WorldWideScience

Sample records for chromatographic columns

  1. Chromatographic Properties of Silica-Based Monolithic HPLC Columns

    OpenAIRE

    Smith, Jennifer Houston

    2002-01-01

    Silica-based monolithic HPLC columns contain a novel chromatographic support in which the traditional particulate packing has been replaced with a single, continuous network (monolith) of porous silica. The main advantage of such a network is decreased backpressure due to macropores (2 μm) throughout the network. This allows high flow rates, and hence fast analyses that are unattainable with traditional particulate columns. The Chromolith SpeedROD⠢ (EM Science, Gibbstown NJ) is a commercia...

  2. [A novel multiple-channel apparatus for packing capillary chromatographic column and its application].

    Science.gov (United States)

    Lü, Yayao; Hao, Feiran; Wang, Huanhuan; Fu, Bin; Qian, Xiaohong; Zhang, Yangjun

    2015-11-01

    A novel multiple-channel apparatus for packing capillary chromatographic column was designed and manufactured for packing six capillary chromatographic columns with close column efficiency at the same time. Briefly, it consists of a magnetic stirrer, a liquid chromatographic pump and a multiple-channel can. The reagents used for preparing ODS (C18) slurry and stirring condition of the magnetic stirrer were optimized in the study. Two batches of capillary chromatographic columns were packed under the optimum condition, and these packed capillary chromatographic columns were evaluated in the terms of peak capacity, sequence coverage, retention times of three peptide ions and column pressure using the tryptic digest of a bovine serum albumin (BSA) and detected by LC-MS in electrospray ionization (ESI) mode. The experimental results showed that the six capillary chromatographic columns packed at the same time had close column efficiencies, however, the column efficiencies of twelve capillary chromatographic columns packed at two times were significantly different. In addition, there was no significant column efficiency difference when packing one or six capillary chromatographic columns at the same time. The multiple-channel apparatus designed by us is simple, time-saving, and can be applied to pack capillary chromatographic columns with similar column efficiencies, thus it is of evident advantage over traditional one-channel apparatus. PMID:26939361

  3. CHROMATOGRAPHIC REFOLDING OF PROTEINS: MOLECULAR ACTION AND COLUMN CONTROL

    Institute of Scientific and Technical Information of China (English)

    Fangwei Wang; Yongdong Liu; Jing Chen; Zhiguo Su

    2005-01-01

    Protein expression in E. coli often results in the formation of a kind of protein aggregate called inclusion body. Conversion of the inactive protein aggregate into biologically active protein is a key step in production of recombinant products. Conventional dilution refolding technique suffers from disadvantages of low recovery and low concentration. Various chromatographic refolding techniques have been developed over the last few years. These include size-exclusion chromatography, ion exchange chromatography, hydrophobic interaction chromatography and different affinity chromatography. A successful strategy is the use of gradient elution in column control which provides a gentle and gradual change of the solution environment for the macromolecule to refold at nano-scale. The gradient refolding at column scale could minimize misfolding and aggregation which are induced by sudden change of the solution in conventional refolding operation.

  4. Radio Column Chromatographic Assay of H3-Labelled Substances

    International Nuclear Information System (INIS)

    Combined radio-chromatographic investigations of H3-labelled substances are an integral part of the majority of biochemical experiments with H3-labelled compounds. H3-radio paper chromatography yields, in a scanner with a windowless flow counter, a counting efficiency of 0,5 -1,5%, depending largely on the thickness of the paper and the self-absorption of the labelled compound. The radio gas chromatography of tritiated compounds presents no major problem. Successful use is being made of a combination of a gas chromatograph with a flow ionization chamber and vibrating reed electrometer, a system originated by K. E. Wilzbach and P. Riessz, and improved by H. Dutton, L. Mason and L. Blair. Through the use of ''Teflon'' and silicone-rubber for the insulating parts of the flow ion chamber, it can be operated at close to 300oC. Radio column chromatography with tritium holds little promise, when the column effluent is spread out as a shallow layer and slowly passes under a windowless flow counter or a scintillation counter, as was successfully tried with C14. Liquid scintillation spectrometry is likely to be the chosen method. Essentially, there are two different approaches feasible. These have been compared: 1. The column effluent is passed through a coil of plastic scintillator tubing, which is wound around a ''Plexiglas'' cylinder and placed in a bath of silicone oil in a light pipe with TiO2-reflector. Similarly, the HP-containing effluent can be directed through a test vial, filled - very much as in Steinberg's method - with plastic scintillator beads. These two approaches, that operate highly satisfactorily in the case of C14, offer low counting efficiencies of less than 1% for H3 due to the unfavourable surface to volume ratio. 2. The column effluent is combined 1:30 with a mixture of 3:2 toluene/ethanol by the action of a magnet-vibrator before being assayed while passing through a K40-free glass - coiled between the analyser- and monitor-phototubes. In order to

  5. Ion chromatographic separation of inorganic ions using a combination of hydrophilic interaction chromatographic column and cation-exchange resin column

    Institute of Scientific and Technical Information of China (English)

    Kaori ARAI; Masanobu MORI; Takahiro HIRONAGA; Hideyuki ITABASHI; Kazuhiko TANAKA

    2012-01-01

    A combination of hydrophilic interaction chromatographic ( HILIC ) column and a weakly acidic cation-exchange resin (WCX) column was used for simultaneous separation of inorganic anions and cations by ion chromatography ( IC ).Firstly,the capability of HILIC column for the separation of analyte ions was evaluated under acidic eluent conditions.The columns used were SeQuant ZIC-HILIC (ZIC-HILIC) with a sulfobetainezwitterion stationary phase (ZIC-HILIC) and Acclaim HILIC-10 with a diol stationary phase (HILIC-10).When using tartaric acid as the eluent,the HILIC columns indicated strong retentions for anions,based on ion-pair interaction.Especially,HILIC-10 could strongly retain anions compared with ZIC-HILIC. The selectivity for analyte anions of HILIC-10 with 5 mmol/L tartaric acid eluent was in the order of I- > NO3- > Br- > Cl- >H2PO4-.However,since HILIC-10 could not separate analyte cations,a WCX column (TSKgel Super IC-A/C) was connected after the HILIC column in series.The combination column system of HILIC and WCX columns could successfully separate ten ions (Na+,NH4+,K+,Mg2+,Ca2+,H2PO4-,Cl-,Br-,NO3- and I-) with elution of 4 mmol/L tartaric acid plus 8 mmol/L 18-crown-6.The relative standard deviations (RSDs) of analyte ions by the system were in the ranges of 0.02% - 0.05% in retention times and 0.18% - 5.3% in peak areas through three-time successive injections.The limits of detection at signal-to-noise ratio of 3 were 0.24 - 0.30 μmol/L for the cations and 0.31 - 1.2 μmol/L for the anions.This system was applied for the simultaneous determination of the cations and the anions in a vegetable juice sample with satisfactory results.

  6. Gas Chromatograph Method Optimization Trade Study for RESOLVE: 20-meter Column v. 8-meter Column

    Science.gov (United States)

    Huz, Kateryna

    2014-01-01

    RESOLVE is the payload on a Class D mission, Resource Prospector, which will prospect for water and other volatile resources at a lunar pole. The RESOLVE payload's primary scientific purpose includes determining the presence of water on the moon in the lunar regolith. In order to detect the water, a gas chromatograph (GC) will be used in conjunction with a mass spectrometer (MS). The goal of the experiment was to compare two GC column lengths and recommend which would be best for RESOLVE's purposes. Throughout the experiment, an Inficon Fusion GC and an Inficon Micro GC 3000 were used. The Fusion had a 20m long column with 0.25mm internal diameter (Id). The Micro GC 3000 had an 8m long column with a 0.32mm Id. By varying the column temperature and column pressure while holding all other parameters constant, the ideal conditions for testing with each column length in their individual instrument configurations were determined. The criteria used for determining the optimal method parameters included (in no particular order) (1) quickest run time, (2) peak sharpness, and (3) peak separation. After testing numerous combinations of temperature and pressure, the parameters for each column length that resulted in the most optimal data given my three criteria were selected. The ideal temperature and pressure for the 20m column were 95 C and 50psig. At this temperature and pressure, the peaks were separated and the retention times were shorter compared to other combinations. The Inficon Micro GC 3000 operated better at lower temperature mainly due to the shorter 8m column. The optimal column temperature and pressure were 70 C and 30psig. The Inficon Micro GC 3000 8m column had worse separation than the Inficon Fusion 20m column, but was able to separate water within a shorter run time. Therefore, the most significant tradeoff between the two column lengths was peak separation of the sample versus run time. After performing several tests, it was concluded that better

  7. Morphological and chromatographic characterization of molecularly imprinted monolithic columns

    Czech Academy of Sciences Publication Activity Database

    Širc, Jakub; Bosáková, Z.; Coufal, P.; Michálek, Jiří; Přádný, Martin; Hobzová, Radka; Hradil, Jiří

    2007-01-01

    Roč. 117, - (2007), s. 1-15. ISSN 1618-7229 Institutional research plan: CEZ:AV0Z40500505 Keywords : molecularly imprinted polymers * monolithic columns * morphology Subject RIV: CD - Macromolecular Chemistry Impact factor: 0.917, year: 2007

  8. High Performance Liquid Chromatographic Analysis of Phytoplankton Pigments Using a C16-Amide Column

    Science.gov (United States)

    A reverse-phase high performance liquid chromatographic (RP-HPLC) method was developed to analyze in a single run, most polar and non-polar chlorophylls and carotenoids from marine phytoplankton. The method is based on a RP-C16-Amide column and a ternary gradient system consistin...

  9. New SPE column packing material. Retention assessment method and its application for the radionuclide chromatographic separation

    International Nuclear Information System (INIS)

    The preparation of the OASISR-HLB sorbent based solid phase extraction (SPE) resins and their application for the 177Lu radioisotope separation were investigated. Di-(2-ethylhexyl) orthophosphoric acid (HDEHP) impregnated OASIS-HLB sorbent based SPE resins (OASIS-HDEHP) were successfully developed from this investigation. The wettable porosity structure of the moderately extractant impregnated OASIS-HDEHP resins is favorable for the effective diffusion of polar and ionic solutes giving good separation performance. Its good wetting ability offers ease of packing into conventional chromatographic columns. Their off-gassing-free operation makes OASIS-HDEHP columns good for long term use with highly consistent elution dynamics (several dozens of separations perfectly achievable on the same column). The simple method for the capacity factor (k') evaluation was developed to facilitate the characterization of the SPE chromatographic resin column. A competent procedure using OASISE30RS resin (one member of the OASIS-HDEHP resin group) for the separation of no-carrier added (n.c.a) 177Lu from the bulk amount of Yb target was developed. This separation procedure has showed very good performance with several prominent advantages such as the much shorter separation time (5-6 hours) and high reproducibility. Its high adsorption capacity for Yb and Lu makes it ideal for the separation of the bulky sample (50 mg Yb target for the 20 g weight resin column) for the production of the several Ci of 177Lu radioactivity. (author)

  10. Characterization of a chromatographic column for the production of 90Sr

    International Nuclear Information System (INIS)

    The experiments carried out with the objective of developing a method for 90Sr production, associated to that of 99Mo from 235U fission, which is routinely performed at Centro Atomico Ezeiza, Comision Nacional de Energia Atomica, are described. The project consists of strontium separation from a nitric solution containing uranium and a variety of fission products, by retention and subsequent elution in selective chromatographic columns. Both these columns and the conditions for their use in a routine production process have been characterized. The experiments show good Sr-Ba separation, high concentration of activity for the obtained 90Sr, and minimal losses; in addition, the non-existence of significant radiation damage, as a limiting factor of the separative capacity of the columns, has been verified. (author)

  11. Optimization of an improved single-column chromatographic process for the separation of enantiomers.

    Science.gov (United States)

    Kazi, Monzure-Khoda; Medi, Bijan; Amanullah, Mohammad

    2012-03-30

    This work addresses optimization of an improved single-column chromatographic (ISCC) process for the separation of guaifenesin enantiomers. Conventional feed injection and fraction collection systems have been replaced with customized components facilitating simultaneous separation and online monitoring with the ultimate objective of application of an optimizing controller. Injection volume, cycle time, desorbent flow rate, feed concentration, and three cut intervals are considered as decision variables. A multi-objective optimization technique based on genetic algorithm (GA) is adopted to achieve maximum productivity and minimum desorbent requirement in the region constrained by product specifications and hardware limitations. The optimization results along with the contribution of decision variables are discussed using Pareto fronts that identify non-dominated solutions. Optimization results of a similar simulated moving bed process have also been included to facilitate comparison with a continuous chromatographic process. PMID:22364669

  12. Evaluation of two commercial capillary columns for the enantioselective gas chromatographic separation of organophosphorus pesticides.

    Science.gov (United States)

    Fidalgo-Used, Natalia; Blanco-González, Elisa; Sanz-Medel, Alfredo

    2006-12-15

    The separation of the enantiomers of 13 organophosphorus pesticides (OPPs) has been investigated by gas chromatography (GC) with flame ionisation detection (FID) using two different commercially available chiral columns, Chirasil-Val (l-valine-tert-butylamide) and CP-Chirasil-Dex CB (heptakis (2,3,6-tri-O-metil)-beta-cyclodextrin). Using the Chirasil-Val column no chiral resolution was obtained for the OPPs investigated under any tested experimental condition. The use of the CP-Chirasil-Dex CB stationary phase enabled good individual enantiomeric separation of two OPPs, ruelene and trichlorfon and partial separation of naled, chloretoxyphos, isophenphos and metamidophos. Also, the obtained chromatographic results showed that Chirasil-Dex could resolve enantiomers through the combination of different mechanism (e.g. formation of inclusion complexes and/or interactions outside the cyclodextrin cavity). Under optimised conditions, precision, linearity range and detection limits were evaluated for the enantiomers of ruelene and trichlorfon using CP-Chirasil-Dex CB column and electron capture detection (ECD). By using the GC-ECD method the enantiomers of these OPPs could be satisfactorily detected at very low concentration levels. The detection limits observed were 1.5ngmL(-1) and 11.5ngmL(-1) for the enantiomers of trichlorfon and ruelene, respectively. PMID:18970881

  13. A purge-and-trap capillary column gas chromatographic method for the measurement of halocarbons in water and air

    Energy Technology Data Exchange (ETDEWEB)

    Happell, J.D.; Wallace, D.W.R.; Wills, K.D.; Wilke, R.J.; Neill, C.C.

    1996-06-01

    This report describes an automated, accurate, precise and sensitive capillary column purge- and -trap method capable of quantifying CFC-12, CFC-11, CFC-113, CH{sub 3}CCL{sub 3}, and CCL{sub 4} during a single chromatographic analysis in either water or gas phase samples.

  14. Studies on column size scale-up and flow profile in conical shape liquid chromatographic column of 10° by visualization method

    Institute of Scientific and Technical Information of China (English)

    Guan Wenna; Tan Feng; Guan Yafeng

    2006-01-01

    An improved visualization device made of polymethyl methacrylate (PMMA) was used to study the 3D flow profile inside conical columns of a 10° opening angle packed with C18 phase.The outside wall of the conical columns was rectangular in shape in order to improve the transparency property of the column wall and reduce the deformation of the image for better observation of the flow profiles of colored solutes inside the column.The influence of flow rate,particle size and shape on the flow profile of a colored band were studied on a 5-cm-long column and a scaled-up column of four fold in volume.It was found that the flow rates of the mobile phase had little influence on the flat flow profile of the iodine band while the properties of the stationary phase had a certain influence on them.We observed that the flow profiles of the scaled-up column were flat during the whole chromatographic process,and the efficiency and resolution of the column were also increased in accordance with theoretical prediction.The experimental results proved that the 10° conical columns can be proportionally scaled up while still keeping the flat flow profile,sample load per unit volume of packing material,and column efficiency,which are superior to the conventional column.

  15. Separation of molybdenum from uranium by chromatographic extraction using silica-TBP column

    International Nuclear Information System (INIS)

    Separation of molybdenum from uranium as the first step of development in producing 99Mo that will be irradiated using accelerator in PTAPB for nuclear medicine has been carried out. Chromatographic extraction was conducted using TBP (Tributyl phosphate) as the extractant that was impregnated in silica as the stationary phase, and simulated mixture of uranyl nitrate and molybdenum 5 - 10 ml with the concentration of 100 - 339.4 gU/L and 200 - 300 ppm respectively was used as the mobile phase. The 50.5 cm column extraction made from glass was packed with material of silica-TBP up to a height of 10 cm with a weight of 7 gram and a diameter of 1.2 cm. The feed was poured from the top of the column with a flow rate of 0.5 ml per minute and every two minutes (1 ml) the sample was analyzed. The uranium impregnated in silica-TBP was yellow in colour while molybdenum was colourless and passed through the column. The effluent that consisted of molybdenum was determined by Spectronic-20 at a wavelength of 460 nm in the form of complex Mo(SCN)5 molybdenum with orange in colour. The uranium attached to silica-TBP was eluded with warm HNO3 0.1 N (temperature of 60 °C) and analyzed titrimetrically using Titan method. At 10 ml mixture feed volume with molybdenum concentration of 300 ppm and uranium 100 gU/L, a separation factor (α) of 7.49 was obtained. (author)

  16. Quantitative liquid chromatographic determination of cefatrizine in serum and urine by fluorescence detection after post-column derivatization.

    Science.gov (United States)

    Crombez, E; Van der Weken, G; Van den Bossche, W; De Moerloose, P

    1979-09-21

    A fast, specific and sensitive high-performance liquid chromatographic procedure for the determination of cefatrizine, an orally active cephalosporin, in serum and urine is proposed. The drug is determined by the internal standard method, using cephradine as the internal standard. The separation is carried out on a reversed-phase column, filled with octadecylsilane chemically bonded microparticles. The eluent is a mixture of acetonitrile with 0.025 M sodium phosphate buffer (pH 7). Quantitation is effected by fluorescence detection of the fluorophores formed after post-column derivatization with fluorescamine in a packed-bed reactor. The chromatographic conditions and the conditions for the post-column derivatization are discussed. The method has been applied to serum and urine samples, which were analysed after deproteinization with trichloroacetic acid and injection of the clear supernatant. The accuracy and reproducibility of the procedure were investigated by the determination of the cefatrizine content in spiked serum and urine samples. PMID:528641

  17. Column chromatographic boron isotope separation at 5 and 17 MPa with diluted boric acid solution.

    Science.gov (United States)

    Musashi, Masaaki; Oi, Takao; Matsuo, Motoyuki; Nomura, Masao

    2008-08-01

    Boron isotopic fractionation factor (S) between boron taken up in strongly basic anion exchange resin and boron in aqueous solution was determined by breakthrough column chromatography at 5 and 17 MPa at 25 degrees C, using 0.1 mM boric acid solution as feed solution. The S values obtained were 1.018 and 1.012, respectively, which were smaller than the value reported by using the same chromatographic method at the atmospheric pressure at 25 degrees C with the boron concentration of 10mM, but were larger than the values under the same condition with much higher concentration of 100 and 501 mM. Calculations based on the theory of isotope distribution between two phases estimated that 21% (5 MPa) and 47% (17 MPa) of boron taken up in the resin phase was in the three-coordinated B(OH)(3)-form, instead of in the four-coordinated B(OH)(4)-form, at high pressures even with a very diluted boric acid solution. We discussed the present results by introducing (1) hydration and (2) a partial molar volume difference between isotopic molecules. Borate may have been partially dehydrated upon transfer from the solution phase to the resin phase at high pressures, which resulted in smaller S values compared with those at the atmospheric pressure. Instead, it may be possible that the difference in the isotopic partial molar volume difference between B(OH)(3) and B(OH)(4)(-) caused the S value to decrease with increasing pressure. PMID:18585727

  18. [Diol column as stationary phase for high performance liquid chromatographic analysis of carbohydrates in drinks with evaporative light scattering detection].

    Science.gov (United States)

    Wei, Y; Guo, L; Ding, M Y

    2001-11-01

    A high performance liquid chromatographic method with a diol column and evaporative light scattering detector (ELSD) was established for the direct analysis of fructose, glucose, sucrose, maltose and raffinose in mixture. A separation column (Lichrospher 100 Diol, 250 mm x 4.0 mm i.d., 5 microns, Hewlett-Packard, USA) and a guard column (Zorbax Rx-SIL, 12.5 mm x 4.6 mm i.d., 5 microns) were used. The mobile phase was a mixture of dichloromethane-methanol (3.2:1, volume ratio). Regression equations revealed linear relationship (correlation coefficients: 0.995-0.999) between the mass of carbohydrates injected and the peak area of carbohydrates detected by ELSD. The detection limits of ELSD (S/N = 3) were about 0.20 microgram for all carbohydrates. This system could be used for the routine analysis of simple carbohydrates in some common drinks on market. PMID:12545463

  19. A Sensitive Liquid Chromatographic Method for the Analysis of Clarithromycin with Pre-Column Derivatization: Application to a Bioequivalence Study

    Directory of Open Access Journals (Sweden)

    Amir Farshchi

    2009-03-01

    Full Text Available Objective(sA sensitive liquid chromatographic method for the analysis of clarithromycin- a macrolide antibiotic- in human serum, using pre-column derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl is described. Materials and MethodsThe method involved liquid–liquid extraction of the drug and an internal standard (amantadine followed by pre-column derivatization of the analytes with FMOC-Cl. A mixture of 0.05 M phosphate buffer containing triethylamine (2 ml/l; pH 3.8 and methanol (17:83, v/v was used as mobile phase and chromatographic separation was achieved on a Shimpack CLC-ODS column. The eluate was monitored by a fluorescence detector with respective excitation and emission wavelengths of 265 and 315 nm. ResultsThe analytical method was linear over the concentration range of 0.025-10 μg/ml of clarithromycin in human serum with a limit of quantification of 0.025 μg/ml. The assay is sensitive enough to measure drug levels obtained in human single dose studies.ConclusionIn the present method, sensitivity and the running time of analysis have been improved and successfully applied in a bioequivalence study of three different clarithromycin preparations in 12 healthy volunteers.

  20. Optimisation of a gas chromatographic method for trace gaseous impurities in nitrogen trifluoride by column sequence reversal.

    Science.gov (United States)

    de Coning, Johannes Petrus; Swinley, John McNeil

    2008-02-01

    Highly reactive fluorinated gaseous matrices require special equipment and techniques for the gas chromatographic analysis of trace impurities in these gases. The impurities that were analysed at the low mg/L levels included dioxygen (O2), dinitrogen (N2), carbon dioxide (CO2), carbon monoxide (CO), sulfur hexafluoride (SF6), methane (CH4) and nitrous oxide (N2O). Carbon tetrafluoride (CF4) is also present in the product at levels of 20-400mg/L and had to be analysed as well. This paper compares the use of a custom-built dual-channel gas chromatograph utilising single column back flush switching on one channel for the determination of O2, N2, CH4 and CO with column sequence reversal on a second channel for the determination of CO2, N2O, SF6 and CF4 to a similar system using a combination of dual-column back flush and heart-cut configurations. Pulsed discharge helium ionisation detectors were used on both channels in both configurations. PMID:18155712

  1. Development of High Precision Metal Micro-Electro-Mechanical-Systems Column for Portable Surface Acoustic Wave Gas Chromatograph

    Science.gov (United States)

    Iwaya, Takamitsu; Akao, Shingo; Sakamoto, Toshihiro; Tsuji, Toshihiro; Nakaso, Noritaka; Yamanaka, Kazushi

    2012-07-01

    In the field of environmental measurement and security, a portable gas chromatograph (GC) is required for the on-site analysis of multiple hazardous gases. Although the gas separation column has been downsized using micro-electro-mechanical-systems (MEMS) technology, an MEMS column made of silicon and glass still does not have sufficient robustness and a sufficiently low fabrication cost for a portable GC. In this study, we fabricated a robust and inexpensive high-precision metal MEMS column by combining diffusion-bonded etched stainless-steel plates with alignment evaluation using acoustic microscopy. The separation performance was evaluated using a desktop GC with a flame ionization detector and we achieved the high separation performance comparable to the best silicon MEMS column fabricated using a dynamic coating method. As an application, we fabricated a palm-size surface acoustic wave (SAW) GC combining this column with a ball SAW sensor and succeeded in separating and detecting a mixture of volatile organic compounds.

  2. Peak deconvolution to correctly assess the band broadening of chromatographic columns.

    Science.gov (United States)

    Vanderheyden, Yoachim; Broeckhoven, Ken; Desmet, Gert

    2016-09-23

    The present study provides experimental evidence for the fact that the peak deconvolution method can be applied to accurately measure the column-only dispersion of the current generation of high speed and high efficiency columns. Unlike the conventional variance difference method, it furthermore preserves any prevailing asymmetry of the column-only peak. This has been demonstrated by testing the same column on three different system configurations, with different extra-column volumes, and showing that, after deconvolution, the resulting column-only peaks coincide very well and produce very similar column-only plate height values (typical relative standard deviation comprising all runs on three different system configurations is 2-2.5%). Extensively studying a large set of theoretically produced peaks (with exactly known variance and asymmetry), it could be shown that the main criterion for the validity of the deconvolution method is that the variance of the system-only peak is minimum 1.5 times smaller than the variance of the column+system peak. The need to add a radial mixer unit to accurately assess the system-only contributions has been demonstrated as well. To illustrate its use and merits, the deconvolution method has been used to establish so-called multiple van Deemter curves, wherein plate height curves relating to different peak width definitions are shown in the same plot. These plots can give new insights in the intrinsic asymmetry of the column-only dispersion. PMID:27578411

  3. Separative analyses of a chromatographic column packed with a core-shell adsorbent for lithium isotope separation

    Energy Technology Data Exchange (ETDEWEB)

    Sugiyama, T.; Sugura, K.; Enokida, Y.; Yamamoto, I. [Nagoya University, Fro-cho, Chikusa-ku, Nagoya (Japan)

    2015-03-15

    Lithium-6 is used as a blanket material for sufficient tritium production in DT fueled fusion reactors. A core-shell type adsorbent was proposed for lithium isotope separation by chromatography. The mass transfer model in a chromatographic column consisted of 4 steps, such as convection and dispersion in the column, transfer through liquid films, intra-particle diffusion and and adsorption or desorption at the local adsorption sites. A model was developed and concentration profiles and time variation in the column were numerically simulated. It became clear that core-shell type adsorbents with thin porous shell were saturated rapidly relatively to fully porous one and established a sharp edge of adsorption band. This is very important feature because lithium isotope separation requires long-distance development of adsorption band. The values of HETP (Height Equivalent of a Theoretical Plate) for core-shell adsorbent packed column were estimated by statistical moments of the step response curve. The value of HETP decreased with the thickness of the porous shell. A core-shell type adsorbent is, then, useful for lithium isotope separation. (authors)

  4. Gas-chromatographic separation of hydrogen isotopes mixtures on capillary molecular sieve 5 A column at 173 K

    International Nuclear Information System (INIS)

    Analysis of a gas mixture of hydrogen species, is not too easy because the differences in their physical-chemical properties are very small; the most different are their masses, and consequently most common analytical method appear to be the mass-spectrometry. However, the impossibility to distinguish between two ions (atomic or molecular) with the same mass renders this method as unapplicable. Another problem is the decay of tritium with production of 3 He. These disadvantages of mass-spectrometry have made that other analytical methods, like gas chromatography, to be considered and developed. Thus, there are many papers about various chromatographic columns especially prepared for hydrogen species separation but the preparation and treatment of these columns are very difficult to reproduce. Besides these, there are two other main disadvantages: column operating temperature is very low and long retention times for hydrogen species (more than half an hour) are required. However, the gas-chromatography method still remains an appropriate one. The method described in this paper was based on using a capillary molecular sieve 5A column which has been operated for this kind of separation. The retention times were relatively short, about 8-9 minutes. The carrier gas was Ne and the detector - TCD. In the paper chromatograms for various carrier flow rates and various hydrogen isotope mixtures are presented. The results demonstrated a quite good efficiency for H2, HD, D2 and a not very good one for orthoH2-paraH2. (authors)

  5. Combined column-mobile phase mixture statistical design optimization of high-performance liquid chromatographic analysis of multicomponent systems.

    Science.gov (United States)

    Breitkreitz, Márcia C; Jardim, Isabel C S F; Bruns, Roy E

    2009-02-27

    A statistical approach for the simultaneous optimization of the mobile and stationary phases used in reversed-phase liquid chromatography is presented. Mixture designs using aqueous mixtures of acetonitrile (ACN), methanol (MeOH) and tetrahydrofuran (THF) organic modifiers were performed simultaneously with column type optimization, according to a split-plot design, to achieve the best separation of compounds in two sample sets: one containing 10 neutral compounds with similar retention factors and another containing 11 pesticides. Combined models were obtained by multiplying a linear model for column type, C8 or C18, by quadratic or special cubic mixture models. Instead of using an objective response function, combined models were built for elementary chromatographic criteria (retention factors, resolution and relative retention) of each solute or pair of solutes and, after their validation, the global separation was accomplished by means of Derringer's desirability functions. For neutral compounds a 37:12:8:43 (v/v/v/v) percentage mixture of ACN:MeOH:THF:H2O with the C18 column and for pesticides a 15:15:70 (v/v/v) ACN:THF:H2O mixture with the C8 column provide excellent resolution of all peaks. PMID:19167715

  6. Separative analyses of a chromatographic column packed with a core-shell adsorbent for lithium isotope separation

    International Nuclear Information System (INIS)

    Lithium-6 is used as a blanket material for sufficient tritium production in DT fueled fusion reactors. A core-shell type adsorbent was proposed for lithium isotope separation by chromatography. The mass transfer model in a chromatographic column consisted of 4 steps, such as convection and dispersion in the column, transfer through liquid films, intra-particle diffusion and and adsorption or desorption at the local adsorption sites. A model was developed and concentration profiles and time variation in the column were numerically simulated. It became clear that core-shell type adsorbents with thin porous shell were saturated rapidly relatively to fully porous one and established a sharp edge of adsorption band. This is very important feature because lithium isotope separation requires long-distance development of adsorption band. The values of HETP (Height Equivalent of a Theoretical Plate) for core-shell adsorbent packed column were estimated by statistical moments of the step response curve. The value of HETP decreased with the thickness of the porous shell. A core-shell type adsorbent is, then, useful for lithium isotope separation. (authors)

  7. Evolutionary multi-objective optimization based comparison of multi-column chromatographic separation processes for a ternary separation.

    Science.gov (United States)

    Heinonen, Jari; Kukkonen, Saku; Sainio, Tuomo

    2014-09-01

    Performance characteristics of two advanced multi-column chromatographic separation processes with discontinuous feed, Multi-Column Recycling Chromatogrphy (MCRC) and Japan Organo (JO), were investigated for a ternary separation using multi-objective optimization with an evolutionary algorithm. Conventional batch process was used as a reference. Fractionation of a concentrated acid hydrolysate of wood biomass into sulfuric acid, monosaccharide, and acetic acid fractions was used as a model system. Comparison of the separation processes was based on selected performance parameters in their optimized states. Flow rates and step durations were taken as decision variables whereas the column configuration and dimensions were fixed. The MCRC process was found to be considerably more efficient than the other processes with respect to eluent consumption. The batch process gave the highest productivity and the JO process the lowest. Both of the multi-column processes gave significantly higher monosaccharide yield than the batch process. When eluent consumption and monosaccharide yield are taken into account together with productivity, the MCRC process was found to be the most efficient in the studied case. PMID:25060000

  8. Column chromatographic separation of Y3+ from Sr2+ by polymeric ionizable crown ether resins

    International Nuclear Information System (INIS)

    Condensation polymers containing subunits of crown ether carboxylic acid monomers are effective stationary phases for the chromatographic separation of Y3+ and Sr2+. The pH range and metal loading capacities for the resins have been determined under equilibrium conditions. The resin can be regenerated for repeated use without losing its separation capability. Altering the molecular structure of the monomer (sym-dibenzo-16-crown-5-oxyacetic acid) by an alkyl substitution on the macrocyclic cavity decreases the loading capacity of the resin

  9. Tracheal relaxant effect of column chromatographic elutes of chloroform fraction of Adhatoda schimperiana leaves in guinea-pigs

    Directory of Open Access Journals (Sweden)

    Zelalem Petros

    2009-01-01

    Full Text Available Adhatoda schimperiana has been used in Ethiopian traditional medicine as a remedy for bronchial asthma. In the present study, tracheal relaxant effect of column chromatographic elutes (CCEs of the chloroform fraction of the leaves of the plant was investigated on guinea-pigs. The intermediate polar CCE of the chloroform fraction showed tracheal relaxant effect as observed by a right-ward shift of the dose-response curve. The maximum response to histamine in presence of the intermediate polar CCE was significantly lower than that of the chloroform fraction (p< 0.05. These results suggest that bioactivity-guided fractionation could show improved tracheal relaxant activity, and the alkaloid-rich fraction of the crude extract might be responsible for the claimed anti-asthmatic effect of the plant.

  10. Column chromatographic method for the separation of cerium from uranium using poly(dibenzo-18-Crown-6)

    International Nuclear Information System (INIS)

    A simple and efficient column chromatographic method has been developed for the separation of U(VI), Ce(III) and other metals using poly (dibenzo-18-crown-6) as stationary phase and hippuric acid as a counter ion. The various eluting agents were found efficient eluents for Ce(III). The capacity of crown polymer for Ce(III) was found to be 0.4±0.01mmol/g. The tolerance limit of various cations and anions for Ce(III) was determined. Ce(III) was quantitatively separated from other metal ions in binary as well as multicomponent mixtures. The good separation yields were obtained and had good reproducibility (±2%). The method incorporated the determination of Ce(III) in real sample. The method was simple, rapid and selective. (author)

  11. Simple automated liquid chromatographic system for splitless nano column gradient separations

    Czech Academy of Sciences Publication Activity Database

    Šesták, Jozef; Duša, Filip; Moravcová, Dana; Kahle, Vladislav

    2013-01-01

    Roč. 1276, FEB (2013), s. 26-32. ISSN 0021-9673 R&D Projects: GA MV VG20112015021; GA MV VG20102015023 Institutional support: RVO:68081715 Keywords : liquid chromatography * automation * splitless gradient * nano columns * alkylphenones Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.258, year: 2013

  12. Mass spectrometric protein characterization in proteome analysis using GELoader tip micro-columns packed with various chromatographic material

    International Nuclear Information System (INIS)

    In the early 90'ies mass spectrometry (MS) was introduced as a tool for identifying proteins in protein sequence databases. Since then it has become an integrated tool in protein characterization and is today routinely used to identify proteins separated by gel electrophoresis. A two-tiered mass spectrometric protein identification strategy has recently been proposed. In the first strategy peptide mass maps obtained from the protein of interest are compared with theoretically derived peptide mass maps from proteins in protein sequence databases. If the protein cannot be identified by this strategy, tandem mass spectrometric sequencing is used to generate enough sequence data to identify the protein in protein sequence databases or expressed sequence tag (EST) databases. However, the above strategies primarily identify a protein relatively to the DNA sequence, in which no information about e.g. post-translational modifications (PTMs) is stored. PTMs are known to modify the function, location, solubility and activity of proteins in the cell, and they are therefore very important for understanding living cells. More than 200 different PTMs are known, of which glycosylation, phosphorylation and proteolytic processing are the most common ones. Mass spectrometric analysis of PTMs on gel-separated proteins requires a higher amount of protein than for identification only. In addition, higher sequence coverage from the peptide mass maps or pre-purification of the modified peptides prior to MS analysis, is necessary for detection of putative modified peptides. In this study a multi-tiered strategy, in which GELoader tip micro-columns packed with increasingly more hydrophobic chromatographic material are used in combination with mass spectrometry, is described. The ultimate aim was to gain increased sequence coverage from peptide mixtures derived from gel-separated proteins, in order to locate modified peptides. Graphite powder is described as an alternative to traditional

  13. A Gas Chromatographic Analysis of Light Hydrocarbons on a Column Packed with Modified Silica Gel

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    A one-meter long column packed with silica gel is used to separate light hydrocarbons. The silica gel has been modified with several kinds of gas chromatography stationary phases. Among these, PEG 2000 shows fairly good effect when using 80-100 meshes silica gel for the separation of mixture of methane, ethane, ethylene, acetylene, propane, propylene and n-, i-butane. The different behavior of silica gel between batch to batch is also found. When silica gel is coated with a small amount of Al2O3 prepared with sol-gel method, better resolution has been observed on a 2-meter column compared with the non-modified silica gel.

  14. Sensitive Detection of Botulinum Neurotoxin Types C and D with an Immunoaffinity Chromatographic Column Test

    OpenAIRE

    Gessler, Frank; Hampe, Katrin; Böhnel, Helge

    2005-01-01

    A sensitive and specific immunoassay for the simultaneous detection of Clostridium botulinum type C (BoNT/C) and type D neurotoxin was developed. Goat anti-mouse immunoglobulin G was bound to polyethylene disks in a small disposable column used for this assay. The sample was preincubated together with monoclonal antibodies specific for the heavy chain of BoNT/C and D and affinity-purified, biotinylated polyclonal antibodies against these neurotoxins. This complex was captured on the assay dis...

  15. High performance liquid chromatographic determination of aflatoxins in chilli, peanut and rice using silica based monolithic column.

    Science.gov (United States)

    Khayoon, Wejdan Shakir; Saad, Bahruddin; Lee, Tien Ping; Salleh, Baharuddin

    2012-07-15

    A simple and rapid high performance liquid chromatographic with fluorescence detection method for the determination of the aflatoxin B1, B2, G1 and G2 in peanuts, rice and chilli was developed. The sample was extracted using acetonitrile:water (90:10, v/v%) and then purified by using ISOLUTE® multimode solid phase extraction. After the pre-column derivatisation, the analytes were separated within 3.7 min using Chromolith® performance RP-18e (100-4.6mm) monolithic column. To assess the possible effects of endogenous components in the food items, matrix-matched calibration was used for the quantification and validation. The recoveries of aflatoxins that were spiked into food samples were 86.38-104.5% and RSDs were aflatoxins in peanut (9), rice (5) and chilli (10) samples. Liquid chromatography-tandem mass spectrometry analysis using triple quadruple analyser and operated in the multiple reaction monitoring modes on the contaminated samples was performed for confirmation. PMID:25683424

  16. Estimation of Chromatographic Columns Performances using Computer Tomography and CFD Simulations

    DEFF Research Database (Denmark)

    Schmidt, Irma; Lottes, Florian; Minceva, Mirjana;

    2011-01-01

    show, that spherical particles seem to be more efficient than irregular ones in terms of HETP, which has to be partly a result of the more homogeneous flow profile they induce. The prediction of column performance in dependence of the structure of the packed bed was simulated by CFD (Computational...... Fluid Dynamics), using a model which besides the hydrodynamics parameters attained by CT also includes adsorption isotherms and mass transfer parameters. The results of the CFD simulation shall help to establish rules for selecting the right adsorption material for a given separation task in advance....

  17. Capillary zone electrophoresis and packed capillary column liquid chromatographic analysis of recombinant human interleukin-4.

    Science.gov (United States)

    Bullock, J

    1993-02-24

    Capillary zone electrophoresis (CZE) and packed capillary column liquid chromatography (micro-LC) have been applied to the analysis of the recombinant human protein interleukin-4 (rhIL-4). Separations for both the parent protein and its enzymatic digest were developed for the purpose of characterizing protein purity and identity. CZE separations of the intact protein were investigated over the pH range of 4.5 to 8.0 using uncoated fused silica capillaries. Gradient reversed-phase micro-LC was performed using 0.32 mm packed capillary columns at flow-rates of 5-6 microliters/min. Emphasis was placed on the ability of these methods to separate close structural variants and degradation products of the protein. Peptide mapping of the tryptic digest of rhIL-4 using a combination of CZE and micro-LC provided complimentary high resolution methods for establishing protein identity. Reproducible separations were achieved using sub-picomol amounts of sample. The advantages and problems encountered with these two techniques for characterizing rhIL-4 were assessed. PMID:8450025

  18. Chromatographic Column Separation of Rare Earth Elements by Resorcinol Formaldehyde Cationic Exchanger Resin

    International Nuclear Information System (INIS)

    Due to increase use of rare earth elements (REEs) in modern technology in the world over the past years, alternative separation method is essentially requested. Therefore, the main objective of this study is oriented to find efficient process for individual separation of light REEs from each other using resorcinol formaldehyde organic resin. In this investigation different type of eluent namely, oxalic acid, sodium hexameta phosphate and hydrazine have been tested for separation process of REEs. Optimizations of some parameters that affect on separation of REEs such as eluent concentration, flow rate and bed height of column have been performed. The results indicated that, 0.08 M of hydrazine as novel eluent at 1 ml/min is efficient for individual separation of REEs. Thus the improved successfully the separation process that more efficiently recovers the economically valuable REEs. The preliminary investigation has given promising results for lanthanides separation and production using resorcinol formaldehyde resin as stationary phase and hydrazine as novel eluent

  19. Monolithic octadecylsilyl-silica gel column for the high-speed ion chromatographic determination of acidity.

    Science.gov (United States)

    Xu, Qun; Tanaka, Kazuhiko; Mori, Masanobu; Helaleh, Murad I H; Hu, Wenzhi; Hasebe, Kiyoshi; Toada, Hiroshi

    2003-05-16

    A monolithic ODS-silica gel column modified by saturating it with lithium dodecylsulfate (Li-DS) was used to demonstrate the high-speed separation of H+ from other mono- and divalent cations, such as Na+, NH4+, K+, Mg2+ and Ca2+ using ion chromatography (IC). Using a 5 mM EDTA-2K solution containing 0.10 mM Li-DS (pH 4.80) as eluent, H+ was eluted with a sharp and symmetrical peak within 1.0 min before other cations at a flow-rate of 1.5 ml min(-1). The rapid elution of H+ and its conductimetric detection could be attributed to the presence of EDTA (HY2-), which can convert H+ ions as anions. i.e. H(+) + H2Y(2-) --> H3Y(-). The acidity of rainwater and deionized water samples was determined using this IC system with satisfactory results. PMID:12830891

  20. Sensitive detection of botulinum neurotoxin types C and D with an immunoaffinity chromatographic column test.

    Science.gov (United States)

    Gessler, Frank; Hampe, Katrin; Böhnel, Helge

    2005-12-01

    A sensitive and specific immunoassay for the simultaneous detection of Clostridium botulinum type C (BoNT/C) and type D neurotoxin was developed. Goat anti-mouse immunoglobulin G was bound to polyethylene disks in a small disposable column used for this assay. The sample was preincubated together with monoclonal antibodies specific for the heavy chain of BoNT/C and D and affinity-purified, biotinylated polyclonal antibodies against these neurotoxins. This complex was captured on the assay disk. Streptavidin-poly-horseradish peroxidase was used as a conjugate, and a precipitating substrate allowed the direct semiquantitative readout of the assay, if necessary. For a more accurate quantitative detection, the substrate can be eluted and measured in a photometer. Depending on the preincubation time, a sensitivity of 1 mouse lethal dose ml(-1) was achieved in culture supernatants. PMID:16332765

  1. Ion chromatographic analysis of tetracyclines using polymeric column and acidic eluent.

    Science.gov (United States)

    Ding, X; Mou, S

    2000-11-01

    High-performance ion chromatography (HPIC) is first successfully used to analyze tetracycline antibiotics (TCs) in this work. The TCs are well separated on a solvent compatible polymeric cation-exchange column within 12 min. Isocratic elution with acetonitrile-hydrochloride is very advantageous for routine analysis. HPIC may be seen as a specific variant of the more common high-performance liquid chromatography (HPLC) for water-soluble and polar pharmaceuticals with low hydrophobicity. The detection limits (signal-to-noise ratio=3:1) of oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC), doxycycline (DC) are 10, 10, 20 and 20 microg l(-1), respectively. Samples are prepared by vortex mixing with an ethylenediaminetetraacetic acid disodium salt (Na2EDTA)-McIlvaine buffer (pH 4.0) solution and the mixture filtrates through a molecular weight cut-off filter. The method has been successfully applied to monitor the OTC removal rate through every reactor in the process of OTC manufacturing wastewater treatment by bio-chemical technology. It is also applicable to determine the TCs residues in milk and milk powder with satisfying results. PMID:11128204

  2. Chemometrics-assisted high performance liquid chromatography-diode array detection strategy to solve varying interfering patterns from different chromatographic columns and sample matrices for beverage analysis.

    Science.gov (United States)

    Yin, Xiao-Li; Wu, Hai-Long; Gu, Hui-Wen; Hu, Yong; Wang, Li; Xia, Hui; Xiang, Shou-Xia; Yu, Ru-Qin

    2016-02-26

    This work reports a chemometrics-assisted high performance liquid chromatography-diode array detection (HPLC-DAD) strategy to solve varying interfering patterns from different chromatographic columns and sample matrices for the rapid simultaneous determination of six synthetic colorants in five kinds of beverages with little sample pretreatment. The investigation was performed using two types of LC columns under the same elution conditions. Although analytes using different columns have different co-elution patterns that appear more seriously in complex backgrounds, all colorants were properly resolved by alternating trilinear decomposition (ATLD) method and accurate chromatographic elution profiles, spectral profiles as well as relative concentrations were obtained. The results were confirmed by those obtained from traditional HPLC-UV method at a particular wavelength and the results of both methods were consistent with each other. All results demonstrated that the proposed chemometrics-assisted HPLC-DAD method is accurate, economical and universal, and can be promisingly applied to solve varying interfering patterns from different chromatographic columns and sample matrices for the analysis of complex food samples. PMID:26830638

  3. Optimization of indigenously developed column for the separation and analysis of all the six hydrogen isotopic combinations in elemental form using gas chromatograph

    International Nuclear Information System (INIS)

    Monitoring the concentrations of the hydrogen isotopes at various stages is highly important to stabilize and maintain the process parameters in a detritiation plant. Gas chromatograph equipped with the in-house prepared column was used for the analysis of gas mixtures containing Hydrogen isotopes, which employs two main factors; separation of these gases based on their affinity for the stationary phase and the substantial difference in their thermal conductivities. The column was prepared using treated γ-Alumina as a stationary phase and packed in 1/8 inch SS tube of length 2.4 meter. Further the column was optimized and its performance study was carried out using Helium as carrier gas. In this paper we have discussed the procedure of optimization and the performance of indigenously prepared column for the separation of H2, HD, HT, D2, DT and T2 using gas chromatography. (author)

  4. Development of post-column enzymic reactors with immobilized alcohol oxidase for use in the high-performance liquid chromatographic assay of alcohols with electrochemical detection.

    Science.gov (United States)

    Tagliaro, F; Schiavon, G; Dorizzi, R; Marigo, M

    1991-01-18

    The development of a very sensitive, direct injection high-performance liquid chromatographic method, using a post-column reactor with immobilized alcohol oxidase, was undertaken with the aim of determining methanol and ethanol levels in microlitre volumes of biological samples. After reversed-phase chromatography to separate methanol and ethanol, the analytes were enzymically converted into the respective aldehydes with formation of stoichiometric amounts of hydrogen peroxide, which could be measured via electrochemical oxidation at a platinum electrode. Some problems were encountered in the development of solid-phase enzymic reactors, using a delicate enzyme, that is prone to lose activity, such as alcohol oxidase. Owing to the slightly alkaline pH required for the optimum activity of alcohol oxidase, polymeric columns seemed to be preferable for the chromatography. HEMA copolymer was chosen as the stationary phase, but the methanol and ethanol peaks eluted close together and posed severe problems of limiting post-column band spreading. Reactors based on coarse supports for enzyme immobilization gave unacceptable band spreading, causing the methanol and ethanol peaks to overlap. On the other hand high-performance liquid chromatographic packings maintained the efficiency of the chromatographic separation, quite independently of the reactor volume. Polymeric supports proved superior to silicas in maintaining the enzyme activity. However, relevant changes in the enzyme substrate specificity were observed after immobilization. PMID:2061376

  5. Alternative chromatographic processes for no-carrier added 177Lu radioisotope separation. Part 1. Multi-column chromatographic process for clinically applicable

    International Nuclear Information System (INIS)

    The conventional multi-column solid phase extraction (SPE) chromatography technique using di-(2-ethylhexyl)orthophosphoric acid (HDEHP) impregnated OASIS-HLB sorbent based SPE resins (OASIS-HDEHP) was developed for the separation of no-carrier added (n.c.a) 177Lu from the bulk quantity of ytterbium target. This technique exploited the large variation of lutetium metal ion distribution coefficients in the varying acidity of the HCl solution-OASIS-HDEHP resin systems for the consecutive loading-eluting cycles performed on different columns. The production batches of several hundred mCi n.c.a 177Lu radioisotope separated from 50 mg Yb target activated in a nuclear reactor of medium neutron flux (Φ = 5 x 1013 n x cm-2 x s-1) were successfully performed using the above mentioned separation technique. With the target irradiation in a reactor of thermal neutron flux Φ = 2 x 1014 n x cm-2 x s-1 or the parallel run of several separation units, many Ci-s of n.c.a 177Lu can be profitably produced. The OASIS-HDEHP resin based multi-column SPE chromatography technique makes the separation process simple and economic and offers an automation capability for operation in highly radioactive hazardous environments. (author)

  6. Alternative chromatographic processes for no-carrier added 177Lu radioisotope separation. Part 2. The conventional column chromatographic separation combined with HPLC for high purity

    International Nuclear Information System (INIS)

    HPLC technique combined with the simple conventional column solid phase extraction (SPE) chromatography using di-(2-ethylhexyl)orthophosphoric acid (HDEHP) impregnated OASIS-HLB sorbent based SPE resins (OASIS-HDEHP ) was developed for the separation of no-carrier added (n.c.a) 177Lu from the bulk quantity of ytterbium target. This combination strategy was based on combining the advantages of the better resolution of HPLC separation of n.c.a 177Lu from the few milligram level Yb target with the high capacity of the OASISHDEHP column for the separation of 177Lu from the bulk Yb target. The production batches of several hundred mCi activity of n.c.a 177Lu radioisotope separated from 50 mg Yb target activated in a nuclear reactor of medium neutron flux (Φ = 5 x 1013 n x cm-2 x s-1) were successfully performed using this combined separation technique. With the target irradiation in a reactor of higher thermal neutron flux or with the parallel run of several separation units, several Ci-s of n.c.a 177Lu can be profitably produced on a commercial production basis. (author)

  7. Controlled ultraviolet (UV) photoinitiated fabrication of monolithic porous layer open tubular (monoPLOT) capillary columns for chromatographic applications

    OpenAIRE

    Collins, David; Nesterenko, Ekaterina; Brabazon, Dermot; Paull, Brett

    2012-01-01

    An automated column fabrication technique that is based on a ultraviolet (UV) light-emitting diode (LED) array oven, and provides precisely controlled "in-capillary" ultraviolet (UV) initiated polymerization at 365 nm, is presented for the production of open tubular monolithic porous polymer layer capillary (monoPLOT) columns of varying length, inner diameter (ID), and porous layer thickness. The developed approach allows the preparation of columns of varying length, because of an automated c...

  8. Measurement of the eddy diffusion term in chromatographic columns. I. Application to the first generation of 4.6mm I.D. monolithic columns.

    Science.gov (United States)

    Gritti, Fabrice; Guiochon, Georges

    2011-08-01

    The corrected heights equivalent to a theoretical plate (HETP) of three 4.6mm I.D. monolithic Onyx-C(18) columns (Onyx, Phenomenex, Torrance, CA) of different lengths (2.5, 5, and 10 cm) are reported for retained (toluene, naphthalene) and non-retained (uracil, caffeine) small molecules. The moments of the peak profiles were measured according to the accurate numerical integration method. Correction for the extra-column contributions was systematically applied. The peak parking method was used in order to measure the bulk diffusion coefficients of the sample molecules, their longitudinal diffusion terms, and the eddy diffusion term of the three monolithic columns. The experimental results demonstrate that the maximum efficiency was 60,000 plates/m for retained compounds. The column length has a large impact on the plate height of non-retained species. These observations were unambiguously explained by a large trans-column eddy diffusion term in the van Deemter HETP equation. This large trans-rod eddy diffusion term is due to the combination of a large trans-rod velocity bias (≃3%), a small radial dispersion coefficient in silica monolithic columns, and a poorly designed distribution and collection of the sample streamlets at the inlet and outlet of the monolithic rod. Improving the performance of large I.D. monolithic columns will require (1) a detailed knowledge of the actual flow distribution across and along these monolithic rod and (2) the design of appropriate inlet and outlet distributors designed to minimize the nefarious impact of the radial flow heterogeneity on band broadening. PMID:21733524

  9. Column chromatographic separation of Y{sup 3+} from Sr{sup 2+} by polymeric ionizable crown ether resins

    Energy Technology Data Exchange (ETDEWEB)

    Wood, D.J.; Elshani, S.; Wai, C.M. [Idaho Univ., Moscow, ID (United States). Dept. of Chemistry; Bartsch, R.A. [Texas Tech Univ., Lubbock, TX (United States). Dept. of Chemistry; Huntley, M.; Hartenstein, [Westinghouse Idaho Nuclear Co., Inc., Idaho Falls, ID (United States)

    1993-10-01

    Condensation polmers containing subunits of crown ether carboxylic acid monomers are effective stationary phases for the chromatographic separation of Y{sup 3+} and Sr{sup 2+}. The pH range and metal loading capacities for the resins have been determined under equilibrium conditions. The resin can be regenerated for repeated use without losing its separation capability. Altering the molecular structure of the monomer (sym-dibenzo-16-crown-5-oxyacetic acid) by an alkyl substitution on the macrocyclic cavity decreases the loading capacity of the resin.

  10. Column chromatographic separation of Y[sup 3+] from Sr[sup 2+] by polymeric ionizable crown ether resins

    Energy Technology Data Exchange (ETDEWEB)

    Wood, D.J.; Elshani, S.; Wai, C.M. (Department of Chemistry, University of Idaho, Moscow (United States)); Bartsch, R.A. (Department of Chemistry, Texas Tech University, Lubbock, (United States)); Huntley, M.; Hartenstein, S. (Westinghouse Idaho Nuclear Company, Inc., Idaho Falls, ID (United States))

    1993-12-20

    Condensation polymers containing subunits of crown ether carboxylic acid monomers are effective stationary phases for the chromatographic separation of Y[sup 3+] and Sr[sup 2+]. The pH range and metal loading capacities for the resins have been determined under equilibrium conditions. The resin can be regenerated for repeated use without losing its separation capability. Altering the molecular structure of the monomer (sym-dibenzo-16-crown-5-oxyacetic acid) by an alkyl substitution on the macrocyclic cavity decreases the loading capacity of the resin.

  11. Development and characterisation of an immunoaffinity chromatographic column for the on-line determination of the pesticide triclopyr.

    Science.gov (United States)

    Sanchez, F G; Diaz, A N; Herrera, R G; San Jose, L P

    2007-02-28

    An immunoaffinity column for the selective extraction and concentration of the herbicide triclopyr from water samples and quantification on line by HPLC has been developed. The immunoaffinity device was prepared by immobilising triclopyr antibodies to hydrazide derivatized azlactona beds. Efficient desorption of bound triclopyr was achieved with 70% ethanol/water solution. The column was evaluated regarding selectivity, recovery, capacity, saturation volume and reusability. Obtained results show that immunoaffinity chromatography (IAC) can be used for quantitative extraction, concentration and determination of triclopyr from water samples. PMID:19071466

  12. Analytical application of poly[dibenzo-18-crown-6] for column chromatographic separation of Nd(III) from Ce(III), U(VI) and other elements

    International Nuclear Information System (INIS)

    This research is dedicated to the study of analytical application of poly[dibenzo-18-crown-6] for separation of Nd(III) from possible lanthanides, actinides and other metal ions. A simple and efficient column chromatographic method has been developed using poly [dibenzo-18-crown-6] as stationary phase and hippuric acid as a counter ion. The capacity of crown polymer for Nd(III) was found to be 0.55 ± 0.01 mmol/g. Nd(III) was quantitatively separated from Ce(III), U(VI) and other elements in binary as well as multicomponent mixtures. Separation yields were good and reproducible (±2 %). This method has important application for separation of Nd(III) from Ce(III) rapidly and selectively. (author)

  13. Second-order Data by Flow Injection Analysis with Spectrophotometric Diode-array Detection and Incorporated Gel-filtration Chromatographic Column

    DEFF Research Database (Denmark)

    Bechmann, Iben Ellegaard

    1997-01-01

    heparin. It is shown that the rank of the involved sample data matrices corresponds to the number of chemical components present in the sample. The PARAFAC (parallel factor analysis) algorithm combined with multiple linear regression and the tri-PLS (tri-linear partial least-squares regression), which......A flow injection analysis (FIA) system furnished with a gel-filtration chromatographic column and with photodiode-array detection was used for the generation of second-order data. The system presented is a model system in which the analytes are blue dextran, potassium hexacyanoferrate(III) and...... unknown interferents are satisfactory. However, the predictions obtained by tri-PLS are slightly better than those obtained using PARAFAC regression algorithm. (C) 1997 Elsevier Science B.V....

  14. Radical-mediated step-growth: Preparation of hybrid polymer monolithic columns with fine control of nanostructural and chromatographic characteristics.

    Science.gov (United States)

    Alves, Filipa; Nischang, Ivo

    2015-09-18

    The currently most successful type of porous polymer monoliths utilized in chromatography is prepared by free-radical cross-linking (co)polymerization in porogenic solvents and a single-step molding process. Though such types of materials are well-recognized in the scientific community, they suffer from their multi-scale heterogeneity originating from the nanoscale through to their microscale and ultimately limited performance on their macroscale. This is in particular true when estimating their performance under equilibrium (i.e. isocratic) elution conditions for retained compounds. In this contribution, we study a new concept in the preparation of porous monolithic hybrid materials based on polyhedral oligomeric vinylsilsesquioxanes which undergo radical mediated step-growth cross-linking with thiol-linkers. Fundamental characterization of this new entry of materials is performed via a variety of characterization approaches including infrared and Raman spectroscopies, thermogravimetric analysis, gel fraction, dry-state surface area analysis, and visualization of the capillary-scale porous structure by scanning electron microscopy. This characterization identifies that a rational choice of experimental conditions in monolith preparation leads to destined and desirable materials' properties, in particular with experimentally accessible near-ideal nanoscale network structures. With the obtained structural informations at hand, we finally evidence the monoliths' tailored chromatographic performance by isocratic elution experiments of structurally similar small molecules under reversed-phase type of chromatographic conditions. This validates the fundamental origin for an improved performance of these types of monolithic materials under solvated conditions that has its foundation established in the creation of near-ideal nanoscale networks of material. This identified ideality is manifested in an enhanced and almost retention-insensitive performance in liquid

  15. Determination of marker pteridins and biopterin reduced forms, tetrahydrobiopterin and dihydrobiopterin, in human urine, using a post-column photoinduced fluorescence liquid chromatographic derivatization method

    Energy Technology Data Exchange (ETDEWEB)

    Canada-Canada, Florentina, E-mail: floricanada@gmail.com [Department of Analytical Chemistry, University of Extremadura, 06071 Badajoz (Spain); Espinosa-Mansilla, Anunciacion; Munoz de la Pena, Arsenio; Mancha de Llanos, Alicia [Department of Analytical Chemistry, University of Extremadura, 06071 Badajoz (Spain)

    2009-08-19

    A liquid chromatographic method for the simultaneous analysis of marker pteridins and biopterin reduced forms, in urine samples is proposed. A Zorbax Eclipse XDB-C18 column was used for the chromatographic separation, using a 98/2 (v/v), citrate buffer (pH 5.5)-acetonitrile mobile phase, in isocratic mode. A post-column photoderivatization was carried out with an on-line photoreactor, located between a diode array detector (DAD) and a fast scanning fluorescence detector (FSFD). Neopterin (NEO), biopterin (BIO), pterin (PT) and dihydrobiopterin (BH2) were determined by measuring native fluorescence, using the photoreactor in OFF-mode, and tetrahydrobiopterin (BH4) was determined by measuring of the induced fluorescence of the generated photoproducts, using the photoreactor in ON-mode. In addition, Creatinine (CREA), as a reference of metabolites excrection in urine, was simultaneously determined using the DAD detector. Detection limits were 0.2, 13.0, 0.3, 0.3 and 3.5 ng mL{sup -1}, for NEO, BH2, BIO, PT and BH4, respectively, and 0.4 {mu}g mL{sup -1} for CREA. Ratio values for NEO/CREA, PT/CREA, BH4/CREA, BH2/CREA, NEO/BIO and BIO{sub total}/CREA, in urine samples, of healthy children and adults, phenylketonuric children and infected mononucleosis children, are reported. A comparative study, about the mean values obtained for each of the compounds, by the present procedure and by the classical iodine oxidation method (Fukushimas method), has been performed, in urine samples belonging to healthy volunteers. The values obtained were BH4/CREA: 0.41, BH2/CREA: 0.31 and BIO{sub total}/CREA: 0.73, by the proposed method, and BH4/CREA: 0.35, BH2/CREA: 0.20 and BIO{sub total}/CREA: 0.48, by iodine oxidation method.

  16. Determination of marker pteridins and biopterin reduced forms, tetrahydrobiopterin and dihydrobiopterin, in human urine, using a post-column photoinduced fluorescence liquid chromatographic derivatization method

    International Nuclear Information System (INIS)

    A liquid chromatographic method for the simultaneous analysis of marker pteridins and biopterin reduced forms, in urine samples is proposed. A Zorbax Eclipse XDB-C18 column was used for the chromatographic separation, using a 98/2 (v/v), citrate buffer (pH 5.5)-acetonitrile mobile phase, in isocratic mode. A post-column photoderivatization was carried out with an on-line photoreactor, located between a diode array detector (DAD) and a fast scanning fluorescence detector (FSFD). Neopterin (NEO), biopterin (BIO), pterin (PT) and dihydrobiopterin (BH2) were determined by measuring native fluorescence, using the photoreactor in OFF-mode, and tetrahydrobiopterin (BH4) was determined by measuring of the induced fluorescence of the generated photoproducts, using the photoreactor in ON-mode. In addition, Creatinine (CREA), as a reference of metabolites excrection in urine, was simultaneously determined using the DAD detector. Detection limits were 0.2, 13.0, 0.3, 0.3 and 3.5 ng mL-1, for NEO, BH2, BIO, PT and BH4, respectively, and 0.4 μg mL-1 for CREA. Ratio values for NEO/CREA, PT/CREA, BH4/CREA, BH2/CREA, NEO/BIO and BIOtotal/CREA, in urine samples, of healthy children and adults, phenylketonuric children and infected mononucleosis children, are reported. A comparative study, about the mean values obtained for each of the compounds, by the present procedure and by the classical iodine oxidation method (Fukushimas method), has been performed, in urine samples belonging to healthy volunteers. The values obtained were BH4/CREA: 0.41, BH2/CREA: 0.31 and BIOtotal/CREA: 0.73, by the proposed method, and BH4/CREA: 0.35, BH2/CREA: 0.20 and BIOtotal/CREA: 0.48, by iodine oxidation method.

  17. Evaluation of poly(90% biscyanopropyl/10% cyanopropylphenyl siloxane) capillary columns for the gas chromatographic quantification of trans fatty acids in non-hydrogenated vegetable oils.

    Science.gov (United States)

    Delmonte, Pierluigi

    2016-08-19

    Current gas chromatographic (GC) methods for the analysis of fatty acids (FA) were optimized primarily for the quantification of the trans 18:1 FAs (18:1 tFAs) produced during the partial hydrogenation of fats and oils. Recent regulatory action regarding the application of partial hydrogenation in the processing of edible fats and oils may reshape the FA composition of these products. The higher content in 18:3 tFAs compared to 18:1 tFAs of most refined non-hydrogenated vegetable oils (RNHVO), and the challenge in their quantification applying current methods, suggest the need for new methodologies. This manuscript describes a simple GC method for the analysis of FAs in RNHVOs utilizing a 100m (0.25mm I.D.) capillary column coated with poly(90% biscyanopropyl/10% cyanopropylphenyl siloxane) (90% BCS). The optimization of the chromatographic conditions and the detection of co-eluting compounds were carried out by applying comprehensive two dimensional gas chromatography with online reduction (GC-OR×GC). Results showed that 90% BCS capillary columns operated at the elution temperature of 162°C provide the separation of the 18:1, 18:2 and 18:3 tFAs, contained in RNHVOs, from other components. A minor constituent of Canola oil, 16:3n-3, partially co-eluted with trans-18:1 FAMEs. This simple GC method showed the ability to measure trans-fat in RNHVOs at the level of 0.5g/100g, providing comparable quantitative results to the more complex GC×GC methodology. PMID:27470095

  18. Evaluation of an extraction chromatographic resin containing CMPO and ionic liquid for actinide ion uptake from acidic feeds. Pt. II. Batch actinide sorption, radiolytic degradation and column studies

    Energy Technology Data Exchange (ETDEWEB)

    Ansari, Seraj Ahmed; Mohapatra, Prasanta Kumar [Bhabha Atomic Reseach Centre, Mumbai (India). Radiochimistry Div.

    2014-10-01

    Extraction chromatographic resin prepared by impregnating CMPO-RTIL (C{sub 8}mim{sup +} . NTf{sub 2}{sup -}) on Chromosrob-W for the removal of trivalent actinides and lanthanides from aqueous solutions showed a significant improvement over the previously reported CMPO-n-dodecane resin. The resin was characterized by thermal analysis, for surface area by BET and for surface morphology by SEM. The K{sub d} value of Am(III) by CMPO-RTIL resin was found to be 5805 and 3.8 x 10{sup 4} with 3 M and 0.01 M HNO{sub 3}, respectively. The high K{sub d} values at lower acidity suggested metal ion uptake following a cation exchange mechanism usually seen with ionic liquid based solvents and use of 0.01 M EDTA resulted in a K{sub d} value of 0.11 which was subsequently used as the strippant. Uptake of other actinide ions such as UO{sub 2}{sup 2+}, Pu{sup 4+}, Np{sup 4+} and fission product element ions such as Eu{sup 3+}, Sr{sup 2+} and Cs{sup +} was also studied. Column studies using a feed containing 1 g/L Eu(III) in 3 M HNO{sub 3} suggested complete uptake of the metal ion up to passing 7 mL of the feed solution which corresponded to a column capacity of 7 mg of Eu. The loaded Eu(III) from the columns could be efficiently eluted with 0.01 M EDTA. The column capacity for Eu(III) was measured in the successive cycles of loading and elution and was found to be stable up to 60 d. The results suggested the possible application of the resins in the treatment of dilute laboratory radioactive waste. (orig.)

