Home About us Contact
|
Home About us Contact | ||
|
|
||
Effective Length (effective + length)
Kinds of Effective Length Selected AbstractsSPE and large-volume sample stacking in MEKC for determination of doxycycline in biological fluids: Comparison of direct injection to SPE-MEKCELECTROPHORESIS, Issue 21 2008Rade Injac Abstract A novel and simple method has been developed for the determination of doxycycline (DOX) in biological fluids. The method is based on SPE, large-volume sample stacking (LVSS) and MEKC with UV-DAD detection. Six SPE cartridges have been used in investigation for sample clean up and pre-concentration (Supelco® LC-8, LC-18, LC-SCX, and LC-WCX, as well as StrataÔ-X and X-C). DOX was determined on a 56,cm (effective length 50,cm)×50,,m id fused-silica capillary. The BGE was 20,mM borate buffer, pH 9.3, containing 80,mM SDS and 7.5%,v/v of methanol (30,s×50,mbar), and the temperature and voltage were 25°C and 30,kV, respectively. The analytical wavelength was set at 210,nm. Under optimized conditions it is possible to determine DOX in human serum, urine, semen, tears and saliva with recovery of 97.5% (RSD 2.5%). The method was shown to be sensitive (LOD is 1,,g/L) and precise (intra-day RSD 0.2 and 2.4%; inter-days 0.4 and 3.5% for migration time and peak area, respectively). Results for developed SPE-LVSS-MEKC were compared with LVSS-MEKC method with direct sample injection. The new LVSS-MEKC method is presented as a useful technique for rapid determination without extraction procedure of DOX in human urine and serum, using 80,mM of SDS, 10%,v/v of methanol and 40,mM borate buffer (pH 9.3; 30,s×50,mbar; 25°C; 30,kV; 350,nm), but not for the other biological fluids, according to lower sensitivity of the method and because of the sample composition. [source] Determination of uranium, iron, copper, and nickel from ore samples by MEKC using N,N,-ethylene bis(salicylaldimine) as complexing reagentELECTROPHORESIS, Issue 3 2008Muhammed Aslam Mirza Abstract An analytical procedure has been developed for the separation of dioxouranium(VI), iron(III), copper(II), nickel(II), cobalt(II), cobalt(III), palladium(II), and thorium(IV) by MEKC using N,N,-ethylene bis(salicylaldimine) (H2SA2en) as a complexing reagent with total runtime <4.5,min. SDS was used as micellar medium at pH,8 with sodium tetraborate buffer (0.1,M). An uncoated fused-silica capillary with an effective length of 50,cm×75,,m id was used with an applied voltage of 30,kV with photodiode array detection at 231,nm. Linear calibrations were obtained within 0.111,1000,,g/mL of each element with LODs within 37,325,ng/mL. The developed method was tested for analysis of uranium ore samples indicating its presence within 103,1789,,g/g with RSD within 0.79,1.87%. Likewise copper, nickel, and iron in their combined matrix were also simultaneously determined with RSD 0.4,1.6% (n,=,6). [source] Determination of glyoxal and methylglyoxal in the serum of diabetic patients by MEKC using stilbenediamine as derivatizing reagentELECTROPHORESIS, Issue 21 2007Muhammad A. Mirza Abstract An analytical method has been developed for the separation of glyoxal (Go), methylglyoxal (MGo), and dimethylglyoxal (DMGo) by MEKC using stilbenediamine (SD) as derivatizing reagent, separation time 6.5,min, SDS as micellar medium at pH,8, and sodium tetraborate (0.1,M) as buffer. Uncoated fused-silica capillary, effective length 50,cm×75,,m id; applied voltage 20,kV and photodiode array detection, were used. Calibration was linear within 0.02,150,,g/mL with detection limits 3.5,5.8,ng/mL. Go and MGo, observed for diabetic and healthy volunteers, were within 0.098,0.193,,g/mL Go and 0.106,0.245,,g/mL MGo with RSD 1.6,3.5 and 1.7,3.4%, respectively, in diabetics against 0.016,0.046,,g/mL Go and 0.021,0.066,,g/mL MGo with RSDs 1.5,3.5 and 1.4,3.6%, respectively, in healthy volunteers. Go and MGo in diabetics were also measured by standard addition and DMGo as an internal standard. Additives do not contribute significantly to Go and MGo matrix. [source] Determination of 1-methylhistidine and 3-methylhistidine by capillary and chip electrophoresis with contactless conductivity detectionELECTROPHORESIS, Issue 13 2007Petr T, ma Dr. Abstract CE with capacitively coupled contactless detection (C4D) was used to determine 3-methylhistidine (3-MH) and 1-methylhistidine (1-MH). The C4D response to 3-MH was studied in a BGE consisting of 500,mM acetic acid and ammonia at varying concentration and the results were compared with the theory. Complete separation of a model mixture of 3-MH, 1-MH, and histidine (His) was attained in two optimized BGEs, one containing 500,mM HAc, 20,mM NH4OH, and 0.1 % m/v hydroxyethylcellulose (HEC), pH,3.4 (I) and the other consisting of 100,mM morpholinoethanesulfonic acid (MES), 25,mM