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Ion exclusion chromatography of aromatic acids.  


The determination of aromatic acids by ion exclusion chromatography is challenging due to peak tailing and the long retention time of hydrophobic solutes. This review discusses the retention mechanisms and the factors affecting retention, eluents and detection methods used in ion exclusion chromatography of aromatic acids such as mono-, di-, tri- and tetra-carboxylic acids, amino acids, sulfonates and phenol. In addition, the different approaches used to improve the chromatographic separation of these compounds are also discussed. These approaches include introducing an internal gradient of the ionic strength, using vacancy ion exclusion chromatography, employing a hydrophilic cation exchange resin or adding a modifier such as heptanol to the dilute sulfuric acid mobile phase. The applications of these methods in the analysis of aromatic acids are provided with a table summarizing the stationary phases, the mobile phases and the detection methods. PMID:23420808

Mansour, Fotouh R; Kirkpatrick, Christine L; Danielson, Neil D



Exclusion Chromatography  

NSDL National Science Digital Library

This site contains a brief description of the separation mechanism in size exclusion chromatography. The picture helps visualize the separation, but the site features a simplified and idealized presentation useful for students new to the concept.

Kimball, John W.


Ion-Exclusion Chromatography for Analyzing Organics in Water  

NASA Technical Reports Server (NTRS)

A liquid-chromatography technique has been developed for use in the quantitative analysis of urea (and of other nonvolatile organic compounds typically found with urea) dissolved in water. The technique involves the use of a column that contains an ion-exclusion resin; heretofore, this column has been sold for use in analyzing monosaccharides and food softeners, but not for analyzing water supplies. The prior technique commonly used to analyze water for urea content has been one of high-performance liquid chromatography (HPLC), with reliance on hydrophobic interactions between analytes in a water sample and long-chain alkyl groups bonded to an HPLC column. The prior technique has proven inadequate because of a strong tendency toward co-elution of urea with other compounds. Co-elution often causes the urea and other compounds to be crowded into a narrow region of the chromatogram (see left part of figure), thereby giving rise to low chromatographic resolution and misidentification of compounds. It is possible to quantitate urea or another analyte via ultraviolet- and visible-light absorbance measurements, but in order to perform such measurements, it is necessary to dilute the sample, causing a significant loss of sensitivity. The ion-exclusion resin used in the improved technique is sulfonated polystyrene in the calcium form. Whereas the alkyl-chain column used in the prior technique separates compounds on the basis of polarity only, the ion-exclusion-resin column used in the improved technique separates compounds on the basis of both molecular size and electric charge. As a result, the degree of separation is increased: instead of being crowded together into a single chromatographic peak only about 1 to 2 minutes wide as in the prior technique, the chromatographic peaks of different compounds are now separated from each other and spread out over a range about 33 minutes wide (see right part of figure), and the urea peak can readily be distinguished from the other peaks. Although the analysis takes more time in the improved technique, this disadvantage is offset by two important advantages: Sensitivity is increased. The minimum concentration of urea that can be measured is reduced (to between 1/5 and 1/3 of that of the prior technique) because it is not necessary to dilute the sample. The separation of peaks facilitates the identification and quantitation of the various compounds. The resolution of the compounds other than urea makes it possible to identify those compounds by use of mass spectrometry.

Sauer, Richard; Rutz, Jeffrey A.; Schultz, John R.




EPA Science Inventory

The theory of ion chromatography as a technique for analyzing ionic substances is discussed. The application of ion chromatography for analyzing ambient air samples is specifically described, with emphasis on determining sulfate, nitrate, and ammonium ions in aerosols, and sulfur...


Separation of Aliphatic and Aromatic Carboxylic Acids by Conventional and Ultra High Performance Ion Exclusion Chromatography  

PubMed Central

An ion exclusion chromatography (IELC) comparison between a conventional ion exchange column and an ultra-high performance liquid chromatography (UHPLC) dynamically surfactant modified C18 column for the separation of an aliphatic carboxylic acid and two aromatic carboxylic acids is presented. Professional software is used to optimize the conventional IELC separation conditions for acetylsalicylic acid and the hydrolysis products: salicylic acid and acetic acid. Four different variables are simultaneously optimized including H2SO4 concentration, pH, flow rate, and sample injection volume. Thirty different runs are suggested by the software. The resolutions and the time of each run are calculated and feed back to the software to predict the optimum conditions. Derringer’s desirability functions are used to evaluate the test conditions and those with the highest desirability value are utilized to separate acetylsalicylic acid, salicylic acid, and acetic acid. These conditions include using a 0.35 mM H2SO4 (pH 3.93) eluent at a flow rate of 1 mL min-1 and an injection volume of 72 ?L. To decrease the run time and improve the performance, a UHPLC C18 column is used after dynamic modification with sodium dodecyl sulfate. Using pure water as a mobile phase, a shorter analysis time and better resolution are achieved. In addition, the elution order is different from the IELC method which indicates the contribution of the reversed-phase mode to the separation mechanism. PMID:24285874

Mansour, Fotouh R.; Kirkpatrick, Christine L.; Danielson, Neil D.



Ion chromatography  

Microsoft Academic Search

Ion chromatography makes it possible to separate and measure low concentrations of up to 8 or 10 different anions in a single chromatographic run that takes only a few minutes. The method also works well for cations. Alkali metal ions, ammonium, magnesium, calcium, strontium, and a growing list of other metal cations and amine cations can also be rapidly separated

James S. Fritz



A process for separating acid-sugar mixtures using ion exclusion chromatography  

SciTech Connect

Work using a low-temperature concentrated sulfuric acid hydrolysis process to convert the cellulosic fraction of corn stover to monomeric sugars demonstrated the high conversion efficiencies possible with that process. The TVA work also confirmed the need for a cost-effective acid-sugar separation process. A preparative-scale ion-exclusion chromatography (IEC) system was designed, constructed, and tested with a variety of synthetic solutions and actual hydrolyzates. Although significant dispersion was observed initially, design changes were effective in minimizing this phenomenon. Data collected during the operation of the preparative-scale system were used in the design and construction of an IEC miniplant capable of processing larger volumes of synthetic solutions or hydrolyzates and in the design of an extraction-assisted IEC system. The data were also used to assess the viability of a continuous feed IEC system. This paper includes a discussion of the IEC process, provides overall material balances for various IEC process scenarios, and presents a discussion on process economics.

Hester, R.D.; Hartfield, S.W. [University of Southern Mississippi, Hattiesburg, MS (United States); Farina, G.E. [Tennessee Valley Authority, Muscle Shoals, AL (United States)



Separation of acid and sugar by ion exclusion chromatography. An application in the conversion of cellulose to ethanol  

SciTech Connect

The production of fuel grade alcohol by fermentation from sugars obtained by the acid hydrolysis of cellulose has been hindered by costly methods of cleansing the acid in the sugar stream. An economical and environmentally acceptable acid-sugar separation process based on ion exclusion chromatography has been developed and analyzed. This process recovers the acid for reuse in hydrolysis without producing landfill waste allowing a concentrated acid hydrolysis process to be commercially feasible.

Hartfield, S.; Hester, R. [Univ. of Southern Mississippi, Hattiesburg, MS (United States)



Optimization of the determination of organic acids and sugars in fruit juices by ion-exclusion liquid chromatography  

Microsoft Academic Search

An HPLC method for the determination of the main organic acids and sugars in fruit juices is proposed. Nine acids (including oxalic, citric, malic, quinic, galacturonic, ascorbic, succinic, and fumaric acid) and three sugars (sucrose, glucose and fructose) were separated by ion-exclusion chromatography using a resin-based Aminex HPX 87H column after a sample clean-up with Sax cartridges. In spite of

Fabio Chinnici; Umberto Spinabelli; Claudio Riponi; Aureliano Amati



Determination of short chain carboxylic acids in vegetable oils and fats using ion exclusion chromatography electrospray ionization mass spectrometry.  


A new method for quantification of short chain C1-C6 carboxylic acids in vegetable oils and fats by employing Liquid Chromatography Mass Spectrometry (LC-MS) has been developed. The method requires minor sample preparation and applies non-conventional Electrospray Ionization (ESI) liquid phase chemistry. Samples are first dissolved in chloroform and then extracted using water that has been spiked with stable isotope labeled internal standards that are used for signal normalization and absolute quantification of selected acids. The analytes are separated using Ion Exclusion Chromatography (IEC) and detected with Electrospray Ionization Mass Spectrometry (ESI-MS) as deprotonated molecules. Prior to ionization the eluent that contains hydrochloric acid is modified post-column to ensure good ionization efficiency of the analytes. The averaged within run precision and between run precision were generally lower than 8%. The accuracy was between 85 and 115% for most of the analytes. The Lower Limit of Quantification (LLOQ) ranged from 0.006 to 7mg/kg. It is shown that this method offers good selectivity in cases where UV detection fails to produce reliable results. PMID:25627971

Viidanoja, Jyrki



Ion Exchange Chromatography  

NSDL National Science Digital Library

This website contains an ion chromatography simulator that can be run online or can be downloaded. The simulator focuses on separations of proteins using Ion Chromatography. Also included is linked reference information, an example of a homework assignment using the simulator, and some information on protein structures.


Qualitative analysis of some carboxylic acids by ion-exclusion chromatography with atmospheric pressure chemical ionization mass spectrometric detection  

Microsoft Academic Search

A simple, selective and sensitive method for the determination of carboxylic acids has been developed. A mixture of formic, acetic, propionic, valeric, isovaleric, isobutyric, and isocaproic acids has been separated on a polymethacrylate-based weak acidic cation-exchange resin (TSK gel OA pak-A) based on an ion-exclusion chromatographic mechanism with detection using UV-photodiode array, conductivity and atmospheric pressure chemical ionization mass spectrometry

Murad I. H. Helaleh; Kazuhiko Tanaka; Hiroshi Taoda; Wenzhi Hu; Kiyoshi Hasebe; Paul R. Haddad



Ion Chromatography: An Account of Its Conception and Early Development  

ERIC Educational Resources Information Center

The conception of ion chromatography and its development into a technique ready for commercialization is described. The pioneering development pointed the way to make ion exclusion an important member of the repertoire of IC methods.

Small, Hamish



Ion Pairing Chromatography  

Microsoft Academic Search

The present state of ion-pair chromatography (IPC) is reviewed. Emphasis is placed on the theoretical modeling of the retention behavior of charged, zwitterionic, and neutral solutes, since the theory provides the generally good understanding of the factors affecting the separation. Although stoichiometric models were credited with the first easy-to-understand demonstration of the retention mechanism of IPC, they were thermodynamic models,

Teresa Cecchi



A novel ion-exclusion chromatography-mass spectrometry method to measure concentrations and cycling rates of carbohydrates and amino sugars in freshwaters.  


The concentrations of free neutral carbohydrates and amino sugars were determined in freshwater samples of distinct matrix complexity, including meso-, eu- and dystrophic lakes and ponds, using high-performance ion-exclusion chromatography (HPIEC) coupled to mass spectrometry (MS). In contrast to other methods, our approach allowed the quantification of free neutral carbohydrates and amino sugars at low nM concentrations without derivatization, de-salting or pre-concentration. New sample preparation procedures were applied prior to injection employing syringe and hollow fiber filtration. Analytes were separated on a strong cation exchange resin under 100% aqueous conditions using 0.1% formic acid as a mobile phase. To minimize background noise in MS, analytes were detected in a multiple reaction monitoring scan mode with double ion filtering. Detection limits of carbohydrates and amino sugars ranged between 0.2 and 2nM at a signal-to-noise ratio >5. Error ranged between 1 and 12% at 0.5-500nM levels. Using a stable isotope dilution approach, both the utilization and recycling of glucose in Lake Zurich was observed. In contrast, N-acetyl-glucosamine was equally rapidly consumed but there was no visible de novo production. The simple and rapid sample preparation makes our protocol suitable for routine analyses of organic compounds in freshwater samples. Application of stable isotope tracers along with accurate measures of carbohydrate and amino sugar concentrations enables novel insights into the compound in situ dynamics. PMID:25242224

Hor?ák, Karel; Pernthaler, Jakob



Size exclusion chromatography of plasmid DNA isoforms  

Microsoft Academic Search

There is considerable interest in using size exclusion chromatography (SEC) to analyze and purify specific plasmid isoforms, but there is currently no fundamental understanding of the effects of plasmid size and morphology on plasmid behavior in SEC. Experiments were performed for plasmids from 3.0 to 17.0kbp in size. The linear and open-circular isoforms were generated from the supercoiled plasmid by

David R. Latulippe; Andrew L. Zydney



Size-exclusion chromatography of perfluorosulfonated ionomers  

Microsoft Academic Search

A size-exclusion chromatography (SEC) method in N,N-dimethylformamide containing 0.1M LiNO3 is shown to be suitable for the determination of molar mass distributions of three classes of perfluorosulfonated ionomers, including Nafion®. Autoclaving sample preparation is optimized to prepare molecular solutions free of aggregates, and a solvent exchange method concentrates the autoclaved samples to enable the use of molar-mass-sensitive detection. Calibration curves

T. H. Mourey; L. A. Slater; R. C. Galipo; R. J. Koestner



Application of a microwave-assisted extraction method for the extraction of organic acids from Greek cheeses and sheep milk yoghurt and subsequent analysis by ion-exclusion liquid chromatography  

Microsoft Academic Search

A method for the determination of 13 organic acids (OA) in Greek cheeses and sheep milk yoghurt was proposed and assessed. The method was based on microwave-assisted extraction (MAE) of OA by an aqueous solution (10mM) of sulphuric acid; extracts were subsequently analysed by ion-exclusion liquid chromatography associated with PhotoDiode Array detection (IE-LC–PDA). Chromatographic conditions (column temperature and mobile-phase composition)

E. N. Papadakis; A. Polychroniadou




EPA Science Inventory

A Dionex Model 10 Ion Chromatograph was evaluated for the measurement of anionic species in water. The theoretical effect of hydrogen ion activity (pH) on the elution time of phosphate and arsenate was tested and empirical selectivity coefficients were determined for the major pr...


