concentrations of less than 0.03 M for a flow rate of 40 ml h^-1. The reactor electrode shows a Nernstian slope of 57 mV/decade for 5·10^-5–3·10^-2 M urea. The response is independent of variations in the flow rate, enzyme activity or temperature of the reactor.     

Rapid linear scale-up of a protein separation by centrifugal partition chromatography

The scaling up of the separation of two proteins with an aqueous two-phase system (ATPS) from 176 mg with a 500 ml laboratory scale centrifugal partition chromatography (CPC) column to 2.2g with a 6.25 litre pilot-scale column is presented. A model sample system of a mixture of lysozyme and myoglobin was chosen for this study using an ATPS system comprising 12.5% (w/w) PEG-1000:12.5% (w/w) K2HPO4. It was found that the maximum sample concentration possible without precipitation was 2.2mg/ml for each constituent. The optimisation of rotor speed, mobile phase flow rate and sample loading was performed on a laboratory-scale device. It was found that a centrifuge speed of 2000 rpm (224 'g'), 10 ml/min mobile phase flow rate with a 43 ml (10% of active column volume) sample volume gave optimum operating conditions. This was linearly scaled up to pilot scale by increasing mobile phase flow rate, fraction size and sample loading in the ratio of the system capacities (i.e. 12.5:1). Flow rate was therefore increased from 10 ml/min to 125 ml/min, fraction size from 10 ml to 125 ml and sample loading from 43 ml to 500 ml. Rotor speed however was reduced from 2000 rpm on the laboratory device to 1293 rpm on the pilot-scale device to maintain the same 224 'g' field in each chamber, as the pilot-scale CPC unit has a larger rotor radius than the laboratory one. Resolution increased from Rs=1.28 on the 500 ml rotor to Rs=1.88 on the 6.25 litre rotor, giving potential throughputs in batch mode of over 40 g/day.     

Separation and Removal of Mercury(II) from Water Samples Using (Acetylacetone)‐2‐Thiol‐Phenyleneimine Immobilized on Anion‐Exchange Resin Prior to Determination by Cold Vapor Inductively Coupled Plasma Atomic Emission Spectroscopy

Abstract

(Acetylacetone)‐2‐thiol‐phenyleneimine (H₂L) immobilized on an anion‐exchange resin (Dowex) was used for separation and removal of mercury from natural water samples and for preconcentration prior to its determination by cold vapor inductively coupled plasma atomic emission spectroscopy. The metal was eluted from the column using a solution of 10% thiourea in 0.1 M HCl. The modified resin is higly selective with an exchange capacity of 1.60 mmol g^?1. Various parameters like pH, column flow rate, and desorbing agents are optimized. The proposed method has a linear calibration range of 15–1000 ng/ml Hg(II), with a relative standard deviation at the 15 ng/ml level of 3.5%. The precision of the method (evaluated as the relative standard deviation obtained after analyzing six series of five replicates) was ±4.2% at the 50 ng/ml level of Hg(II). The method has been used for routine determination of trace levels of mercury species in natural waters. The potential application of modified resin for the removal of mercury(II) from two natural water samples (top water and lake water) spiked with 50 ng/ml of mercury (II) was studied by ICP‐AES, and the results proved that excellent percent extraction of mercury(II) from both natural water samples was obtained by column method using modified resin.     

Photocatalytic degradation of ammonia and butyric acid in plug-flow reactor: Degradation kinetic modeling with contribution of mass transfer

Photocatalytic treatment of polluted air by odorous contaminants – ammonia and butyric acid – is investigated in a plug-flow reactor covered by non-woven fiber textile coated with TiO₂. For the first time, the single-component degradation pathway of ammonia by photocatalysis at ambient condition is highlighted. It appears fundamentally different compared to the butyric acid degradation pathway. The ammonia degradation pathway highlights a possible auto-accelerated behavior of the reaction. The chemical degradation kinetics follows the Langmuir–Hinshelwood model, though observed oxidation rates depend upon flow conditions in the reactor. Thus, interpretation of degradation results through a model considering the Langmuir–Hinshelwood approach and mass transfer phenomenon is presented. This model succeeds with a pair of determined kinetic constants and mass transfer coefficients to describe experimental results for different flow rates and for both pollutants, though they present wide dissimilarities in their degradation pathways.     