LiOH, and 0.1 % m/v HEC, pH,5.5 (II). These optimized BGEs were tested in CE/C4D analyses of urine. Promising results were obtained for separation and determination of 3-MH, 1-MH, and His on a silicon microchip, using aluminum strips as the C4D electrodes; the three analytes were baseline-separated within less than 30,s with a separation channel effective length of 38,mm. The LOD were satisfactory and amounted to 26.4,,M for 3-MH and 18.3,,M for 1-MH. [source] Effects of lactate and acetate on the determination of serum ethyl glucuronide by CZEELECTROPHORESIS, Issue 23 2006Michaela Mrázková Abstract The analysis of ethyl glucuronide,(EtG), a marker of recent alcohol consumption, in serum with an optimized CZE assay is reported. The method uses a 0.1-mm,id fused-silica capillary of 50,cm effective length that is coated with linear polyacrylamide, a pH,4.4 nicotinic acid/,-aminocaproic acid (EACA) BGE, reversed polarity and indirect analyte detection. The assay is based on a 1:1 dilution of serum with deionized water and has LODs for EtG, lactate and acetate of 3.8×10,7,M, 2.60×10,6,M and 2.18×10,6,M, respectively. Separation of EtG from endogenous macro- and microcomponents (anionic serum components of high and low concentration, respectively) and its quantification are shown to be possible for a wide range of lactate (stacker) and acetate (destacker) concentrations, macrocomponents that have an impact on the CZE behavior of EtG and that change after intake of ethanol. The assay has been successfully applied to the analysis of EtG, lactate and acetate in (i),sera of volunteers that ingested known amounts of alcohol and (ii),samples of patients that were classified (teetotalers and social drinkers vs. alcohol abusers) via analysis of carbohydrate-deficient transferrin. [source] Development of off-line and on-line capillary electrophoresis methods for the screening and characterization of adenosine kinase inhibitors and substratesELECTROPHORESIS, Issue 12 2006Jamshed Iqbal Abstract Fast and convenient CE assays were developed for the screening of adenosine kinase,(AK) inhibitors and substrates. In the first method, the enzymatic reaction was performed in a test tube and the samples were subsequently injected into the capillary by pressure and detected by their UV absorbance at 260,nm. An MEKC method using borate buffer (pH,9.5) containing 100,mM SDS (method,A) was suitable for separating alternative substrates (nucleosides). For the CE determination of AMP formed as a product of the AK reaction, a phosphate buffer (pH,7.5 or 8.5) was used and a constant current (95,,A) was applied (method,B). The methods employing a fused-silica capillary and normal polarity mode provided good resolution of substrates and products of the enzymatic reaction and a short analysis time of less than 10,min. To further optimize and miniaturize the AK assays, the enzymatic reaction was performed directly in the capillary, prior to separation and quantitation of the product employing electrophoretically mediated microanalysis (EMMA, method,C). After hydrodynamic injection of a plug of reaction buffer (20,mM Tris-HCl, 0.2,mM MgCl2, pH,7.4), followed by a plug containing the enzyme, and subsequent injection of a plug of reaction buffer containing 1,mM,ATP, 100,,M adenosine, and 20,,M,UMP as an internal standard,(I.S.), as well as various concentrations of an inhibitor, the reaction was initiated by the application of 5,kV separation voltage (negative polarity) for 0.20,min to let the plugs interpenetrate. The voltage was turned off for 5,min (zero-potential amplification) and again turned on at a constant current of ,60,,A to elute the products within 7,min. The method employing a polyacrylamide-coated capillary of 20,cm effective length and reverse polarity mode provided good resolution of substrates and products. Dose,response curves and calculated Ki values for standard antagonists obtained by CE were in excellent agreement with data obtained by the standard radioactive assay. [source] Capillary electrophoretic chiral separation of hydroxychloroquine and its metabolites in the microsomal fraction of liver homogenatesELECTROPHORESIS, Issue 5-6 2006Carmem Dickow Cardoso Abstract A rapid, selective, and low-cost chiral capillary electrophoretic method was developed for the simultaneous analysis of hydroxychloroquine (HCQ) and its three chiral metabolites: desethylchloroquine (DCQ), desethylhydroxychloroquine (DHCQ), and bisdesethylchloroquine (BDCQ) in the microsomal fraction of liver homogenates. After liquid,liquid extraction using toluene as extracting solvent, the drug and metabolites were resolved on a fused-silica capillary (50,,m ID, 50,cm total length, and 42,cm effective length), using 100,mmol/L of Tris/phosphate buffer, pH,9.0 containing 1% w/v sulfated-,-CD and 30,mg/mL