Direct determination of Si isotope ratios in natural waters and commercial Si standards by ion exclusion chromatography multicollector inductively coupled plasma mass spectrometry.  


Silicon isotope ratios in natural waters and several commercial Si standards were determined by online ion exclusion chromatography (IEC) multicollector inductively couple plasma mass spectrometry (MC-ICPMS). As recent studies have shown that mass-independent fractionation (MIF) also exists in MC-ICPMS, e.g., Nd, Ce, W, Sr, Hf, Ge, Hg, and Pb isotopes, the nature of mass bias for Si isotopes was thus investigated. MIF was observed for Si isotopes on both Neptune and Neptune plus MC-ICPMS instruments in this study. Therefore, a standard-sample bracketing (SSB) mass bias correction model, capable of correcting both mass-dependent and mass-independent bias, was employed to obtain accurate Si isotope ratio results in all samples by using NBS28 Si standard as the bracketing standard. Medium resolution was used for all measurements in order to resolve polyatomic interferences on Si isotopes. NBS28 Si standard solutions prepared in nutrient-free seawater and 0.1% NaOH matrix, respectively, were used for the method validation and subjected to the online IEC MC-ICPMS determination of Si isotope ratios. Values of -0.01 ± 0.06 and 0.00 ± 0.06 ‰ (1 SD, n = 10) and -0.01 ± 0.03 and 0.01 ± 0.06 ‰ (1 SD, n = 10) for ?(29/28)Si and ?(30/28)Si, respectively, were obtained, confirming accurate results can be obtained using the reported method for natural waters. Significant variations in Si isotope ratios from -0.72 ± 0.09 to -0.24 ± 0.03 ‰ (1 SD, n = 10) and -1.36 ± 0.11 to -0.46 ± 0.04 ‰ (1 SD, n = 10) for ?(29/28)Si and ?(30/28)Si, respectively, were found among commercial Si standards of NIST SRM3150, SCP Si, and Sigma-Aldrich Si. Values of -0.06 ± 0.07 and -0.20 ± 0.11 ‰ (1 SD, n = 10) for ?(29/28)Si and ?(30/28)Si, respectively, were obtained for the MOOS-3 seawater whereas 0.59 ± 0.11 and 1.19 ± 0.15 ‰ (1SD, n = 10) for ?(29/28)Si and ?(30/28)Si, respectively, were obtained for the SLRS-5 river water. To the best of our knowledge this is the first report of an application of online IEC MC-ICPMS for the high accuracy and precision determination of Si isotope ratios in natural waters. The reported method provides for a relatively rapid (10 min per run) and simple online technique that requires no sample pretreatment for the Si isotope ratio measurements. PMID:25162683

Yang, Lu; Zhou, Lian; Hu, Zhaochu; Gao, Shan



Dichloropentafluoropropanes as solvents for size exclusion chromatography.  


We have found that HCFC225s (HCFC225ca: 3,3-dichloro-1,1,1,2,2-pentafluoropropane, HCFC225cb: 1,3-dichloro-1,1,2,2,3-pentafluoropropane) are superior mobile phases for size exclusion chromatography (SEC). As alternatives of CFC113, they have been shown to possess a number of excellent properties, such as low flammability, low viscosity, low cost, high purity, and environmental and operational friendliness. In addition, they have distinct advantages for the SEC measurement, because they solubilize some kinds of acrylate such as poly(methyl methacrylate) (PMMA) and commercial monodispersed PMMA can be used to prepare calibration curves necessary for the measurement of equivalent molecular weight of some polymers. Furthermore, we propose an HCFC225/1,1,1,3,3,3-hexafluoroisopropanol mixed solvent for use in the SEC of poly(ethylene terephthalate) (PET) and polyamides. Poly(2-(perfluorooctyl)ethyl acrylate), whose PMMA equivalent weight average molecular weight was 118,100 Da, was evaluated by a multi-angle laser light scattering (MALLS) detector to have an absolute molecular weight of 439,000 Da. The difference can be attributed to the molecular size of the polyfluorinated polymer compared to the non-fluorinated one. The possible application of this novel mobile phase system for molecular size and molecular weight characterization of perfluoropolyethers, PET, nylon 6 and nylon 6,6 are also discussed. PMID:14763738

Isemura, Tsuguhide; Kakita, Reiko; Kawahara, Kengo



Ion Exchange and Liquid Column Chromatography.  

ERIC Educational Resources Information Center

Emphasizes recent advances in principles and methodology in ion exchange and chromatography. Two tables list representative examples for inorganic ions and organic compounds. Cites 544 references. (CS)

Walton, Harold F.



Analysis of energetic materials by ion chromatography  

Microsoft Academic Search

Ion chromatography is a rapid, sensitive, and selective method for ion analysis in a variety of matrices. Ion chromatography was used to determine levels on chloride and chlorate in potassium perchlorate. Comparisons were made with the specific ion electrons method presently being used for these analyses. Also to be discussed are ion chromatographic methods for determining ammonium in boron potassium




Longitudinal diffusion in size-exclusion chromatography: a stop-flow size-exclusion chromatography study.  


Band broadening in size-exclusion chromatography (SEC) has an adverse effect upon calculated molecular mass averages, distributions, and dilute solution data generated using single- and multi-detector systems. In the past, the longitudinal diffusion contribution to band broadening in SEC has been considered negligible. This assumption has been investigated by using a stop-flow methodology (SF-SEC) that maximizes the potential for longitudinal diffusion while minimizing that for mass transfer. Under the given experimental conditions, the effects of B-term band broadening were manifest only below 30 KDa, irrespective of chemical functionality or molecular mass polydispersity. This type of broadening was found to be flow rate-independent for a representative high molecular mass polymer. PMID:11695865

Striegel, A M



Analysis of energetic materials by ion chromatography  

SciTech Connect

Ion chromatography is a rapid, sensitive, and selective method for ion analysis in a variety of matrices. Ion chromatography was used to determine levels on chloride and chlorate in potassium perchlorate. Comparisons were made with the specific ion electrons method presently being used for these analyses. Also to be discussed are ion chromatographic methods for determining ammonium in boron potassium nitrate, and chloride and ammonium in CP.

Hershey, M.K.



Using Ion Exchange Chromatography to Separate Proteins  

NSDL National Science Digital Library

This activity website, hosted by the National Health Museum Activities Exchange, explores protein purification using ion chromatography. Students will separate a positively charged lysozyme from a negatively charged albumin at a neutral pH using ion exchange chromatography. The site includes information for the teacher, instructions and follow-up questions for students, and a list of supplies.

Ellyn A. Daugherty


Using Ion Exchange Chromatography to Separate and Quantify Complex Ions  

ERIC Educational Resources Information Center

Ion exchange chromatography is an important technique in the separation of charged species, particularly in biological, inorganic, and environmental samples. In this experiment, students are supplied with a mixture of two substitution-inert complex ions. They separate the complexes by ion exchange chromatography using a "flash"…

Johnson, Brian J.



Static and dynamic polystyrene dimensions in relation to the blob model and size-exclusion chromatography  

E-print Network

-exclusion chromatography Z. Gallot, G. Pouyet and A. Schmitt Centre de Recherches sur les Macromolécules, 6, rue, chromatographie d'exclusion stérique) pour une série de polystyrènes linéaires en solution dans un bon solvant-over spatial). En chromatographie d'exclusion stérique, nous montrons qu'il est possible d'établir plusieurs

Paris-Sud XI, Université de



NSDL National Science Digital Library

The North Carolina Community College System BioNetwork's interactive eLearning tools (IETs) are reusable chunks of training that can be deployed in a variety of courses or training programs. IETs are designed to enhance, not replace hands-on training. Learners are able to enter a hands-on lab experience better prepared and more confident. This particular IET delves into chromatography including the basics, the three types (affinity, ion exchange, size exclusion), and the parts and functions associated with chromatography.


Measurements of Protein-Protein Interactions by Size Exclusion Chromatography  

E-print Network

A method is presented for determining second virial coefficients B_2 of protein solutions from retention time measurements in size exclusion chromatography (SEC). We determine B_2 by analyzing the concentration dependance of the chromatographic partition coefficient. We show the ability of this method to track the evolution of B_2 from positive to negative values in lysozyme and bovine serum albumin solutions. Our SEC results agree quantitatively with data obtained by light scattering.

J. Bloustine; V. Berejnov; S. Fraden



Determining persistence length by size-exclusion chromatography  

Microsoft Academic Search

Several methods for determining persistence length from size-exclusion chromatography data are evaluated for a stiff polymer, poly(n-hexyl isocyanate) (PHIC), and the more flexible poly[2,7-(9,9 di-n-hexylfluorene)]. The molar mass dependence of the root-mean-square radius obtained from light scattering detection is used to calculate the persistence length of PHIC, based on the Kratky–Porod wormlike chain model. The persistence length estimate is in

Thomas Mourey; Kim Le; Trevor Bryan; Shiying Zheng; Grace Bennett




EPA Science Inventory

An analytical method was developed for the determination of lactic acid, formic acid, acetic acid, propionic acid, and butyric acid in environmental microcosm samples using ion-exclusion chromatography. The chromatographic behavior of various eluents was studied to determine the ...


Size-exclusion chromatography system for macromolecular interaction analysis  


A low pressure, microcomputer controlled system employing high performance liquid chromatography (HPLC) allows for precise analysis of the interaction of two reversibly associating macromolecules such as proteins. Since a macromolecular complex migrates faster than its components during size-exclusion chromatography, the difference between the elution profile of a mixture of two macromolecules and the summation of the elution profiles of the two components provides a quantifiable indication of the degree of molecular interaction. This delta profile is used to qualitatively reveal the presence or absence of significant interaction or to rank the relative degree of interaction in comparing samples and, in combination with a computer simulation, is further used to quantify the magnitude of the interaction in an arrangement wherein a microcomputer is coupled to analytical instrumentation in a novel manner.

Stevens, Fred J. (Downers Grove, IL)



Determination of glyphosate by ion chromatography  

Microsoft Academic Search

An ion chromatography system for the determination of glyphosate was described. Ion chromatograph was carried out by suppressed conductivity detection (DX-100). The eluent contained 9 mmol l?1 Na2CO3 and 4 mmol l?1 NaOH. The detection limit was 0.042 ?g ml?1 (S\\/N=3). The relative standard deviation was 1.99% and the correlation coefficient of the calibration curve for area was 0.9995. The

Yan Zhu; Feifang Zhang; Changlun Tong; Weiping Liu



Analyzing insulin samples by size-exclusion chromatography: a column degradation study.  