  19. Evaluation of an extraction chromatographic resin containing CMPO and ionic liquid for actinide ion uptake from acidic feeds. Pt. II. Batch actinide sorption, radiolytic degradation and column studies

    International Nuclear Information System (INIS)

    Extraction chromatographic resin prepared by impregnating CMPO-RTIL (C8mim+ . NTf2-) on Chromosrob-W for the removal of trivalent actinides and lanthanides from aqueous solutions showed a significant improvement over the previously reported CMPO-n-dodecane resin. The resin was characterized by thermal analysis, for surface area by BET and for surface morphology by SEM. The Kd value of Am(III) by CMPO-RTIL resin was found to be 5805 and 3.8 x 104 with 3 M and 0.01 M HNO3, respectively. The high Kd values at lower acidity suggested metal ion uptake following a cation exchange mechanism usually seen with ionic liquid based solvents and use of 0.01 M EDTA resulted in a Kd value of 0.11 which was subsequently used as the strippant. Uptake of other actinide ions such as UO22+, Pu4+, Np4+ and fission product element ions such as Eu3+, Sr2+ and Cs+ was also studied. Column studies using a feed containing 1 g/L Eu(III) in 3 M HNO3 suggested complete uptake of the metal ion up to passing 7 mL of the feed solution which corresponded to a column capacity of 7 mg of Eu. The loaded Eu(III) from the columns could be efficiently eluted with 0.01 M EDTA. The column capacity for Eu(III) was measured in the successive cycles of loading and elution and was found to be stable up to 60 d. The results suggested the possible application of the resins in the treatment of dilute laboratory radioactive waste. (orig.)

  20. Simultaneous determination of twelve benzodiazepines in human serum using a new reversed-phase chromatographic column on a 2-microns porous microspherical silica gel.

    Science.gov (United States)

    Tanaka, E; Terada, M; Misawa, S; Wakasugi, C

    1996-06-28

    A high-performance liquid chromatographic method has been developed for the simultaneous analysis of twelve frequently used benzodiazepines (BZPs) (bromazepam, clonazepam, chlordiazepoxide, estazolam, etizolam, flutazoram, haloxazolam, lorazepam, nitrazepam, oxazolam, triazolam and diazepam, internal standard) by using commercially available 2 or 5 microns particle size reversed-phase columns and a microflow cell-equipped ultraviolet detector. The separation was achieved using a C18 reversed-phase column (condition 1: 100 x 4.6 mm I.D., particle size 2 microns, TSK gel Super-ODS: conditon 2: 100 x 4.6 mm I.D., particle size 5 microns, Hypersil ODS-C18). The mobile phase was composed of methanol-5 mM NaH2PO4 (pH 6) (45:55, v/v), and the flow-rate was 0.65 ml/min (condition 1 and 2). The absorbance of the eluent was monitored at 254 nm. Retention times under condition 1 were shorter than those of condition 2. When the twelve benzodiazepines were determined, sensitivity and limits of quantification were about four to ten times better under condition 1 than under condition 2. The rate of recovery and linearity in condition 1 were approximately the same as those in condition 2. These results show that a new ODS filler with a particle size of 2 microns was more sensitive, provided better separation and was more rapid than that with conventional ODS filler. PMID:8832439

  1. Chromatographic behavior of 12 polar pteridines in hydrophilic interaction chromatography using five different HILIC columns coupled with tandem mass spectrometry.

    Science.gov (United States)

    Xiong, Xin; Liu, Yanmeng

    2016-04-01

    Retention characteristic of 5 hydrophilic interaction chromatography (HILIC) columns, containing neutral and possibly negatively charged support (silica, diol and amide), cationic phase (triazole) and zwitterionic phase (sulfobetaine), that are commercially available were studied for the separation of a group of 12 polar pteridines. The main factors influencing the retention and selectivity of pteridines for these different HILIC systems have been studied in liquid chromatography-tandem mass spectrometry (LC-MS/MS) conditions: mobile phase composition, buffer type, pH and concentration and the separation mechanism was also investigated. Results of the effects of organic modifier, buffer pH and ion strength indicate that the retention mechanism is a mixed-mode of adsorption and ion exchange, and optimization of HILIC analyses depends on the ionization state of the analytes. For silica, diol, amide and sulfobetaine phases, hydrophilic partitioning mainly contributes to the retention, while electrostatic interactions and hydrogen-bonding should be considered to understand the elution orders for triazole phase. An zwitterionic phase (ZIC-HILIC) provided the stronger retention for all pteridines than other tested columns. PMID:26838435

  2. Preperation and performance of {sup 99}Mo/{sup 99m}Tc chromatographic column generator based on zirconium molybdosilicate

    Energy Technology Data Exchange (ETDEWEB)

    Mostafa, M.; Saber, H.M.; El-Sadek, A.A. [Atomic Energy Authority, Cairo (Egypt). Hot Labs. Center; Nassar, M.Y. [Benha Univ. (Egypt). Chemistry Dept.

    2016-08-01

    Zirconium molybdosilicate (ZrMoSi) gel prepared using {sup 99}Mo radiotracer via peroxo route was used as a base material for {sup 99}Mo/{sup 99m}Tc column generator. The {sup 99m}Tc elution yield and {sup 99}Mo breakthrough in the eluate were studied as a function of the pH-value of gel precipitation, gel drying temperature and Zr: Mo: Si molar ratio. Precipitation pH-value of 2, drying temperature of 100 C and Zr: Mo: Si molar ratio of 0.5: 0.5: 1 were found to be the optimum conditions achieving {sup 99m}Tc elution yield of 82% and {sup 99}Mo breakthrough of 1.0 x 10{sup -3}%. The gel prepared with the optimum conditions was characterized by BET surface area and pore size analyzer, IR spectroscopy, thermal analysis (TGA and DTA), XRD, XRF and FESEM. Technetium-99m eluted from the optimum ZrMoSi {sup 99}Mo/{sup 99m}Tc generator was found to have a high radiochemical purity (98% as {sup 99m}TcO{sub 4}{sup -}) and chemical purity meeting criteria of clinical grade.

  3. On-line coupling of an ion chromatograph to the ICP-MS: Separations with a cation exchange chromatography column

    Energy Technology Data Exchange (ETDEWEB)

    Roellin, Stefan [Studsvik Nuclear AB, Nykoeping (Sweden)

    1999-12-01

    An ion chromatography system was coupled on-line to the ICP-MS. All separations were made with a cation exchange chromatography column. Fundamental laws about elution parameters affecting individual retention times and elution forms are explained by applying a proper ion exchange mechanism for the isocratic elution (separations with constant eluent concentration) of mono-, di-, tri-, and tetravalent cations and the actinide species MO{sub 2}{sup +} and MO{sub 2}{sup 2+}. A separation method with two eluents has been investigated to separate mono- from divalent ions in order to separate isobaric overlaps of Rb/Sr and Cs/Ba. The ions normally formed by actinides in aqueous solutions in the oxidation states III to VI are M{sup 3+}, M{sup 4+}, MO{sub 2}{sup +} and MO{sub 2}{sup 2+} respectively. Elution parameters were investigated to separate all four actinide species from each other in order to separate isobaric overlaps of the actinides Np, Pu, U and Am. A major question of concern over the possible release of actinides to the environment is the speciation of actinides within their four possible oxidation states. To check the possibility of speciation analysis with ion chromatography, a separation method was investigated to separate U{sup 4+} and UO{sub 2}{sup 2+} without changing the redox species composition during the separation. First results of Pu speciation analysis showed that Pu could be eluted as three different species. Pu(VI) was always eluting at the same time as Np(V). This was surprising as Pu(VI) is expected to have the same chemical characteristics as U(VI) and thus was expected to elute at the same time as U(VI)

  4. Development of a coupled-column liquid chromatographic-tandem mass spectrometric method for the direct determination of betamethasone in urine.

    Science.gov (United States)

    Polettini, A; Marrubini Bouland, G; Montagna, M

    1998-08-25

    Different hyphenated liquid chromatographic (LC) and mass spectrometric (MS) techniques were investigated in order to set-up a method for the fast, direct analysis of betamethasone in hydrolysed and non-hydrolysed urine using large-volume sample injection. After the optimisation of the LC parameters using a traditional UV detector and of the thermospray and mass spectrometric parameters by flow injection, urine samples (0.5 ml) were submitted to analysis by either LC combined with tandem mass spectrometry (MS-MS), coupled-column LC (LC-LC) combined with single quadrupole MS, and LC-LC-MS-MS. Both the three-step configurations (LC-MS-MS and LC-LC-MS) did not provide satisfactory results: loss of sensitivity was noted in the case of LC-MS-MS (likely due to reduced efficiency in the ionisation of betamethasone in the thermospray owing to the presence of large amounts of matrix interference), while in the case of LC-LC-MS a high chemical noise resulting in insufficient selectivity of detection was observed. On the contrary, LC-LC-MS-MS analysis proved to meet the demand of high speed of analysis (sample throughput, 4.5 h(-1)), selectivity, and sensitivity (LOQ, 1 ng/ml; LOD, 0.2 ng/ml). Notwithstanding the complex analytical system adopted, the developed procedure was manageable and very robust, provided that at the beginning of each analytical session the performance of the system was controlled by checking the retention time of the analytes on the first analytical column with UV detection and by optimising vaporiser temperature of the thermospray by flow injection. PMID:9746249

  5. Modelling of microalgal growth and lipid production in Dunaliella tertiolecta using nitrogen-phosphorus-potassium fertilizer medium in sintered disk chromatographic glass bubble column.

    Science.gov (United States)

    Kumar, Anup; Guria, Chandan; Chitres, G; Chakraborty, Arunangshu; Pathak, A K

    2016-10-01

    A comprehensive mathematical model involving NPK-10:26:26 fertilizer, NaCl, NaHCO3, light and temperature operating variables for Dunaliella tertiolecta cultivation is formulated to predict microalgae-biomass and lipid productivity. Proposed model includes Monod/Andrews kinetics for the absorption of essential nutrients into algae-biomass and Droop model involving internal nutrient cell quota for microalgae growth, assuming algae-biomass is composed of sugar, functional-pool and neutral-lipid. Biokinetic model parameters are determined by minimizing the residual-sum-of-square-errors between experimental and computed microalgae-biomass and lipid productivity using genetic algorithm. Developed model is validated with the experiments of Dunaliella tertiolecta cultivation using air-agitated sintered-disk chromatographic glass-bubble column and the effects of operating variables on microalgae-biomass and lipid productivity is investigated. Finally, parametric sensitivity analysis is carried out to know the sensitivity of model parameters on the obtained results in the input parameter space. Proposed model may be helpful in scale-up studies and implementation of model-based control strategy in large-scale algal cultivation. PMID:27450983

  6. Development and validation of a reversed-phase column liquid chromatographic method for the determination of five cephalosporins in pharmaceutical preparations.

    Science.gov (United States)

    Elkady, Ehab F; Abbas, Samah S

    2011-01-01

    A new, simple, rapid, and precise RP-HPLC method has been developed and validated for the determination of five cephalosporins, namely, cefalexin, cefoperazone, ceftriaxone, ceftazidime, and cefepime. The method has been applied successfully for simultaneous determination of cefalexin in a binary mixture with sodium benzoate in a suspension, and cefoperazone in a binary mixture with sulbactam in vials. Chromatographic separation was achieved on a Waters microBondapak C18 column (250 x 4.6 mm id, 10 pm particle size) using the mobile phase monobasic potassium phosphate (50 mM, pH 4.6)-acetonitrile (80 + 20, v/v) with UV detection. A flow rate of 1 mL/min was applied. Linearity, accuracy, and precision were found to be acceptable over the concentration range of 30-300, 3-30, and 15-120 microg/mL for the studied cephalosporins, sodium benzoate, and sulbactam, respectively. The optimized method proved to be specific, robust, and accurate for QC of the cited drugs in their pharmaceutical preparations. PMID:22165008

  7. Validated stability indicating liquid chromatographic determination of ebastine in pharmaceuticals after pre column derivatization: Application to tablets and content uniformity testing

    Directory of Open Access Journals (Sweden)

    Eid Manal

    2011-05-01

    Full Text Available Abstract An accurate, simple, sensitive and selective reversed phase liquid chromatographic method has been developed for the determination of ebastine in its pharmaceutical preparations. The proposed method depends on the complexation ability of the studied drug with Zn2+ ions. Reversed phase chromatography was conducted using an ODS C18 (150 × 4.6 mm id stainless steel column at ambient temperature with UV-detection at 260 nm. A mobile phase containing 0.025%w/v Zn2+ in a mixture of (acetonitril/methanol; 1/4 and Britton Robinson buffer (65:35, v/v adjusted to pH 4.2, has been used for the determination of ebastine at a flow rate of 1 ml/min. The calibration curve was rectilinear over the concentration range of 0.3 - 6.0 μg/ml with a detection limit (LOD of 0.13 μg/ml, and quantification limit (LOQ of 0.26 μg/ml. The proposed method was successfully applied for the analysis of ebastine in its dosage forms, the obtained results were favorably compared with those obtained by a comparison method. Furthermore, content uniformity testing of the studied pharmaceutical formulations was also conducted. The composition of the complex as well as its stability constant was also investigated. Moreover, the proposed method was found to be a stability indicating one and was utilized to investigate the kinetics of alkaline and ultraviolet induced degradation of the drug. The first-order rate constant and half life of the degradation products were calculated.

  8. Chromatographic separation of simulants of nerve and blister agents by combining one- and two-channel columns with different stationary phases.

    Science.gov (United States)

    Yuan, Huan; Du, Xiaosong; Li, Yi; Zhao, Xulan; Xu, Ming

    2016-04-01

    A two-channel gas chromatography column and a single-channel column were made by deep reactive-ion etching technology. The two short columns were coated with different stationary phases, and then linked without a modulator. This is to aim at increasing the sample capacity and achieving a higher separation efficiency in complex environments. The results show that the capacity of the connected column is approximately 4 and 1.5 times larger than that of the single- and two-channel columns, respectively. The linked column was utilized to separate a six-component mixture, composed of three simulants of nerve and blister agents and three interfering vapors. The results demonstrate that the combined column has a remarkably higher separation efficiency than the individual columns, and an acceptable resolution is achieved although the total length of the linked column is only 1.5 m. PMID:26843525

  9. Influence of batch-to-batch reproducibility of Luna C-18(2) packing material, nature of column wall material, and column diameter on the liquid chromatographic analysis of basic analytes

    NARCIS (Netherlands)

    Vervoort, RJM; Ruyter, E; Debets, AJJ; Claessens, HA; Cramers, CA; de Jong, GJ

    2001-01-01

    This paper discusses aspects arising on transferring liquid chromatography (LC) methods developed on conventional size columns to micro LC, i.e. the influence of batch-to-batch reproducibility of packing material, the nature of the column wall material, and the column inner diameter. it was shown th

  10. Comparison of phenyl-type columns in the development of a fast liquid chromatographic system for eighteen opiates commonly found in forensic toxicology.

    Science.gov (United States)

    Dams, R; Lambert, W E; Clauwaert, K M; De Leenheer, A P

    2000-10-27

    We report a precise and reliable method for the detection of 18 of the most commonly found opiates on the Belgian legal and illicit market, by ion-exchange, reversed-phase high-performance liquid chromatography, using a conventional phenyl-type analytical column (150x4.6 mm I.D., particle size 5 microm) and diode-array detection. We also describe a performance (efficiency and sensitivity) comparison of this column to a recently developed "high-speed" column (53x7.0 mm I.D., particle size 3 microm) packed with the same stationary phase, and used under slightly adjusted flow and gradient conditions. The final method, using the "high-speed" column, showed a significant reduction (55%) in analysis time without loss of resolution and sensitivity. PMID:11093666

  11. Simultaneous spectrophotometric determination of phosphate and silicate ions in river water by using ion-exclusion chromatographic separation and post-column derivatization

    OpenAIRE

    Nakatani, Nobutake; Kozaki, Daisuke; Masuda, Wakako; Nakagoshi, Nobukazu; Hasebe, Kiyoshi; Mori, Masanobu; Tanaka, Kazuhiko

    2008-01-01

    The simultaneous spectrophotometric determination of phosphate and silicate ions in river water was examined by using ion-exclusion chromatography and post-column derivatization. Phosphate and silicate ions were separated by the ion-exclusion column packed with a polymethacrylate-based weakly acidic cation-exchange resin in the H+-form (TSKgel Super IC-A/C) by using ultra pure water as an eluent. After the postcolumn derivatization with molybdate and ascorbic acid, so-called molybdenum-blue, ...

  12. High-separation efficiency micro-fabricated multi-capillary gas chromatographic columns for simulants of the nerve agents and blister agents

    OpenAIRE

    Li, Yi; Du, Xiaosong; Wang, Yang; Tai, Huiling; Qiu, Dong; Lin, Qinghao; Jiang, Yadong

    2014-01-01

    To achieve both high speed and separation efficiency in the separation of a mixture of nerve and blister agent simulants, a high-aspect-ratio micro-fabricated multi-capillary column (MCC, a 50-cm-long, 450-μm-deep, and 60-μm-wide four-capillary column) was fabricated by the application of the microelectromechanical system (MEMS) techniques. Mixtures of chemical warfare agent (CWA) simulants - dimethyl methylphosphonate (DMMP), triethyl phosphate (TEP), and methyl salicylate - were used as sam...

  13. The use of selective extraction chromatographic columns as an alternative to solvent extraction for the separation of uranium followed by the use of Arsenazo III as a colorimetric reagent for uranium determination

    International Nuclear Information System (INIS)

    The use of U/TEVA reg-sign Spec columns as an alternative to solvent extraction for separation of uranium prior to its determination by various techniques (calorimetric, phosphorescence, and mass spectroscopy) was investigated. U/TEVA reg-sign Spec columns have several advantages over the widely used 4-methyl-2-pentanone solvent extraction method. Among the advantages are: (1) no hazardous liquid organic waste, that creates regulatory waste disposal problems, is generated; (2) a clean separation of U from Zr, F, and fission products is obtained; (3) the sample preparation time is reduced; and (4) the exposure of analysts to ionizing radiation is reduced because the entire procedure may be performed in a hot cell using remote operations. This study also investigated the use of Arsenazo III (1,8-dihydroxynapthalene-3,6-disulfonic acid-2,7-bis [-phenylarsonic acid]) as a calorimetric reagent to determine uranium concentrations over a wide range in waste streams and product streams at the Idaho Chemical Processing Plant. Process and waste stream samples were passed through a U/TEVA reg-sign Spec column to selectively remove the uranium. The uranium bearing fraction is compatible with the pH range for color development with Arsenazo III. Arsenazo III may be added to the uranium fraction, at a 3:1 mole ratio (Arsenazo:Uranium) at the high end of the method (10 μ/mL). Arsenazo III forms a highly stable complex with uranium. Stability tests from this and other studies show that the colored complex of Arsenazo III with U(VI) forms within one minute and remains stable for several hours. The complex with U(VI) varies in color with pH. However, with excess reagent, the color is varying shades of purple. Since the samples were passed through a highly selective extraction chromatographic column prior to adding the calorimetric reagent, no interferences were observed

  14. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Nakamoto, Akihiro [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nishida, Manami [Hiroshima University Technical Center, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Saito, Takeshi [Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, Shimokasuya 143, Isehara, Kanagawa 259-1143 (Japan); Kishiyama, Izumi; Miyazaki, Shota [GL Sciences Inc., Sayamagahara 237-2, Iruma, Saitama 358-0032 (Japan); Murakami, Katsunori [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nagao, Masataka [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Namura, Akira, E-mail: namera@hiroshima-u.ac.jp [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan)

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d{sub 5} was used as an internal standard. The linear ranges were 0.01-5.0 {mu}g mL{sup -1} for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 {mu}g mL{sup -1} for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation {>=}0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 {mu}g mL{sup -1} of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio {>=} 3) in urine was 5 ng mL{sup -1} for MA and MDMA and 10 ng mL{sup -1} for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  15. Simultaneous high-performance liquid chromatographic determination of nitrate, nitrite, and organic pesticides in soil solution using a multidimensional column with ultraviolet detection

    International Nuclear Information System (INIS)

    In many fertilizer trials, the amount of nitrate-nitrogen in soil solution must be quantified frequently because nitrate is easily leached. Because pesticides are generally applied to cropland with fertilizers, quantitative information is needed on the concentration of these chemicals still available in the soil. Information on nitrite, nitrate and pesticide concentrations in food, water and environmental samples is essential because of their toxicity and potential for groundwater and surface water contamination. Most of the methods currently used for nitrate determination also account for nitrite, because nitrite and some organics act as interferences. Some of the existing analytical methods require sample reduction or derivatization, complex solvent mixtures or large sample volumes which make analysis times long. A High-Performance Liquid Chromatography (HPLC) method has been developed for the simultaneous determination of nitrate, nitrite and organic pesticides in soil solution samples and extracts using a multidimensional separator column with ultraviolet detection at 220 nm. The method is rapid and requires small sample volumes (20 μL). It is a sensitive method which is suitable for routine analyses of up to 100 samples per day. A comparison of this method with standard ion chromatography with conductivity detection showed very good agreement between the two methods for the analysis of NO3- and NO2-

  16. A fluorous porous polymer monolith photo-patterned chromatographic column for the separation of a flourous/fluorescently labeled peptide within a microchip.

    Science.gov (United States)

    Xu, Zhenpo; Oleschuk, Richard D

    2014-02-01

    A fluorous porous polymer stationary phase is photo-patterned within a glass microfluidic chip to conduct CEC. During free radical-initiated polymerization, extraneous polymer forms and contributes to excessive microfluidic channel clogging. Nitrobenzene is explored as free radical quencher to limit clogging by minimizing extraneous polymer formation and a number of initiator to quencher ratios are explored with a 0.5:1 quencher (nitrobenzene): initiator (benzoin methyl ether) molar ratio shown to be optimal. The microchip patterned with a fluorous monolith was used to carry out the electrochromatographic analysis of a mixture containing fluorescent and fluorous labeling products. The fluorous monolithic column shows fluorous selectivity for compounds labeled with perfluoromethylene tags and a custom peptide is synthesized that possesses functional groups that can be both fluorescently and fluorously labeled. MALDI MS was used to identify the labeled fragments and microchip based electrochromatography was used to analyze the resulting labeling mixture. This is the first report to our knowledge that uses fluorous porous polymer monolith within a microchip to separate analytes using fluorous-fluorous interactions. PMID:24170603

  17. Column chromatographic separation of Ce(III) from U(VI) and other elements in hippuric acid medium as an analytical application of poly[dibenzo-18-crown-6

    International Nuclear Information System (INIS)

    A simple and efficient column chromatographic method has been developed for the separation of Ce(III) from U(VI) and Ni(II)/Zn(II)/Cd(II)/Co(II)/Ba(II) etc. using poly[dibenzo-18-crown-6] as stationary phase and hippuric acid as a counter ion. HCl and H2SO4 were most efficient eluting agents for Ce(III). The capacity of crown polymer for Ce(III) was found to be 0.285 ± 0.01 mmol/g. The tolerance limits of various cations and anions for Ce(III) were determined. Ce(III) was quantitatively separated from U(VI) and Ni(II)/Zn(II)/Cd(II)/Co(II)/Ba(II) in binary as well as multicomponent mixtures. The good separation yields were obtained and had good reproducibility (±2 %). The method incorporated the determination of Ce(III) in real sample. The method was simple, rapid and selective. (author)

  18. Optimization of the gas chromatographic separations

    International Nuclear Information System (INIS)

    A review and a critical study on the optimization of the gas chromatographic separations are made. After dealing with the fundamental gas chromatographic equations, some methods of expressing column performances are discussed: performance indices, performance parameters, resolution and effective plate number per unit time. This is completed with a comparative study on performances of various types of columns. Moreover, optimization methods for operating chromatographic conditions are extensively dealt with: as resolution optimization, separation time, and normalization techniques for the time of analysis in order to achieve the maximum resolution at constant time. Finally, some others non operating parameters such as: selectivity of stationary phases, column preparation and optimization methods by means of computers are studied. (Author) 68 refs

  19. Experimental investigation of liquid chromatography columns by means of computed tomography

    DEFF Research Database (Denmark)

    Astrath, D.U.; Lottes, F.; Vu, Duc Thuong;

    2007-01-01

    The efficiency of packed chromatographic columns was investigated experimentally by means of computed tomography (CT) techniques. The measurements were carried out by monitoring tracer fronts in situ inside the chromatographic columns. The experimental results were fitted using the equilibrium di...

  20. 柱前衍生高效液相色谱法测定食品中黄曲霉毒素B1、B2、G1、G2%The aflatoxin B1 ,B2 ,G1 and G2 in food were decontaminated by high performance liquid chromatograph with a sample was derived before column

    Institute of Scientific and Technical Information of China (English)

    王阳; 曹忠波

    2011-01-01

    目的:通过采用多功能小柱,利用高效液相色谱仪对食品中黄曲霉毒素B1、B2、G1、G2同时进行检测.方法:样品经体积分数为90%的乙腈溶液提取,提取液通过多功能小柱净化、浓缩,三氟乙酸(TFA)柱前衍生,C18色谱柱分离,荧光检测器检测,外标法定量.结果:4种黄曲霉毒素经过衍生后线性良好,对添加黄曲霉毒素的样品进行加标回收,回收率在80.4%~94.5%,精密度<10%.结论:该方法操作简便,线性范围广,效果良好.%Objective:The aflatoy in B1, B2, G1 and G2 in food were decontaminated by a many- sided column and detected simultaneously by high performance liquid chromatograph. Methods: The sample was extracted by acetonitrile solution with a volume fraction 90%, and then the extracted solution was decontaminated and concentrated by column, derived before trifluoroacetic acid (TFA) column, separated by C18 chromatographic column ,detected by fluorescence detector and quantified by external standard method,as seen,the four aflatoxins after derivation had good linearity. Results: The standard recovery rate of food samples with addition of aflatoxins was 80.4% ~ 94.5%, the RSD was below 10%. Conclusion: It shows the method is simple, the linear scope is wide, the result is good.

  1. On the Retention Behaviors of 13 Residual Organophosphorus Pesticides in Broccoli on Different Chromatographic Columns in Gas Chromatography%西兰花中13种有机含磷农药在不同色谱柱上的色谱保留行为

    Institute of Scientific and Technical Information of China (English)

    徐霞; 朱智伟; 应兴华

    2012-01-01

    应用AgilentGC6890气相色谱仪(附FPD检测器)对13种残留于西兰花中的有机含磷农药(OPP’s)在4种不同极性的毛细管色谱柱(即DB-1、DB-5、DB-1701及DB-35MS)上的保留行为作了研究。结果表明:采用由DB-5及DB-1701串联组成的色谱柱单元,西兰花中13种残留OPP’s可达到有效分离和测定。%The retention of 13 organophosphorus pesticides (OPP' s) in broccoli on 4 capillary chromatographic columns with different polarities, namely DB-1, DB-5, DB-1701 and DB-35MS was studied using the gas chromatograph Agilant GC 6890 with FPD detector. As shown by the experimental results, by combining use of the DB-5 and DB-1701 columns in series, residues of the 13 OPP's in broccoli were effectively separated and determined.

  2. Evaluation of glycidyl methacrylate-based monolith functionalized with weak anion exchange moiety inside 0.5 mm i.d. column for liquid chromatographic separation of DNA

    Directory of Open Access Journals (Sweden)

    Aprilia Nur Tasfiyati

    2016-03-01

    Full Text Available In this study, the organic polymer monolith was developed as a weak anion exchanger column in high performance liquid chromatography for DNA separation. Methacrylate-based monolithic column was prepared in microbore silicosteel column (100 × 0.5 mm i.d. by in-situ polymerization reaction using glycidyl methacrylate as monomer; ethylene dimethacrylate as crosslinker; 1-propanol, 1,4-butanediol, and water as porogenic solvents, with the presence of initiator α,α′-azobisisobutyronitrile (AIBN. The monolith matrix was modified with diethylamine to create weak anion exchanger via ring opening reaction of epoxy groups. The morphology of the monolithic column was studied by SEM. The properties of the monolithic column, such as permeability, mechanical stability, binding capacity and pore size distribution, were characterized in detail. From the results of the characterization, monoliths poly-(GMA-co-EDMA with total monomer percentage (%T 40 and crosslinker percentage (%C 25 was found to be the ideal composition of monomer and crosslinker. It has good mechanical stability and high permeability, adequate molecular recognition sites (represented with binding capacity value of 36 mg ml−1, and has relatively equal proportion of flow-through pore and mesopores (37.2% and 41.1% respectively. Poly-(GMA-co-EDMA with %T 40 and %C 25 can successfully separate oligo(dT12–18 and 50 bp DNA ladder with good resolution.

  3. Investigations into the chromatographic optimization of combined gas chromatographic/FTIR/MS

    Science.gov (United States)

    Wulff, Ditmar

    1989-12-01

    Even with the explosive growth and acceptance of GC/MS it has some analytical limitations. Several of these deficiencies can be overcome with information provided by GC/FTIR. Combining a GC/MS and a GC/FTIR into one system provides economies of sample, time, space, and money as well as a higher confidence qualitative result. The later results from the ability of the mass spectro -meter to give molecular fragment information with strength in homolog identification while the infrared spectrometer gives class specific-functional group and geometrical isomer data. Several configurations of the combined light pipe GC/FTIR/MS are evaluated looking toward ease of use, information content, and data evaluation. The combined system's sensitivity, chromatographic integrity, and gas chromatographic column choices and their operational parameters are discussed. The series arrangement with the GC column effluent passing through the FTIR light pipe and then serially to the MS is compared to the post column split of the column effluent to the FTIR and MS as well as to the configuration using two GC columns. Operational recommendations are given to maximize chromatographic resolution, detector sensitivity, and sample throughput. Examples are shown illustrating the combined systems operation. All parameters discussed apply to work done on the HP 5890A GC, the HP5965A IRD, and the HP 5970B MSD.

  4. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

    Science.gov (United States)

    Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

    1996-01-01

    A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

  5. Chromatographic profiling: From samples to information

    OpenAIRE

    S. Peters

    2013-01-01

    Chromatography exists for over a hundred years and has become an important part of analytical chemistry. With the development of new instrumentations and columns that can measure more analytes at higher sensitivities simultaneously a new tool has been made possible: chromatographic profiling. Here, samples are measured untargeted and their entire profiles are then correlated to their properties, the chemical process or whatever type of research question needed to be answered. One special type...

  6. Ion-exclusion chromatographic behavior of aliphatic carboxylic acids and benzenecarboxylic acids on a sulfonated styrene--divinylbenzene co-polymer resin column with sulfuric acid containing various alcohols as eluent.

    Science.gov (United States)

    Ohta, Kazutoku; Towata, Atsuya; Ohashi, Masayoshi

    2003-05-16

    The addition of C1-C7 alcohols (methanol, ethanol, propanol, butanol, heptanol, hexanol and heptanol) to dilute sulfuric acid as eluent in ion-exclusion chromatography using a highly sulfonated styrene-divinylbenzene co-polymer resin (TSKgel SCX) in the H+ form as the stationary phase was carried out for the simultaneous separations of both (a) C1-C7 aliphatic carboxylic acids (formic, acetic, propionic, isobutyric, butyric, isovaleric, valeric, 2-methylvaleric, isocaproic, caproic, 2,2-dimethyl-n-valeric, 2-methylhexanoic, 5-methylhexanoic and heptanoic acids) and (b) benzenecarboxylic acids (pyromellitic, hemimellitic, trimellitic, o-phthalic, m-phthalic, p-phthalic, benzoic and salicylic acids and phenol). Heptanol was the most effective modifier in ion-exclusion chromatography for the improvement of peak shapes and a reduction in retention volumes for higher aliphatic carboxylic acids and benzenecarboxylic acids. Excellent simultaneous separation and relatively highly sensitive conductimetric detection for these C1-C7 aliphatic carboxylic acids were achieved on the TSKgel SCX column (150 x 6 mm I.D.) in 30 min using 0.5 mM sulfuric acid containing 0.025% heptanol as eluent. Excellent simultaneous separation and highly sensitive UV detection at 200 nm for these benzenecarboxylic acids were also achieved on the TSKgel SCX column in 30 min using 5 mM sulfuric acid containing 0.075% heptanol as eluent. PMID:12830881

  7. A Novel High Performance Liquid Chromatographic Method for Simultaneous Determination of Ceftriaxone and Sulbactam in Sulbactomax

    OpenAIRE

    Shrivastava, Sanjay Mohan; Singh, Rajkumar; Tariq, Abu; Siddiqui, Masoom Raza; Yadav, Jitendar; Negi, P. S.; Chaudhary, Manu

    2009-01-01

    An isocratic liquid chromatographic method with UV detection at 220 nm is described for simultaneous determination of ceftriaxone sodium and sulbactam sodium in Sulbactomax. Chromatographic separation of two drugs was achieved on a Hypersil ODS C-18 column using a mobile phase consisting of a binary mixture of acetonitrile and tetrabutyl ammonium hydroxide adjusted to pH7.0 with orthophosphoric acid in ratio 70:30. The developed Liquid Chromatographic method offers symmetric peak shape, good ...

  8. Determination of hexachlorocyclohexane pesticide residues in wool fat by a combined high-performance liquid chromatographic-gas-liquid chromatographic method

    International Nuclear Information System (INIS)

    Beta- and gamma-hexachlorocyclohexane residues were determined in twelve wool fat samples by using a combined high-performance liquid chromatographic (HPLC)-gas-liquid chromatographic (GLC) method. After extraction and chromatographic clean-up on a silca-gel column, the sample was further purified by HPLC on a reversed-phase C-18 column with methanol as the mobile phase. The final determination was effected by GLC with a 1-mCi nickel-63 electron-capture detector. The analytical method was checked by addition of carbon-14-labelled lindane and measurement of the radioactivity in a liquid scintillation counter. (Auth.)

  9. Ion-exclusion chromatographic separations of C1-C6 aliphatic carboxylic acids on a sulfonated styrene-divinylbenzene co-polymer resin column with 5-methylhexanoic acid as eluent.

    Science.gov (United States)

    Ohta, Kazutoku; Towata, Atsuya; Ohashi, Masayoshi

    2003-05-16

    The application of C7 aliphatic carboxylic acids (heptanoic, 2-methylhexanoic, 5-methylhexanoic and 2,2-dimethyl-n-valeric acids) as eluents in ion-exclusion chromatography with conductimetric detection for C1-C6 aliphatic carboxylic acids (formic, acetic, propionic, isobutyric, butyric, isovaleric, valeric, isocaproic and caproic acids) was carried out using a highly sulfonated styrene-divinylbenzene co-polymer resin (TSKgel SCX) in the H+ form as a stationary phase. When using 0.05 mM sulfuric acid at pH 4.0 as the eluent, peak shapes of hydrophobic carboxylic acids (isovaleric, valeric, isocaproic and caproic acids) were tailed strongly. In contrast, when using 1 mM these C7 carboxylic acids at pH ca. 4 as the eluents, although system peaks (vacant peaks) corresponding to these C7 carboxylic acids appeared, peak shapes of these hydrophobic acids were improved drastically. Excellent simultaneous separation and relatively high sensitive conductimetric detection for these C1-C6 aliphatic carboxylic acids were achieved in 25 min on the TSKgel SCX column (150 x 6 mm I.D.) using 1 mM 5-methylhexanoic acid at pH 4.0 as the eluent. PMID:12830882

  10. Gas chromatographic separation of methoxylated polychlorinated biphenyl atropisomers

    OpenAIRE

    Kania-Korwel, Izabela; Vyas, Sandhya M.; Song, Yang; Lehmler, Hans-Joachim

    2008-01-01

    Several polychlorinated biphenyls (PCBs) and their hydroxylated metabolites display axial chirality. Here we describe an enantioselective, gas chromatographic separation of methylated derivatives of hydroxylated (OH-)PCB atropisomers (MeO-PCB) using a chemically bonded β-cyclodextrin column (Chirasil-Dex). The atropisomers of several MeO-PCBs could be separated on this column with resolutions ranging from 0.42–0.87 under isothermal or temperature-programmed conditions. In addition, the enanti...

  11. HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC SEPARATION OF THE ENANTIOMERS OF ORGANOPHOSPHORUS PESTICIDES ON POLYSACCHARIDE CHIRAL STATIONARY PHASES

    Science.gov (United States)

    High-performance liquid chromatographic separation of the individual enantiomers of 12 organophosphorus pesticides (OPs) was obtained on polysaccharide enantioselective HPLC columns using alkane-alcohol mobile phase. The OP pesticides were crotoxyphos, dialifor, fonofos, fenamiph...

  12. Column flotation

    Energy Technology Data Exchange (ETDEWEB)

    Kohmuench, J.N.; Norrgran, D.A.; Luttrell, E.; Luttrell, G.H. [Virginia Tech. (United States)

    2008-04-15

    Over the last decade, column flotation has been recognised in the industry to be most efficient and economical means of recovering fine coal while maximizing product grade. When designed properly, flotation columns provide a high combustible recovery while maintaining a low product ash. The paper looks at the benefits of using column flotation for fine coal recovery. 2 refs., 5 figs.

  13. Transport Characteristics of Porous Solids Derived from Chromatographic Measurements

    Czech Academy of Sciences Publication Activity Database

    Šolcová, Olga; Schneider, Petr

    2002-01-01

    Roč. 144, - (2002), s. 475-482. ISSN 0167-2991 R&D Projects: GA ČR GA104/01/0546; GA AV ČR IAA4072915 Keywords : transport parameters * diffusion coefficients * chromatographic column Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.468, year: 2002

  14. Nanofluidic Size-Exclusion Chromatograph

    Science.gov (United States)

    Feldman, Sabrina; Svehla, Danielle; Grunthaner, Frank; Feldman, Jason; Shakkottai, P.

    2004-01-01

    Efforts are under way to develop a nanofluidic size-exclusion chromatograph (SEC), which would be a compact, robust, lightweight instrument for separating molecules of interest according to their sizes and measuring their relative abundances in small samples. About as large as a deck of playing cards, the nanofluidic SEC would serve, in effect, as a laboratory on a chip that would perform the functions of a much larger, conventional, bench-top SEC and ancillary equipment, while consuming much less power and much smaller quantities of reagent and sample materials. Its compactness and low power demand would render it attractive for field applications in which, typically, it would be used to identify and quantitate a broad range of polar and nonpolar organic compounds in soil, ice, and water samples. Size-exclusion chromatography is a special case of high-performance liquid chromatography. In a conventional SEC, a sample plug is driven by pressure along a column packed with silica or polymer beads that contain uniform nanopores. The interstices between, and the pores in, the beads collectively constitute a size-exclusion network. Molecules follow different paths through the size-exclusion network, such that characteristic elution times can be related to sizes of molecules: basically, smaller molecules reach the downstream end of the column after the larger ones do because the smaller ones enter minor pores and stay there for a while, whereas the larger ones do not enter the pores. The volume accessible to molecules gradually diminishes as their size increases. All molecules bigger than a pore size elute together. For most substances, the elution times and sizes of molecules can be correlated directly with molecular weights. Hence, by measuring the flux of molecules arriving at the downstream end as a function of time, one can obtain a liquid mass spectrum for the molecules present in a sample over a broad range of molecular weights.

  15. HILIC separation mechanisms of tetracyclines on amino bonded silica column

    Science.gov (United States)

    Effects of mobile phase variations on the chromatographic separation on amino bonded silica column in hydrophilic interaction chromatography (HILIC) were investigated for four zwitterionic tetracyclines (TCs): oxytetracycline, doxycycline, chlortetracycline and tetracycline. A mixed-mode retention m...

  16. A chromatographic device with automatic registration of concentration of stable and radioactive rare-earth elements in flow

    International Nuclear Information System (INIS)

    Described is a chromatographic device with automatic registration of concentration of stable and radioactive rare-earth elements (REE) in flow. Presented is separation of the mixture of stable and radioactive REE by 0.05 mol. solution of diethylenetriaminepentaacetic acid with automatic control of REE filtrate at the exit from the chromatographic column

  17. Chromatographic decontamination of medium-activity waste concentrates

    International Nuclear Information System (INIS)

    The chromatographic decontamination of a MAW concentrate was carried out in a laboratory plant in 1-l-batches in the following way: In order to purify the nitric MAW concentrate from its solid and organic contamination products, it is passed through a filter and an absorber (SM7) for organic species. Subsequently the purified solution runs on-line through all following columns. First the main activity carrier cesium (137Cs, 134Cs) is transferred to ammonium molybdate phosphate (AMP-1) by means of a newly developed fluidized bed process. In the further course, 125Sb is separated on metal oxides (Sb2O5, MnO2) and the three-valued actinides/lanthanides on an extraction-chromatographic CMPO column. Finally the remaining 106Ru and 60Co activities are separated on dimethylglyoximes (DMG) coated on active carbon. (orig./RB)

  18. Enantiomer separation of polychlorinated biphenyls on chiral chromatographic columns of cellulose and amylose by high-performance liquid chromatography%多氯联苯在纤维素和直链淀粉衍生物类手性色谱柱上的拆分

    Institute of Scientific and Technical Information of China (English)

    尹文华; 吴丞往; 方力; 张安平

    2012-01-01

    由于多氯联苯(Polychlorinated biphenyls)的纯对映体样品非常难得,国内外大多数的研究工作仅局限于外消旋体,而较少对其对映体的环境行为、生物毒性进行研究.采用三种不同的手性色谱柱对21种手性多氯联苯在不同流动相体系进行了拆分.最终有17种手性多氯联苯达到基线或部分分离,在纯正己烷流动相体系的拆分效果最佳.直链淀粉-三(5-氯-2-甲基苯基氨基甲酸酯)固定相具有很强的手性识别能力,Lux 3u Amylose-2柱可以作为Lux 3u Cellulose-1柱手性拆分的很好补充.当手性多氯联苯分子只含一个4号位氯代或同时含有5,5,号位氯代时,三种手性色谱柱较难对其分离完全.该方法分离速度快,可以作为纯对映体样品的制备方法.%Due to the enantiomer of polychlorinated biphenyls is rare, most of researches were focused on racemes, rather than environmental behavior or biotoxicity of enantiomer at home and abroad. The work investigated enantiomeric separation of 21 kinds of polychlorinated biphenyls with different chiral chromatographic columns by high-performance liquid chromatography. 17 kinds of PCBs achieved baseline or were at least partially separated. This was proved to be the most efficient for the chiral separation of 100% n-hexane mobile phase. As a kind of chiral stationary phases (CSPs), amylose tris (5-chlorine 2-methylphenylcarbamate) has a strong capacity of chiral recognition. Lux 3u Amylose-2 CSP is a great complementary for the chiral separation of Lux 3u Cellulose-1 CSP. The separations are difficult to be achieved for these three CSPs when polychlorinated biphenyls with chlorine substitution only in 4 position or in 5, 5' positions simultaneously. However, this approach could be used to obtain pure enantiomer of PCBs.

  19. Chromatographic separation of alkaline phosphatase from dental enamel

    DEFF Research Database (Denmark)

    Moe, D; Kirkeby, S; Salling, E

    1989-01-01

    Alkaline phosphatase (AP) was prepared from partly mineralized bovine enamel by extraction in phosphate buffer, centrifugation and various chromatographic techniques. Chromatofocusing showed that the enamel enzyme possessed five isoelectric points at the acid pH level ranging from pH 5.7 to pH 4.......4. Three enzyme peaks were eluted using low pressure chromatography with a Bio-gel column. With a HPLC gel filtration column the separation of the enamel extract resulted in only one peak with AP activity. The fractions of this peak were used to produce an antibody against bovine AP....

  20. Gas chromatographic analysis of trace gas impurities in tungsten hexafluoride.

    Science.gov (United States)

    Laurens, J B; de Coning, J P; Swinley, J M

    2001-03-01

    Highly reactive fluorinated gaseous matrices require special equipment and techniques for the gas chromatographic analysis of trace impurities in these gases. The impurities that were analysed at the low-microg/l levels included oxygen, nitrogen, carbon dioxide, carbon monoxide, sulfur hexafluoride and hydrogen. This paper describes the use of a system utilising backflush column switching to protect the columns and detectors in the analysis of trace gas impurities in tungsten hexafluoride. Two separate channels were used for the analysis of H2, O2, N2, CO, CO2 and SF6 impurities with pulsed discharge helium ionisation detection. PMID:11269587

  1. Reverse phase-high performance liquid chromatographic separation of lighter lanthanides using salicylic acid as eluent

    International Nuclear Information System (INIS)

    Reversed Phase High Performance Liquid Chromatography (RP-HPLC) using salicylic acid as eluent was studied on unmodified reversed phase column to achieve the separation of lighter lanthanides (La, Ce, Pr, Nd and Sm ). Various chromatographic parameters namely concentrations of eluent and modifier, pH of mobile phase etc. were studied systematically to arrive at optimum chromatographic conditions. This methodology provides satisfactorily separation for the lighter lanthanide elements. (author)

  2. Column: lef

    NARCIS (Netherlands)

    Reep, Frans van der

    2012-01-01

    1e alinea column: Ook in je beleggingsbeslissingen is het voor echte performance wellicht tijd om eens voorbij best practices (dan word je namelijk hoogstens tweede) te kijken naar next practices. Als je op zeker speelt, verdien je weinig geld. Want anderen gingen je al voor. Maar kun je nog meer op

  3. Chromatographic separation of cholesterol in foods.

    Science.gov (United States)

    Fenton, M

    1992-10-30

    Based on the current literature and on experience gained in the laboratory, a simplified procedure using direct saponification (0.4 M potassium hydroxide in ethanol and heating at 60 degrees C for 1 h) is the most appropriate method for the determination of total cholesterol in foods. Extraction of the unsaponifiable matter with hexane is efficient and no extra clean-up is required before quantification. An internal standard, 5 alpha-cholestane or epicoprostanol, should be added to the sample prior to saponification and, together with reference standards, carried through the entire procedure to ensure accurate results. A significant improvement in cholesterol methodology has been achieved by decreasing the sample size and performing all the sample preparation steps in a single tube. The method has the advantages of elimination of an initial solvent extraction for total lipids and errors resulting from multiple extractions, transfers, filtration and wash steps after saponification. The resulting hexane extract, which contains a variety of sterols and fat soluble vitamins, requires an efficient capillary column for complete resolution of cholesterol from the other compounds present. The development of fused-silica capillary columns using cross-linked and bonded liquid phases has provided high thermal stability, inertness and separation efficiency and, together with automated cold on-column gas chromatographic injection systems, has resulted in reproducible cholesterol determinations in either underivatized or derivatized form. If free cholesterol and its esters need to be determined separately, they are initially extracted with other lipids with chloroform-methanol followed by their separation by column or thin-layer chromatography and subsequently analysed by gas or liquid chromatography. Although capillary gas chromatography offers superior efficiency in separation, the inherent benefits of liquid chromatography makes it a potential alternative. Isotope dilution

  4. Chromatographic separation and concentration of quercetin and (+)-catechin using mesoporous composites based on MCM-41

    Science.gov (United States)

    Karpov, S. I.; Belanova, N. A.; Korabel'nikova, E. O.; Nedosekina, I. V.; Roessner, F.; Selemenev, V. F.

    2015-05-01

    Data on chromatographic separation of quercetin and (+)-catechin-flavonoids with similar physicochemical (including sorption) properties—are presented. The highest efficiency of chromatographic process at high sorption capacity of the material with respect to quercetin and slightly lower capacity for (+)-catechin were observed when silylated composites of ordered MCM-41 type materials were used. The application of acetonitrile as a solvent increased the sorption capacity of the material and can be recommended for separation of related polyphenol substances and their determination using ordered MCM-41 modified with trimethylchlorosilane as a stationary phase in a chromatographic column.

  5. Optimization of the gas chromatographic separations; Optimacion de las separaciones cromatograficas en fase gaseosa

    Energy Technology Data Exchange (ETDEWEB)

    Gasco Sanchez, L.

    1973-07-01

    A review and a critical study on the optimization of the gas chromatographic separations are made. After dealing with the fundamental gas chromatographic equations, some methods of expressing column performances are discussed: performance indices, performance parameters, resolution and effective plate number per unit time. This is completed with a comparative study on performances of various types of columns. Moreover, optimization methods for operating chromatographic conditions are extensively dealt with: as resolution optimization, separation time, and normalization techniques for the time of analysis in order to achieve the maximum resolution at constant time. Finally, some others non operating parameters such as: selectivity of stationary phases, column preparation and optimization methods by means of computers are studied. (Author) 68 refs.

  6. Shrinking-core modeling of binary chromatographic breakthrough.

    Science.gov (United States)

    Traylor, Steven J; Xu, Xuankuo; Lenhoff, Abraham M

    2011-04-22

    Most chromatographic processes involve separation of two or more species, so development of a simple, accurate multicomponent chromatographic model can be valuable for improving process efficiency and yield. We consider the case of breakthrough chromatography, which has been considered in great depth for single-component modeling but to a much more limited degree for multicomponent breakthrough. We use the shrinking core model, which provides a reasonable approximation of particle uptake for proteins under strong binding conditions. Analytical column solutions for single-component systems are extended here to predict binary breakthrough chromatographic behavior for conditions under which the external transport resistance is negligible. Analytical results for the location and profile of displacement effects and expected breakthrough curves are derived for limiting cases. More generally, straightforward numerical results have also been obtained through simultaneous solution of a set of simple ordinary differential equations. Exploration of the model parameter space yields results consistent with theoretical expectations. Additionally, both analytical and numerical predictions compare favorably with experimental column breakthrough data for lysozyme-cytochrome c mixtures on the strong cation exchanger SP Sepharose FF. Especially significant is the ability of the model to predict experimentally observed displacement profiles of the more weakly adsorbed species (in this case cytochrome c). The ability to model displacement behavior using simple analytical and numerical techniques is a significant improvement over current methods. PMID:21411102

  7. High-performance liquid chromatographic analysis of ampicillin.

    Science.gov (United States)

    Tsuji, K; Robertson, J H

    1975-09-01

    A high-pressure liquid chromatographic method for the analysis of ampicillin is described. The method uses a 1-m long stainless steel column packed with anionic exchange resin, with a mobile phase of 0.02 M NaNO3 in 0.01 M pH 9.15 borate buffer at a flow rate of 0.45 ml/min. The degradation products of ampicillin, penicillenic and penicilloic acids of ampicillin, can be separated and quantitated in less than 12 min of chromatographic time. The relative standard deviation for the analysis of ampicillin is less than 1%, and the method is sensitive to approximately 20 ng of ampicillin/sample injected. The method was applied to the analysis of various pharmaceutical preparations of ampicillin. It is also applicable, with a slight modification, for the analysis of penicillins G and V. PMID:1185575

  8. Ion Exchange and Thin Layer Chromatographic Separation and Identification of Amino Acids in a Mixture: An Experiment for General Chemistry and Biotechnology Laboratories

    Science.gov (United States)

    Brunauer, Linda S.; Caslavka, Katelyn E.; Van Groningen, Karinne

    2014-01-01

    A multiday laboratory exercise is described that is suitable for first-year undergraduate chemistry, biochemistry, or biotechnology students. Students gain experience in performing chromatographic separations of biomolecules, in both a column and thin layer chromatography (TLC) format. Students chromatographically separate amino acids (AA) in an…

  9. Identification of humic-like substances (HULIS) in oxygenated organic aerosols using NMR and AMS factor analyses and liquid chromatographic techniques

    NARCIS (Netherlands)

    Paglione, M.; Kiendler-Scharr, A.; Mensah, A.A.; Finessi, E.; Giulianelli, L.; Sandrini, S.; Facchini, M.C.; Fuzzi, S.; Schlag, P.; Piazzalunga, A.; Tagliavini, E.; Henzing, J.S.; Decesari, S.

    2014-01-01

    The atmospheric organic aerosol composition is characterized by a great diversity of functional groups and chemical species, challenging simple classification schemes. Traditional offline chemical methods identify chemical classes based on the retention behaviour on chromatographic columns and absor

  10. Identification of humic-like substances (HULIS) in oxygenated organic aerosols using NMR and AMS factor analyses and liquid chromatographic techniques

    NARCIS (Netherlands)

    Paglione, M.; Kiendler-Scharr, A.; Mensah, A. A.; Finessi, E.; Giulianelli, L.; Sandrini, S.; Facchini, M. C.; Fuzzi, S.; Schlag, P.; Piazzalunga, A.; Tagliavini, E.; Henzing, J. S.; Decesari, S.

    2013-01-01

    The atmospheric organic aerosol composition is characterized by a great diversity of functional groups and chemical species challenging simple classification schemes. Traditional off-line chemical methods identified chemical classes based on the retention behavior on chromatographic columns and abso

  11. LIQUID CHROMATOGRAPHIC SEPARATION OF THE ENANTIOMERS OF TRANS-CHLORDANE, CIS-CHLORDANE, HEPTACHLOR, HEPTACHLOR EPOXIDE AND ALPHA-HEXACHLOROCYCLOHEXANE WITH APPLICATION TO SMALL-SCALE PREPARATIVE SEPARATION

    Science.gov (United States)

    Analytical high-performance liquid chromatographic separations of the individual enantiomers of five polychlorinated compounds were obtained on polysaccharide stereoselective HPLC columns. The enantiomers of the pesticides trans-chlordane, cis-chlordane and heptachlor were separa...

  12. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    International Nuclear Information System (INIS)

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  13. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    Energy Technology Data Exchange (ETDEWEB)

    Ying Liu

    2004-12-19

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  14. A Simple Design to Realize Micro-column Separation by Conventional Analytical HPLC

    Institute of Scientific and Technical Information of China (English)

    GONG,Wenjun; ZHANG,Junxia; ZHANG,Yuping; ZHANG,Yijun; TIAN,Mengkui; WU,Dafu

    2009-01-01

    The conventional analytical HPLC was successfully developed for micro-column separation by using a simple eluate splitting system,self-preparation of packing column and on-capillary column detector in our laboratory.Porous inlet frit in fused silica capillary was rapidly prepared by sintering stainless steel powders under 500 meshes for about 20 s.The use of such frits or metal meshes in capillary to retain C18 particles of chromatographic packing was demonstrated to be stable and specially robust with continuous packing and long chromatographic runs.Furthermore,the chromatographic behavior was detailedly evaluated by changing the flow rate and the percentage of mobile phase using the prepared capillary column.Under the optimal experimental conditions,baseline separation of the model analytes including thiourea,benzene,toluene,ethylbenzene was obtained with a high column efficiency near 70000N (plates/m) by the developed capillary-HPLC.

  15. High-performance liquid chromatographic method for potency determination of amoxicillin in commercial preparations and for stability studies.

    OpenAIRE

    Hsu, M. C.; Hsu, P W

    1992-01-01

    A reversed-phase column liquid chromatographic method was developed for the assay of amoxicillin and its preparations. The linear calibration range was 0.2 to 2.0 mg/ml (r = 0.9998), and recoveries were generally greater than 99%. The high-performance liquid chromatographic assay results were compared with those obtained from a microbiological assay of bulk drug substance and capsule, injection, and granule formulations containing amoxicillin and degraded amoxicillin. At the 99% confidence le...

  16. Mathematical model for multicomponent separations on the continuous annular chromatograph

    International Nuclear Information System (INIS)

    A model for multicomponent separations on ion exchange columns has been adapted for use in studying the performance of the continuous annular chromatograph. The model accurately predicts solute peak positions in the column effluent and qualitatively predicts trends in solute effluent resolution as a function of increasing bandwidth of the solute feed pulse. The major virtues of the model are its simplicity in terms of the calculations involved and the fact that it incorporates the nonlinear solute-resin binding isotherms common in many ion exchange separations. Because dispersion effects are not accounted for in the model, discrepancies exist between the shapes of the effluent peaks predicted by the model and those determined experimentally

  17. Mathematical model for multicomponent separations on the continuous annular chromatograph

    Energy Technology Data Exchange (ETDEWEB)

    Bratzler, R.L.; Begovich, J.M.

    1980-12-01

    A model for multicomponent separations on ion exchange columns has been adapted for use in studying the performance of the continuous annular chromatograph. The model accurately predicts solute peak positions in the column effluent and qualitatively predicts trends in solute effluent resolution as a function of increasing bandwidth of the solute feed pulse. The major virtues of the model are its simplicity in terms of the calculations involved and the fact that it incorporates the nonlinear solute-resin binding isotherms common in many ion exchange separations. Because dispersion effects are not accounted for in the model, discrepancies exist between the shapes of the effluent peaks predicted by the model and those determined experimentally.

  18. Liquid chromatographic determination of carbadox residues in animal feed.

    Science.gov (United States)

    Roybal, J E; Munns, R K; Shimoda, W

    1985-01-01

    A liquid chromatographic (LC) method for determining residues of carbadox in the 0.01-10 ppm range in swine feed is described. Carbadox is extracted from ground feed with 25% acidified methanol-CHCl3, removed from emulsion-forming coextractables via an alumina column, separated from highly colored pigments by acid-base liquid-liquid partitioning, and finally isolated from interferences on a second alumina column. Isocratic reverse phase LC at 305 nm is used for quantitation. The average overall recovery at the 0.1, 0.5, and 1.0 ppm spike levels was 83.0% with a standard deviation of 2.04% and a coefficient of variation of 2.46%. PMID:4030635

  19. Chromatographic separation of germanium and arsenic for the production of high purity (77)As.

    Science.gov (United States)

    Gott, Matthew D; DeGraffenreid, Anthony J; Feng, Yutian; Phipps, Michael D; Wycoff, Donald E; Embree, Mary F; Cutler, Cathy S; Ketring, Alan R; Jurisson, Silvia S

    2016-04-01

    A simple column chromatographic method was developed to isolate (77)As (94±6% (EtOH/HCl); 74±11 (MeOH)) from germanium for potential use in radioimmunotherapy. The separation of arsenic from germanium was based on their relative affinities for different chromatographic materials in aqueous and organic environments. Using an organic or mixed mobile phase, germanium was selectively retained on a silica gel column as germanate, while arsenic was eluted from the column as arsenate. Subsequently, enriched (76)Ge (98±2) was recovered for reuse by elution with aqueous solution (neutral to basic). Greater than 98% radiolabeling yield of a (77)As-trithiol was observed from methanol separated [(77)As]arsenate [17]. PMID:26947162

  20. Chromatographic and spectroscopic characterization of a red pigment obtained from Bothryodiplodia theobromae

    International Nuclear Information System (INIS)

    A great variety of metabolites is obtained during the microbiological production of jasmonates from the fungus Bothryodiplodia theobromae. Many of them have not been characterized and can present interesting bioactive properties for their possible application. To achieve the identification, characterization and quantification of these metabolites constitutes a novel and complex analytic problem that is necessary to approach and that it can be solved using different chromatographic and spectroscopic methods. In this paper, the study of chromatographic and spectroscopic characterization of the resultant aqueous fraction obtained from the separation procedure by liquid-liquid extraction with solvents of different polarity of the broth of fermentation is shown. The aqueous fraction obtained was the most purified and was spectroscopically characterized by UV and to IR and chromatographically by TLC and HPLC. To define the chromatographic profile of this fraction, the chromatographic conditions were established by HPLC using an RP-18 column and this fraction was purified by column of Sephadex LH-20 and obtained a compound that suggests a structure similar to a flavonoid of the anthocyanin type

  1. Ion Chromatographic Analyses of Sea Waters, Brines and Related Samples

    Directory of Open Access Journals (Sweden)

    Nataša Gros

    2013-06-01

    Full Text Available This review focuses on the ion chromatographic methods for the analyses of natural waters with high ionic strength. At the beginning a natural diversity in ionic composition of waters is highlighted and terminology clarified. In continuation a brief overview of other review articles of potential interest is given. A review of ion chromatographic methods is organized in four sections. The first section comprises articles focused on the determination of ionic composition of water samples as completely as possible. The sections—Selected Anions, Selected Cations and Metals—follow. The most essential experimental conditions used in different methods are summarized in tables for a rapid comparison. Techniques encountered in the reviewed articles comprise: direct determinations of ions in untreated samples with ion- or ion-exclusion chromatography, or electrostatic ion chromatography; matrix elimination with column-switching; pre-concentration with a chelation ion chromatography and purge-and-trap pre-concentration. Different detection methods were used: non-suppressed conductometric or suppressed conductometric, direct spectrometric or spectrometric after a post-column derivetization, and inductively coupled plasma in combination with optical emission or mass spectrometry.

  2. Vibrational Spectroscopy of Chromatographic Interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Jeanne E. Pemberton

    2011-03-10

    Chromatographic separations play a central role in DOE-supported fundamental research related to energy, biological systems, the environment, and nuclear science. The overall portfolio of research activities in the Separations and Analysis Program within the DOE Office of Basic Energy Sciences includes support for activities designed to develop a molecular-level understanding of the chemical processes that underlie separations for both large-scale and analytical-scale purposes. The research effort funded by this grant award was a continuation of DOE-supported research to develop vibrational spectroscopic methods to characterize the interfacial details of separations processes at a molecular level.

  3. Allyl-silica Hybrid Monoliths For Chromatographic Application

    Science.gov (United States)

    Guo, Wenjuan

    Column technology continues to be the most investigated topics in the separation world, since the column is the place where the chromatographic separation happens, making it the heart of the separation system. Allyl-silica hybrid monolithic material has been exploited as support material and potential stationary phases for liquid chromatography; the stationary phase anchored to the silica surface by Si-C bond, which is more pH stable than traditional stationary phase. First, nuclear magnetic resonance spectroscopy has been used to study the sol in the synthesis of allyl-silica hybrid monoliths. Allyl-trimethoxysilane (allyl-TrMOS), dimethyldimethoxysilane (DMDMOS) and tetramethoxysilane (TMOS) have been served as co-precursors in the sol-gel synthesis of organo-silica hybrid monolithic columns for liquid chromatography (LC). 29Si nuclear magnetic resonance (NMR) and 1H NMR spectroscopy were employed to monitor reaction profiles for the acid-catalyzed hydrolysis and initial condensation reactions of the individual precursor and the hybrid system. 29Si-NMR has also been used to identify different silane species formed during the reactions. The overall hydrolysis rate has been found to follow the trend DMDMOS > allyl-TrMOS > TMOS, if each precursor is reacted individually (homo-polymerization). Precursors show different hydrolysis rate when reacted together in the hybrid system than they are reacted individually. Cross-condensation products of TMOS and DMDMOS (QD) arise about 10 minutes of initiation of the reaction. The allyl-silica monolithic columns for capillary liquid chromatography can only be prepared in capillaries with 50 im internal diameter with acceptable performance. One of the most prominent problems related to the synthesis of silica monolithic structures is the volume shrinkage. The synthesis of allylfunctionalized silica hybrid monolithic structures has been studied in an attempt to reduce the volume shrinkage during aging, drying and heat treatment

  4. Procedure for the production of PZC based chromatographic Tc-99m generator to be available for clinical application

    International Nuclear Information System (INIS)

    The chemical synthesis for the preparation of polymer compound of Zirconium (PZC) and the column pre-loading procedure for the preparation of PZC based chromatographic Tc-99m generators were described in detail. In-process documentation, flow-chart of process, specific Tc-99m generator designs and picturially illustrative description of Tc-99 generator production process were systematically reported. The column pre-loading procedure was highly evaluated as a competent technology for the preparation of PZC based Tc-99m chromatographic generator of high performance using (n,γ)99 Mo of low specific radioactivity produced on low power research reactors. (author)

  5. Liquid Chromatographic Determination of Alogliptin in Bulk and in its Pharmaceutical Preparation

    OpenAIRE

    El-Bagary, Ramzia I.; Elkady, Ehab F.; Ayoub, Bassam M.

    2012-01-01

    In this work, a reversed-phase liquid chromatographic (RP-LC) method has been developed for the determination of alogliptin (ALG) based on isocratic elution using a mobile phase consisting of potassium dihydrogen phosphate buffer pH (4.6)-acetonitrile (20:80, v/v) at a flow rate of 1 mL min−1 with UV detection at 215 nm. Chromatographic separation was achieved on a Symmetry® cyanide column (150 mm × 4.6 mm, 5 μm). Linearity, accuracy and precision were found to be acceptable over the concentr...

  6. REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR THE ANALYSIS OF GLIPIZIDE IN PHARMACEUTICAL DOSAGE FORMS

    OpenAIRE

    Sheikh Rahila; Karigar Asif

    2010-01-01

    A rapid and sensitive reverse phase high performance liquid chromatographic methods depicted for the qualitative and quantitative assay of glipizide in pharmaceutical dosage forms. Glipizide was chromatographed on reverse phase C18 column with mobile phase consisting of 0.05 M Potassium Dihydrogen Orthophosphate: Methanol [15: 85 %v/v, pH 7.0 ± 0.05, adjusted with 1% Triethylamine]. The mobile phase was pumped at a flow rate 1 mL/min. Quantification was achieved by monitoring the ultraviolet ...

  7. Reversed-phase liquid chromatography testing. Role of organic solvent through an extended set of columns.

    Science.gov (United States)

    Le Mapihan, K; Vial, J; Jardy, A

    2005-09-23

    Column testing is a primary concerns for analysts. It is of use not only for the choice of set of development columns with different behaviors, but also for a substitution column in a validated method or as a quality control of new batches of stationary phase. A validated chromatographic procedure for column testing was applied to 42 commercially available columns, including alkyl, polar embedded and Aqua type stationary phases. This procedure was based on the use of two different solvents: MeOH and MeCN; and two different solvent/aqueous buffer fractions. Principal component analysis has been combined to hierarchical cluster analysis to provide both rational and objective classifications. The solvent effects were then studied on the obtained representations, revealing the necessity for considering both the solvent nature and its fraction in RPLC column testing. Differences observed depending on the solvent nature and fractions revealed quite different chromatographic behaviors according to these parameters. PMID:16130728

  8. [Development of online conventional array-based two-dimensional liquid chromatographic system for proteins separation in human plasma].