Electron caputure detection in high-speed narrow-bore capillary gas chromatography: Fast and sensitive analysis of PCBs and pesticides

In this work the combination of high-speed narrow-bore capillary GC with electron capture detection is evaluated. The make-up gas flow rate is a key parameter in the successful coupling of narrowbore columns and ECD detection. The make-up flow has to be as high as possible to eliminate peak tailing caused by the large detection cell volume. The sensitivities at these elevated make-up flow rates (400 to 1000 ml/min), measured for some pesticides like HCB and dieldrin, were very good. Detection limits for these compounds of 0.1 pg were obtained, resulting in minimum detectable concentrations of approximately 0.2 ppb. The performance of the system is illustrated by several high-speed analyses of environmentally relevant samples of PCBs and pesticides.     

Removal of ammonia from waste air streams with clinoptilolite tuff in its natural and treated forms

Natural and impregnated clinoptilolite tuffs were studied to assess their potential to remove ammonia from air and, in a subsequent application, to use the spent adsorbent as a fertilizer. H₂SO₄, H₃PO₄ and HNO₃, as agents containing important plant nutrients compatible with soil, were selected for impregnation to enhance sorption capacity of the natural clinoptilolite tuffs for ammonia removal. Sorbents were characterized using N₂ adsorption isotherms at 77 K, X-ray analysis and high pressure mercury porosimetry. Ammonia breakthrough curves on fixed beds of sorbent were determined using appropriate NH₃ and H₂O input concentrations, flow rates and temperatures similar to the conditions in animal breeding farms. Impregnated clinoptilolite tuffs showed adsorption capacities comparable to SSP-4, an activated carbon that is commercially used for NH₃ removal. Impregnations with H₂SO₄ and HNO₃ are particularly important, since such modified adsorbents exhibit relatively high breakthrough capacities, thus rendering them potentially useful for practical applications in controlling ammonia emissions. The main contribution to the sorption capacity enhancement on impregnated clinoptilolite tuff samples seems to be due to the chemical reaction of ammonia with acids remaining in the macro- and mesopores.     

Development of an integrated microfluidic platform for dynamic oxygen sensing and delivery in a flowing medium

This paper describes a platform for real-time sensing of dissolved oxygen in a flowing microfluidic environment using an oxygen-sensitive luminescent dye (platinum octaethylporphyrin ketone) integrated into a micro-oxygenator device. Using a phase-based detection method, the luminescent decay lifetime of the dye was consistent with the linear Stern-Volmer relationship using both gaseous and aqueous samples. Maximum sensor resolution varied between 120-780 ppb across a range of dissolved oxygen (DO) concentrations ranging from 0-42.5 ppm. The sensor was subsequently used to determine the convective mass-transfer characteristics of a multi-layer polydimethylsiloxane (PDMS) microfluidic oxygenator. The membrane-based oxygenator showed excellent agreement with an analytical convection model, and the integrated oxygen sensor was accurate across a wide range of tested flow rates (0.05-5 mL min(-1)). The device is unique for its ease of fabrication and highly flexible configuration, as well as the novel incorporation of oxygen delivery and detection in a single micro-device. Potential applications include tissue engineering, cell culturing, and miniaturized bio-assays that require the delivery and/or detection of precise quantities of oxygen within a microfluidic construct.     

Sensitive and simultaneous determination of HIV protease inhibitors in rat biological samples by liquid chromatography-mass spectrometry

A sensitive and simultaneous liquid chromatographic-mass spectrometric (LC/MS) method for the determination of current four HIV protease inhibitors (PIs), indinavir (IDV), saquinavir (SQV), nelfinavir (NFV) and amprenavir (APV) in rat plasma and liver dialysate by a microdialysis method was described. An isocratic LC/MS method in combination with atmospheric pressure chemical ionization was developed for the determination of these four PIs in biological samples in the same run. The analytes including an internal standard were extracted from 100 microL of plasma or 150 microL of liver dialysate samples by salting-out with 100 microL of ice-cold 2 M K(3)PO(4) followed by ether extraction. The separation of analytes was carried out on a reversed-phase semi-micro column using 50% of acetonitrile containing 1% acetic acid as mobile phase at a flow rate of 0.2mL/min(-1). The separation was completed within 5 min. Precision, recovery and limits of detection indicated that the method was suitable for the quantitative determination of these PIs in rat plasma or liver dialysate. This simple, sensitive and highly specific LC/MS method is suitable for pharmacokinetic studies and therapeutic drug monitoring in AIDS patients who receive double protease therapy.     