Investigating insulin analogs and probing their intrinsic stability at physiological temperature, we observed significant degradation in the size-exclusion chromatography (SEC) signal over a moderate number of insulin sample injections, which generated concerns about the quality of the separations. Therefore, our research goal was to identify the cause(s) for the observed signal degradation and attempt to mitigate the degradation in order to extend SEC column lifespan. In these studies, we used multiangle light scattering, nuclear magnetic resonance, and gas chromatography-mass spectrometry methods to evaluate column degradation. The results from these studies illustrate: (1) that zinc ions introduced by the insulin product produced the observed column performance issues; and (2) that including ethylenediaminetetraacetic acid, a zinc chelator, in the mobile phase helped to maintain column performance. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 104:1555-1560, 2015. PMID:25581527

Teska, Brandon M; Kumar, Amit; Carpenter, John F; Wempe, Michael F



Recycling Size Exclusion Chromatography for the Analysis and Separation of Nanocrystalline Gold  

E-print Network

Recycling Size Exclusion Chromatography for the Analysis and Separation of Nanocrystalline Gold Ali University, MS-60 6100 Main Street, Houston, Texas 77025 Recycling size exclusion chromatography (RSEC here the application of this method to gold nanocrystals stabilized by thiols. Alternate recycling

Richards-Kortum, Rebecca


The determination of some anions using ion chromatography and ion chromatography-graphite furnace atomic absorption spectrometry  

E-print Network


Hillman, Daniel C



Determination of molecular weight of heparin by size exclusion chromatography with universal calibration  

E-print Network

Determination of molecular weight of heparin by size exclusion chromatography with universal chromatography using ``universal cali- bration.'' A universal calibration curve was constructed for Superose 12 chromatography (SEC).1 * Corresponding author. Fax: 1-317-274-6879. E-mail address: (P

Dubin, Paul D.


Improving size-exclusion chromatography separation for glycogen.  


Glycogen is a hyperbranched glucose polymer comprised of glycogen ? particles, which can also form much larger composite ? particles. The recent discovery using size-exclusion chromatography (SEC) that fewer, smaller, ? particles are found in diabetic-mouse liver compared to healthy mice highlights the need to achieve greater accuracy in the size separation methods used to analyze ? and ? particles. While past studies have used dimethyl sulfoxide as the SEC eluent to analyze the molecular size and structure of native glycogen, an aqueous eluent has not been rigorously tested and compared with dimethyl sulfoxide. The conditions for SEC of pig-liver glycogen, phytoglycogen and oyster glycogen were optimized by comparing two different eluents, aqueous 50 mM NH?NO?/0.02% NaN? and dimethyl sulfoxide/0.5% LiBr, run through different column materials and pore sizes at various flow rates. The aqueous system gave distinct size separation of ?- and ?-particle peaks, allowing for a more detailed and quantitative analysis and comparison between liver glycogen samples. This greater resolution has also revealed key differences between the structure of liver glycogen and phytoglycogen. PMID:24508396

Sullivan, Mitchell A; Powell, Prudence O; Witt, Torsten; Vilaplana, Francisco; Roura, Eugeni; Gilbert, Robert G





... high pressure liquid, or ion exchange chromatography. In general, chromatography takes advantage of the differences in the chemicals you want to separate, such as their size, electric charge, or ability to stick to (bind) to ...


Size exclusion chromatography/mass spectrometry applied to the analysis of polysaccharides.  


A novel method for analysing polysaccharide materials is described which employs size-exclusion chromatography (SEC) followed by detection by on-line electrospray ionisation mass spectrometry (ESI-MS) and off-line matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOFMS). It is demonstrated through SEC/ESI ion trap mass spectrometry that the formation of multiply charged oligomer ions, which bind up to five sodium cations, allows the rapid analysis of polysaccharide ions with molecular weights in excess of 9 kDa. MALDI spectra generated from fractionation of the effluent collected from the same SEC separation are shown to be in good agreement with the ESI spectra with respect to molecular weight distributions and types of ions generated. ESI and MALDI mass spectra of samples obtained from sequential graded ethanol precipitation and SEC fractionation of acid and enzymatically digested arabinoxylan polysaccharides show important structural differences between polysaccharide fragments. In addition, a comparison is made between the mass spectra of native and permethylated SEC-separated fragments of acid and enzymatically treated arabinogalactan. Linkage information of the permethylated arabinogalactan oligomers can be rapidly established through the use of on-line SEC/ESI-MS( n) experiments. PMID:11746893

Deery, M J; Stimson, E; Chappell, C G



Ion Chromatography Analysis of Dibutyl Phosphoric Acid  

SciTech Connect

Analysis of dibutyl phosphate (DBP), a degradation product of tributyl phosphate (TBP), has long been a problem analysis by Ion Chromatography at the Savannah River Site. Due to the presence of UO{sub 2}{sup +2} and high NO{sub 3}{sup {minus}1} concentrations, inadequate recovery and separation of DBP on the chromatographic column had rendered the analysis undependable and very inconsistent, thus causing high uncertainties in the data. The method presented here by the Savannah River Technology Center (SRTC)/Analytical Development Section (ADS) addresses the sample preparation problems encountered when analyzing for DBP in the presence of uranium and nitrate. The data presented reflects the improvements made to decrease data uncertainty and increase data accuracy and precision.

Ray, R.J.



Determination of UV stabilizers in pet bottles by high performance?size exclusion chromatography  

Microsoft Academic Search

A Size Exclusion Chromatography?High Performance Liquid Chromatography (SEC?HPLC) method to determine antioxidants and UV stabilizers in PET bottles has been developed. In only a single run a synthetic mixture of the stabilizers was separated and quantified. The detection limit obtained for BHT, Tinuvin 326, Cyasorb UV 5411, and Tinuvin P was about 0.1 ?g\\/g and for Irgafos 168 it was

M. Monteiro; C. Nerín; F. G. R. Reyes



Human Plasma Proteome Analysis by Multidimensional Chromatography Prefractionation and Linear Ion Trap Mass  

E-print Network

Human Plasma Proteome Analysis by Multidimensional Chromatography Prefractionation and Linear Ion chromatography has attracted extensive attention, but most published works have focused on the fractionation strong cation exchange chromatography and reversed-phase chromatography. The resulting 30 samples were

Tian, Weidong


Degradation of Ultra-High Molar Mass Polymers in Size-Exclusion Chromatography  

Technology Transfer Automated Retrieval System (TEKTRAN)

The degradation of high molar mass polymers during size-exclusion chromatography (SEC) analysis has been a topic of interest for several decades. Should a polymer degrade during analysis, the accuracy of the molar mass (M) and architectural information obtained will be compromised. To this effect,...


Molecular structure characterization of linear and branched polystyrene blends by size exclusion chromatography coupled with viscometry  

Microsoft Academic Search

Owing to their low polydispersity and their well controlled molecular architecture, 3-arms stars polystyrenes made by anionic synthesis are suitable models to study the solution properties of long chain branched polymers. A fine characterization of such polymers by size exclusion chromatography–viscometry has shown that they often contain unwanted linear chains, leading to chromatograms presenting overlapping peaks. A mathematical procedure has

A. Kaivez; X. A. Gallez; D. Daoust; J. Devaux; P. Godard



Persistence length of carboxymethyl cellulose as evaluated from size exclusion chromatography and potentiometric titrations  

Microsoft Academic Search

The intrinsic persistence length of carboxymethyl cellulose (CMC) is determined by size exclusion chromatography in combination with multiangle laser light scattering (SEC-MALLS) as well as from potentiometric titrations. Samples with degree of substitution (ds) ranging from 0.75 to 1.25 were investigated. The relation between molar mass M and radius of gyration Rg as obtained by SEC-MALLS is determined in 0.02,

C. W. Hoogendam; A. de Keizer; M. A. Cohen Stuart; B. H. Bijsterbosch; J. A. M. Smit; Dijk van J. A. P. P; Horst van der P. M; J. G. Batelaan



Characterization of poly(diethoxyphosphazene) by size exclusion chromatography and viscometry  

Microsoft Academic Search

Two samples of poly(diethoxyphosphazene) (PDEP) having very different molecular weights have been studied by viscometry and size exclusion chromatography in THF solution. The results obtained, together with light scattering data of these samples, allow the calculation of the Mark-Houwink constants a=0.65 and K=2.5 10-4 in THF at 25°C. The method of calculation employed takes into account the great polydispersity of

Maria P. Tarazona; Julio Bravo; Maria M. Rodrigo; Enrique Saiz



Polystyrene-equivalent molecular weight versus true molecular weight in size-exclusion chromatography  

Microsoft Academic Search

The evaluation of the size-exclusion chromatography (SEC) concentration elution curves by means of a calibration dependence obtained in a given SEC set for a polymer different from the polymer to be analyzed results in an error in the determination of both molecular weight and molecular-weight distribution (MWD). The problem is analyzed assuming the validity of the universal-calibration concept. The differences

Miloš Netopil??k; Pavel Kratochv??l



Practical experience with on-line ion chromatography  

SciTech Connect

Bettis is heavily involved in on-line ion chromatography and has gained much experience with the systems. This paper serves to pass that experience along to any users, current or prospective, that are interested in the systems. On-line IC is extremely dynamic and the developments over the past few years have helped to produce systems that can provide technical and productivity improvements. The potential uses of the systems are only beginning to be tapped. It is the information provided herein maybe useful to any interested in on-line ion chromatography.

Lynch, G.J.



Automated Precursor Ion Exclusion During LC-MS/MS Data Acquisition for Optimal Ion Identification  

NASA Astrophysics Data System (ADS)

Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is widely used for characterizing multiple samples of complex mixtures with similar compositions. This article addresses a data acquisition strategy for collecting a maximal number of unique, high-quality MS/MS during LC-MS/MS analysis of multiple samples. Based on the concept that a component only needs to be identified once when analyzing multiple samples with similar compositions, an automated intersample data-dependent acquisition strategy was developed. The strategy is based on precursor ion exclusion (PIE) and is implemented in MassAnalyzer in an automated fashion for Thermo Scientific (San Jose, CA, USA) mass spectrometers. In this method, MassAnalyzer submits one sample at a time to the sample queue. After data acquisition of each sample, MassAnalyzer automatically analyzes the data to generate a PIE list based on the MS/MS precursor ions, merges this list with the list generated from previous runs, adds the list to the MS method file, and submits the next sample to the queue. The PIE list contains both m/z value and time window for each precursor ion, and is generated intelligently so that if an MS/MS is insufficient for identifying the peak of interest, it will be collected again near the top of the peak in the next run. Therefore, the strategy maximizes both quality and the number of unique MS/MS. When automated PIE was used to acquire LC-MS/MS data of an antibody tryptic digest and a soy hydrolysate sample, the number of identified ions increased by 52 % and 93 %, respectively, compared with data acquired without using PIE.

Zhang, Zhongqi



Synthesis of novel size exclusion chromatography support by surface initiated aqueous atom transfer radical polymerization.  


We report the use of aqueous surface-initiated atom transfer radical polymerization (SI-ATRP) to grow polymer brushes from a "gigaporous" polymeric chromatography support for use as a novel size exclusion chromatography medium. Poly(N,N-dimethylacrylamide) (PDMA) was grown from hydrolyzable surface initiators via SI-ATRP catalyzed by 1,1,4,7,10,10-hexamethyltriethylenetetramine (HMTETA)/CuCl. Grafted polymer was characterized semiquantitatively by ATR-FTIR and also cleaved and quantitatively characterized for mass, molecular weight, and polydispersity via analytical SEC/MALLS. The synthesis provides control over graft density and allows the creation of dense brushes. Incorporation of negative surface charge was found to be crucial for improving the initiation efficiency. As polymer molecular weight and density could be controlled through reaction conditions, the resulting low-polydispersity grafted polymer brush medium is shown to be suitable for use as a customizable size exclusion chromatography medium for investigating the principals of entropic interaction chromatography. All packed media investigated showed size-dependent partitioning of solutes, even for low graft density systems. Increasing the molecular weight of the grafts allowed solutes more access to the volume fraction in the column available for partitioning. Compared to low graft density media, increased graft density caused eluted solute probes to be retained less within the column and allowed for greater size discrimination of probes whose molecular weights were less than 10(4) kDa. PMID:17924673

Coad, Bryan R; Kizhakkedathu, Jayachandran N; Haynes, Charles A; Brooks, Donald E



Grafting zwitterionic polymer onto cryogel surface enhances protein retention in steric exclusion chromatography on cryogel monolith.  


Cryogel monoliths with interconnected macropores (10-100?m) and hydrophilic surfaces can be employed as chromatography media for protein retention in steric exclusion chromatography (SXC). SXC is based on the principle that the exclusion of polyethylene glycol (PEG) on both a hydrophilic chromatography surface and a protein favors their association, leading to the protein retention on the chromatography surface. Elution of the retained protein can be achieved by reducing PEG concentration. In this work, the surface of polyacrylamide-based cryogel monolith was modified by grafting zwitterionic poly(carboxybetaine methacrylate) (pCBMA), leading the increase in the surface hydrophilicity. Observation by scanning electron microscopy revealed the presence of the grafted pCBMA chain clusters on the cryogel surface, but pCBMA grafting did not result in the changes of the physical properties of the monolith column, and the columns maintained good recyclability in SXC. The effect of the surface grafting on the SXC behavior of ?-globulin was investigated in a wide flow rate range (0.6-12cm/min). It was found that the dynamic retention capacity increased 1.4-1.8 times by the zwitterionic polymer grafting in the flow rate range of 1.5-12cm/min. The mechanism of enhanced protein retention on the zwitterionic polymer-grafted surface was proposed. The research proved that zwitterionic polymer modification was promising for the development of new materials for SXC applications. PMID:25757821

Tao, Shi-Peng; Zheng, Jie; Sun, Yan



Mineral Separation in a CELSS by Ion-exchange Chromatography  

NASA Technical Reports Server (NTRS)

Operational parameters pertinent to ion exchange chromatography separation were identified. The experiments were performed with 9 mm diameter ion exchange columns and conventional column accessories. The cation separation beds were packed with AG 50W-X2 strong acid cation exchange resin in H(+) form and 200-400 dry mesh particle size. The stripper beds used in some experiments were packed with AG 1-XB strong base cation exchange resin in OH(-) form and 200-400 dry mesh particle size.