    Science.gov (United States)

    Huang, Zhi; Hong, Guangfeng; Gao, Mingxia; Zhang, Xiangmin

    2014-04-01

    Human plasma is one of the proteins-containing samples most difficult to characterize on account of the wide dynamic concentration range of its intact proteins. Herein, we developed a high-throughput conventional array-based two-dimensional liquid chromatographic system for proteins separation in human plasma in online mode. In the system, a conventional strong-anion exchange chromatographic column was used as the first separation dimension and eight parallel conventional reversed-phase liquid chromatographic columns were integrated as the second separation dimension. The fractions from the first dimension were sequentially transferred into the corresponding reversed-phase liquid chromatographic precolumns for retention and enrichment using a 10-port electrically actuated multi-position valve. The second dimensional solvent flow was directly and identically split into 8 channels. The fractions were concurrently back-flushed from the precolumns into the 8 conventional RP columns and were separated simultaneously. An 8-channel fraction collector was refitted to collect the reversed-phase liquid chromatographic fractions for further investigation. Bicinchoninic acid (BCA) dyein solution was conveniently used for high-abundance protein location. Two separation dimensions were relatively independent parts, as well as each channel of the second dimensional array separation. Therefore, the new system could improve the separation throughput and total peak capacity. The system was successfully applied for the separation of human plasma intact proteins. The results indicated the established system is an effective method for removing high abundance proteins in plasma and in-depth research in plasma proteomics. PMID:25069321

  9. Monolithic molecularly imprinted polymeric capillary columns for isolation of aflatoxins.

    Science.gov (United States)

    Szumski, Michał; Grzywiński, Damian; Prus, Wojciech; Buszewski, Bogusław

    2014-10-17

    Monolithic molecularly imprinted polymers extraction columns have been prepared in fused-silica capillaries by UV or thermal polymerization in a two-step process. First, a poly-(trimethylolpropane trimethacrylate) (polyTRIM) core monolith was synthesized either by UV or thermal polymerization. Then it was grafted with the mixture of methacrylic acid (MAA) as a functional monomer, ethylene dimethacrylate (EDMA) as a cross-linking agent, 5,7-dimethoxycoumarin (DMC) as an aflatoxin-mimicking template, toluene as a porogen solvent and 2,2-azobis-(2-methylpropionitrile) (AIBN) as an initiator of the polymerization reaction. Different thermal condition of the photografting and different concentrations of the grafting mixture were tested during polymerization. The extraction capillary columns were evaluated in the terms of their hydrodynamic and chromatographic properties. Retention coefficients for aflatoxin B1 and DMC were used for assessment of the selectivity and imprinting factor. The obtained results indicate that the temperature of photografting and concentration of the grafting mixture are key parameters that determine the quality of the prepared MIPs. From the MIP columns characterized by the highest permeability the column of the highest imprinting factor was applied for isolation of aflatoxins B1, B2, G1 and G2 from the model aqueous sample followed by on-line chromatographic separation. The process was performed using a micro-MISPE-microLC-LIF system of a novel design, which allowed for detection of the eluates from the sample preparation part as well as from the chromatographic separation. PMID:25218633

  10. High-pressure liquid chromatographic method for the determination of patulin in apple butter.

    Science.gov (United States)

    Ware, G M

    1975-07-01

    Patulin is extracted from apple butter samples with ethyl acetate and the extract is cleaned up on a silica gel column, using benzene-ethyl acetate (75+25) as the eluant. High-pressure liquid chromatography, using a 25 cm ZorbaxSil column, isooctane-ethyl ether-acetic acid (750+250+0.5) as the mobile solvent, and a 254 nm ultraviolet detector, is used for the determinative step. Under these conditions, patulin is eluted before 5-hydroxymethylfurfural, a component of apple butter which interferes with other liquid chromatographic and thin layer chromatographic methods. Recoveries of patulin added at levels of 34.6, 138.4, and 276.8 mug/kg ranged from 89.0 to 112.1%. PMID:168176

  11. Optimization of Chromatographic Conditions for Detecting Ellagic Acid in Pomegranate Peels Using HPLC Method

    Institute of Scientific and Technical Information of China (English)

    2012-01-01

    [Objective] This study aimed to optimize the chromatographic conditions for detecting ellagic acid in pomegranate peels using HPLC method. [Method] By using 0.2 mg/ml ellagic acid standard solution, on the basis of single-factor experiment and orthogonal experiment, chromatographic conditions (mobile phase ratio, flow rate, col- umn temperature) for detecting ellagic acid using HPLC were optimized. Based on the optimal chromatographic conditions, the ellagic acid content in experimental pomegranate peels was determined. [Resull] The optimal chromatographic conditions for detecting ellagic acid in pomegranate peels using HPLC method are: 1.2% phos- phoric acid:acetonitrile=85:15, column temperature of 35 ℃, and flow rate of 1.0 ml/min. The linear regression equation of ellagic acid is: y=2.9e+0.6x+4.4e+5 (FF=9 999). Ac- cording to the standard addition recovery test, the average recovery rate of ellagic acid is 98.20%, and RSD is 0.60%. Under above optimized chromatographic condi- tions, ellagic acid can be well separated from other interfering components in pomegranate peels, with shorter peak time and ideal effect, which is convenient for the detection in production practices. [Conclusion] This study laid the foundation for detecting ellagic acid in pomegranate peels using HPLC method.

  12. Planar chromatographic method development using the PRISMA optimization system and flow charts.

    Science.gov (United States)

    Nyiredy, Sz

    2002-01-01

    This study presents a modern planar chromatographic method-development procedure, based on the "PRISMA" optimization system, in which the optimum separation is achieved systematically and the structures and properties of the substances to be separated are not known. The procedure consists of three stages. In the first of these the basic conditions the stationary phase, vapor phase, and individual solvents are selected with a TLC procedure (generally in nonsaturated chromatographic chambers). In the second stage, the optimum combination of the selected solvents is determined with the PRISMA model. The third part of the procedure includes the selection of the development mode (circular, linear, or anticircular); the selection of an appropriate forced-flow chromatographic technique (over-pressured layer chromatography or rotation planar chromatography) with high-performance thin-layer chromatographic plates; the transfer of the optimized mobile phase to the various analytical, planar, or column preparative liquid chromatographic techniques; and the selection of the operating conditions. For practical reasons, the optimization process is presented with the help of flow charts. PMID:12515358

  13. A Novel Chromatographic Method Allows On-line Reanalysis of the Proteome* S⃞

    OpenAIRE

    Waanders, Leonie F.; Almeida, Reinaldo de; Prosser, Simon; Cox, Jürgen; Eikel, Daniel; Allen, Mark H.; Schultz, Gary A.; Mann, Matthias

    2008-01-01

    Liquid chromatography combined with electrospray ionization is widely used for direct analysis of polar and labile molecules by LCMS. The on-line coupling in LCMS is a major strength but also causes a principal limitation that each eluting analyte has to be analyzed immediately and is not available for detailed interrogation after the LCMS run. Here we developed a new chromatographic strategy, which removes this limitation. After column separation the flow is split, one portion is analyzed di...

  14. A Novel and Effective Chromatographic Approach to the Separation of Isoflavone Derivatives from Pueraria lobata

    OpenAIRE

    Jiang Fu; Wenguang Jing; Weihao Wang; Sha Chen; Jun Zhang; An Liu

    2015-01-01

    A novel and effective chromatographic approach to the separation and purification of isoflavone compounds from Pueraria lobata is described. The method is based on flash chromatography (FC), coupled to preparative high performance liquid chromatography (prep-HPLC) via a six-way valve. The FC step comprised tandem reversed phase columns, pre-packed with MCI gel (Mitsubishi Chemical Corp., Tokyo, Japan) and C18 (Fuji Silysia Chemical Ltd, Osaka, Japan) resin, respectively, and was designed to s...

  15. All Silicon Micro-GC Column Temperature Programming Using Axial Heating

    Directory of Open Access Journals (Sweden)

    Milad Navaei

    2015-07-01

    Full Text Available In this work we present a high performance micro gas chromatograph column with a novel two dimensional axial heating technique for faster and more precise temperature programming, resulting in an improved separation performance. Three different axial resistive heater designs were simulated theoretically on a 3.0 m × 300 μm × 50 μm column for the highest temperature gradient on a 22 by 22 μm column. The best design was then micro-fabricated and evaluated experimentally. The simulation results showed that simultaneous temperature gradients in time and distance along the column are possible by geometric optimization of the heater when using forced convection. The gradients along the column continuously refocused eluting bands, offsetting part of the chromatographic band spreading. The utility of this method was further investigated for a test mixture of three hydrocarbons (hexane, octane, and decane.

  16. Reversed-phase high-performance liquid chromatographic method for the assay of oxytetracycline.

    Science.gov (United States)

    Barnes, W N; Ray, A; Bates, L J

    1985-10-25

    The British Pharmacopoeia monograph for oxytetracycline calcium describes an high-performance liquid chromatographic (HPLC) assay which requires packing of the column by the analyst. Presented in this report is an HPLC method for the assay of oxytetracycline which employs a commercially available reversed-phase column and a solvent system which gives improved separation of the antibiotic from common impurities. Results obtained using this method for both bulk and dosage forms of oxytetracycline are in accord with the results of the microbiological assays. PMID:4086631

  17. Chromatographic methods of the measurements of the chloride compounds in troposphere and stratosphere

    International Nuclear Information System (INIS)

    The paper contains a description of various chromatographic techniques used for the analysis of the tropospheric techniques used for the analysis of the tropospheric and stratospheric halogenated compounds. The types of the column packings used for separation of halogenated compounds are described. Model chromatograms illustrating the separation of halogenated compounds are presented. The methods of the air sampling and injection for the packed and capillary columns were described. The methods of the preparation of gas calibration mixtures are presented. Operational conditions for electron capture detector used by the authors of quoted paper are also given. (author). 66 refs, 29 figs, 13 tabs

  18. Stationary phase modulation in liquid chromatography through the serial coupling of columns: A review.

    Science.gov (United States)

    Alvarez-Segura, T; Torres-Lapasió, J R; Ortiz-Bolsico, C; García-Alvarez-Coque, M C

    2016-06-01

    Liquid chromatography with single columns often does not succeed in the analysis of complex samples, in terms of resolution and analysis time. A relatively simple solution to enhance chromatographic resolution is the modulation of the stationary phase through the serial coupling of columns. This can be implemented with any type of column using compatible elution conditions and conventional instruments. This review describes the key features of column coupling and published procedures, where two or more columns were coupled in series to solve separation problems. In all reports, the authors could not resolve their samples with single columns, whereas significant enhancement in chromatographic performance was obtained when the columns were combined. Particularly interesting is the reduction in the analysis time in the isocratic mode, which alleviates the "general elution problem" of liquid chromatography, and may represent a stimulus for the proposal of new procedures, especially in combination with mass spectrometric, electrochemical and refractometric detection. Developments proposed to make the serial coupling of columns useful in routine and research laboratories are outlined, including optimisation strategies that facilitate the selection of the appropriate column combination and elution conditions (solvent content, flow rate or temperature) in both isocratic and gradient modes. The availability of zero dead volume couplers, able to connect standard columns, and the commercialisation of short columns with multiple lengths, have expanded the possibilities of success. PMID:27155298

  19. Predictability of enantiomeric chromatographic behavior on various chiral stationary phases using typical reversed phase modeling software.

    Science.gov (United States)

    Wagdy, Hebatallah A; Hanafi, Rasha S; El-Nashar, Rasha M; Aboul-Enein, Hassan Y

    2013-09-01

    Pharmaceutical companies worldwide tend to apply chiral chromatographic separation techniques in their mass production strategy rather than asymmetric synthesis. The present work aims to investigate the predictability of chromatographic behavior of enantiomers using DryLab HPLC method development software, which is typically used to predict the effect of changing various chromatographic parameters on resolution in the reversed phase mode. Three different types of chiral stationary phases were tested for predictability: macrocyclic antibiotics-based columns (Chirobiotic V and T), polysaccharide-based chiral column (Chiralpak AD-RH), and protein-based chiral column (Ultron ES-OVM). Preliminary basic runs were implemented, then exported to DryLab after peak tracking was accomplished. Prediction of the effect of % organic mobile phase on separation was possible for separations on Chirobiotic V for several probes: racemic propranolol with 97.80% accuracy; mixture of racemates of propranolol and terbutaline sulphate, as well as, racemates of propranolol and salbutamol sulphate with average 90.46% accuracy for the effect of percent organic mobile phase and average 98.39% for the effect of pH; and racemic warfarin with 93.45% accuracy for the effect of percent organic mobile phase and average 99.64% for the effect of pH. It can be concluded that Chirobiotic V reversed phase retention mechanism follows the solvophobic theory. PMID:23775938

  20. Standard Format for Chromatographic-polarimetric System small samples assessment

    International Nuclear Information System (INIS)

    The treatment of samples containing optically active substances to be evaluated as part of quality control of raw material entering industrial process, and also during the modifications exerted on it to obtain the desired final composition is still and unsolved problem for many industries. That is the case of sugarcane industry. Sometimes the troubles implied are enlarged because samples to be evaluated are not bigger than one milliliter. Reduction of gel beds in G-10 and G-50 chromatographic columns having an inner diameter of 16 mm, instead of 25, and bed heights adjustable to requirements by means of sliding stoppers to increase analytical power were evaluated with glucose and sucrose standards in concentrations from 1 to 10 g/dL, using aliquots of 1 ml without undesirable dilutions that could affect either detection or chromatographic profile. Assays with seaweed extracts gave good results that are shown. It is established the advantage to know concentration of a separated substance by the height of its peak and the savings in time and reagents resulting . Sample expanded uncertainty in both systems is compared. It is also presented several programs for data acquisition, storing and processing. (Author)

  1. Gas Chromatographic Retention Indices of 2-chlorobenzylidenemalononitrile and its Analogues

    Directory of Open Access Journals (Sweden)

    P. K. Gutch

    2012-09-01

    Full Text Available Normal 0 false false false EN-GB X-NONE X-NONE Riot control agent, 2-chlorobenzylidenemalononitrile (CS and its analogues have both skin irritating and lacrymating properties. Herein, we report retention indices (RI of CS and its thirteen analogues relative to the homologues n-alkanes series. These values are determined on nonpolar BP-1 and polar BP-10 capillary column under programmed temperature and isothermal chromatographic condition. The analogues differ in substitution at ortho or para position of phenyl ring and retention indices are found to vary according to the nature of the substituent.Defence Science Journal, 2012, 62(5, pp.319-323, DOI:http://dx.doi.org/10.14429/dsj.62.1167

  2. Development and Validation of a Stability-Indicating High Performance Liquid Chromatographic (HPLC) Method for the Determination of Related Substances of Micafungin Sodium in Drug Substances

    OpenAIRE

    Zuyue Sun; Yongwei Luo; Xin Su; Xiang Meng; Shengsheng Zhu

    2013-01-01

    An isocratic, sensitive and stability-indicating high performance liquid chromatographic (HPLC) method for separation and determination of the related substances of micafungin sodium was developed. The chromatographic separation was achieved on Agilent Zorbax SB-C18 column (250 × 4.6 mm, 5 μm). Forced degradation study confirmed that the newly developed method was specific and selective to the degradation products. The performance of the method was validated according to the present ICH guide...

  3. Hydrodynamic impact of particle shape in slurry packed liquid chromatography columns

    DEFF Research Database (Denmark)

    Lottes, F.; Arlt, W.; Minceva, M.;

    2009-01-01

    We report on a series of flow velocity and efficiency profiles, which were measured across the cross section of preparative chromatographic columns packed with different stationary phase materials using computed tomography. It is shown that this non-invasive technique is very useful for visualiza......We report on a series of flow velocity and efficiency profiles, which were measured across the cross section of preparative chromatographic columns packed with different stationary phase materials using computed tomography. It is shown that this non-invasive technique is very useful for...

  4. A performance comparison of commercially available strontium extraction chromatography columns

    International Nuclear Information System (INIS)

    Extraction chromatographic separations following a nuclear event will require both speed and accuracy. Ideally these separations will be carried out using commercially available products. Because 90Sr is a likely material to be used in a radioactivity dispersal device, commercially available products for the separation of strontium were tested to evaluate differences in their elution profiles that may affect elution procedures. Gravity flow columns show better resolution, but vacuum flow columns allow rapid processing and are still adequate for purification if multiple aqueous conditions can be employed in the elution strategy. (author)

  5. Chromatographic resolution of angiotensin II receptor antagonists (sartans).

    Science.gov (United States)

    Tahir, Muhammad Saqlain; Adnan, Ahmad; Syed, Quratulain

    2016-08-01

    First time a simple, sensitive and unified quantification method has been developed to analyze the complete class of angiotensin II receptor antagonists which are used in the treatment of hypertension either alone or in combination with some other drugs. The most important advantage of developed method was that the eight separate drugs can be determined on a single chromatographic system without modifications in detection wavelength and mobile phase. The drugs were separated on a Purospher Star 4.6mm×25cm, 5μm, C18 column maintained at 40°C with 1mLmin(-1) flow rate using ultra violet detection at 254nm. Good separation (Rs>2.0) was achieved in a short analysis allowing simultaneous determination of all eight sartans. The effect of variation in flow rate, detection wavelength and column oven temperature was also studied. The proposed method was statistically validated in terms of precision, accuracy, linearity, specificity and robustness. The newly developed method proved to be specific, robust and accurate for the quantification of eight sartans in commercial pharmaceutical formulations. PMID:27258943

  6. Gas chromatographic validated method for quantification of ayurvedic polyherbal formulation

    Directory of Open Access Journals (Sweden)

    Navdeep Saini

    2015-01-01

    Full Text Available A new gas chromatographic-flame ionization detector (GC-FID method was developed for quantification of ayurvedic polyherbal formulation. The GC-FID method was found highly accurate, sensitive, simple and precise. This method was validated as per international conference on harmonization (ICH guidelines. Experimental work was performed by nonpolar capillary column (Zb-5, 5%-Phenyl-95%-dimethylpolysiloxane. Film thickness of capillary column (Zb-5 was (0.25 μm and length 30 m × 0.25 mm i.d. The temperature of the oven, injector and detector were 200, 210 and 280°C respectively. Data processing system was applied to obtain data. The standards and test samples were prepared in absolute ethanol. The principle constituents t-Anethol, d-Limonene, cuminaldehyde and thymol were found in ayurvedic polyherbal formulation. The ICH validation parameters for the proposed procedure, recovery (limit 98.85-100.76%, precision (<1.00%, limits of detection, limits of quantification and linearity (r2 = 0.995 ± 0.002 were observed under acceptance limit. Validation results were statistically calculated. The result shows that method is selective and reproducible for quantification of ayurvedic polyherbal formulation. The presented GC method can be applied for the routine analysis of principle constituents as well as ayurvedic polyherbal formulation.

  7. High-Performance Liquid Chromatographic-Tandem Mass Spectrometric Determination of Itraconazole in Human Plasma for Bioavailability and Bioequivalence Studies

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Young Wook; Nam, Dae Young; Kang, Kyoung Hoon; Ha, Kyung Wook; Han, In Hee; Chang, Byung Kon; Yoon, Mi Kyeong; Lee, Jae Hwi [Chung-Ang University, Seoul (Korea, Republic of)

    2006-02-15

    A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC C{sub 18} column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole.

  8. High-Performance Liquid Chromatographic-Tandem Mass Spectrometric Determination of Itraconazole in Human Plasma for Bioavailability and Bioequivalence Studies

    International Nuclear Information System (INIS)

    A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC C18 column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole

  9. Slender CRC Columns

    DEFF Research Database (Denmark)

    Aarup, Bendt; Jensen, Lars Rom; Ellegaard, Peter

    2005-01-01

    CRC is a high-performance steel fibre reinforced concrete with a typical compressive strength of 150 MPa. Design methods for a number of structural elements have been developed since CRC was invented in 1986, but the current project set out to further investigate the range of columns for which...... current design guides can be used. The columns tested had a slenderness varying from 1.11 to 12.76 and a reinforcement ratio (area of rebar to area of concrete) ranging from 0 to 8.8 %. A total of 77 tests were carried out - 61 columns were tested in ambient conditions and 16 columns were tested in...... standard fire conditions. The tests showed good correlation between test results and results calculated according to established deisgn guides. The fire tests demonstrate that the load capacity of slender columns can be reduced very quickly due to thermal stresses and a reduction of stiffness - also in...

  10. Chromatographic analysis of wheatgrass extracts

    Directory of Open Access Journals (Sweden)

    Masood Shah Khan

    2015-01-01

    Full Text Available Aim: Wheatgrass (WG is the shoot of Triticum aestivum Linn. belongs to the family Gramineae, and possess high chlorophyll content and essential vitamins, minerals, vital enzymes, amino acids, dietary fibers etc., It has been shown to possess anti-cancer, anti-ulcer, antioxidant, and anti-arthritic activity due to the presence of biologically active compounds, and minerals. Therefore, in the present study, high-performance thin layer chromatography (HPTLC, and high-performance liquid chromatography (HPLC methods for qualitative and quantitative analysis have been proposed, which will help in quality evaluation of wheat grass extract. Materials and Methods: Samples for analysis were prepared in methanol and water simply by sonication. These were applied on pre-coated silica plate and chromatograms were developed using toluene: Ethyl acetate: Formic acid. HPLC analysis was done on Waters HPLC system using water, methanol, and acetonitrile as mobile phase. Merck C18 column has been used. Results: HPTLC finger printing of alcoholic extracts of WG was carried out and found 10–11 spots at different wavelengths 254, 366, and 435 nm. HPLC fingerprinting produced 22 peaks at 256 nm. Quantitative HPTLC analysis was done to determine the gallic acid content, and was found to be 0.077% w/w in aqueous extract. By HPLC, the content of gallic acid and rutin was found to be 0.07%, and 0.04% w/w in aqueous extract of WG. Conclusion: The developed HPLC and HPTLC fingerprinting method can be used for the quality control, and standardization of WG and its extracts used as nutritional supplement.

  11. Analysis of chromatograph systems using orthogonal collocation

    Science.gov (United States)

    Woodrow, P. T.

    1974-01-01

    Research is generating fundamental engineering design techniques and concepts for the chromatographic separator of a chemical analysis system for an unmanned, Martian roving vehicle. A chromatograph model is developed which incorporates previously neglected transport mechanisms. The numerical technique of orthogonal collocation is studied. To establish the utility of the method, three models of increasing complexity are considered, the latter two being limiting cases of the derived model: (1) a simple, diffusion-convection model; (2) a rate of adsorption limited, inter-intraparticle model; and (3) an inter-intraparticle model with negligible mass transfer resistance.

  12. Synthesis of porous polyaromatic column packings for GC analysis of extraterrestrial atmospheres

    Science.gov (United States)

    Woeller, F. H.; Pollock, G. E.

    1978-01-01

    The preparation of a polymer for the Pioneer-Venus Large Probe Gas Chromatograph and another polymer for gas-chromatographic analysis of the Jovian atmosphere is described. Technical-grade divinylbenzene is used as a reliable and economical source of monomer for the preparation of polymer beads. The discussion covers monomeric preparation, polymerization apparatus, first-stage polymer beads, second-stage polymer beads, amino-polymer, columns and gas-chromatographic testing instrumentation used. The polymer for the Pioneer-Venus gas chromatograph is also suitable for ammonia but not for amine analysis. However, the polymer for the analysis of the Jovian atmosphere is a chemically derivatized aromatic polymer that is suitable for amine analysis. The two-stage polymerization produces a highly efficient polymer packing clearly superior to others prepared by adjusted dilution of the aqueous-organic suspension system.

  13. Distillation Column Flooding Predictor

    Energy Technology Data Exchange (ETDEWEB)

    George E. Dzyacky

    2010-11-23

    The Flooding Predictor™ is a patented advanced control technology proven in research at the Separations Research Program, University of Texas at Austin, to increase distillation column throughput by over 6%, while also increasing energy efficiency by 10%. The research was conducted under a U. S. Department of Energy Cooperative Agreement awarded to George Dzyacky of 2ndpoint, LLC. The Flooding Predictor™ works by detecting the incipient flood point and controlling the column closer to its actual hydraulic limit than historical practices have allowed. Further, the technology uses existing column instrumentation, meaning no additional refining infrastructure is required. Refiners often push distillation columns to maximize throughput, improve separation, or simply to achieve day-to-day optimization. Attempting to achieve such operating objectives is a tricky undertaking that can result in flooding. Operators and advanced control strategies alike rely on the conventional use of delta-pressure instrumentation to approximate the column’s approach to flood. But column delta-pressure is more an inference of the column’s approach to flood than it is an actual measurement of it. As a consequence, delta pressure limits are established conservatively in order to operate in a regime where the column is never expected to flood. As a result, there is much “left on the table” when operating in such a regime, i.e. the capacity difference between controlling the column to an upper delta-pressure limit and controlling it to the actual hydraulic limit. The Flooding Predictor™, an innovative pattern recognition technology, controls columns at their actual hydraulic limit, which research shows leads to a throughput increase of over 6%. Controlling closer to the hydraulic limit also permits operation in a sweet spot of increased energy-efficiency. In this region of increased column loading, the Flooding Predictor is able to exploit the benefits of higher liquid

  14. 40 CFR 799.6786 - TSCA water solubility: Generator column method.

    Science.gov (United States)

    2010-07-01

    ... and allowing the water to reach the HPLC detector, as indicated by a negative reading. As soon as this..., and the aqueous solubility of organic liquids. Journal of Organic Chemistry 33:347-350 (1968). (3... a coupled column liquid chromatographic technique. Analytical Chemistry 50:175-179 (1978). (6)...

  15. Study PWA8 resin for chromatographic uranium concentration

    International Nuclear Information System (INIS)

    For many years nuclear industry have been using resins as filler of chromatographic columns. These methods are specific and give reliable results in different applications, for those reasons are extremely useful as separation process. Currently the nuclear industry is growing and this brings new issues such as the need of reduction of the amount of waste, the optimization of the production process and others that the chromatography could solve with great results. AMBERLITETM PWA8 resin is an anion exchange resin which can be used for the removal of uranium from drinking water. In addition to high exchange capacity, this resin has excellent physical stability and a wide range of pH in which is operational. With the idea of concentrating uranium from wastes solution as main goal we made different experiments to understand the AMBERLITETM PWA8 and obtain the most important characteristics like; pH working range; capacity; activation and elution procedures. These procedures were developed and optimized the capacity was determined using a batch experiment and we obtain that the maximum capacity is 882,5 U ug /resin gr at a pH of 4,2. Following on from these results chromatographic experiments were performed in which both were obtained the percentage of recovery and the concentration factor. The percent recovery (% R) calculated as the percentage ratio between the total mass and the load mass eluted (% R = eluted mass / total mass * 100) was 94% with a concentration factor of 5 times From these results it is intended to concentrate wastes solutions from the fuel cycle processes with two main goals: decreasing volume for storage and for future reusing of the uranium coming from production. (author)

  16. Green Chromatographic Separation of Coumarin and Vanillins Using Subcritical Water as the Mobile Phase.

    Science.gov (United States)

    Kayan, Berkant; Akay, Sema; Yang, Yu

    2016-08-01

    Pure water was used as the eluent for separation of coumarin, vanillin and ethyl vanillin at temperatures ranging from 100 to 200°C using a homemade subcritical water chromatography (SBWC) system. Chromatographic separations were performed on five commercial columns including XTerra MS C18, XBridge C18, Zorbax RRHD Eclipse Plus, Zorbax SB-Phenyl and Zorbax SB-C18 columns. The retention time of all three solutes decreased with increasing water temperature. The shortest retention time among all acceptable separations, less than 4 min, was achieved on the Zorbax SB-C18 column at 200°C. While separations on the XTerra MS C18 column resulted in fronting peaks and a degradation peak from ethyl vanillin on the Zorbax RRHD Eclipse Plus column was observed, all three other columns yielded reasonable separations under SBWC conditions. In addition to separation of the standard test mixture, separation of coumarin contained in a skincare cream sample was also carried out using SBWC. PMID:27060112

  17. Comparison among three anion exchange chromatographic supports to capture erythropoietin from cell culture supernatant

    Institute of Scientific and Technical Information of China (English)

    Lourdes HERNNDEZ; Diobel STEWART; Lourdes ZUMALACRREGUI; Daniel AMARO

    2015-01-01

    Affinity and ion exchange conventional chromatography have been used to capture erythropoietin ( EPO)from mammalian cell culture supernatant. Currently,chromatographic adsorbent perfusion is available, however a limited number of applications have been found in the literature. In this work,three anion exchange chromatographic supports( gel,membrane and monolithic)were evaluated in the capture step of the recombi-nant erythropoietin purification process. The influences of load and flow rate on each support performance were analyzed. Also the purity of the EPO molecules was determined. A productivity analysis,as a decision tool for larger scale implementation,was done. As a conclusion,the evaluated supports are technically suitable to cap-ture EPO with adequate recovery and good purity. However,the monolithic column admits high operating velocity,showing the highest adsorption capacity and productivity.

  18. Investigation on the performance of polymer zirconium compound (PZC) for chromatographic Tc-99m generator preparation

    International Nuclear Information System (INIS)

    The performance of PZC was investigated for chromatographic Tc-99m generator preparation. Mo-adsorption of PZC in different Mo-solutions and Tc-99m elution of 99Mo-PZC column were studied. Mo- adsorption capacity of higher than 250mgMo/gPZC and Tc-99m elution yield of higher than 80% were achieved with PZC adsorbent. Mo-99 breakthrough of 0.02% and Molybdenum element breakthrough of around 5μg Mo/ml were found in Tc-99m eluate. A good relationship between the Mo-content of adsorption solution and the Mo-adsorption capacity, adsorption percentage, Mo-breakthrough and Tc-99m elution yield was found. The preparation of PZC based Tc-99m chromatographic generator with 4 gram weight of PZC was successfully conducted. (author)

  19. 40 CFR 1065.267 - Gas chromatograph.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 32 2010-07-01 2010-07-01 false Gas chromatograph. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon Measurements § 1065.267 Gas...

  20. Chromatographic techniques for petroleum and related products

    Energy Technology Data Exchange (ETDEWEB)

    Barman, B.N.; Cebolla, V.L.; Membrado, L. [Equilon Enterprises LLC, Houston, TX (USA)

    2000-07-01

    Recent developments in chromatographic techniques for the separation and quantitative characterization of petroleum and related products are highlighted. Specifically, scope, applicability and versatility of individual techniques such as gas chromatography, liquid chromatography, supercritical fluid chromatography, thin-layer chromatography, and size-exclusion chromatography are discussed in some detail.

  1. A low-power pressure-and temperature-programmed separation system for a micro gas chromatograph.

    Energy Technology Data Exchange (ETDEWEB)

    Sacks, Richard D. (University of Michigan, Ann Arbor, MI); Robinson, Alex Lockwood (Advanced Sensor Technologies, Albuquerque, NM); Lambertus, Gordon R. (University of Michigan, Ann Arbor, MI); Potkay, Joseph A. (University of Michigan, Ann Arbor, MI); Wise, Kensall D. (University of Michigan, Ann Arbor, MI)

    2006-10-01

    This thesis presents the theory, design, fabrication and testing of the microvalves and columns necessary in a pressure- and temperature-programmed micro gas chromatograph ({micro}GC). Two microcolumn designs are investigated: a bonded Si-glass column having a rectangular cross section and a vapor-deposited silicon oxynitride (Sion) column having a roughly circular cross section. Both microcolumns contain integrated heaters and sensors for rapid, controlled heating. The 3.2 cm x 3.2 cm, 3 m-long silicon-glass column, coated with a non-polar polydimethylsiloxane (PDMS) stationary phase, separates 30 volatile organic compounds (VOCs) in less than 6 min. This is the most efficient micromachined column reported to date, producing greater than 4000 plates/m. The 2.7 mm x 1.4 mm Sion column eliminates the glass sealing plate and silicon substrate using deposited dielectrics and is the lowest power and fastest GC column reported to date; it requires only 11 mW to raise the column temperature by 100 C and has a response time of 11s and natural temperature ramp rate of 580 C/min. A 1 m-long PDMS-coated Sion microcolumn separates 10 VOCs in 52s. A system-based design approach was used for both columns.

  2. Solvent extraction columns

    International Nuclear Information System (INIS)

    In pulsed columns for use in solvent extraction processes, e.g. the reprocessing of nuclear fuel, the horizontal perforated plates inside the column are separated by interplate spacers manufactured from metallic neutron absorbing material. The spacer may be in the form of a spiral or concentric circles separated by radial limbs, or may be of egg-box construction. Suitable neutron absorbing materials include stainless steel containing boron or gadolinium, hafnium metal or alloys of hafnium. (UK)

  3. Direct zonal liquid chromatographic method for the kinetic study of actinomycin-DNA binding.

    Science.gov (United States)

    Vidal-Madjar, Claire; Florentina, Cañada-Cañada; Gherghi, Ioanna; Jaulmes, Alain; Pantazaki, Anastasia; Taverna, Myriam

    2004-07-01

    The binding of an anticancer drug (actinomycin D or ACTD) to double-stranded DNA (dsDNA) was studied by means of high-performance liquid chromatography (HPLC). ACTD is an antitumor antibiotic containing one chromophore group and two pentapeptidic lactone cycles that binds dsDNA. Incubations of ACTD with DNA were performed at physiological pH. The complexed and free ligand concentrations of the mixture were quantified at 440 nm from their separation on a size-exclusion chromatographic (SEC) column using the same buffer for the elution and the sample incubation. The DNA and the ACTD-DNA complexes were eluted at the column exclusion volume while the ligand was retained on the support. An apparent binding curve was obtained by plotting the amount emerging at the exclusion column volume against that eluted at free ACTD retention volume. A dissociating effect was evidenced and the binding parameters were significantly different from those obtained at equilibrium by visible absorbance titration. The equilibrium binding parameters determined by absorption spectroscopy were used as starting data in the numerical simulations of the chromatographic process. The results showed a strong dependency of the apparent binding parameters on the reaction kinetics. Finally the comparison of the apparent binding curve obtained from the HPLC experiments and from the numerical simulations permitted an evaluation of the dissociation rate constant (kd = 0.004 s(-1)). PMID:15296384

  4. Fully automated high-performance liquid chromatographic assay for the analysis of free catecholamines in urine.

    Science.gov (United States)

    Said, R; Robinet, D; Barbier, C; Sartre, J; Huguet, C

    1990-08-24

    A totally automated and reliable high-performance liquid chromatographic method is described for the routine determination of free catecholamines (norepinephrine, epinephrine and dopamine) in urine. The catecholamines were isolated from urine samples using small alumina columns. A standard automated method for pH adjustment of urine before the extraction step has been developed. The extraction was performed on an ASPEC (Automatic Sample Preparation with Extraction Columns, Gilson). The eluate was collected in a separate tube and then automatically injected into the chromatographic column. The catecholamines were separated by reversed-phase ion-pair liquid chromatography and quantified by fluorescence detection. No manual intervention was required during the extraction and separation procedure. One sample may be run every 15 min, ca. 96 samples in 24 h. Analytical recoveries for all three catecholamines are 63-87%, and the detection limits are 0.01, 0.01, and 0.03 microM for norepinephrine, epinephrine and dopamine, respectively, which is highly satisfactory for urine. Day-to-day coefficients of variation were less than 10%. PMID:2277100

  5. Zinc isotope separation with crown ether by column chromatography

    International Nuclear Information System (INIS)

    Depleted 64Zn is a new useful material and can be widely used in the cooling water treatment in light water nuclear power plants. In the present work, column chromatographic zinc isotope separation was performed by crown ether resin which was synthesized by ourselfs, the experimental results shown that benzo-15-crown-5 resin could effectively separate the zinc isotopes. High temperature could improve the separation coefficient, while the migration distance has no effect on separation coefficient. The height equivalent to a theoretical plate increase with the increasing of the migration distance. The separation coefficients (68Zn/64Zn=6.03 x 10-4, 66Zn/64Zn=3.52 x 10-4, respectively) and the height equivalent to a theoretical plate (0.204 cm) were obtained by 20 meters chromatographic operation with the temperature of 328 K. (authors)

  6. The separation of sup(99m)Tc from 99Mo through an aluminium oxide chromatographic columm

    International Nuclear Information System (INIS)

    The separation of sup(99m)Tc from 99Mo using the chromatographic method is studied. Alumina is used as adsorbent. The pH values for adsorption of carrier-free 99Mo on columns filled with ordinary alumina and with that thermically treated at 10000C for five hours, and the separation conditions of sup(99m)Tc using physiologic solution as eluent are determined. The sup(99m)Tc separation yields of both columns are compared and the quality of the products obtained by successive elutions for 10 days is analyzed. (Author)

  7. Development and validation of a gas chromatographic method for the assay of memantine hydrochloride in pure and tablet dosage forms

    OpenAIRE

    Siddappa K; Mallikarjun Metre; Mahesh Tambe; Mallikarjun Kote; Chandrakanth Reddy

    2011-01-01

    A gas chromatographic method has been developed and validated for the determination of memantine hydrochloride (MMT) in pure and pharmaceutical preparations. The detection was carried out using flame ionization detector. Separation was achieved on a DB-624 fused silica packed capillary column (30 m x 0.320 mm x 1.8 μm). Nitrogen was used as a carrier gas at a flow rate of 40 mL/min. The column temperature was maintained at 300°C while the temperature of injection port and detector were ...

  8. Biomimetic chromatographic analysis of selenium species: Application for the estimation of their pharmacokinetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Tsopelas, Fotios [National Technical University of Athens, Laboratory of Inorganic and Analytical Chemistry, School of Chemical Engineering, Athens (Greece); University of Athens, Laboratory of Pharmaceutical Chemistry, School of Pharmacy, Athens (Greece); Tsantili-Kakoulidou, Anna [University of Athens, Laboratory of Pharmaceutical Chemistry, School of Pharmacy, Athens (Greece); Ochsenkuehn-Petropoulou, Maria [National Technical University of Athens, Laboratory of Inorganic and Analytical Chemistry, School of Chemical Engineering, Athens (Greece)

    2010-07-15

    The retention behavior of selenites, selenates, seleno-dl-methionine, selenocystine, selenocystamine, selenourea, dimethyl selenide, and dimethyl diselenide was investigated by means of biomimetic liquid chromatography. For this purpose, two immobilized artificial membrane (IAM) columns, namely, IAM.PC.DD2 and IAM.PC.MG, and two immobilized plasma protein columns, human serum albumin (HSA) and {alpha}{sub 1}-acid glycoprotein (AGP) columns, were employed using different mobile phase conditions in respect to pH and buffer composition. In general, satisfactory interrelations between retention factors obtained with the two IAM stationary phases and HSA/AGP columns were obtained. Large differences were observed between biomimetic retention factors and octanol-water logD values, since the latter fail to describe electrostatic interactions. In contrast, despite the column diversity, the net retention outcome on all four biomimetic columns was quite similar, especially in the presence of phosphate-buffered saline, which by its effective shielding alleviates the differences between the stationary phases. Of the two IAM columns, IAM.PC.DD2 showed better performance when compared with HSA and AGP columns as well as to octanol-water partitioning. Biomimetic chromatographic indices were further used to estimate the percentage of human oral absorption and plasma protein binding of the eight selenium species investigated, according to equations previously reported in the literature. The estimated values of human oral absorption imply moderate absorption only for dimethyl diselenide, which also may exhibit considerable plasma protein binding. Moderate affinity for plasma proteins should also be expected for dimethyl selenide and selenocystamine. (orig.)

  9. A New Validated Liquid Chromatographic Method for the Determination of Loratadine and its Impurities

    OpenAIRE

    Ramulu, Gajjela; Ravindra Kumar, Yalavarthi; Vyas, Krishnamurthy; Suryanarayana, Mulukutla V.; Mukkanti, Khagga

    2011-01-01

    An improved gradient, reversed-phase liquid chromatographic (RP-LC) method was developed and subsequently validated for the determination of Loratadine and its impurities/degradation products in pharmaceutical drug substance. Separation was achieved with Inertsil ODS-3V, 250 × 4.6 mm, 5μ column with gradient elution at a flow rate of 1.0 mL min−1. UV detection was performed at 220 nm. The described method is linear over a range of LOQ (0.044, 0.088, 0.084, and 0.072 μg mL−1 for impurity-B, im...

  10. High performance liquid chromatographic determination of 123-I labeled tamoxifen metabolites in human plasma

    International Nuclear Information System (INIS)

    A high-performance liquid chromatographic procedure for the quantitation of [123I]Iodomethyl-N,N-diethyltamoxifen (ITX), a radioligand for human breast cancer imaging, in human plasma is described. Separation was effected on a RP-C18 column, using a mixture of acetonitrile-water-triethylamine (70/30/0.5, v/v). ITX was rapidly cleared from human plasma and metabolites appeared as early as 7.5 min p.i. Quantitative assessment of metabolites in plasma over time allowed recalculation of the ITX plasma time-activity curve. Implications of ITX metabolite formation for breast tumour imaging are discussed

  11. A nonlinear model for gas chromatograph systems

    Science.gov (United States)

    Feinberg, M. P.

    1975-01-01

    Fundamental engineering design techniques and concepts were studied for the optimization of a gas chromatograph-mass spectrometer chemical analysis system suitable for use on an unmanned, Martian roving vehicle. Previously developed mathematical models of the gas chromatograph are found to be inadequate for predicting peak heights and spreading for some experimental conditions and chemical systems. A modification to the existing equilibrium adsorption model is required; the Langmuir isotherm replaces the linear isotherm. The numerical technique of Crank-Nicolson was studied for use with the linear isotherm to determine the utility of the method. Modifications are made to the method eliminate unnecessary calculations which result in an overall reduction of the computation time of about 42 percent. The Langmuir isotherm is considered which takes into account the composition-dependent effects on the thermodynamic parameter, mRo.

  12. Amalgam-chromatographic separation of magnesium isotopes

    International Nuclear Information System (INIS)

    Separation of magnesium isotopes within Mg(Hg)-MgI2 system (in dimethylformamide) is conducted under amalgam-chromatographic conditions. Separation maximal degree, that is (1.09), for 24 Mg and 26 Mg and separation coefficient (α = 1.0089±0.006) are determined. Light isotopes are found to concentrate in the amalgam. Technique of thermal conversion of flows within amalgam-dimethylformamide system is suggested on the basis of reversible reaction of Ca-Mg element exchange

  13. Chromatographic determination of flumequine in food samples by post-column derivatisation with terbium(III)

    International Nuclear Information System (INIS)

    The potential usefulness of terbium(III) as reagent for the luminescent determination of flumequine residues in food samples has been studied using both fluorescence (FL) and time-resolved (TR) modes and both batch (B) and integrated liquid chromatography (LC)/derivatisation approaches. The system was optimised in each instance to establish the analytical features of the four methods. The dynamic ranges of the calibration graphs, obtained with standard solutions of flumequine, were (ng mL-1): B-FL 0.18-600; B-TR 2.4-150; LC-FL 3.7-1000 and LC-TR 52-3000. The detection limits were also obtained giving the following values (ng mL-1): B-FL 0.055; B-TR 0.7; LC-FL 1.1 and LC-TR 15. The precision, expressed as the percentage of relative standard deviation, was equal or lower than 5.1% in all instances. The LC methods, which avoid the interference of other quinolone antibiotics, were applied to the analysis of chicken muscle and liver, and whole milk samples. The sample pre-treatment only consisted of a deproteinisation step. The validation procedure for the analysis of samples was carried out using EC recommendations, and the decision limit and detection capability were calculated. The recoveries obtained ranged from 95.0% to 103.8%

  14. Chromatographic determination of flumequine in food samples by post-column derivatisation with terbium(III)

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez-Diaz, R.C. [Department of Analytical Chemistry, ' Marie Curie Annex' Building, Campus of Rabanales, University of Cordoba, E-14071 Cordoba (Spain); Fernandez-Romero, J.M. [Department of Analytical Chemistry, ' Marie Curie Annex' Building, Campus of Rabanales, University of Cordoba, E-14071 Cordoba (Spain); Aguilar-Caballos, M.P. [Department of Analytical Chemistry, ' Marie Curie Annex' Building, Campus of Rabanales, University of Cordoba, E-14071 Cordoba (Spain); Gomez-Hens, A. [Department of Analytical Chemistry, ' Marie Curie Annex' Building, Campus of Rabanales, University of Cordoba, E-14071 Cordoba (Spain)]. E-mail: qa1gohea@uco.es

    2006-09-25

    The potential usefulness of terbium(III) as reagent for the luminescent determination of flumequine residues in food samples has been studied using both fluorescence (FL) and time-resolved (TR) modes and both batch (B) and integrated liquid chromatography (LC)/derivatisation approaches. The system was optimised in each instance to establish the analytical features of the four methods. The dynamic ranges of the calibration graphs, obtained with standard solutions of flumequine, were (ng mL{sup -1}): B-FL 0.18-600; B-TR 2.4-150; LC-FL 3.7-1000 and LC-TR 52-3000. The detection limits were also obtained giving the following values (ng mL{sup -1}): B-FL 0.055; B-TR 0.7; LC-FL 1.1 and LC-TR 15. The precision, expressed as the percentage of relative standard deviation, was equal or lower than 5.1% in all instances. The LC methods, which avoid the interference of other quinolone antibiotics, were applied to the analysis of chicken muscle and liver, and whole milk samples. The sample pre-treatment only consisted of a deproteinisation step. The validation procedure for the analysis of samples was carried out using EC recommendations, and the decision limit and detection capability were calculated. The recoveries obtained ranged from 95.0% to 103.8%.

  15. Ion Chromatographic Determination of low level Perchlorate in Natural Waters

    International Nuclear Information System (INIS)

    Perchlorate (ClO4-) is a persistent contaminant of drinking-, surface-, and ground-water, and of soils. Possible contributions of ClO4- contamination are the military, the space program, and supporting industries and fertilizers. Perchlorate has long been known to have a negative effect on the thyroid gland. It has been added to the United States Environmental Protection Agency's (EPA) Contaminant candidate List (CCL) in 1998, so that ClO4 can be regulated at a concentration safe to humans. This paper describes the determination of trace level ClO4- in various matrices utilizing ion chromatographic method. The method utilizes a Dionex IonPac AS11 column with suppressed conductivity detection, 1500ul sample loop, and a 100 mN NaOH eluent at a flow rate of 1.0ml/min. These parameters allow a method detection limit (MDL) of 0.277ug/1 and a short retention time of 8 minutes. A quality control, proficiency testing samples from the EPA and a number of environmental samples from New York State (ground water) and California (ground and surface waters) were analyzed by this technique. Concentrations measured were in the range of 1.9-217 ug/1. No evidence of ClO4- was found in various commonly used fertilizers. (author)

  16. Extraction chromatographic studies on a strontium selective crown ether

    International Nuclear Information System (INIS)

    Selective adsorption of radiostrontium from nitric acid medium on a chromatographic resin material consisting of di-t-butyl cyclohexano 18 crown 6/n-octanol sorbed onto amberlite XAD-7 (particle size: 100-150μm) has been carried out. The column capacity is evaluated as ∼ 21 mg of Sr per gram of the resin material. The separation of radiostrontium from several metal ions present in environmental and biological samples viz. Li, Na, K, Mg, Ca, Al, Fe, Co, Ni, Zn and Cd has been achieved. A promising separation method for 90Y from 90Sr-90Y mixture has also been developed. Nitric acid concentration has no observable effect on the elution profile of 90Y as the entire amount of the loaded 90Y activity can be eluted by 1.5 ml of the acid in a wide concentration range (0. 1 - 10 M). Half-life of the eluted 90Y sample is calculated as 63.75 ± 0.40 hours by following the decay profile. Repeated elutions using 1.5 ml of 3 M HNO3 after loading 200 μCi of 90Sr - 90Y revealed that the product with ∼ 98% radiochemical purity could be obtained up to the 12th run beyond which the contamination due to 90Sr increased significantly. (author)

  17. Slender CRC Columns

    OpenAIRE

    Aarup, Bendt; Jensen, Lars Rom; Ellegaard, Peter

    2005-01-01

    CRC is a high-performance steel fibre reinforced concrete with a typical compressive strength of 150 MPa. Design methods for a number of structural elements have been developed since CRC was invented in 1986, but the current project set out to further investigate the range of columns for which current design guides can be used. The columns tested had a slenderness varying from 1.11 to 12.76 and a reinforcement ratio (area of rebar to area of concrete) ranging from 0 to 8.8 %. A total of 77 te...

  18. A new chromatographic-method for fast separation of active proteins

    Institute of Scientific and Technical Information of China (English)

    KE CongYu; GENG XinDu

    2008-01-01

    A new method with only a single chromatographic column to accomplish the separation of intact pro-tein molecules by the combination of ion exchange chromatography and hydrophobic interaction chromatography is firstly presented. By selecting twice a suitable stationary phase, mobile phase, buffer exchange condition, and sample injection, some proteins usually required to separate with two-dimensional chromatography can now be accomplished only using the single column in one hour. In addition, the separated proteins can maintain their original three- or four-dimensional molecular structure. It would be expected that this method can also provide a new thought for sample pre-frac-tionation in proteomic investigation, especially, for the limitation of sample source.

  19. Qualification of an Agilent Technologies 7890A gas chromatograph used in the biotechnology industry

    International Nuclear Information System (INIS)

    The drug manufacture is governed by strict international standards that guarantee reproducibility and consistency of results. The qualification of the instruments used in the productive processes, as well as in the characterization of products and their quality control are prerequisites to the validation of any analytical technique using them. One of the instrumental techniques used in the biotechnical industry is Gas Chromatography. A standard of pure caffeine was used for analysis in addition to a HP-5 30 m x 0,32 mm d.i. and 0,33 μm thick film column was used in a Gas Chromatograph coupled with a Flame Ionization Detector. For the testing of the different modules involved in the analysis (injector, column, oven and detector), an experimental design was made to estimate several parameters

  20. Rapid gas-liquid chromatographic method for determination of sulfamethazine in swine feed.

    Science.gov (United States)

    Munns, R K; Roybal, J E

    1982-09-01

    A gas-liquid chromatographic method is described for the quantitative determination of trace amounts of sulfamethazine in swine feed. Sulfamethazine is extracted in ammoniated acetone and isolated from other extractants on a Sephadex LH-20 column. The eluate is methylated with diazomethane and evaporated to dryness. The residue is dissolved in a solvent containing an internal standard of methyl sulfasymazine before being injected onto an OV-25 GLC column. An estimation of precision was established by assaying 10 sets of swine feed fortified with 0.5, 1,2, and 5 ppm SMZ. Mean recoveries were 96.0, 94.3, 93.5, and 94.0%, respectively, with an average coefficient of variation of 3.07%. The critical steps and ruggedness of the method were also determined. PMID:7130074

  1. Rapid gas-liquid chromatographic method for determination of sulfathiazole in swine feed.

    Science.gov (United States)

    Munns, R K; Roybal, J E

    1983-03-01

    A gas-liquid chromatographic (GLC) method for determining residues of sulfathiazole (STZ) in swine feed has been developed. Feed is extracted first with acetone and then with ammonia-acetone. STZ is isolated from other feed extractives on a Sephadex LH-20 column with methanol-toluene. The sulfa residues are methylated with diazomethane, and the eluate is evaporated to dryness. A solution containing an internal standard of methyl sulfasymazine is used to dilute the sample before injection onto an OV-25 GLC column. The precision of the method was determined by assaying 10 sets of feed spiked at 0.5, 1, 2, and 5 ppm STZ. The mean recoveries and coefficients of variation were 90.2 (5.90), 89.5 (4.67), 87.4 (5.62), and 87.7% (4.29), respectively. The critical steps of the method, including the stability of STZ, were also determined. PMID:6853414

  2. Column: Job crafting

    NARCIS (Netherlands)

    Reep, Frans van der

    2012-01-01

    1e alinea column: Organisaties dienen tegenwoordig randvoorwaarden te creëren waarbij ook behoeftes van de medewerkers aan autonomie, identificatie en zingeving worden vervuld. In organisaties die dit snappen geven de medewerkers zelf vorm aan eigen functie zodat die voldoet aan de behoeftes van de

  3. European Analytical Column

    DEFF Research Database (Denmark)

    Karlberg, B.; Grasserbauer, M.; Andersen, Jens Enevold Thaulov

    2009-01-01

    The European Analytical Column has once more invited a guest columnist to give his views on various matters related to analytical chemistry in Europe. This year, we have invited Professor Manfred Grasserbauer of the Vienna University of Technology to present some of the current challenges for...

  4. A hybrid FIA/HPLC system incorporating monolithic column chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Adcock, Jacqui L. [School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3217 (Australia); Francis, Paul S. [School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3217 (Australia)], E-mail: psf@deakin.edu.au; Agg, Kent M. [School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3217 (Australia); Marshall, Graham D. [GlobalFIA, Fox Island, WA 98333 (United States); Barnett, Neil W. [School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3217 (Australia)

    2007-09-26

    We have combined the generation of solvent gradients using milliGAT pumps, chromatographic separations with monolithic columns and chemiluminescence detection in an instrument manifold that approaches the automation and separation efficiency of HPLC, whilst maintaining the positive attributes of flow injection analysis (FIA), such as manifold versatility, speed of analysis and portability. As preliminary demonstrations of this hybrid FIA/HPLC system, we have determined six opiate alkaloids (morphine, pseudomorphine, codeine, oripavine, ethylmorphine and thebaine) and four biogenic amines (vanilmandelic acid, serotonin, 5-hydroxyindole-3-acetic acid and homovanillic acid) in human urine, using tris(2,2'-bipyridyl)ruthenium(III) and acidic potassium permanganate chemiluminescence detection.

  5. A hybrid FIA/HPLC system incorporating monolithic column chromatography

    International Nuclear Information System (INIS)

    We have combined the generation of solvent gradients using milliGAT pumps, chromatographic separations with monolithic columns and chemiluminescence detection in an instrument manifold that approaches the automation and separation efficiency of HPLC, whilst maintaining the positive attributes of flow injection analysis (FIA), such as manifold versatility, speed of analysis and portability. As preliminary demonstrations of this hybrid FIA/HPLC system, we have determined six opiate alkaloids (morphine, pseudomorphine, codeine, oripavine, ethylmorphine and thebaine) and four biogenic amines (vanilmandelic acid, serotonin, 5-hydroxyindole-3-acetic acid and homovanillic acid) in human urine, using tris(2,2'-bipyridyl)ruthenium(III) and acidic potassium permanganate chemiluminescence detection

  6. Mechanism of simultaneously refolding and purification of proteins by hydrophobic interaction chromatographic unit and applications

    Institute of Scientific and Technical Information of China (English)

    GENG; Xindu(耿信笃); BAI; Quan(白泉)

    2002-01-01

    The hydrophobic amino acid residues of a denatured protein molecule tend to react with the particles of the stationary phase of hydrophobic interaction chromatography (STHIC). These hydrophobic interactions prevent the denatured protein molecules from aggregating with each other. The STHIC can provide high enough energy to a denatured protein molecule to make it dehydration and to refold it into its native or various intermediate states. The outcome not only depends on the specific interactions between amino acids, the structure of STHIC, but also depends on the association between the STHIC and mobile phase. The mechanism of protein refolding and the principle of its quality control by HPHIC were also presented. By appropriate selection of the chromatographic condition, several denatured proteins can be refolded and separated simultaneously in a single chromatographic run. A specially designed unit, with diameter much larger than its length, was designed and employed for both laboratory and preparative scales. That unit for the simultaneous renaturation and purification of proteins (USRPP) had the following four functions: to completely remove denaturant, to renature proteins, to separate renatured proteins from impurities, and to easily recycle waste denaturant. The efficiencies of refolding and purification of proteins by the USRPP are almost comparable to a usual long chromatographic column in laboratory. In preparative scale, USRPP can be easily, rapidly, and economically applied requiring a low pressure gradient. As an example, recombinant human interferon-? is employed to elucidate the application of the preparative USRPP.

  7. Application of gas chromatographic method in simultaneous measurements of helium, argon and neon concentration in groundwaters

    Science.gov (United States)

    Najman, J.; Bielewski, J.; Sliwka, I.

    2012-04-01

    Helium concentration in groundwater is a fine indicator in water dating in a range from a hundred to tens of thousands of years. Gas chromatography (GC) measurements of helium can be used as an alternative to mass spectrometry (MS) determinations of 4He for groundwater dating [1]. Argon and neon concentrations mainly serve for determining the temperature of recharge and the air excess which is needed to correct measured values of helium concentration [2] . A chromatographic measurement system of helium, argon and neon concentration in groundwater is presented [3]. Water samples are taken from groundwater with a precise procedure without contamination with air in a special stainless steel vessels of volume equal to 2900 cm3. Helium is extracted from water samples using the head-space method. After enrichment by cryotrap method helium is analyzed in the gas chromatograph equipped with the thermal conductivity detector (TCD) with detection limit of about 2.8 ng He. The helium limit of detection of presented method is 1,2·10-8 cm3STP/gH2O [4]. We are currently working on adapting the method of cryogenic enrichment of helium concentration for simultaneous measurements of the concentration of helium, argon and neon using single sample of groundwater. Neon will be measured with the thermal conductivity detector and capillary column filled with molecular sieve 5A. Argon will be analyzed also with the thermal conductivity detector and packed column filled with molecular sieve 5A. This work was supported by grant No. N N525 3488 38 from the polish National Science Centre. [1] A. Zuber, W. Ciężkowski, K. Różański (red.), Tracer methods in hydrogeological studies - a methodological guide. Wroclaw University of Technology Publishing House, Wroclaw, 2007 (in polish). [2] P. Mochalski, Chromatographic method for the determination of Ar, Ne and N2 in water, Ph.D. thesis, Institute of Nuclear Physics Polish Academy of Sciences in Krakow, 2003 (in polish). [3] A. Żurek, P

  8. Purification of large plasmids with methacrylate monolithic columns.

    Science.gov (United States)

    Krajnc, Nika Lendero; Smrekar, Franci; Cerne, Jasmina; Raspor, Peter; Modic, Martina; Krgovic, Danijela; Strancar, Ales; Podgornik, Ales

    2009-08-01

    The rapid evolution of gene therapy and DNA vaccines results in an increasing interest in producing large quantities of pharmaceutical grade plasmid DNA. Most current clinical trials involve plasmids of 10 kb or smaller in size, however, future requirements for multigene vectors including extensive control regions may require the production of larger plasmids, e. g., 20 kb and bigger. The objective of this study was to examine certain process conditions for purification of large plasmids with the size of up to 93 kb. Since there is a lack of knowledge about production and purification of bigger plasmid DNA, cell lysis and storage conditions were investigated. The impact of chromatographic system and methacrylate monolithic column on the degradation of plasmid molecules under nonbinding conditions at different flow rates was studied. Furthermore, capacity measurements varying salt concentration in loading buffer were performed and the capacities up to 13 mg of plasmid per mL of the monolithic column were obtained. The capacity flow independence in the range from 130 to 370 cm/h was observed. Using high resolution monolithic column the separation of linear and supercoiled isoforms of large plasmids was obtained. Last but not least, since the baseline separation of RNA and pDNA was achieved, the one step purification on larger CIM DEAE 8 mL tube monolithic column was performed and the fractions were analyzed by CIM analytical monolithic columns. PMID:19598166

  9. Derringer desirability and kinetic plot LC-column comparison approach for MS-compatible lipopeptide analysis

    Directory of Open Access Journals (Sweden)

    Matthias D’Hondt

    2014-06-01

    In total, the performance of four different C18 columns, including one UPLC column, were evaluated using two parallel approaches. First, a Derringer desirability function was used, whereby six single and multiple chromatographic response values were rescaled into one overall D-value per column. Using this approach, the YMC Pack Pro C18 column was ranked as the best column for general MS-compatible lipopeptide separation. Secondly, the kinetic plot approach was used to compare the different columns at different flow rate ranges. As the optimal kinetic column performance is obtained at its maximal pressure, the length elongation factor λ (Pmax/Pexp was used to transform the obtained experimental data (retention times and peak capacities and construct kinetic performance limit (KPL curves, allowing a direct visual and unbiased comparison of the selected columns, whereby the YMC Triart C18 UPLC and ACE C18 columns performed as best. Finally, differences in column performance and the (disadvantages of both approaches are discussed.

  10. Selective determination of ammonium ions by high-speed ion-exclusion chromatography on a weakly basic anion-exchange resin column.

    Science.gov (United States)

    Mori, Masanobu; Tanaka, Kazuhiko; Helaleh, Murad I H; Xu, Qun; Ikedo, Mikaru; Ogura, Yutaka; Sato, Shinji; Hu, Wenzhi; Hasebe, Kiyoshi

    2003-05-16

    This paper describes an ion-exclusion chromatographic system for the rapid and selective determination of ammonium ion. The optimized ion-exclusion chromatographic system was established with a polymethacrylate-based weakly basic anion-exchange resin column (TSKgel DEAE-5PW) as the separation column, an aqueous solution containing 0.05 mM tetramethylammonium hydroxide (pH 9.10) as eluent with conductimetric detection for the analyte determination. Under the optimum chromatographic conditions, ammonium ion was determined within 2.3 min with a detection limit (S/N=3) better than 0.125 microM. Ammonium ion in rain and river waters was precisely determined using this ion-exclusion chromatographic system. PMID:12830892

  11. Host cell protein impurities in chromatographic polishing steps for monoclonal antibody purification.

    Science.gov (United States)

    Levy, Nicholas E; Valente, Kristin N; Lee, Kelvin H; Lenhoff, Abraham M

    2016-06-01

    Downstream purification of monoclonal antibodies (mAbs) is normally performed using a platform process that is empirically tuned to optimize impurity removal for each new product. A more fundamental understanding of impurities and the product itself would provide insights into the rational design of efficient downstream processes. This work examines the chromatographic properties of Chinese hamster ovary host cell protein (HCP) impurities in non-affinity chromatographic resins commonly used in polishing steps for monoclonal antibody purification: ion-exchange, hydrophobic interaction, and multimodal. Using proteomic analysis, the specific HCP impurities that elute close to mAb products are identified for these resins at typical downstream processing conditions. Additionally, the interactions of HCP impurities with mAb products are profiled to determine the total extent of product association and the specific HCP species that form associative complexes under conditions encountered in polishing columns. Product association and co-elution were both identified as viable mechanisms of HCP retention for the non-affinity resins tested here. A relatively large sub-population of HCP impurities was found to co-elute or associate with mAbs in each polishing column, but only a small population of HCPs-including lipoprotein lipase, chrondroitin sulfate proteoglycan 4, nidogen-1, and SPARC-were identified as difficult to remove across an entire downstream mAb process. Biotechnol. Bioeng. 2016;113: 1260-1272. © 2015 Wiley Periodicals, Inc. PMID:26550778

  12. Liquid chromatographic determination with fluorescence detection of B6 vitamers and riboflavin in milk and pharmaceuticals

    International Nuclear Information System (INIS)

    A simple, reliable and selective high performance liquid chromatographic method with fluorescence detection at different programmed wavelengths has been developed for the simultaneous analysis of B6 vitamers (pyridoxal 5'-phosphate, 4-pyridoxic acid, pyridoxal, pyridoxine and pyridoxamine) and Vitamin B2 in commercial vitaminized milk and in woman milk. The chromatographic separations were performed on a reversed phase octyl column by using a mobile phase consisting of sodium pentanesulfonate in 1% acetic acid-methanol-tetrahydrofuran under gradient elution conditions. The fluorescence intensity of pyridoxal 5'-phosphate was enhanced by post-column photochemical conversion, giving significantly different fluorescence spectra by a on-line photoreactor switched OFF and ON under irradiation at 254 nm. In addition, a simple and rapid method in isocratic conditions without the need of photochemical conversion was proposed for the analysis of Vitamin B6 and Vitamin B2 in pharmaceuticals. Linearity, precision, recovery, selectivity and sensitivity were found satisfactory for each analysed compound. Quantitation limits ranged from 26 to 240 fmol

  13. Derringer desirability and kinetic plot LC-column comparison approach for MS-compatible lipopeptide analysis

    Institute of Scientific and Technical Information of China (English)

    Matthias D’Hondt; Frederick Verbeke; Sofie Stalmans; Bert Gevaert; Evelien Wynendaele; Bart De Spiegeleern

    2014-01-01

    Lipopeptides are currently re-emerging as an interesting subgroup in the peptide research field, having historical applications as antibacterial and antifungal agents and new potential applications as antiviral, antitumor, immune-modulating and cell-penetrating compounds. However, due to their specific structure, chromatographic analysis often requires special buffer systems or the use of trifluoroacetic acid, limiting mass spectrometry detection. Therefore, we used a traditional aqueous/acetonitrile based gradient system, containing 0.1% (m/v) formic acid, to separate four pharmaceutically relevant lipopeptides (polymyxin B1, caspofungin, daptomycin and gramicidin A1), which were selected based upon hierarchical cluster analysis (HCA) and principal component analysis (PCA). In total, the performance of four different C18 columns, including one UPLC column, were evaluated using two parallel approaches. First, a Derringer desirability function was used, whereby six single and multiple chromatographic response values were rescaled into one overall D-value per column. Using this approach, the YMC Pack Pro C18 column was ranked as the best column for general MS-compatible lipopeptide separation. Secondly, the kinetic plot approach was used to compare the different columns at different flow rate ranges. As the optimal kinetic column performance is obtained at its maximal pressure, the length elongation factorλ(Pmax/Pexp) was used to transform the obtained experimental data (retention times and peak capacities) and construct kinetic performance limit (KPL) curves, allowing a direct visual and unbiased comparison of the selected columns, whereby the YMC Triart C18 UPLC and ACE C18 columns performed as best. Finally, differences in column performance and the (dis)advantages of both approaches are discussed.

  14. Biohydrogen. Chromatographic analysis is his component

    International Nuclear Information System (INIS)

    The method of preparation of artificial biohydrogen is perfected for research of processes of its dehydration and separation into pure hydrogen and carbon dioxide in order to use hydrogen as an energy carrier. The method of chromatographic analysis of biohydrogen components is perfected. Calibration of device in the interval of concentrations 0-100 % is conducted. It is determined that active coal of SKT-2A is an optimum adsorbent for separation of gas mixture into the pure components of H2 and CO2, and neon is an optimum gas-transmitter.