hydroxypropyl-,-CD. Detection was carried out at 220,nm. The extraction procedure was efficient in removing endogenous interferents, and low values (,15%) for CVs and deviation from theoretical values were demonstrated for both within-day and between-day assays. The quantitation limit was 125,ng/mL with linear response over the 125,2000,ng/mL of concentration range for all metabolites. After validation, the method was used for an in vitro metabolism study of HCQ. The major HCQ metabolite formed by microsomal enzymes was (,)-(R)-DHCQ. [source] Second-order analysis and design of steel structures allowing for member and frame imperfectionsINTERNATIONAL JOURNAL FOR NUMERICAL METHODS IN ENGINEERING, Issue 5 2005J. X. Gu Abstract Conventional linear analysis is deficient in handling the design of slender frames since the effective length and other non-linear effects are difficult to assess accurately. Some proposed non-linear analyses cannot be directly employed for practical design since they are unable to re-produce the buckling curves of the basic structural element, a simple column under axial force, by a single element per member. This paper describes an advanced element, using the same physical significance as the advanced and second-order analysis proposed by a number of researchers and the BS5950(2000) and AS4100 (1995), for practical design of slender steel frames. The proposed element captures the physical behaviour of a structural member that the buckling strength of the member can be predicted using a single element per member and without assuming any effective length. Copyright © 2004 John Wiley & Sons, Ltd. [source] Fast CE analysis of adrenergic amines in different parts of Citrus aurantium fruit and dietary supplementsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 16 2010Laura Mercolini Abstract A CE method has been developed for the simultaneous analysis of the adrenergic amines synephrine, octopamine and tyramine in Citrus aurantium (bitter orange) fruit extracts and in dietary supplements. The analytes were separated on a fused silica capillary (50,,m id, 40.0,cm effective length, 48.5,cm total length) using a BGE composed of phosphate buffer (pH 2.5, 50,mM) and applying a 30,kV potential. The samples were injected hydrodynamically at 50,mbar for 25,s. The use of photodiode array detection (,=195,nm) allowed the quantification of the analytes and the control of peak purity. The method has been fully validated, obtaining satisfactory values of precision and extraction yield. The analytes are extracted with water from the dried whole fruits or fruit parts (endocarp, mesocarp and exocarp) or from the commercial formulations and directly injected into the CE apparatus. The results obtained were satisfactory in terms of precision (RSD <,5.7%) and accuracy (recovery >,89%). Thus, the method has demonstrated to be suitable for the qualitative and quantitative determination of synephrine, octopamine and tyramine in C. aurantium extracts, for dietary supplement quality control and for food adulteration identification. [source] Analysis of aromatic and terpenic constituents of pepper extracts by capillary electrochromatographyJOURNAL OF SEPARATION SCIENCE, JSS, Issue 4 2007Alessandro Musenga Abstract An original method based on CEC has been developed for the determination of aromatic and terpenic compounds in extracts of spices obtained from Piper nigrum. The method is based on the use of a fused silica capillary (effective length: 23.5 cm, internal diameter: 100 ,m) packed with a C18 sorbent (packing length: 23 cm, particle size: 5 ,m). The mobile phase is a 50 mM, pH 6.0 ammonium acetate/ACN (10:90 v/v) mixture. Applying a 30 kV voltage, the following 11 compounds were separated and analysed: terpinen-4-ol, caryophyllene oxide, limonene, ,-pinene, 3-carene, ,-pinene, ,-humulene, ,-caryophyllene, ,-phellandrene, eugenol and piperine. Compound determination is carried out using a diode-array detector set at 265 and 338 nm for ,-phellandrene and piperine, respectively, and at 210 nm (reference subtraction at 282 nm) for all the other analytes. The optimised method has been validated with good results in terms of linearity, limits of quantitation, detection and precision. The CEC method was successfully applied to the analysis of essential oils and methanolic extracts of ,black', ,white' and ,green' pepper. [source] Analysis of gastrodin and tetramethylpyrazine in traditional Chinese preparations by micellar electrokinetic chromatographyJOURNAL OF SEPARATION SCIENCE, JSS, Issue 6-7 2003Wang Rongying Abstract A simple, rapid, and accurate micellar electrokinetic chromatographic method has been developed for determination of gastrodin and tetramethylpyrazine in three traditional Chinese preparations: Zhennaoning jiaonang, Yangxue shengfa