Ballou, E. V.; Spitze, L. A.; Wong, F. W.; Wydeven, T.; Johnson, C. C.



Using Ion Chromatography to Analyze Inorganic Disinfection By-products  

Microsoft Academic Search

Ion chromatography is used to analyze drinking water for inorganic disinfection by-products—the oxyhalides of chlorine and bromine—following disinfection. A previous study found chlorite ion (ClO??) to be unstable in drinking water. This investigation focused on stabilizing and preserving ClO?? by studying several agents known to quench its reaction with species present in drinking water. Based on the initial stability study,

Daniel P. Hautman; Michele Bolyard




EPA Science Inventory

The report describes the key elements required to develop a sampling and analysis program for a wet scrubber using ion chromatography as the main analytical technique. The first part of the report describes a sampling program for two different types of wet scrubbers: the venturi/...


Forensic Identification of Inorganic Explosives by Ion Chromatography  

Microsoft Academic Search

While there is a great deal of published literature describing methods for the analysis of organic explosives by various methods, there are comparatively few publications concerning the analysis of explosives based on inorganic chemicals. This mini?review examines the literature that is concerned with the analysis of such explosives, commonly referred to as improvised explosive devices, using ion chromatography. Pertinent details

Greg W. Dicinoski; Robert A. Shellie; Paul R. Haddad




EPA Science Inventory

A method using ion chromatography (IC) for the analysis of ferrous (Fe 2+) and ferric (Fe 3+) ions in soil extracts has been developed. This method uses an ion exchange column with detection at 520 nm after post-column derivatization. Selectivity is achieved by using an anionic...


Application of Ion Chromatography to the Investigation of Real-World Samples Rebecca J. Whelan,*1  

E-print Network

Application of Ion Chromatography to the Investigation of Real-World Samples Rebecca J. Whelan,*1 Experiment #4: Ion Chromatography Handout prepared by David Rakestraw, Rebecca Whelan, Theresa Hannon, and Cheol Keun Chung I. Summary of Laboratory In this laboratory we will use ion chromatography to analyze

Zare, Richard N.


Size-exclusion chromatography-from high-performance to ultra-performance.  


Size-exclusion chromatography (SEC) enables measurement of the average molecular weights and molecular-weight distributions of polymers. Because these characteristics may, in turn, be correlated with important performance characteristics of plastics, SEC is an essential analytical technique for characterization of macromolecules. Although SEC is one of the oldest instrumental chromatographic techniques, it is still under continuous development, as a result of the great demand for increased resolution and faster analysis in SEC. Ultra-high-pressure size-exclusion chromatography (UHPSEC) was recently introduced to satisfy the growing demands of analytical chemists. Using instrumentation capable of generating very high pressures and columns packed with small particles, this technique enables greater separation efficiency and faster analysis than are achieved with conventional SEC. UHPSEC is especially advantageous for high-resolution analysis of oligomers, for very rapid polymer separations, and as a second dimension in comprehensive two-dimensional liquid chromatography of polymers. In this paper we discuss the benefits of UHPSEC for separation of macromolecules, with examples from the literature. PMID:25116601

Uliyanchenko, Elena



Size-exclusion chromatography for the determination of the boiling point distribution of high-boiling petroleum fractions.  


The paper describes a new procedure for the determination of boiling point distribution of high-boiling petroleum fractions using size-exclusion chromatography with refractive index detection. Thus far, the determination of boiling range distribution by chromatography has been accomplished using simulated distillation with gas chromatography with flame ionization detection. This study revealed that in spite of substantial differences in the separation mechanism and the detection mode, the size-exclusion chromatography technique yields similar results for the determination of boiling point distribution compared with simulated distillation and novel empty column gas chromatography. The developed procedure using size-exclusion chromatography has a substantial applicability, especially for the determination of exact final boiling point values for high-boiling mixtures, for which a standard high-temperature simulated distillation would have to be used. In this case, the precision of final boiling point determination is low due to the high final temperatures of the gas chromatograph oven and an insufficient thermal stability of both the gas chromatography stationary phase and the sample. Additionally, the use of high-performance liquid chromatography detectors more sensitive than refractive index detection allows a lower detection limit for high-molar-mass aromatic compounds, and thus increases the sensitivity of final boiling point determination. PMID:25545251

Boczkaj, Grzegorz; Przyjazny, Andrzej; Kami?ski, Marian



Determination of UV stabilizers in PET bottles by high performance-size exclusion chromatography.  


A Size Exclusion Chromatography-High Performance Liquid Chromatography (SECHPLC) method to determine antioxidants and UV stabilizers in PET bottles has been developed. In only a single run a synthetic mixture of the stabilizers was separated and quantified. The detection limit obtained for BHT, Tinuvin 326, Cyasorb UV 5411, and Tinuvin P was about 0.1 microgram/g and for Irgafos 168 it was 1.0 microgram. RSD values were lower than 3%. Tinuvin P was identified and quantified in PET bottle extracts. Olive oil, soybean oil and sunflower oil showed well defined separation from Tinuvin P at the same conditions of analysis. Cyclic dimers were identified in the PET extracts. PMID:8799719

Monteiro, M; Nerín, C; Reyes, F G



Size-exclusion chromatography study of the molecular-weight distribution of gamma-irradiated pullulan.  


The polyelectrolyte behavior of gamma-irradiated pullulan in aqueous solutions leads to secondary effects of adsorption on a Shodex OHPak KB 806 column gel during size-exclusion chromatography. Suppression of the polyelectrolyte properties of gamma-irradiated pullulan is achieved by using a 0.05 M aqueous solution of NaH2PO4 (pH 4.95) as the mobile phase. Under these conditions, adequate molecular-weight distributions of gamma-irradiated pullulan samples are obtained. PMID:10744337

Shingel, K I; Tsarenkov, V M; Petrov, P T



Using size exclusion chromatography-RPLC and RPLC-CIEF as two-dimensional separation strategies for protein profiling  

SciTech Connect

Bottom-up proteomics (analyzing peptides that result from protein digestion) has demonstrated capability for broad proteome coverage and good throughput. However, due to incomplete sequence coverage, this approach is not ideally suited to the study of modified proteins. The modification complement of a protein can best be elucidated by analyzing the intact protein. Two-dimensional gel electrophoresis, typically coupled with the analysis of peptides that result from in-gel digestion, is the most frequently applied protein separation technique in MS-based proteomics. As an alternative, numerous column-based liquid phase techniques, which are generally more amenable to automation, are being investigated. In this work, the combination of size exclusion chromatography (SEC) fractionation with reversed-phase liquid chromatography (RPLC)-Fourier-transform ion cyclotron resonance (FTICR)-mass spectrometry (MS) is compared with the combination of RPLC fractionation with capillary isoelectric focusing (CIEF)-FTICR-MS for the analysis of the Shewanella oneidensis proteome. SEC-RPLC-FTICR-MS allowed the detection of 297 proteins, as opposed to 166 using RPLC-CIEF-FTICR-MS, indicating that approaches based on LC-MS provide better coverage. However, there were significant differences in the sets of proteins detected and both approaches provide a basis for accurately quantifying changes in protein and modified protein abundances.

Simson, David C.; Ahn, Seonghee; Pasa-Tolic, Liljiana; Bogdanov, Bogdan; Brewer, Heather M.; Vilkov, Andrey N.; Anderson, Gordon A.; Lipton, Mary S.; Smith, Richard D.



Determination of chloride in geological samples by ion chromatography  

USGS Publications Warehouse

Samples of silicate rocks are prepared by sodium carbonate fusion and then treated by ion chromatography. The method was tested for geological standards with chloride concentration between 0.003 and 3%. Observed chloride concentrations comparedd favorably with literature values. The relative standard deviation and detection limit for the method were 8% and 7 ppm, respectively. Up to 30 determination per 24-hour period were possible. ?? 1983.

Wilson, S.A.; Gent, C.A.



Determining Inorganic Disinfection By-products by Ion Chromatography  

Microsoft Academic Search

Disinfection by-products will soon be regulated by the US Environmental Protection Agency under the 1986 amendments to the Safe Drinking Water Act. Because of its sensitivity and precision, ion chromatography is a good choice for analyzing by-products of chlorine dioxide and ozone, i.e., chlorite, chlorate, and bromate, as well as several other anions. Los productos de desinfección pronto serán regulados

John D. Pfaff; Carol A. Brockhoff




NSDL National Science Digital Library

In this activity, by the Concord Consortium's Molecular Literacy project, students "learn about the phases of molecular separation, and then experiment with paper and ion chromatography." The activity itself is a java-based interactive resource built upon the free, open source Molecular Workbench software. In addition, visitors will find an overview of the activity, assessments, and concepts and their correlation to AAAS and NSES standards.


Determination of lignin by size exclusion chromatography using multi angle laser light scattering.  


A method was developed using high-performance size exclusion liquid chromatography (HPSEC) with multi-angle laser light scattering (MALLS), quasi-elastic light scattering (QELS), interferometric refractometry (RI) and UV detection to characterize and monitor lignin. The combination proved very effective at tracking changes in molecular conformation of lignin molecules over time; i.e. changes in molecular weight distribution, radius of gyration, and hydrodynamic radius. Until this study, UV detection (280 nm) had been the primary lignin determination method for chromatography. Three different HPLC columns were used to study the effects of pH, flow conditions, and mobile phase compositions (dimethyl sulphoxide, water, 0.1M NaOH, and lithium bromide) on the chromatography of lignin. Since light scattering accuracy is highly dependent on solute concentration, both the UV and RI detectors were calibrated for use as concentration detectors. Shodex Asahipak GS-320 HQ column with 0.1M NaOH (pH 12.0) run at 0.5 ml/min was found to give the highest separation and most consistent recovery. The study also revealed that the lignin aggregated at pH below 8.5. This aggregation was detected only by MALLS and was not observed on UV or RI detectors. It is very important to take this loss in apparent concentration due to aggregation into consideration before collecting reliable depolymerization data. PMID:16566937

Gidh, Aarti V; Decker, Stephen R; Vinzant, Todd B; Himmel, Michael E; Williford, Clint



Determination of selected anions in water by ion chromatography  

USGS Publications Warehouse

Ion chromatography is a rapid, sensitive, precise, and accurate method for the determination of major anions in rainwater and surface waters. Simultaneous analyses of a single sample for bromide, chloride, fluoride, nitrate, nitrite, orthophosphate, and sulfate require approximately 20 minutes to obtain a chromatogram. Minimum detection limits range from 0.01 mg/L for fluoride to 0.20 mg/L for chloride and sulfate. Relative standard deviations were less than 9% for all anions except nitrite in Standard Reference Water Samples. Only one reference sample contained nitrite and its concentration was near the minimum level of detection. Similar precision was found for chloride, nitrate, and sulfate at concentrations less than 5 mg/L in rainfall samples. Precision for fluoride ranged from 12 to 22%, but is attributed to the low concentrations in these samples. The other anions were not detected. To determine accuracy of results, several samples were spiked with known concentrations of fluoride, chloride, nitrate, and sulfate; recoveries ranged from 96 to 103%. Known amounts of bromide and phosphate were added, separately, to several other waters, which contained bromide or phosphate. Recovery of added bromide and phosphate ranged from approximately 95 to 104%. No recovery data were obtained for nitrite. Chloride, nitrate, nitrite, orthophosphate, and sulfate, in several samples, were also determined independently by automated colorimetric procedures. An automated ion-selective electrode method was used to determine fluoride. Results are in agreement with results obtained by ion chromatography. (USGS).