  15. Development of Gas Chromatographic Mass Spectrometry.

    Science.gov (United States)

    Hites, Ronald A

    2016-07-19

    Gas chromatographic mass spectrometry is now widely used for the quantitation and identification of organic compounds in almost any imaginable sample. These applications include the measurement of chlorinated dioxins in soil samples, the identification of illicit drugs in human blood, and the quantitation of accelerants in arson investigations, to name just a few. How did GC/MS get so popular? It turns out that it required parallel developments in mass spectrometry, gas chromatography, and computing and that no one person "invented" the technique. This Perspective traces this history from the 1950s until today. PMID:27384908

  16. Development of a micro gas chromatograph for the analysis of hydrogen isotope gas mixtures in the fusion fuel cycle

    International Nuclear Information System (INIS)

    Analysis of hydrogen isotopes is very important in the fuel cycle system of fusion reactors. Gas chromatography with a cryogenic separation column is one of the most extensively used methods for the analysis of hydrogen isotopes. Micro gas chromatograph (micro GC) with a cryogenic column is expected to improve the analysis time, that is a major disadvantage of conventional GC. The present authors have modified the micro GC to use its separation column at cryogenic temperature. In previous work a micro packed column has been tested and indicated fairly good performance. In this work a capillary column was tested at cryogenic temperature for more improvement of analysis time. Obtained retention time of H2, HD and D2 were about 43, 47 and 54 s, respectively, for the column with 0.53 mm of I.D., 4.0 m of length and 0.08 mm of film thickness. Peak resolution between H2 and HD was about 1.12. These results suggest that the column developed in this work attained the practical level for the separation and short analysis time. The estimation of the retention time was carried out using the dispersion model. The retention times of HT, DT and T2 were also estimated using the reduced mass

  17. Chromatographic behaviour of steroidal saponins studied by high-performance liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Kite, Geoffrey C; Porter, Elaine A; Simmonds, Monique S J

    2007-05-01

    The chromatographic behaviour of steroidal saponins found in Anemarrhena asphodeloides, Asparagus officinalis, Convallaria majalis, Digitalis purpurea and Ruscus aculeatus was studied by HPLC-MS using a C-18 reversed-phase column and aqueous acetonitrile or aqueous methanol mobile phase gradients, with or without the addition of 1% acetic acid. The behaviour was compared to that of triterpene saponins found in Aesculus hippocastanum, Centella asiatica, Panax notoginseng and Potentilla tormentilla. Inclusion of methanol in the mobile phase under acidic conditions was found to cause furostanol saponins hydroxylated at C-22 to chromatograph as broad peaks, whereas the peak shapes of the spirostanol saponins and triterpene saponins studied remained acceptable. In aqueous methanol mobile phases without the addition of acid, furostanol saponins chromatographed with good peak shape, but each C-22 hydroxylated furostanol saponin was accompanied by a second chromatographic peak identified as its C-22 methyl ether. Methanolic extracts analysed in non-acidified aqueous acetonitrile mobile phases also resolved pairs of C-22 hydroxy and C-22 methoxy furostanol saponins. The C-22 methyl ether of deglucoruscoside was found to convert to deglucoruscoside during chromatography in acidified aqueous acetonitrile, or by dissolving in water. Poor chromatography of furostanol saponins in acidified aqueous methanol is due to the interconversion of the C-22 hydroxy and C-22 methoxy forms. It is recommended that initial analysis of saponins by HPLC-MS using a C-18 stationary phase is performed using acidified aqueous acetonitrile mobile phase gradients. The existence of naturally-occurring furostanol saponins methoxylated at C-22 can be investigated with aqueous acetonitrile mobile phases and avoiding methanol in the extraction solvent. PMID:17391684

  18. High performance liquid chromatographic separation of eight drugs collected in Chinese Pharmacopoeia 2010 on amylose ramification chiral stationary phase

    Directory of Open Access Journals (Sweden)

    Yan Wang

    2012-10-01

    Full Text Available The enantiomers separation of eight pharmaceutical racemates collected in Chinese Pharmacopoeia 2010 (Ch.P2010, including nitrendipine, felodipine, omeprazole, praziquantel, sulpiride, clenbuterol hydrochloride, verapamil hydrochloride and chlorphenamine maleate, was performed on chiral stationary phase of amylose ramification by high performance liquid chromatography (HPLC on Chiralpak AD-H column and Chiralpak AS-H column with the mobile phase consisted of isopropanol and n-hexane. The detection wavelength and the flow rate were set at 254 nm and 0.7 mL/min, respectively. The effects of proportion of organic additives, alcohol displacer and temperature on the separation were investigated. The results indicated that eight chiral drugs were separated on chiral stationary phase of amylase ramification in normal phase chromatographic system. The chromatographic retention and resolution of enantiomers were adjusted by factors, including the changes of the concentration of alcohol displacer in mobile phase, organic alkaline modifier and column temperature. It was shown that the resolution was improved with reducing concentration of alcohol displacer. When the concentration of organic alkaline modifier was 0.2%, the resolution and the peak shape were fairly good. Most racemates mentioned above had the best resolution at column temperature of 25 °C. The best temperature should be kept unchanged in the process of separation so as to obtain stable separation results.

  19. Decoding the Pantheon Columns

    OpenAIRE

    Gerd Grasshoff; Christian Berndt

    2014-01-01

    The goal of this study has been to reconstruct the design principles underlying the construction of the Pantheon’s portico columns as well as to demonstrate how digital investigation methods and models can be used to improve our understanding of ancient architectural knowledge. Thanks to the data of the Bern Digital Pantheon Model, a synthesis of all the scanned surface points obtained during a digitization campaign of the Karman Center for Advanced Studies in the Humanities of the University...

  20. Kinetic performance evaluation and perspectives of contemporary packed column capillary electrochromatography.

    Science.gov (United States)

    De Smet, Seppe; Lynen, Frederic

    2014-08-15

    Capillary electrochromatography (CEC) is in essence a highly efficient and fast separation technique but practical constraints limit the current performance, robustness and routine implementation of the technique. In this work the kinetic performance limit (KPL) curve was used to evaluate commercial packed column CEC; this firstly in order to assess the broader applicability of the kinetic plot approach in electrodriven chromatographic techniques, and secondly to allow a more general unbiased comparison with HPLC performance. Evaluations were performed with a mixture of well retained and electrophoretically neutral phenones, to allow the observation of only chromatographic processes. Initial CEC retention time irreproducibility issues were solved by applying high acetonitrile content (80%) in the mobile phase, and solute retention was increased by increasing the phenone chain length. Comparison was performed with HPLC, with a column packed with an identical stationary phase to allow measurement of the performance under optimal conditions, and not with μ-LC on the CEC column as extra column peak broadening phenomena would thereby negatively affect the μ-LC performance. This comparison demonstrated that current HPLC performance largely outcompetes what is achievable with contemporary packed column CEC. Interestingly, significantly improved CEC performance could be obtained at lower temperatures (10°C) indicating a persistent degree of joule heating phenomena taking place in the contemporary packed column (100μm) CEC approach. Effective suppression of the latter opens possibilities for increasing the applicable voltage and outperforming HPLC and UHPLC. PMID:24958031

  1. RIGID GIGAPOROUS CHROMATOGRAPHIC MEDIA AND THEIR POTENTIAL IMPACT ON DOWNSTREAM PROCESSING

    Institute of Scientific and Technical Information of China (English)

    Tingyue Gu; Weiqing Zhou; Guanghui Ma; Zhiguo Su

    2005-01-01

    More and more biomolecules are being produced by the biotechnology industry for applications ranging from medicine and food to engineering materials. Liquid chromatography plays a center-stage role in a typical downstream process producing biomolecules such as recombinant proteins. Rigid gigaporous media are porous particles possessing large transecting through-pores with a pore-to-particle diameter ratio of dpore/dparticle> 0.01. They allow convective flow in the large through-pores, while the smaller diffusion-pores (typically several hundred angstroms in size) supply the needed surface areas. Because of the transecting gigapores, a portion of the mobile phase flows through the pores in addition to fluid flow in the interstitial spaces between the particles in a packed-bed column. This considerably lowers the operating column pressure drop. This lower pressure drop makes axial-direction scale-up of chromatographic columns possible to avoid pancake columns that invariably degrade separation resolution. The large gigapores also make the binding sites on the diffusion pore surfaces more accessible, thus increasing the loading capacity of large protein molecules that can be hindered sterically if only diffusion pores are present. This work discusses the development of rigid gigaporous media and their potential impact on the design of multi-stage downstream process from the angle of multi-scale analysis.

  2. Fast Chromatographic Method for Explosive Profiling

    Directory of Open Access Journals (Sweden)

    Pierre-Hugues Stefanuto

    2015-05-01

    Full Text Available Security control is becoming a major global issue in strategic locations, such as airports, official buildings, and transit stations. The agencies responsible for public security need powerful and sensitive tools to detect warfare agents and explosives. Volatile signature detection is one of the fastest and easiest ways to achieve this task. However, explosive chemicals have low volatility making their detection challenging. In this research, we developed and evaluated fast chromatographic methods to improve the characterization of volatile signatures from explosives samples. The headspace of explosives was sampled with solid phase micro-extraction fiber (SPME. Following this step, classical gas chromatography (GC and comprehensive two-dimensional GC (GC×GC were used for analysis. A fast GC approach allows the elution temperature of each analyte to be decreased, resulting in decreased thermal degradation of sensitive compounds (e.g., nitro explosives. Using fast GC×GC, the limit of detection is further decreased based on the cryo-focusing effect of the modulator. Sampling of explosives and chromatographic separation were optimized, and the methods then applied to commercial explosives samples. Implementation of fast GC methods will be valuable in the future for defense and security forensics applications.

  3. Determination of solute descriptors by chromatographic methods

    International Nuclear Information System (INIS)

    The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298 K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

  4. Chromatographic analysis of heterogeneous sorption systems

    International Nuclear Information System (INIS)

    This thesis deals with the chromatographic behavior of sorbates involved in three types of heterogeneous sorption systems: (1) a system with simultaneous ion exchange and electrolyte adsorption: (2) a system with various types of sorption sites; and (3) a multiphase system. The local equilibria between the phases are assumed, and the theory of shock waves and the concept of coherence are used to predict the dynamic behavior of these systems. For the type-1 system, a simplified model with a Langmuir type sorption isotherm is proposed. Through case studies and experiments, it is shown that electrolyte adsorption may play an important role in the migration of solutes through geologic media. For the type-2 system, a new concept of sorption affinity is proposed for predicting the chromatographic property of a general competitive sorption. In addition, some concrete expressions of affinity order are derived and examined to show the usefulness of the concept. For the type-3 system, a set of equations governing the multiphase transport of sorbates are formulated and applied to the colliod-facilitated governing the multiphase transport of radionuclides. Through numerical calculation, several conditions under which such transport is important are presented and examined

  5. Behavior of Columns During Earthquakes

    Data.gov (United States)

    National Oceanic and Atmospheric Administration, Department of Commerce — The behavior of columns during earthquakes is very important since column failures may lead to additional structural failures and result in total building...

  6. Determination of Two Columns Performance

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    When protein is analyzed by high performance liquid chromatography (HPLC), the selection of column is one of the most important factors. There are four quality control parameters for the column, which are theoretical plates n, capacity facto

  7. Identification and quantification of flavonoids in human urine samples by column switching liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Salka E.; Freese, R.; Cornett, C.;

    2000-01-01

    A rapid and sensitive high-performance liquid chromatographic mass spectrometric (HPLC-MS) method is described for the determination and quantification of 12 dietary flavonoid glycosides and aglycons in human urine samples. Chromatographic separation of the analytes of interest was achieved by...... column-switching, using the first column (a Zorbax 300SB C-3 column) for sample cleanup and eluting the heart-cut flavonoid fraction onto the second column (a Zorbax SE C-18 column) for separation and detection by ultraviolet and atmospheric pressure chemical ionization MS using single ion monitoring in...... variation for the analysis of the 12 different flavonoids in quality control urine samples were 12.3% on average (range 11.0-13.7%, n = 24, reproducibility) and the repeatability of the assay were 5.0% (mean, range 0.1-14.8%, it = 12). A subset of 10 urine samples from a human dietary intervention study...

  8. High performance liquid chromatographic determination of vanadium in crude oils and cobalt and iron in pharmaceutical preparations

    International Nuclear Information System (INIS)

    High performance liquid Chromatographic (HPLC) method has ben developed for the determination of vanadium in crude oils, based on acid decomposition of oils, followed by complexation with bis (salicylaldehyde) tetramethyl ethylenediamine (H2SA2Ten). The complex is extracted in organic phase and is separated from copper and nickel using normal phase HPLC column. Detection is achieved using spectrophtmetric detector. The vanadium in oil is obtained at sub microgram/g level. Similarly cobalt(II), cobalt(III) and iron(II) are separated on reversed phase HPLC column. Pre column derivatization is used to develop HPLC method for the determination of cobalt and iron in pharmaceutical preparations. Finally results are compared using atomic absorption spectrometer. (author)

  9. Modeling Transport in Gas Chromatography Columns for the Micro-ChemLab

    International Nuclear Information System (INIS)

    The gas chromatography (GC) column is a critical component in the microsystem for chemical detection ((mu)ChemLab(trademark)) being developed at Sandia. The goal is to etch a meter-long GC column onto a 1-cm(sup 2) silicon chip while maintaining good chromatographic performance. Our design strategy is to use a modeling and simulation approach. We have developed an analytical tool that models the transport and surface interaction process to achieve an optimized design of the GC column. This analytical tool has a flow module and a separation module. The flow module considers both the compressibility and slip flow effects that may significantly influence the gas transport in a long and narrow column. The separation module models analyte transport and physico-chemical interaction with the coated surface in the GC column. It predicts the column efficiency and performance. Results of our analysis will be presented in this paper. In addition to the analytical tool, we have also developed a time-dependent adsorption/desorption model and incorporated this model into a computational fluid dynamics (CFD) code to simulate analyte transport and separation process in GC columns. CFD simulations can capture the complex three-dimensional flow and transport dynamics, whereas the analytical tool cannot. Different column geometries have been studied, and results will be presented in this paper. Overall we have demonstrated that the modeling and simulation approach can guide the design of the GC column and will reduce the number of iterations in the device development

  10. Column and Batch Experiments

    Directory of Open Access Journals (Sweden)

    Jorge L. Gardea-Torresdey

    2005-01-01

    Full Text Available Batch and column experiments were performed to determine the Cu(II binding capacity of silica-immobilized humin biomass. For column studies, 500 bed volumes of a 0.1 mM Cu(II solution were passed through humin packed columns at the flow rates of 1, 1.5, 2, and 3 mL/min. The biopolymer showed an average Cu binding capacity of 12 ± 1.5 mg/g and a Cu recovery of about 96.5 % ± 1.5. The breakthrough points for Cu(II alone were approximately 420, 390, 385, and 300 bed volumes for the flow rates of 1, 1.5, 2 and 3 mL/min, respectively. The interference studies demonstrated that at low concentrations, the hard cations Ca(II and Mg(II did not seem to represent a major interference on Cu(II binding to the humin biopolymer. The selectivity showed by this biopolymer was Cu(II>Ca(II>Mg(II. On the other hand, batch experiments showed that Ca(II + Mg(II at 100mM each reduced the Cu(II binding to 73 %. However, 1000 mM concentrations of Ca(II and Mg(II, separately and in mixture, reduced the Cu(II binding to 47 %, 44 % and 31 %, respectively. The results of this study showed that immobilized humin in a silica matrix could represent an inexpensive bio-source for Cu removal from contaminated water, even in the presence of low concentrations of the hard cations Ca(II and Mg(II.

  11. Column: Every Last Byte

    Directory of Open Access Journals (Sweden)

    Simson Garfinkel

    2011-06-01

    Full Text Available Inheritance powder is the name that was given to poisons, especially arsenic, that were commonly used in the 17th and early 18th centuries to hasten the death of the elderly. For most of the 17th century, arsenic was deadly but undetectable, making it nearly impossible to prove that someone had been poisoned. The first arsenic test produced a gas—hardly something that a scientist could show to a judge. Faced with a growing epidemic of poisonings, doctors and chemists spent decades searching for something better.(see PDF for full column

  12. Packed column supercritical fluid chromatography of sodium stearyl fumarate aqueous suspension.

    Science.gov (United States)

    Gyllenhaal, Olle

    2006-03-01

    A method for the determination of sodium stearyl fumarate aqueous suspension is described. This straightforward method is based on homogenisation of the sample, dilution of a known aliquot with methanol to a suitable clear solution and mixing with an internal standard; (S)-naproxen. Separation and quantification is performed by packed column supercritical fluid chromatography on a commercial tartaric acid network polymeric column (tertbutylbenzoyl) with UV-detection at 214 nm. The precision of the presented method upon repeated analysis of a 20 mg/ml suspension is 0.5% (n = 8), and the yield is near 100%. Less than 5 min is required for the chromatographic separation with a resolution of about 3 to the internal standard. With some modification of the chromatographic conditions water samples can also be analysed. PMID:16174559

  13. Development of inlaid electrodes for whole column electrochemical detection in HPLC.

    Science.gov (United States)

    Seo, Jung-Ho; Leow, Pei Ling; Cho, Si-Hyeong; Lim, Hyun-Woo; Kim, Jin-Young; Patel, Bhavik Anil; Park, Jin-Goo; O'Hare, Danny

    2009-08-01

    An electrochemical microfluidic device has been fabricated on PET (polyethylene terephthalate) substrate using an imprinting method. The imprinting transfers patterns from a stamp into a substrate mechanically. However, a blanket mould imprinting process has been introduced to embed the photolithographically produced gold metal electrode lines into the PET substrate resulting in an individually addressable array flush to better than 100 nm. The device formed one wall of a packed chromatography column. The array was electrochemically characterised using standard redox probes in both stagnant conditions and under flow. Both numerical modelling and experimental data show improved sensitivity under flow and a limiting current which scaled linearly with the cube root of the volume flow rate. A chromatographic separation of the bioanalytical significant neurotransmitter dopamine (DA) and its metabolite DOPAC was achieved and electrochemically detected at multiple locations within the column. The PET device was stable and robust to leaks to pressures well in excess of those required for chromatographic separations. PMID:19606303

  14. Separation of rare earth by column chromatography using organic resins XAD/DEPHA

    International Nuclear Information System (INIS)

    The designation of light and heavy rare earth was used the fractionation used in separation processes. In this study the process of separation of rare earth, in groups, by chromatographic column consisting in fixing of cations these elements in an organic resin Amberlite XAD16 functionalized with the extracting agent DEPHA and another portion functionalized with a mixture of extractors DEPHA/TOP. The preparation of these resins was performed in two forms, one directly as the extracting agent to the resin and the other to be used in ethyl alcohol. Conditioned resins were introduced in chromatographic columns in separation of groups, light and heavy, using a standard solution of cerium nitrate and standard solution of holmium nitrate groups to represent light and heavy respectively. The characterization technique used to identify the rare earth elements was Spectrometry X-Ray Fluorescence (XRF). The results using the technique of chromatography were satisfactory, obtaining 100% separation of the elements. (author)

  15. Gas Chromatographic Detectors for Exobiology Flight Experiments

    Science.gov (United States)

    Kojiro, Daniel R.; Humphry, Donald E.; Takeuchi, Nori; Chang, Sherwood (Technical Monitor)

    1997-01-01

    Exobiology flight experiments require highly sensitive instrumentation for in situ chemical analysis of the volatile chemical species that occur in the atmospheres and surfaces of various bodies within the solar system. The complex mixtures encountered place a heavy burden on the analytical instrumentation to detect and identify all species present. Future missions to Mars', comets, or planetary moons such as Europa, will perform experiments with complex analyses. In addition, instrumentation for such missions must perform under severely restricted conditions with limited resources. To meet these analytical requirements, improved methods and highly sensitive yet smaller instruments must continually be developed with increasingly greater capabilities. We describe here efforts to achieve this objective, for past and future missions, through the development of new or the improvement of existing sensitive, miniaturized gas chromatographic detectors.

  16. Multiscale peak alignment for chromatographic datasets.

    Science.gov (United States)

    Zhang, Zhi-Min; Liang, Yi-Zeng; Lu, Hong-Mei; Tan, Bin-Bin; Xu, Xiao-Na; Ferro, Miguel

    2012-02-01

    Chromatography has been extensively applied in many fields, such as metabolomics and quality control of herbal medicines. Preprocessing, especially peak alignment, is a time-consuming task prior to the extraction of useful information from the datasets by chemometrics and statistics. To accurately and rapidly align shift peaks among one-dimensional chromatograms, multiscale peak alignment (MSPA) is presented in this research. Peaks of each chromatogram were detected based on continuous wavelet transform (CWT) and aligned against a reference chromatogram from large to small scale gradually, and the aligning procedure is accelerated by fast Fourier transform cross correlation. The presented method was compared with two widely used alignment methods on chromatographic dataset, which demonstrates that MSPA can preserve the shapes of peaks and has an excellent speed during alignment. Furthermore, MSPA method is robust and not sensitive to noise and baseline. MSPA was implemented and is available at http://code.google.com/p/mspa. PMID:22222564

  17. Simple gas chromatographic method for furfural analysis.

    Science.gov (United States)

    Gaspar, Elvira M S M; Lopes, João F

    2009-04-01

    A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF), 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect, temperature, adsorption and desorption times. The method is simple and accurate (RSDHMF; GC-TOF-MS: 0.3, 1.2 and 0.9 ngmL(-1) for 2-F, 5-MF and 5-HMF, respectively). It was applied to different commercial food matrices: honey, white, demerara, brown and yellow table sugars, and white and red balsamic vinegars. This one-step, sensitive and direct method for the analysis of furfurals will contribute to characterise and quantify their presence in the human diet. PMID:18976770

  18. FTIR gas chromatographic analysis of perfumes

    Science.gov (United States)

    Diederich, H.; Stout, Phillip J.; Hill, Stephen L.; Krishnan, K.

    1992-03-01

    Perfumes, natural or synthetic, are complex mixtures consisting of numerous components. Gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) techniques have been extensively utilized for the analysis of perfumes and essential oils. A limited number of perfume samples have also been analyzed by FT-IR gas chromatographic (GC-FTIR) techniques. Most of the latter studies have been performed using the conventional light pipe (LP) based GC-FTIR systems. In recent years, cold-trapping (in a matrix or neat) GC-FTIR systems have become available. The cold-trapping systems are capable of sub-nanogram sensitivities. In this paper, comparison data between the LP and the neat cold-trapping GC- FTIR systems is presented. The neat cold-trapping interface is known as Tracer. The results of GC-FTIR analysis of some commercial perfumes is also presented. For comparison of LP and Tracer GC-FTIR systems, a reference (synthetic) mixture containing 16 major and numerous minor constituents was used. The components of the mixture are the compounds commonly encountered in commercial perfumes. The GC-FTIR spectra of the reference mixture was obtained under identical chromatographic conditions from an LP and a Tracer system. A comparison of the two sets of data thus generated do indeed show the enhanced sensitivity level of the Tracer system. The comparison also shows that some of the major components detected by the Tracer system were absent from the LP data. Closer examination reveals that these compounds undergo thermal decomposition on contact with the hot gold surface that is part of the LP system. GC-FTIR data were obtained for three commercial perfume samples. The major components of these samples could easily be identified by spectra search against a digitized spectral library created using the Tracer data from the reference mixture.

  19. HPLC method development for the online-coupling of chromatographic Perilla frutescens extract separation with xanthine oxidase enzymatic assay.

    Science.gov (United States)

    Kaufmann, Christine M; Grassmann, Johanna; Letzel, Thomas

    2016-05-30

    Enzyme-regulatory effects of compounds contained in complex mixtures can be unveiled by coupling a continuous-flow enzyme assay to a chromatographic separation. A temperature-elevated separation was developed and the performance was tested using Perilla frutescens plant extracts of various polarity (water, methanol, ethanol/water). Owning to the need of maintaining sufficient enzymatic activity, only low organic solvent concentrations can be added to the mobile phase. Hence, to broaden the spectrum of eluting compounds, two different organic solvents and various contents were tested. The chromatographic performance and elution was further improved by the application of a moderate temperature gradient to the column. By taking the effect of eluent composition as well as calculated logD values and molecular structure of known extract compounds into account, unknown features were tentatively assigned. The method used allowed the successful observation of an enzymatic inhibition caused by P. frutescens extract. PMID:26986639

  20. Automated metal-free multiple-column nanoLC for improved phosphopeptide analysis sensitivity and throughput

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Rui; Ding, Shi-Jian; Shen, Yufeng; Camp, David G.; Livesay, Eric A.; Udseth, Harold R.; Smith, Richard D.

    2009-03-15

    We report on the development and characterization of an automated metal-free nanoscale multiple-capillary system for reversed-phase liquid chromatography-mass spectrometry analysis of phosphopeptides. The system incorporates a capillary column (50 um i.d. × 30 cm, packed with 5 um C18 particles) coupled on-line to a solid phase extraction column (150 um i.d. × 4 cm, packed with 5 um C18 particles). Electrospray ionization tips are constructed on the packed capillary column to couple the reversed-phase liquid chromatographic separation to a linear ion trap tandem mass spectrometer.

  1. Quasi-adiabatic vacuum-based column housing for very high-pressure liquid chromatography.

    Science.gov (United States)

    Gritti, Fabrice; Gilar, Martin; Jarrell, Joseph A

    2016-07-22

    A prototype vacuum-based (10(-6)Torr) column housing was built to thermally isolate the chromatographic column from the external air environment. The heat transfer mechanism is solely controlled by surface radiation, which was minimized by wrapping the column with low-emissivity aluminum tape. The adiabaticity of the column housing was quantitatively assessed from the measurement of the operational pressure and fluid temperature at the outlet of a 2.1mm×100mm column (sub-2 μm particles). The pressure drop along the column was raised up to 1kbar. The enthalpy balance of the eluent (water, acetonitrile, and one water/acetonitrile mixture, 70/30, v/v) showed that less than 1% of the viscous heat generated by friction of the fluid against the packed bed was lost to the external air environment. Such a vacuum-based column oven minimizes the amplitude of the radial temperature gradients across the column diameter and maximizes its resolving power. PMID:27324623

  2. Chromatographic isolation of 144Ce and 144Pr from the wastes of irradiated uranium treatment

    International Nuclear Information System (INIS)

    A two-step chromatographic technique was elaborated to isolate 144Ce, 144Pr from a solution of uranium fission products in 6M HNO3. The oxidation to Ce(III) by bromate and selective adsorption of 144Ce(IV) on anion exchange column were used to concentrate and purify 144Ce. Some impurities of uranium, 95Zr, 95Nb, 106Ru remain in 144Ce solution after the first step of its isolation. The final purification is achieved by passing the 6M HNO3 solution of 144Ce(IV) through the HDEHP-coated teflon column. The decontamination factors of 144Ce from main fission products are given. 7.2 mCi of (144Ce+144Pr) are recovered from each gram of irradiated uranium trioxide with the yield greater than 99%. An improvement of known generator was carried out to elute a purer 144Pr from maternal 144Ce(IV) adsorbed on the anion exchange column. (author)

  3. Ion-chromatographic determination of carbocisteine in pharmaceuticals based on non-suppressed conductimetric detection.

    Science.gov (United States)

    Megoulas, Nikolaos C; Koupparis, Michael A

    2004-02-13

    A novel method for the determination of carbocisteine (S-CMC), a mucolytic and expectorant drug with an acidic amino acid structure, was developed and validated, using non-suppressed ion-chromatographic system with conductimetric detection, and anion or cation exchange columns. Among the various combinations of column type and eluent composition tested, a cation exchange column with a 0.25 mM tri-fluoroacetic acid (TFA) as eluent in isocratic mode at 1.2 ml/min gave the best results. S-CMC was very well separated from all common amino acids (resolution > 2.6). The retention time was 3.5 min and the asymmetry factor 1.1. A linear calibration curve from 17 to 400 microg/ml (r = 0.99994), with a detection limit of 0.14 microg (5.6 microg/ml-25 microl injection volume) and a precision of 1.5% R.S.D. (100 microg/ml, n = 3) was achieved. The proposed method was applied for the determination of S-CMC content in intensely colored commercial formulations (syrups). No interference from excipients was found and the only pretreatment step was the appropriate dilution with the mobile phase. Recovery from standard additions was ranged from 96.0 to 104.9% and precision (R.S.D., n = 3) 1.8-3.6%. PMID:14763743

  4. Liquid-liquid contractor columns

    International Nuclear Information System (INIS)

    A liquid-liquid contactor column has a solvent input and an aqueous phase input. Lighter phase liquid is discharged and heavier phase is moved by an air lift to a receiver. The air supply line to the air lift includes valve and a pressure sensing transducer senses pressure in line and sends electric signals to signal processing unit which may for example close down operation of the column, or effect other changes to maintain operating characteristics of the column. The column could be pulsed by means which also send signals to unit, and could deliver to an external settler. (author)

  5. Anion exchange chromatographic distribution of human monoclonal immunoglobulin G is determined by heavy chain subclass and level of sialic acid expression

    Directory of Open Access Journals (Sweden)

    Ilić Vesna

    2012-01-01

    Full Text Available Anion exchange chromatography is widely accepted method for purification of immunoglobulins. In this work, we used human monoclonal immunoglobulin G (IgG with structure and solubility of normal human IgG as a model for studying chromatographic behavior of particular molecular forms of IgG. Human sera with monoclonal IgG were fractionated on strong anion exchanger, Q Sepharose Fast Flow. With 20 mM Tris pH 7.5 as a start buffer, 42% of human monoclonal IgG passed through column, and 58% of them remained adsorbed. Bound monoclonal IgG were eluted from the exchanger by linear increasing of concentration of NaCl from 0 to 0.5 M. Chromatographic distribution of human monoclonal IgG correlated with their electrophoretic mobility in agarose gels, and it was dependent on γ heavy chain isotype. Light chain type, as well as serum concentration of monoclonal IgG did not influence their chromatographic behavior. The level of heavy chain sialic acid expression, but not of galactose and N-acetylglucosamine, significantly determined chromatographic distribution of serum monoclonal IgG. Additionally to the information on the chromatographic behavior of human monoclonal IgG, we believe that presented data could provide useful information about the possible use of Q Sepharose Fast Flow matrix for the isolation of specific molecular forms of human IgG.

  6. [Preparation of an agglomerated ion chromatographic stationary phase with 2,3-ionene and its application in SO4(2-) analysis].

    Science.gov (United States)

    Wang, Muhua; Liu, Junwei; Huang, Zhongping; Zhang, Jiajie; Zhu, Yan

    2015-07-01

    The poly-electrolyte cation functional group of 2,3-ionene was synthesized with tetramethyl ethylenediamine and 1,3-dibromopropane as the raw materials. Multiporous polystyrene-divinylbenzene microsphere particles (PS-DVB) were produced by swelling method with polystyrene as seeds and sulfonated. Then the 2,3-ionene was bonded on the sulfonated multi-porous polystyrene-divinylbenzene microsphere particles by agglomeration to get the agglomerative ion-exchange stationary phase. After optimizing the synthetic conditions, the new stationary phase was characterized by the techniques including scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and elemental analysis. The chromatographic column was packed by slurry method and applied in the analysis of SO4(2-) with a conductivity detector. SO4(2-) and other six common anions including F-, Cl-, NO2(-), Br-, NO3(-), PO4(3-), were separated and analyzed rapidly on the self-regulating chromatographic column within 8 min. The linear range was from 0.5 to 50 mg/L with correlation coefficient (r) of 0.9992. The LOD was 0.04 mg/L with S/N of 3. The relative standard deviations (RSDs, n = 6) were 2.4% and 3.1% for the peak area and retention time, respectively. The recoveries were between 99.2% and 101.8%. The retention times of SO4(2-) did not change significantly after long time use of the self-regulating chromatographic column. The self-regulating chromatographic column is suitable for the detection of SO4(2-) in complex matrix samples. PMID:26672194

  7. Chromatographic separation and inductively coupled plasma atomic emission spectrometric determination of the rare earth metals contained in terbium

    International Nuclear Information System (INIS)

    The chromatographic separation of rare earth elements (REEs), prior to inductively coupled plasma atomic emission spectrometric (ICP-AES) measurements, using a column packed with 2-ethylexyl hydrogen 2-ethyl-hexylphosphonate (PC-88A)-loaded polymer resin in order to exclude spectral interferences was examined. A favourable separation of trace amounts of metals (La, Nd and Sm) from a large amount of terbium was achieved simply by elution with dilute hydrochloric acid. Trace lanthanum and neodymium in metallic terbium were determined by separation of the analyte ions from the matrix element followed by ICP-AES analysis. (author). 16 refs.; 5 figs.; 2 tabs

  8. High-performance liquid chromatographic determination of L-aspartyl-L-phenylalanine methyl ester in various food products and formulations.

    Science.gov (United States)

    Fox, L; Anthony, G D; Lau, E P

    1976-09-01

    A simple, rapid, and specific high-performance liquid chromatographic (HPLC) procedure is described for the analysis of the chemical sweetener L-aspartyl-L-phenylalanine methyl ester (aspartame). Using a strong cation exchange column and pressures less than 1000 psig, an analysis can be performed in less than 15 min. The technique has been applied to a wide range of food products and formulations. No interferences were found in the samples studied. Recoveries are quantitative, and the coefficients of variation for replicate analyses are less than or equal to 2.5%. PMID:965327

  9. Hydrophilic interaction chromatographic analysis of anthocyanins.

    Science.gov (United States)

    Willemse, Chandré M; Stander, Maria A; de Villiers, André

    2013-12-01

    Hydrophilic interaction chromatography (HILIC) provides an alternative separation mode for the analysis of phenolic compounds, in which aqueous-organic mobile phases with polar stationary phases are used. This paper reports the evaluation of HILIC for the analysis of the natural pigments anthocyanins, which are of importance because of their chromophoric properties and a range of health benefits associated with their consumption. Several HILIC stationary phases (silica, diol, amine, cyanopropyl and amide) and mobile phase combinations were evaluated, with the latter proving particularly important due to the distinctive chromatographic behaviour of anthocyanins. Diode array detection was used for selective detection of anthocyanins, while high resolution quadrupole-time-of-flight mass spectrometry (Q-TOF-MS) was used for compound identification. The potential of HILIC separation is demonstrated for a range of anthocyanins varying in glycosylation and acylation patterns found in blueberries, grape skins, black beans, red cabbage and red radish. HILIC is shown to be a complementary separation method to reversed phase liquid chromatography (RP-LC) due to the alternative retention mechanism. PMID:24188998

  10. Decomposition of pilocarpine eye drops assessed by a highly efficient high pressure liquid chromatographic method.

    Science.gov (United States)

    Kuks, P F; Weekers, L E; Goldhoorn, P B

    1990-10-19

    A rapid high-resolution high pressure liquid chromatographic method was developed for assaying pilocarpine. Pilocarpine in ophthalmic solutions decomposes fairly rapidly to give isopilocarpine, pilocarpic acid and isopilocarpic acid. The quality of an ophthalmic solution can be assessed by assaying these decomposition products. Existing high pressure liquid chromatographic methods suffer from long analysis times and poor resolution. The new method uses as the mobile phase 6 ml/l of triethylamine in water (pH 2.3, adjusted with 85% phosphoric acid) at a flow of 1.5 ml/min and as the stationary phase a C18-silica 125 x 4.6 mm column. 2-Amino-1-phenyl-1,3-propanediol is used as an internal standard. Complete separation was obtained within 8 min. Pilocarpine eye drops were stored under different conditions and then analysed for decomposition products. During heat treatment, decomposition to isopilocarpine predominated over decomposition to pilocarpic or isopilocarpic acid. However, when stored at room temperature or in a refrigerator, formation of pilocarpic acid clearly prevailed. Thus, from assessment of decomposition products, the cause of decomposition can be established. PMID:2255589

  11. Gas chromatographic method for the determination of lumefantrine in antimalarial finished pharmaceutical products

    Directory of Open Access Journals (Sweden)

    Sultan Suleman

    2015-09-01

    Full Text Available A simple method has been developed and validated for quantitative determination of lumefantrine in antimalarial finished pharmaceutical products using gas chromatography coupled to flame ionization detector. Lumefantrine was silylated with N,O–bis(trimethyl-silyltrifluoro-acetamide at 70°C for 30 minutes, and chromatographic separation was conducted on a fused silica capillary (HP-5, 30 m length × 0.32 mm i.d., 0.25 μm film thickness column. Evaluation of the method within analytical quality-by-design principles, including a central composite face-centered design for the sample derivatization process and Plackett–Burman robustness verification of the chromatographic conditions, indicated that the method has acceptable specificity toward excipients and degradants, accuracy [mean recovery = 99.5%, relative standard deviation (RSD = 1.0%], linearity (=0.9986, precision (intraday = 96.1% of the label claim, RSD = 0.9%; interday = 96.3% label claim, RSD = 0.9%, and high sensitivity with detection limits of 0.01 μg/mL. The developed method was successfully applied to analyze the lumefantrine content of marketed fixed-dose combination antimalarial finished pharmaceutical products.

  12. REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR THE ANALYSIS OF GLIPIZIDE IN PHARMACEUTICAL DOSAGE FORMS

    Directory of Open Access Journals (Sweden)

    Sheikh Rahila

    2010-12-01

    Full Text Available A rapid and sensitive reverse phase high performance liquid chromatographic methods depicted for the qualitative and quantitative assay of glipizide in pharmaceutical dosage forms. Glipizide was chromatographed on reverse phase C18 column with mobile phase consisting of 0.05 M Potassium Dihydrogen Orthophosphate: Methanol [15: 85 %v/v, pH 7.0 ± 0.05, adjusted with 1% Triethylamine]. The mobile phase was pumped at a flow rate 1 mL/min. Quantification was achieved by monitoring the ultraviolet absorbance at 225 ηm. The average retention time for Glipizide was found to be 3.21 ± 0.07. With this method, linearity was observed in the range of 10 – 2000 ηg/ml. The LOD and LOQ were found to be 5 ηg/ml and 15 ηg/ml respectively. The method was applicable for the analysis of drug in tablet formulation. The results of analysis were validated statistically.

  13. Simple high-performance liquid chromatographic method for the determination of medroxyprogesterone acetate in human plasma.

    Science.gov (United States)

    Read, J; Mould, G; Stevenson, D

    1985-06-14

    The high-performance liquid chromatographic (HPLC) method was developed as a simple, reliable alternative to available methods for measuring plasma concentrations of medroxyprogesterone acetate (MPA). The HPLC method has been successfully automated and is suitable for the rapid, inexpensive analysis of large batches of plasma samples. The best approach involves a solvent extraction followed by HPLC separation and analysis. MPA can be efficiently extracted, at all pH values, by nonpolar solvents. The Spherisorb 5-ODS2 HPLC column provides excellent separation of MPA from endogenous steroids of similar structure and from extraneous plasma blank peaks. A batch of 30-40 samples can be prepared by HPLC analysis in 2-3 hours, with a chromatographic run time of 10 minutes/sample. Calibration curves between 5-250 ng/ml show a good correlation between peak height ratio and MPA concentration, even at low levels. Plasma concentrations of MPA in patients receiving 1 g/day were between 12.6-270 ng/ml in this study, suggesting that the sensitivity of this method, 10 ng/ml, is sufficient for monitoring therapeutic concentrations of MPA. The results show a wide individual variation in plasma concentrations following similar dosing schedules--a finding reported by other workers. PMID:3161906

  14. Mass spectrometric and high-performance liquid chromatographic studies of medroxyprogesterone acetate metabolites in human plasma.

    Science.gov (United States)

    Sturm, G; Häberlein, H; Bauer, T; Plaum, T; Stalker, D J

    1991-01-01

    Medroxyprogesterone acetate (MPA) treatment has been shown to exert several beneficial effects in cancer patients. It has been suggested that such effects are due in part to the metabolites derived from MPA in vivo. The first results are reported on the identification of 2 alpha-hydroxy- and 21-hydroxy-MPA, 20-dihydro-MPA, 17 alpha-acetoxy-2 alpha,3 beta-dihydroxy-6 alpha-methylpregn-1,4-dien-20-one and two X,21-dihydroxy-MPAs, one of them presumably being 6 alpha-hydroxymethyl-21-hydroxy-MPA, in patient's plasma by high-performance liquid chromatographic (HPLC), gas chromatographic-mass spectrometric and NMR methods. Additionally, the presence of other metabolites such as di- and tetrahydro-MPAs and 6,21-dihydroxy-MPA, found in urine and other samples, was demonstrated in plasma. For routine clinical examinations an HPLC method is described for determination of, e.g., the unreduced MPA metabolite group in Sep-Pak-ODS column extracts of patients' plasma. PMID:1827448

  15. Investigations on the chromatographic behaviour of zwitterionic stationary phases used in hydrophilic interaction chromatography.

    Science.gov (United States)

    Chirita, Raluca-Ioana; West, Caroline; Zubrzycki, Sandrine; Finaru, Adriana-Luminita; Elfakir, Claire

    2011-09-01

    Two commercial stationary phases possessing a sulfobetaine zwitterionic bonded ligand (ZIC-HILIC and Nucleodur HILIC) were compared under hydrophilic interaction chromatographic (HILIC) conditions. First of all, the separation of 12 model compounds chosen among neurotransmitters and presenting a diversity of ionization states (anionic, cationic and zwitterionic) was studied under varied operating conditions. The effects of the percentage of acetonitrile, ammonium acetate concentration and temperature of the mobile phase were compared on the two columns. Secondly, a generally applicable retention model was established, based on chromatographic retention data (logk) acquired for 76 model compounds. The chosen compounds are small molecules presenting a wide diversity of molecular structures and are relevant to biomedical and pharmaceutical studies. To account for their retention behaviour, a modified version of the solvation parameter model was designed: two additional molecular descriptors were introduced, to account for ionic interactions with anionic and cationic species. The retention equations obtained allow a rationalization of the interactions contributing to retention and separation in the HILIC systems considered. PMID:21571288

  16. An advanced hybrid reprocessing system based on UF6 volatilization and chromatographic separation

    International Nuclear Information System (INIS)

    To recover U, Pu, MA (Np, Am, Cm) and some specific fission products FPs (Cs, Sr, Tc, etc.) from various spent nuclear fuels (LWR/FBR: Oxide, Metal Fuels), we are studying an advanced hybrid reprocessing system based on UF6 volatilization (Pyro) and chromatographic separation (Aqueous). Spent fuels are de-cladded by means of thermal and mechanical methods and then applied to the fluorination/volatilization process, which selectively recovers the most amount of U. Then, the remained fuel components are converted to oxides and dissolved by HNO3 solution. Compared to U, since Pu, MA and FPs are significantly less abundant in spent fuels, the scale of the aqueous separation process could become reasonably small and result in less waste. For the chromatographic separation processes, we have prepared different types of porous silica-based organic/inorganic adsorbents with fast diffusion kinetics, improved chemical stability and low pressure drop in a packed column. So they are advantageously applicable to efficient separation of the actinides and FP elements from the fuel dissolved solution. In this work, adsorption and separation behavior of representative actinides and FP elements was studied. Small scale separation tests using simulated and genuine fuel dissolved solutions were carried out to verify the feasibility of the proposed process. (authors)

  17. Extraction chromatographic studies of zirconium(IV) with n-capric acid

    International Nuclear Information System (INIS)

    A selective method has been developed for reversed phase extraction chromatographic studies of zirconium(IV) with high molecular weight carboxylic acid, n-capric acid as a stationary phase on a column of silica gel. Quantitative extraction of zirconium(IV) has been achieved from 0.01 M acetic acid solution in the pH range 2.5-5.0. The extracted zirconium(IV) has been stripped with nitric acid (4 M) and estimated spectrophotometrically. THe effect of variables as pH, stripping agents, flow rate on extraction and elution have been studied. Exchange capacity of the exchanger and breakthrough capacity have been determined. Zirconium(IV) has been separated from various elements. Zirconium(IV) has also been separated from several synthetic multicomponent mixtures. (author). 10 refs., 4 tabs., 1 fig

  18. The chromatographic analysis of oligosaccharides and preparation of 1-kestose and nystose in yacon.

    Science.gov (United States)

    Zhu, Zhen-Yuan; Lian, Hong-Yu; Si, Chuan-Ling; Liu, Yang; Liu, Nian; Chen, Jing; Ding, Li-Na; Yao, Qiang; Zhang, Yongmin

    2012-05-01

    The thin-layer chromatographic analysis of the crude oligosaccharides extracted from yacon revealed the presence of glucose, fructose, sucrose, 1-kestose and nystose. The qualitative and quantitative analysis was carried out on oligosaccharides by high pressure liquid chromatography and the results showed that the contents of d-glucose, fructose, sucrose, 1-kestose, nystose and 1-fructofuranosyl nystose in oligosaccharides were 38.30%, 16.44%, 14.58%, 12.29%, 12.17%, 6.20%, respectively. The content of the fructooligosaccharides in oligosaccharides was 30.66%. The crude oligosaccharides were separated and purified by silica gel column chromatography. The two fractions obtained from crude oligosaccharides were 1-kestose and nystose, which were identified by mass spectra. The yield of 1-kestose and nystose were 10.36% and 9.73%, respectively. The purity of 1-kestose was 82.9% and of nystose was 73.6%. PMID:22013906

  19. Radioactivation gold determination in natural waters with extraction-chromatographic separation

    International Nuclear Information System (INIS)

    Ground water 50 ml samples were evaporated to dryness, the residues were packed into Al foils, irradiated for 2 days by 1.8x1013 n/cm2sec neutron flux, then dissolved in aqua regia, evaporated, and diluted with distilled water. Au was then separated on an extraction-chromatographic column using (n-C8H17)3N on powdered Teflon. The sorption efficiency of 198Au was 98-9%. Thiourea was used as eluent. Amounts of Au in water were calculated from the photopeaks of 0.41 MeV by comparing with standard reference 198Au samples. The sensitivity of the method was 10-10-10-11 g/ml water. Without accounting for the irradiation time, 12-15 samples could be analyzed per working day

  20. Identification of meat treated with ionizing radiation by capillary gas chromatographic determination of radiolytically produced hydrocarbons

    International Nuclear Information System (INIS)

    When triglycerides or fatty acids are irradiated, some of the major stable products are hydrocarbons formed from the loss of CO2 and CH3COOH in various free-radical reactions. A capillary gas chromatographic procedure has been developed to monitor the presence of these radiolytically generated hydrocarbons in meats treated with ionizing radiation. Several lipid extraction procedures for isolating the radiolytically generated hydrocarbons from the irradiated meat were compared. The radiolytically generated hydrocarbons were separated from the extracted lipids on a Florisil column and determined by capillary gas chromatography. The yield of these radiolytically generated hydrocarbons was linear with absorbed dose. Data indicating the utility of this-methodology to identify meat products (poultry, beef, and pork) treated with ionizing radiation are presented

  1. High-performance liquid chromatographic determination of methyl anthranilate, hydroxymethylfurfural and related compounds in honey.

    Science.gov (United States)

    Nozal, M J; Bernal, J L; Toribio, L; Jiménez, J J; Martín, M T

    2001-05-11

    A high-performance liquid chromatographic method for determining 5-hydroxymethyl-2-furaldehyde (hydroxymethylfurfural), 2-furaldehyde (furfural), furan-2-carboxylic acid (2-furoic acid), furan-3-carboxylic acid (3-furoic acid), furan-3-carboxaldehyde (3-furaldehyde) and 2-aminobenzoic acid methyl ester (methyl anthranilate) in honey and honeydew samples is described. To prevent matrix interference and to isolate the compounds, a clean-up step which implies a solid-phase extraction on polymeric cartridges and an elution with 0.5 ml methanol is recommended. The compounds are separated on a reversed-phase column with a gradient of (A) 1% aqueous acetic acid-acetonitrile (97:3, v/v) and (B) acetonitrile-water (50:50, v/v), with UV detection at 250 nm. The method is applied to the analysis of samples from different botanical origin. PMID:11403496

  2. Rapid separation of non-polar and weakly polar analytes with metal-organic framework MAF-5 coated capillary column.

    Science.gov (United States)

    Tian, Jingyu; Lu, Cuiming; He, Chun-Ting; Lu, Tong-Bu; Ouyang, Gangfeng

    2016-05-15

    Metal-organic frameworks (MOFs) have attracted widespread attention due to their unique characters such as high surface area, high thermal and chemical stability, diverse structure topology and tunable pore size. The study first exploited a porous metal organic framework MAF-5 ([Zn[(eim)2], Heim=2-ethylimidazole) as stationary phase for gas chromatography by a novel dynamic coating method. The column efficiency of the 184 silicone@MAF-5 capillary column was up to 9045 platesm(-1) for benzene. The column is very promising for the rapid separation of polycyclic aromatic hydrocarbons (PAHs) and organochlorine pesticides (OCPs). And the column showed good reproducibility, retention time, peak area, high resolution, and a wide linear range. The determined thermodynamic parameters and chromatographic retention of all probe molecules on the 184 silicone@MAF-5 column showed the separation of analytes is a complex balance of thermodynamic and kinetic factors. PMID:26992522

  3. Polystyrene-co-Divinylbenzene PolyHIPE Monoliths in 1.0 mm Column Formats for Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Sidratul Choudhury

    2016-03-01

    Full Text Available The reversed phase liquid chromatographic (RP-HPLC separation of small molecules using a polystyrene-co-divinylbenzene (PS-co-DVB polyHIPE stationary phases housed within 1.0 mm i.d. silcosteel columns is presented within this study. A 90% PS-co-DVB polyHIPE was covalently attached to the walls of the column housing by prior wall modification with 3-(trimethoxysilyl propyl methacrylate and could withstand operating backpressures in excess of 200 bar at a flow rate of 1.2 mL/min. Permeability studies revealed that the monolith swelled slightly in 100% acetonitrile relative to 100% water but could nevertheless be used to separate five alkylbenzenes using a flow rate of 40 µL/min (linear velocity: 0.57 mm/s. Remarkable column-to-column reproducibility is shown with retention factor variation between 2.6% and 6.1% for two separately prepared columns.

  4. Rayleigh light scattering detection of three α1-adrenoceptor antagonists coupled with high performance liquid chromatograph

    Science.gov (United States)

    Li, Ai Ping; Peng, Huanjun; Peng, Jing Dong; Zhou, Ming Qiong; Zhang, Jing

    2015-08-01

    Herein, a Rayleigh light-scattering (RLS) detection method combined with high performance liquid chromatograph (HPLC) without any post-column probe was developed for the separation and determination of three α1-adrenoceptor antagonists. The quantitative analysis is benefiting from RLS signal enhancement upon addition of methanol which induced molecular aggregation to form an hydrophobic interface between aggregates and water that produce a sort of superficial enhanced scattering effect. A good chromatographic separation among the compounds was achieved using a Gemini 5u C18 reversed phase column (250 mm × 4.6 mm; 4 μm) with a mobile phase consisting of methanol and ammonium acetate-formic acid buffer solution (25 mM; pH = 3.0) at the flow rate of 0.7 mL min-1. The RLS signal was monitored at λex = λem = 354 nm. A limit of detection (LOD) of 0.065-0.70 μg L-1 was reached and a linear range was found between peak height and concentration in the range of 0.75-15 μg L-1 for doxazosin mesylate (DOX), 0.075-3.0 μg L-1 for prazosin hydrochloride (PRH), and 0.25-5 μg L-1 for terazosin hydrochloride (TEH), with linear regression coefficients all above 0.999. Recoveries from spiked urine samples were 88.4-99.0% which is within acceptable limits. The proposed method is convenient, reliable and sensitive which has been used successfully in human urine samples.

  5. PATTERN RECOGNITION STUDIES OF COMPLEX CHROMATOGRAPHIC DATA SETS

    Science.gov (United States)

    Chromatographic fingerprinting of complex biological samples is an active research area with a large and growing literature. Multivariate statistical and pattern recognition techniques can be effective methods for the analysis of such complex data. However, the classification of ...

  6. Performance tests on new chromatographic material for 99Mo-99mTc generators

    International Nuclear Information System (INIS)

    Technetium-99m continues to be the main workhorse of nuclear medicine in the Philippines. Almost 13TBq of 99mTc was imported to the country in 2002 supplied as 99mTc-99Mo generators. These generators make use of fission molybdenum adsorbed onto an alumina column. Problems associated with the alumina chromatographic generators arise due to safety and economic issues that would be remedied by gel-type generators using low specific activity reactor-produced molybdenum-99 adsorbed on a high capacity gel column material. The Philippine Nuclear Research Institute (PNRI) exerted efforts in this direction by developing a gel-type column, which showed satisfactory molybdenum adsorptive capacity. Likewise, Kaken Co. in Japan in cooperation with Japan Atomic Energy Research Institute (JAERI) developed a dried form of a gel-type polyzirconium compound (PZC). It is a ready-to-use high molybdenum capacity column material for adsorbing reactor-produced molybedum-99. The performance of this material is being tested under the framework of the FNCA project on Research Reactor Utilization. Performance tests on four batches of PZC were performed using fission molybdenum eluted from a 99Mo- 99mTc generator. A total of 3.3 GBq 99Mo was extracted from an alumina column of a commercial generator and mixed with carrier molybdenum solution. About 0.67 GBq was loaded into each of the 12 x 90 mm column. One batch was prepared and distributed in 1999 and tests showed very poor elution yield of 30%. Three recent batches of PZC (2002) gave elution yields of 71% (Range of 69-75). The adsorptive capacity is 99% with about 4% desorption rate. Elution volume is at 5-6 ml. Daily elution for five days gave from 1.6 to 5.5% variability. The tests were performed all at the same time and a trend of improving elution yield and consistency of daily elution yield was observed with the time of testing nearer to the sample preparation date. X-ray diffraction analysis showed an amorphous structure for all

  7. Chromatographic behavior of strontium selective extractive scintillators

    International Nuclear Information System (INIS)

    This paper presents the characterization of three extractive scintillation resins for simultaneous quantification and detection of radioactive strontium in aqueous solutions. Extractive scintillation resins combine extraction chromatography with scintillation radiation detection to selectively quantify non-gamma-ray emitting radionuclides in acidified solutions into a single step. The extractive scintillating resins are produced by impregnating macroporous acrylic or polystyrene resin with organic fluors PPO and DM-POPOP. The scintillating macroporous resin was subsequently impregnated with DtBuCH18C6-crown in 1-octanol or a proprietary chelating agent to produce Sr ES 3, Sr ES 10 and Sr ES 12. Resins were characterized using a combination of batch and flow-cell (column) experiments. Flow-cell experiments were conducted by packing 1.6 mm inner diameter translucent polytetrafluoroethylene tubing with the extractive scintillating resin to produce a ∼0.2 ml pore volume column. The tubing was subsequently coiled and placed between two 28.6 mm diameter photomultiplier tubes connected in coincidence. This arrangement allowed for real-time quantification of the radioactivity that was retained by the extractive scintillating resin. All extractive scintillating resins exhibited satisfied separation factor for Sr-90/Y-90 and good regeneration capability in multiplied loading. (authors)

  8. Mush Column Magma Chambers

    Science.gov (United States)

    Marsh, B. D.

    2002-12-01

    Magma chambers are a necessary concept in understanding the chemical and physical evolution of magma. The concept may well be similar to a transfer function in circuit or time series analysis. It does what needs to be done to transform source magma into eruptible magma. In gravity and geodetic interpretations the causative body is (usually of necessity) geometrically simple and of limited vertical extent; it is clearly difficult to `see' through the uppermost manifestation of the concentrated magma. The presence of plutons in the upper crust has reinforced the view that magma chambers are large pots of magma, but as in the physical representation of a transfer function, actual magma chambers are clearly distinct from virtual magma chambers. Two key features to understanding magmatic systems are that they are vertically integrated over large distances (e.g., 30-100 km), and that all local magmatic processes are controlled by solidification fronts. Heat transfer considerations show that any viable volcanic system must be supported by a vertically extensive plumbing system. Field and geophysical studies point to a common theme of an interconnected stack of sill-like structures extending to great depth. This is a magmatic Mush Column. The large-scale (10s of km) structure resembles the vertical structure inferred at large volcanic centers like Hawaii (e.g., Ryan et al.), and the fine scale (10s to 100s of m) structure is exemplified by ophiolites and deeply eroded sill complexes like the Ferrar dolerites of the McMurdo Dry Valleys, Antarctica. The local length scales of the sill reservoirs and interconnecting conduits produce a rich spectrum of crystallization environments with distinct solidification time scales. Extensive horizontal and vertical mushy walls provide conditions conducive to specific processes of differentiation from solidification front instability to sidewall porous flow and wall rock slumping. The size, strength, and time series of eruptive behavior

  9. Analysis and chromatographic purification of eicosanoids multiply labeled by tritium

    International Nuclear Information System (INIS)

    We show the possibility of analysis and chromatographic purification of eicosanoids triply labeled by tritium. The described methods allow us to isolate chromatographically pure products obtained by selective hydrogenatin, chemical, and enzyme methods, with radiochemical purity at least 95-97%. The following methods are used to analyze the reaction mixtures and to isolate the tritium-labeled eicosanoids: gas-liquid chromatography, high-efficiency liquid chromatography, and thin-layer chromatography on supports impregnated with silver nitrate

  10. Chromatographic transport of alkaline buffers through reservoir rock

    International Nuclear Information System (INIS)

    Use of relatively low-pH alkaline buffers, such as sodium carbonate or sodium silicate, is explored as a means for overcoming sodium/hydrogen ion-exchange delay in alkaline waterflooding. A local-equilibrium chromatographic model is outlined to describe the concentration velocities for injection of alkaline buffers into a linear porous medium that exhibits reversible sodium/hydrogen exchange. The theory predicts a buffer ion-exchange wave that is substantially faster than that for equivalent-pH sodium hydroxide solutions. New experimental displacement data are presented for NaOH over a pH range from 11 to 13 and for 0.1, 0.5, and 1.0 wt% Na/sub 2/CO/sub 3/ flowing through a 1 wt% NaCl brine saturated Berea sandstone core at 500C [1220F]. To permit a complete description of the system, column effluent concentrations are measured for sodium ions, hydroxide ions, H/sup 3/-tagged water, and /sup 14/C-tagged carbonate. The experiments confirm that Na/sub 2/CO/sub 3/ propagates through the Berea sand at a higher rate than NaOH. For example, at pH=11.4, Na/sub 2/CO/sub 3/ migrates with a velocity that is 3.5 times faster than NaOH. Comparison of experiment with the ion-exchange chromatography theory shows good agreement. The authors successfully model the concentration histories of tritium-labeled water, total carbon, sodium, and hydroxide, all with no adjustable parameters. This work establishes with both theory and experiment that buffered alkali significantly increases the propagation speed of hydroxide in reservoir sands in comparison with unbuffered alkali at equivalent sodium and hydroxide concentrations. Because lower-pH buffered alkali can also protect against rock dissolution loss, the validated reduction of buffer ion-exchange lag considerably improves the promise of the alkaline flooding process for field application

  11. Comparison of thin layer chromatographic and gas chromatographic determination of propoxur residues in a cocoa ecosystem

    International Nuclear Information System (INIS)

    The fate of propoxur in a cocoa ecosystem has been studied using thin layer chromatographic (TLC) and gas chromatographic (GC) methods. Residues of propoxur as determined by both TLC and GC were not significantly different. TLC analysis of propoxur residues in soil, cocoa leaves and pods did not require any rigorous cleanup since residues measured from cleaned extracts and without cleanup were not significantly different. The residue levels of propoxur in the soil were found to decrease rapidly and, by the 21st day, none was detected in the topsoil (0-15 cm). Evidence of leaching of propoxur residues in the soil has also been demonstrated. The amount left in the top soil after the first seven days were 27%, 23% and 24% of the initial one as determined by the TLC without cleanup, TLC with cleanup and GLC, respectively. No propoxur residue was detected in topsoil 21 days after spraying. About 38% of pesticides detected on the cocoa pod on the day of treatment remained on the pod seven days after treatment. The residue detected on the leaves on the day of treatment was higher than that in or on the soil. This decreased rapidly to 1.7% in 21 days compared to 16% for the soil and 23% for the pod. (author)

  12. Computer assisted optimization of liquid chromatographic separations of small molecules using mixed-mode stationary phases.

    Science.gov (United States)

    Ordoñez, Edgar Y; Benito Quintana, José; Rodil, Rosario; Cela, Rafael

    2012-05-18

    Mixed-mode stationary phases are gaining adepts in liquid chromatography (LC) as more and more applications are published and new commercial columns appear in the market ought to their ability to retain and separate analytes with multiple functionalities. The increased number of adjustable variables gives these columns an enhanced value for the chromatographer, but, on the other hand, it complicates the process of developing satisfactory separations when complex samples must be analyzed. Thus, the availability of computer assisted methods development (CAMD) tools is highly desirable in this field. Therefore, the first specific tool for the CAMD of LC separations in mixed-mode columns is presented. The tool consists in two processes. The first one develops a retention model for peaks in a predefined experimental domain of pH and buffer concentration. In this domain, the retention as a function of the proportion of organic modifier is modeled using a two-stage re-calibration process departing from isocratic retention data and then, from gradient elutions. With this two-stage approach, reliability is gained. In the second process, the model is finally interpolated and used for the unattended optimization of the different possible elution modes available in these columns. This optimization process is driven by an evolutionary algorithm. The development and application of this new chemometrics tool is demonstrated by the optimization of a mixture of neutral and ionizable compounds. Hence, several different types of gradients were generated, showing a good agreement between simulated and experimental data, with retention time errors lower than 5% in most cases. On the other hand, classical CAMD tools, such as design of experiments, were unable to efficiently deal with mixed-mode optimizations, rendering errors above 30% for several compounds. PMID:22494641

  13. Relating pressure tuned coupled column ensembles with the solvation parameter model for tunable selectivity in gas chromatography.

    Science.gov (United States)

    Sharif, Khan M; Kulsing, Chadin; Chin, Sung-Tong; Marriott, Philip J

    2016-07-15

    The differential pressure drop of carrier gas by tuning the junction point pressure of a coupled column gas chromatographic system leads to a unique selectivity of the overall separation, which can be tested using a mixture of compounds with a wide range of polarity. This study demonstrates a pressure tuning (PT) GC system employing a microfluidic Deans switch located at the mid-point of the two capillary columns. This PT system allowed variations of inlet-outlet pressure differences of the two columns in a range of 52-17psi for the upstream column and 31-11psi for the downstream column. Peak shifting (differential migration) of compounds due to PT difference are related to a first order regression equation in a Plackett-Burman factorial study. Increased first (upstream) column pressure drop makes the second column characteristics more significant in the coupled column retention behavior, and conversely increased second (downstream) column pressure drop makes the first column characteristics more apparent; such variation can result in component swapping between polar and non-polar compounds. The coupled column system selectivity was evaluated in terms of linear solvation energy relationship (LSER) parameters, and their relation with different pressure drop effects has been constructed by applying multivariate principle component analysis (PCA). It has been found that the coupled column PT system descriptors provide a result that shows a clear clustering of different pressure settings, somewhat intermediate between those of the two commercial columns. This is equivalent to that obtained from a conventional single-column GC analysis where the interaction energy contributed from the stationary phases can be significantly adjusted by choice of midpoint PT. This result provides a foundation for pressure differentiation for selectivity enhancement. PMID:27302688

  14. High performance liquid chromatographic method for the determination of cinepazide maleate and its application to a pharmacokinetic study in rats.

    Science.gov (United States)

    Zhao, Jinyi; Song, Ying; Wang, Hujun; Sun, Yuan; Liu, Meiyou; Lu, Chengtao; Li, Yan; Wang, Shan; Zhu, Xiaohe; Hai, Wenli; Wen, Aidong; Jia, Yanyan

    2014-04-15

    A simple and reliable high performance liquid chromatographic (HPLC) method has been developed and validated to quantify cinepazide maleate, a calcium blocker, in rat plasma. Cinepazide maleate and Tinidazole (internal standard) have been extracted by a simple liquid-liquid extraction before injection into chromatographic system. Chromatographic separation was achieved on a reversed phase C18 column with a mobile phase consisted of a water mixture of 10mM potassium dihydrogen phosphate (pH=4.5):methanol (40:60, v/v), pumped at flow rate of 1.0mL/min, and detected at 303nm. The method exhibited a linear range of 0.12-120μg/mL in blank rat plasma, with the lower detection limit of 0.06μg/mL. The method was statistically validated for linearity, accuracy, precision, selectivity and stability following FDA guidelines. The intra- and inter-assay coefficients of variation did not exceed ±15% from the nominal concentration. The accuracy of cinepazide maleate was within ±15% of the theoretical value. The assay has been applied successfully in a pharmacokinetic study of cinepazide maleate after a single intravenous at three doses in rat. And cinepazide maleate injection can improve the bioavailability of cinepazide maleate greatly, and has a dose-dependence profile in rats. PMID:24674989

  15. Extraction-chromatographic generator of technetium-99m. Principles of functioning and exploiting conditions

    International Nuclear Information System (INIS)

    Technetium-99m pharmaceuticals are spin-off products resulting from the decomposition of the 99Mo radioactive nuclide; they occupy leading positions in world medical diagnostics. Technetium-99m is β -relay product of radioactive nuclide of molybdenum-99. For dividing of genetically connected pair of 99Mo / 99mTc is using generators sets, in which accumulation of technetium-99m lasts for period of 22 hours. 99mTc generators could be subdivided for 3 basic types: chromatographic (sorbtioned), sublimated and extractioned ones. Extraction technology is concentrated, and it lets to receive solutions with high specific activity even from low level activity molybdenum-99, which is produced by reaction of radioactive capture 98Mo (n,γ ) 99Mo form natural molybdenum targets. Main defects of extracted generators: big size of extractors; necessity to control over procedure of separation extracting substance from water phase with the idea to decrease its wastes with visual or other method; long-time period to proceed preparation (1,5 - 2 hours), mainly because of extracting substance evaporation period; high requirements to personnel. Pointed defects prevent to use extracted generators directly in medical radiological laboratories. NPI at TPU developed an extraction-chromatographic generator with the mobile compact extraction device, based on the 'black box' principle. Its construction ensures self-regulation of phase division level. Total volume of extraction substance is not more then 80 cm3 with 110 mm high. It can be transported in safe box without unpacking directly in medical establishments. Frequent extraction with the same low volume of extracting substance provides high level of yield of technetium-99m. Subdividing of radioactive nuclide is going at chromatographic column with Al2O3 sorbent. Extraction-chromatographic generator at the same time then technetium-99m products became lower price let's to solve problem to provide regional clinics, there are middle

  16. Extraction-chromatographic generator of technetium-99m. Principle of functioning and exploiting conditions

    International Nuclear Information System (INIS)

    Full text: Technetium-99m pharmaceuticals are spin-off products resulting from the decomposition of the 99Mo radioactive nuclide; they occupy leading positions in world medical diagnostics. Technetium-99m is β -relay product of radioactive nuclide of molybdenum-99. For dividing of genetically connected pair of 99Mo / 99mTc is using generators sets, in which accumulation of technetium-99m lasts for period of 22 hours. 99m Tc generators could be subdivided for 3 basic types: chromatographic (sorbtioned), sublimated and extractioned ones. Extraction technology is concentrated, and it lets to receive solutions with high specific activity even from low level activity molybdenum-99, which is produced by reaction of radioactive capture 98Mo (n,γ ) 99Mo form natural molybdenum targets. Main defects of extracted generators: big size of extractors; necessity to control over procedure of separation extracting substance from water phase with the idea to decrease its wastes with visual or other method; long-time period to proceed preparation (1,5 - 2 hours), mainly because of extracting substance evaporation period; high requirements to personnel. Pointed defects prevent to use extracted generators directly in medical radiological laboratories. NPI at TPU developed an extraction-chromatographic generator with the mobile compact extraction device, based on the 'black box' principle. Its construction ensures self-regulation of phase division level. Total volume of extraction substance is not more then 80 cm3 with 110 mm high. It can be transported in safe box without unpacking directly in medical establishments. Frequent extraction with the same low volume of extracting substance provides high level of yield of technetium-99m. Subdividing of radioactive nuclide is going at chromatographic column with Al2O3 sorbent. Extraction-chromatographic generator at the same time then technetium-99m products became lower price let's to solve problem to provide regional clinics, there are

  17. Stability of column-supported steel cylinders with engaged columns

    OpenAIRE

    DOERICH, Cornelia; Vanlaere, Wesley; Lagae, Guy; Rotter, J. Michael

    2009-01-01

    p. 2535-2546 Steel silos are often supported on a small number of columns to facilitate emptying operations. The connection between these columns and an elevated cylindrical metal silo shell is a long-standing difficult problem in shell analysis. The presence of local supports beneath a cylinder leads to stress concentrations in the cylindrical wall just above the supports, which can cause buckling or plastic collapse and consequently failure of the entire structure. Engaged co...

  18. Direct probing of chromatography columns by laser-induced fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    McGuffin, V.L.

