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M Particles (m + particle)
Selected AbstractsThe application of novel 1.7 ,m ethylene bridged hybrid particles for hydrophilic interaction chromatographyJOURNAL OF SEPARATION SCIENCE, JSS, Issue 9 2008Eric S. Grumbach Abstract An un-derivatized 1.7 ,m ethylene bridged hybrid (BEH) particle was evaluated for its utility in retaining polar species in hydrophilic interaction chromatography (HILIC), and was compared to a 3 ,m un-derivatized silica material. Retentivity as a function of mobile phase pH, polar modifier and ACN content was examined. Also, the efficiency of the two particle substrates was compared by plotting HETP vs. linear velocity. Improved chemical resistance of the un-derivatized BEH particle was compared to un-derivatized silica at pH 5, demonstrating no performance deterioration over the course of 2000 injections for the BEH particle, while the silica particle deteriorated rapidly after 800 injections. Lastly, ESI-MS sensitivity as a function of particle size and separation mode was demonstrated. A 2.2 to 4.7-times higher ESI-MS response was observed on the 1.7 ,m particle compared to the 3 ,m particle, whereas a 5.6 to 8.8-times higher ESI-MS response was observed using HILIC as when compared to traditional RP chromatography. [source] Analysis of urinary metabolites for metabolomic study by pressurized CECELECTROPHORESIS, Issue 23 2007Guoxiang Xie Abstract A new approach for the metabolomic study of urinary samples using pressurized CEC (pCEC) with gradient elution is proposed as an alternative chromatographic separation tool with higher degree of resolution, selectivity, sensitivity, and efficiency. The pCEC separation of urinary samples was performed on a RP column packed with C18, 5,,m particles with an ACN/water mobile phase containing TFA. The effects of the acid modifiers, applied voltage, mobile phase, and detection wavelength were systematically evaluated using eight spiked standards, as well as urine samples. A typical analytical trial of urine samples from Sprague Dawley (S.D.) rats exposed to high-energy diet was carried out following sample pretreatment. Significant differences in urinary metabolic profiles were observed between the high energy diet-induced obesity rats and the healthy control rats at the 6th,wk postdose. Multivariate statistical analysis revealed the differential metabolites in response to the diet, which were partially validated with the putative standards. This work suggests that such a pCEC-based separation and analysis method may provide a new and cost-effective platform for metabolomic study uniquely positioned between the conventional chromatographic tools such as HPLC, and hyphenated analytical techniques such as LC-MS. [source] Synthesis and characterization of fullerene grafted poly(,-caprolactone)JOURNAL OF APPLIED POLYMER SCIENCE, Issue 6 2008Weihua Kai Abstract The fullerene grafted poly(,-caprolactone) (PCL) was successfully synthesized with a graft efficiency of 80%. The fullerene moieties grafted onto the PCL chain aggregate into 1,2 ,m particles so that a physical pseudo -network is formed. Because of the existence of the network structure, the fullerene grafted PCL film can retain its shape at much higher temperatures than that of pure PCL film, as observed in dynamic mechanical tests. It shows a hydrophobic gelling behavior in chloroform solution. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008 [source] A simple and rapid high-performance liquid chromatographic (HPLC) method for 5-fluorouracil (5-FU) assay in plasma and possible detection of patients with impaired dihydropyrimidine dehydrogenase (DPD) activityJOURNAL OF CLINICAL PHARMACY & THERAPEUTICS, Issue 4 2004J. Ciccolini PharmD PhD Summary Background:, Dihydropyrimidine dehydrogenase (DPD) gene polymorphism may lead to severe toxicity with 5-fluorouracil (5-FU), a major anticancer drug extensively used in clinical oncology. Drug monitoring combined with early detection of patients at risk would enable timely dose adaptation so as to maintain drug concentrations within a therapeutic window. However, the best method to identify such patients remains to be determined. Objective:, The aim of this study was to develop a rapid and simple high-performance liquid chromatographic (HPLC) method for estimating uracil/dihydrouracil (U/UH2) ratio in plasma, as an index of DPD status, and for assaying 5-FU as part of drug level monitoring. Method:, Assay of 5-FU, and U/UH2 detection were performed on a HPLC system equipped with UV detector. Analytes were separated at room temperature using a 5 ,m particles, 25 cm RP-18 X-Terra column. The mobile-phase consisted of a KH2PO4 salt solution (0·05 m) + 0·1% triethylamine (TEA) pumped at 0·4 mL/min. Detection of 5-FU and 5-bromouracil were performed at 254 nm; U and UH2 elution was monitored at 210 nm. Results:, The method was sensitive and specific