Fishman, Marvin J.; Pyen, Grace



Fluorescence-Detectino Size-Exclusion Chromatography for Precrystallization Screening of Integral Membrane Proteins  

SciTech Connect

Formation of well-ordered crystals of membrane proteins is a bottleneck for structure determination by X-ray crystallography. Nevertheless, one can increase the probability of successful crystallization by precrystallization screening, a process by which one analyzes the monodispersity and stability of the protein-detergent complex. Traditionally, this has required microgram to milligram quantities of purified protein and a concomitant investment of time and resources. Here, we describe a rapid and efficient precrystallization screening strategy in which the target protein is covalently fused to green fluorescent protein (GFP) and the resulting unpurified protein is analyzed by fluorescence-detection size-exclusion chromatography (FSEC). This strategy requires only nanogram quantities of unpurified protein and allows one to evaluate localization and expression level, the degree of monodispersity, and the approximate molecular mass. We show the application of this precrystallization screening to four membrane proteins derived from prokaryotic or eukaryotic organisms.

Kawate,T.; Gouaux, E.



Extraction and Separation of Polysaccharides from Laminaria japonica by Size-Exclusion Chromatography.  


A large number of studies have suggested that polysaccharides, such as fucoidan and laminarin, in various seaweeds have significant biological properties. A different distribution of molecular weights is a prominent sign of many polysaccharides. Therefore, a simple, fast and reliable high-performance size-exclusion chromatography (HPSEC) method was proposed to separate fucoidan and laminarin from Laminaria japonica. After evaluating the different separation conditions for HPSEC, such as the type of mobile phase and flow rate, an acid extraction method was established and optimized by a systematic investigation of the influencing factors. Under the optimal conditions, 169.2 and 383.8 mg g(-1) of fucoidan and laminarin, respectively, were extracted. This method is suitable for the extraction and separation of polysaccharides with good reproducibility of the retention time, acceptable linearity, small relative standard deviation and low detection limits. PMID:25013027

Zhang, Heng; Row, Kyung Ho



Improved potency assay for recombinant bovine somatotropin by high-performance size-exclusion chromatography.  


A high-performance size-exclusion chromatographic method was developed for the determination of potency of recombinant bovine somatotropin (rbST) monomer and the estimation of dimer and soluble aggregates in bulk drug substances. These proteins can be completely extracted from bulk drug substances with sodium borate-ethylenediamine-tetraacetic acid disodium salt (EDTA) at pH 9.5 and separated on TSK G3000SW column with a mobile phase of pH 7.3 sodium borate-EDTA. The results demonstrated that this method was a non-denaturing assay for the determination of potency of rbST monomer and the data obtained in this study correlated well with data of the hypophysectomized rat body weight gain bioassay. The rbST monomer and dimer in the separation were verified by liquid chromatography-electrospray mass spectrometry. This method was optimized and validated. PMID:8673254

Chang, J P; Ferguson, T H; Record, P A; Dickson, D A; Kiehl, D E; Kennington, A S



Optimization of conditions for high-performance size-exclusion chromatography of different soil humic acids.  


A method of high-performance size-exclusion chromatography (HPSEC) for a wide variety of soil humic acids (HAs) was developed. Two types of soil HAs (Cambisol and Andosol HAs), which have substantially different chemical properties, showed different effects of salt and organic solvent concentrations in the eluent on chromatograms. A Shodex OHpak SB-805 HQ column with 10 mM sodium phosphate buffer (pH 7.0) containing 25% of acetonitrile (v/v) was found to be applicable for different HAs, and showed high reproducibility and recovery (87.0 - 94.5%). The Cambisol HA was fractionated into five fractions using an ultrafiltration with different molecular-weight cut-offs. The order of the molecular weights of the five fractions calculated from the HPSEC analysis corresponded to that defined by ultrafiltration. This supported the reliability of the method. PMID:18469466

Asakawa, Daichi; Kiyota, Takuro; Yanagi, Yukiko; Fujitake, Nobuhide



Considerations in the use of high-pressure size exclusion chromatography (HPSEC) for determining molecular weights of aquatic humic substances  

Microsoft Academic Search

High-pressure size exclusion chromatography (HPSEC) is a powerful technique for determining molecular weight (MW) distributions of aquatic humic substances (HS). Previous researchers have shown that HPSEC can provide values of weight average molecular weight (Mw), number average molecular weight (Mn), and polydispersity (?) that are comparable to values determined by other techniques such as vapor pressure osmometry and field flow

Qunhui Zhou; Stephen E. Cabaniss; Patricia A. Maurice




ERIC Educational Resources Information Center

This booklet presents some activities on chromatography. Directions for preparing leaf pigment extracts using alcohol are given, and paper chromatography and thin-layer chromatography are described as modifications of the basic principles of chromatography. (KHR)

Brantley, L. Reed, Sr.; Demanche, Edna L.; Klemm, E. Barbara; Kyselka, Will; Phillips, Edwin A.; Pottenger, Francis M.; Yamamoto, Karen N.; Young, Donald B.


What can in situ ion chromatography offer for Mars exploration?  


The successes of the Mars exploration program have led to our unprecedented knowledge of the geological, mineralogical, and elemental composition of the martian surface. To date, however, only one mission, the Phoenix lander, has specifically set out to determine the soluble chemistry of the martian surface. The surprising results, including the detection of perchlorate, demonstrated both the importance of performing soluble ion measurements and the need for improved instrumentation to unambiguously identify all the species present. Ion chromatography (IC) is the state-of-the-art technique for soluble ion analysis on Earth and would therefore be the ideal instrument to send to Mars. A flight IC system must necessarily be small, lightweight, low-power, and have low eluent consumption. We demonstrate here a breadboard system that addresses these issues by using capillary IC at low flow rates with an optimized eluent generator and suppressor. A mix of 12 ions known or plausible for the martian soil, including 4 (oxy)chlorine species, has been separated at flow rates ranging from 1 to 10 ?L/min, requiring as little as 200 psi at 1.0 ?L/min. This allowed the use of pneumatic displacement pumping from a pressurized aluminum eluent reservoir and the elimination of the high-pressure pump entirely (the single heaviest and most energy-intensive component). All ions could be separated and detected effectively from 0.5 to 100 ?M, even when millimolar concentrations of perchlorate were present in the same mixtures. PMID:24963874

Shelor, C Phillip; Dasgupta, Purnendu K; Aubrey, Andrew; Davila, Alfonso F; Lee, Michael C; McKay, Christopher P; Liu, Yan; Noell, Aaron C



Hydrodynamic versus size exclusion chromatography characterization of alternan and comparison to off-line MALS.  


Alternan is an ultrahigh molar mass polysaccharide composed of alternating ?-(1?3) and ?-(1?6) repeat units and that also possesses long-chain branching. Its molar mass distribution (MMD) can extend into the hundreds of millions of grams per mole. Characterizing alternan by means of size exclusion chromatography (SEC) is a lengthy process and an incomplete one because even under the best possible experimental conditions, the polysaccharide appears to degrade during its passage through the SEC columns. As an alternative to SEC, we have investigated the use of hydrodynamic chromatography (HDC) as a possible characterization technique for alternan. Results from packed-column HDC with multiangle static light scattering (MALS) detection compare favorably to results from off-line MALS analysis, and HDC results are obtained in a fraction of the time needed for SEC. The largest molar mass alternan did appear to undergo some degradation during HDC as a result of interstitial stresses in the column bed. This could be remedied by the use of columns with larger packing particles. Evidence of long-chain branching in alternan is provided via a comparison of the intrinsic viscosities and viscometric radii of the polysaccharide to those of a pullulan standard and of a theoretical pullulan of molar mass equal to those of the alternans examined. PMID:20690593

Isenberg, Samantha L; Brewer, Amandaa K; Côté, Gregory L; Striegel, André M



Thermodynamic equilibrium of the solute distribution in size-exclusion chromatography.  


Our understanding of the nature of solute retention in size-exclusion chromatography (SEC) is predicated upon an equilibrium, entropy-controlled, size-exclusion mechanism. The entropic nature of the separation depends, in turn, upon the solute distribution coefficient (K(SEC) being at (or close to) thermodynamic equilibrium. Classic experiments to confirm this assumption were performed over thirty years ago. Here, we combine information obtained from both flow and static mixing SEC experiments to show that the solute distribution in SEC is in thermodynamic equilibrium over a molar mass range extending one order of magnitude higher than previously measured (from 2 x 10(3) to 1.1 x 10(6) Da) using crosslinked polystyrene packing material of identical pore size (10(4) A). The differences between our observations and previous ones conducted over three decades ago are ascribed, principally, to advances in stationary phase synthesis and column technology for SEC in particular and, secondarily, to improvements in the performance of the various instrumental components of liquid chromatographic systems in general. PMID:15088744

Striegel, André M



Molecular size fractionation of soil humic acids using preparative high performance size-exclusion chromatography.  


High performance size-exclusion chromatography (HPSEC) is useful for the molecular size separation of soil humic acids (HAs), but there is no method available for various HAs with different chemical properties. In this paper the authors propose a new preparative HPSEC method for various soil HAs. Three soil HAs with different chemical properties were fractionated by a Shodex OHpak SB-2004 HQ column with 10mM sodium phosphate buffer (pH 7.0)/acetonitrile (3:1, v/v) as an eluent. The HAs eluted within a reasonable column range time (12-25 min) without peak tailing. Preparative HPSEC chromatograms of these HAs indicated that non-size-exclusion effects were suppressed. The separated fractions were analyzed by HPSEC to determine their apparent molecular weights. These decreased sequentially from fraction 1 to fraction 10, suggesting that the HAs had been separated by their molecular size. The size-separated fractions of the soil HA were mixed to compare them with unfractionated HA. The analytical HPSEC chromatogram of the mixed HA was almost identical to that of the unfractionated HA. It appears that the HAs do not adsorb specifically to the column during preparative HPSEC. Our preparative HPSEC method allows for rapid and reproducible separation of various soil HAs by molecular size. PMID:21820122

Asakawa, Daichi; Iimura, Yasuo; Kiyota, Takuro; Yanagi, Yukiko; Fujitake, Nobuhide



Determination of sulphite in wines using suppressed ion chromatography.  


Suppressed ion chromatography with the use of a conductivity detector was developed for the determination of sulphite ions in wine samples. When a mixed solution of sodium carbonate, sodium bicarbonate, and acetone was used as the mobile phase, simultaneous determination of eight inorganic anions (i.e., fluoride, chloride, nitrite, nitrate, sulphite, phosphate, sulphate, and thiosulphate) was completed in approximately 25 min. Linearity, reproducibility, and detection limits were determined for the proposed method. In the case of sulphite detection, a linear calibration curve with a good correlation coefficient of 0.9992 was obtained from the peak height of sulphite with a relative standard deviation (n = 6) 1.48%. In addition, the detection limit of sulphite was 0.27 mg/L at a signal-to-noise ratio of 3. Further, the developed method was applied for the determination of sulphite contained in several wine samples. PMID:25529696

Yoshikawa, Kenji; Uekusa, Yuki; Sakuragawa, Akio



Ion chromatography detection of fluoride in calcium carbonate.  


Fluoride in aquatic systems is increasing due to anthropogenic pollution, but little is known about how this fluoride affects organisms that live in and around aquatic habitats. Fluoride can bioaccumulate in structures comprised of calcium carbonate, such as shells and skeletons of both freshwater and saltwater species as diverse as snails, corals, and coccolithophorid algae. In this article, ion chromatography (IC) techniques are developed to detect and quantify fluoride in a matrix of calcium carbonate. Solid samples are dissolved in hydrochloric acid, pretreated to remove the majority of the chloride ions, and then analyzed using IC. With these methods, the 3? limit of detection is 0.2 mg of fluoride/kg of calcium carbonate. PMID:21859530

Lefler, Jamie E; Ivey, Michelle M



Ion Exclusion by Sub 2-nm Carbon Nanotube Pores  

SciTech Connect

Carbon nanotubes offer an outstanding platform for studying molecular transport at nanoscale, and have become promising materials for nanofluidics and membrane technology due to their unique combination of physical, chemical, mechanical, and electronic properties. In particular, both simulations and experiments have proved that fluid flow through carbon nanotubes of nanometer size diameter is exceptionally fast compared to what continuum hydrodynamic theories would predict when applied on this length scale, and also, compared to conventional membranes with pores of similar size, such as zeolites. For a variety of applications such as separation technology, molecular sensing, drug delivery, and biomimetics, selectivity is required together with fast flow. In particular, for water desalination, coupling the enhancement of the water flux with selective ion transport could drastically reduce the cost of brackish and seawater desalting. In this work, we study the ion selectivity of membranes made of aligned double-walled carbon nanotubes with sub-2 nm diameter. Negatively charged groups are introduced at the opening of the carbon nanotubes by oxygen plasma treatment. Reverse osmosis experiments coupled with capillary electrophoresis analysis of permeate and feed show significant anion and cation rejection. Ion exclusion declines by increasing ionic strength (concentration) of the feed and by lowering solution pH; also, the highest rejection is observed for the A{sub m}{sup Z{sub A}} C{sub n}{sup Z{sub C}} salts (A=anion, C=cation, z= valence) with the greatest Z{sub A}/Z{sub C} ratio. Our results strongly support a Donnan-type rejection mechanism, dominated by electrostatic interactions between fixed membrane charges and mobile ions, while steric and hydrodynamic effects appear to be less important. Comparison with commercial nanofiltration membranes for water softening reveals that our carbon nanotube membranes provides far superior water fluxes for similar ion rejection capabilities.