    1992-12-07

    This report summarizes the progress and accomplishments of this research project from September 1, 1989 to February 28, 1993. During this period, we have accomplished all of the primary scientific objectives of the research proposal: (1) constructed and evaluated a laser-induced fluorescence detection system that allows direct examination of the chromatographic column, (2) examined nonequilibrium processes that occur upon solute injection and elution, (3) examined solute retention in liquid chromatography as a function of temperature and pressure, (4) examined solute zone dispersion in liquid chromatography as a function of temperature and pressure, and (5) developed appropriate theoretical models to describe these phenomena. In each of these studies, substantial knowledge has been gained of the fundamental processes that are responsible for chromatographic separations. In addition to these primary research objectives, we have made significant progress in three related areas: (1) examined pyrene as a fluorescent polarity probe insupercritical fluids and liquids as a function of temperature and pressure, (2) developed methods for the class-selective identification of polynuclear aromatic hydrocarbons in coal-derived fluids by microcolumn liquid chromatography with fluorescence quenching detection, and (3) developed methods for the determination of saturated and unsaturated (including omega-3) fatty acids in fish oil extracts by microcolumn liquid chromatography with laser-induced fluorescence detection. In these studies, the advanced separation and detection techniques developed in our laboratory are applied to practical problems of environmental and biomedical significance.

  19. Liquid-liquid extraction columns

    International Nuclear Information System (INIS)

    The patent concerns liquid-liquid extraction columns in which solute transfer across the liquid-liquid interface sets up Marangoni instabilities which give rise to interfacial turbulence. The phenomenon has been observed to occur in the solvent extraction of uranium and/or plutonium from an aqueous nitric phase using tributyl phosphate with odourless kerosens. The invention provides a method of quantifying the degree of Marangoni instabilities in a column-type liquid-liquid extraction column, and determining a value for the solute free characteristic velocity parameter. The method also gives a measure of the extent to which the characteristic velocity is modified by the Marangoni instability. (U.K.)

  20. Liquid-liquid extraction columns

    Energy Technology Data Exchange (ETDEWEB)

    Batey, W.; Lonie, S.J.; Thompson, P.J.; Thornton, J.D.

    1987-11-11

    The patent concerns liquid-liquid extraction columns in which solute transfer across the liquid-liquid interface sets up Marangoni instabilities which give rise to interfacial turbulence. The phenomenon has been observed to occur in the solvent extraction of uranium and/or plutonium from an aqueous nitric phase using tributyl phosphate with odourless kerosens. The invention provides a method of quantifying the degree of Marangoni instabilities in a column-type liquid-liquid extraction column, and determining a value for the solute free characteristic velocity parameter. The method also gives a measure of the extent to which the characteristic velocity is modified by the Marangoni instability. (U.K.).

  1. Improved column-based radiochemical processing of the generator produced 68Ga

    International Nuclear Information System (INIS)

    An improved chemical strategy for processing of the generator produced 68Ga was developed based on processing of the original 68Ge/68Ga generator eluate on a micro-column. Direct pre-concentration and purification of the eluted 68Ga is performed on a cation-exchange resin in hydrochloric acid/acetone media. A supplementary step based on a second micro-column filled with a second resin allows direct re-adsorption of 68Ga eluted from the cation exchanger. 68Ga is finally striped from the second resin with a small volume of pure water. For this purpose a strong anion exchanger and a novel extraction chromatographic resin based on tetraalkyldiglycolamides are characterized. The strategy allows online pre-concentration and purification of 68Ga from the original generator eluate. The supplementary column allows transferring 68Ga with high radionuclide and chemical quality in the aqueous solution with small volume and low acidity useful for direct radiolabeling reactions.

  2. Recent advances in the preparation and application of monolithic capillary columns in separation science.

    Science.gov (United States)

    Hong, Tingting; Yang, Xi; Xu, Yujing; Ji, Yibing

    2016-08-10

    Novel column technologies involving various materials and efficient reactions have been investigated for the fabrication of monolithic capillary columns in the field of analytical chemistry. In addition to the development of these miniaturized systems, a variety of microscale separation applications have achieved noteworthy results, providing a stepping stone for new types of chromatographic columns with improved efficiency and selectivity. Three novel strategies for the preparation of capillary monoliths, including ionic liquid-based approaches, nanoparticle-based approaches and "click chemistry", are highlighted in this review. Furthermore, we present the employment of state-of-the-art capillary monolithic stationary phases for enantioseparation, solid-phase microextraction, mixed-mode separation and immobilized enzyme reactors. The review concludes with recommendations for future studies and improvements in this field of research. PMID:27282747

  3. Green approach using monolithic column for simultaneous determination of coformulated drugs.

    Science.gov (United States)

    Yehia, Ali M; Mohamed, Heba M

    2016-06-01

    Green chemistry and sustainability is now entirely encompassed across the majority of pharmaceutical companies and research labs. Researchers' attention is careworn toward implementing the green analytical chemistry principles for more eco-friendly analytical methodologies. Solvents play a dominant role in determining the greenness of the analytical procedure. Using safer solvents, the greenness profile of the methodology could be increased remarkably. In this context, a green chromatographic method has been developed and validated for the simultaneous determination of phenylephrine, paracetamol, and guaifenesin in their ternary pharmaceutical mixture. The chromatographic separation was carried out using monolithic column and green solvents as mobile phase. The use of monolithic column allows efficient separation protocols at higher flow rates, which results in short time of analysis. Two-factor three-level experimental design was used to optimize the chromatographic conditions. The greenness profile of the proposed methodology was assessed using eco-scale as a green metrics and was found to be an excellent green method with regard to the usage and production of hazardous chemicals and solvents, energy consumption, and amount of produced waste. The proposed method improved the environmental impact without compromising the analytical performance criteria and could be used as a safer alternate for the routine analysis of the studied drugs. PMID:27062581

  4. Water Column Sonar Data Collection

    Data.gov (United States)

    National Oceanic and Atmospheric Administration, Department of Commerce — The collection and analysis of water column sonar data is a relatively new avenue of research into the marine environment. Primary uses include assessing biological...

  5. In-line gas chromatographic apparatus for measuring the hydrophobic micropore volume (HMV) and contaminant transformation in mineral micropores

    International Nuclear Information System (INIS)

    Desorption of hydrophobic organic compounds from micropores is characteristically slow compared to surface adsorption and partitioning. The slow-desorbing mass of a hydrophobic probe molecule can be used to calculate the hydrophobic micropore volume (HMV) of microporous solids. A gas chromatographic apparatus is described that allows characterization of the sorbed mass with respect to the desorption rate. The method is demonstrated using a dealuminated zeolite and an aquifer sand as the model and reference sorbents, respectively, and trichloroethylene (TCE) as the probe molecule. A glass column packed with the microporous sorbent is coupled directly to a gas chromatograph that is equipped with flame ionization and electron capture detectors. Sorption and desorption of TCE on the sorbent was measured by sampling the influent and effluent of the column using a combination of switching and injection valves. For geosorbents, the HMV is quantified based on Gurvitsch's rule from the mass of TCE desorbed at a rate that is characteristic for micropores. Instrumental requirements, design considerations, hardware details, detector calibration, performance, and data analysis are discussed along with applications. The method is novel and complements traditional vacuum gravimetric and piezometric techniques, which quantify the total pore volume under vacuum conditions. The HMV is more relevant than the total micropore volume for predicting the fate and transport of organic contaminants in the subsurface. Sorption in hydrophobic micropores strongly impacts the mobility of organic contaminants, and their chemical and biological transformations. The apparatus can serve as a tool for characterizing microprous solids and investigating contaminant-solid interactions.

  6. Liquid chromatographic determination with fluorescence detection of B{sub 6} vitamers and riboflavin in milk and pharmaceuticals

    Energy Technology Data Exchange (ETDEWEB)

    Gatti, R. [Dipartimento di Scienze Farmaceutiche, Universita di Bologna, Via Belmeloro 6, 40126 Bologna (Italy)]. E-mail: rita.gatti2@unibo.it; Gioia, M.G. [Dipartimento di Scienze Farmaceutiche, Universita di Bologna, Via Belmeloro 6, 40126 Bologna (Italy)

    2005-05-04

    A simple, reliable and selective high performance liquid chromatographic method with fluorescence detection at different programmed wavelengths has been developed for the simultaneous analysis of B{sub 6} vitamers (pyridoxal 5'-phosphate, 4-pyridoxic acid, pyridoxal, pyridoxine and pyridoxamine) and Vitamin B{sub 2} in commercial vitaminized milk and in woman milk. The chromatographic separations were performed on a reversed phase octyl column by using a mobile phase consisting of sodium pentanesulfonate in 1% acetic acid-methanol-tetrahydrofuran under gradient elution conditions. The fluorescence intensity of pyridoxal 5'-phosphate was enhanced by post-column photochemical conversion, giving significantly different fluorescence spectra by a on-line photoreactor switched OFF and ON under irradiation at 254 nm. In addition, a simple and rapid method in isocratic conditions without the need of photochemical conversion was proposed for the analysis of Vitamin B{sub 6} and Vitamin B{sub 2} in pharmaceuticals. Linearity, precision, recovery, selectivity and sensitivity were found satisfactory for each analysed compound. Quantitation limits ranged from 26 to 240 fmol.

  7. Chromatographic biopanning for the selection of peptides with high specificity to Pb2+ from phage displayed peptide library.

    Science.gov (United States)

    Nian, Rui; Kim, Duck Sang; Nguyen, Thuong; Tan, Lihan; Kim, Chan-Wha; Yoo, Ik-Keun; Choe, Woo-Seok

    2010-09-17

    Toxic heavy metal pollution is a global problem occurring in air, soil as well as water. There is a need for a more cost effective, renewable remediation technique, but most importantly, for a recovery method that is selective for one specific metal of concern. Phage display technology has been used as a powerful tool in the discovery of peptides capable of exhibiting specific affinity to various metals or metal ions. However, traditional phage display is mainly conducted in batch mode, resulting in only one equilibrium state hence low-efficiency selection. It is also unable to monitor the selection process in real time mode. In this study, phage display technique was incorporated with chromatography procedure with the use of a monolithic column, facilitating multiple phage-binding equilibrium states and online monitoring of the selection process in search of affinity peptides to Pb2+. In total, 17 candidate peptides were found and their specificity toward Pb2+ was further investigated with bead-based enzyme immunoassay (EIA). A highly specific Pb2+ binding peptide ThrAsnThrLeuSerAsnAsn (TNTLSNN) was obtained. Based on our knowledge, this is the first report on a new chromatographic biopanning method coupled with monolithic column for the selection of metal ion specific binding peptides. It is expected that this monolith-based chromatographic biopanning will provide a promising approach for a high throughput screening of affinity peptides cognitive of a wide range of target species. PMID:20709321

  8. Practical design of stepped columns

    OpenAIRE

    Girao Coelho, A.M.; Simao, P.D.; Bijlaard, F.S.K.

    2012-01-01

    This paper deals with buckling aspects of the design of stepped columns in heavy mill buildings. In these structures, columns have to carry significant axial loads that usually act eccentrically and strength reducing bending moments due to lateral loads. A simple physical model for buckling behaviour analysis is proposed and formulated using the differential equations of equilibrium. The exact solution of the governing equations is found by using symbolic computation. Effective buckling lengt...

  9. Application of a Modified Gas Chromatograph to Analyze Space Experiment Combustion Gases on Space Shuttle Mission STS-94

    Science.gov (United States)

    Coho, William K.; Weiland, Karen J.; VanZandt, David M.

    1998-01-01

    A space experiment designed to study the behavior of combustion without the gravitational effects of buoyancy was launched aboard the Space Shuttle Columbia on July 1, 1997. The space experiment, designated as Combustion Module-1 (CM-1), was one of several manifested on the Microgravity Sciences Laboratory - 1 (MSL-1) mission. The launch, designated STS-94, had the Spacelab Module as the payload, in which the MSL-1 experiments were conducted by the Shuttle crewmembers. CM-1 was designed to accommodate two different combustion experiments during MSL-1. One experiment, the Structure of Flame Balls at Low Lewis-number experiment (SOFBALL), required gas chromatography analysis to verify the composition of the known, premixed gases prior to combustion, and to determine the remaining reactant and the products resulting from the combustion process in microgravity. A commercial, off-the-shelf, dual-channel micro gas chromatograph was procured and modified to interface with the CM-1 Fluids Supply Package and the CM-1 Combustion Chamber, to accommodate two different carrier gases, each flowing through its own independent column module, to withstand the launch environment of the Space Shuttle, to accept Spacelab electrical power, and to meet the Spacelab flight requirements for electromagnetic interference (EMI) and offgassing. The GC data was down linked to the Marshall Space Flight Center for near-real time analysis, and stored on-orbit for post-flight analysis. The gas chromatograph operated successfully during the entire SOFBALL experiment and collected 309 runs. Because of the constraints imposed upon the gas chromatograph by the CM-1 hardware, system and operations, it was unable to measure the gases to the required accuracy. Future improvements to the system for a re-flight of the SOFBALL experiment are expected to enable the gas chromatograph to meet all the requirements.

  10. A Novel and Effective Chromatographic Approach to the Separation of Isoflavone Derivatives from Pueraria lobata

    Directory of Open Access Journals (Sweden)

    Jiang Fu

    2015-03-01

    Full Text Available A novel and effective chromatographic approach to the separation and purification of isoflavone compounds from Pueraria lobata is described. The method is based on flash chromatography (FC, coupled to preparative high performance liquid chromatography (prep-HPLC via a six-way valve. The FC step comprised tandem reversed phase columns, pre-packed with MCI gel (Mitsubishi Chemical Corp., Tokyo, Japan and C18 (Fuji Silysia Chemical Ltd, Osaka, Japan resin, respectively, and was designed to separate a crude Pueraria lobata extract into several preliminary fractions. Fractions containing the target compounds were then directly injected via the six-way valve into prep-HPLC columns, without further treatment, for final isolation and purification. Nine isoflavonoids were successfully isolated, three through an online mode and the other six through an offline mode. The purities of all compounds exceeded 95.0%, as determined by HPLC with an UV-vis photodiode array detector. The convenience, low solvent consumption, and time-saving advantages of this method offer an attractive and promising approach to the isolation of natural products.

  11. Simple gas chromatographic system for analysis of microbial respiratory gases

    Science.gov (United States)

    Carle, G. C.

    1972-01-01

    Dual column ambient temperature system, consisting of pair of capillary columns, microbead thermistor detector and micro gas-sampling valve, is used in remote life-detection equipment for space experiments. Performance outweighs advantage gained by utilizing single-column systems to reduce weight, conserve carrier gas and operate at lower power levels.

  12. Research on the separation properties of empty-column gas chromatography (EC-GC) and conditions for simulated distillation (SIMDIS)

    OpenAIRE

    Boczkaj, Grzegorz; Kamiński, Marian

    2013-01-01

    Previous studies have revealed it is possible to separate a high-boiling mixture by gas chromatography in empty fused-silica capillary tubing rather than in columns coated with stationary phase. Chromatographic separation occurs solely on the basis of the different boiling points of the substances separated. The high similarity of such separations to those in classic distillation seems advantageous when gas chromatography is used for simulated distillation. This paper presents results from fu...

  13. Temperature Effects on Retention and Separation of PAHs in Reversed-Phase Liquid Chromatography Using Columns Packed with Fully Porous and Core-Shell Particles

    OpenAIRE

    Christophe Waterlot; Anaïs Goulas

    2016-01-01

    Effects of temperature on the reversed-phase chromatographic behavior of PAHs were investigated on three columns. The first was the recent C18 column (250 mm × 4.6 mm) packed with 5 µm core-shell particles while the others were more conventional C18 columns (250 mm × 4.6 mm) packed with fully porous particles. Among the 16 PAHs studied, special attention has been paid to two pairs of PAHs, fluorene/acenaphthene and chrysene/benzo[a]anthracene, which often present coeluting problems. Due to th...

  14. Determination of Organic Acids in Apple and Cider by Liquid Chromatography with ordinary and narrow-bore columns. A Comparative Study

    OpenAIRE

    Blanco-Gomis, Domingo; Morán, M.J. (María); Gutiérrez, M.D. (María); Mangas, J.J. (Juan)

    2013-01-01

    Two narrow-bore columns packed with octadecylsilane of various particle sizes were used to compare their efficiency for the separation of organic acids in apple and cider with that of ordinary columns. The best simultaneous resolution of quinic, malic, shikimic, lactic, acetic, citric and succinic acid was accomplished by using a 100 × 2.1 mm ID, 3-μm Spherisorb ODS-2 column and a phosphate buffer as the mobile phase. This chromatographic system provided a separation efficiency comparable to ...

  15. Modeling of extraction chromatographic reprocessing-partitioning processes

    International Nuclear Information System (INIS)

    A numerical code was developed to simulate extraction chromatographic reprocessing-partitioning processes. The mathematical model considers axial dispersion in the fixed bed and the two-films approach to represent the mass transfer kinetics. Several correlations to estimate distribution coefficients were used to simulate different extraction systems. The mass transfer coefficients were obtained fitting simulated curves with the experimental data. Simulations of Uranium - Plutonium - HNO3 - fission products - tri-n-butyl phosphate (TBP) extraction chromatographic system were carried out and compared with laboratory experiments using actual irradiated uranium target solution as tracer. The separation and recovery of lanthanides and actinides elements, from simulated raffinate solution containing Am and Eu tracers, in the octylphenyl-N,Ndiisobutylcarbamoylmetylphosphine oxide (CMPO) - tri-n-butyl phosphate (TBP) - HNO3 extraction chromatographic system, was simulated too. The simulated elution profiles were in agreement with the experimental data obtained. (author)

  16. Physicochemical and chromatographic method of characterization of Matricaria recutita tinctures

    Directory of Open Access Journals (Sweden)

    Jonathan Parra

    2016-02-01

    Full Text Available Context: The pharmacological activity of medicinal products containing plant materials depends on their specific components. However, these components are not characterized in their entirety in all cases. Therefore, manufacturing processes must be duly characterized and validated. Aims: To characterize a chamomile (Matricaria recutita tincture through chemometric analysis of chromatographic data in order to establish quality parameters for its production. Methods: Various chamomile tinctures were manufactured and the precision and robustness of the production process for each was verified. The physicochemical properties of the tinctures were characterized and their chromatographic digital fingerprints analysed through chemometric methods. Results: A good correlation between the physicochemical characterization and the chromatographic analysis was demonstrated. The preparation methodology was proved to be repeatable as long as the source of the plant material is not altered. Conclusions: The principal component multivariate analysis of chromatograms was a helpful and simple tool for the characterization and traceability of the production method.

  17. Analysis of Aflatoxin B1 in Iranian Foods Using HPLC and a Monolithic Column and Estimation of its Dietary Intake

    OpenAIRE

    Yazdanpanah, Hassan; Zarghi, Afshin; Shafaati, Ali Reza; FOROUTAN, SEYED MOHSEN; Aboul-Fathi, Farshid; Khoddam, Arash; Nazari, Firoozeh; Shaki, Fatemeh

    2013-01-01

    A high performance liquid chromatographic method was developed for determination of aflatoxin B1 (AFB1) in foods using a monolithic column with sample clean up on an immunoaffinity column. The method was validated for analysis of AFB1 in rice, bread, puffed corn snack, wheat flour and peanut samples. The average recoveries for AFB1 in different foods ranged from 94.4 to 102.5% with the coefficient of variation lower than 10% for all foods. Limit of detection was 0.01 ng/g. A survey of AFB1 wa...

  18. QbD-oriented development and validation of a bioanalytical method for nevirapine with enhanced liquid-liquid extraction and chromatographic separation.

    Science.gov (United States)

    Beg, Sarwar; Chaudhary, Vandna; Sharma, Gajanand; Garg, Babita; Panda, Sagar Suman; Singh, Bhupinder

    2016-06-01

    The present studies describe the systematic quality by design (QbD)-oriented development and validation of a simple, rapid, sensitive and cost-effective reversed-phase HPLC bioanalytical method for nevirapine in rat plasma. Chromatographic separation was carried out on a C18 column using isocratic 68:9:23% v/v elution of methanol, acetonitrile and water (pH 3, adjusted by orthophosphoric acid) at a flow rate of 1.0 mL/min using UV detection at 230 nm. A Box-Behnken design was applied for chromatographic method optimization taking mobile phase ratio, pH and flow rate as the critical method parameters (CMPs) from screening studies. Peak area, retention time, theoretical plates and peak tailing were measured as the critical analytical attributes (CAAs). Further, the bioanalytical liquid-liquid extraction process was optimized using an optimal design by selecting extraction time, centrifugation speed and temperature as the CMPs for percentage recovery of nevirapine as the CAA. The search for an optimum chromatographic solution was conducted through numerical desirability function. Validation studies performed as per the US Food and Drug Administration requirements revealed results within the acceptance limit. In a nutshell, the studies successfully demonstrate the utility of analytical QbD approach for the rational development of a bioanalytical method with enhanced chromatographic separation and recovery of nevirapine in rat plasma. Copyright © 2015 John Wiley & Sons, Ltd. PMID:26352459

  19. Development of Chromatographic Fingerprints of Eurycoma longifolia (Tongkat Ali) Roots Using Online Solid Phase Extraction-Liquid Chromatography (SPE-LC).

    Science.gov (United States)

    Zaini, Nor Nasriah; Osman, Rozita; Juahir, Hafizan; Saim, Norashikin

    2016-01-01

    E. longifolia is attracting interest due to its pharmacological properties and pro-vitality effects. In this study, an online SPE-LC approach using polystyrene divinyl benzene (PSDVB) and C18 columns was developed in obtaining chromatographic fingerprints of E. longifolia. E. longifolia root samples were extracted using pressurized liquid extraction (PLE) technique prior to online SPE-LC. The effects of mobile phase compositions and column switching time on the chromatographic fingerprint were optimized. Validation of the developed method was studied based on eurycomanone. Linearity was in the range of 5 to 50 µg∙mL(-1) (r² = 0.997) with 3.2% relative standard deviation of peak area. The developed method was used to analyze 14 E. longifolia root samples and 10 products (capsules). Selected chemometric techniques: cluster analysis (CA), discriminant analysis (DA), and principal component analysis (PCA) were applied to the fingerprint datasets of 37 selected peaks to evaluate the ability of the chromatographic fingerprint in classifying quality of E. longifolia. Three groups were obtained using CA. DA yielded 100% correlation coefficient with 19 discriminant compounds. Using PCA, E. longifolia root samples were clearly discriminated from the products. This study showed that the developed online SPE-LC method was able to provide comprehensive evaluation of E. longifolia samples for quality control purposes. PMID:27144555

  20. Partial least squares model and design of experiments toward the analysis of the metabolome of Jatropha gossypifolia leaves: Extraction and chromatographic fingerprint optimization.

    Science.gov (United States)

    Pilon, Alan Cesar; Carnevale Neto, Fausto; Freire, Rafael Teixeira; Cardoso, Patrícia; Carneiro, Renato Lajarim; Da Silva Bolzani, Vanderlan; Castro-Gamboa, Ian

    2016-03-01

    A major challenge in metabolomic studies is how to extract and analyze an entire metabolome. So far, no single method was able to clearly complete this task in an efficient and reproducible way. In this work we proposed a sequential strategy for the extraction and chromatographic separation of metabolites from leaves Jatropha gossypifolia using a design of experiments and partial least square model. The effect of 14 different solvents on extraction process was evaluated and an optimized separation condition on liquid chromatography was estimated considering mobile phase composition and analysis time. The initial conditions of extraction using methanol and separation in 30 min between 5 and 100% water/methanol (1:1 v/v) with 0.1% of acetic acid, 20 μL sample volume, 3.0 mL min(-1) flow rate and 25°C column temperature led to 107 chromatographic peaks. After the optimization strategy using i-propanol/chloroform (1:1 v/v) for extraction, linear gradient elution of 60 min between 5 and 100% water/(acetonitrile/methanol 68:32 v/v with 0.1% of acetic acid), 30 μL sample volume, 2.0 mL min(-1) flow rate, and 30°C column temperature, we detected 140 chromatographic peaks, 30.84% more peaks compared to initial method. This is a reliable strategy using a limited number of experiments for metabolomics protocols. PMID:26757030

  1. Extraction chromatographic separation of minor actinides from PUREX high-level wastes using CMPO

    International Nuclear Information System (INIS)

    An extraction chromatographic technique using octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO) adsorbed on chromosorb-102 (CAC) has been tested as an alternative to the TRUEX solvent extraction process, where CMPO has been used as the extracting agent to recover minor actinides from high-activity waste (HAW) solutions of PUREX origin. The batchwise uptake behavior of U(VI), Pu(IV), Am(III), Eu(III), Zr(IV), Fe(III), Ru(III), and TcO4- from a nitric acid medium by CAC has been studied. The uptake of actinides and lanthanides are higher than those of other fission products and inert materials. The batchwise loading experiments in the presence of Nd(III)/U(VI) have shown that at lower concentrations of these metal ions, the uptake of Pu(IV), U(VI), and Am(III) are reasonably high. Studies on loading of Nd(III), U(VI), and Pu(IV) on a column containing 1.7 g of CAC have shown that Nd(III) (30 mg) and U(VI) (90 mg) could be loaded, while Pu(IV) (∼0.6) was loaded on a small column containing 100 mg of CAC without any break-through. Further, a synthetic HAW solution as such and the actual PUREX HAW solution, after depleting the uranium content by a 30% tributyl-phosphate contact, were loaded on a CAC column. The effluents did not contain any alpha activity above the background level. The activities could subsequently be eluted with 0.0.4 M HNO3 (americium and rare earths), 0.01 M oxalic acid (plutonium), and 0.25 M Na2CO3 [U(VI)]. The recoveries of these metal ions were found to be >99%

  2. Application of extraction chromatographic technique in the recovery of actinides from Purex waste solutions using CMPO

    International Nuclear Information System (INIS)

    Extraction chromatographic technique using octyl(phenyl)-N,N-diisobutylcarbomoylmethylphosphine oxide (CMPO) adsorbed on chromosorb-102 (CAC) has been developed as a potential alternative to the Truex process, where CMPO has been deployed as the extracting agent to recover minor actinides from the high active waste (HAW) solution of Purex origin. In this connection, the batch-wise uptake behaviour of U(VI), Pu(VI), Am(III), Eu(III), Zr(IV), Fe(III), Ru(III) and TcO4 from nitric acid medium by CAC has been studied. The uptake of actinides and lanthanides are higher than those of other fission products and inert materials. The batch-wise loading experiments in presence of Nd(III)/U(VI) have shown that at lower concentration of these metal ions, the uptake of Pu(IV), U(VI) and Am(III) are reasonably high. Studies on loading of Nd(III), U(VI) and Pu(IV) on a column containing 1.7 g CAC have shown that Nd(III) (30 mg) and U(VI) (90 mg) could be loaded, while Pu(IV) (∼0.6 mg) was loaded on a small column containing 100 mg CAC without any breakthrough. Further, a synthetic HAW solution and the actual Purex HAW solution were loaded on a CAC column. The effluents did not contain any alpha activity above the background level. The activities could subsequently be eluted with 0.04 M HNO3 (Am and RE), 0.01 M oxalic acid (Pu) and 0.25 MNa2CO3 solution (U(VI)). The recoveries of these metal ions were found to be > 99%. The eluted Am and rare earth fraction is an important source for 147Pm. This process is amenable for further scaling up. (author). 17 refs., 5 figs., 8 tabs

  3. NOx retention in scrubbing column

    International Nuclear Information System (INIS)

    During the UO2 dissolution in nitric acid, some different species of NOx are released. The off gas can either be refluxed to the dissolver or be released and retained on special columns. The final composition of the solution is the main parameter to take in account. A process for nitrous gases retention using scubber columns containing H2O or diluted HNO3 is presented. Chemiluminescence measurement was employed to NOx evalution before and after scrubbing. Gas flow, temperature, residence time are the main parameters considered in this paper. For the dissolution of 100g UO2 in 8M nitric acid, a 6NL/h O2 flow was the best condition for the NO/NO2 oxidation with maximum adsorption in the scrubber columns. (author)

  4. Micro-fabricated semi-packed column for gas chromatography by using functionalized parylene as a stationary phase

    International Nuclear Information System (INIS)

    The conformal coating of effective stationary phases onto micro-fabricated columns having complex geometries such as semi-packed columns poses a real challenge. Here, we report for the first time the conformal coating of a semi-packed column with amino-functionalized parylene diX-AM (poly-aminomethyl-[2,2]-paracyclophane), which was found to be an effective stationary-phase material for the chromatography of short-retention-time compounds. A semi-packed column (consisting of a zigzag array of 30 µm square micro-pillars in a 1.0 m long, 180 µm wide and 230 µm deep channel) and an open tubular column (1.0 m long, 160 µm wide and 230 µm deep channel) used for comparison purposes were micro-fabricated on silicon that was subsequently coated with diX-AM parylene and thermally bonded. The chromatograms recorded on a commercial gas chromatograph demonstrated the usefulness of the conformal diX-AM coating as a stationary phase for semi-packed columns. The separation efficiency of the semi-packed column was found to be more than ten times that of the open tubular column

  5. Non-targeted chromatographic analyses of cuticular wax flavonoids from Physalis alkekengi L.

    Science.gov (United States)

    Kranjc, Eva; Albreht, Alen; Vovk, Irena; Makuc, Damjan; Plavec, Janez

    2016-03-11

    Since Chinese lantern (Physalis alkekengi L.) represents a rich source of various bioactive secondary metabolites, there is an urge for its detailed characterization. Non-polar flavonoid aglycones represent one of the few bioactive species found in plant's cuticular waxes. The separation of flavonoids is already extensively covered in the literature, but methods dedicated to separation and identification of methylated flavonoids are rather scarce. In the present study a non-targeted approach for the separation, isolation and identification of methylated flavonoids present in P. alkekengi L. var. franchetii cuticular waxes was established. A rapid and simple separation on HPTLC silica gel was developed for preliminary screening of flavonoids. Fast HPLC-UV-MS(n) and HPLC-UV methods using a C6-Phenyl and a C18 stationary phase were also developed, respectively. In both cases, the right combination of temperature and tetrahydrofuran, as a mobile phase modifier, were shown to be crucial for a baseline separation of all studied compounds. By employing a semi-preparative analog of the C18 column, a simultaneous isolation of pure unknown analytes was achieved. Using these developed methods in combination with NMR, four 3-O-methylated flavonols were detected and identified in P. alkekengi L. var. franchetii cuticular waxes: myricetin 3,7,3'-trimethyl ether, quercetin 3,7-dimethyl ether, myricetin 3,7,3',5'-tetramethyl ether and quercetin 3,7,3'-trimethyl ether. Moreover, the simple and fast isocratic HPLC-UV-MS(n) method (under 8min) should prove useful in quality control of P. alkekengi L. var. franchetii by enabling chromatographic fingerprinting of external methylated flavonols. Finally, a rationale for the mechanism of separation of these metabolites by HPLC is also given, which establishes a foundation for future development of chromatographic methods for methylated flavonols and related compounds. PMID:26875116

  6. Quantitative analysis of Glycyrrhizic acid from a polyherbal preparation using liquid chromatographic technique

    Directory of Open Access Journals (Sweden)

    Amit K De

    2012-01-01

    Full Text Available Glycyrrhizic acid has been used in Indian traditional medicine for ages. It is obtained from the root extract of Glycyrrhizaglabra. There is seasonal variation of Glycyrrhizic acid content in the roots of the plant. So a proper method for quantification of the same is necessary from the polyherbal preparation available in the market. A simple, rapid, sensitive and specific reverse phase high performance liquid chromatographic method have been developed for the quantitative estimation of glycyrrhizic acid from polyherbal preparation containing aqueous root extract of Glycyrrhizaglabra using a photodiode array detector. The identity confirmation was carried out using mass spectrometry. Baseline resolution of the glycyrrhizic acid peak was achieved on a reverse phase C18 column (125 mm × 4.0 mm, 5 μ using an isocratic mobile phase consisting of 5.3 mM phosphate buffer and acetonitrile in the ratio 65:35 v/v. Chromatograms were monitored at 252 nm.5.3 mM phosphate buffer was replaced with 0.5mM ammonium acetate buffer in the mobile phase when MS detector was used. The method was found to be linear in the concentration range of 12.4 to124 μg/ml with a correlation co-efficient of 0.999. The limit of detection and the limit of quantitation were 3.08 μg/ml and 10.27 μg/ml respectively. The average recovery from three spike levels was 99.93 ± 0.26%. Identity confirmation of the chromatographic peak was achieved by electrospray ionization mass spectrometry and similar molecular ion peak was obtained for both sample and standard. The developed method is suitable for the routine analysis, stability testing and assay of glycyrrhizic acid from polyherbal preparations containing aqueous extracts of Glycyrrhizaglabra.

  7. Quantitative analysis of Glycyrrhizic acid from a polyherbal preparation using liquid chromatographic technique.

    Directory of Open Access Journals (Sweden)

    Amit K De

    2012-01-01

    Full Text Available Glycyrrhizic acid has been used in Indian traditional medicine for ages. It is obtained from the root extract of Glycyrrhizaglabra. There is seasonal variation of Glycyrrhizic acid content in the roots of the plant. So a proper method for quantification of the same is necessary from the polyherbal preparation available in the market. A simple, rapid, sensitive and specific reverse phase high performance liquid chromatographic method have been developed for the quantitative estimation of glycyrrhizic acid from polyherbal preparation containing aqueous root extract of Glycyrrhizaglabra using a photodiode array detector. The identity confirmation was carried out using mass spectrometry. Baseline resolution of the glycyrrhizic acid peak was achieved on a reverse phase C18 column (125 mm × 4.0 mm, 5 μ using an isocratic mobile phase consisting of 5.3 mM phosphate buffer and acetonitrile in the ratio 65:35 v/v. Chromatograms were monitored at 252 nm.5.3 mM phosphate buffer was replaced with 0.5mM ammonium acetate buffer in the mobile phase when MS detector was used. The method was found to be linear in the concentration range of 12.4 to124 μg/ml with a correlation co-efficient of 0.999. The limit of detection and the limit of quantitation were 3.08 μg/ml and 10.27 μg/ml respectively. The average recovery from three spike levels was 99.93 ± 0.26%. Identity confirmation of the chromatographic peak was achieved by electrospray ionization mass spectrometry and similar molecular ion peak was obtained for both sample and standard. The developed method is suitable for the routine analysis, stability testing and assay of glycyrrhizic acid from polyherbal preparations containing aqueous extracts of Glycyrrhizaglabra.

  8. Chromatographic fingerprints analysis for evaluation of Ginkgo Biloba products

    Science.gov (United States)

    The leaf extract of Ginkgo biloba has purported value for improving mental capacities in Alzheimer’s patients. The flavonoids and the terpene lactones are considered to be the two main active components that influence human health. This paper compared an LC/UV chromatographic fingerprint method wi...

  9. Chromatographic profiles of Ginkgo biloba leaves and selected products

    Science.gov (United States)

    An LC-DAD-ESI/MS method was developed to obtain chromatographic profiles for the flavonoids and terpene lactones of Ginkgo biloba leaves and selected G. biloba products. The method was used to identify 46 glycosylated flavonols and flavones, 3 free flavonol aglycones, catechin, 10 biflavones, a dihy...

  10. Confocal Raman microscopy of protein adsorbed in chromatographic particles.

    Science.gov (United States)

    Xiao, Yuewu; Stone, Thomas; Bell, David; Gillespie, Christopher; Portoles, Marta

    2012-09-01

    Confocal Raman microscopy is a nondestructive analytical technique that combines the chemical information from vibrational spectroscopy with the spatial resolution of confocal microscopy. It was applied, for the first time, to measure conformation and distribution of protein adsorbed in wetted chromatographic particles. Monoclonal antibody was loaded into the Fractogel EMD SO(3) (M) cation exchanger at 2 mS/cm or 10 mS/cm. Amide I and III frequencies in the Raman spectrum of the adsorbed protein suggest that there are no detectable changes of the original β-sheet conformation in the chromatographic particles. Protein depth profile measurements indicate that, when the conductivity is increased from 2 mS/cm to 10 mS/cm, there is a change in mass transport mechanism for protein adsorption, from the shrinking-core model to the homogeneous-diffusion model. In this study, the use of confocal Raman microscopy to measure protein distribution in chromatographic particles fundamentally agrees with previous confocal laser scanning microscopic investigations, but confocal Raman spectroscopy enjoys additional advantages: use of unlabeled protein to eliminate fluorescent labeling, ability for characterization of protein secondary structure, and ability for spectral normalization to provide a nondestructive experimental approach to correct light attenuation effects caused by refractive index (RI) mismatching in semiopaque chromatographic particles. PMID:22803776

  11. Optimizing Chromatographic Separation: An Experiment Using an HPLC Simulator

    Science.gov (United States)

    Shalliker, R. A.; Kayillo, S.; Dennis, G. R.

    2008-01-01

    Optimization of a chromatographic separation within the time constraints of a laboratory session is practically impossible. However, by employing a HPLC simulator, experiments can be designed that allow students to develop an appreciation of the complexities involved in optimization procedures. In the present exercise, a HPLC simulator from "JCE…

  12. [A gas chromatographic method for determining acetaldehyde in cadaver blood].

    Science.gov (United States)

    Savich, V I; Valladares, Kh A; Gusakov, Iu A; Skachko, Z M

    1990-01-01

    Gas-chromatographic method of acetaldehyde detection in blood of subjects who died of alcoholic intoxication is suggested. Method is simple, does not require additional expenses, can be readily used in medicolegal practice and in difficult cases it may help the expert to make an objective conclusion on the cause of death. PMID:2087747

  13. Bioanalytical method transfer considerations of chromatographic-based assays.

    Science.gov (United States)

    Williard, Clark V

    2016-07-01

    Bioanalysis is an important part of the modern drug development process. The business practice of outsourcing and transferring bioanalytical methods from laboratory to laboratory has increasingly become a crucial strategy for successful and efficient delivery of therapies to the market. This chapter discusses important considerations when transferring various types of chromatographic-based assays in today's pharmaceutical research and development environment. PMID:27277876

  14. Physicochemical and chromatographic method of characterization of Matricaria recutita tinctures

    OpenAIRE

    Jonathan Parra; Pedro M. García-Barrantes; Gerardo Rodríguez; Beatriz Badilla

    2016-01-01

    Context: The pharmacological activity of medicinal products containing plant materials depends on their specific components. However, these components are not characterized in their entirety in all cases. Therefore, manufacturing processes must be duly characterized and validated. Aims: To characterize a chamomile (Matricaria recutita) tincture through chemometric analysis of chromatographic data in order to establish quality parameters for its production. Methods: Various chamomile t...

  15. Column Holdup Formula of Soil Solute Transport

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    The shortcomings of the present two formulae for describing column holdup are analyzed and deductions are made to find a new formula. The column holdup, Hw, described by the new formula is dimensional,and related to soil solute transport kinesis and column physical properties. Compared with the other two column holdups, Hw is feasible to describe dimensional column holdup during solute transport process. The relationships between Hw and retardation factor, R, in different solute transport boundary conditions are established.

  16. Relationship between chromatographic resolution and amide structure of chiral 2-hydroxy acids as O-(-)-menthoxycarbonylated diastereomeric derivatives for enantiomeric separation on achiral gas chromatography.

    Science.gov (United States)

    Cha, Eunju; Kim, Sohee; Lee, Kang Mi; Kim, Ho Jun; Kim, Ki Hun; Kwon, Oh-Seung; Park, Ki Duk; Lee, Jaeick

    2016-02-15

    The relationship between chromatographic resolution and amide structure of chiral 2-hydroxy acids as O-(-)-menthoxycarbonylated diastereomeric derivatives on achiral gas chromatography was investigated to elucidate the best diastereomeric conformation for enantiomeric separation of chiral 2-hydroxy acids. Thirteen chiral 2-hydroxy acids were converted into nine different diastereomeric O-(-)-menthoxycarbonylated amide derivatives using the primary, secondary and cyclic amines to achieve complete enantiomeric separation through an achiral column. Each enantiomeric pair of 2-hydroxy acids as O-(-)-menthoxycarbonylated tert-butylamide derivatives was resolved on both the DB-5 and DB-17 columns with resolution factors ranging from 1.7 to 4.8 and 1.7 to 3.4, respectively. The results revealed that the structure of the amide moiety is shown to significantly affect chromatographic resolution. In addition, O-(-)-menthoxycarbonylated tert-butylamide derivatives were shown to be the best diastereomeric conformations for enantiomeric separation of 2-hydroxy acids. When comparing with our previous O-trifluoroacetylated(-)-menthyl ester derivatization method, the present results suggested that size differences between groups attached to the chiral center and conformational rigidity can have stronger effects on resolution than the distance between chiral centers. The elution of R- and S-stereoisomers was affected by the class of amine; i.e., primary, secondary, or cyclic, regardless of the substituents on the amine group, the structure of the 2-hydroxy acid, and the polarity of the column. PMID:26800225

  17. Chromatographic purification of neutron capture molybdenum-99 from cross-contaminant radionuclides

    International Nuclear Information System (INIS)

    Technetium-99m is called the work horse, for many reasons, in nuclear medicine diagnostic purposes. It is produced as the β-decay of 99Mo radionuclide. Molybdenum-99 gel type generators are considered as a suitable alternative of the conventional chromatographic alumina columns loaded with fission molybdenum-99. 99Mo neutron-capture is cross-contaminated with radionuclides originated from activation of chemical impurities in the Mo target such 60C0, 65Zn, 95Zr, 175Hf, 181Hf, 86Rb, 134Cs, 141Ce, 152Eu, 140La,51Cr, 124Sb,46Sc, 54Mn, 59Fe and / or fast neutrons interactions with the stable isotopes of molybdenum such as 92mNb, 95Nb and 95Zr. To prevent contamination of the eluted 99mTc, successive purification methods were made. After complete dissolution of the irradiated target wrapped with thin Al foil in 5 M NaOH solution, hydrogen peroxide was added to start precipitation of Fe(OH)3. The formed Fe (III) minerals allow complete elimination of some radio contaminants from the molybdate solute such as 152Eu, 140La,141Ce, 45Mn and 92mNb in addition to partial elimination of 46Sc, 60Co and 59Fe radionuclides. The remaining supernatant was acidified by concentrated nitric acid to ph 9.5 for precipitation of Al(OH)3 with complete elimination of radio contaminants such as 95Zr 175Hf, 181Hf, 65Zn, 124Sb, 51Cr, 46Sc, 60Co and 59Fe. 134Cs and 86Rb radionuclides were not affected by precipitation of Fe(OH)3 or Al(OH)3. Chromatographic column of potassium nickel hexacyanoferrate (II) (KNHCF) has high affinity towards elimination of 134Cs and 86Rb radionuclides. Highly pure molybdate-99Mo solution was processed for preparation of zirconium molybdate gel generator with 99mTc eluate of high radionuclidic, radiochemical and chemical purity suitable for use in medical purposes.

  18. Simultaneous determination of iodide and iodate in povidone iodine solution by ion chromatography with homemade and exchange capacity controllable columns and column-switching technique.

    Science.gov (United States)

    Huang, Zhongping; Zhu, Zuoyi; Subhani, Qamar; Yan, Wenwu; Guo, Weiqiang; Zhu, Yan

    2012-08-17

    A simple ion chromatographic method for simultaneous detection of iodide and iodate in a single running was proposed, with columns packed with homemade functionalized polystyrene-divinylbenzene (PS-DVB) resins and column-switching technique. Homemade resins were functionalized with controllable amounts of quaternary ammonium groups. The low-capacity anion-exchange column and high-capacity anion-exchange column were prepared, due to the resins having different exchange capacities. With this method, iodide and iodate in povidone iodine solution were detected simultaneously in a short time with iodide being eluted off first. A series of standard solutions consisting of target anions of various concentrations from 0.01 mg/L to 100 mg/L were analyzed. Each anion exhibited satisfactory linearity, with correlation coefficient r ≥ 0.9990. The detection limits (LODs) for iodide and iodate obtained by injecting 100 μL of sample were 5.66 and 14.83 μg/L (S/N=3), respectively. A spiking study was performed with satisfactory recoveries between 101.2% and 100.6% for iodide and iodate. PMID:22771256

  19. Industry perspective on the validation of column-based separation processes for the purification of proteins. Parenteral Drug Association.

    Science.gov (United States)

    1992-01-01

    Validation of column-based separations is necessary to ensure the quality and safety of protein and peptide products produced by rDNA, peptide synthesis, and hybridoma technologies. Process validation for column-based separations includes qualification of raw materials, equipment, and the purification process. Combined with in-process control and quality control of the final product, column validation ensures that a uniform product is produced consistently from batch to batch. In the best case, validation is designed into the process. During process design, techniques are selected which can remove impurities and contaminants. Equipment and chromatographic media which can perform reproducibly are selected. Column performance standards, cleaning and regeneration routines, and column life should be considered as early as possible. Clearance studies should be planned and implemented to ensure that a product is produced with the requisite purity. There are no explicit rules for process validation of column-based separation processes. This document is intended to serve as a starting point for those needing to validate column-based separation processes. PMID:1522447

  20. [Rapid determination of trace iodate using monolithic column ion-pair chromatography coupled with direct conductivity detection].

    Science.gov (United States)

    Liu, Yuzhen; Yu, Hong; Li, Siwen

    2011-10-01

    A method was developed on a monolithic column for the fast determination of trace iodate (IO(3)- ) by ion-pair chromatography with direct conductivity detection. The analytes were separated using a mobile phase of tetrabutylammonium hydroxide (TBA)-phthalic acid-acetonitrile on a reversed-phase silica-based monolithic column. The effects of eluent, flow rate and column temperature on the retention of iodate were investigated. The optimized chromatographic conditions for the determination of the anion were as follows: 0. 25 mmol/L TBA-0. 18 mmol/L phthalic acid-3% acetonitrile (pH 5.5) as mobile phase, a flow rate of 4.0 mL/min and a column temperature of 30 degrees C. Under the optimal conditions, retention time of iodate was less than 0. 5 min and the baseline separation of iodate was achieved without any interference by other anions (Cl-, NO , SO4(2)-, I- ). The detection limit (S/N= 3) was 0.36 mg/L for IO(3)- . Relative standard deviation (RSD, n = 5) of chromatographic peak area and retention time were 0. 35% and 0. 28%, respectively. The proposed method was applied to the determination of trace iodate in iodized medicine. The spiked recovery of iodate was 96. 4%. The method is rapid, simple, accurate, reliable, and practical. PMID:22268363

  1. Modeling of column apparatus processes

    CERN Document Server

    Boyadjiev, Christo; Boyadjiev, Boyan; Popova-Krumova, Petya

    2016-01-01

    This book presents a new approach for the modeling of chemical and interphase mass transfer processes in industrial column apparatuses, using convection-diffusion and average-concentration models. The convection-diffusion type models are used for a qualitative analysis of the processes and to assess the main, small and slight physical effects, and then reject the slight effects. As a result, the process mechanism can be identified. It also introduces average concentration models for quantitative analysis, which use the average values of the velocity and concentration over the cross-sectional area of the column. The new models are used to analyze different processes (simple and complex chemical reactions, absorption, adsorption and catalytic reactions), and make it possible to model the processes of gas purification with sulfur dioxide, which form the basis of several patents.

  2. Metal-Organic Framework Thin Films as Stationary Phases in Microfabricated Gas-Chromatography Columns.

    Energy Technology Data Exchange (ETDEWEB)

    Read, Douglas [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Sillerud, Colin Halliday [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2016-01-01

    The overarching goal of this project is to integrate Sandia's microfabricated gas-chromatography ( GC) columns with a stationary phase material that is capable of retaining high-volatility chemicals and permanent gases. The successful integration of such a material with GCs would dramatically expand the repertoire of detectable compounds for Sandia's various microanalysis systems. One such promising class of candidate materials is metal-organic frameworks (MOFs). In this report we detail our methods for controlled deposition of HKUST-1 MOF stationary phases within GC columns. We demonstrate: the chromatographic separation of natural gas; a method for determining MOF film thickness from chromatography alone; and the first-reported GC x GC separation of natural gas -- in general -- let alone for two disparate MOF stationary phases. In addition we determine the fundamental thermodynamic constant for mass sorption, the partition coefficient, for HKUST-1 and several light hydrocarbons and select toxic industrial chemicals.

  3. SPEEDUPtrademark ion exchange column model

    International Nuclear Information System (INIS)

    A transient model to describe the process of loading a solute onto the granular fixed bed in an ion exchange (IX) column has been developed using the SpeedUptrademark software package. SpeedUp offers the advantage of smooth integration into other existing SpeedUp flowsheet models. The mathematical algorithm of a porous particle diffusion model was adopted to account for convection, axial dispersion, film mass transfer, and pore diffusion. The method of orthogonal collocation on finite elements was employed to solve the governing transport equations. The model allows the use of a non-linear Langmuir isotherm based on an effective binary ionic exchange process. The SpeedUp column model was tested by comparing to the analytical solutions of three transport problems from the ion exchange literature. In addition, a sample calculation of a train of three crystalline silicotitanate (CST) IX columns in series was made using both the SpeedUp model and Purdue University's VERSE-LC code. All test cases showed excellent agreement between the SpeedUp model results and the test data. The model can be readily used for SuperLigtrademark ion exchange resins, once the experimental data are complete

  4. Simultaneous high performance liquid chromatographic determination of vanadium, nickel, iron and copper in crude petroleum oils using bis(acetylpivalylmethane)ethylenediimine as a complexing reagent.

    Science.gov (United States)

    Khuhawar, M Y; Lanjwani, S N

    1996-05-01

    A method is described for the simultaneous high performance liquid chromatographic (HPLC) determination of copper, iron, nickel and vanadium, based on complexation of analytes by bis(acetylpivalylmethane)ethylenediimine (H(2)APM(2)en) followed by solvent extraction and HPLC separation on a reversed-phase. C-18, 5 microm column with UV detection at 260 nm. The method has been applied to the determination of metals in crude petroleum oils collected from the South Indus Basin oil fields. The results obtained are compared with those obtained by flame atomic absorption spectrometry. PMID:18966546

  5. Determination of Trace Amount of Polycyclic Aromatic Hydrocarbons in Urban Sewage by Solid-phase Extraction Coupled with High Performance Liquid Chromatograph

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    [Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From the aspects of solid-phase extraction column,elution solvent,elution volume,elution speed and so forth,the test conditions of SPE-HPLC method were optimized,and trace amount of PAHs in urban sewage was determined.[Result] The optimized solid-phase extraction conditions were SUPELCLEAN LC-18 so...

  6. A novel molecular distance edge vector as applied to chemical modeling of quantitative structure-retention relationships: Various gas chromatographic retention behaviors of polychlorinated dibenzo-furans on different polarity-varying stationary phases

    Institute of Scientific and Technical Information of China (English)

    DENG Hong; HUANG Ping; HU Yinyu; YE Nancy; LI Zhiliang

    2005-01-01

    Based on the identical group as a pseudo atom instead of a typical atom, a novel modified molecular distance-edge (MDE) vector μ was developed in our laboratory to characterize chemical structure of polychlorinated dibenzofurans (PCDFs) congeners and/or isomers. Quantitative structure-retention relationships (QSRRs) between the new VMDE parameters and gas chromatographic (GC) retention behavior of PCDFs were then generated by multiple linear regression (MLR) method for non-polar, moderately polar, and polar stationary phases. Four excellent models with high correlation coefficients, R=0.984-0.995, were proposed for non-polar columns (DB-5, SE-54, OV-101). For the moderately polar columns (OV-1701), the correlation coefficient of the developed good model is only 0.958. For the polar columns (SP-2300), the QSRR model is poor with R=0.884. Then cross validation with leave-one out of procedure (CV) is performed in high correlation with the non-polar (Rcv=992-0.974) and weakly polar (Rcv=921) columns and in little correlation (Rcv=0.834) with the polar columns. These results show that the new μ vector is suitable for describing the retention behaviors of PCDFs on non-polar and moderately polar stationary phases and not for the various gas chromatographic retention behaviors of PCDFs on the different polarity-varying stationary phases.

  7. Development and Validation of Liquid Chromatographic Method for Estimation of Naringin in Nanoformulation

    Directory of Open Access Journals (Sweden)

    Kranti P. Musmade

    2014-01-01

    Full Text Available A simple, precise, accurate, rapid, and sensitive reverse phase high performance liquid chromatography (RP-HPLC method with UV detection has been developed and validated for quantification of naringin (NAR in novel pharmaceutical formulation. NAR is a polyphenolic flavonoid present in most of the citrus plants having variety of pharmacological activities. Method optimization was carried out by considering the various parameters such as effect of pH and column. The analyte was separated by employing a C18 (250.0 × 4.6 mm, 5 μm column at ambient temperature in isocratic conditions using phosphate buffer pH 3.5: acetonitrile (75 : 25% v/v as mobile phase pumped at a flow rate of 1.0 mL/min. UV detection was carried out at 282 nm. The developed method was validated according to ICH guidelines Q2(R1. The method was found to be precise and accurate on statistical evaluation with a linearity range of 0.1 to 20.0 μg/mL for NAR. The intra- and interday precision studies showed good reproducibility with coefficients of variation (CV less than 1.0%. The mean recovery of NAR was found to be 99.33 ± 0.16%. The proposed method was found to be highly accurate, sensitive, and robust. The proposed liquid chromatographic method was successfully employed for the routine analysis of said compound in developed novel nanopharmaceuticals. The presence of excipients did not show any interference on the determination of NAR, indicating method specificity.

  8. Thin Layer Chromatographic Analysis of Beta-Lactam Antibiotics

    Directory of Open Access Journals (Sweden)

    Gabriel Hancu

    2013-08-01

    Full Text Available Purpose: The paper describes some thin layer chromatographic procedures that allow simple and rapid separation and identification of penicillins and cephalosporins from complex mixtures. Methods: Using silicagel GF254 as stationary phase and selecting different mobile phases we succeeded in the separation of the studied beta-lactamins. Our aim was not only to develop a simple, rapid and efficient method for their separation but also the optimization of the analytical conditions. Results: No system will separate all the beta-lactams, but they could be identified when supplementary information is used from color reactions and/or by using additional chromatographic systems. Conclusions: The right combination of solvent system and detection method allows the identification of the studied penicillins and cephalosporins and can be successfully used in the preliminary analysis beta-lactam antibiotics.

  9. Preparation of chromatographic and solid-solvent extraction 99mTc generators using gel-type targets

    International Nuclear Information System (INIS)

    We have studied two types of targets zirconium-molybdate (ZrMo) and titanium-molybdate (TiMo) prepared by precipitating reaction between ammonium-molybdate and zirconium-chloride or titanium-chloride solutions, respectively. Other types of targets were also prepared by co-precipitating ZrMo or TiMo with hydrous manganese-dioxide, hydrous silica, and hydrous titanium-dioxide or by impregnated ZrMo or TiMo with Iodate anions. The results on extraction of Tc-99m from neutron irradiated TiMo solid phase using solvents such as MEK, aceton, ethylic ether, chloroform, etc showed that separation yield (SY) of Tc-99m in case of aceton extraction was from 70% to 80% and in other cases non higher than 40%. The Tc-99m elution curves and column kinetic in case of aceton extraction (after evaporation of aceton and recovery of Tc-99m in 0,9% NaCl solution) was superior than in case chromatographic generator using saline eluant. As result obtained, two types of generators were successfully prepared and put into use: Chromatographic generator using titanium-molybdate target as packing material and saline as eluant. Solid-solvent extraction 99mTc generator using titanium-molybdate target (as solid phase) and aceton as extracting solvent. (author)

  10. Micellar high performance liquid chromatographic determination of flunixin meglumine in bulk, pharmaceutical dosage forms, bovine liver and kidney

    Directory of Open Access Journals (Sweden)

    Fathalla F. Belal

    2015-03-01

    Full Text Available A simple, sensitive and rapid liquid chromatographic method was developed and validated for the analysis of flunixin meglumine (flunixin-M in bulk, pharmaceutical dosage forms, bovine liver and kidney. Analytical separation was performed in less than 4 min using a C18 column with UV detection at 284 nm. A micellar solution composed of 0.15 M sodium dodecyl sulphate, 8% n-butanol and 0.3% triethylamine in 0.02 M phosphoric acid buffered at pH 7.0 was used as the mobile phase. The method was fully validated in accordance with the International Conference on Harmonization (ICH guidelines. The limit of detection and the limit of quantitation were 0.02 and 0.06 μg mL−1, respectively. The recoveries obtained were in range of 95.58–106.94% for bovine liver and kidney. High extraction efficiency was obtained without matrix interference in the extraction process and in the subsequent chromatographic determination. The method showed good repeatability, linearity and sensitivity according to the evaluation of the validation parameters.

  11. Chromatographic separation of actinides and lanthanides from fission products on CMPO/SiO2-P extraction resin

    International Nuclear Information System (INIS)

    Since several years, IRI is developing an alternative for the PUREX process, based on chromatographic separations. Next to other advantages, this process shall allow partitioning of the minor actinides. At SCK x CEN, previous chromatographic experiments using LWR fuel dissolved in concentrated nitric acid, showed that Am and Cm do not adsorb onto the proposed AR-01 anion exchanger and elute simultaneously with the fission products, while U, Pu, and Np are retained quantitatively and can then be further separated and purified. After such a test, the fractions containing Am, Cm and fission products were pooled and loaded onto a CMPO/SiO2-P column. IRI had prepared this silica-based extraction resin by impregnating CMPO into a styrene-divinylbenzene copolymer, which was immobilized in porous silica particles. Earlier experiments with simulated HL W solutions in nitric acid had revealed that it allows separating the trivalent actinides (Am, Cm) and lanthanides (Ce, Nd, Eu,..) from fission products such as Cs, Sr and Ru. The present hot cell experiment using real LWR fuel confirms these results. (orig.)

  12. Simple and rapid high-performance liquid chromatographic method for the determination of aspartame and its metabolites in foods.

    Science.gov (United States)

    Gibbs, B F; Alli, I; Mulligan, C N

    1996-02-23

    A method for the determination of aspartame (N-L-alpha-aspartyl-L-phenylalanine methyl ester) and its metabolites, applicable on a routine quality assurance basis, is described. Liquid samples (diet Coke, 7-Up, Pepsi, etc.) were injected directly onto a mini-cartridge reversed-phase column on a high-performance liquid chromatographic system, whereas solid samples (Equal, hot chocolate powder, pudding, etc.) were extracted with water. Optimising chromatographic conditions resulted in resolved components of interest within 12 min. The by-products were confirmed by mass spectrometry. Although the method was developed on a two-pump HPLC system fitted with a diode-array detector, it is straightforward and can be transformed to the simplest HPLC configuration. Using a single-piston pump (with damper), a fixed-wavelength detector and a recorder/integrator, the degradation of products can be monitored as they decompose. The results obtained were in harmony with previously reported tedious methods. The method is simple, rapid, quantitative and does not involve complex, hazardous or toxic chemistry. PMID:8900578

  13. Chromatographic fingerprinting analysis of Zhizhu Wan preparation by high-performance liquid chromatography coupled with photodiode array detector

    Directory of Open Access Journals (Sweden)

    Hui Sun

    2014-01-01

    Full Text Available Background: Traditional Chinese medicine (TCM formula has been used for over 1000 years and most of them contain complicate chemical constituents. Chromatographic fingerprinting has been widely accepted as a crucial method for qualitative and quantitative analyses for TCM. Zhi Zhu Wan (ZZW, a classical Chinese medical formula, has been commonly used for the treatment of gastrointestinal disease, which pose a serious challenge to its quality control. Materials and Methods: In this work, a sensitive and reliable method of high-performance liquid chromatography coupled with photodiode array detector (HPLC-PDA was developed to control the quality of ZZW for chemical fingerprint analysis and quantitative analysis of four major bioactive constituents, including hesperidin, naringin, neohesperidin, and atractylenolide I. The chromatographic separation was performed on a Waters Symmetry C18 column (4.6 mm × 250 mm, 5 μm particle size, with an aqueous 0.095% phosphate acid and acetonitrile mobile phase gradient. Results: Optimization of other experimental conditions was validated with satisfactory accuracy, precision, repeatability, and recovery. In quantitative analysis, the four components showed good regression (R > 0.9994 within test ranges, and the recovery method ranged from 99.32% to 100.630%. HPLC fingerprints of the ZZW samples were compared by performing similarity analysis. Conclusion: The results indicated that the newly developed HPLC-PDA fingerprint method would be suitable for quality control of ZZW.

  14. A VALIDATED REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR THE DETERMINATION OF DOXOFYLINE IN PURE AND PHARMACEUTICAL FORMULATIONS

    Directory of Open Access Journals (Sweden)

    Lanka Venkateswararao

    2013-02-01

    Full Text Available A novel reverse phase high performance liquid chromatographic method (RP-HPLC was developed and validated for the determination of doxofylline (DXF in pharmaceutical formulations. Agilent 1100 series HPLC instrument equipped with variable wavelength programmable UV-Visible detector and a chromosil C18 (250mm x 4.6mm, 5μm column with an auto injector was used for the present investigation. A volume of 20µL of working standard of concentration 25µg/mL was injected into the chromatographic system, the component was separated by using the mobile phase of the mixture of potassium dihydrogen phosphate buffer of pH 5.5 and acetonitrile in the ratio 75:25(v/v at a flow rate of 1.0 mL/min and the detection of the components was carried out at a wavelength of 275nm. Chemstation software was used for the data acquisition through out the analysis. The system suitable parameters such as number of theoretical plates, tailing factor and resolution were found to be satisfactory. The retention time of the component was found to be at 4.814 minutes. The proposed method was validated in terms of precision, accuracy, linearity, limit of detection, limit of quantification, robustness and ruggedness. The developed method was found to be rapid, simple and sensitive hence it could be used as an alternative method in assay of the doxofylline in any pharmaceutical industries.

  15. Preparation of chromatographic and solid-solvent extraction {sup 99m}Tc generators using gel-type targets

    Energy Technology Data Exchange (ETDEWEB)

    Le Van So [Radioisotope Department, Nuclear Research Institute, Dalat (Viet Nam)

    2000-10-01

    We have studied two types of targets zirconium-molybdate (ZrMo) and titanium-molybdate (TiMo) prepared by precipitating reaction between ammonium-molybdate and zirconium-chloride or titanium-chloride solutions, respectively. Other types of targets were also prepared by co-precipitating ZrMo or TiMo with hydrous manganese-dioxide, hydrous silica, and hydrous titanium-dioxide or by impregnated ZrMo or TiMo with Iodate anions. The results on extraction of Tc-99m from neutron irradiated TiMo solid phase using solvents such as MEK, aceton, ethylic ether, chloroform, etc showed that separation yield (SY) of Tc-99m in case of aceton extraction was from 70% to 80% and in other cases non higher than 40%. The Tc-99m elution curves and column kinetic in case of aceton extraction (after evaporation of aceton and recovery of Tc-99m in 0,9% NaCl solution) was superior than in case chromatographic generator using saline eluant. As result obtained, two types of generators were successfully prepared and put into use: Chromatographic generator using titanium-molybdate target as packing material and saline as eluant. Solid-solvent extraction {sup 99m}Tc generator using titanium-molybdate target (as solid phase) and aceton as extracting solvent. (author)

  16. High-performance liquid chromatographic strategies for the determination and confirmation of anticoagulant rodenticide residues in animal tissues.

    Science.gov (United States)

    Hunter, K

    1985-03-15

    A comprehensive approach to the analysis of anticoagulant rodenticide residues in animal tissues based on high-performance liquid chromatography (HPLC) has been developed. Residues of warfarin, coumatetralyl, difenacoum, brodifacoum, bromadiolone, diphacinone and chlorophacinone were extracted with chloroformacetone (1:1, v/v). Extracts were cleaned-up by an integrated gel permeation and adsorption chromatographic procedure which divided the rodenticides into two groups. Residues were then determined and confirmed using normal-phase, ion-pair and weak ion-exchange HPLC techniques. Ion-pair gradient separation resolved all seven rodenticides in a single chromatographic analysis. UV detection methods were employed for all seven rodenticides. Use of a diode array detection system permitted additional confirmation of residues down to 0.1 mg kg-1 by matching UV spectra and derivatives of spectra. Sensitive fluorescence detection was possible for the coumarin-based rodenticides but not for diphacinone and chlorophacinone. Post-column pH-switching fluorescence detection methods were shown to be superior to other methods of fluorescence detection of coumarin-based rodenticides. Recoveries from spiked liver tissue were around 90% at levels from 0.05 to 1 mg kg-1. Detection limits of around 0.002 mg kg-1 for most rodenticides and of 0.01 mg kg-1 for warfarin could be achieved with animal tissue extracts. PMID:3988841

  17. Development and validation of high-perfomance liquid chromatographic method for determination of ofloxacin and lomefloxacin in human plasma

    Directory of Open Access Journals (Sweden)

    DRAGICA ZENDELOVSKA

    2005-12-01

    Full Text Available Ahigh-performance liquid chromatographicmethod for the determination of ofloxacin and lomefloxacin in human plasma has been developed and validated. The effect of organic modifiers on the retention of the investigated drugs was investigated. Asimple isocratic chromatographic assay with UV-detection at 280 nm was performed on a Hibar Lichrospher 100 RP 8 column (250×4.6 mm, 5 mm. Merck, Germany using a mixture of acetonitrile and 0.5 % triethylamine in water (pH adjusted to 2.5 with H3PO4 (15:85, V/V as the mobile phase at flow rate of 1.2 mL min-1. The calibration curves were linear in the concentration ragne of 0.5 – 6.0 mg mL-1 for ofloxacin and 0.2-4.5 mg mL-1 for lomefloxacin.

  18. Chemical Compositions, Chromatographic Fingerprints and Antioxidant Activities of Andrographis Herba

    OpenAIRE

    Yang Zhao; Chun-Pin Kao; Kun-Chang Wu; Chi-Ren Liao; Yu-Ling Ho; Yuan-Shiun Chang

    2014-01-01

    This paper describes the development of an HPLC-UV-MS method for quantitative determination of andrographolide and dehydroandrographolide in Andrographis Herba and establishment of its chromatographic fingerprint. The method was validated for linearity, limit of detection and quantification, inter- and intra-day precisions, repeatability, stability and recovery. All the validation results of quantitative determination and fingerprinting methods were satisfactory. The developed method was then...

  19. Two Chromatographic Methods for the Determination of Some Antimigraine Drugs

    OpenAIRE

    El-Bagary, Ramzia I.; Mohammed, Nashwah G.; Nasr, Heba A.

    2012-01-01

    Two stability indicating chromatographic methods were proposed for the determination of almotriptan, eletriptan, and rizatriptan, in presence of their acid degradation products. The first method is a quantitative densitometric thin layer chromatography. The developing systems were; acetonitrile: methanol: dichloromethane: ammonia (10:6:3:1 v/v), ethyl acetate: methanol: ammonia (15:4:1 v/v), and methanol: acetonitrile: ammonia (9:4:1 v/v) for almotriptan, eletriptan and rizatriptan respective...