for assaying 5-FU within the 5,500 ng/mL concentration range, which covers exposure levels currently met in clinical practice. The method was simple, and relatively cheap, and rapid, with an analytical run time of about 30 min. Data from a patient with 5-FU toxicity suggest that the method was capable of identifying DPD metabolic phenotype in cancer patients, based on measurement of plasma U/UH2 ratio. Conclusion:, The method described should be suitable both for detecting patients at high risk of 5-FU toxicity, and for drug level monitoring during chemotherapy. [source] Transglutaminase Catalysis of Modified Whey Protein DispersionsJOURNAL OF FOOD SCIENCE, Issue 4 2010Debra A. Clare ABSTRACT:, Transglutaminase (TGase) cross-linking reactions were accomplished using a heat-modified whey protein concentrate (mWPC) substrate after pH adjustment to 8. Based on earlier reports, the degree of lactosylation with respect to ,-lactoglobulin was lower in mWPC dispersions than measured in commercial whey concentrate (cWPC) protein solutions. In this study, a higher concentration of free sulfhydryl groups was detected in soluble supernatant fractions. Both factors potentially impact the availability of reactive lysine/glutaminyl residues required for TGase reactivity. The addition of 10 mM dithiothreitol (DTT) to the substrate mix, CBZ-glutaminyl glycine and hydroxylamine, revealed a 3.6-fold increase in TGase activity, likely due in part to maintenance of the catalytic cysteine residue in a reduced state. Furthermore, inclusion of DTT to mWPC dispersions significantly raised the apparent viscosity, independently of enzyme modification, while the rate of polymerization increased 2-fold based on OPA assay measurements. Limited cross-linking slightly increased the apparent viscosity, whereas extensive coupling lowered these values compared to equivalent nonenzyme-treated mWPC samples. Carbohydrate-staining revealed formation of glyco-polymers due to covalent linkages between glucosamine and mWPC proteins after TGase processing. Again, the apparent viscosity decreased after extensive enzymatic modification. Larger particles, sized 11.28 ,m, were observed in the structural matrix of TGase-mWPC-fixed samples compared to 8 ,m particles in control mWPC samples as viewed in scanning electron micrographs. Ultimately, the functional characteristics of TGase-mWPC ingredients may be custom-designed to deliver alternative functional attributes by adjusting the experimental reaction conditions under which catalysis is achieved. Practical Application: Taken together, these results suggest that unique TGase-mWPC and/or TGase-mWPC-glucosamine ingredients may be designed to provide novel, value-added, polymeric/glyco-polymeric protein products that afford added benefit for the milk industry. [source] Rheological Characteristics of Pimento Purée: Theoretical InterpretationJOURNAL OF FOOD SCIENCE, Issue 7 2002E. Cepedaand ABSTRACT: Rheological characteristics of pimento purée were investigated at different temperatures (5 to 40 °C). The purée serum was a cloudy liquid (0to40 ,m particles) with Newtonian behavior, and flow activation energy of 25.9 kJ/ mol. The power law model was applied to fit the pseudoplastic behavior of pimento purée. The activation energy for flow, evaluated with the Arrhenius-Guzman equation, was low and depended on the variety. A modified Krieger-Dougherty model with 2 parameters was proposed to describe the effect of wet pulp fraction on the relative viscosity. In the semi-empirical model, the colloidal contribution to the viscosity at low shear rate and the parameter variations with the shear rate were considered. [source] Measuring velocity distributions of viscous fluids using positron emission particle tracking (PEPT)AICHE JOURNAL, Issue 7 2004S. Bakalis Abstract Positron emission particle tracking (PEPT) can be used to trace the path of a radioactive particle within opaque fluids in pilot-scale equipment; the method can track particles through several centimeters of metal. PEPT has been successfully used to follow isokinetic tracers in viscous fluids and thus to measure velocity distributions under both isothermal and nonisothermal conditions in pipe flow. The accuracy of the method decreased as the measured velocities increased; the faster the particle traveled, the less accurate its detection. For velocities of up to 0.5 m/s the accuracy of the method was acceptable. Agreement between experimentally measured and theoretical velocity distributions was very good, for a range of fluids and process conditions. As tracer particles are used, there were problems ensuring that all parts of the measurement volume were sampled. This is possible to overcome to an extent by adjusting particle size; 600-,m tracers did not pass within 1 mm from the tube wall, whereas 240-,m particles passed much closer to the boundaries of the flow. © 2004 American Institute of Chemical