Fornasiero, F; Park, H G; Holt, J K; Stadermann, M; Grigoropoulos, C P; Noy, A; Bakajin, O



Derivatization patterns among starch chain populations assessed by ion-exchange chromatography: A model system approach.  


Reaction patterns of wheat starch derivatized with a fluorescent probe (model reaction system) were investigated over the course of a reaction period (0.5, 4, 12, or 24h). Debranched derivatives were fractionated into three populations (Unbound, Bound-1, Bound-2) based on charge density via anion-exchange chromatography, with each ion-exchanged fraction further analyzed by size-exclusion chromatography (refractive index [RI] and fluorescence [FL] detection) to assess proportions and patterns of reaction on amylose (AM) and amylopectin (AP) long (LC), medium (MC), and short (SC) branch chains. Approximately 11-12% of the total chains accounted for 63-75% of the FL recovered in the two bound fractions. FL peaks representing AM, AP-LC, AP-MC, AP-SC, and intermediate material (eluted with AM based on molecular size, but reacted more akin to AP-LC) were monitored over the reaction period. Fractionation behaviors varied amongst starch chains, attributable to the impact of the granule structure on molecular reaction patterns. PMID:25817689

Hong, Jung Sun; Huber, Kerry C



Peptide Orientation Affects Selectivity in Ion-Exchange Chromatography  

SciTech Connect

Here we demonstrate that separation of proteolytic peptides, having the same net charge and one basic residue, is affected by their specific orientation toward the stationary phase in ion-exchange chromatography. In electrostatic repulsion-hydrophilic interaction chromatography (ERLIC) with an anion-exchange material, the C-terminus of the peptides is, on average, oriented toward the stationary phase. In cation exchange, the average peptide orientation is the opposite. Data with synthetic peptides, serving as orientation probes, indicate that in tryptic/Lys-C peptides the C-terminal carboxyl group appears to be in a zwitterionic bond with the side chain of the C-terminal Lys/Arg residue. In effect, the side chain is then less basic than the N-terminus, accounting for the specific orientation of tryptic and Lys-C peptides. Analyses of larger sets of peptides, generated from lysates by either Lys-N, Lys-C, or trypsin, reveal that specific peptide orientation affects the ability of harged side chains, such as phosphate residues, to influence retention. Phosphorylated residues that are remote in the sequence from the binding site affect retention less than those that are closer. When a peptide contains multiple charged sites, then orientation is observed to be less rigid and retention tends to be governed by the peptide’s net charge rather than its sequence. These general observations could be of value in confirming a peptide’s identification and, in particular, phosphosite assignments in proteomics analyses. More generally, orientation accounts for the ability of chromatography to separate peptides of the same compositionbut different sequence.

Alpert, Andrew J.; Petritis, Konstantinos; Kangas, Lars J.; Smith, Richard D.; Mechtler, Karl; Mitulovic, Goran; Mohammed, Shabaz; Heck, Albert J.



Peptide Orientation Affects Selectivity in Ion-Exchange Chromatography  

SciTech Connect

Here we demonstrate that separation of proteolytic peptides, having the same net charge and one basic residue, is affected by their specific orientation toward the stationary phase in ion-exchange chromatography. In electrostatic repulsion-hydrophilic interaction chromatography (ERLIC) with an anion-exchange material, the C-terminus of the peptides is, on average, oriented toward the stationary phase. In cation exchange, the average peptide orientation is the opposite. Data with synthetic peptides, serving as orientation probes, indicate that in tryptic/ Lys-C peptides the C-terminal carboxyl group appears to be in a zwitterionic bond with the side chain of the C-terminal Lys/Arg residue. In effect, the side chain is then less basic than the N-terminus, accounting for the specific orientation of tryptic and Lys-C peptides. Analyses of larger sets of peptides, generated from lysates by either Lys-N, Lys-C, or trypsin, reveal that specific peptide orientation affects the ability of charged side chains, such as phosphate residues, to influence retention. Phosphorylated residues that are remote in the sequence from the binding site affect retention less than those that are closer. When a peptide contains multiple charged sites, then orientation is observed to be less rigid and retention tends to be governed by the peptide’s net charge rather than its sequence. These general observations could be of value in confirming a peptide’s identification and, in particular, phosphosite assignments in proteomics analyses. More generally, orientation accounts for the ability of chromatography to separate peptides of the same composition but different sequence.

Alpert, Andrew J.; Petritis, Konstantinos; Kangas, Lars J.; Smith, R. D.; Mechtler, Karl; Mitulovic, Goran; Mohammed, Shabaz; Heck, Albert J.



A multifunctional dual membrane electrodialytic eluent generator for capillary ion chromatography  

Microsoft Academic Search

A multifunctional electrodialytic generator (EDG) for capillary ion chromatography (CIC) is described. The same device can generate acidic, basic or saline eluents. Two oppositely charged ion exchange beads are used to fabricate the EDG; the dual ion exchanger configuration ensures the production of gas-free eluent, obviating the need of a gas removal device used with single ion exchanger EDG's. The

Bingcheng Yang; Feifang Zhang; Xinmiao Liang; Purnendu K. Dasgupta



Molecular weight distribution characterization of hydrophobe-modified hydroxyethyl cellulose by size-exclusion chromatography.  


Size-exclusion chromatography (SEC) of hydrophobe-modified hydroxyethyl cellulose (HmHEC) is challenging because polymer chains are not isolated in solution due to association of hydrophobic groups and hydrophobic interaction with column packing materials. An approach to neutralize these hydrophobic interactions was developed by adding ?-cyclodextrin (?-CD) to the aqueous eluent. SEC mass recovery, especially for the higher molecular weight chains, increased with increasing concentration of ?-CD in the eluent. A ?-CD concentration of 0.75wt% in the eluent was determined to be optimal for the HmHEC polymers studied. These conditions enabled precise determinations of apparent molecular weight distributions exhibiting less than 2% relative standard deviation in the measured weight-average molecular weight (MW) for five injections on three studied samples and showed no significant differences in MW determined on two different days. The developed technology was shown to be very robust for characterizing HmHEC having MW from 500kg/mol to 2000kg/mol, and it can be potentially applied to other hydrophobe-modified polymers. PMID:25092594

Li, Yongfu; Meunier, David M; Partain, Emmett M



Size exclusion chromatography for analyses of fibroin in silk: optimization of sampling and separation conditions  

NASA Astrophysics Data System (ADS)

A direct goal of this paper was to improve the methods of sample preparation and separation for analyses of fibroin polypeptide with the use of size exclusion chromatography (SEC). The motivation for the study arises from our interest in natural polymers included in historic textile and paper artifacts, and is a logical response to the urgent need for developing rationale-based methods for materials conservation. The first step is to develop a reliable analytical tool which would give insight into fibroin structure and its changes caused by both natural and artificial ageing. To investigate the influence of preparation conditions, two sets of artificially aged samples were prepared (with and without NaCl in sample solution) and measured by the means of SEC with multi angle laser light scattering detector. It was shown that dialysis of fibroin dissolved in LiBr solution allows removal of the salt which destroys stacks chromatographic columns and prevents reproducible analyses. Salt rich (NaCl) water solutions of fibroin improved the quality of chromatograms.

Pawcenis, Dominika; Koperska, Monika A.; Milczarek, Jakub M.; ?ojewski, Tomasz; ?ojewska, Joanna



Analysis of a MIL-L-27502 lubricant from a gas-turbine engine test by size-exclusion chromatography  

NASA Technical Reports Server (NTRS)

Size exclusion chromatography was used to determine the chemical degradation of MIL-L-27502 oil samples from a gas turbine engine test run at a bulk oil temperature of 216 C. Results revealed a progressive loss of primary ester and additive depletion and the formation of higher molecular weight products with time. The high molecular weight products absorbed strongly in the ultraviolet indicating the presence of chromophoric groups.

Jones, W. R., Jr.; Morales, W.



Molar mass distribution of hydroxypropyl cellulose by size exclusion chromatography with dual light scattering and refractometric detection  

Microsoft Academic Search

Physico-chemical properties of cellulose derivatives are of considerable interest in many technical applications, for example, in the food and drug industry. Efficient and careful characterisation of these properties is thus highly desirable. In this study, two different size exclusion chromatography (SEC) systems, connected on-line either to a low-angle laser light scattering detector (LALLS) or to a multi-angle laser light scattering

Bengt Wittgren; Bed?ich Porsch



Electrophoresis and size-exclusion chromatography of humic substances extracted from detritus and soils of different geneses  

Microsoft Academic Search

Electrophoresis in 10% polyacrylamide gel in the presence of denaturants and size-exclusion chromatography in Sephadex G-75\\u000a in 7 M urea were used for the comparative analysis of humic substances isolated from a typical chernozem, soddy-podzolic soil,\\u000a and chestnut soil and from the easily decomposable organic matter (plant detritus) contained in these soils. After the electrophoresis,\\u000a the gel with naturally colored

O. E. Trubetskaya; O. A. Trubetskoi; B. A. Borisov; N. F. Ganzhara



Electrophoresis and size-exclusion chromatography of humic substances extracted from detritus and soils of different geneses  

Microsoft Academic Search

Electrophoresis in 10% polyacrylamide gel in the presence of denaturants and size-exclusion chromatography in Sephadex G-75 in 7 M urea were used for the comparative analysis of humic substances isolated from a typical chernozem, soddy-podzolic soil, and chestnut soil and from the easily decomposable organic matter (plant detritus) contained in these soils. After the electrophoresis, the gel with naturally colored

O. E. Trubetskaya; O. A. Trubetskoi; B. A. Borisov; N. F. Ganzhara



Molar mass determination of poly(octadecene-alt-maleic anhydride) copolymers by size exclusion chromatography and dilute solution viscometry  

Microsoft Academic Search

The number average molar mass Mn of poly(octadecene-alt-maleic anhydride) (PODMA) copolymers calculated from data obtained by size exclusion chromatography (SEC) using a polystyrene (PS) calibration was found to be inaccurate. The use of SEC combined with dilute solution viscometry enabled a method to be developed using an iterative approach, which does not require knowledge of the Mark–Houwink constants for PODMA

Mark C Davies; John V Dawkins; Douglas J Hourston; Elizabeth Meehan



Evaluation of the “effective volume shift” method for axial dispersion corrections in multi-detector size exclusion chromatography  

Microsoft Academic Search

Band broadening in size exclusion chromatography (SEC) causes errors in the calculated molar mass distribution even when molar-mass-sensitive detectors are used. These errors can be partially corrected by shifting the elution volume of the molar-mass-sensitive detector chromatogram relative to the concentration detector chromatogram, and then re-calculating the molar mass distribution. In this paper a computer simulation of multi-detector SEC of

Christian Jackson



A comparison of calibration procedures for the analysis of broad molecular weight distributions using size exclusion chromatography with multiple detection  

Microsoft Academic Search

A range of well characterized broad polymer standards has been analysed using size exclusion chromatography (s.e.c.), with differential refractive index, low angle laser light scattering (LALLS) and differential viscometry (DV) as on-line detection methods. This study highlights the importance of accurate and precise estimation of the inter detector delay (IDD) parameter and shows that the conventional methods of IDD measurement

Michael D. Zammit; Thomas P. Davis



Unraveling the mystery of natural rubber biosythesis part I: investigation of the composition and growth of in vitro natural rubber using high resolution size exclusion chromatography  

Technology Transfer Automated Retrieval System (TEKTRAN)

Monitoring the growth of in vitro natural rubberwas accomplished by high resolution size exclusion chromatography, SEC.Washed rubber particles isolated from H. brasiliensis latex, containing the rubber transferase enzyme, were used to catalyze the polymerization of synthetic isopentenyl pyrophosphat...