  20. Chromatographic methods for the bioanalysis of pyrethroid pesticides.

    Science.gov (United States)

    Gullick, Darren R; Mott, Kyle B; Bartlett, Michael G

    2016-05-01

    Reliable analytical methods are needed for the determination of pyrethroid pesticides residues in biological tissues such as whole blood and plasma, meat, eggs, milk, brain, liver, and adipose tissue for monitoring of levels in livestock and for human risk assessment. A review of the current literature is given, with consideration to extraction techniques, sample preparation, and chromatographic approaches including both conventional and new technologies. Copyright © 2016 John Wiley & Sons, Ltd. PMID:26916501

  1. Chromatographic and electrophoretic methods for nanodisc purification and analysis

    DEFF Research Database (Denmark)

    Justesen, Bo Højen; Günther-Pomorski, Thomas

    2014-01-01

    Soluble nanoscale lipid bilayers, termed nanodiscs, are widely used in science for studying the membrane-anchored and integral membrane protein complexes under defined experimental conditions. Although their formation occurs by a self-assembly process, nanodisc purification and the verification of...... proper reconstitution are still major challenges during the sample preparation. This review gives an overview of the methods used for purifying and analyzing nanodiscs and nanodisc-reconstituted membrane proteins, with an emphasis on the chromatographic and electrophoretic approaches....

  2. Scandium(3) purification from concomitant impurities by chromatographic methods

    International Nuclear Information System (INIS)

    The process of scandium(3) purification from concomitant impurities (rare earths, Zr(4), Th(4), Fe(3)) using sorptional chromatography has been studied by tracer technique. The relevant sorbents have been chosen and the optimal conditions for scandium isolation have been ascertained. It is shown that employment of sorption-chromatographic methods for scandium purification permits obtaining scandium(3) preparation of 99.99% purity

  3. An Exact Algorithm for IP Column Generation

    OpenAIRE

    Vanderbeck, François; Wolsey, Laurence

    1994-01-01

    An exact column generation algorithm for integer programs with a large (implicit) number of columns is presented. The family of problems that can be treated includes not only standard partitioning problems such as bin packing and certain vehicle routing problems in which the columns generated have 0 - 1 components and a right hand side vector of 1 's, but also the cutting stock problem in which the columns and right hand side are nonnegative integer vectors. We develop a combined branching an...

  4. FRP rupture strains in FRP wrapped columns

    OpenAIRE

    Li, Shiqing

    2012-01-01

    Applying lateral confinement to concrete columns using fibre-reinforced polymer (FRP) composites is a very promising technique. FRP rupture is the typical failure mode of FRP wrapped columns under axial compression. numerous experiments have shown that the FRP rupture strain in an FRP wrapped circular column is significantly lower than the FRP ultimate rupture strain determined from flat coupon test of FRP. Despite a large number of studies on the application of FRP confined columns, the mech...

  5. Kinetics and equilibria of the chromatographic separation of maltose and trehalose.

    Science.gov (United States)

    He, Dengjun; Zhou, Jiachun; Xia, Quanming; Jiang, Lihua; Qiu, Yongjun; Zhao, Liming

    2015-07-01

    Trehalose, a nonreducing disaccharide, has been extensively applied to food, cosmetics, and pharmaceutical goods. The resultant solution of trehalose prepared by enzymatic methods includes high amounts of maltose. However, it is quite difficult to separate maltose and trehalose on an industrial scale because of their similar properties. In this paper, a high-performance resin was selected as a stationary phase to separate trehalose and maltose, and the resolution of these sugars was 0.59. The potential of a cation exchange resin was investigated as the stationary phase in separating trehalose and maltose using deionized water as the mobile phase. Based on the equilibrium dispersive model, the axial dispersion coefficients and overall mass transfer coefficients of maltose and trehalose were determined by moment analysis at two different temperatures, 50 and 70°C. Other parameters, including the column void and the adsorption isotherms, were also determined and applied to simulate the elution curves of trehalose and maltose. The simulated results matched the experimental data, validating the parameters. The optimized parameters are critical to the chromatographic separation of trehalose and maltose on an industrial scale. PMID:25873564

  6. Preparation of Medium Cation Exchange Stationary Phase of Polymeric Matrix and Their Chromatographic Properties

    Institute of Scientific and Technical Information of China (English)

    CHEN,Gang; GONG,Bo-Lin; BAI,Quan; GENG,Xin-Du

    2007-01-01

    Based on the monodisperse poly(glycidyl methacrylate-co-ethylenedimethacrylate) beads (PGMA/EDMA) with macropore as a medium, a new hydrophilic medium cation exchange (MCX) stationary phase for HPLC was synthesized by a new chemically modified method. The stationary phase was evaluated with the property of ion exchange, separability, reproducibility, hydrophilicity, effect of salt concentration, salt types, column loading and pH on the separation and retention of proteins in detail. It was found that it follows ion exchange chromatographic (IEC)retention mechanism. The measured bioactivity recovery for lysozyme was (96±5)%. The dynamic protein loading capacity of the synthesized MCX packings was 21.8 mg/g. Five proteins were almost completely separated within 6.0 min at a flow rate of 4 mL/min using the synthesized MCX resin. The MCX resin was also used for the rapid separation and purification of lysozyme from egg white with only one step. The purity and specific bioactivity of the purified lysozyme was found more than 95% and 70345 U/mg, respectively.

  7. Method modification for liquid chromatographic determination of thiamine, riboflavin, and pyridoxine in medical foods.

    Science.gov (United States)

    Chase, G W; Landen, W O; Soliman, A G; Eitenmiller, R R

    1993-01-01

    A reversed-phased ion pair liquid chromatographic method developed for the simultaneous determination of thiamine (B1), riboflavin (B2), and pyridoxine (B6) in perchloric acid extracts of infant formulas was modified to include medical foods. UV detection of B1 and B2 was replaced by fluorescence detection, which resulted in improved sensitivity and specificity. B1 was detected by fluorescence after conversion to thiochrome by a postcolumn reaction with sodium hydroxide and potassium ferricyanide. The method uses a mobile phase of water, acetonitrile, hexanesulfonic acid sodium salt, ammonium hydroxide, and phosphoric acid adjusted to pH 3.6. The column is a 300 x 3.9 mm Nova Pak C18. Limits of detection were 0.05 microgram/mL for B1 and B2 and 0.01 microgram/mL for B6 by fluorescence detection. The system reproducibility was evaluated by completing 10 repetitive determinations on a medical food that gave a coefficient of variation of 5.9, 6.0, and 10.7% for B1, B2, and B6, respectively. Mean recoveries (n = 10) were 111, 96.3, and 113% for B1, B2, and B6, respectively. The results compared favorably with those by AOAC Official Methods 942.23, 940.33, and 961.15 for B1, B2, and B6, respectively. PMID:8286968

  8. Furosine as a pasta quality marker: evaluation by an innovative and fast chromatographic approach.

    Science.gov (United States)

    Giannetti, Vanessa; Mariani, Maurizio Boccacci; Mannino, Paola

    2013-07-01

    A fast and simple high-performance liquid chromatography method suitable for determining furosine level in heat-treated food samples was developed. The analysis of furosine was performed by a novel mixed-mode column that provides multiple and simultaneous retention mechanisms including cation-exchange, anion-exchange, reversed-phase, or hydrophilic interaction. Each retention mechanism could be independently controlled by setting chromatographic conditions. Adequate retention and selectivity of polar charged furosine were achieved by adjusting mobile phase pH, buffer concentration, organic content, and ionic strength. The optimized method was successfully applied to determinate furosine in durum wheat semolina pasta samples. Furosine level in pasta may be used as a reliable marker of health and nutritional damage occurring during pasta manufacture. Indeed, a low content of furosine is generally related to high nutritional quality of food and application of mild heat treatments. A wide range of dry pasta samples, collected from both supermarkets (large-scale retail trade) and shops selling local products, were analyzed. Variable amounts of furosine, ranging from 107 to 506 mg/100 g of protein, were found in pasta samples. The proposed method allows to discriminate products submitted to different time-temperature conditions during the drying process. At the same time, it may be used to highlight potential label fraud. PMID:23772758

  9. Gas chromatographic method for the determination of hexaconazole residues in black tea

    Institute of Scientific and Technical Information of China (English)

    Chinnachamy KARTHIKA; Paul James SACHIN

    2008-01-01

    A highly reliable, quantitative and sensitive analytical method for determining the residues of the fungicide, hexaconazole in black tea is described. The proposed method is based on liquid-liquid extraction followed by gas chromatographic determination, using nitrogen phosphorus detector (GC-NPD) for the identification and quantitation of hexaconazole. The most was cleaned up by adsorption column chromatography using activated florisil. Performance of the method was assessed by evaluating quality parameters such as recovery value, repeatability, reproducibility, linearity and limits of detection and quantitation. When the method was assessed for repeatability, the percentage of recovery ranged between 86% and 96% while the relative standard deviation was between 0.30% and 2.35%. In studies on reproducibility the recovery ranged from 81% to 85% and relative standard deviation from 1.68% to 5.13%, implying that the method was reliable. A field trial was conducted to verify the application of this method with real samples. Results prove that the validated method was suitable for extracting hexaconazole residues.

  10. Application of radioisotopes to a gas-chromatographic detector for direct indication of concentration

    International Nuclear Information System (INIS)

    During the last few years, numerous types of detecting devices, including ionization detectors, have been developed for gas chromatography, but the quantitative evaluation of chromatograms suffers from limited accuracy in the measurement of peak areas. These difficulties have been overcome by the use of a detector based on the principle of ionization by nuclear radiation, but operated as a counter. Such operation is possible owing to the fact that the addition of organic vapours to rare gases lowers the voltage of the plateau-characteristic of a counter. The detector consists of a flow-type counter and a radioisotope source of ionizing radiation, together with a suitable scaler. The power supply of the counter is set several hundred volts lower than the starting voltage of the unit when operated with a rare gas alone. When a fraction is emerging from the chromatographic column, the detector registers the incident radiation. The number of counts accumulated by the scaler over the 'peak' is a direct measure of the concentration of the sample fraction under consideration. The performance of various counters of different geometry is described, and preliminary results concerning the sensitivity and the dependence of count rate upon concentration are discussed. (author)

  11. Simultaneous determination of a quaternary mixture of oxomemazine, sodium benzoate, guaifenesin and paracetamol by chromatographic methods

    Directory of Open Access Journals (Sweden)

    Nehal F. Farid

    2014-12-01

    Full Text Available The aim of the present work was to develop simple, accurate, sensitive and selective methods for the simultaneous determination of oxomemazine (Ox, sodium benzoate (SB, guaifenesin (Gu, andparacetamol (Par. Two methods were described and validated for the simultaneous determination of the four drugs in syrup and suppositories. The first method was a reversed phase HPLC and UVdetection at 220 nm. The assay was performed using C 18 column and an isocratic elution using acetonitrile – methanol – 35 mM KH2PO4 (20: 5: 75; by volume, pH was adjusted to 2.9 ± 0.1 as the mobile phase. The flow rate was 1.5 mL/min and separation was achieved in less than 15 min. The second method was a TLC- spectrodensitometric method, used to separate, identify and quantify the four drugs when present in combination. The drugs were applied on silica gel plates and development was made using methylene chloride- methanol- acetic acid- 33% ammonia (89: 8.4: 2: 0.6, by volume as a mobile phase. The bands of the four drugs were quantified by scanning spectrodensitometricaly at 270 nm. The suggested chromatographic methods were validated and applied successfully to the analysis of the syrup and suppositories.

  12. One-step chromatographic procedure for purification of B-phycoerythrin from Porphyridium cruentum.

    Science.gov (United States)

    Tang, Zhihong; Jilu Zhao; Ju, Bao; Li, Wenjun; Wen, Shaohong; Pu, Yang; Qin, Song

    2016-07-01

    B-phycoerythrin (B-PE) was separated and purified from microalga Porphyridium cruentum using one-step chromatographic method. Phycobiliproteins in P. cruentum was extracted by osmotic shock and initially purified by ultrafiltration. Further purification was carried out with a SOURCE 15Q exchange column and analytical grade B-PE was obtained with a purity ratio (A545/A280) of 5.1 and a yield of 68.5%. It showed a double absorption peaks at 545 nm and 565 nm and a shoulder peak at 498 nm, and displayed a fluorescence emission maximum at 580 nm. The analysis by sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) showed a bulky band between 18 and 20 kDa which could be assigned to subunits α and β and a low intensity band of 27 kDa assigned to γ subunit. Our protocol provides attractive alternative to consider for the purification procedure to obtain analytical grade B-PE at commercial level. PMID:26851659

  13. Rapid liquid chromatographic determination of dimetridazole and ipronidazole in swine feed.

    Science.gov (United States)

    Roybal, J E; Munns, R K; Hurlbut, J A; Shimoda, W; Morrison, T R; Vieira, C L

    1987-01-01

    A simple and rapid method is described for the determination of dimetridazole (DMZ) and ipronidazole (IPR) in swine feeds at various levels (0.11-110 ppm). The drugs are released from feed by prewetting with a buffer, followed by extraction with either methanol or methylene chloride, depending on the drug level; if necessary, an acid-base cleanup is used before the liquid chromatographic analysis. The analytes are separated on a C18 column and monitored at 320 nm for detection and quantitation. Recoveries of DMZ from several feed formulations averaged 108% at the 92.8 ppm level with a standard deviation (SD) of 4.00% and a coefficient of variation (CV) of 3.70%, 101% at the 11.2 ppm level with an SD of 11.9% and a CV of 11.8%, and 100% at the 0.112 ppm level with an SD of 9.27% and a CV of 9.25%. Recoveries of IPR averaged 77.1% at the 12.9 ppm level with an SD of 1.75% and a CV of 2.27%; IPR recoveries averaged 35.2% at the 0.129 ppm level with an SD of 3.39% and a CV of 9.63%. PMID:3624165

  14. RAPID CHROMATOGRAPHIC AND SPECTROPHOTOMETRIC DETERMINATION OF CITALOPRAM IN RELEVANCE TO PHARMACEUTICAL ANALYSIS

    Directory of Open Access Journals (Sweden)

    R. S. Das et al.

    2012-01-01

    Full Text Available This paper describes the study to measure the sensitivity and accuracy of two techniques, chromatography and spectrophotometry for the direct determination of citalopram in pharmaceutical formulations. Chromatography was performed on SE-30 column (1 m × 3 mm i.d using Nitrogen as a carrier gas (flow rate of 40 ml/min, having retention time of 12.8 min. Calibration curve was found linear in the range of 200-400 µg/ml. LOD and LOQ values were found as 1.1726 µg/ml and 3.5535 µg/ml respectively and the recoveries were in the range of 98.36–100.07%. In spectrophotometry method the absorption spectra were measured at 240 nm for standard and tablets form. Calibration curve was found linear in the range of 2-4 µg/ml. LOD and LOQ values were found as 40.59 ng/ml and 123.0 ng/ml respectively. Recoveries were in the range of 98.53–100.78%. The experimental results obtained indicate that the above proposed methods are specific, sensitive and accurate for the determination of citalopram in pharmaceutical formulations. These methods were also compared statistically and found that there was no significant difference between the two methods in terms of accuracy and precision. Whilst, the chromatographic method developed will applicable for its detection in biological matrices also.

  15. Development and validation of a chromatographic method for determining Clematichinenoside AR and related impurities

    Directory of Open Access Journals (Sweden)

    Zhou Yang

    2012-12-01

    Full Text Available Abstract Background Clematichinenoside AR is a promising lead compound for the treatment of rheumatoid arthritis. A systematic research for the related impurities in AR bulk samples is still lacking. For the safe use of this natural product in future clinical practice, the structure and content of each constituent, including the main ingredient as well as the impurities in AR bulk sample must be characterized in detail. Results A simple and stability indicating RP-HPLC method was developed and validated for determining the purity of clematichinenoside AR (AR, a natural product from the roots of Clematis manshurica Rupr. (Ranunculaceae with the potential of treating rheumatoid arthritis. Five impurities were characterized, and impurity 2 (Clematomandshurica saponin F is a new triterpenoid saponin isolated from this product. Optimum separation for clematichinenoside AR and five related impurities was carried out on an Agilent octadecylsilane bonded silica gel column (TC-C18, 4.6 mm ×150 mm, 5 μm using a gradient HPLC method. The validation results showed good sensitivity, specificity, linearity(r2>0.9992 precision(RSD Conclusion Five related impurities of clematichinenoside AR were characterized, including a new triterpenoid saponins firstly found in clematichinenoside AR bulk samples. In the simple chromatographic method for determining clematichinenoside AR and its related impurities in bulk samples, the correction factor was better for the quality control in the relative stable concentrations.

  16. Chromatographic Separation of Xanthine Derivatives on Single and Mixed-Template Imprinted Polymers

    International Nuclear Information System (INIS)

    We developed in the present study molecular imprinted polymers (MIPs), using single templates (pentoxifylline, caffeine and theophylline) and mixed-templates (pentoxifylline-caffeine, pentoxifylline-theophylline and caffeine-theophylline). The MIPs were prepared with methacrylic acid (MAA) as the monomer, ethylene glycol dimetharylate (EGDMA) as the crosslinker and 2,2'-azobis(isobutyronitrile) (AIBN) as the initiator. The obtained polymer particles (particle size after grinding was about 25-35 μm) were packed into a HPLC column (3.9 mm i.d. Χ 150 mm). The selectivity and chromatographic characteristics of the MIPs were studied using acetonitrile as the mobile phase at a flow rate of 0.8 mL/min. UV detector wavelength was set at 270 nm. Different single template MIPs showed different molecular recognitions to the templates and the structurally analogues, according to the rigidity and steric hindrance of the compounds. Recognition was improved on the mixed-template MIPs as a result of the cooperation or sum effect of the templates, whereas on the pentoxifylline-theophylline imprinted polymer, the highest selectivity and affinity were obtained. Separations of the test compounds on different polymers were also investigated

  17. Chromatographic Separation of Xanthine Derivatives on Single and Mixed-Template Imprinted Polymers

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Dexian; Hong, Seung Pyo; Row, Kyung Ho [Inha University, Incheon (Korea, Republic of)

    2004-03-15

    We developed in the present study molecular imprinted polymers (MIP{sub s}), using single templates (pentoxifylline, caffeine and theophylline) and mixed-templates (pentoxifylline-caffeine, pentoxifylline-theophylline and caffeine-theophylline). The MIP{sub s} were prepared with methacrylic acid (MAA) as the monomer, ethylene glycol dimetharylate (EGDMA) as the crosslinker and 2,2'-azobis(isobutyronitrile) (AIBN) as the initiator. The obtained polymer particles (particle size after grinding was about 25-35 {mu}m) were packed into a HPLC column (3.9 mm i.d. {Chi} 150 mm). The selectivity and chromatographic characteristics of the MIP{sub s} were studied using acetonitrile as the mobile phase at a flow rate of 0.8 mL/min. UV detector wavelength was set at 270 nm. Different single template MIP{sub s} showed different molecular recognitions to the templates and the structurally analogues, according to the rigidity and steric hindrance of the compounds. Recognition was improved on the mixed-template MIP{sub s} as a result of the cooperation or sum effect of the templates, whereas on the pentoxifylline-theophylline imprinted polymer, the highest selectivity and affinity were obtained. Separations of the test compounds on different polymers were also investigated

  18. Stability-indicating liquid Chromatographic assaymethod for Opthalmic solutions containing combination of Dexamethasone and Chloramphenicol

    International Nuclear Information System (INIS)

    A selective high-performance chromatographic procedure for the stability monitoring of ophthalmic solutions containing a combination of dexamethasone and chloramphenicolis demonstrated. The separation of the active components and the degradation product of chloramphenicol (1-amino-1-(4-nitrophenyl)-propane-1, 3diol) was achieved on a u-Bondapack C-18 column ( 5 um, 300 mm x 3.9 mm) maintained at ambient temperature (15-20C) by utilizing a mobile phase consisting acidified water (5% actified water with glacial acetic acid ) : acetonitrile : triethyl amine 700 : 300 : 2and pH was adjusted to 5.0 by using 10 M Na OH. The flow rate was 1.5 ml min-1; and elutes were followed with UV-detection at 254 nm. Complete resolution of dexamethasone, chloramphenicol and its hydrolytic product could be attained. The sensitivity, accuracy and specificity were tested. The method was successfully applied in post-marketing stability of the commercial batches of ophthalmic solutions. (author)

  19. High-performance liquid chromatographic determination of triclosan and triclocarban in cosmetic products.

    Science.gov (United States)

    Liu, T; Wu, D

    2012-10-01

    A high-performance liquid chromatographic (HPLC) method for the determination of triclosan and triclocarban in cosmetic products was developed. Triclosan and triclocarban quantities in 168 of cosmetics were investigated and statistical analyzed with this method. The optimal condition are as follows: An Agilent SB-C8 analytical column (250 × 4.6 mm, 5μm) was utilized, and mixed buffer solution of methanol and 0.01 mol L(-1) phosphate (pH 3.0) (72 : 28, V/V) were used for isocratic elution at a total flow rate of 1.0 mL min(-1) . It is found the calibration curves had a good linear regression with UV detection (280 nm) within test range of 0-110 μg mL(-1) with the correlation coefficients of 0.999 in all cases. This method is simple, selective, convenient, and reproducible for the determination of triclosan and triclocarban in commercial cosmetic products. PMID:22809056

  20. Liquid Chromatographic Determination of Pioglitazone in Pharmaceuticals, Serum and Urine Samples

    Directory of Open Access Journals (Sweden)

    Shahnaz Perveen

    2011-12-01

    Full Text Available A rapid and reliable analytical method based on high-performance liquid chromatography (HPLC with UV detection (221nm has been developed for the determination of the anti-hyperglycemic agent Pioglitazone in pharmaceutical formulations and biological fluids (serum and urine after clean-up with solid-phase extraction. Chromatographic separation was achieved with a Chromolith® Performance RP-18e (100×4.6mm column using mobile phase composition of acetonitrile: mixed phosphate buffer (pH 2.5; 10mM (30:70, v/v with a flow rate of 2.0mL/min. The total run time was 2 min. under optimized conditions. The calibration curve was found to be linear in the range of 1-10 µg mL-1 with regression coefficient of 0.9996, and the lower limit of detection 72 ng/20µL injection. The method has been validated for the system suitability, linearity, precision and accuracy, limits of detection, specificity, stability and robustness. The %recovery of Pioglitazone in pharmaceutical formulations was found to be 104.7%. The assay has been applied successfully to the pharmaceutical Tablet samples and biological fluids (serum and urine of healthy volunteers.

  1. Chromatographic evaluation and antimicrobial activity of Neem (Azadirachta indica A. Juss., Meliaceae leaves hydroalcoholic extracts

    Directory of Open Access Journals (Sweden)

    Priscila D. Alves

    2009-06-01

    Full Text Available Neem (Azadirachta indica is an Indian tree well known for its several pharmacological activities, including antimicrobial activity. More than 300 composites have already been isolated and azadirachtin (AZA is its main active component. In the present work, Neem leaves hydroalcoholic extracts were prepared by percolation in 96% ethanol different concentrations (50%, 60%, 70%, 80% and 90% (v/v. The presence of AZA was tested by TLC by eluting the extracts and a standard solution of AZA through a chromatographic plate developed with anisaldehyde/sulfuric acid solution followed by heating. By HPLC, extracts elution took place on a C18 column, water:acetonitrile (60:40 as mobile phase, 1.0 mL/min flow rate and detection at λ217 nm. The extracts did not display AZA spots or peaks, however, they were tested against Gram-positive and Gram-negative bacteria, yeasts and a mold fungus. The extracts were tested in different increasing concentrations, in order to detect a dose-dependent relationship of the activity. Despite the absence of AZA, the 70% and 80% (v/v ethanol extracts showed activity against Staphylococcus aureus. However, this activity was not dose-dependent according to Tukey's test (q0,05;3;7.

  2. The partition chromatograph separation-spectrometry for the determination of 29 trace elements in PuO2

    International Nuclear Information System (INIS)

    The partition chromatograph separation-spectrometry for the determination of 29 trace elements in PuO2 is described. A dissolving sample with electromagnetical mixer was designed. The oil bath of high boiling point was employed for dissolving sample. 30 mg PuO2 could be dissolved completely about 20 minuts. The column partition chromatograph was used in which mixing extraction agent of TBP and TIOA (1:1) was employed as stationary phase, PTFCE powder as support, 3.5 N nitric acid as mobile phase. The determined trace elements were separated from 30 mg PuO2 and collected in 1 ml receiving liquid. In which the low content of Pu did not interfere the determination. The indium was used as extra base, the indium and yttrium were used as inside marking elements. 29 trace elements (Cd, Ba, Be, Fe, Co, Si, B, Ga, Sc, P, Mn, Cr, W, Mg, Mo, Pb, Ni, Al, Ti, La, Ca, V, Ce, Cu, Ag, Zn, Li, Na, K) were determined cooperatively by ISP-28 type and ISP-51 type spectrograph using solution dry residue of high pressure spark. The range of the determination of the trace elements varies from 3 x 10-6 to 3 x 10-2%. The recovery of this method varies from 83-120%. The precision is within +- 28%. The plutonium absorbed in the column can be desorbed by 4 N methanoic acid, for example, 30 mg PuO2 can be desorbed quantitatively by 2 ml such desorbing agent

  3. Thermal pretreatments of superficially porous silica particles for high-performance liquid chromatography: Surface control, structural characterization and chromatographic evaluation.

    Science.gov (United States)

    Mignot, Mélanie; Sebban, Muriel; Tchapla, Alain; Mercier, Olivier; Cardinael, Pascal; Peulon-Agasse, Valérie

    2015-11-01

    This study reports the impact of thermal pretreatment between 400 and 1100°C on superficially porous silica particles (e.g. core-shell, fused-core; here abbreviated as SPP silica). The different thermally pretreated SPP silica (400°C, 900°C and 1100°C) were chemically bonded with an octadecyl chain under microwave irradiation. The bare SPP silica, thermally untreated and pretreated, as well as the chemically bonded phases (CBPs) were fully characterized by elemental analysis, diffuse reflectance infrared Fourier transform spectroscopy (DRIFT), and solid state cross polarization magic angle spinning (CP-MAS) (29)Si NMR. The chromatographic properties of the overall set of C18-thermally pretreated SPP silica stationary phases were determined using the Tanaka test. Complementary, the simplified Veuthey test was used to deeply study the silanol activity, considering a set of 7 basic solutes with various physicochemical properties. Both tests were also performed on different commercial SPP silica columns and different types of bonding chemistry (C18, Phenyl-hexyl, RP-amide, C30, aQ). Multivariate data analyses (hierarchical cluster analysis and principal component analysis) were carried out to define groups of stationary phases with similar chromatographic properties and situate them in relation to those commercially available. These different C18-thermally pretreated SPP silicas represented a wide range of stationary phases as they were spread out along the score plot. Moreover, this study highlighted that the thermal pretreatment improved the chemical stability of the SPP silica compare to untreated SPP silica and untreated porous silica. Consequently, higher thermal pretreatment can be applied (up to 900°C) before functionalization without destruction of the silica matrix. Indeed, a significantly lower dissolution of the thermally pretreated SPP silica under aggressive conditions could allow the use of the corresponding functionalized stationary phases at high

  4. Development of a harmonised method for the profiling of amphetamines: III. Development of the gas chromatographic method.

    Science.gov (United States)

    Andersson, Kjell; Jalava, Kaisa; Lock, Eric; Finnon, Yvonne; Huizer, Henk; Kaa, Elisabet; Lopes, Alvaro; Poortman-van der Meer, Anneke; Cole, Michael D; Dahlén, Johan; Sippola, Erkki

    2007-06-14

    This study focused on gas chromatographic analysis of target compounds found in illicit amphetamine synthesised by the Leuckart reaction, reductive amination of benzyl methyl ketone, and the nitrostyrene route. The analytical method was investigated and optimised with respect to introduction of amphetamine samples into the gas chromatograph and separation and detection of the target substances. Sample introduction using split and splitless injection was tested at different injector temperatures, and their ability to transfer the target compounds to the GC column was evaluated using cold on column injection as a reference. Taking the results from both techniques into consideration a temperature of 250 degrees C was considered to be the best compromise. The most efficient separation was achieved with a DB-35MS capillary column (35% diphenyl 65% dimethyl silicone; 30 m x 0.25 mm, d(f) 0.25 microm) and an oven temperature program that started at 90 degrees C (1 min) and was increased by 8 degrees C/min to 300 degrees C (10 min). Reproducibility, repeatability, linearity, and limits of determination for the flame ionisation detector (FID), nitrogen phosphorous detector (NPD), and mass spectrometry (MS) in scan mode and selected ion monitoring (SIM) mode were evaluated. In addition, selectivity was studied applying FID and MS in both scan and SIM mode. It was found that reproducibility, repeatability, and limits of determination were similar for FID, NPD, and MS in scan mode. Moreover, the linearity was better when applying FID or NPD whereas the selectivity was better when utilising the MS. Finally, the introduction of target compounds to the GC column when applying injection volumes of 0.2 microl, 1 microl, 2 microl, and 4 microl with splitless injection respectively 1 microl with split injection (split ratio, 1:40) were compared. It was demonstrated that splitless injections of 1 microl, 2 microl, and 4 microl could be employed in the developed method, while split

  5. Reversed-phase high-performance liquid chromatographic approach to determine total lymphocyte concentrations of 6-thioguanine, methylmercaptopurine and methylthioguanine in humans.

    Science.gov (United States)

    Erdmann, G R; Steury, J C; Carleton, B C; Stafford, R J; Bostrom, B C; Canafax, D M

    1991-11-15

    A reversed-phase high-performance liquid chromatographic (HPLC) procedure was developed to quantify intracellular lymphocyte 6-thioguanine, methylmercaptopurine and methylthioguanine. The free base of each metabolite was obtained by acid hydrolysis, which allowed for a total determination of thiopurine metabolites. 6-Thioguanine was analyzed on an octadecylsilane column using acetonitrile-10 mM sodium phosphate (11:89), pH 7, containing 0.06% tetrabutylammonium chloride. 6-Thioguanine was oxidized with potassium permanganate, and fluorescence was measured at 330 nm excitation and 410 nm emission. Methylmercaptopurine and methylthioguanine were separated on a cyanopropylsilane column using methanol-40 mM sodium phosphate (22:78), pH 2.7, and detected by ultraviolet absorbance at 314 and 290 nm, respectively. PMID:1810943

  6. Comparative studies of peak intensities and chromatographic separation of proteolytic digests, PTMs, and intact proteins obtained by nanoLC-ESI MS analysis at room and elevated temperatures.

    Science.gov (United States)

    Moskovets, Eugene V; Ivanov, Alexander R

    2016-06-01

    This work demonstrates that the chromatographic separation performed at highly stabilized elevated temperature results in significant improvements in sensitivity, quantitative accuracy, chromatographic resolution, and run-to-run reproducibility of nanoLC-MS analysis of complex peptides mixtures. A newly developed platform was shown to provide conditions for accurate temperature stabilization and temperature homogeneity when performing nanoLC-ESI MS analysis. We quantitatively assessed and compared the recovery of peptides and small proteins from nanoLC columns at room and elevated temperatures. We found that analyses performed at highly stabilized elevated temperatures led to improved detection sensitivity, reproducibility, and chromatographic resolution in reversed-phase LC separation of unmodified peptides (both hydrophilic and hydrophobic), post-translationally modified peptides (O-phosphorylated), and small intact proteins. The analytical benefits of elevated temperatures for qualitative and quantitative proteomic LC-MS profiling were demonstrated using mixtures of synthetic peptides, tryptic digests of mixtures of model proteins, and digested total lysates of isolated rat kidney mitochondria. The effect of elevated temperature on the ion suppression was also demonstrated. Graphical Abstract A fragment of overlaid LC retention time-m/z planar views demonstrates the improved separation performance in the analysis of a complex peptide mixture at elevated temperature. Retention time-m/z 2D peptide features detected at 60 °C (magenta) were matched and aligned with features detected at room temperature (green). PMID:26898204

  7. A versatile noninvasive method for adsorber quantification in batch and column chromatography based on the ionic capacity.

    Science.gov (United States)

    Huuk, Thiemo C; Briskot, Till; Hahn, Tobias; Hubbuch, Jürgen

    2016-05-01

    Within the Quality by Design (QbD) framework proposed by the International Conference on Harmonisation (ICH), high-throughput process development (HTPD) and mechanistic modeling are of outstanding importance for future biopharmaceutical chromatography process development. In order to compare the data derived from different column scales or batch chromatographies, the amount of adsorber has to be quantified with the same noninvasive method. Similarly, an important requirement for the implementation of mechanistic modeling is the reliable determination of column characteristics such as the ionic capacity Λ for ion-exchange chromatography with the same method at all scales and formats. We developed a method to determine the ionic capacity in column and batch chromatography, based on the adsorption/desorption of the natural, uv-detectable amino acid histidine. In column chromatography, this method produces results comparable to those of classical acid-base titration. In contrast to acid-base titration, this method can be adapted to robotic batch chromatographic experiments. We are able to convert the adsorber volumes in batch chromatography to the equivalent volume of a compressed column. In a case study, we demonstrate that this method increases the quality of SMA parameters fitted to batch adsorption isotherms, and the capability to predict column breakthrough experiments. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:666-677, 2016. PMID:27324662

  8. Synthesis of a specific monolithic column with artificial recognition sites for L-glutamic acid via cryo-crosslinking of imprinted nanoparticles.

    Science.gov (United States)

    Göktürk, Ilgım; Üzek, Recep; Uzun, Lokman; Denizli, Adil

    2016-06-01

    In this study, a new molecular imprinting (MIP)-based monolithic cryogel column was prepared using chemically crosslinked molecularly imprinted nanoparticles, to achieve a simplified chromatographic separation (SPE) for a model compound, L-glutamic acid (L-Glu). Cryogelation through crosslinking of imprinted nanoparticles forms stable monolithic cryogel columns. This technique reduces the leakage of nanoparticles and increases the surface area, while protecting the structural features of the cryogel for stable and efficient recognition of the template molecule. A non-imprinted monolithic cryogel column (NIP) was also prepared, using non-imprinted nanoparticles produced without the addition of L-Glu during polymerization. The molecularly imprinted monolithic cryogel column (MIP) indicates apparent recognition selectivity and a good adsorption capacity compared to the NIP. Also, we have achieved a significant increase in the adsorption capacity, using the advantage of high surface area of the nanoparticles. PMID:25749280

  9. Axisymmetric collapses of granular columns

    Science.gov (United States)

    Lube, Gert; Huppert, Herbert E.; Sparks, R. Stephen J.; Hallworth, Mark A.

    2004-06-01

    Experimental observations of the collapse of initially vertical columns of small grains are presented. The experiments were performed mainly with dry grains of salt or sand, with some additional experiments using couscous, sugar or rice. Some of the experimental flows were analysed using high-speed video. There are three different flow regimes, dependent on the value of the aspect ratio a {=} h_i/r_i, where h_i and r_i are the initial height and radius of the granular column respectively. The differing forms of flow behaviour are described for each regime. In all cases a central, conically sided region of angle approximately 59(°) , corresponding to an aspect ratio of 1.7, remains undisturbed throughout the motion. The main experimental results for the final extent of the deposit and the time for emplacement are systematically collapsed in a quantitative way independent of any friction coefficients. Along with the kinematic data for the rate of spread of the front of the collapsing column, this is interpreted as indicating that frictional effects between individual grains in the bulk of the moving flow only play a role in the last instant of the flow, as it comes to an abrupt halt. For a {<} 1.7, the measured final runout radius, r_infty, is related to the initial radius by r_infty {=} r_i(1 {+} 1.24a); while for 1.7 {<} a the corresponding relationship is r_infty {=} r_i(1 {+} 1.6a(1/2) ). The time, t_infty, taken for the grains to reach r_infty is given by t_infty {=} 3(h_i/g)(1/2} {=} 3(r_i/g)({1/2}a^{1/2)) , where g is the gravitational acceleration. The insights and conclusions gained from these experiments can be applied to a wide range of industrial and natural flows of concentrated particles. For example, the observation of the rapid deposition of the grains can help explain details of the emplacement of pyroclastic flows resulting from the explosive eruption of volcanoes.

  10. Liquid chromatographic determination of methylxanthines and catechins in herbal preparations containing guaraná.

    Science.gov (United States)

    Carlson, M; Thompson, R D

    1998-01-01

    Herbal preparations derived from the dried seeds of guaraná (Paullinia cupana) have become a popular nutritional supplement used for stimulatory purposes. Once considered a drug substance in the United States, guaraná currently is classified as a food additive and dietary supplement. The pharmacological activity of guaraná-containing products is primarily due to methylxanthine alkaloids. For guaraná preparations, methylxanthine levels and, more significantly, the presence of several polyphenol compounds (i.e., catechins) provide phytochemical markers of authenticity. Methylxanthines and polyphenols are extracted from sample matrix with a heated phosphate buffer-methanol solution, the cooled extract is filtered, and the extract is injected into the liquid chromatographic (LC) system. A Nova-Pak C18 column eluted with phosphate buffer-methanol mobile phase (pH = 3.50) and monitored at 272 nm gave satisfactory resolution for the methylxanthines theobromine, theophylline, caffeine and the polyphenols (+)-catechin and (-)-epicatechin. Twenty-four products including dried seeds, dried paste, seed powders, tablets, and capsule formulations were assayed and conclusions were drawn about their authenticity. The LC system responded linearly to methylxanthines over the 100-fold range in concentration from 0.043 to 4.30 micrograms/mL for theobromine and caffeine and from 0.041 to 4.10 micrograms/mL for theophylline. Precision data for the 3 methylxanthines obtained from 10 different products (n = 5) gave relative standard deviation (RSD) values of 1.18-15.52% within a concentration range of 0.01-52.28 mg/g. Recoveries of methylxanthines from fortified products varied from 87.5 to 120.0%. The response for catechins was linear over a 200-fold range in concentration of 0.05-10.0 micrograms/mL. Precision data from 5 products (n = 5) gave RSD values of 1.08-5.54% within a concentration range of 0.34-32.65 mg/g. Recoveries from these products ranged from 87.7 to 109.7%. Results

  11. Recombinant protein purification using gradient-assisted simulated moving bed hydrophobic interaction chromatography. Part I: selection of chromatographic system and estimation of adsorption isotherms.

    Science.gov (United States)

    Palani, Sivakumar; Gueorguieva, Ludmila; Rinas, Ursula; Seidel-Morgenstern, Andreas; Jayaraman, Guhan

    2011-09-16

    The design of gradient simulated moving bed (SMB) chromatographic processes requires an appropriate selection of the chromatographic system followed by the determination of adsorption isotherm parameters in the relevant range of mobile phase conditions. The determination of these parameters can be quite difficult for recombinant target proteins present in complex protein mixtures. The first part of this work includes the estimation of adsorption isotherm parameters for streptokinase and a lumped impurity fraction present in an Escherichia coli cell lysate for a hydrophobic interaction chromatography (HIC) matrix. Perturbation experiments were carried out using a Butyl Sepharose matrix with purified recombinant protein on buffer equilibrated columns as well as with crude cell lysate saturated columns. The Henry constants estimated for streptokinase were found to exhibit in a wide range a linear dependence on the salt concentration in the mobile phase. These parameters were applied in subsequent investigations to design a simulated moving bed (SMB) process capable to purify in a continuous manner recombinant streptokinase from the E. coli cell lysate. PMID:21816402

  12. A new integrated membrane filtration and chromatographic device.

    Science.gov (United States)

    Xu, Yanke; Sirkar, Kamalesh K; Dai, Xiao-Ping; Luo, Robert G

    2005-01-01

    To improve protein separation, a novel integrated device combining membrane filtration and chromatography has been developed. The device basically consists of a hollow fiber filtration module whose shell side is filled with chromatographic resin beads. However, there is an essentially impermeable coated zone near the hollow fiber module outlet. The integrated device enjoys the advantages of both membrane filtration and chromatography; it also allows one to load the chromatographic media directly from the fermentation broth or lysate and separate the adsorbed proteins through the subsequent elution step in a cyclic process. Interfacial polymerization was carried out to coat the bottom section of the hollow fiber membrane; the rest of the hollow fiber membrane remained unaffected. Myoglobin (Mb) and alpha-lactalbumin (alpha-LA) were primarily used as model proteins in a binary mixture; binary mixtures of Mb and bovine serum albumin (BSA) were also investigated. Separation behaviors of binary protein mixtures were studied in devices having either an ultrafiltration (UF) or a microfiltration (MF) membrane. Experimental results show that the breakthrough time and the protein loading capacities were dramatically improved after introducing the impermeable coating in both UF and MF modules. For a synthetic yeast fermentation broth feed, four loading-washing-elution-reequilibration-based cyclic runs for separation of Mb and alpha-LA were performed in the device using a MF membrane with a coated zone without cleaning in between. The Mb and alpha-LA elution profiles for the four consecutive runs were almost superimposable. Due to lower transmembrane flux in this device plus the periodical washing-elution during the chromatographic separation, fouling was not a problem, unlike in conventional microfiltration. PMID:15801803

  13. Characterization of a natural dye by spectroscopic and chromatographic techniques

    OpenAIRE

    Espinosa Morales, Y.; Reyes, J.; Hermosín, Bernardo; Azamar-Barrios, J. A.

    2012-01-01

    Natural dyes have been extracted from both plants and animal to give color to textiles and handicrafts. This is the case of purple dye extracted from Justicia spicigera Schldt, an acanthaceae used as a color source since pre-Hispanic period in the Mayan area of Mexico and Central America. Spectroscopic (UV-Vis and FT-IR) and chromatographic (PY-GC/MS) techniques were employed in order to characterize some of their chemical properties. UV-VIS absorption spectra indicates a λmaxpeak at 581 nm, ...

  14. Methods and apparatus for analysis of chromatographic migration patterns

    Science.gov (United States)

    Stockham, Thomas G.; Ives, Jeffrey T.

    1993-01-01

    A method and apparatus for sharpening signal peaks in a signal representing the distribution of biological or chemical components of a mixture separated by a chromatographic technique such as, but not limited to, electrophoresis. A key step in the method is the use of a blind deconvolution technique, presently embodied as homomorphic filtering, to reduce the contribution of a blurring function to the signal encoding the peaks of the distribution. The invention further includes steps and apparatus directed to determination of a nucleotide sequence from a set of four such signals representing DNA sequence data derived by electrophoretic means.

  15. Oscillating water column structural model

    Energy Technology Data Exchange (ETDEWEB)

    Copeland, Guild [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Bull, Diana L [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Jepsen, Richard Alan [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Gordon, Margaret Ellen [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2014-09-01

    An oscillating water column (OWC) wave energy converter is a structure with an opening to the ocean below the free surface, i.e. a structure with a moonpool. Two structural models for a non-axisymmetric terminator design OWC, the Backward Bent Duct Buoy (BBDB) are discussed in this report. The results of this structural model design study are intended to inform experiments and modeling underway in support of the U.S. Department of Energy (DOE) initiated Reference Model Project (RMP). A detailed design developed by Re Vision Consulting used stiffeners and girders to stabilize the structure against the hydrostatic loads experienced by a BBDB device. Additional support plates were added to this structure to account for loads arising from the mooring line attachment points. A simplified structure was designed in a modular fashion. This simplified design allows easy alterations to the buoyancy chambers and uncomplicated analysis of resulting changes in buoyancy.

  16. Development, modelling, optimisation and scale-up of chromatographic purification of a therapeutic protein

    DEFF Research Database (Denmark)

    Mollerup, Jørgen; Hansen, Thomas Budde; Kidal, Steffen;

    2007-01-01

    Development of a chromatographic purification step proceeds through a number of stages. High-throughput screening techniques are used to identify suitable resins. This technique is also suitable for the design of a capture step and some intermediate chromatographic steps, but development and true...... by industry. The theory of residence time based scale-up is developed and applied. (c) 2007 Elsevier B.V. All rights reserved....... chromatographic separations. Application of simulation of chromatographic processes supports innovation, efficiency and thus quality by design in biopharmaceutical development, manufacturing, and quality assurance and it enhances process understanding to facilitate innovation and risk-based regulatory decisions......Development of a chromatographic purification step proceeds through a number of stages. High-throughput screening techniques are used to identify suitable resins. This technique is also suitable for the design of a capture step and some intermediate chromatographic steps, but development and true...

  17. 蓝萼香茶菜高效液相指纹图谱研究%Study on chromatographic fingerprint of Isodon japonica by HPLC

    Institute of Scientific and Technical Information of China (English)

    杨丽霞; 朱晓红; 刘必旺

    2015-01-01

    Objective:To study and establish the chromatographic fingerprint of Isodon japonica by RP-HPLC. Methods:The chromatographic conditions were as follows.A Diamonsil C18 column was used and the mobile phase was composed of methanol and water (70:30). The flow rate was 1.0 mL/min,the column temperature was 20 ℃ and the detection wave-length was set at 231 nm. Results:The chromatographic fingerprint of Isodon japonica was established. The similarity of 5 batches of Isodon japonica was not lower than 0.962 7. Conclusion:The quality of Isodon japonica can be controlled ef-fectively by HPLC fingerprint.%目的:采用RP-HPLC法建立蓝萼香茶菜药材的指纹图谱. 方法:采用Diamonsil钻石C18色谱柱(250 mm ×4.6 mm, 5μm);流动相为甲醇-水(体积比70:30),流速为1.0 mL/min,柱温为20℃,检测波长为231 nm. 结果:建立了蓝萼香茶菜药材的RP-HPLC指纹图谱,5批蓝萼香茶菜药材指纹图谱R≥0.962 7.结论:采用RP-HPLC指纹图谱检测技术可以有效控制蓝萼香茶菜药材的内在质量.

  18. Study on chromatographic fingerprint of Isodon japonica by HPLC%蓝萼香茶菜高效液相指纹图谱研究

    Institute of Scientific and Technical Information of China (English)

    杨丽霞; 朱晓红; 刘必旺

    2015-01-01

    Objective:To study and establish the chromatographic fingerprint of Isodon japonica by RP-HPLC. Methods:The chromatographic conditions were as follows.A Diamonsil C18 column was used and the mobile phase was composed of methanol and water (70:30). The flow rate was 1.0 mL/min,the column temperature was 20 ℃ and the detection wave-length was set at 231 nm. Results:The chromatographic fingerprint of Isodon japonica was established. The similarity of 5 batches of Isodon japonica was not lower than 0.962 7. Conclusion:The quality of Isodon japonica can be controlled ef-fectively by HPLC fingerprint.%目的:采用RP-HPLC法建立蓝萼香茶菜药材的指纹图谱. 方法:采用Diamonsil钻石C18色谱柱(250 mm ×4.6 mm, 5μm);流动相为甲醇-水(体积比70:30),流速为1.0 mL/min,柱温为20℃,检测波长为231 nm. 结果:建立了蓝萼香茶菜药材的RP-HPLC指纹图谱,5批蓝萼香茶菜药材指纹图谱R≥0.962 7.结论:采用RP-HPLC指纹图谱检测技术可以有效控制蓝萼香茶菜药材的内在质量.

  19. Use of polymeric reversed-phase columns for the characterization of polypeptides extracted from human pancreata. II. Effect of the stationary phase.

    Science.gov (United States)

    Welinder, B S

    1991-03-29

    The potential value of eight commercial available polymer-based reversed-phase (RP) columns for peptide and protein separations was evaluated using crude acetic acid extracts of normal and diabetic human pancreata and mixtures of pure polypeptides as samples. All columns were characterized with acetic acid gradients in water as mobile phase, and different chromatographic profiles were obtained depending on the type of polymer column (bare or derivatized) and the type of ligand. Some of the columns were virtually free from effects related to the polymer skeleton whereas in others the separation was influenced by both the ligand and the polymeric backbone. Two selected polymeric RP columns were, together with a silica-based C4 column, further characterized with acetonitrile gradients in trifluoroacetic acid (TFA), and the separation temperature was found to have a drastic effect on the separation efficiency for proteins with mol. wt. greater than 6000 dalton. No such effect was seen for polypeptides with mol. wt. less than 6000 dalton. Mixtures of pure peptides and proteins were separated using acetic acid gradients in water, acetonitrile or isopropanol, and normally the highest efficiency was found with the use of acetonitrile as mobile phase modifier. Isopropanol was less suitable as an organic modifier. The separation of the beta-lactoglobulin A- and B-chains may be used to give a rapid estimate of the chromatographic usability of polymer-based RP-columns for peptide and protein separations in acetic acid gradients in water and in acetonitrile gradients. Recoveries for insulin, proinsulin, growth hormone, ovalbumin and human serum albumin were measured for several polymer-based RP columns eluted with acetic acid gradients in water and with acetonitrile-based mobile phases. The highest recoveries of serum albumin and ovalbumin were found after elution with acetic acid gradients in water. PMID:1874841

  20. Development and validation of a gas chromatographic method for the assay of memantine hydrochloride in pure and tablet dosage forms

    Directory of Open Access Journals (Sweden)

    Siddappa K.

    2011-01-01

    Full Text Available A gas chromatographic method has been developed and validated for the determination of memantine hydrochloride (MMT in pure and pharmaceutical preparations. The detection was carried out using flame ionization detector. Separation was achieved on a DB-624 fused silica packed capillary column (30 m x 0.320 mm x 1.8 μm. Nitrogen was used as a carrier gas at a flow rate of 40 mL/min. The column temperature was maintained at 300°C while the temperature of injection port and detector were maintained at 270° and 300°C, respectively. Gabapentin (GPN was used as an internal standard. The procedure gave a linear response over the concentration range of 0.5-3.5 mg/mL with sufficient reproducibility. The method has been applied successfully for the determination of MMT in pure and pharmaceutical formulations. The excipients present in the formulations did not interfere with the assay procedure. The recovery values were found to be in the range of 99.85-100.1% with RSD values less than 1%. The results obtained from this method were compared with the reference method (HPTLC reported in literature and no significant difference was found statistically.

  1. Basic investigations on the trace analysis of lanthanides and actinides by gas chromatographic separation of its hexafluoroacetyl acetonates

    International Nuclear Information System (INIS)

    The fundamental knowledge for the sensitive gas chromatographic trace analysis of lanthanides and actinides as β-diketone complexes have been studied. The planned analysis method includes the steps: Extraction of the metals from acidic aqueous solution as β-diketone metallate; separation of the complexes on a GC column with back-washing of the solvent; individual detection of the complexes with ECD detectors. The systematic asigning of the properties of most of the at present available β-diketones led to hexafluoracetyl acetone as the best suitable ligand. Due to its 6 fluorine atoms, metal amounts of upto 10-4 mol can be determined in the column feeding solution. Its chemistry in aqueous solution and its extraction chemistry prove to be extremely complex and were investigated in detail. The result is quantitative extraction possibilities for the lanthanides and firstly, neptunium, in the form of mixed complexes with donor molecules. Their thermal behaviour (stability and volatility) were then investigated with thermogravimetric methods. (orig./RB)

  2. A database of chromatographic properties and mass spectra of fatty acid methyl esters from omega-3 products.

    Science.gov (United States)

    Wasta, Ziar; Mjøs, Svein A

    2013-07-19

    Fatty acids in products claimed to contain oils with the omega-3 fatty acids eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) were analyzed as fatty acid methyl esters by gas chromatography-mass spectrometry using electron impact ionization. To cover the variation in products on the market, the 20 products that were studied in detail were selected from a larger sample set by statistical methodology. The samples were analyzed on two different stationary phases (polyethylene glycol and cyanopropyl) and the fatty acid methyl esters were identified by methodology that combines the mass spectra and retention indices into a single score value. More that 100 fatty acids had a chromatographic area above 0.1% of the total, in at least one product. Retention indices are reported as equivalent chain lengths, and overlap patterns on the two columns are discussed. Both columns were found suitable for analysis of major and nutritionally important fatty acids, but the large number of minor compounds that may act as interferents will be problematic if low limits of quantification are required in analyses of similar sample types. A database of mass spectral libraries and equivalent chain lengths of the detected compounds has been compiled and is available online. PMID:23773584

  3. Automated chromatographic system with polarimetric detection laser applied in the control of fermentation processes and seaweed extracts characterization

    International Nuclear Information System (INIS)

    There are presented applications and innovations of chromatographic and polarimetric systems in which develop methodologies for measuring the input molasses and the resulting product of a fermentation process of alcohol from a rich honey and evaluation of the fermentation process honey servery in obtaining a drink native to the Yucatan region. Composition was assessed optically active substances in seaweed, of interest to the pharmaceutical industry. The findings provide measurements alternative raw materials and products of the sugar industry, beekeeping and pharmaceutical liquid chromatography with automated polarimetric detection reduces measurement times up to 15 min, making it comparable to the times of high chromatography resolution, significantly reducing operating costs. By chromatography system with polarimetric detection (SCDP) is new columns have included standard size designed by the authors, which allow process samples with volumes up to 1 ml and reduce measurement time to 15 min, decreasing to 5 times the volume sample and halving the time of measurement. Was evaluated determining the concentration of substances using the peaks of the chromatograms obtained for the different columns and calculate the uncertainty of measurements. The results relating to the improvement of a data acquisition program (ADQUIPOL v.2.0) and new programs for the preparation of chromatograms (CROMAPOL CROMAPOL V.1.0 and V.1.2) provide important benefits, which allow a considerable saving of time the processing of the results and can be applied in other chromatography systems with the appropriate adjustments. (Author)

  4. Application of Analytical Quality by Design concept for bilastine and its degradation impurities determination by hydrophilic interaction liquid chromatographic method.

    Science.gov (United States)

    Terzić, Jelena; Popović, Igor; Stajić, Ana; Tumpa, Anja; Jančić-Stojanović, Biljana

    2016-06-01

    This paper deals with the development of hydrophilic interaction liquid chromatographic (HILIC) method for the analysis of bilastine and its degradation impurities following Analytical Quality by Design approach. It is the first time that the method for bilastine and its impurities is proposed. The main objective was to identify the conditions where an adequate separation in minimal analysis duration could be achieved within a robust region. Critical process parameters which have the most influence on method performance were defined as acetonitrile content in the mobile phase, pH of the aqueous phase and ammonium acetate concentration in the aqueous phase. Box-Behnken design was applied for establishing a relationship between critical process parameters and critical quality attributes. The defined mathematical models and Monte Carlo simulations were used to identify the design space. Fractional factorial design was applied for experimental robustness testing and the method is validated to verify the adequacy of selected optimal conditions: the analytical column Luna(®) HILIC (100mm×4.6mm, 5μm particle size); mobile phase consisted of acetonitrile-aqueous phase (50mM ammonium acetate, pH adjusted to 5.3 with glacial acetic acid) (90.5:9.5, v/v); column temperature 30°C, mobile phase flow rate 1mLmin(-1), wavelength of detection 275nm. PMID:27131148

  5. Sensitive and convenient high-performance liquid chromatographic method for the determination of mitomycin C in human plasma.

    Science.gov (United States)

    Joseph, G; Biederbick, W; Woschée, U; Theisohn, M; Klaus, W

    1997-09-26

    An improved high-performance liquid chromatographic assay for the cytostatic drug mitomycin C in plasma is presented. The principal steps are precipitation of plasma proteins with acetonitrile, lyophilization of the supernatant and reversed-phase chromatography on a Hypersil ODS 5 microm column with 0.01 M NaH2PO4 buffer (pH 6.5)-methanol (70:30, v/v) in isocratic mode. At a flow-rate of 1.3 ml/min a column pressure of 180-220 bar resulted. Porfiromycin served as internal standard. UV detection was performed at 365 nm. Quantitation limit based on a coefficient of variation <10% in intra- and inter-day assay was 5 microg/l mitomycin C, detection limit based on a signal-to-noise ratio of 3 was 1 microg/l. Recovery was 100% and linearity was shown for the whole range of concentration (1-500 microg/l). None of the five drugs used during chemoembolisation interfered with the assay in vitro. The assay meets the requirements for pharmacokinetic studies of mitomycin C in patients as regards sensitivity and ease of use. PMID:9367216

  6. Fast gas chromatographic residue analysis in animal feed using split injection and atmospheric pressure chemical ionisation tandem mass spectrometry.

    Science.gov (United States)

    Tienstra, M; Portolés, T; Hernández, F; Mol, J G J

    2015-11-27

    Significant speed improvement for instrumental runtime would make GC–MS much more attractive for determination of pesticides and contaminants and as complementary technique to LC–MS. This was the trigger to develop a fast method (time between injections less than 10 min) for the determination of pesticides and PCBs that are not (or less) amenable to LC–MS. A key factor in achieving shorter analysis time was the use of split injection (1:10) which allowed the use of a much higher initial GC oven temperature. A shorter column (15 m), higher temperature ramp, and higher carrier gas flow rate (6 mL/min) further contributed to analysis-time reduction. Chromatographic resolution was slightly compromised but still well fit-for-purpose. Due to the high sensitivity of the technique used (GC–APCI-triple quadrupole MS/MS), quantification and identification were still possible down to the 10 μg/kg level, which was demonstrated by successful validation of the method for complex feed matrices according to EU guidelines. Other advantages of the method included a better compatibility of acetonitrile extracts (e.g. QuEChERS) with GC, and a reduced transfer of co-extractants into the GC column and mass spectrometer. PMID:26601712

  7. Temperature Control of Gas Chromatograph Based on Switched Delayed System Techniques

    OpenAIRE

    Xiao-Liang Wang; Ming-Xu Zhang; Kun-Zhi Liu; Xi-Ming Sun

    2014-01-01

    We address the temperature control problem of the gas chromatograph. We model the temperature control system of the gas chromatograph into a switched delayed system and analyze the stability by common Lyapunov functional technique. The PI controller parameters can be given based on the proposed linear matrix inequalities (LMIs) condition and the designed controller can make the temperature of gas chromatograph track the reference signal asymptotically. An experiment is given to illustrate the...

  8. Temperature Control of Gas Chromatograph Based on Switched Delayed System Techniques

    Directory of Open Access Journals (Sweden)

    Xiao-Liang Wang

    2014-01-01

    Full Text Available We address the temperature control problem of the gas chromatograph. We model the temperature control system of the gas chromatograph into a switched delayed system and analyze the stability by common Lyapunov functional technique. The PI controller parameters can be given based on the proposed linear matrix inequalities (LMIs condition and the designed controller can make the temperature of gas chromatograph track the reference signal asymptotically. An experiment is given to illustrate the effectiveness of the stability criterion.

  9. Evaluation and application of a mixed-mode chromatographic stationary phase in two-dimensional liquid chromatography for the separation of traditional Chinese medicine.

    Science.gov (United States)

    Wei, Zhishen; Fu, Qing; Cai, Jianfeng; Huan, Liyun; Zhao, Jianchao; Shi, Hui; Jin, Yu; Liang, Xinmiao

    2016-06-01

    In this study, two mixed-mode chromatography stationary phases (C8SAX and C8SCX) were evaluated and used to establish a two-dimensional liquid chromatography system for the separation of traditional Chinese medicine. The chromatographic properties of the mixed-mode columns were systematically evaluated by comparing with other three columns of C8, strong anion exchanger, and strong cation exchanger. The result showed that C8SAX and C8SCX had a mixed-mode retention mechanism including electrostatic interaction and hydrophobic interaction. Especially, they were suitable for separating acidic and/or basic compounds and their separation selectivities could be easily adjusted by changing pH value. Then, several off-line 2D-LC systems based on the C8SAX in the first dimension and C8SAX, C8SCX, or C8 columns in the second dimension were developed to analyze a traditional Chinese medicine-Uncaria rhynchophylla. The two-dimensional liquid chromatography system of C8SAX (pH 3.0) × C8SAX (pH 6.0) exhibited the most effective peak distribution. Finally, fractions of U. rhynchophylla prepared from the first dimension were successfully separated on the C8SAX column with a gradient pH. Thus, the mixed-mode stationary phase could provide a platform to separate the traditional Chinese medicine in practical applications. PMID:27159545

  10. Liquid chromatographic fractionations of mixtures of polystyrene oligomers

    International Nuclear Information System (INIS)

    Oligomer mixtures of 800, 2200, and 4000 molecular weight polystyrene have been fractionated using silica and bonded phase columns under similar conditions of solvent gradient and flow rate. Using a hexane tetrahydrofuran gradient, the silica and nitro phases were best in that they separated 41 and 43 oligomers, respectively. At the other extreme, a phenyl bonded phase column gave virtually no resolution using a water/THF gradient, and a cyano bonded phase column, using the earlier hexane/tetrahydrofuran system, resolved only 10 oligomers. Amino and octadecyl bonded phase columns gave results intermediate between these two extremes. The strength of the solvent used to dissolve the sample was found to be of critical importance. Use of too good a sample solvent seriously degraded the attainable resolution. When number-average and weight-average molecular weights for an 800 molecular weight polystyrene sample were calculated from the oligomer distribution, the silica column gave values which were most consistent with those reported from other methods. 5 figures, 4 tables

  11. Cryogenic gas separation with liquid exchanging columns

    International Nuclear Information System (INIS)

    An arrangement of distillation columns is disclosed for subambient distillative separation of 2 mixture of non-condensable gases wherein two columns which exchange liquid achieve a given level of separation over a smaller temperature range than that required by a single column producing the same separation. The arrangement is useful for air separation to produce medium purity (90 to 99%) O2 and/or N2

  12. Interstitial gas effect on vibrated granular columns

    OpenAIRE

    Pastenes, Javier,; Géminard, Jean-Christophe; Melo, Francisco

    2014-01-01

    Vibrated granular materials have been intensively used to investigate particle segregation, convection and heaping. We report on the behavior of a column of heavy grains bouncing on an oscillating solid surface. Measurements indicate that, for weak effects of the interstitial gas, the temporal variations of the pressure at the base of the column are satisfactorily described by considering that the column, in spite of the observed dilation, behaves like a porous solid. In addition, direct obse...

  13. Dynamic Effects of Diabatization in Distillation Columns

    OpenAIRE

    Bisgaard, Thomas; Huusom, Jakob Kjøbsted; Abildskov, Jens

    2012-01-01

    The dynamic eects of diabatization in distillation columns are investigated in simulation with primary focus on the heat-integrated distillation column (HIDiC). A generic, dynamic, rst-principle model has been formulated, which is exible to describe various diabatic distillation congurations. Dynamic Relative Gain Array and Singular Value Analysis have been applied in a comparative study of a conventional distillation column and a HIDiC. The study showed increased input-output coupling due to...

  14. Transverse Reinforcement in Reinforced Concrete Columns

    Science.gov (United States)

    Gramblička, Štefan; Veróny, Peter

    2013-11-01

    In the article we are dealing with the influence of transverse reinforcement to the resistance of a cross-section of the reinforced concrete columns and also with the effective detailing of the column reinforcement. We are verifying the correctness of design guides for detailing of transverse reinforcement. We are also taking into account the diameter of stirrups and its influence over transverse deformation of column.

  15. 3D printed titanium micro-bore columns containing polymer monoliths for reversed-phase liquid chromatography.

    Science.gov (United States)

    Gupta, Vipul; Talebi, Mohammad; Deverell, Jeremy; Sandron, Sara; Nesterenko, Pavel N; Heery, Brendan; Thompson, Fletcher; Beirne, Stephen; Wallace, Gordon G; Paull, Brett

    2016-03-01

    The potential of 3D selective laser melting (SLM) technology to produce compact, temperature and pressure stable titanium alloy chromatographic columns is explored. A micro bore channel (0.9 mm I.D. × 600 mm long) was produced within a 5 × 30 × 30 mm titanium alloy (Ti-6Al-4V) cuboid, in form of a double handed spiral. A poly(butyl methacrylate-co-ethyleneglycoldimethacrylate) (BuMA-co-EDMA) monolithic stationary phase was thermally polymerised within the channel for application in reversed-phase high-performance liquid chromatography. The prepared monolithic column was applied to the liquid chromatographic separation of intact proteins and peptides. Peak capacities of 69-76 (for 6-8 proteins respectively) were observed during isothermal separation of proteins at 44 °C which were further increased to 73-77 using a thermal step gradient with programmed temperature from 60 °C to 35 °C using an in-house built direct-contact heater/cooler platform based upon matching sized Peltier thermoelectric modules. Rapid temperature gradients were possible due to direct-contact between the planar metal column and the Peltier module, and the high thermal conductivity of the titanium column as compared to a similar stainless steel printed column. The separation of peptides released from a digestion of E.coli was also achieved in less than 35 min with ca. 40 distinguishable peaks at 210 nm. PMID:26873472

  16. Effects of temperature and mobile-phase composition on retentions in column liquid chromatography. [Hydroxyl-terminated polybutadiene

    Energy Technology Data Exchange (ETDEWEB)

    Hsu, A.

    1982-08-01

    Binary-additive mobile phase systems were investigated for a more exact control over chromatography. If the mobile phase was nonpolar binary solvents (e.g., n-hexane and dichloromethane), trace amounts of THF and/or ACN could be added to control solute retentions as a function of solvent composition. Temperature also plays an important role in the coverage of modifier molecules on the surface of the adsorbent. Higher efficiencies were obtained at lower temperatures. For chromatographic systems having large extra-column volumes, higher column temperature will also reduce column efficiency. Solvophobic effects and polar-group selectivity control the chromatographic behavior of phenols in reversed-phase liquid chromatography (RPLC). The former effect predominates with the THF system, and the latter with the MeOH system. Substituent groups decrease the hydrophobic effect of phenols in aqueous media. However, owing to steric effects, ortho-substituted phenols usually eluted later. Separation of the phenols was also found with 35% MeOH/H/sub 2/O eluent. Application of window diagrams led to baseline separation with 22% THF/H/sub 2/O. Optimum column temperature was 42/sup 0/C with a Zorbax C8 microbore column. The enthalpy-entropy compensation principle was applied to the retention data observed with reversed-phase systems. Relative retention data were found to provide a more consistent compensation temperature. RPLC was shown to be useful in the separation of high molecular-weight compounds such as hydroxyl-terminated polybutadiene (HTPB). HMDS-treated HTPB eluted without difficulty from silical gel. Sample overload can provide unique separations in GPC. (DLC)

  17. Gas chromatographic isolation technique for compound-specific radiocarbon analysis

    International Nuclear Information System (INIS)

    Full text: We present here a gas chromatographic isolation technique for the compound-specific radiocarbon analysis of biomarkers from the marine sediments. The biomarkers of fatty acids, hydrocarbon and sterols were isolated with enough amount for radiocarbon analysis using a preparative capillary gas chromatograph (PCGC) system. The PCGC systems used here is composed of an HP 6890 GC with FID, a cooled injection system (CIS, Gerstel, Germany), a zero-dead-volume effluent splitter, and a cryogenic preparative collection device (PFC, Gerstel). For AMS analysis, we need to separate and recover sufficient quantity of target individual compounds (>50 μgC). Yields of target compounds from C14 n-alkanes to C40 to C30 n-alkanes and approximately that of 80% for higher molecular weights compounds more than C30 n-alkanes. Compound specific radiocarbon analysis of organic compounds, as well as compound-specific stable isotope analysis, provide valuable information on the origins and carbon cycling in marine system. Above PCGC conditions, we applied compound-specific radiocarbon analysis to the marine sediments from western north Pacific, which showed the possibility of a useful chronology tool for estimating the age of sediment using organic matter in paleoceanographic study, in the area where enough amounts of planktonic foraminifera for radiocarbon analysis by accelerator mass spectrometry (AMS) are difficult to obtain due to dissolution of calcium carbonate. (author)

  18. Quantitative structure-(chromatographic) retention relationship models for dissociating compounds.

    Science.gov (United States)

    Kubik, Łukasz; Wiczling, Paweł

    2016-08-01

    The aim of this work was to develop mathematical models relating the hydrophobicity and dissociation constant of an analyte with its structure, which would be useful in predicting analyte retention times in reversed-phase liquid chromatography. For that purpose a large and diverse group of 115 drugs was used to build three QSRR models combining retention-related parameters (logkw-chromatographic measure of hydrophobicity, S-slope factor from Snyder-Soczewinski equation, and pKa) with structural descriptors calculated by means of molecular modeling for both dissociated and nondissociated forms of analytes. Lasso, Stepwise and PLS regressions were used to build statistical models. Moreover a simple QSRR equations based on lipophilicity and dissociation constant parameters calculated in the ACD/Labs software were proposed and compared with quantum chemistry-based QSRR equations. The obtained relationships were further used to predict chromatographic retention times. The predictive performances of the obtained models were assessed using 10-fold cross-validation and external validation. The QSRR equations developed were simple and were characterized by satisfactory predictive performance. Application of quantum chemistry-based and ACD-based descriptors leads to similar accuracy of retention times' prediction. PMID:26960942

  19. Reinforced concrete columns of variable cross section

    OpenAIRE

    Brant, N.F.A.