Engineers AIChE J, 50: 1606,1613, 2004 [source] Micellar and aqueous-organic liquid chromatography using sub-2,,m packings for fast separation of natural phenolic compoundsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 13 2010Jun Cao Abstract The objective of the present work was to investigate the chromatographic behavior of natural phenolic compounds in micellar and aqueous-organic LC using a short column packed with 1.8,,m particles. Firstly, the effect of ACN and SDS on elution strength and selectivity was examined by isocratic submicellar (0,30% ACN/5% 1-butanol/1,6,mM SDS) and micellar (0,30% ACN/5% 1-butanol/40,60,mM SDS) systems. The varied concentrations of two modifiers in the mobile phases revealed different eluting power. Then, the application of organic modifier gradient was discussed in both submicellar and micellar LC using mobile phases of 4,mM SDS/5% 1-butanol or 50,mM SDS/5% 1-butanol containing ACN gradient from 0 to 30%, respectively. For micellar system, the separation was found to be better in gradient than isocratic elution. Additionally, the sensitivity of aqueous-organic LC was examined. The mobile phase was a mixture of ACN and water employing gradient elution at a flow rate of 0.5,mL/min, with analysis time below 9,min. It was found that separation efficiency was significantly better compared with micellar LC. Besides, the aqueous-organic LC has been applied to separation of various phenolic compounds in Yangwei granule or Radix Astragali samples. [source] Hydrophilic interaction and reversed-phase ultra-performance liquid chromatography TOF-MS for metabonomic analysis of Zucker rat urineJOURNAL OF SEPARATION SCIENCE, JSS, Issue 9 2008Helen G. Gika Abstract Hydrophilic interaction chromatography (HILIC) provides a complementary technique to RP methods for the retention of polar analytes for LC-MS-based metabonomic studies. Combining the advantages of both RP and HILIC separations with the efficient and rapid separations obtained using sub-2 ,m particles via the recently introduced ultra-performance LC (UPLC) enables increased coverage of the metabolites present in biological samples to be achieved. Here an HILIC-UPLC-MS method was developed to provide metabolite profiles for urine samples obtained from male Zucker rats. The resulting data were compared with results obtained for the same samples by RP-UPLC-MS and demonstrated the complementary nature of the two separations with both methods enabling discrimination between the different sample types. Interestingly sample type differentiation was based on different markers. [source] Pharmaceutical analysis by supercritical fluid chromatography: Optimization of the mobile phase composition on a 2-ethylpyridine columnJOURNAL OF SEPARATION SCIENCE, JSS, Issue 8 2008Claudio Brunelli Abstract The separation of neutral, acidic, and basic pharmaceuticals with diverse physicochemical properties by packed column supercritical fluid chromatography (pSFC) on a 2-ethylpyridine column (25 cm×4.6 mm id, 3 ,m particles) is presented. The optimization strategy involved separations at 100% methanol (MeOH) and at 50% MeOH/50% ACN while keeping the peak symmetry additives formic acid (FA) and isopropylamine (IPA) at constant levels of 0.25% v/v. By plotting the adjusted retention times as a function of the MeOH/ACN ratio, an optimal modifier ratio composition of 65% MeOH/35% ACN was found. The total set of 26 neutral, acidic, and basic pharmaceuticals was analyzed and the optimal composition experimentally verified. This mobile phase composition is currently used in pharmaceutical method development and open-access generic screening environments. [source] Fundamental and practical aspects of ultrahigh pressure liquid chromatography for fast separationsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 8 2007Naijun Wu Abstract The ongoing development of HPLC has been focused on increasing the speed and efficiency of separations over the past decade. The advances in separation speed have been primarily related to the development of column technology and instrumentation. Relatively short columns packed with sub-2 ,m particles provide high-speed separations while maintaining or increasing resolution. Ultrahigh pressure pump systems have been developed to overcome the high-pressure drop generated by such sub-2 ,m packings. In this review, fundamental and practical aspects of ultrahigh pressure or ultrahigh performance liquid chromatography (U-HPLC) are discussed. Applications of fast U-HPLC separations are also presented. [source] Effect of Calcination Conditions and Excess Alkali Carbonate on the Phase Formation and Particle Morphology of Na0.5K0.5NbO3 PowdersJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 5 2007Pornsuda Bomlai Sodium-potassium niobate [Na0.5K0.5NbO3] powders were prepared following the conventional mixed oxide method. An orthorhombic XRD pattern, consistent with single-phase