Single-step isolation of extracellular vesicles by size-exclusion chromatography  

PubMed Central

Background Isolation of extracellular vesicles from plasma is a challenge due to the presence of proteins and lipoproteins. Isolation of vesicles using differential centrifugation or density-gradient ultracentrifugation results in co-isolation of contaminants such as protein aggregates and incomplete separation of vesicles from lipoproteins, respectively. Aim To develop a single-step protocol to isolate vesicles from human body fluids. Methods Platelet-free supernatant, derived from platelet concentrates, was loaded on a sepharose CL-2B column to perform size-exclusion chromatography (SEC; n=3). Fractions were collected and analysed by nanoparticle tracking analysis, resistive pulse sensing, flow cytometry and transmission electron microscopy. The concentrations of high-density lipoprotein cholesterol (HDL) and protein were measured in each fraction. Results Fractions 9–12 contained the highest concentrations of particles larger than 70 nm and platelet-derived vesicles (46%±6 and 61%±2 of totals present in all collected fractions, respectively), but less than 5% of HDL and less than 1% of protein (4.8%±1 and 0.65%±0.3, respectively). HDL was present mainly in fractions 18–20 (32%±2 of total), and protein in fractions 19–21 (36%±2 of total). Compared to the starting material, recovery of platelet-derived vesicles was 43%±23 in fractions 9–12, with an 8-fold and 70-fold enrichment compared to HDL and protein. Conclusions SEC efficiently isolates extracellular vesicles with a diameter larger than 70 nm from platelet-free supernatant of platelet concentrates. Application SEC will improve studies on the dimensional, structural and functional properties of extracellular vesicles. PMID:25279113

Böing, Anita N.; van der Pol, Edwin; Grootemaat, Anita E.; Coumans, Frank A. W.; Sturk, Auguste; Nieuwland, Rienk



Speciation of trace elements in proteins in human and bovine serum by size exclusion chromatography and inductively coupled plasma-mass spectrometry with a magnetic sector mass spectrometer.  


Proteins are separated by size exclusion chromatography while atomic ions from the inorganic elements are detected on-line by inductively coupled plasma-mass spectrometry. A double focusing mass analyzer provides very high sensitivity, low background, and sufficient spectral resolution to separate the atomic ions of interest from most polyatomic ions at the same nominal m/z value. The chromatograms show the distribution of the elements of interest between protein-bound and free fractions and provide the approximate molecular weights of those protein fractions that contain the elements monitored. The distribution of various elements, including V, Mo, Fe, Co, Mn, and lanthanides, in human or bovine serum samples are shown. Alkali metals and Tl are present primarily as free metal ions and are not bound to proteins. Inorganic elements spiked into the serum samples can be followed into various proteins. EDTA does not remove Fe, Pb, Sn, or Th from the proteins but does extract Mn from some proteins. Procedures for determining the effects of breaking disulfide linkages on the metal binding characteristics of proteins are also described. PMID:10550683

Wang, J; Houk, R S; Dreessen, D; Wiederin, D R




NSDL National Science Digital Library

This site provides fundamental background information about chromatography, including plate theory, rate theory, the mechanisms of separations, and qualitative and quantitative aspects of chromatography. The format is a series of PowerPoint-like presentations available in PDF format.

Hardy, James K.


Determination of Cyanogenic Compounds in Edible Plants by Ion Chromatography  

PubMed Central

Cyanogenic glycosides are HCN-producing phytotoxins; HCN is a powerful and a rapidly acting poison. It is not difficult to find plants containing these compounds in the food supply and/or in medicinal herb collections. The objective of this study was to investigate the distribution of total cyanide in nine genera (Dolichos, Ginkgo, Hordeum, Linum, Phaseolus, Prunus, Phyllostachys, Phytolacca, and Portulaca) of edible plants and the effect of the processing on cyanide concentration. Total cyanide content was measured by ion chromatography following acid hydrolysis and distillation. Kernels of Prunus genus are used medicinally, but they possess the highest level of total cyanide of up to 2259.81 CN?/g dry weight. Trace amounts of cyanogenic compounds were detected in foodstuffs such as mungbeans and bamboo shoots. Currently, except for the WHO guideline for cassava, there is no global standard for the allowed amount of cyanogenic compounds in foodstuffs. However, our data emphasize the need for the guidelines if plants containing cyanogenic glycosidesare to be developed as dietary supplements. PMID:24278641

Cho, Hye-Jeon; Do, Byung-Kyung; Shim, Soon-Mi; Lee, Dong-Ha; Nah, Ahn-Hee; Choi, Youn-Ju; Lee, Sook-Yeon



Fluoride and aluminum release from restorative materials using ion chromatography  

PubMed Central

Objective The aim of this study was to determine the amounts of fluoride and aluminum released from different restorative materials stored in artificial saliva and double-distilled water. Material and Methods Cylindrical specimens (10 x 1 mm) were prepared from 4 different restorative materials (Kavitan Plus, Vitremer, Dyract Extra, and Surefil). For each material, 20 specimens were prepared, 10 of which were stored in 5 mL artificial saliva and 10 of which were stored in 5 mL of double-distilled water. Concentrations of fluoride and aluminum in the solutions were measured using ion chromatography. Measurements were taken daily for one week and then weekly for two additional weeks. Data were analyzed using two-way ANOVA and Duncan's multiple range tests (p<0.05). Results The highest amounts of both fluoride and aluminum were released by the resin-modified glass ionomer cement Vitremer in double-distilled water (p<0.05). All materials released significantly more fluoride in double-distilled water than in artificial saliva (p<0.05). In artificial saliva, none of the materials were observed to release aluminum. Conclusion It was concluded that storage media and method of analysis should be taken into account when the fluoride and aluminum release from dental materials is assessed. PMID:22437674

OKTE, Zeynep; BAYRAK, Sule; FIDANCI, Ulvi Reha; SEL, Tevhide



Thin layer chromatography-ion mobility spectrometry (TLC-IMS).  


Ion mobility spectrometry (IMS) is a fast and sensitive analytical method which operates at the atmospheric pressure. To enhance the capability of IMS for the analysis of mixtures, it is often used with preseparation techniques, such as GC or HPLC. Here, we report for the first time the coupling of the thin-layer chromatography and IMS. A variety of coupling schemes were tried that included direct electrospray from the TLC strip tip, indirect electrospray from a needle connected to the TLC strip, introducing the moving solvent into the injection port, and, the simplest way, offline introduction of scratched or cut pieces of strips into the IMS injection port. In this study a special solvent tank was designed and the TLC strip was mounted horizontally where the solvent would flow down. A very small funnel right below the TLC tip collected the solvent and transferred it to a needle via a capillary tubing. Using the TLC-ESI-IMS technique, acceptable separations were achieved for two component mixtures of morphine-papaverine and acridine-papaverine. A special injection port was designed to host the pieces cut off the TLC. The method was successfully used to identify each spot on the TLC by IMS in a few seconds. PMID:25419999

Ilbeigi, Vahideh; Tabrizchi, Mahmoud



Analysis of anions in beer using ion chromatography  

PubMed Central

The majority of anions found in beer are a consequence of impurities derived from the water used during the brewing process. The process of beer manufacture consists of malting, brewing and fermentation followed by maturation before filtration and finally storage. Strict quality control is required because the presence of certain anions outside strictly defined tolerance limits can affect the flavour characteristics of the finished product. The anions present were quantified using the technique of ion chromatography with the Metrohm modular system following sample preparation. The analysis produced a result of the order 200 mg l-1 for chloride, phosphate and sulphate and around 20 mg l-1 for nitrate. If the chloride level exceeds 250 mg l-1, then the sweetness of the beer is enhanced, but yeast flocculation can be hindered. An excess of sulphate can give a sharp, dry edge to hopped beers and excessive amounts of nitrate have been found to harm the yeast metabolism after conversion to the nitrite form. As water is a primary ingredient within beer, its quality and type is a fundamental factor in establishing many of the distinctive regional beers that can be found in the United Kingdom and is thus monitored carefully. PMID:18924733

Bruce, Jonathan



Hyphenation of liquid chromatography to ion trap mass spectrometry to identify minor components in polypeptide antibiotics  

Microsoft Academic Search

The application of liquid chromatography–ion trap mass spectrometry for the characterization of linear and cyclic polypeptide antibiotics was investigated. The aim was on-line identification of impurities in those antibiotic complexes without recourse to time-consuming isolation and purification procedures. Hyphenated techniques, such as liquid chromatography coupled to mass spectrometry, are ideally suited for this purpose. Characterization was performed with an ion

C. Govaerts; E. Adams; Ann Van Schepdael; J. Hoogmartens




NSDL National Science Digital Library

This lab activity from the Biotechnology Alliance for Suncoast Biology Educators covers background information on the basic types of chromatography and has the student separate pigments extracted from pens and plant leaves using paper chromatography. The lesson includes the materials needed and the demonstration procedures.

Keirle, Matt


Rapid One-Step Isolation of Mouse Liver Catalase by Immobilized Metal Ion Affinity Chromatography  

Microsoft Academic Search

A novel and rapid procedure for the isolation of catalase from mouse liver, after prior treatment with the peroxisome proliferator perfluorooctanoic acid was developed using immobilized metal ion affinity chromatography involving chelation with zinc ions. The purification developed is simple, rapid (requiring 3 hours from cytosol or peroxisomal matrix to homogeneous proteins), reproducible, and yields virtually complete overall recovery of

Qian Yang; Joseph W. DePierre




EPA Science Inventory

Four collection protocols for the heart-cutting procedure in ion chromatography were compared statistically to determine the best method for use in the analysis of trace ions in water. In the comparison, the protocols were applied in the analysis of 0.1 to 0.4-ppm AS(V) added to ...



EPA Science Inventory

An analytical method was developed for the analysis of the NO2 collected by a passive diffusion controlled atmospheric sampling device. The method measured the total amount of nitrite ion using ion chromatography. The precision obtained under field conditions, defined as twice th...


High resolution separation of recombinant monoclonal antibodies by size-exclusion ultra-high performance liquid chromatography (SE-UHPLC).  


Size-exclusion chromatography (SEC) is an important mode of separation used in monoclonal antibody (mAb) characterization and quality control. SEC separates mAbs into three major species: high molecular weight species, main peak (predominantly monomer), and low molecular weight species. However, mAb SEC separations have low resolution between the different sized species, and the analysis is slow with low sample throughput. The introduction of size-exclusion ultra-high performance liquid chromatography (SE-UHPLC) columns offers a new opportunity to improve both the resolution and throughput of SEC analysis. This study demonstrates that SE-UHPLC columns deliver better resolution of size variants in a shorter period of time than conventional SEC columns. For example, an SE-UHPLC column 300-mm in length produced separation of mAb Fab/c fragments in less than 10min, in comparison to a conventional SEC column output, where these fragments co-elute with the main peak. Furthermore, we observed that high back pressure does not generate HMWS under optimized mobile phase conditions for mAbs. The platform SE-UHPLC method has been demonstrated to be suitable for the analysis of multiple mAbs, with greatly improved sample throughput and peak resolution of mAb size variants. PMID:25766848

Yang, Renee; Tang, Yun; Zhang, Bing; Lu, Xuemei; Liu, Alice; Zhang, Yonghua Taylor



Ion-exchange chromatography separation applied to mineral recycle in closed systems  

NASA Technical Reports Server (NTRS)

As part of the controlled ecological life support system (CELSS) program, a study is being made of mineral separation on ion-exchange columns. The purpose of the mineral separation step is to allow minerals to be recycled from the oxidized waste products of plants, man, and animals for hydroponic food production. In the CELSS application, relatively large quantities of minerals in a broad concentration range must be recovered by the desired system, rather than the trace quantities and very low concentrations treated in analytical applications of ion-exchange chromatography. Experiments have been carried out to assess the parameters pertinent to the scale-up of ion-exchange chromatography and to determine feasibility. Preliminary conclusions are that the column scale-up is in a reasonable size range for the CELSS application. The recycling of a suitable eluent, however, remains a major challenge to the suitability of using ion exchange chromatography in closed systems.

Ballou, E.; Spitze, L. A.; Wong, F. W.; Wydeven, T.; Johnson, C. C.



[Determination of hydrazine ion in explosion dust of liquid explosive by ion chromatography].  


A method for the determination of hydrazine ion in explosion dust of liquid explosive has been established by ion chromatography. The hydrazine ion in an explosion dust sample was extracted with deionized water by sonification and centrifugation. The large molecules and solid particles in supernatant were removed by an OnGuard II RP column and a 0.22 microm filtration membrane, respectively. The filtrate was separated on an IonPac CS-12A column with isocratic elution of 5 mmol/L methanesulfonic acid (MSA). Then 0.1 mol/L NaOH solution was post-column added and the resultant solution was detected by an ampere detector with golden electrode. The results showed that, the calibration curve was linear in the range of 0.02 - 2.0 mg/L with a correlation coefficient (r2 ) of 0.999 7. The limits of detection (LOD, S/N = 3) and quantification (LOQ, S/N = 10) of hydrazine were 5.0 microg/L and 16.6 microg/L, respectively. The recoveries ranged between 95.4% and 99.1% with the relative standard deviations (RSDs, n = 5) of 2.1% - 3.3%. The hydrazine content in a real explosion dust sample of liquid explosive was 10.3 mg/kg by this method. The method is simple, accurate, and suitable for the quantitative detection of hydrazine ions in explosion dust of liquid explosive, and the method can meet the needs of the criminal evidence identification work. PMID:24392633

Wang, Yong; Geng, Qing; Zuo, Yuexian; Zhou, Xinwen; Lian, Hongzhen; Pan, Guangwen




NSDL National Science Digital Library

In this activity, explore chromatography and the various colors that make up the ink in markers. Use this activity to investigate cohesion and adhesion. The online version of this activity is set up so that learners solve a mystery.