    1984-01-01

    The results of a series of 19 full scale tests carried out on pin-ended reinforced concrete columns are reported. The columns tested had either tapered rectangular sections along the length or octagonal cross sections. All columns, except the last 6, were subjected to uniaxial eccentricities at one of the ends (the stronger end), and a nominally concentric load at the other end. For the case of the last six columns the loading applied at the stronger end was biaxially eccentric. For each of t...

  20. Picobubble enhanced column flotation of fine coal

    Energy Technology Data Exchange (ETDEWEB)

    Tao, D.; Yu, S.; Parekh, B.K. [University of Kentucky, Lexington, KY (United States). Mining Engineering

    2006-07-01

    The purpose is to study the effectiveness of picobubbles in the column flotation of -28 mesh fine coal particles. A flotation column with a picobubble generator was developed and tested for enhancing the recovery of ultrafine coal particles. The picobubble generator was designed using the hydrodynamic cavitation principle. A metallurgical and a steam coal were tested in the apparatus. The results show that the use of picobubbles in a 2in. flotation column increased the recovery of fine coal by 10 to 30%. The recovery rate varied with feed rate, collector dosage, and other column conditions. 40 refs., 8 figs., 2 tabs.

  1. Computer-aided optimization of gas chromatographic separation

    International Nuclear Information System (INIS)

    The use of computer-aided optimization of separations has become widely used in liquid chromatography (LC) in the past few years, but its application is seldom used in gas chromatography (GC). In LC, adjustment of isocratic mobile phase strength and gradient steepness is a powerful technique to control relative peak spacing (selectivity). In contrast, improvement of GC separation usually is achieved by increasing the column plate number (via increases in column length), and/or by changing the column type. In this paper, we will discuss examples of isothermal, temperature programmed, and multi-step temperature programmed optimization of GC separation. These results will be compared to those obtained by LC using commercial software

  2. Punching Shear Behavior of RC Slab-Column Connections with Nonrectangular Columns

    Institute of Scientific and Technical Information of China (English)

    Liu Wenting; Huang Chengkui; Zhang Ruihe

    2005-01-01

    This paper present an experimental study on the RC slab-column connections with nonrectangular columns, namely cross-shaped column, T-shaped column and L-shaped column. The punching shear deformation and strength characteristics of slab-column connections with nonrectangular columns under punching shear load are investigated. Nine specimens with the three kinds of nonrectangular columns and two reference specimens with square columns are tested. The tested ultimate loads, deformations, and failure modes of specimens are presented and discussed. Test results reveal that the punching shear strength and ductility of the connections with nonrectangular columns are higher than those of the corresponding connections with square columns, and also prove that the application of nonrectangular columns to flat-plate structure was feasible. Based on the test results, one method of calculating punching shear strength of connections with nonrectangular columns is proposed, which conforms with the current design practice of China. The test results on the punching shear strength are compared with the predictions of the formulas proposed by codes of several different countrie; and the predictions given by ACI code and China code are found to be conservative as the reinforcement ratio is increased.

  3. CHROMATOGRAPHIC SEPERATION AND PURIFICATION OF HUMAN CHORIONIC GONADOTROPIN

    Institute of Scientific and Technical Information of China (English)

    WangHaifeng; XuYutai; 等

    1995-01-01

    Separation and purification of human chorionic gonadotropion(HCG) in the urine sample of early pregnant women by D3520 resin adsorption chromatography is reported.The crude product obtained by DEAE-Cellulose 23 and DEAE-Sephadex A50 column chromatography showed a high activity of HCG. Further purification of the sample by gel filtration chromatography on a Sephadex G75 column gives a final preparation of 6000-6500 IU/mg.The preparation meets the requirements of the pyrogn test in Chinese Law of Pharmacopeia.

  4. Rapid and simultaneous determination of imidazolium and pyridinium ionic liquid cations by ion-pair chromatography using a monolithic column

    Institute of Scientific and Technical Information of China (English)

    Xu Huang; Hong Yu; Ying Jie Dong

    2012-01-01

    A method for rapid and simultaneous determination of imidazolium and pyridinium ionic liquid cations by ion-pair chromatography with ultraviolet detection was developed.Chromatographic separations were performed on a reversed-phase silica-based monolithic column using 1-heptanesulfonic acid sodium-acetonitrile as mobile phase.The effects of ion-pair reagent and acetonitrile concentration on retention of the cations were investigated.The retention times of the cations accord with carbon number rule.The method has been successfully applied to the determination of four ionic liquids synthesized by organic chemistry laboratory.

  5. Simultaneous effect of organic modifier and physicochemical parameters of barbiturates on their retention on a narrow-bore PGC column.

    Science.gov (United States)

    Forgács, Esther; Cserháti, Tibor; Miksik, Ivan; Echardt, Adam; Deyl, Zdenek

    2004-02-01

    The retention time of 22 barbituric acid derivatives was measured on a narrow-bore porous graphitized carbon (PGC) column using water-dioxane mixtures as mobile phases. The capacity factor (k), theoretical plate number (N), and asymmetry factor (AF) were calculated for each solute in each mobile phase. The relationships between chromatographic characteristics and physicochemical parameters of solutes were elucidated by stepwise regression analysis (SRA). SRA indicated that the binding of barbiturates to the PGC surface is of mixed character electrostatic and apolar interactive forces are equally involved. Sterical correspondence between the surface of the stationary phase and the solutes also exert a significant influence on the retention behavior. PMID:14698263

  6. Column flotation in an oilsand application

    Energy Technology Data Exchange (ETDEWEB)

    Wiwchar, K.; Dang, L.; Marks, A.; Mbaja, E. [Suncor Energy Inc. Oil Sands, Fort McMurray, AB (Canada); Furey, J. [Canadian Process Technologies Inc., Vancouver, BC (Canada)

    2004-07-01

    In March 2003, Suncor Energy Inc. began pilot operation of a flotation column designed by Canadian Process Technologies Inc. (CPT). Oilsands from the Suncor mine are mixed with hot process water and the bitumen is slurried in a pipeline. Large separation cells float off the bitumen product, which is then steam or static deaerated and sent to a secondary extraction plant for further cleaning. The tailings flotation froth product is processed at the final tails pumphouse where it is recycled to the oilsand feed. This pilot operation tested the performance of the CPT column against the performance of scavenger banks that use middlings streams. It was determined that if the flotation column recovery results surpassed the scavenger banks, columns would replace the Denver scavenger banks used in existing extraction plants. Pilot scale tests used a CPT 4 foot diameter flotation column. Previous bench scale tests at the University of Alberta were based on 2.4 inch and 20 inch diameter columns. The columns received middlings stream feed from deep cone separation cells. The column operates in parallel with a set of WEMCO flotation cells. The evaluation compared the recovery, tails losses, and concentrate quality of the two systems. All types of mine ore grades were tested. In order to optimize recovery and final product quality, adjustments were made to wash water flow and temperature, sparger nozzle size and location, sparger air/water flow rates, and column residence time. Column flotation is typically used in the final stages of sulphide cleaning and flotation of phosphate or iron ore. Preliminary results indicate that the use of the CPT flotation column in an oilsand application was successful and may prove to be an inexpensive method to recover bitumen from a middlings stream and to produce a product suitable for froth treatment. 2 refs., 1 tab., 5 figs.

  7. Column: Factors Affecting Data Decay

    Directory of Open Access Journals (Sweden)

    Kevin Fairbanks

    2012-06-01

    Full Text Available In nuclear physics, the phrase decay rate is used to denote the rate that atoms and other particles spontaneously decompose. Uranium-235 famously decays into a variety of daughter isotopes including Thorium and Neptunium, which themselves decay to others. Decay rates are widely observed and wildly different depending on many factors, both internal and external. U-235 has a half-life of 703,800,000 years, for example, while free neutrons have a half-life of 611 seconds and neutrons in an atomic nucleus are stable.We posit that data in computer systems also experiences some kind of statistical decay process and thus also has a discernible decay rate. Like atomic decay, data decay fluctuates wildly. But unlike atomic decay, data decay rates are the result of so many different interplaying processes that we currently do not understand them well enough to come up with quantifiable numbers. Nevertheless, we believe that it is useful to discuss some of the factors that impact the data decay rate, for these factors frequently determine whether useful data about a subject can be recovered by forensic investigation.(see PDF for full column

  8. CFD simulation of bubble column

    Energy Technology Data Exchange (ETDEWEB)

    Ekambara, K., E-mail: ekambara@ualberta.c [Department of Chemical and Materials Engineering, University of Alberta, 536 CME Building, Edmonton, AB, T6G 2G6 (Canada); Dhotre, M.T. [Thermal-Hydraulics Laboratory, Nuclear Energy and Safety Department, Paul Scherrer Institute, CH-5232 Villigen PSI (Switzerland)

    2010-05-15

    Three-dimensional simulations of gas-liquid flow in the bubble column using the Euler-Euler approach is presented. The attempt is made to assess the performance and applicability of different turbulence models namely, k-epsilon, k-epsilon RNG, k-omega, Reynolds stress model (RSM) and large eddy simulation (LES) using a commercial code (ANSYS-CFX). For this purpose, the predictions are compared against the experimental data of . Performance of the turbulence models is assessed on basis of comparison of axial liquid velocity, fractional gas hold-up, turbulent kinetic energy and turbulent eddy dissipation rate. All the non-drag (turbulent dispersion, virtual mass and lift force) and drag force were incorporated in the model. The low-Reynolds number treatment of the k-omega yields a better qualitative prediction than the k-epsilon model. The RSM predictions are comparable with LES results and seemed to give better prediction near the sparger, where the flow is more anisotropic and gives a clue why RANS approaches fails to predict the flow in this region. However, the large eddy simulations showed good agreement with the experimental data, but requires higher computational time than RSM.

  9. Application of gas-liquid chromatography to the analysis of essential oils. Part XVII. Fingerprinting of essential oils by temperature-programmed gas-liquid chromatography using capillary columns with non-polar stationary phases. Analytical methods committee.

    Science.gov (United States)

    1997-10-01

    Problems in obtaining reproducible results when 'fingerprinting' essential oils by temperature-programmed gas-liquid chromatography have been reported on in Parts VII and VIII of this series. Those reports were concerned with the general problems and the use of packed columns. This report is concerned with the use of capillary columns and non-polar stationary phases. A collaborative study using capillary columns with non-polar stationary phases has resulted in a method which specifies the 'g-pack value' of a column and gives reproducible relative retention indices for the test compounds limonene, acetophenone, linalol, naphthalene, linalyl acetate and cinnamyl alcohol. The method has been applied successfully to the examination of oil of rosemary. A recommended method is given for the reproducible temperature-programmed gas-liquid chromatographic fingerprinting of essential oils using capillary columns with non-polar stationary phases. PMID:9463975

  10. High-performance liquid chromatographic determination of memantine hydrochloride in rat plasma using sensitive fluorometric derivatization.

    Science.gov (United States)

    Xie, Mei-Fen; Zhou, Wei; Tong, Xin-Yi; Chen, Yi-Le; Cai, Yi; Li, Yan; Duan, Geng-Li

    2011-02-01

    In this study, we investigated a simple, sensitive and reliable liquid chromatography-fluorescence detection method for the determination of memantine hydrochloride in rat plasma which was based on derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl). For the first time, FMOC-Cl was introduced into derivatization of memantine hydrochloride in rat plasma. The amino groups of memantine hydrochloride and amantadine hydrochloride (internal standard) were trapped with FMOC-Cl to form memantine hydrochloride-FMOC-Cl and amantadine hydrochloride-FMOC-Cl compositions, which can be very compatible for LC-FLD. Precipitation of plasma proteins by acetonitrile was followed by vortex mixing and centrifugation. Chromatographic separation was performed on a C(18) column (DIAMONSIL 150 × 4.6 mm, id 5 μm) with a mobile phase consisting of acetonitrile and water at a flow rate of 1.0 mL/min. The retention times of memantine hydrochloride-FMOC-Cl and amantadine hydrochloride-FMOC-Cl compositions were 23.69 and 40.27 min, respectively. Optimal conditions for the derivatization of memantine hydrochloride were also described. The limit of quantification (LOQ) was 25 ng/mL for memantine hydrochloride in plasma, the linear range was 0.025-5.0 μg/mL in plasma with a correlation coefficient (r) of 0.9999. The relative standard deviations (RSDs) of intra-day and inter-day assays were 4.46-12.19 and 5.23-11.50%, respectively. The validated method was successfully applied to the determination of memantine hydrochloride in rat plasma samples. PMID:21268245

  11. Extraction chromatographic separation of Sr, Pu and Am in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Sidhu, Rajdeep

    2004-04-01

    An accurate determination of radionuclides from various sources in the environment is essential for assessment of the potential hazards and suitable countermeasures both in case of an authorised release, accidents and routine surveillance. Due to the short range of alpha and beta radiation, the accurate determination of pure alpha and beta emitters must always include radiochemical separations to separate the analytes from the matrix and from other interfering stable and radioactive nuclides. Hence, the procedures used for their determination are usually tedious and involve several preconcentration and separation steps. This work deals with the determination of {sup 90}Sr, {sup 241}Am, {sup 238}Pu, {sup 239,240}Pu and {sup 244}Cm, whic some of the most important artificial radionuclides. Due to either absence or low yield of gamma radiation, a secure determination of low concentrations of all these nuclides requires a dedicated chemistry. Selective extraction chromatographic resins (TRU- and Sr-Resin) have been utilised to develop new procedures for the analyses of Pu, Am and Cm isotopes in seawater and both these and {sup 90}Sr in soil, sediment, urine and low-level liquid radioactive effluents. The proposed method for the analyses of Pu and Am in seawater offers a quick and secure mode for the determination of these radionuclides in marine waters. Combined pre-concentration of actinides and strontium (oxalate or phosphate precipitation) followed by dual column separation on TRU- and Sr-Resin significantly reduces the through put time and costs compared to traditional ion exchange and precipitation methods. The greatest gain in productivity and environmental friendliness is achieved in Sr separations using Sr-Resin instead of precipitations involving fuming nitric acid and oxalate, hydroxide, chromate and carbonate precipitations. (author)

  12. Optimal performance of single-column chromatography and simulated moving bed processes for the separation of optical isomers

    International Nuclear Information System (INIS)

    Chromatography has been established as the method of choice for the separation and purification of optically pure drugs which has a market size of about 250 billion USD. Single column chromatography (SCC) is commonly used in the development and testing phase of drug development while multi-column Simulated Moving Bed (SMB) chromatography is more suitable for large scale production due to its continuous nature. In this study, optimal performance of SCC and SMB processes for the separation of optical isomers under linear and overloaded separation conditions has been investigated. The performance indicators, namely productivity and desorbent requirement have been compared under geometric similarity for the separation of a mixture of guaifenesin, and Tröger's base enantiomers. SCC process has been analyzed under equilibrium assumption i.e., assuming infinite column efficiency, and zero dispersion, and its optimal performance parameters are compared with the optimal prediction of an SMB process by triangle theory. Simulation results obtained using actual experimental data indicate that SCC may compete with SMB in terms of productivity depending on the molecules to be separated. Besides, insights into the process performances in terms of degree of freedom and relationship between the optimal operating point and solubility limit of the optical isomers have been ascertained. This investigation enables appropriate selection of single or multi-column chromatographic processes based on column packing properties and isotherm parameters.

  13. Optimal performance of single-column chromatography and simulated moving bed processes for the separation of optical isomers

    Science.gov (United States)

    Medi, Bijan; Kazi, Monzure-Khoda; Amanullah, Mohammad

    2013-06-01

    Chromatography has been established as the method of choice for the separation and purification of optically pure drugs which has a market size of about 250 billion USD. Single column chromatography (SCC) is commonly used in the development and testing phase of drug development while multi-column Simulated Moving Bed (SMB) chromatography is more suitable for large scale production due to its continuous nature. In this study, optimal performance of SCC and SMB processes for the separation of optical isomers under linear and overloaded separation conditions has been investigated. The performance indicators, namely productivity and desorbent requirement have been compared under geometric similarity for the separation of a mixture of guaifenesin, and Tröger's base enantiomers. SCC process has been analyzed under equilibrium assumption i.e., assuming infinite column efficiency, and zero dispersion, and its optimal performance parameters are compared with the optimal prediction of an SMB process by triangle theory. Simulation results obtained using actual experimental data indicate that SCC may compete with SMB in terms of productivity depending on the molecules to be separated. Besides, insights into the process performances in terms of degree of freedom and relationship between the optimal operating point and solubility limit of the optical isomers have been ascertained. This investigation enables appropriate selection of single or multi-column chromatographic processes based on column packing properties and isotherm parameters.

  14. A gas chromatographic instrument for measurement of hydrogen cyanide in the lower atmosphere

    Directory of Open Access Journals (Sweden)

    J. L. Ambrose

    2012-06-01

    Full Text Available A gas-chromatographic (GC instrument was developed for measuring hydrogen cyanide (HCN in the lower atmosphere. The main features of the instrument are (1 a cryogen-free cooler for sample dehumidification and enrichment, (2 a porous polymer PLOT column for analyte separation, (3 a flame thermionic detector (FTD for sensitive and selective detection, and (4 a dynamic dilution system for calibration. We deployed the instrument for a ∼4 month period from January–June, 2010 at the AIRMAP atmospheric monitoring station Thompson Farm 2 (THF2 in rural Durham, NH. A subset of measurements made during 3–31 March is presented here with a detailed description of the instrument features and performance characteristics. The temporal resolution of the measurements was ~20 min, with a 75 s sample capture time. The 1σ measurement precision was <10% and the instrument response linearity was excellent on a calibration scale of 0.10–0.75 ppbv (±5%. The estimated method detection limit (MDL and accuracy were 0.021 ppbv and 15%, respectively. From 3–31 March 2010, ambient HCN mixing ratios ranged from 0.15–1.0 ppbv (±15%, with a mean value of 0.36 ± 0.16 ppbv (1σ. The approximate mean background HCN mixing ratio of 0.20 ± 0.04 ppbv appeared to agree well with tropospheric column measurements reported previously. The GC-FTD HCN measurements were strongly correlated with acetonitrile (CH3CN measured concurrently with a proton transfer-reaction mass spectrometer (PTR-MS, as anticipated given our understanding that the nitriles share a common primary biomass burning source to the global atmosphere. The nitriles were overall only weakly correlated with carbon monoxide (CO, which is reasonable considering the greater diversity of sources for CO. However, strong correlations with CO were observed on several nights under stable atmospheric conditions and suggest regional combustion-based sources for the nitriles. These results demonstrate that

  15. Similarity analyses of chromatographic herbal fingerprints: A review

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •Similarity analyses of herbal fingerprints are reviewed. •Different (dis)similarity approaches are discussed. •(Dis)similarity-metrics and exploratory-analysis approaches are illustrated. •Correlation and distance-based measures are overviewed. •Similarity analyses illustrated by several case studies. -- Abstract: Herbal medicines are becoming again more popular in the developed countries because being “natural” and people thus often assume that they are inherently safe. Herbs have also been used worldwide for many centuries in the traditional medicines. The concern of their safety and efficacy has grown since increasing western interest. Herbal materials and their extracts are very complex, often including hundreds of compounds. A thorough understanding of their chemical composition is essential for conducting a safety risk assessment. However, herbal material can show considerable variability. The chemical constituents and their amounts in a herb can be different, due to growing conditions, such as climate and soil, the drying process, the harvest season, etc. Among the analytical methods, chromatographic fingerprinting has been recommended as a potential and reliable methodology for the identification and quality control of herbal medicines. Identification is needed to avoid fraud and adulteration. Currently, analyzing chromatographic herbal fingerprint data sets has become one of the most applied tools in quality assessment of herbal materials. Mostly, the entire chromatographic profiles are used to identify or to evaluate the quality of the herbs investigated. Occasionally only a limited number of compounds are considered. One approach to the safety risk assessment is to determine whether the herbal material is substantially equivalent to that which is either readily consumed in the diet, has a history of application or has earlier been commercialized i.e. to what is considered as reference material. In order

  16. Similarity analyses of chromatographic herbal fingerprints: A review

    Energy Technology Data Exchange (ETDEWEB)

    Goodarzi, Mohammad [Department of Analytical Chemistry and Pharmaceutical Technology, Center for Pharmaceutical Research, Vrije Universiteit Brussel, Laarbeeklaan 103, B-1090 Brussels (Belgium); Russell, Paul J. [Safety and Environmental Assurance Centre, Unilever, Colworth Science Park, Sharnbrook, Bedfordshire MK44 1LQ (United Kingdom); Vander Heyden, Yvan, E-mail: yvanvdh@vub.ac.be [Department of Analytical Chemistry and Pharmaceutical Technology, Center for Pharmaceutical Research, Vrije Universiteit Brussel, Laarbeeklaan 103, B-1090 Brussels (Belgium)

    2013-12-04

    Graphical abstract: -- Highlights: •Similarity analyses of herbal fingerprints are reviewed. •Different (dis)similarity approaches are discussed. •(Dis)similarity-metrics and exploratory-analysis approaches are illustrated. •Correlation and distance-based measures are overviewed. •Similarity analyses illustrated by several case studies. -- Abstract: Herbal medicines are becoming again more popular in the developed countries because being “natural” and people thus often assume that they are inherently safe. Herbs have also been used worldwide for many centuries in the traditional medicines. The concern of their safety and efficacy has grown since increasing western interest. Herbal materials and their extracts are very complex, often including hundreds of compounds. A thorough understanding of their chemical composition is essential for conducting a safety risk assessment. However, herbal material can show considerable variability. The chemical constituents and their amounts in a herb can be different, due to growing conditions, such as climate and soil, the drying process, the harvest season, etc. Among the analytical methods, chromatographic fingerprinting has been recommended as a potential and reliable methodology for the identification and quality control of herbal medicines. Identification is needed to avoid fraud and adulteration. Currently, analyzing chromatographic herbal fingerprint data sets has become one of the most applied tools in quality assessment of herbal materials. Mostly, the entire chromatographic profiles are used to identify or to evaluate the quality of the herbs investigated. Occasionally only a limited number of compounds are considered. One approach to the safety risk assessment is to determine whether the herbal material is substantially equivalent to that which is either readily consumed in the diet, has a history of application or has earlier been commercialized i.e. to what is considered as reference material. In order

  17. Rasch models with exchangeable rows and columns

    DEFF Research Database (Denmark)

    Lauritzen, Steffen Lilholt

    The article studies distributions of doubly infinite binary matrices with exchangeable rows and columns which satify the further property that the probability of any $m \\times n$ submatrix is a function of the row- and column sums of that matrix. We show that any such distribution is a (unique...

  18. Ion chromatographic system with a novel switching suppression device.

    Science.gov (United States)

    Sato, Shinji; Ogura, Yutaka; Miyanaga, Akiyoshi; Sugimoto, Tadanori; Tanaka, Kazuhiko; Moriyama, Hiroyuki

    2002-05-17

    Ion chromatography (IC) has been a powerful tool for measuring ionic species in environmental samples such as tap, river and drain waters. Suppressor modules (membrane and disposable column types) have been used for reducing the background of a baseline. A new type of suppressor device, which has a suppressor resin and switching valve was developed. Fresh ionic resin is introduced into a groove for each analysis to perform the suppression of the working eluent. The eluent composition for obtaining higher sensitivity and better resolutions among ionic species and carbonate ion was also investigated. Although carbonate buffers are used for ion separation in general, the separation of carbonate ion from other ions was not achieved. A borate eluent resulted in good resolutions and higher sensitivity. A new column was also developed for obtaining higher column efficiency and resolution. The optimization of anion separation using a new IC system (IC-2001) that consists of a new suppressor device, an anion-exchange column (TSKgel SuperIC-Anion, 150x4.6 mm), an autosampler, a conductivity cell and a pump in a compact module is described. PMID:12108667

  19. How to Calculate Molecular Column Density

    CERN Document Server

    Mangum, Jeffrey G

    2015-01-01

    The calculation of the molecular column density from molecular spectral (rotational or ro-vibrational) transition measurements is one of the most basic quantities derived from molecular spectroscopy. Starting from first principles where we describe the basic physics behind the radiative and collisional excitation of molecules and the radiative transfer of their emission, we derive a general expression for the molecular column density. As the calculation of the molecular column density involves a knowledge of the molecular energy level degeneracies, rotational partition functions, dipole moment matrix elements, and line strengths, we include generalized derivations of these molecule-specific quantities. Given that approximations to the column density equation are often useful, we explore the optically thin, optically thick, and low-frequency limits to our derived general molecular column density relation. We also evaluate the limitations of the common assumption that the molecular excitation temperature is con...

  20. Modeling of column apparatuses: A review

    Energy Technology Data Exchange (ETDEWEB)

    Doichinova, M., E-mail: mar-doych@mail.bg, E-mail: petyabs@yahoo.com; Popova-Krumova, P., E-mail: mar-doych@mail.bg, E-mail: petyabs@yahoo.com [Institute of Chemical Engineering, Bulgarian Academy of Sciences, Acad. St.Angelov str., Bl. 103, 1113 Sofia (Bulgaria)

    2013-12-18

    This paper presents a review of the modeling method on the base of the physical approximations of the mechanics of continua, which have been developed for processes in column apparatuses. This method includes diffusion type of model for modeling of mass transfer with chemical reaction in column apparatuses with and without circulation zones. The diffusion type of model is used for modeling of scale effect in column apparatuses too. The study concluded that the proposal method is possibility for investigation the influence of radial non uniformity of the velocity distribution on the process efficiency, influence of zones breadths on the mass transfer efficiency in the column. The method of the column apparatuses modeling can be used for modeling of physical and chemical absorption, chemical adsorption, homogeneous and heterogeneous (catalytic) chemical reactions, airlift reactors for chemical and photochemical reactions.

  1. Pressure Drop Measurements on Distillation Columns

    Institute of Scientific and Technical Information of China (English)

    T.J. Cai; M.R. Resetarits

    2011-01-01

    Pressure drops are of major importance for distillation/absorption columns. This paper mainly discusses how to correctly measure, interpret and use pressure drop data. The possible causes of incorrect pressure drop measurements are studied including the effects of pressure tap dimensions, locations, and vapor condensation etc. The effect of the static head of vapor on the pressure drop data and column pressures is evaluated. Variations of sectional pressure drops along the column are investigated based on the experimental data obtained from commercial size distillation columns at Fractionation Research, Inc. (FRI). For a packed column, it is found that the spacing between the liquid distributor and the top of the bed affects the overall pressure drop measurements, which is confirmed by a fundamental fluid dynamics analysis.

  2. Standardization of the measurement of dihydro testosterone by radioimmunoassay by after celite column chromatography

    International Nuclear Information System (INIS)

    We developed a method for measuring dihydro testosterone after previous chromatography. One ml of serum containing 1000 cpm of tritiated dihydro testosterone was extracted with hexane ethyl acetate (2:3) dried diluted with non saturated iso octane and injected in the column previously washed with 3.5 ml of pure iso octane. The serum was eluted from the column with pure iso octane (3.5 ml) followed by 5% ethyl acetate in iso octane. The quantity of tritiated dihydro testosterone which was recovered 50% and 80%in all assays. This paper measured dihydro testosterone e testosterone and testosterone/dihydro testosterone ratio in the following groups. GROUP I: Forty one normal adult subjects in basal conditions, with chronological age varying from 19 to 40 years old. GROUP II: Six normal adult subjects with chronological age between 21 and 33 years old, evaluated in basal conditions and after stimulus with 6000 UI of human chorionic Gonadotropin. GROUP III: Seven pre-puberal children with chronological age varying from 2 to 7 years old. GROUP IV: Eight patients with chronological age varying from 13 to 33 years old with male pseudo- hermaphroditism due to 5-alpha-reductase deficiency in basal conditions. This paper conclude that the measurement of dihydro testosterone in celite column chromatograph is an affordable, easy-to-perform method which was able to identify patients with male pseudo-hermaphroditism due to 5-alpha-reductase deficiency. (author)

  3. Fast determination of biogenic amines in beverages by a core-shell particle column.

    Science.gov (United States)

    Preti, Raffaella; Antonelli, Marta Letizia; Bernacchia, Roberta; Vinci, Giuliana

    2015-11-15

    A fast and reliable HPLC method for the determination of 11 biogenic amines in beverages has been performed. After pre-column derivatization with dansyl-chloride a Kinetex C18 core-shell particle column (100 mm × 4.6 mm, 2.6 μm particle size) has been employed and the biogenic amines were identified and quantified in a total run time of 13 min with ultraviolet (UV) or fluorescence detection (FLD). Chromatographic conditions such as column temperature (kept at 50 °C), gradient elution and flow rate have been optimized and the method has been tested on red wine and fruit nectar. The proposed method is enhanced in terms of reduced analysis time and eluent consumption with respect of classical HPLC method as to be comparable to UHPLC methods. Green and cost-effective, this method can be used as a quality-control tool for routine quantitative analysis of biogenic amines in beverages for the average laboratory. PMID:25977063

  4. Simple determination of terbutaline in dog plasma by column-switching liquid chromatography.

    Science.gov (United States)

    Zhang, Y; Zhang, Z R

    2004-06-15

    Terbutaline is a beta-adrenergic receptor antagonist that acts as a bronchodilator in the treatment of asthma and chronic bronchitis. In the present work, a column-switching high-performance liquid chromatographic method was developed to monitor terbutaline sulphate in dog plasma. The system consists of a C2 pre-column (PC) and a C18 analytical column connected in series via a switching valve. Atenolol was used as the internal standard. Good linearity was achieved in the range of 5-800 ng/ml plasma. The mean intra- and inter-assay variation coefficients for this analysis were 2.3 and 4.7%, respectively. The average recovery for terbutaline was 87.4% from plasma. The mean concentration after three freeze-thaw cycles was 99.4% of the normal value. The analytical sensitivity and accuracy of this assay is adequate for characterisation of the pharmacokinetics of oral administration of terbutaline to dogs and has been successfully used to provide pharmacokinetic data using pulsatile and immediate-release tablets. PMID:15135092

  5. Separation of human immunoglobulin G subclasses on a protein A monolith column.

    Science.gov (United States)

    Leblebici, Pelin; Leblebici, M Enis; Ferreira-da-Silva, Frederico; Rodrigues, Alírio E; Pais, Luís S

    2014-07-01

    Monolithic columns have attracted significant attention for the purification of large biomolecules. In the present study, a step gradient elution method was evaluated for the separation of human immunoglobulin G (hIgG) into its subclasses on CIM (convective interaction media) r-protein A (recombinant protein A) monolithic column. hIgG was loaded onto the column and bound protein was eluted with a pH gradient. The subclass content of the eluted fractions was analyzed by enzyme-linked immunosorbent assay (ELISA). Results showed that separation of IgG3 from the other three subclasses can be successfully achieved with high selectivity (100%) and throughput on monolithic media. It was also revealed that enriched fractions of IgG1 and IgG2 could be obtained from purified hIgG in a 28min long chromatographic run. Three fractions with high IgG1 content (89.1%, 94.3% and 88.8%) were recovered. Furthermore, IgG2 was enriched to 64% successfully. A rapid step gradient elution scheme without any additives in buffers was proven to obtain enriched preparations of the two important subclasses with high throughput. The separation time can be reduced even more by increasing the flow rate without any loss in selectivity, which will be beneficial in industrial scale applications. PMID:24907548

  6. The setup of an extraction system coupled to a hydrogen isotopes distillation column

    International Nuclear Information System (INIS)

    Among the most difficult problems of cryogenic distillation one stands apart: the extraction of the heavy fraction. By an optimal design of the cycle scheme, this problem could be avoided. A 'worst case scenario' is usually occurring when the extracted fraction consists of one prevalent isotope such as hydrogen and small amounts of the other two hydrogen isotopes (deuterium and/or tritium). This situation is further complicated by two parameters of the distillation column: the extraction flow rate and the hold-up. The present work proposes the conceptual design of an extraction system associated to the cryogenic distillation column used in hydrogen separation processes. During this process, the heavy fraction (DT, T2) is separated, its concentration being the highest at the bottom of the distillation column. From this place the extraction of the gaseous phase can now begin. Being filled with adsorbent, the extraction system is used to temporarily store the heavy fraction. Also the extraction system provides samples for the gas Chromatograph. The research work is focused on the existent pilot plant for tritium and deuterium separation from our institute to validate the experiments carried out until now. (authors)

  7. Determination of nutrients in the presence of high chloride concentrations by column-switching ion chromatography.

    Science.gov (United States)

    Bruno, P; Caselli, M; de Gennaro, G; De Tommaso, B; Lastella, G; Mastrolitti, S

    2003-06-27

    Determination of inorganic anions in waters of high salinity is one of the most difficult task in analytical chemistry. A simple column-switching method, based on an original chromatographic set-up, for the determination of nutrients (nitrate, nitrite and phosphate) in chloride rich aqueous matrices is presented. A pre-separation system (made of two in line pre-columns, Dionex AG9-HC 4 mm) connected to an analytical column (Dionex AS9-HC 4 mm) by a four way pneumatic valve, allows chloride to be eluted off into the waste and nutrients to be separated and detected by a conductimeter and/or a UV spectrophotometer. Neither chemical pre-treatment nor sample dilution are required; sample matrices presenting a large range of chloride concentrations can be investigated. Moreover by using this technology, automation for routine analysis, low analysis time and low costs can be achieved. LODs of 100, 300, 1000 microg/l for nitrate, nitrite and phosphate, respectively, have been obtained by spiking a synthetic sea water sample containing 20,000 mg/l of chloride and 3000 mg/l of sulphate. Analyte calibration curves of analytes are linear (r>0.99) in the range between the LODs and 60 mg/l. This method was applied to nutrients determination in sea water samples collected near a river outlet. PMID:12899303

  8. Multiple chromatographic fingerprinting and its application to the quality control of herbal medicines

    Energy Technology Data Exchange (ETDEWEB)

    Fan Xiaohui [Pharmaceutical Informatics Institute, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310027 (China); Cheng Yiyu [Pharmaceutical Informatics Institute, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310027 (China)]. E-mail: chengyy@zju.edu.cn; Ye Zhengliang [Pharmaceutical Informatics Institute, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310027 (China); Lin Ruichao [National Institute for the Control of Pharmaceutical and Biological Products, Beijing 100050 (China); Qian Zhongzhi [Committee of Chinese Pharmacopoeia, Beijing 100061 (China)

    2006-01-12

    Recently, chromatographic fingerprinting has become one of the most powerful approaches to quality control of herbal medicines. However, the performance of reported chromatographic fingerprinting constructed by single chromatogram sometimes turns out to be inadequate for complex herbal medicines, such as multi-herb botanical drug products. In this study, multiple chromatographic fingerprinting, which consists of more than one chromatographic fingerprint and represents the whole characteristics of chemical constitutions of the complex medicine, is proposed as a potential strategy in this complicated case. As a typical example, a binary chromatographic fingerprinting of 'Danshen Dropping Pill' (DSDP), the best-sold traditional Chinese medicine in China, was developed. First, two HPLC fingerprints that, respectively, represent chemical characteristics of depsides and saponins of DSDP were developed, which were used to construct binary chromatographic fingerprints of DSDP. Moreover, the authentication and validation of the binary fingerprints were performed. Then, a data-level information fusion method was employed to capture the chemical information encoded in two chromatographic fingerprints. Based on the fusion results, the lot-to-lot consistency and frauds can be determined either using similarity measure or by chemometrics approach. The application of binary chromatographic fingerprinting to consistency assessment and frauds detection of DSDP clearly demonstrated that the proposed method was a powerful approach to quality control of complex herbal medicines.

  9. Multiple chromatographic fingerprinting and its application to the quality control of herbal medicines

    International Nuclear Information System (INIS)

    Recently, chromatographic fingerprinting has become one of the most powerful approaches to quality control of herbal medicines. However, the performance of reported chromatographic fingerprinting constructed by single chromatogram sometimes turns out to be inadequate for complex herbal medicines, such as multi-herb botanical drug products. In this study, multiple chromatographic fingerprinting, which consists of more than one chromatographic fingerprint and represents the whole characteristics of chemical constitutions of the complex medicine, is proposed as a potential strategy in this complicated case. As a typical example, a binary chromatographic fingerprinting of 'Danshen Dropping Pill' (DSDP), the best-sold traditional Chinese medicine in China, was developed. First, two HPLC fingerprints that, respectively, represent chemical characteristics of depsides and saponins of DSDP were developed, which were used to construct binary chromatographic fingerprints of DSDP. Moreover, the authentication and validation of the binary fingerprints were performed. Then, a data-level information fusion method was employed to capture the chemical information encoded in two chromatographic fingerprints. Based on the fusion results, the lot-to-lot consistency and frauds can be determined either using similarity measure or by chemometrics approach. The application of binary chromatographic fingerprinting to consistency assessment and frauds detection of DSDP clearly demonstrated that the proposed method was a powerful approach to quality control of complex herbal medicines

  10. A novel two-dimensional liquid chromatographic system for the online toxicity prediction of pharmaceuticals and related substances

    Energy Technology Data Exchange (ETDEWEB)

    Li, Jian; Xu, Li [Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030 (China); Shi, Zhi-guo, E-mail: shizg@whu.edu.cn [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu, Min [Hubei Instrument for Food and Drug Control, Wuhan (China)

    2015-08-15

    Highlights: • A novel two-dimensional liquid chromatographic system was developed. • The 1st dimension was ODS to separate components in the sample. • The 2nd dimension was biopartitioning micellar chromatography to predict toxicity. • The system was used to screen toxicity of pharmaceuticals and related substances. • It was promising for fast online toxicity screening of complex sample in one step. - Abstract: In this study, a novel two-dimensional liquid chromatographic (2D-LC) system was developed for simultaneous separation and toxicity prediction of pharmaceutical and its related substances. A conventional ODS column was used on the 1st-D to separate the sample; while, bio-partitioning micellar chromatography served as the 2nd-D to predict toxicity of the components. The established system was tested for the toxicity of ibuprofen and its impurities with known toxicity. With only one injection, ibuprofen and its impurities were separated on the 1st-D; and LC50 values of individual impurity were obtained based on the quantitative retention–activity relationships, which agreed well with the reported data. Furthermore, LC50 values of photolysis transformation products (TPs) of carprofen, ketoprofen and diclofenac acid (as unknown compounds) were screened in this 2D-LC system, which could be an indicator of the toxicity of these TPs and was meaningful for the environmental monitoring and drinking water treatment. The established 2D-LC system was cost-effective, time-saving and reliable, and was promising for fast online screening of toxicity of known and unknown analytes in the complex sample in a single step. It may find applications in environment, pharmaceutical and food, etc.

  11. A novel two-dimensional liquid chromatographic system for the online toxicity prediction of pharmaceuticals and related substances

    International Nuclear Information System (INIS)

    Highlights: • A novel two-dimensional liquid chromatographic system was developed. • The 1st dimension was ODS to separate components in the sample. • The 2nd dimension was biopartitioning micellar chromatography to predict toxicity. • The system was used to screen toxicity of pharmaceuticals and related substances. • It was promising for fast online toxicity screening of complex sample in one step. - Abstract: In this study, a novel two-dimensional liquid chromatographic (2D-LC) system was developed for simultaneous separation and toxicity prediction of pharmaceutical and its related substances. A conventional ODS column was used on the 1st-D to separate the sample; while, bio-partitioning micellar chromatography served as the 2nd-D to predict toxicity of the components. The established system was tested for the toxicity of ibuprofen and its impurities with known toxicity. With only one injection, ibuprofen and its impurities were separated on the 1st-D; and LC50 values of individual impurity were obtained based on the quantitative retention–activity relationships, which agreed well with the reported data. Furthermore, LC50 values of photolysis transformation products (TPs) of carprofen, ketoprofen and diclofenac acid (as unknown compounds) were screened in this 2D-LC system, which could be an indicator of the toxicity of these TPs and was meaningful for the environmental monitoring and drinking water treatment. The established 2D-LC system was cost-effective, time-saving and reliable, and was promising for fast online screening of toxicity of known and unknown analytes in the complex sample in a single step. It may find applications in environment, pharmaceutical and food, etc

  12. Chromatographic separation of radioactive noble gases from xenon

    CERN Document Server

    Akerib, D S; Bai, X; Bailey, A J; Balajthy, J; Beltrame, P; Bernard, E P; Bernstein, A; Biesiadzinski, T P; Boulton, E M; Bramante, R; Cahn, S B; Carmona-Benitez, M C; Chan, C; Chiller, A A; Chiller, C; Coffey, T; Currie, A; Cutter, J E; Davison, T J R; Dobi, A; Dobson, J E Y; Druszkiewicz, E; Edwards, B N; Faham, C H; Fiorucci, S; Gaitskell, R J; Gehman, V M; Ghag, C; Gibson, K R; Gilchriese, M G D; Hall, C R; Hanhardt, M; Haselschwardt, S J; Hertel, S A; Hogan, D P; Horn, M; Huang, D Q; Ignarra, C M; Ihm, M; Jacobsen, R G; Ji, W; Kamdin, K; Kazkaz, K; Khaitan, D; Knoche, R; Larsen, N A; Lee, C; Lenardo, B G; Lesko, K T; Lindote, A; Lopes, M I; Manalaysay, A; Mannino, R L; Marzioni, M F; McKinsey, D N; Mei, D -M; Mock, J; Moongweluwan, M; Morad, J A; Murphy, A St J; Nehrkorn, C; Nelson, H N; Neves, F; O'Sullivan, K; Oliver-Mallory, K C; Palladino, K J; Pease, E K; Pech, K; Phelps, P; Reichhart, L; Rhyne, C; Shaw, S; Shutt, T A; Silva, C; Solovov, V N; Sorensen, P; Stephenson, S; Sumner, T J; Szydagis, M; Taylor, D J; Taylor, W; Tennyson, B P; Terman, P A; Tiedt, D R; To, W H; Tripathi, M; Tvrznikova, L; Uvarov, S; Verbus, J R; Webb, R C; White, J T; Whitis, T J; Witherell, M S; Wolfs, F L H; Yazdani, K; Young, S K; Zhang, C

    2016-01-01

    The Large Underground Xenon (LUX) experiment operates at the Sanford Underground Research Facility to detect nuclear recoils from the hypothetical Weakly Interacting Massive Particles (WIMPs) on a liquid xenon target. Liquid xenon typically contains trace amounts of the noble radioactive isotopes $^{85}$Kr and $^{39}$Ar that are not removed by the {\\em in situ} gas purification system. The decays of these isotopes at concentrations typical of research-grade xenon would be a dominant background for a WIMP search exmperiment. To remove these impurities from the liquid xenon, a chromatographic separation system based on adsorption on activated charcoal was built. 400\\,kg of xenon was processed, reducing the average concentration of krypton from 130\\,ppb to 3.5\\,ppt as measured by a cold-trap assisted mass spectroscopy system. A 50 kg batch spiked to 0.001 g/g of krypton was processed twice and reduced to an upper limit of 0.2 ppt.

  13. Gradient ion-pair chromatographic method for the determination of iron N,N'-ethylenediamine-di-(2-hydroxy-5-sulfophenylacetate) by high performance liquid chromatography-atmospheric pressure ionization electrospray mass spectrometry.

    Science.gov (United States)

    García-Marco, Sonia; Cremonini, Mauro A; Esteban, Pedro; Yunta, Felipe; Hernández-Apaolaza, Lourdes; Placucci, Giuseppe; Lucena, Juan J

    2005-01-28

    The most effective remedy for iron deficiency is the use of synthetic iron chelates, specifically chelates derived from polyaminecarboxylic acids as EDDHSA (N,N'-ethylenediamine-di-(2-hidroxy-5-sulfophenylacetic) acid). A gradient ion-pair chromatographic method was developed to quantify the total amount of chelated iron in EDDHSA/Fe3+ fertilizers. Two mobile phases were used containing, respectively, 35 and 75% acetonitrile in a 0.005 M tetrabutylammonium hydroxide aqueous solution at pH 6.0. The stationary phase was a reverse phase C-18 column (150mm x 3.9mm i.d., dp = 5 microm). Two chromatographic peaks appeared and were identified by Electrospray Mass Spectrometry. The first peak corresponds to the monomer of EDDHSA/Fe3+ and the second peak has been assigned to condensation molecules. Quality parameters indicate that the method is suitable for the quantification of iron chelate by EDDHSA fertilizers. PMID:15729821

  14. Determination of Imidacloprid and metabolites by liquid chromatography with an electrochemical detector and post column photochemical reactor

    International Nuclear Information System (INIS)

    A procedure for the determination of Imidacloprid and its main metabolites was set up by means of liquid chromatography with an electrochemical detector and post-column photochemical reactor (LC-hν-ED). Sample clean-up was developed for bees, filter paper and maize leaves. Chromatographic conditions were based on a reversed-phase C-18 column operated by phosphate buffer 50 mM/CH3CN (80/20, v/v) at pH 2.9. Detection of Imidacloprid and its metabolites was performed at a potential of 800 mV after photoactivation at 254 nm. Compared to conventional techniques such as gas chromatography/mass spectrometry (GC/MS) or LC coupled to other detectors, the present method allows simultaneous trace-level determination of both Imidacloprid (0.6 ng ml-1) and its main metabolites (2.4 ng ml-1)

  15. Microwaves Scattering by Underdense Inhomogeneous Plasma Column

    Science.gov (United States)

    Zhang, Lin; Ouyang, Jiting

    2016-03-01

    The scattering characteristics of microwaves (MWs) by an underdense inhomogeneous plasma column have been investigated. The plasma column is generated by hollow cathode discharge (HCD) in a glass tube filled with low pressure argon. The plasma density in the column can be varied by adjusting the discharge current. The scattering power of X-band MWs by the column is measured at different discharge currents and receiving angles. The results show that the column can affect the properties of scattering wave significantly regardless of its plasma frequency much lower than the incident wave frequency. The power peak of the scattering wave shifts away from 0° to about ±15° direction. The finite-different time-domain (FDTD) method is employed to analyze the wave scattering by plasma column with different electron density distributions. The reflected MW power from a metal plate located behind the column is also measured to investigate the scattering effect on reducing MW reflectivity of a metal target. This study is expected to deepen the understanding of plasma-electromagnetic wave interaction and expand the applications concerning plasma antenna and plasma stealth.

  16. Redesigned Air-Column Resonance Apparatus

    Science.gov (United States)

    Singh, Gurbax; Graf, Erlend H.

    2003-02-01

    This paper describes a redesigned air-column resonance apparatus that offers several advantages over the traditional one.2 It does away with water or the long rod to vary the length of the air column. Instead a specially designed piston is moved inside a plastic or glass tube by external magnets to vary the length of the air column. Plastic tubes of various sizes are commercially available,3 but we salvaged one from an old commercial resonance apparatus. The tube has 2.85-cm inner and 3.15-cm outer diameter, respectively. The redesigned resonance apparatus can be operated in either the horizontal or the vertical position.

  17. COLUMN-ORIENTED DATABASE MANAGEMENT SYSTEMS

    OpenAIRE

    Shevchenko, l.O.; National Aviation University, Kyiv

    2012-01-01

    In the following thesis I will present column-oriented database. Among other things, I will answer on a question why there is a need for a column-oriented database. In recent years there have been a lot of attention regarding a column-oriented database, even if the existence of a columnar database management systems dates back in the early seventies of the last century. I will compare both systems for a database management – a colum-oriented database system and a row-oriented database system ...

  18. Dynamic effects of diabatization in distillation columns

    DEFF Research Database (Denmark)

    Bisgaard, Thomas; Huusom, Jakob Kjøbsted; Abildskov, Jens

    2013-01-01

    The dynamic effects of diabatization in distillation columns are investigated in simulation emphasizing the heat-integrated distillation column (HIDiC). A generic, dynamic, first-principle model has been formulated, which is flexible enough to describe various diabatic distillation configurations....... Dynamic Relative Gain Array and Singular Value Analysis have been applied in a comparative study of a conventional distillation column and a HIDiC. The study showed increased input-output coupling due to diabatization. Feasible SISO control structures for the HIDiC were also found and control...

  19. Buckling driven debonding in sandwich columns

    DEFF Research Database (Denmark)

    Østergaard, Rasmus Christian

    2008-01-01

    A compression loaded sandwich column that contains a debond is analyzed using a geometrically non-linear finite element model. The model includes a cohesive zone along one face sheet/core interface whereby the debond can extend by interface crack growth. Two geometrical imperfections are introduced......; a global imperfection of the sandwich column axis and a local imperfection of the debonded face sheet axis. The model predicts the sandwich column to be very sensitive to the initial debond length and the local face sheet imperfection. The study shows that the sensitivity to the face sheet...

  20. Dynamic Effects of Diabatization in Distillation Columns

    DEFF Research Database (Denmark)

    Bisgaard, Thomas; Huusom, Jakob Kjøbsted; Abildskov, Jens

    2012-01-01

    The dynamic eects of diabatization in distillation columns are investigated in simulation with primary focus on the heat-integrated distillation column (HIDiC). A generic, dynamic, rst-principle model has been formulated, which is exible to describe various diabatic distillation congurations....... Dynamic Relative Gain Array and Singular Value Analysis have been applied in a comparative study of a conventional distillation column and a HIDiC. The study showed increased input-output coupling due to diabatization. Feasible SISO control structures for the HIDiC were also found. Control...

  1. Characterization of oil in the water column on the surface after chemical dispersion

    International Nuclear Information System (INIS)

    Changes in oil composition during chemical dispersion were analysed. A gas chromatographic method was used to study the oil in a water column and also on the surface. The objective of the study was to determine dispersant effectiveness and behavior, and in particular to understand why the effectiveness of surfactants decrease as the oil weathers. It was found that in dispersed oil higher alkanes are present in lower concentration than in starting oil. The higher alkanes are concentrated in the surface oil and are less dispersible. Molecular weight and n-alkane fraction were found to be directly related. It was concluded that the main reason for dispersant effectiveness decrease with weathering is the loss of the highly dispersible small aliphatics which are lost through evaporation. 5 refs., 6 tabs., 3 figs

  2. Determination of Five Organic Acids in Radix Isatidis by Column Partition Chromatography and Capillary Zone Electrophoresis

    Institute of Scientific and Technical Information of China (English)

    CHAIYi-fen; JISong-gang; ZHANGGuo-qing; LIUChang-hai

    2003-01-01

    Aim To determine five organic acids in Radix lsatidis. Method The extraction method and the column partition chromatographic conditiom were studied. Then a capillary zone dectrophorefic method was set up for the determina-tion. Results The linear ranges of quinazolinone acid, n-anthranilic acid, benzoic acid, salicylic acid, and syringic acid were 5.52 - 92.0μg·mL-1 , 5.12 - 102μg·mL-1 , 2.28 - 84.4μg·mL-1, 4.78 - 159 μg·mL-1, and 1.74- 87.0μg·mL-1 respectively. Conclusion The established method is accurate and simple.

  3. 29 CFR 1926.756 - Beams and columns.

    Science.gov (United States)

    2010-07-01

    ... (.46 m) from the extreme outer face of the column in each direction at the top of the column shaft. (e) Perimeter columns. Perimeter columns shall not be erected unless: (1) The perimeter columns extend a minimum of 48 inches (1.2 m) above the finished floor to permit installation of perimeter safety cables...

  4. Gas chromatographic measurement of the radiolytic products of irradiated pork

    International Nuclear Information System (INIS)

    The radiolytic products of irradiated pork were isolated, analyzed and identified by the techniques of vacuum distillation, GC-MS. The higher boiling point compounds in fat were collected by cold-finger and its lower boiling point compounds were recovered on a short precolumn packed with alumina, and the volatiles of lean pork were collected on a short column packed with TCEP/Chromosovb. Some experimental conditions were studied. 49 compounds were identified. These compounds include hydrocarbons and sulphides etc. (author)

  5. Liquid chromatographic enantioseparation of the brominated flame retardant 2,3-dibromopropyl-2,4,6-tribromophenyl ether (DPTE) and enantiomer fractions in seal blubber.

    Science.gov (United States)

    Vetter, Walter; Recke, Roland von der; Ostrowicz, Patrizia; Rosenfelder, Natalie

    2010-01-01

    Enantioselective analyses of the chiral brominated flame retardant 2,3-dibromopropyl-2,4,6-tribromophenyl ether (DPTE) are the focus of this work. High performance liquid chromatography (HPLC) equipped with a column that had a chiral stationary phase consisting of a modified cellulose derivative allowed for the fractionation of the enantiomers of DPTE. The enantiomeric excess was 98.2% for enantiomer 1 and 99% for enantiomer 2. Polarimetric measurements verified that the first eluting enantiomer originated from (-)-DPTE and the second peak originated from (+)-DPTE. Two gas chromatographic columns allowed for the direct enantioresolution of DPTE. The elution order of DPTE enantiomers was the same as observed in the chiral HPLC system ((-)-DPTE before (+)-DPTE). The best enantioseparation was achieved on a Chirasil-DEX CB column, which was used to analyze the enantiomer fractions of DPTE in blubber and brain samples of hooded seals (Cystophora cristata) and harp seals (Phoca groenlandica) from the Barents and Greenland Seas. Analyses were carried out by means of gas chromatography/electron capture negative ion mass spectrometry operated in the selected ion monitoring (GC/ECNI-MS-SIM) mode. In both matrices, only minute deviations from the racemate were observed (maximum +/-3% excess of (-)-DPTE). However, the samples from the Barents Sea were either racemic or showed a slight excess of (+)-DPTE (up to 2.5%), whereas all samples from the Greenland Sea contained a slight excess (up to 4%) of (-)-DPTE. PMID:19863996

  6. Noise analysis and column FPN suppression technology

    Directory of Open Access Journals (Sweden)

    Xiao-Fen Jia

    2013-01-01

    Full Text Available Noise is an important indicator that affects the image quality. Among the different processing strategies implemented in image sensors, the effect on the noise is complicated. The two types of noise that influences the imaging quality of the digital camera are analyzed firstly. The optical signal and reset signal of the typical correlated double sampling (CDS are read out through two column amplifiers (CA, respectively. The performance of the two column amplifiers are not exactly the same, resulting in itself will bring the column FPN. To suppress the column FPN effectively, a single amplifier CDS scheme is proposed, which have only one CA, the power consumption and area of the proposed CDS circuit is reduced by half.

  7. PRTR ion exchange vault column sampling

    International Nuclear Information System (INIS)

    This report documents ion exchange column sampling and Non Destructive Assay (NDA) results from activities in 1994, for the Plutonium Recycle Test Reactor (PRTR) ion exchange vault. The objective was to obtain sufficient information to prepare disposal documentation for the ion exchange columns found in the PRTR Ion exchange vault. This activity also allowed for the monitoring of the liquid level in the lower vault. The sampling activity contained five separate activities: (1) Sampling an ion exchange column and analyzing the ion exchange media for purpose of waste disposal; (2) Gamma and neutron NDA testing on ion exchange columns located in the upper vault; (3) Lower vault liquid level measurement; (4) Radiological survey of the upper vault; and (5) Secure the vault pending waste disposal

  8. Whose Cortical Column Would that Be?

    OpenAIRE

    Nuno Miguel M Amorim Da Costa

    2010-01-01

    The cortical column has been an invaluable concept to explain the functional organization of the neocortex. While this idea was born out of experiments that cleverly combined electrophysiological recordings with anatomy, no one has ‘seen’ the anatomy of a column. All we know is that when we record through the cortex of primates, ungulates, and carnivores in a trajectory perpendicular to its surface there is a remarkable constancy in the receptive field properties of the neurons re...

  9. Simplified design method for slender hybrid columns

    OpenAIRE

    pisey, keo; Somja, Hugues; Nguyen, Quang-Huy; Hjiaj, Mohammed

    2015-01-01

    International audience This paper deals with numerical investigations on second-order effects in slender RC columns reinforced by several steel sections, namely hybrid columns, subjected to combined axial load and uniaxial bending moment. A FE model is developed in which geometrical and material nonlinearities as well as the partial interaction effect between the steel profiles and the surrounding concrete are taken into account. This model is then used to perform an extensive numerical pa...

  10. Magnetic Shaping of Molten Metal Columns

    Science.gov (United States)

    Shercliff, J. A.

    1981-04-01

    In continuous casting the vertically falling liquid column may be shaped by externally applied, horizontal, high-frequency magnetic fields. The free-boundary problem with allowance for surface tension is solved in a two-dimensional approximation by combined complex-variable and numerical methods in the cases where the far field is either uniform or of quadrupole form, or where the field is produced by four vertical conductors centred on the column. Stirring of the fluid is ignored.

  11. Gas separation by a continuous membrane column

    International Nuclear Information System (INIS)

    The continuous membrane column provides a revolutionary new separation technique. In gaseous diffusion the continuous membrane column is used to separate as highly concentrated products both the most permeable and least permeable gases from a feed mixture of any composition. The main features of the column are countercurrent enrichment, high reflux and minimal backmixing. The new method eliminates the need for numerous interstage compressors and extensive product stream recycling found in conventional gaseous diffusion cascades. Experiments are carried out for systems of CO2-O2,O2-N2 (air), and CO2-N2 mixtures using continuous membrane columns made out of silicone rubber membrane. Also, a theoretical model is developed to interpret the experimental data. The agreement between theory and experiment is excellent. The maximum degree of separation can be achieved at total reflux. It is experimentally verified that the maximum degree of enrichment attainable by a conventional method can easily be exceeded without limit when a continuous membrane column is employed. Finally, a comparative study has been conducted for a conventional gas permeator and a continuous membrane column

  12. Strength of Concrete Filled Steel Tubular Columns

    Institute of Scientific and Technical Information of China (English)

    Muhammad Naseem Baig; FAN Jiansheng; NIE Jianguo

    2006-01-01

    Composite columns of steel and concrete have been used and studied world wide, but filled tubular columns need more attention. This paper presents an experimental study on the behavior of short concrete filled steel tubular columns (CFT) axially loaded in compression to failure. A total of 28 specimens (16 were filled with concrete and 12 were kept hollow) with different cross-sections were tested to investigate the load capacity. The length-to-diameter ratios of these columns were between 4 and 9. Parameters for the tests were tube shape and diameter-to-thickness ratio. Some of the concrete filled columns had internal bracing of #3 deformed bars. The test results are compared with the theoretical results and previous studies. The results show that the confinement effect on concrete does play a role in increasing the compressive strengths to almost 60% in some cases. Based on the test results, an equation to estimate the ultimate axial compressive loading capacities is also proposed for square CFT columns.

  13. Use of coextraction and suppression of extraction in extraction-chromatographic separation of elements

    International Nuclear Information System (INIS)

    TBP, solutions of hydrobromic acid, indium and polytetrafluoroethylene powder, carrier for TBP, were used to study the effects of coextraction and extraction suppression on extraction-chromatographic behaviour of microamounts of elements in the presence of macroamounts of other elements. Possibility of using these effects under extraction-chromatographic element separation were considered. A new method for extraction-chromatographic separation of scandium microamounts from the mixture of large amount of elements (Y, Cd, Ce, Eu, Lu, Hf, Ta, W, Np and other) was suggested. 15 refs.; 3 figs

  14. Identification of humic-like substances (HULIS) in oxygenated organic aerosols using NMR and AMS factor analyses and liquid chromatographic techniques

    Science.gov (United States)

    Paglione, M.; Kiendler-Scharr, A.; Mensah, A. A.; Finessi, E.; Giulianelli, L.; Sandrini, S.; Facchini, M. C.; Fuzzi, S.; Schlag, P.; Piazzalunga, A.; Tagliavini, E.; Henzing, J. S.; Decesari, S.

    2014-01-01

    The atmospheric organic aerosol composition is characterized by a great diversity of functional groups and chemical species, challenging simple classification schemes. Traditional offline chemical methods identify chemical classes based on the retention behaviour on chromatographic columns and absorbing beds. Such an approach led to the isolation of complex mixtures of compounds such as the humic-like substances (HULIS). More recently, online aerosol mass spectrometry (AMS) was employed to identify chemical classes by extracting fragmentation patterns from experimental data series using statistical methods (factor analysis), providing simplified schemes for the classification of oxygenated organic aerosols (OOAs) on the basis of the distribution of oxygen-containing functionalities. The analysis of numerous AMS data sets suggested the occurrence of very oxidized OOAs which were postulated to correspond to HULIS. However, only a few efforts were made to test the correspondence of the AMS classes of OOAs with the traditional classifications from the offline methods. In this paper, we consider a case study representative of polluted continental regional background environments. We examine the AMS factors for OOAs identified by positive matrix factorization (PMF) and compare them to chemical classes of water-soluble organic carbon (WSOC) analysed offline on a set of filters collected in parallel. WSOC fractionation was performed by means of factor analysis applied to proton nuclear magnetic resonance (NMR) spectroscopic data, and by applying an ion-exchange chromatographic method for direct quantification of HULIS. Results show that the very oxidized low-volatility OOAs from AMS correlate with the NMR factor showing HULIS features and also with true "chromatographic" HULIS. On the other hand, UV/VIS-absorbing polyacids (or HULIS {sensu stricto}) isolated on ion-exchange beds were only a fraction of the AMS and NMR organic carbon fractions showing functional groups

  15. Measurements of organic molecular markers in California using comprehensive 2-Dimensional Gas Chromatograph High-Resolution Time-of-Flight Mass Spectrometry (GCxGC-HRTOF-MS)

    Science.gov (United States)

    Chan, A. W.; Isaacman, G. A.; Worton, D. R.; Kreisberg, N. M.; Schilling, K. A.; Craven, J. S.; Metcalf, A. R.; Hersey, S. P.; Rubitschun, C. L.; Lin, Y. H.; Offenberg, J. H.; Surratt, J. D.; Seinfeld, J.; Hering, S. V.; Goldstein, A. H.

    2011-12-01

    Understanding the sources and transformation processes of organic aerosol requires detailed speciation of organic compounds. Molecular markers specific to individual sources help determine the contribution of each source to organic aerosol emissions. In previous work using one-dimensional gas-chromatograph mass spectrometry (GC/MS), less than 10-20% of the organic fraction has been identified, with a large contribution of unresolved complex mixture (UCM). Two-dimensional gas-chromatograph is a novel technique which provides excellent resolution to separate compounds buried in this complex mixture. In addition to a volatility-based chromatographic separation, compounds are further separated on a second column based on their polarities. Here we report measurements of more than 200 resolved compounds observed on filters collected during CalNex 2010 in Bakersfield and Pasadena, and during a large biomass burning event in the Los Angeles area (Station Fire). High volume filter samples are thermally desorbed in a Gerstel Thermal Desorption System (TDS2) and preconcentrated on a cooled inlet (CIS). The compounds are then analyzed by comprehensive 2-dimensional GC using a Zoex modulator, followed by high-resolution mass spectrometry (Tofwerks). Compound identification is carried out by comparison of retention times with known standards, mass spectral library match, and identification of molecular fragments by exact mass. A wide range of compounds are observed: n-alkanes, polyaromatic hydrocarbons, and oxygenated compounds such as acids, esters and ketones. While levoglucosan was observed in organic aerosol produced during the Station Fire, many other compounds revealed by two-dimensional GC (such as resin acids, lignin pyrolysis products) show elevated signals, suggesting that other molecular markers can provide additional information about aerosol formation processes during biomass burning events.

  16. Load introduction into concrete-filled steel tubular columns

    OpenAIRE

    Mollazadeh, Mohammad Hassan

    2015-01-01

    Concrete-Filled Steel Tubular (CFST) columns are increasingly being used because of their many advantages, including high strength, high ductility, and higher fire resistance than conventional steel or concrete columns of the same size. In order to maximise the advantages of CFST column, composite action of the column should be ensured. In realistic structures, the load is not directly applied to the entire CFST column section and is introduced from the beam-column connection. Simple shear c...

  17. Duplex stainless steel columns and beam-columns in case of fire

    OpenAIRE

    Lopes, N.; Vila Real, P. M. M.; Simoes da Silva, L.; Franssen, Jean-Marc

    2008-01-01

    It is the purpose of this paper to evaluate the accuracy and safety of the currently prescribed design rules in Eurocode 3: Part 1.2 for the evaluation of the resistance of duplex stainless steel columns and beam-columns. This evaluation is carried out by performing numerical simulations on Class1 and Class 2 stainless steel H-columns. These numerical simulations are performed using the program SAFIR. Eurocode 3 states that stainless steel structural members, subjected to high ...

  18. Column Strengthening with TRC: Influences of the Column Geometry onto the Confinement Effect

    OpenAIRE

    Regine Ortlepp; Andy Lorenz; Manfred Curbach

    2009-01-01

    The increase of the load-carrying capacity of columns being reinforced with Textile Reinforced Concrete (TRC) is partly achieved by the additional concrete cover. But then it is also decisively caused by the confinement effect of the textile reinforcement. The confinement is thereby producing a three-axial state of stress within the concrete core of the column. The effectiveness of such a confinement is especially dependent on the geometry of the concrete column to be strengthened. At rectang...