Na0.5K0.5NbO3, was obtained after calcination at 900°C for 6 h. Introducing 5 mol% excess Na2CO3 and K2CO3 into the starting mixture allowed milder calcination conditions to be used, for example 800°C for 2 h. Primary particles in 5 mol% excess samples were cuboid, with maximum sizes of ,2.5 ,m. Equiaxed 0.3,0.4-,m particles were formed for non-excess powders, and also for powders prepared with 1 and 3 mol% excess alkali carbonates. The results suggest liquid formation during calcination of the excess 5-mol% starting powders. [source] Mechanochemical Formation of Metal,Ceramic CompositesJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 1 2000Nicholas J. Welham A mechanical activation technique has been used to form composites of alumina with titanium carbide, nitride, or carbonitride, both with and without elemental iron. The composites were formed by reacting elemental aluminum with either ilmenite (FeTiO3) or rutile (TiO2) concentrates in the presence of carbon and/or nitrogen in a ball-mill at ambient temperature. The reaction was complete for the ilmenite samples after milling but was completed only for rutile under hot pressing conditions. Microhardness measurements indicated that the composites had hardnesses in the range 19,30 GPa (1740,2750 VHN), with only a small variation within each sample. Elemental mapping of the pressed pellets indicated that titanium and aluminum were evenly distributed on a submicrometer level whereas iron tended to coalesce into <20 ,m particles in the presence of TiC. The coalescence decreased with the carbon content of the hard material until iron was evenly distributed with TiN. A superstoichiometric amount of aluminum led to the formation of iron,aluminum phases which decreased the iron coalescence. The XRD crystallite size of the alumina was 30,50 nm and was 25,50 nm for the titanium phases, confirming the extremely fine microstructure. [source] Combustion Measurements of Fuel-Rich Aluminum and Molybdenum Oxide Nano-Composite MixturesPROPELLANTS, EXPLOSIVES, PYROTECHNICS, Issue 2 2010Tim Bazyn Abstract Fuel rich nano-composite powders of aluminum and molybdenum oxide were tested for ignition and combustion behind the incident and reflected shock waves in a shock tube. The powders consisted of approximately 10,,m particles, each of which contained Al and MoO3 mixed by mechanical alloying on the nano-scale. These powders were aluminum rich with composition ratios of 4,:,1, 8,:,1, and 16,:,1 Al,:,MoO3 by mass. Ignition tests were performed behind incident shocks for temperatures in the range of 900 to 1500,K. From these tests, ignition delay times were obtained, and some information on combustion duration was also derived. Samples were tested in air at 0.2,MPa, and compared against nano-Al, 2.7,,m Al, and 10,,m Al baselines. Ignition results for the baseline Al cases were as expected: 10,,m Al not igniting until 2000,K, 2,,m Al igniting down to ,1400,K, and n-Al igniting as low as 1150,K. The thermite samples showed considerable improvement in ignition characteristics. At the lowest temperature tested (900,K), both the 8,:,1 and 4,:,1 samples ignited within 250,,s. The 16,:,1 sample (94% Al) ignited down to 1050,K , which represents an improvement of roughly 1000,K over baseline Al with only a small energetic penalty. In all cases, the ignition delay increased as the amount of MoO3 in the composite was reduced. The 4,:,1 nano-composite material ignited as fast or faster than the n-Al samples. Ignition delay increased with decreasing temperature, as expected. Emission spectra and temperature data were also taken for all samples using high-speed pyrometry and time-integrated spectroscopy. In these cases, measurements were made behind the reflected shock using end-wall loading, though the conditions (temperature, pressure, and gas composition) were identical to the incident shock tests. Spectroscopy showed strong AlO features in all the samples, and the spectra fit well to an equilibrium temperature. Broadband, low resolution spectra were also fit to continuum, gray body temperatures. In general, the observed temperatures were reasonably close to 3500,K, which is similar to the combustion temperatures of pure aluminum under these conditions. [source] Increasing throughput and information content for in vitro drug metabolism experiments using ultra-performance liquid chromatography coupled to a quadrupole time-of-flight mass spectrometerRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 6 2005Jose Castro-Perez The field of drug metabolism has been revolutionized by liquid chromatography/mass spectrometry (LC/MS) applications with new technologies such as triple quadrupoles, ion traps and time-of-flight (ToF) instrumentation. Over the years, these developments have often relied on the improvements to the mass spectrometer hardware and software, which has allowed users to benefit from lower levels of detection and