Oxygen permeation study in a tubular Ba0.5Sr0.5Co0.8Fe0.2O3-δ oxygen permeable membrane

Dense tubular Ba_0.5Sr_0.5Co_0.8Fe_0.2O_3−δ (BSCFO) membranes were successfully prepared by the plastic extrusion method. The oxygen permeation flux was determined at different oxygen partial pressures in the shell side and different temperatures between 700 and 900 °C. The oxygen vacancy diffusion coefficients (D_v) at different temperatures were calculated from the dependence of oxygen permeation flux on the oxygen partial pressure term based on the surface current exchange model. No unsteady-state of oxygen permeation flux was observed at the initial stage in our experiments. The reason is the equilibrium time is too short (less than 10 min) to observe the unsteady-state in time. The increase of the helium flow rate can increase the oxygen permeation flux, which is due to the decrease of the oxygen partial pressure in the tube side with increasing of the helium flow rate. The oxygen permeation flux can also be affected by the air flow rate in the shell side when the air flow rate is lower than 150 ml/min. But the oxygen permeation flux is insensitive to the air flow rate when the air flow is higher than 150 ml/min. The membrane tube was operated steadily for 150 h with oxygen permeation flux of 1.12 ml/(cm² min) at 875 °C. X-ray diffraction (XRD) and energy dispersive spectroscopy (EDS) analysis showed that both the surface exposed to air and the surface exposed to helium of the BSCFO membrane tube after permeation for 150 h are similar to the fresh membrane tube in composition and structure. These results indicated that the membrane tube exhibits high structure stability.     

A multi-commuted flow injection system with a multi-channel propulsion unit placed before detection: Spectrophotometric determination of ammonium

A flow system with a multi-channel peristaltic pump placed before the solenoid valves is proposed to overcome some limitations attributed to multi-commuted flow injection systems: the negative pressure can lead to the formation of unwanted air bubbles and limits the use of devices for separation processes (gas diffusion, dialysis or ion-exchange). The proposed approach was applied to the colorimetric determination of ammonium nitrogen. In alkaline medium, ammonium is converted into ammonia, which diffuses over the membrane, causing a pH change and subsequently a colour change in the acceptor stream (bromothymol blue solution). The system allowed the re-circulation of the acceptor solution and was applied to ammonium determination in surface and tap water, providing relative standard deviations lower than 1.5%. A stopped flow approach in the acceptor stream was adopted to attain a low quantification limit (42 μg L⁻¹) and a linear dynamic range of 50–1000 μg L⁻¹ with a determination rate of 20 h⁻¹.     

On-line collection/concentration and detection of sulfur dioxide in air by flow-injection spectrophotometry coupled with a chromatomembrane cell.

A simple and rapid procedure for SO2 determination in air was developed by using a flow injection analysis (FIA) system coupled with a 3-hole chromatomembrane cell (CMC). The CMC was applied for the on-line collection/concentration of SO2 from air into a solution of 2 g l(-1) triethanolamine (TEA) solution as an absorbing solution: SO2 was converted to SO3(2-) in the alkaline absorbing solution. The solution containing absorbed SO2 was introduced into the carrier stream of the FIA system. The amount of SO3(2-) in the absorbing solution was measured by spectrophotometry with a mixed reagent of pararosaniline and formaldehyde, and was converted to the concentration of SO2 in the air sample. A calibration graph prepared by using standard sodium sulfite aqueous solutions was adopted for the determination of SO3(2-) in the absorbing solution. The SO2 concentration in indoor air examined was found to be 22.7 +/- 0.2 ppbv using 20 ml of air sample with the air flow rate of 5 ml min(-1), where the relative standard deviation was 1.7%. The detection limit for aqueous solutions and air samples were 6.9 x 10(-8) M and 0.48 ppbv, respectively. The measuring time for one sample was about 10 min when a 20 ml air sample was used. The interferences from common anionic species, formaldehyde and acetaldehyde, were also examined.     

Removal of ammonia emissions from waste air in a biotrickling filter: pilot-scale demonstration in real conditions

This study was aimed at testing the possibility of using a biotrickling filter for the treatment of waste air resulting from animal farming. For this purpose, a laboratory and pilot biotrickling filter with a moving bed were constructed. In the first case, the removal of ammonia emissions from waste air, by means of ammonia nitrogen utilization by present micro-organisms under laboratory conditions, was tested. The mass load of the biotrickling filter was gradually increased by slowly increasing the ammonia concentration. In the second case, the pilot biotrickling filter with a moving bed was installed inside a pig farm and it was tested under real operation conditions. In the first case, the highest value of the laboratory biotrickling filter’s elimination capacity was 6.2 g_NH3 m⁻³ of filling h⁻¹. The elimination capacity of the pilot filter was 1.6 g_NH3 m⁻³ of filling h⁻¹. The source of carbon for the present micro-organisms was a 1% sucrose solution, which simulated waste water with high content of COD_CR. [<-define what COD is, if mentioned for the first time] At the same time there was almost 89% decrease in waste water pollution. It was also shown that the contribution of the ammonia nitrogen utilization by the present micro-organisms to the removal of ammonia from the waste air was 90%.