  19. Simultaneous determination of ten anticoagulant rodenticides in tissues by column-switching UHPLC-ESI-MS/MS.

    Science.gov (United States)

    Maršálek, Petr; Modrá, Helena; Doubková, Veronika; Večerek, Vladimír

    2015-10-01

    This paper describes the development of a method for the simultaneous determination of ten anticoagulant rodenticides (coumafuryl, warfarin, pindone, coumatetralyl, coumachlor, difenacoum, bromadiolone, brodifacoum, chlorophacinone and flocoumafen) in the liver and kidney based on column-switching liquid chromatography coupled with heated electrospray ionization tandem mass spectrometry. The simple sample preparation includes extraction with methanol. A C18 trapping column was used for online solid-phase extraction before analytical separation with the mobile phase comprising a mixture of 0.1% formic acid in water, methanol and acetonitrile. Chromatographic separation was achieved using a Thermo Hypersil ultra high-performance liquid chromatography (UHPLC) C18 column with the mobile phase consisting of 5 mM ammonium formate buffer (pH = 9) and methanol. The column-switching procedure ensured no matrix effects during electrospray ionization (ESI). Extraction recoveries ranged between 91 and 100% for liver and between 89 and 97% for kidney. The method showed good linearity up to 750 ng g(-1). The limit of detection ranged between 0.001 and 0.022 ng g(-1) for liver and between 0.001 and 0.028 ng g(-1) for kidney. The developed method was successfully used in several animal poisoning cases. PMID:26280206

  20. Preconcentration procedures for phthalate esters combined with chromatographic analysis.

    Science.gov (United States)

    Lv, Xueju; Hao, Yi; Jia, Qiong

    2013-08-01

    Phthalate esters are endocrine disrupters or mutagens. They are widely used as plasticizers and can be usually found in environmental samples, such as food, soil and polluted air. However, it is difficult to directly determine phthalate esters owing to their relatively low concentration and complex matrices. Therefore, preconcentration and separation have become increasingly important. In recent years, many preconcentration methods have been successfully developed and widely used, such as liquid-liquid extraction, dispersive liquid-liquid microextraction and solid-phase extraction. These preconcentration methods for phthalate esters can be applied to various real samples, water, soil, air, food and cosmetics. The aim of this paper is to review recent literature studies (primarily from the last five years) about preconcentration techniques for phthalate esters coupled with chromatographic analysis. The following text describes several preconcentration approaches, including liquid-liquid extraction, dispersive liquid-liquid microextraction, cloud point extraction, solid-phase extraction, solid-phase microextraction and stir bar sorptive extraction. Their advantages and disadvantages are also summarized. PMID:23696389

  1. Chemical Compositions, Chromatographic Fingerprints and Antioxidant Activities of Andrographis Herba

    Directory of Open Access Journals (Sweden)

    Yang Zhao

    2014-11-01

    Full Text Available This paper describes the development of an HPLC-UV-MS method for quantitative determination of andrographolide and dehydroandrographolide in Andrographis Herba and establishment of its chromatographic fingerprint. The method was validated for linearity, limit of detection and quantification, inter- and intra-day precisions, repeatability, stability and recovery. All the validation results of quantitative determination and fingerprinting methods were satisfactory. The developed method was then applied to assay the contents of andrographolide and dehydroandrographolide and to acquire the fingerprints of all the collected Andrographis Herba samples. Furthermore, similarity analysis and principal component analysis were used to reveal the similarities and differences between the samples on the basis of the characteristic peaks. More importantly, the DPPH free radical-scavenging and ferric reducing capacities of the Andrographis Herba samples were assayed. By bivariate correlation analysis, we found that six compounds are positively correlated to DPPH free radical scavenging and ferric reducing capacities, and four compounds are negatively correlated to DPPH free radical scavenging and ferric reducing capacities.

  2. Authenticity analysis of pear juice employing chromatographic fingerprinting.

    Science.gov (United States)

    Willems, Jamie L; Low, Nicholas H

    2014-12-01

    Pear juice is predominately composed of carbohydrates/polyols (>95% of the total soluble solids), making it susceptible to adulteration by the addition of less expensive commercial sweeteners. In this research, the major carbohydrate and polyol (fructose, glucose, sucrose, and sorbitol) content of 32 pure pear juices representing five world producing regions and three years of production was determined. Additionally, methods employing oligosaccharide profiling to detect the debasing of these samples with four commercial sweeteners (HFCS 55 and 90, TIS, and HIS) were developed using capillary gas chromatography with flame ionization detection (CGC-FID) and high-performance liquid chromatography with pulsed amperometric detection (HPAE-PAD). Detection limits for the four commercial sweeteners ranged from 0.5 to 5.0% (v/v). In addition, the developed CGC-FID method could be used to (a) detect the addition of pear to apple juice via arbutin detection and (b) determine if a pear juice was produced using enzymatic liquefaction via the presence of O-β-d-glucopyranosyl-(1→4)-d-glucopyranose (cellobiose), all within a single chromatographic analysis. PMID:25384245

  3. Detection of geosmin and 2-methylisoborneol by liquid-liquid extraction-gas chromatograph mass spectrum (LLE-GCMS)and solid phase extraction-gas chromatograph mass spectrum (SPE-GCMS)

    Institute of Scientific and Technical Information of China (English)

    MA Xiaoyan; GAO Naiyun; CHEN Beibei; LI Qingsong; ZHANG Qiaoli; GU Guofen

    2007-01-01

    Two sample preparation methods were introduced and compared in this paper to establish a simple,quick and exact analysis of geosmin and 2-methylisoborneol.LC-18 column was employed in solid phase extraction (SPE),1.0 mL of hexane was adopted in liquid-liquid extraction(LLE),and the extracts were analyzed by gas chromatograph mass spectrum (GCMS) in selected ion mode.Mean recoveries of SPE were low for 2-methylisoborneol (2-MIB)and geosmin (GSM) with values below 50%.For LLE,the recoveries were satisfyingly above 50% for 2-MIB and 80% for GSM.Detection limits of the LLE method were as low as 1.0 ng/L for GSM and 5.0 ng/L for 2-MIB.A year-long investigation on odor chemicals of drinking water in Shanghai demonstrated that in the summer,there was a serious odor problem induced by a high concentration of 2-MIB.The highest concentration of 152.82 ng/L appeared in July in raw water,while GSM flocculation was minimal with concentrations below odor threshold.

  4. Structural Decoupling and Disturbance Rejection in a Distillation Column

    DEFF Research Database (Denmark)

    Bahar, Mehrdad; Jantzen, Jan; Commault, C.;

    1996-01-01

    Introduction, distillation column model, input-output decoupling, disturbance rejection, concluding remarks, references.......Introduction, distillation column model, input-output decoupling, disturbance rejection, concluding remarks, references....

  5. Adamantyl-group containing mixed-mode acrylamide-based continuous beds for capillary electrochromatography. Part III. Optimization of the chromatographic efficiency.

    Science.gov (United States)

    Al-Massaedh, Ayat Allah; Pyell, Ute

    2014-01-17

    In a previous article we described the synthesis of amphiphilic monolithic stationary phases by in situ free radical copolymerization of cyclodextrin-solubilized N-adamantyl acrylamide, piperazinediacrylamide, methacrylamide and vinylsulfonic acid in aqueous medium in pre-treated fused silica capillaries of 100μ.m I.D. In this work, a series of N-adamantyl-group containing acrylamide-based continuous beds is synthesized under variation of different synthesis parameters. The studied synthesis parameters are (i) concentration of the lyotropic salt ammonium sulfate, (ii) concentration of the initiator ammonium persulfate, and (iii) concentration of the negatively charged monomer vinylsulfonic acid in the polymerization mixture. The influence of the synthesis parameters on the chromatographic efficiency is studied under isocratic conditions for a homologues series of alkylphenones in the reversed-phase mode at constant composition of the mobile phase via capillary electrochromatography with varied electric field strength. With varied concentration of the lyotropic salt ammonium sulfate or varied concentration of the initiator ammonium persulfate in the polymerization mixture, a strong impact on the chromatographic efficiency is observed, while there is only a minor influence when varying the molar fraction of the charged monomer VSA. The absence of a significant influence of extra-column band broadening effects on the determined efficiency is confirmed. There is a good repeatability (with respect to capillary-to-capillary variation and run-to-run variation) reached for the theoretical plate heights obtained for DMF and selected alkylphenones in the reversed-phase mode. PMID:24296296

  6. Preparation and characterization of cerium(IV) tellurium molybdate gel and its application as a bed for chromatographic 99Mo/99mTc generator

    International Nuclear Information System (INIS)

    Cerium(IV) tellurium molybdate was prepared as a new gel bed for chromatographic 99Mo/99mTc generator. The gel material prepared with the optimum conditions was characterized with IR spectroscopy, thermal analysis, XRD, EDX and FESEM. The highest precipitation yield of 99Mo within the formed gel was found to be 97.6% at a Ce:Te:Mo molar ratio of 1:0.2:1. The prepared 99Mo/99mTc chromatographic column based on Ce(IV) tellurium molybdate gel bed showed a good performance. The 99mTc elution yield was 77.8±3.0% with a radionuclidic purity of ≥ 99.99%, radiochemical purity of 96.5±1.3% (as 99mTcO4-) and pH-value in the range of 5-7. Molybdenum and cerium levels in 99mTc eluates did not exceed 1 and 0.3 ppm, respectively, while no tellurium was detected. (author)

  7. Chromatographic methods enabling the characterization of stationary phases and retention prediction in high-performance liquid chromatography and supercritical fluid chromatography.

    Science.gov (United States)

    Sykora, David; Vozka, Jiri; Tesarova, Eva

    2016-01-01

    In the scope of the present review, the current status of high-performance liquid chromatography/ultra-high performance liquid chromatography and supercritical fluid chromatography is briefly provided. These techniques and their retention mechanisms are compared. Various alternative approaches utilized for the determination and description of the retention processes in these two systems are mapped. Two frequently used concepts, linear-free energy relationships, and hydrophobic subtraction models, used for the characterization of the retention interactions, are discussed. Principles and selected applications of the both methods are also covered. Then the models applied for the prediction of retention behavior of solutes on stationary phases are outlined. The procedures utilized for the sorbent/column classification are also covered. Simple chromatographic tests frequently used for the basic characterization and mutual comparison of stationary phases are summarized and briefly commented on. The importance of a statistical evaluation of complex retention data obtained from the chromatographic measurements is outlined. Finally, computer simulations aiming at the facilitation of the quest to optimize separation conditions for a given mixture of analytes are touched upon. PMID:26497150

  8. Development and Validation of A Stability-Indicating Liquid Chromatographic Method for Determination of Valsartan and Hydrochlorthiazide Using Quality by Design

    Directory of Open Access Journals (Sweden)

    Ashok K. Shakya

    2016-05-01

    Full Text Available The present paper involves the analytical quality by design (AQbD-based development of a simple, rapid, accurate and precise stability-indicating method for the estimation of valsartan and hydrochlorothiazide. Optimized mobile phase (v/v/v was water (containing 0.25 ml/L triethylamine, methanol and acetonitrile (50:38:37, pH adjusted to 3.0±0.1. Chromatographic separation was achieved on Hypersil®-Gold C18 (150 x 4.6 mm, 5 µm, Thermo Fisher Scientific, USA, column at 25 ± 2 °C. The method was validated as per the “International Conference on Harmonisation” (ICH guidelines. Chromatographic run time was 10.0 minutes. The linearity range for valsartan and hydrochlorothiazide were 1.25-64.00 µg/ml and 0.195-10.00 µg/ml respectively. The limits of detection (LOD for valsartan and hydrochlorothiazide were 0.253 and 0.0226 μg/ml while the limits of quantitations (LOQ were 0.767 and 0.068 μg/ml respectively, using 10µl sample. Stability studies indicate that the degradation of valsartan was higher during oxidative stress than other stress.

  9. A very simple high-performance liquid chromatographic method with fluorescence detection for the determination of gemifloxacin in human breast milk.

    Science.gov (United States)

    Sagirli, Olcay; Demirci, Seda; Önal, Armağan

    2015-12-01

    A high-performance liquid chromatographic method with fluorescence detection was developed and validated for the determination of gemifloxacin in human breast milk. The proposed method allows the determination of gemifloxacin in breast milk samples without complex sample preparation. The samples were mixed with a mobile phase and filtered with a 0.45 µm polytetrafluoroethylene filter before analysis. Chromatographic separation was carried out on a C18 column (150 × 4.6 mm, 5 µm I.D.) using methanol:50 mM ortho-phosphoric acid solution (40:60) as the mobile phase with a 1.0 mL/min flow rate. Quantitation was performed using fluorescence detection with an excitation wavelength at 272 nm and an emission wavelength at 395 nm. The linear range was found to be 0.1-2.5 µg/mL. The method was applied successfully for the determination of gemifloxacin in breast milk obtained from a breastfeeding mother after oral administration of a single tablet that included 320 mg gemifloxacin per gemifloxacin tablet. PMID:25808579

  10. Determination of Li, Na, K and Cs in UO2 by flame ASS/flame AES with prion TBP levextrel resin chromatographic separation

    International Nuclear Information System (INIS)

    An analytical method for the determination of Li, Na, K and Cs in uranium dioxide is developed. The uranium dioxide powder is dissolved in nitric acid, then the sample solution is passed through a TBP levextrel chromatographic column. 5.5 mol · l-1 HNO3 is used as eluent. The eluate is analysed by air-C2H2AAS for Li, Na and K, and air-C2H2 AES for Cs, respectively. The concentration range determined Li, Na, K and Cs in UO2 is 2 x 10-6-20 x 10-6 for 0.5 g sample. The recovery is from 96% to 103% and RSD is 3%, 5%, 7% and 6% for Li, Na, K and Cs, respectively. This method is simple and reliant. It was accepted as a national standard analytical method in China now

  11. Extraction chromatographic studies on Am(III) and U(VI) using Cyanex-923 impregnated Chromosorb W in nitric acid medium

    International Nuclear Information System (INIS)

    The uptake of Am(III) and U(VI) has been investigated under varying nitric acid concentrations (0.01-3 M HNO3) by an extraction chromatographic resin material viz. Cyanex-923 coated on Chromosorb W. Whereas quantitative sorption of U(VI) was observed throughout the [HNO3] range, DAm values showed a maximum at 0.1 M HNO3. Presence of 5 M NaNO3 enhanced the DAm values significantly up to 0.1 M HNO3. In column experiments, breakthrough capacity was evaluated as 42 ± 2 mg of Nd(Am) per gram of the resin material. 1.5 ml of 8 M HNO3 was sufficient to elute ∼ 98.5% of the sorbed Nd(Am). (author)

  12. Modified normal-phase ion-pair chromatographic methods for the facile separation and purification of imidazolium-based ionic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Urban, ND; Schenkel, MR; Robertson, LA; Noble, RD; Gin, DL

    2012-07-04

    lmidazolium- and oligo(imidazolium)-based ionic organic compounds are important in the design of room-temperature ionic liquid materials; however, the chromatographic analysis and separation of such compounds are often difficult. A convenient and inexpensive method for effective thin-layer chromatography (TLC) analysis and column chromatography separation of imidazolium-based ionic compounds is presented. Normal-phase ion-pair TLC is used to effectively analyze homologous mixtures of these ionic compounds. Subsequent separation of the mixtures is performed using ion-pair flash chromatography on normal-phase silica gel, yielding high levels of recovery. This method also results in a complete exchange of the counter anion on the imidazolium compounds to the anion of the ion-pair reagent. (C) 2012 Elsevier Ltd. All rights reserved.

  13. The use of chromatographic indexes to study the biodegradation of crude oil in cold/icy seawater

    International Nuclear Information System (INIS)

    A group of five protected mesocosms (3.5 m3 each) was used to study the biodegradation of dispersed crude oil in cold and icy seawater. A wide range of oil concentrations was tested over four experiments lasting two weeks to six months. Various oil treatments were studied with respect to the natural bacterial degradation: chemically dispersed and untreated crude oil; and oil adsorbed on, and released from, an immersed substrate. The study was concerned with oil accommodated in the water column, accumulated in surface (sheens and emulsions), and collected in sediment traps. The oil biodegradation was assessed by means of the following gas chromatographic indexes: C17/pristane; C18/phytane; n-alkanes/isoprenoids; pristane/phytane; naphthalene/phenanthrene; 2-methyl naphthalene/1-methyl naphthalene; and methylnaphthalenes/total substituted naphthalenes. A combined index of biodegradation defined from the most significant hydrocarbon ratios is proposed to evaluate the overall biodegradation of dissolved compounds and oil droplets, involving both aliphatic and aromatic hydrocarbons. Coupled with mesocosm facilities, this approach appears very convenient to determine the potential degradability of crude oils by natural indigenous microflora. 26 refs., 11 figs., 2 tabs

  14. Development and validation of a fast chromatographic method for screening and quantification of legal and illegal skin whitening agents.

    Science.gov (United States)

    Desmedt, B; Rogiers, V; Courselle, P; De Beer, J O; De Paepe, K; Deconinck, E

    2013-09-01

    During the last years, the EU market is flooded by illegal cosmetics via the Internet and a so-called "black market". Among these, skin-bleaching products represent an important group. They contain, according to the current European cosmetic legislation (Directive 76/768/EEC), a number of illegal active substances including hydroquinone, tretinoin and corticosteroids. These may provoke as well local as systemic toxic effects, being the reason for their banning from the EU market. To control this market there is a need for a fast screening method capable of detecting illegal ingredients in the wide variety of existing bleaching cosmetic formulations. In this paper the development and validation of an ultra high pressure liquid chromatographic (UHPLC) method is described. The proposed method makes use of a Waters Acquity BEH shield RP18 column with a gradient using 25 mM ammonium borate buffer (pH 10) and acetonitrile. This method is not only able to detect the major illegal (hydroquinone, tretinoin and six dermatologic active corticosteroids) and legal whitening agents, the latter having restrictions with respect to concentration and application (kojic acid, arbutin, nicotinamide and salicylic acid), but can also quantify these in a run time of 12 min. The method was successfully validated using the "total error" approach in accordance with the validation requirements of ISO-17025. During the validation a variety of cosmetic matrices including creams, lotions and soaps were taken into consideration. PMID:23708434

  15. Development of liquid chromatographic enantiomer separation methods and validation for the estimation of (R)-enantiomer in eslicarbazepine acetate.

    Science.gov (United States)

    Mone, Mahesh Kumar; Chandrasekhar, K B

    2011-01-01

    Chiral separation method development was carried out for eslicarbazepine acetate and its (R)-enantiomer on diverse chiral stationary phases. Better chiral selectivity was observed on cellulose tris-(3,5-dichlorophenylcarbamate) immobilized column (Chiralpak IC-3). Under polar organic mode (POM), with 100% acetonitrile as mobile phase and 0.5 ml/min flow, a resolution close to three was achieved. With normal phase (NP) mobile phase consisting dichloromethane:ethanol (90:10, v/v) and 1.0 ml/min flow, a resolution close to six was achieved. Detection was done by UV at 220 and 240 nm respectively. Both the methods were found to be robust and were validated with respect to robustness, precision, linearity, limit of detection, limit of quantification and accuracy. The proposed methods are suitable for the accurate estimation of (R)-enantiomer in bulk drug samples up to 0.1% when a 1mg/ml analyte test solution is chromatographed. PMID:20832962

  16. Development and validation of a reversed phase liquid chromatographic method for analysis of oxytetracycline and related impurities.

    Science.gov (United States)

    Kahsay, Getu; Shraim, Fairouz; Villatte, Philippe; Rotger, Jacques; Cassus-Coussère, Céline; Van Schepdael, Ann; Hoogmartens, Jos; Adams, Erwin

    2013-03-01

    A simple, robust and fast high-performance liquid chromatographic method is described for the analysis of oxytetracycline and its related impurities. The principal peak and impurities are all baseline separated in 20 min using an Inertsil C₈ (150 mm × 4.6 mm, 5 μm) column kept at 50 °C. The mobile phase consists of a gradient mixture of mobile phases A (0.05% trifluoroacetic acid in water) and B (acetonitrile-methanol-tetrahydrofuran, 80:15:5, v/v/v) pumped at a flow rate of 1.3 ml/min. UV detection was performed at 254 nm. The developed method was validated for its robustness, sensitivity, precision and linearity in the range from limit of quantification (LOQ) to 120%. The limits of detection (LOD) and LOQ were found to be 0.08 μg/ml and 0.32 μg/ml, respectively. This method allows the separation of oxytetracycline from all known and 5 unknown impurities, which is better than previously reported in the literature. Moreover, the simple mobile phase composition devoid of non-volatile buffers made the method suitable to interface with mass spectrometry for further characterization of unknown impurities. The developed method has been applied for determination of related substances in oxytetracycline bulk samples available from four manufacturers. The validation results demonstrate that the method is reliable for quantification of oxytetracycline and its impurities. PMID:23277151

  17. Evaluation of the application of some gas chromatographic methods for the determination of properties of synthetic fuels

    Science.gov (United States)

    Antoine, A. C.

    1979-01-01

    The purpose of the investigation was to evaluate the applicability, to some synthetic fuels, of some gas chromatographic methods now under development for use with petroleum based fuels. Thirty-two jet and diesel fuel samples which were prepared from oil shale and coal syncrudes were examined. The boiling range distribution of each was determined by gas chromatography, and from that data distillation properties were calculated. The calculated results gave sufficient agreement with the measured values that the equations could be useable in their present form. Bulk fuel properties were calculated for the sixteen JP-5 and Diesel No. 2 type fuels. The results show that the equations would not give useable results. Capillary column gas chromatography was used to determine the n-alkane content of the eight JP-5 type samples and the results related to the observed freezing points. The results show that the concentrations of the long straight chain molecules in the fuels exert influence on the freezing point but are not the complete controlling factor.

  18. Determination of thymol in human plasma by automated headspace solid-phase microextraction-gas chromatographic analysis.

    Science.gov (United States)

    Kohlert, Claudia; Abel, Gudrun; Schmid, Eleonora; Veit, Markus

    2002-02-01

    A reliable and sensitive method was developed for determination of thymol in human plasma by automated headspace solid-phase microextraction (SPME). After enzymatic cleavage of thymol sulfate thymol was extracted by a 65 microm polydimethylsiloxane-divinylbenzene crimped fiber (Supelco) after addition of sodium chloride and phosphoric acid (85%). Desorption of the fiber was performed in the injection port of a gas chromatograph at 220 degrees C (HP 5890; 50 m x 0.2 mm I.D., 0.2 microm HP Innowax capillary column; flame ionization detection). Fibers were used repeatedly up to 40 analysis. The recovery was 5% after 35 min of extraction. The calibration curve was linear in the range of 8.1-203.5 ng ml(-1) with a limit of quantitation (LOQ) of 8.1 ng ml(-1). The within-day and between-day precision and accuracy were thymol-containing herbal extract only thymol sulfate, no free thymol, could be detected in human plasma, thus analysis of thymol was after enzymatic cleavage of thymol sulfate. It is concluded that the newly developed automated method can be used in clinical trials on bioavailability and pharmacokinetics of thymol-containing herbal medicinal products. PMID:11863281

  19. Multivariate curve resolution of incomplete fused multiset data from chromatographic and spectrophotometric analyses for drug photostability studies

    International Nuclear Information System (INIS)

    Highlights: • A new MCR-ALS algorithm is proposed for the analysis of incomplete fused multiset. • Resolution of the data allowed the description of amiloride kinetic photodegradation. • The new MCR-ALS algorithm can be easily applied to other drugs and chemicals. - Abstract: An advanced and powerful chemometric approach is proposed for the analysis of incomplete multiset data obtained by fusion of hyphenated liquid chromatographic DAD/MS data with UV spectrophotometric data from acid–base titration and kinetic degradation experiments. Column- and row-wise augmented data blocks were combined and simultaneously processed by means of a new version of the multivariate curve resolution-alternating least squares (MCR-ALS) technique, including the simultaneous analysis of incomplete multiset data from different instrumental techniques. The proposed procedure was applied to the detailed study of the kinetic photodegradation process of the amiloride (AML) drug. All chemical species involved in the degradation and equilibrium reactions were resolved and the pH dependent kinetic pathway described

  20. Micellar electrokinetic capillary chromatographic determination of artificial sweeteners in low-Joule soft drinks and other foods.

    Science.gov (United States)

    Thompson, C O; Trenerry, V C; Kemmery, B

    1995-03-10

    A rapid method for the determination of artificial sweeteners in low-Joule soft drinks and other foods by micellar electrokinetic capillary chromatography (MEKC) is described. Caffeine, benzoic acid and sorbic acid, which are often added to soft drinks, can also be determined with this procedure. The artificial sweeteners, aspartame, saccharin, acesulfame-K, alitame and dulcin, and the other food additives are well separated in less than 12 min using an uncoated fused-silica capillary column with a buffer consisting of 0.05 M sodium deoxycholate, 0.01 M potassium dihydrogenorthophosphate, 0.01 M sodium borate operating at 20 kV. Dehydroacetic acid was used as the internal standard for the determinations. The levels of artificial sweeteners, preservatives and caffeine were in good agreement with those determined by the high-performance liquid chromatographic (HPLC) procedure currently used in our Laboratory. The MEKC procedure has the same order of repeatability, is faster and less costly to operate than the HPLC method. PMID:7704194

  1. Comparison of various extraction methods for policosanol from rice bran wax and establishment of chromatographic fingerprint of policosanol.

    Science.gov (United States)

    Wang, Mei-Fei; Lian, Hong-Zhen; Mao, Li; Zhou, Jing-Ping; Gong, Hui-Juan; Qian, Bao-Yong; Fang, Yan; Li, Jie

    2007-07-11

    A capillary gas chromatographic (GC) method has been developed for the separation and determination of policosanol components extracted from rice bran wax. A Varian CP-sil 8 CB column was employed, and an oven temperature was programmed. Gas chromatography-mass spectrometry (GC-MS) was used to identify the composition of policosanol. Quantitative analysis was carried out by means of hydrogen flame ionization detector (FID) with dinonyl phthalate (DNP) as internal standard. The results indicated that the extract obtained by dry saponification has the highest contents of octacosanol and triacontanol among extracts by all used extraction methods including dry saponification, saponification in alcohol, saponification in water (neutralized and non-neutralized), and transesterification. Meanwhile, the GC-MS fingerprint of policosanol extracted by dry saponification has been established. Euclidean distance similarity calculation showed remarkable consistency of compositions and contents among 12 batches of policosanol from a rice bran wax variety. This protocol provided a rapid and feasible method for quality control of policosanol products. PMID:17564456

  2. Multivariate curve resolution of incomplete fused multiset data from chromatographic and spectrophotometric analyses for drug photostability studies

    Energy Technology Data Exchange (ETDEWEB)

    Luca, Michele De, E-mail: michele.deluca@unical.it [Department of Pharmacy, Health and Nutritional Sciences, University of Calabria, Via P. Bucci, Rende, CS 87036 (Italy); Ragno, Gaetano; Ioele, Giuseppina [Department of Pharmacy, Health and Nutritional Sciences, University of Calabria, Via P. Bucci, Rende, CS 87036 (Italy); Tauler, Romà [Department of Environmental Chemistry, IDAEA-CSIC, C/Jordi Girona, 18-26, Barcelona 08034 (Spain)

    2014-07-21

    Highlights: • A new MCR-ALS algorithm is proposed for the analysis of incomplete fused multiset. • Resolution of the data allowed the description of amiloride kinetic photodegradation. • The new MCR-ALS algorithm can be easily applied to other drugs and chemicals. - Abstract: An advanced and powerful chemometric approach is proposed for the analysis of incomplete multiset data obtained by fusion of hyphenated liquid chromatographic DAD/MS data with UV spectrophotometric data from acid–base titration and kinetic degradation experiments. Column- and row-wise augmented data blocks were combined and simultaneously processed by means of a new version of the multivariate curve resolution-alternating least squares (MCR-ALS) technique, including the simultaneous analysis of incomplete multiset data from different instrumental techniques. The proposed procedure was applied to the detailed study of the kinetic photodegradation process of the amiloride (AML) drug. All chemical species involved in the degradation and equilibrium reactions were resolved and the pH dependent kinetic pathway described.

  3. A general static-headspace gas chromatographic method for determination of residual benzene in oral liquid pharmaceutical products.

    Science.gov (United States)

    Liu, Hui; Tang, Qinglin; Markovich, Robert J; Rustum, Abu M

    2011-01-25

    Sodium benzoate is used in oral liquid pharmaceutical products for its anti-microbial properties. The benzoate salts present in liquid pharmaceutical products can potentially generate residual levels of free benzene during manufacturing of the drug product and or during the shelf-life of the product under its storage conditions. To ensure the safety and quality of the pharmaceutical products (containing benzoate in the formulation), a selective and sensitive analytical method is required to monitor residual benzene in oral liquid pharmaceutical products. In this paper, we report the development and validation of a general static-headspace gas chromatographic (SH-GC) method to determine residual benzene in oral liquid pharmaceutical products. The liquid pharmaceutical drug product sample is dissolved in dimethylsulfoxide (DMSO) in a GC headspace vial. A DB-624 capillary column (30 m x 0.32 mm I.D. and 1.8 μm film thickness) was used under isothermal conditions with a flame ionization detection (FID). The benzene peak was well separated from all other volatile compounds that are present in the formulation of a number of liquid drug products. This method was successfully validated using a representative oral liquid pharmaceutical drug product. The limit of detection of the method for benzene is 0.5 ppm which met the 2 ppm limit of current ICH guideline for residual benzene in pharmaceutical products. PMID:20926217

  4. Chromatographic separation of cerium(Ⅲ) in L-valine medium using poly[dibenzo-18-crown-6

    Institute of Scientific and Technical Information of China (English)

    SABALE Sandip R; MOHITE Baburao S

    2009-01-01

    A column chromatographic method has been developed for the separation and determination of cerium(Ⅲ) using poly[dibenzo-18-crown-6]. The separation was carried out in L-valine medium. The adsorption of cerium(Ⅲ) was quantitative from 1×10-1 to 1×10-4 mol/L L-valine. Amongst the various eluents, 1.0-8.0 mol/L hydrochloric acid, 1.0-8.0 mol/L hydrobromic acid, 1.0-8.0 mol/L perchloric acid, 1.0-2.0 mol/L sulfuric acid and 4.0-5.0 mol/L acetic acid, were found to be the efficient eluents for cerium(Ⅲ). The capacity of poly[dibenzo-18-crown-6] for cerium(Ⅲ) was (0.428±0.01) mmol/g. The method was applied to the separation of cerium(Ⅲ) from associated elements link uranium(Ⅵ) and thorium(Ⅳ). It was also applied for the determination of cerium(Ⅲ) in geological samples. The method is simple, rapid and selective with good reproducibility (approximately±2% ).

  5. Development and validation of a stability-indicating reverse phase ultra performance liquid chromatographic method for the estimation of nebivolol impurities in active pharmaceutical ingredients and pharmaceutical formulation.

    Science.gov (United States)

    Thummala, Veera Raghava Raju; Lanka, Mohana Krishna

    2015-10-01

    A sensitive, stability-indicating gradient reverse phase ultra performance liquid chromatographic method has been developed for the quantitative estimation of nebivolol impurities in active pharmaceutical ingredient (API) and pharmaceutical formulation. Efficient chromatographic separation was achieved on an Acquity BEH C18 column (100 mm x 2.1 mm, 1.7 μm) with mobile phase of a gradient mixture. The flow rate of the mobile phase was 0.18 mL/min with column temperature of 30 degrees C and detection wavelength of 281 nm. The relative response factor values of (R*)-2-( benzylamino)-1-((S*)-6-fluorochroman-2-yl) ethanol ((R x S*) NBV-), (R)-1-((R)-6-fluorochroman-2-yl)-2-((S)-2-((S)-6-fluoro-chroman-2-yl)-2-hydroxyethyl-amino) ethanol ((RRSS) NBV-3), 1-(chroman-2-yl)-2-(2-(6-fluorochroman-2-yl)-2-hydroxyethyl amino) ethanol (monodesfluoro impurity), (S)-1-((R)-6-fluorochroman-2-yl)-2-((R)-2 (S*)-6-fluoro-chroman-2-yl)-2-hydroxyethylamino) ethanol hydrochloride ((RSRS) NBV-3) and (R*)-1-((S*)-6-fluorochroman-2-yl)-2-((S*)-2-((S*)-6-fluoro-chroman-2-yl)-2-hydroxyethylamino) ethanol ((R* S* S* S*) NBV-2) were 0.65, 0.91, 0.68, 0.92 and 0.91 respectively. Nebivolol formulation sample was subjected to the stress conditions of acid, base, oxidative, hydrolytic, thermal, humidity and photolytic degradation. Nebivolol was found to degrade significantly under peroxide stress condition. The degradation products were well resolved from nebivolol and its impurities. The peak purity test results confirmed that the nebivolol peak was homogenous and pure in all stress samples and the mass balance was found to be more than 98%, thus proving the stability-indicating power of the method. The developed method was validated according to International Conference on Hormonization (ICH) guidelines with respect to specificity, linearity, limits of detection and quantification, accuracy, precision and robustness. PMID:26930962

  6. Miniaturized MEMS-Based Gas Chromatograph for High Inertial Loads Associated with Planetary Missions Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Thorleaf Research, Inc. proposes to develop a rugged, miniaturized, low power MEMS-based gas chromatograph (GC) capable of handling the high inertial loads...

  7. ON THE ORIGIN OF THE HIGH COLUMN DENSITY TURNOVER IN THE H I COLUMN DENSITY DISTRIBUTION

    International Nuclear Information System (INIS)

    We study the high column density regime of the H I column density distribution function and argue that there are two distinct features: a turnover at NHI ≈ 1021 cm–2, which is present at both z = 0 and z ≈ 3, and a lack of systems above NHI ≈ 1022 cm–2 at z = 0. Using observations of the column density distribution, we argue that the H I-H2 transition does not cause the turnover at NHI ≈ 1021 cm–2 but can plausibly explain the turnover at NHI ∼> 1022 cm–2. We compute the H I column density distribution of individual galaxies in the THINGS sample and show that the turnover column density depends only weakly on metallicity. Furthermore, we show that the column density distribution of galaxies, corrected for inclination, is insensitive to the resolution of the H I map or to averaging in radial shells. Our results indicate that the similarity of H I column density distributions at z = 3 and 0 is due to the similarity of the maximum H I surface densities of high-z and low-z disks, set presumably by universal processes that shape properties of the gaseous disks of galaxies. Using fully cosmological simulations, we explore other candidate physical mechanisms that could produce a turnover in the column density distribution. We show that while turbulence within giant molecular clouds cannot affect the damped Lyα column density distribution, stellar feedback can affect it significantly if the feedback is sufficiently effective in removing gas from the central 2-3 kpc of high-redshift galaxies. Finally, we argue that it is meaningful to compare column densities averaged over ∼ kpc scales with those estimated from quasar spectra that probe sub-pc scales due to the steep power spectrum of H I column density fluctuations observed in nearby galaxies.

  8. Post Column Derivatization Using Reaction Flow High Performance Liquid Chromatography Columns.

    Science.gov (United States)

    Jones, Andrew; Pravadali-Cekic, Sercan; Hua, Stanley; Kocic, Danijela; Camenzuli, Michelle; Dennis, Gary; Shalliker, Andrew

    2016-01-01

    A protocol for the use of reaction flow high performance liquid chromatography columns for methods employing post column derivatization (PCD) is presented. A major difficulty in adapting PCD to modern HPLC systems and columns is the need for large volume reaction coils that enable reagent mixing and then the derivatization reaction to take place. This large post column dead volume leads to band broadening, which results in a loss of observed separation efficiency and indeed detection in sensitivity. In reaction flow post column derivatization (RF-PCD) the derivatization reagent(s) are pumped against the flow of mobile phase into either one or two of the outer ports of the reaction flow column where it is mixed with column effluent inside a frit housed within the column end fitting. This technique allows for more efficient mixing of the column effluent and derivatization reagent(s) meaning that the volume of the reaction loops can be minimized or even eliminated altogether. It has been found that RF-PCD methods perform better than conventional PCD methods in terms of observed separation efficiency and signal to noise ratio. A further advantage of RF-PCD techniques is the ability to monitor effluent coming from the central port in its underivatized state. RF-PCD has currently been trialed on a relatively small range of post column reactions, however, there is currently no reason to suggest that RF-PCD could not be adapted to any existing one or two component (as long as both reagents are added at the same time) post column derivatization reaction. PMID:27168419

  9. Counterflow isotachophoresis in a monolithic column.

    Science.gov (United States)

    Liu, Bingwen; Cong, Yongzheng; Ivory, Cornelius F

    2014-09-01

    This study describes stationary counterflow isotachophoresis (ITP) in a poly(acrylamide-co-N,N'-methylenebisacrylamide) monolithic column as a means for improving ITP processing capacity and reducing dispersion. The flow profile in the monolith was predicted using COMSOL's Brinkman Equation application mode, which revealed that the flow profile was mainly determined by monolith permeability. As monolith permeability decreases, the flow profile changes from a parabolic shape to a plug shape. An experimental monolithic column was prepared in a fused-silica capillary using an ultraviolet-initiated polymerization method. A monolithic column made from 8% (wt.) monomer was chosen for the stationary counterflow ITP experiments. Counterflow ITP in the monolithic column showed undistorted analyte zones with significantly reduced dispersion compared to the severe dispersion observed in an open capillary. Particularly, for r-phycoerythrin focused by counterflow ITP, its zone width in the monolithic column was only one-third that observed in an open capillary. These experiments demonstrate that stationary counterflow ITP in monoliths can be a robust and practical electrofocusing method. PMID:24935025

  10. Robust Matrix Completion with Corrupted Columns

    CERN Document Server

    Chen, Yudong; Caramanis, Constantine; Sanghavi, Sujay

    2011-01-01

    This paper considers the problem of matrix completion, when some number of the columns are arbitrarily corrupted, potentially by a malicious adversary. It is well-known that standard algorithms for matrix completion can return arbitrarily poor results, if even a single column is corrupted. What can be done if a large number, or even a constant fraction of columns are corrupted? In this paper, we study this very problem, and develop an efficient algorithm for its solution. Our results show that with a vanishing fraction of observed entries, it is nevertheless possible to succeed in performing matrix completion, even when the number of corrupted columns grows. When the number of corruptions is as high as a constant fraction of the total number of columns, we show that again exact matrix completion is possible, but in this case our algorithm requires many more -- a constant fraction -- of observations. One direct application comes from robust collaborative filtering. Here, some number of users are so-called mani...

  11. Effect of backmixing on pulse column performance

    Energy Technology Data Exchange (ETDEWEB)

    Miao, Y.W.

    1979-05-01

    A critical survey of the published literature concerning dispersed phase holdup and longitudinal mixing in pulsed sieve-plate extraction columns has been made to assess the present state-of-the-art in predicting these two parameters, both of which are of critical importance in the development of an accurate mathematical model of the pulse column. Although there are many conflicting correlations of these variables as a function of column geometry, operating conditions, and physical properties of the liquid systems involved it has been possible to develop new correlations which appear to be useful and which are consistent with much of the available data over the limited range of variables most likely to be encountered in plant sized equipment. The correlations developed were used in a stagewise model of the pulse column to predict product concentrations, solute inventory, and concentration profiles in a column for which limited experimental data were available. Reasonable agreement was obtained between the mathematical model and the experimental data. Complete agreement, however, can only be obtained after a correlation for the extraction efficiency has been developed. The correlation of extraction efficiency was beyond the scope of this work.

  12. Effect of backmixing on pulse column performance

    International Nuclear Information System (INIS)

    A critical survey of the published literature concerning dispersed phase holdup and longitudinal mixing in pulsed sieve-plate extraction columns has been made to assess the present state-of-the-art in predicting these two parameters, both of which are of critical importance in the development of an accurate mathematical model of the pulse column. Although there are many conflicting correlations of these variables as a function of column geometry, operating conditions, and physical properties of the liquid systems involved it has been possible to develop new correlations which appear to be useful and which are consistent with much of the available data over the limited range of variables most likely to be encountered in plant sized equipment. The correlations developed were used in a stagewise model of the pulse column to predict product concentrations, solute inventory, and concentration profiles in a column for which limited experimental data were available. Reasonable agreement was obtained between the mathematical model and the experimental data. Complete agreement, however, can only be obtained after a correlation for the extraction efficiency has been developed. The correlation of extraction efficiency was beyond the scope of this work

  13. Strengthening brick masonry columns using ferrocement

    International Nuclear Information System (INIS)

    Prior to concrete becoming a widely used building material, brick masonry walls and columns were mainly provided in buildings in most parts of the Indo-Pak Sub-Continent. Quite a large number of these old brick masonry buildings have lost strength, which needs to be restored. A research work was carried out to enhance the strength of brick masonry columns through confinement with ferrocement so as to act as a retrofit arrangement in restoring strength of old brick masonry columns. Composite behavior of masonry columns coated with/without ferrocement having 1, 2 and 3 layers of wire meshes were prepared and tested. Bonding agent was also used for some cases. Test results revealed that the application of ferrocement coating on bare masonry columns enhances the compressive strength quite significantly. Ferrocement specimens having 1 layer of wire mesh wrapped inside showed an increase in failure load up to 134% as compared to control specimen. The cracking resistance and stable crack growth mechanism is also improved. The use of bonding agent does not help in improving load carrying capacity however it is effective in controlling the spalling of concrete cover. (author)

  14. Properties of PAN-TBP extraction chromatographic material

    International Nuclear Information System (INIS)

    Three production routes of the preparation of a solid extractant based on tributylphosphate (TBP) embedded in the polyacrylonitrile matrix (PAN) have been studied. The method of direct PAN coagulation with TBP was found to be not viable due to the significant TBP solubility in the coagulation bath. The most suitable PAN-TBP solid extractant was prepared by the well-known impregnation method of ready-made neat PAN beads. The kinetics of uranium extraction from 3 mol L-1 HNO3, the effect of nitrate and nitric acids concentrations on the value of weight distribution coefficients Dg as well as the uranium 'extraction isotherm' were determined for this material. Uranium extraction was rather fast, approximately 1 h was sufficient for the equilibrium achievement. Capacity for the uranium uptake, measured in batch experiments on PAN-TBP for 0.048 mol L-1 of uranium in 3 mol L-1 nitric acid, was found to be q = 0.363 mmol g-1 (58 % of the theoretical capacity). It was concluded that PAN-TBP material behaves like TBP in liquid-liquid extraction. Extraction capacity determined in column experiments was lower (by about 23 %) than expected from the 'extraction isotherm' due to the TBP leaching out of the column. The thus prepared material is therefore not very suitable for multicycle extraction and stripping and can be used once, particularly for the analytical purposes. (author)

  15. Use of tridecylamine for extraction-chromatographic separation of indium, cadmium, zinc, iron and lead

    International Nuclear Information System (INIS)

    Extraction and the chromatographic behaviour of indium, cadmium, zinc, lead, and iron (3) in the system tridecylamine TDA)-toluene-HCl are studied. These data are used to determine the Me:TDA ratio in the ion associates extracted. A scheme of extraction-chromatographic concentration of indium against the background of macrocomponents and a scheme of separation of mixtures of the elements investigated are proposed

  16. Determination of the chemical composition of tea by chromatographic methods: a review

    OpenAIRE

    Alexandr Ya. Yashin; Nemzer, Boris V; Emilie Combet; Yakov I. Yashin

    2015-01-01

    Despite the fact that mankind has been drinking tea for more than 5000 years, its chemical composition has been studied only in recent decades. These studies are primarily carried out using chromatographic methods. This review summarizes the latest information regarding the chemical composition of different tea grades by different chromatographic methods, which has not previously been reviewed in the same scope. Over the last 40 years, the qualitative and quantitative analyses of high volatil...

  17. Isotopic chromatographic-spectral determination of carbon monoxide in helium, neon and nitrogen

    International Nuclear Information System (INIS)

    Isotopic-chromatographic-spectral method is proposed for determination of carbon monoxide in helium, neon and nitrogen using carbon 12, 13 isotope dilution technique as well as cryogenic-adsorption accumulation and chromatographic separation of impurities. The limits for determination of CO in helium, neon and nitrogen are 1 x 10-6, 6 x 10-7 and 7 x 10-7 mol% respectively. Reference samples are not required

  18. Ionic liquids as porogens in the microwave-assisted synthesis of methacrylate monoliths for chromatographic application

    Energy Technology Data Exchange (ETDEWEB)

    Singco, Brenda; Lin, Chen-Lan; Cheng, Yi-Jie; Shih, Yung-Han [Department of Chemistry and Center for Nanotechnology, CYCU (Chung Yuan Christian University), 200 Chung Pei Road, Chung-Li 320, Taiwan (China); Huang, Hsi-Ya, E-mail: hyhuang@cycu.edu.tw [Department of Chemistry and Center for Nanotechnology, CYCU (Chung Yuan Christian University), 200 Chung Pei Road, Chung-Li 320, Taiwan (China)

    2012-10-09

    Highlights: Black-Right-Pointing-Pointer An efficient and cleaner monoliths preparation utilizing ionic liquids in conjunction with microwave Black-Right-Pointing-Pointer These ionic liquids with varied cation alkyl chain and anion type successfully tuned the morphology of different alkyl methacrylates Black-Right-Pointing-Pointer Small molecules and peptide digests separated well in these monoliths. - Abstract: Several imidazolium-based ionic liquids (ILs) with varying cation alkyl chain length (C{sub 4}-C{sub 10}) and anion type (tetrafluoroborate ([BF{sub 4}]{sup -}), hexafluorophosphate ([PF{sub 6}]{sup -}) and bis(trifluoromethylsulfonyl)imide ([Tf{sub 2}N]{sup -})) were used as reaction media in the microwave polymerization of methacrylate-based stationary phases. Scanning electron micrographs and backpressures of poly(butyl methacrylate-ethylene dimethacrylate) (poly(BMA-EDMA)) monoliths synthesized in the presence of these ionic liquids demonstrated that porosity and permeability decreased when cation alkyl chain length and anion hydrophobicity were increased. Performance of these monoliths was assessed for their ability to separate parabens by capillary electrochromatography (CEC). Intra-batch precision (n = 3 columns) for retention time and peak area ranged was 0.80-1.13% and 3.71-4.58%, respectively. In addition, a good repeatability of RSD{sub Retentiontime} = <0.30% and {approx}1.0%, RSD{sub Peakarea} = <1.30% and <4.3%, and RSD{sub Efficiency} = <0.6% and <11.5% for intra-day and inter-day, respectively exemplify monolith performance reliability for poly(BMA-EDMA) fabricated using 1-hexyl-3-methylimidazolium tetrafluoroborate ([C{sub 6}mim][BF{sub 4}]) porogen. This monolith was also tested for its potential in nanoLC to separate protein digests in gradient mode. ILs as porogens also fabricated different alkyl methacrylate (AMA) (C4-C18) monoliths. Furthermore, employing binary IL porogen mixture such as 1-butyl-3-methylimidazolium tetrafluoroborate

  19. Rapid and simultaneous determination of tetrafluoroborate, thiocyanate and hexafluorophosphate by high-performance liquid chromatography using a monolithic column and direct conductivity detection.

    Science.gov (United States)

    Yang, Ling; Yu, Hong; Wang, Yaqin

    2010-01-01

    A method was developed for fast and simultaneous determination of tetrafluoroborate (BF(4)(-)), thiocyanate (SCN(-)) and hexafluorophosphate (PF(6)(-)) by high-performance liquid chromatography using a silica-based monolithic column and direct (non-suppressed) conductivity detection. Chromatographic separation was performed on a Chromolith Speed ROD RP-18e column with tetrabutylammonium hydroxide (TBA) + citric acid + acetonitrile as eluent. The effects of the types of eluent, TBA concentration, acetonitrile volume fraction, eluent pH, column temperature and flow rate on the retention of anions were investigated. The optimized chromatographic conditions were selected. Under the optimal conditions, the baseline separation of BF(4)(-), SCN(-) and PF(6)(-) was achieved without any interference by other anions (F(-), Cl(-), Br(-), I(-), NO(3)(-), ClO(3)(-) and SO(4)(2-)). The detection limit (S/N = 3) was 0.42, 0.46 and 1.42 mg L(-1) for BF(4)(-), SCN(-) and PF(6)(-), respectively. The present method was successfully applied to the determination of BF(4)(-), SCN(-) and PF(6)(-) in ionic liquids. PMID:20702939

  20. Ion-chromatographic estimation of chloride in colloidal graphite suspension

    International Nuclear Information System (INIS)

    Determination of major, minor and trace constituents in the nuclear fuel and structural materials has always been a fascinating field of advanced analytical chemistry. Till few years ago, most of the routine analytical techniques were based on prior chemical separation procedures followed by conventional classical techniques of analysis like gravimetric and volumetric methods. These conventional methods are very cumbersome and time consuming ones along with the requirement of different suitable complexing agents. Also, these classical methods are not suitable for trace elemental analysis. In the present day context, the requirement of trace level measurements in diversified matrices has become order of the day. The trace levels of measurements to be reported are going from ppm to ppt levels with l increase in confidence levels. In this regard, Ion Chromatographic method of analysis assumes a significant and pivotal role in the field of analytical chemistry. The present paper describes the estimation of chloride in graphite suspension using ion chromatography with its prior separation by pyro-hydrolysis technique. The furnace temperature, heating rate, time of heating, pH of collecting solution and sample weight are optimized to get maximum extractability of chloride from the graphite suspension during pyro-hydrolysis. The instrument was calibrated using synthetically prepared chloride standards in the range of 0.1 μlg/ml to 1.0 μg/ml. A suppressor based Metrohm make 850 professional IC is used for the analysis. A mixture of sodium carbonate and bicarbonate solution is used as eluent. The paper describes the complete experimental details. The values obtained by IC are compared with a spectrophotometric method and the comparison is in good agreement. A RSD of ± 5% has been achieved in IC measurements

  1. Computational analysis of ozonation in bubble columns

    International Nuclear Information System (INIS)

    This paper presents a new computational ozonation model based on the principle of computational fluid dynamics along with the kinetics of ozone decay and microbial inactivation to predict the performance of ozone disinfection in fine bubble columns. The model can be represented using a mixture two-phase flow model to simulate the hydrodynamics of the water flow and using two transport equations to track the concentration profiles of ozone and microorganisms along the height of the column, respectively. The applicability of this model was then demonstrated by comparing the simulated ozone concentrations with experimental measurements obtained from a pilot scale fine bubble column. One distinct advantage of this approach is that it does not require the prerequisite assumptions such as plug flow condition, perfect mixing, tanks-in-series, uniform radial or longitudinal dispersion in predicting the performance of disinfection contactors without carrying out expensive and tedious tracer studies. (author)

  2. Neutron camera employing row and column summations

    Science.gov (United States)

    Clonts, Lloyd G.; Diawara, Yacouba; Donahue, Jr, Cornelius; Montcalm, Christopher A.; Riedel, Richard A.; Visscher, Theodore

    2016-06-14

    For each photomultiplier tube in an Anger camera, an R.times.S array of preamplifiers is provided to detect electrons generated within the photomultiplier tube. The outputs of the preamplifiers are digitized to measure the magnitude of the signals from each preamplifier. For each photomultiplier tube, a corresponding summation circuitry including R row summation circuits and S column summation circuits numerically add the magnitudes of the signals from preamplifiers for each row and for each column to generate histograms. For a P.times.Q array of photomultiplier tubes, P.times.Q summation circuitries generate P.times.Q row histograms including R entries and P.times.Q column histograms including S entries. The total set of histograms include P.times.Q.times.(R+S) entries, which can be analyzed by a position calculation circuit to determine the locations of events (detection of a neutron).

  3. Enrichment of tritium by thermal diffusion column

    International Nuclear Information System (INIS)

    Tritium present in H2 or D2, 1.7 x 10-2 Ci/mol, was enriched using a hot-wire type vertical glass thermal-diffusion column with a gas reservoir on top. Four columns with different diameters (mmphi), 8, 20, 30 and 41, were tested, while the temperature of a DC heated nichrome wire along the axis of each column was changed over a range from 200 to 4500C. The maximum equilibrium separation factors in hydrogen and in deuterium were 17 and 4.5 respectively. The optimum diameters were calculated by a modification of Waldmann's equation which can be used for the separation using parallel plates. (author)

  4. Inert carriers for column extraction chromatography

    International Nuclear Information System (INIS)

    Inert carriers used in column extraction chromatography are reviewed. Such carriers are devided into two large groups: hydrophilic carriers which possess high surface energy and are well wetted only with strongly polar liquids (kieselguhrs, silica gels, glasses, cellulose, Al2O3) and water-repellent carriers which possess low surface energy and are well wetted with various organic solvents (polyethylene, polytetrafluorethylene polytrifluorochlorethylene). Properties of various carriers are presented: structure, chemical and radiation stability, adsorption properties, extracting agent capacity. The effect of structure and sizes of particles on the efficiency of chromatography columns is considered. Ways of immovable phase deposition on the carrier and the latter's regeneration. Peculiarities of column packing for preparative and continuous chromatography are discussed

  5. Sorption, degradation, and leaching of tebuthiuron and diuron in soil columns.

    Science.gov (United States)

    Matallo, Marcus B; Spadotto, Claudio A; Luchini, Luiz C; Gomes, Marco A F

    2005-01-01

    A study in small outdoor lysimeters was carried out to determine the leaching of the herbicides tebuthiuron and diuron in different soil types, using undisturbed soil columns. Soil sorption and degradation for both herbicides were also studied in the laboratory. The multi-layered AF (Attenuation Factor) model was evaluated for predicting the herbicides leaching in undisturbed soil columns. Tebuthiuron leached in greater amounts than diuron in both soils. Sorption was well represented by linear and Freundlich equations, however parameters from the linear equations were used in the AF model. In general, both herbicides presented very low sorption, with diuron presenting lower values of sorption coefficient than tebuthiuron in the two soils. Chromatographic data indicated rapid late degradation of diuron and tebuthiuron in both soil types at two different depths. Simple exponential equation was not able to represent degradation, thus a bi-exponential equation was used, and some model adjusting was needed. Average measured amounts of each herbicide were compared with amounts predicted by the multi-layered-soil AF model. The AF model was able to predict leaching amounts in the sandy soil, especially for diuron, however it did not perform well in the clayey soil. PMID:15656160

  6. Simulation of the dynamic packing behavior of preparative chromatography columns via discrete particle modeling.

    Science.gov (United States)

    Dorn, Martin; Hekmat, Dariusch

    2016-03-01

    Preparative packed-bed chromatography using polymer-based, compressible, porous resins is a powerful method for purification of macromolecular bioproducts. During operation, a complex, hysteretic, thus, history-dependent packed bed behavior is often observed but theoretical understanding of the causes is limited. Therefore, a rigorous modeling approach of the chromatography column on the particle scale has been made which takes into account interparticle micromechanics and fluid-particle interactions for the first time. A three-dimensional deterministic model was created by applying Computational Fluid Dynamics (CFD) coupled with the Discrete Element Method (DEM). The column packing behavior during either flow or mechanical compression was investigated in-silico and in laboratory experiments. A pronounced axial compression-relaxation profile was identified that differed for both compression strategies. Void spaces were clearly visible in the packed bed after compression. It was assumed that the observed bed inhomogeneity was because of a force-chain network at the particle scale. The simulation satisfactorily reproduced the measured behavior regarding packing compression as well as pressure-flow dependency. Furthermore, the particle Young's modulus and particle-wall friction as well as interparticle friction were identified as crucial parameters affecting packing dynamics. It was concluded that compaction of the chromatographic bed is rather because of particle rearrangement than particle deformation. © 2015 American Institute of Chemical Engineers Biotechnol. Prog., 32:363-371, 2016. PMID:26588806

  7. Barium-137 M milkers based on 12-molybdo cerate column matrix. Vol. 3

    International Nuclear Information System (INIS)

    The interaction of 134 Cs+ and 131,133 Ba2+ radiotracers (10-4 M for each) in HCl, H N O3, Na Cl, Na N O3, and N H4 Cl solutions on 12-Molybdo cerate (IV) has been studied by batch equilibrium at room temperature. The corresponding distribution coefficients (Kd values in mi/g) were determined as a function of the composition of the reaction medium and drying temperature; 50, 150 and 200 degree C of the molybdate matrix under comparable conditions, Cs+ ions are strongly retained on the adsorbent material than Ba2+ ions. Elution performance of the daughter 134m Ba (T1/2=2.7 min.) from its parent 137 Cs (T1/2=30 y) was investigated on small chromatographic columns of the matrix. Based on the data obtained, 2 g 12-molybdo cerate (IV), dried at 200 degree C, loaded with 1 mCi 137 Cs/137m Ba milkers was prepared. The generated 137m Ba daughter was continuously eluted by passing a mixture solution of 0.1 M HCl + 0.1 M N H4 Cl as eluent through the column bed at flow rates of 1 and 2 m1/min. Eluate assessment proved reproducibility of the elution yields about 58% 137m Ba in 5 m1 eluate. Radionuclidic and chemical purity of the eluate proved to be suitable for use in nuclear medicine and also industrial applications. 6 figs., 1 tab

  8. Determination of asphaltenes in heavy oils using an on-column method

    Energy Technology Data Exchange (ETDEWEB)

    Rogel, E.; Ovalles, C.; Moir, M. [Chevron Energy Technology Co., Richmond, CA (United States); Schabron, J.F. [Western Research Inst., Laramie, WY (United States)

    2009-07-01

    An improved analytical method for determining the asphaltene content in crude oil and petroleum samples was presented. The method used an on-column precipitation technique coupled with an evaporative light scattering detector (ELSD). The column has an inert packing material where the asphaltene was precipitated and re-dissolved using a solvent. Heavy crude oils with asphaltene contents ranging from 5 to 25 per cent w/w were tested. A blend of 90:10 dichloromethane and methanol was used to decrease the influence of hydrocarbon adsorption mechanisms from the polymeric liquid chromatographic phases. A series of laboratory experiments were conducted to compare results obtained using the method with results obtained using traditional gravimetric methods. Regression analysis was used to determine the calibration constants. The study showed that the method can be used as replacement for conventional gravimetric methods when faster results are needed or when sample sizes are small. It was concluded that the method was able to accurately quantify asphaltene contents as low as 120 ppm. 8 refs., 1 tab., 3 figs.

  9. Study of plutonium sorption in aluminia column in the system HNO3-HF

    International Nuclear Information System (INIS)

    The column chromatographic method using alumina has been applied successfully to study the sorption-desorption behavior of plutonium traces in HNO3-HF and HNO3-HF-UO2(NO3)2 systems, aiming to elaborate a process for recovering plutonium traces from reprocessing wastes, mainly in existing solutions where uranium is presented in macro quantities. Basically, the method consists in the sorption of plutonium by percolating a solution containing HNO3(0,1 to 0,8M) or uranyl nitrate (1-50 gU/l) and HF(0,1 to 0,3M) through an Al2O3 collumn. The plutonium is fixed on Al2O3 whereas the uranyl ions is collected in the efluent. The adsorption of Pu-III, Pu-IV and Pu-VI in the presence of HF was determined and Pu-IV can be almost completely sorbed. The Pu-IV is eluted by reduction to Pu-III in the column using 3 M HNO3-0,005M FeSO4 at 500C as elutrient. This method is very simple and can be applied for separation and purification of plutonium (traces) from uranyl nitrate or others coming solutions from wet chemistry of irradiated fuels

  10. Elution of Uranium and Calculation of Plate Number on the Column of Silica-TBP

    International Nuclear Information System (INIS)

    Separation process of 99Mo resulted of irradiated uranyl nitrate with an accelerator as the neutron source by the chromatographic extraction using column containing kiesel gel-TBP will be developed. Kiesel gel (silica) was used as an inert subpart, TBP as a phase stationary and simulated used natural uranyl nitrate of 200-300 g/l with the acidity of 2 N as the mobile phase. The inert support was made by means of kiesel-gel (silica) hydrophobization to change hydrophilic silica to hydrophobic silica, so that it could be impregnated by TBP. Uranium which has been attached to TBP would be eluted by dilute acid at acidity of 0.05; 0.1; 0.2 N HNO3; Warm DW and cool DW. By using 0.1 N HNO3 eluent and warm DW the uranium attached to silica-TBP could be eluted perfectly and more quickly than the three others eluent. Uranium concentration which were absorbed and eluted were analysed titrimetrically by using titan method and it was used to calculate Plate Number (N). The value of N obtained for the column which the inert support of 8 cm in height, 1 cm in diameter, 10 drops per minute by using of 0.1 N HNO3 eluent was 300.6. (author)

  11. Accelerating selected columns of the density matrix computations via approximate column selection

    CERN Document Server

    Damle, Anil; Ying, Lexing

    2016-01-01

    Localized representation of the Kohn-Sham subspace plays an important role in quantum chemistry and materials science. The recently developed selected columns of the density matrix (SCDM) method [J. Chem. Theory Comput. 11, 1463, 2015] is a simple and robust procedure for finding a localized representation of a set of Kohn-Sham orbitals from an insulating system. The SCDM method allows the direct construction of a well conditioned (or even orthonormal) and localized basis for the Kohn-Sham subspace. The SCDM procedure avoids the use of an optimization procedure and does not depend on any adjustable parameters. The most computationally expensive step of the SCDM method is a column pivoted QR factorization that identifies the important columns for constructing the localized basis set. In this paper, we develop a two stage approximate column selection strategy to find the important columns at much lower computational cost. We demonstrate the effectiveness of this process using a dissociation process of a BH$_{3}...

  12. Experimental catalytic isotopic exchange column control

    International Nuclear Information System (INIS)

    Full text: In this paper we present a method for monitoring and control of the experimental catalytic isotopic exchange column which is part of ETRF (experimental tritium removal facility) of the ICIT Rm. Valcea. The initial data acquisition system based on analogue instruments is now upgraded to a fully digital system. Therefore we chose to use Compact Field Point which is a programmable automation controller (PAC) and LabVIEW software. To operate the catalytic isotopic exchange column there are some control loops that need to be operated simultaneously, namely: the heavy water column feed temperature and flow rate; the hydrogen gas column feed temperature; the flow rate and pressure at the top of the column; the water vapor flow rate; the hydrogen gas temperature at the condenser output. The human machine interface (HMI) realized with LabVIEW software is very friendly. The use of the PAC graphics interface makes isotopic exchange process operation easier for operators and researchers. The HMI has the functions to provide visualization of process parameters, to enable interaction with the process and also to provide alarms and event notification to operators about any abnormal situation in the plant. To interact with the process, detailed displays which contain specific control functions to operate the column, can be used. Usually, the faceplate display shows the controlled process variable and the output of the control loop. Furthermore, the set point and the operating mode of the control loop can be changed. Additionally, detailed information is available related to the parameters of PID controller and the different alarms that can be authorized in this control loop with its corresponding values of activation. (authors)

  13. Thermal restraint and fire resistance of columns

    OpenAIRE

    Neves, I. Cabrita; Valente, J. C.; Rodrigues, J. P. Correia

    2002-01-01

    A proposal is made, based on the results of a series of tests and calculations, with the aim of being used as a simple method to correct the value of the critical temperature of steel columns free to elongate, in order to take into account the restraint effect of the structure to which they belong in a practical situation. To better illustrate the possible types of behaviour of heated steel columns with elastic restraint to the thermal elongation, and the reasons why the critical temperature ...

  14. Distillation columns inspection through gamma scanning

    International Nuclear Information System (INIS)

    The application of nuclear energy is very wide and it allows the saving of economic resources since the investigation of a certain process is carried out without stop the plant. The gamma scanning of oil crackingcolumns are practical examples, they allow to determine the hydraulic operation of the inspected columns. A source of Co-60 22mCi and a detector with a crystal of INa(TI) are used. This paper shows the results got from a profile carried out in a column distillation

  15. Dynamics of pulsed plate extraction columns

    International Nuclear Information System (INIS)

    Methods of correlating holdup measurements in pulsed plate columns are reviewed and the use of the droplet characteristic velocity concept is demonstrated using published holdup data determined in the absence of mass transfer. The measurements are well correlated with the phase flowrates and pulse velocity. This is capable of modelling holdup characteristics within the accuracy of currently available data. The form of the dependence of the characteristic velocity upon pulse velocity would appear to be governed by the physical properties of the system and possibly also by the material of construction of the sieve plates. If this is subsequently confirmed, the implications will be significant in terms of column design. (author)

  16. The Development of Gel Media and Columns for Large-Scale Chromatography of Proteins,a Historical Review

    Institute of Scientific and Technical Information of China (English)

    Jan-Christer; Janson

    2002-01-01

    Thr first dedicated protein chromatography media were introduced during the 1950s and 1960s.There was an early awareness of the possibility of using these for production applications within the biopharmaceutical industry.However,the crucial limitation was the fact that those media that were most compatible with proteins lent themselves less favourably to scaling-up.The problems were primarily physical.Thus the fibrous cellulose media showed bed cracking tendencies and the bead shaped polyacrylamide.dextran,and agarose gel media,then available, were too soft to stand the hydrodynamic forces acting in large columns,leading to bed compaction and increased pressure drop.At the time,the best solution to the latter problem,after a number of intermediary solutions were tried,was the introductionof the stacked column concept in which several short column segments were connected by small bore tubing,thus reducing the force acting on the particles in each bed com partment,However,the ultimate remedy,the introduction of chromatographic matrices that combine the desired features of adequate rigidity,macroporosity,biocompatibility,chemical stability(for CIP and SIP0and derivatizability,did not occur until the middle of the 1980s when adequately cross-linked agarose gel media such as Sepharose Fast Flow were made available.The paper also recognizes the many attempts made during the past 50 years to develop continous chromatography columns.Most of the designs are based on an annular bed or on an array of annularly arranged parallel columns continuously fed with samples in a cyclic manner.The introduction of media and columns for expanded bed adsorption followed a demand for rewer pruification steps and shorter process times.In recent years,columns have been ntroduced that allow packing and repacking without needing to open the column.The review provides an historical account of the developments that have led to the present state-of-the-art both regarding large diameter columns

  17. Behaviour of ferrocement columns under static and cyclic loading

    OpenAIRE

    Wang, Jianqi

    2014-01-01

    This thesis presents the results of an experimental, numerical and analytical study to develop a design method for ferrocement columns and reinforced concrete columns strengthened using ferrocement jackets. Two groups tests were conducted, comprising five static loading tests and three cyclic load tests. The static tests had one reinforced concrete column, two ferrocement columns and two strengthened reinforced concrete columns. The cyclic loading tests were conducted on one reinforced concre...

  18. COLUMN-STORE DATABASES: APPROACHES AND OPTIMIZATION TECHNIQUES

    Directory of Open Access Journals (Sweden)

    Tejaswini Apte

    2013-09-01

    Full Text Available Column-Stores database stores data column-by-column. The need for Column-Stores database arose for the efficient query processing in read-intensive relational databases. Also, for read-intensive relational databases,extensive research has performed for efficient data storage and query processing. This paper gives an overview of storage and performance optimization techniques used in Column-Stores.

  19. Column-Store Databases: Approaches and Optimization Techniques

    Directory of Open Access Journals (Sweden)

    Tejaswini Apte

    2013-09-01

    Full Text Available Column-Stores database stores data column-by-column.The need for Column-Stores database arose for the efficient query processing in read-intensive relational databases. Also, for read-intensive relational databases,extensive research has performed for efficient data storage and query processing. This paper gives an overview of storage and performance optimization techniques used in Column-Stores.

  20. Diatextual Analysis of the Advice Column.

    Science.gov (United States)

    Mininni, Giuseppe

    1991-01-01

    Examined rhetorical and argumentative aspects of the "communication contract" stipulated in asking for and providing psychological advice in a mass media setting such as an advice column were examined. Letters from two Italian and two British magazines were used for the study. (14 references) (LB)