ease-of-use. One area in which the development pace has been slower is in high-performance liquid chromatography (HPLC). In the case of metabolite identification, where there are many challenges due to the complex nature of the biological matrices and the diversity of the metabolites produced, there is a need to obtain the most accurate data possible. Reactive or toxic metabolites need to be detected and identified as early as possible in the drug discovery process, in order to reduce the very costly attrition of compounds in late-phase development. High-resolution, exact mass measurement plays a very important role in metabolite identification because it allows the elimination of false positives and the determination of non-trivial metabolites in a much faster throughput environment than any other standard current methodology available to this field. By improving the chromatographic resolution, increased peak capacity can be achieved with a reduction in the number of co-eluting species leading to superior separations. The overall enhancement in the chromatographic resolution and peak capacity is transferred into a net reduction in ion suppression leading to an improvement in the MS sensitivity. To investigate this, a number of in vitro samples were analyzed using an ultra-performance liquid chromatography (UPLC) system, with columns packed with porous 1.7,,m particles, coupled to a hybrid quadrupole time-of-flight (ToF) mass spectrometer. This technique showed very clear examples for fundamental gains in sensitivity, chromatographic resolution and speed of analysis, which are all important factors for the demands of today's HTS in discovery. Copyright © 2005 John Wiley & Sons, Ltd. [source] Fast chiral separation of drugs using columns packed with sub-2 ,m particles and ultra-high pressureCHIRALITY, Issue 3 2010Davy Guillarme Abstract The use of columns packed with sub-2 ,m particles in liquid chromatography with very high pressure conditions (known as UHPLC) was investigated for the fast enantioseparation of drugs. Two different procedures were evaluated and compared using amphetamine derivatives and ,-blockers as model compounds. In one case, cyclodextrins (CD) were directly added to the mobile phase and chiral separations were carried out in less than 5 min. However, this strategy suffered from several drawbacks linked to column lifetime and low chromatographic efficiencies. In the other case, the analysis of enantiomers was carried out after a derivatization procedure using two different reagents, 2,3,4-tri-O-acetyl-,- D -arabinopyranosyl isothiocyanate (AITC) and N -,-(2,4-dinitro-5-fluorophenyl)- L -alaninamide (Marfey's reagent). Separation of several amphetamine derivatives contained within the same sample was achieved in 2,5 min with high efficiency and selectivity. The proposed approach was also successfully applied to the enantiomeric purity determination of (+)-(S)-amphetamine and (+)-(S)-methamphetamine. Similar results were obtained with ,-blockers, and the separation of 10 enantiomers was carried out in less than 3 min, whereas the individual separation of several ,-blocker enantiomers was performed in 1 min or less. Chirality, 2010. © 2009 Wiley-Liss, Inc. [source] The Role of Functional Parameters for Topographical Characterization of Bone-Anchored ImplantsCLINICAL IMPLANT DENTISTRY AND RELATED RESEARCH, Issue 2 2006Anna Arvidsson MSc ABSTRACT Background, The surface topographical characterization of bone-anchored implants has been recommended to be based on amplitude, spatial, and hybrid parameters. There are also functional parameters that have the potential to describe characteristics important for a specific application. Purpose, The aim of the present study was to evaluate if parameters that have been described as functional in engineering applications are also relevant in the topographical characterization of bone-anchored implants. Materials and Methods, The surface topography of threaded titanium implants with different surface roughness (Sa, Sds, and Sdr) was analyzed with an optical interferometer, and five candidating functional parameters (Sbi, Sci, Svi, Sm, and Sc) were calculated. Examples of the same parameters for five commercially available dental implants were also calculated. Results, The highest core fluid retention index (Sci) was displayed by the turned implants, followed by fixtures blasted with 250- and 25-,m particles, respectively. Fixtures blasted with 75-,m Al2O3 particles displayed the lowest Sci value. This is the inverse order of the bone biological ranking based on earlier in vivo studies with the experimental surfaces included in the present study. Conclusion, A low core fluid retention index (Sci) seems favorable for bone-anchored implants. Therefore, it is suggested to include Sci to the set of topographical parameters for bone-anchored implants to possibly predict the biological outcome. [source] | ||||||||||||||||