jiaonang, and Xiaoshuan zaizao wan. Running buffer comprising 50 mM sodium tetraborate and 15 M sodium dodecylsulfate (SDS), pH 9.50, was found to be most suitable for the separation. All experiments was performed with a 47 cm (40 cm effective length)×75 ,m ID uncoated fused-silica capillary and UV detection at 200 nm. The linear calibration ranges were 2.5,200 ,g mL,1 (R = 0.999) for gastrodin and 5.0,200 ,g mL,1 (R = 0.997) for tetramethylpyrazine; the detection limits were 0.5 ,g mL,1 and 0.8 ,g mL,1, respectively. Recoveries of the two analytes from the samples, calculated by use of a method described in detail in the text, were between 94.21 and 104.46%. The amounts of gastrodin and tetramethylpyrazine in the preparations were easily determined within 10 min. [source] Micellar electrokinetic capillary chromatography of methylxanthines-containing beverages: discussion of the molecular species involvedJOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE, Issue 4 2005Alicia B Pomilio Abstract Micellar electrokinetic capillary chromatography (MECC) experimental conditions were applied to 12 samples of methylxanthine-containing infusions of different commercial brands of yerba mate, coffee, tea and cocoa as well as two cola drinks. The best resolution in this mode of automated high-performance capillary electrophoresis (HPCE) was achieved here when using 15 kV voltage in an uncoated fused-silica capillary of 45 cm length (40 cm effective length), 50 mM sodium dodecylsulfate, 90 mM pH 8.5 borate buffer and UV detection. Theobromine, caffeine and theophylline were separated, and the peak splitting due to tautomeric species was observed. Experimental conditions were controlled, keeping constant the size of the elution window in each analysis. The limit of detection was less than 1 mg l,1, the limit of quantitation was 2.5 mg l,1 and the work range was 2.5,300 mg l,1. This HPCE,MECC system has proved suitable for the analysis/quality control of xanthines in beverages for consumption. Roles of various parameters as well as distinctly charged species of each xanthine and the origin of peak splitting in this MECC system are discussed. Copyright © 2004 Society of Chemical Industry [source] Shortest-path network interdiction,NETWORKS: AN INTERNATIONAL JOURNAL, Issue 2 2002Eitan Israeli Abstract We study the problem of interdicting the arcs in a network in order to maximize the shortest s,t path length. "Interdiction" is an attack on an arc that destroys the arc or increases its effective length; there is a limited interdiction budget. We formulate this bilevel, max,min problem as a mixed-integer program (MIP), which can be solved directly, but we develop more efficient decomposition algorithms. One algorithm enhances Benders decomposition by adding generalized integer cutting planes, called "supervalid inequalities" (SVIs), to the master problem. A second algorithm exploits a unique set-covering master problem. Computational results demonstrate orders-of-magnitude improvements of the decomposition algorithms over direct solution of the MIP and show that SVIs also help solve the original MIP faster. Published 2002 Wiley Periodicals, Inc. [source] Modelling advection and diffusion of water isotopologues in leavesPLANT CELL & ENVIRONMENT, Issue 8 2007MATTHIAS CUNTZ ABSTRACT We described advection and diffusion of water isotopologues in leaves in the non-steady state, applied specifically to amphistomatous leaves. This explains the isotopic enrichment of leaf water from the xylem to the mesophyll, and we showed how it relates to earlier models of leaf water enrichment in non-steady state. The effective length or tortuosity factor of isotopologue movement in leaves is unknown and, therefore, is a fitted parameter in the model. We compared the advection,diffusion model to previously published data sets for Lupinus angustifolius and Eucalyptus globulus. Night-time stomatal conductance was not measured in either data set and is therefore another fitted parameter. The model compared very well with the observations of bulk mesophyll water during the whole diel cycle. It compared well with the enrichment at the evaporative sites during the day but showed some deviations at night for E. globulus. It became clear from our analysis that night-time stomatal conductance should be measured in the future and that the temperature dependence of the tracer diffusivities should be accounted for. However, varying mesophyll water volume did not seem critical for obtaining a good prediction of leaf water enrichment, at least in our data sets. In addition, observations of single diurnal cycles do not seem to constrain the effective length that relates to the tortuosity of the water path in the mesophyll. Finally, we showed when simpler models of leaf water enrichment were suitable for applications of leaf water isotopes once weighted with the appropriate gas exchange flux. We showed that taking an unsuitable leaf water enrichment model could lead to large biases when cumulated over only 1 day. [source] Quantitative separation of oxytocin, norfloxacin and diclofenac sodium in milk samples using capillary electrophoresisBIOMEDICAL CHROMATOGRAPHY, Issue 9 2009Amber R. Solangi Abstract A simple, sensitive and rapid method has been developed for simultaneous separation and quantification of three different drugs: oxytocin (OT), norfloxacin (NOR) and diclofenac (DIC) sodium in milk samples using capillary electrophoresis (CE) with UV detection at 220 nm. Factors affecting the separation were pH, concentration of buffer and applied voltage. Separation was obtained in less than 9 min with sodium tetraborate buffer of pH 10.0 and applied voltage 30 kV. The separation was carried out from uncoated fused silica capillary with effective length of 50 cm with 75 µm i.d. The carrier electrolyte gave reproducible separation with calibration plots linear over 0.15,4.0 µg/mL for OT, 5,1000 µg/mL for NOR and 3,125 µg/mL for DIC. The lower limits of detection (LOD) were found to be 50 ng/mL for OT, and 1 µg/mL for NOR and DIC. The method was validated for the analysis of drugs in milk samples and pharmaceutical preparations with recovery of drugs within the range 96,100% with RSD 0.9,2.8%. Copyright © 2009 John Wiley & Sons, Ltd. [source] The capillary electrophoresis separation of benzodiazepine drug using dextran sulfate and SDS as running bufferBIOMEDICAL CHROMATOGRAPHY, Issue 3 2004Yoshio Suzuki Abstract Capillary electrophoresis has been applied the analyses of many clinical drugs due to its rapid, high-resolution separation. In this study, electrokinetic chromatography involving the combination of SDS and dextran sulfate, which are synthetic polymers, was examined in order to obtain high resolution. Use of 2% dextran sulfate (10,000 molecular weight), 20 mm SDS running buffer containing boric acid solution (pH 9.2) and a silica capillary (inner diameter of 75 µm, effective length of 50 cm, 57 cm overall length) afforded separation of 10 kinds of benzodiazepines. The detection limit was 0.2 µg/mL; additionally, reproducibilities were de,ned as the peak height and migration time. The average peak height was 5.92% (2.46,17.61), whereas the average migration time was 0.44% (0.18,0.76; n = 5). This separations system can be applied to the analysis and measurement of other pharmaceuticals as well. Copyright © 2004 John Wiley & Sons, Ltd. [source] Modeling O2 transport within engineered hepatic devicesBIOTECHNOLOGY & BIOENGINEERING, Issue 1 2003Randall E. McClelland Abstract Predicting and improving oxygen transport within bioartificial liver (BAL) devices continues to be an important engineering challenge since oxygen is one of the critical nutrients necessary for maintaining hepatocyte viability and function. Such a computational model would not only help predict outcomes but it would also allow system modifications to be analyzed prior to developing experimental protocols. This would help to facilitate future design improvements while reducing both experimental time and capital resource costs, and is the focus of the current study. Specifically, a computational model of O2 transport through collagen and microporous collagen ECMs is analyzed for hollow fiber (HF), flat plate (FP), and spheroid BAL designs. By modifying the O2 boundary conditions, hepatocyte O2 consumption levels, O2 permeability of the ECM, and ECM void fractions, O2 transport predictions are determined for each system as a function of time and distance. Accuracy of the predictive model is confirmed by comparing computational vs. experimental results for the HF BAL system. The model's results indicate that O2 transport within all three BAL designs can be improved significantly by incorporating the enhancement technique. This technique modifies a diffusion-dominant gel ECM into a porous matrix with diffusive and convective flows that mutually transport O2 through the ECMs. Although tortuous pathways increase the porous ECM's overall effective length of O2 travel, the decreased transport resistances of these pathways allow O2 to permeate more effectively into the ECMs. Furthermore, because the HF design employs convective flow on both its inner and outer ECM surfaces, greater control of O2 transport through its ECM is predicted, as compared with the single O2 source inputs of the flat plate and spheroid systems. The importance of this control is evaluated by showing how modifying the O2 concentration and/or transfer coefficients of the convective flows can affect O2 transport. © 2003 Wiley Periodicals, Inc. Biotechnol Bioeng 82: 12,27, 2003. [source] | |||||||||||||