A simplified ion exchange bead-based KOH electrodialytic generator for capillary ion chromatography.  


A simple potassium hydroxide electrodialytic generator (EDG) with singe membrane configuration is described. In this setup, one cation exchange resin (CER) bead is used to fabricate the EDG in place of the common membrane sheet. The device is implemented simply in a commercial stainless steel (SS) Tee which serves as both the EDG cartridge and the cathodic electrode. The present EDG has much lower internal volume (approximately 0.16(L), which is well suited with capillary ion chromatography system. The device has been tested up pressures to 3200 psi and could be directly deployed on the high-pressure side of the pump. The electrolysis gas can be effectively removed by a segment of PTFE tubing. In the tested range of 0-100mM, the KOH concentration is generated linearly with the applied current being near-Faradaic efficiency. The device permits both isocratic and gradient operation with good reproducibility, as demonstrated by the analysis of anions. PMID:19376345

Yang, Bingcheng; Zhang, Feifang; Liang, Xinmiao




EPA Science Inventory

Selenate, selenite, and arsenate ions were separated from the major anions chloride, nitrate, and sulfate in drinking water, surface water, and groundwater sources by collecting a selected portion of the ion chromatogram, after suppression, on a concentrator column and reinjectin...


Ion-Exchange Celluloses and Their Use in Chromatography  

Microsoft Academic Search

CONTENTS I. Introduction 104 II. Preparation of ion-exchange celluloses 104 III. Properties of ion-exchange celluloses 105 IV. Technique of the application of ion-exchange celluloses 107 V. Uses of ion-exchange celluloses 110 Bibtex entry for this abstract Preferred format for this abstract (see Preferences) Find Similar Abstracts: Use: Authors Title Abstract Text Return: Query Results Return items starting with number Query

E. G. Davidova; V. V. Rachinskii



Selective retention of basic compounds by metal aquo-ion affinity chromatography.  


A novel metal aquo-ion affinity chromatography has been developed for the analysis of basic compounds using heat-treated silica gel containing hydrated metal cations (metal aquo-ions) as the packing material. The packing materials of the metal aquo-ion affinity chromatography were prepared by the immobilization of a single metal component such as Fe(III), Al(III), Ag(I), and Ni(II) on silica gel followed by extensive heat treatment. The immobilized metals form aquo-ions to present cation-exchange ability for basic analytes and the cation-exchange ability for basic analytes depends on pKa of the immobilized metal species. In the present study, to evaluate the retention characteristics of metal aquo-ion affinity chromatography, the on-line solid-phase extraction of drugs was investigated. Obtained data clearly evidence the selective retention capability of metal aquo-ion affinity chromatography for basic analytes with sufficient capacity. PMID:25044622

Asakawa, Yoshiki; Yamamoto, Eiichi; Asakawa, Naoki



Application of ion chromatography to the study of hydrolysis of some halogenated hydrocarbons at ambient temperatures  

NASA Technical Reports Server (NTRS)

The application of ion chromatography to the study of very slow rates of hydrolysis of some halogenated hydrocarbons was investigated. The halide concentrations in the aqueous phase of mixtures of a carbonate buffer (pH = 10.3) and either chloroform (CHC13) or fluorotrichloromethane (CFC13) after aging for various lengths of time at room temperature, were determined by ion chromatography. Hydrolysis of CHC13 caused the C1(-) concentration to increase by about 1500 ppb per day. On the other hand neither the F(-) or C1(-) concentration in the CFC13 mixture increased by as much as 1 ppb per day. The magnitude of errors in the determination of halides prevented any firm conclusions regarding hydrolysis in this mixture. However, these results were used to show how ion chromatography could expedite identification of the hydrolyzing substance as well as investigations of hydrolysis mechanisms.

Otterson, D. A.



Size Exclusion Chromatography: An Experiment for High School and Community College Chemistry and Biotechnology Laboratory Programs  

ERIC Educational Resources Information Center

A simple multiday laboratory exercise suitable for use in a high school or community college chemistry course or a biotechnology advanced placement biology course is described. In this experiment students gain experience in the use of column chromatography as a tool for the separation and characterization of biomolecules, thus expanding their…

Brunauer, Linda S.; Davis, Kathryn K.



Size exclusion chromatography-inductively coupled plasma atomic emission spectrographic study of Fe in bitumens derived from tar sands  

SciTech Connect

This paper reports on bitumens extracted from tar sands from various locations (Utah, California, Kentucky, and Alberta) that were examined by size exclusion chromatography with on-line element-specific detection to study the Fe concentration as a function of size. In most cases, the resulting profiles exhibit unimodal distributions at relatively large molecular size with very similar times for maximum elution. specifically, Sunnyside (Utah) and McKittrick (California) tar-sand bitumens exhibited very intense maxima consistent with extremely high bulk Fe contents. Arroyo Grande (California) exhibited an additional maximum at very large molecular size. This size behavior of the Fe appears to correlate with the large molecular size Ni and V components eluted under the same conditions.

Reynolds, J.G. (Lawrence Livermore National Lab., Livermore, CA (US)); Biggs, W.R. (Chevron Research Co., Richmond, CA (US))



Detector response as a function of molecular weight and its effect on size exclusion chromatography molecular weight determination of polymer distributions  

Microsoft Academic Search

In size exclusion chromatography (SEC), if the response of the detector is not constant with molecular weight, the calculated molecular weights are not a true representation for the sample. Without response factors, or some other method of correcting the response for the specific polymer calibration standards used, the resulting distribution is biased. From literature references, it is known that polystyrene

Simon David Cook; Vicki S. Sible



Analysis of trace inorganic anions in weak acid salts by single pump cycling-column-switching ion chromatography.  


The application of ion chromatography with the single pump cycling-column-switching technique was described for the analysis of trace inorganic anions in weak acid salts within a single run. Due to the hydrogen ions provided by an anion suppressor electrolyzing water, weak acid anions could be transformed into weak acids, existing as molecules, after passing through the suppressor. Therefore, an anion suppressor and ion-exclusion column were adopted to achieve on-line matrix elimination of weak acid anions with high concentration for the analysis of trace inorganic anions in weak acid salts. A series of standard solutions consisting of target anions of various concentrations from 0.005 to 10 mg/L were analyzed, with correlation coefficients r ? 0.9990. The limits of detection were in the range of 0.67 to 1.51 ?g/L, based on the signal-to-noise ratio of 3 and a 25 ?L injection volume. Relative standard deviations for retention time, peak area, and peak height were all less than 2.01%. A spiking study was performed with satisfactory recoveries between 90.3 and 104.4% for all anions. The chromatographic system was successfully applied to the analysis of trace inorganic anions in five weak acid salts. PMID:25641739

Huang, Zhongping; Ni, Chengzhu; Zhu, Zhuyi; Pan, Zaifa; Wang, Lili; Zhu, Yan



Ion-exchange sorption and preparative chromatography of biologically active materials  

SciTech Connect

This book presents information on the following topics: the problems of fine physico-chemical biotechnology; types of highly permeable network polyelectrolytes; methods for studying the permeability and porosity of network polyelectrolytes; the conformation state and flexibility of the structural elements of network polyelectrolytes; ion-exchange processes without the sorption of physiologically active substances; ion exchange, hydration, and swelling; nucleosides, nucleotides, alkaloids, sulfonamides, and miscellaneous physiologically active subtances; sharp front formation for the exchange of ions with the same valences; standard quasi-equilibrium frontal chromatography on ionites; sorption kinetics in ionites with structural heterogeneity; experimental investigations of the diffusivities of organic and physiologically active ions in ionite beads; and increasing the efficiency of low-pressure chromatography by using surface-layer and bidispersed ionites.

Samsonov, G.V.



Aggregation analysis of pharmaceutical human immunoglobulin preparations using size-exclusion chromatography and analytical ultracentrifugation sedimentation velocity.  


In the pharmaceutical industry, analysis of soluble aggregates in pharmaceutical formulations is most commonly performed using size-exclusion chromatography (SEC). However, owing to concerns that aggregates can be overlooked by SEC analysis, it has been suggested that its results should be confirmed with orthogonal methods. One of the main alternative methods for SEC is analytical ultracentrifugation sedimentation velocity (AUC-SV), which has been indicated as an important tool for the measurement of protein aggregation. The present study aimed to show that AUC-SV can be effectively applied for the characterization of marketed immunoglobulin pharmaceutical preparations to support the results obtained by SEC. In addition, the present research aimed to assess the appropriateness of two integration approaches for the quantitative analysis of the SEC results. Thus, the aggregates were measured in seven different preparations of human immunoglobulins by AUC-SV and SEC, and the acquired chromatographic data were processed by using either the vertical drop method or the Gaussian skim approach, implemented in the Empower II chromatography data software (Waters, Tokyo, Japan). The results of aggregation measurements performed using AUC-SV were in good agreement with those obtained using SEC. As expected, the Gaussian skim integration approach inherently provided lower estimates of aggregation content than the results of the vertical drop method. The finding of this study confirmed the complementary nature of AUC-SV to SEC for aggregate composition analysis and underscored the important role that the different integration methods can play in the quantitative interpretation of chromatographic results. PMID:22925901

Krayukhina, Elena; Uchiyama, Susumu; Nojima, Kiyoko; Okada, Yoshiaki; Hamaguchi, Isao; Fukui, Kiichi



Novel determination of phytate by ion chromatography in wild rice and diet composites  

Technology Transfer Automated Retrieval System (TEKTRAN)

We have developed an ion chromatography (IC) assay using ultraviolet (UV) detection following post-column derivatization with ferric nitrate to determine phytate [inositol hexakis phosphate (iP6)] (1) (2) in wild rice samples and other diet composites. Samples were ground to a fine homogeneous powd...


Rapid quantitative method for total brominated vegetable oil in soft drinks using ion chromatography  

Microsoft Academic Search

A simple, quantitative and rapid method for total brominated vegetable oil (BVO) using ion chromatography (IC) with suppressed conductivity detection was developed and successfully applied to soft drinks with results expressed as inorganic bromide anion. The procedure involves extraction of BVO with diethyl ether and treatment with zinc dust in a solution of acetic acid, giving recoveries ranging between 92.5

Ashraf A. Yousef; Alaa B. Abbas; Bassam Sh. Badawi; Wafaa Y. Al-Jowhar; Esam A. Zain; Seham A. El-Mufti




Technology Transfer Automated Retrieval System (TEKTRAN)

Conjugated linoleic acid (CLA; 9c,11t-18:2), present in dairy products and beef, has been reported in animals to have anticarcinogenic, growth-promoting, antiatherogenic, anti-diabetic, and lean body mass-enhancing properties. Silver ion chromatography has, over the decades, become an important met...


Application of Ion Pairing Chromatography to the Analysis of Inorganic Analytes: Review  

Microsoft Academic Search

The separation challenges that keep arising from the constantly evolving practical applications encountered in ion?pair chromatography (IPC) of inorganic analytes and inorganic elements containing compounds are reviewed. Emphasis is placed on species that are most important in the biochemical, biomedical areas or that are of concern in the environmental field. Examples will be given of the analysis and speciation of

Teresa Cecchi



Suppressed ion chromatography for monitoring chemical impurities in steam for geothermal power plants  

Microsoft Academic Search

A suppressed ion chromatography (IC) technique has been evaluated as a chemical monitoring tool for detecting major anions (F?, Cl?, NO3? and SO42?) of condensed steam in geothermal power plants. It is shown that the suppressed IC technique provides a suitable means for preventing possible damage to generating equipment in the geothermal industry. An electrical conductivity detector (0.1 ?S sensitivity)

E Santoyo; S. P Verma; F Sandoval; A Aparicio; R Garc??a




NSDL National Science Digital Library

In this chemistry activity, learners will separate a mixture of FD&C dyes (colors certified and allowed by the US for the Food, Pharmaceutical, Cosmetics & Personal Care industry) to practice chromatography, a separation technique for mixtures. Learners will record their observations on a data table and note trends. This resource includes questions for learners and instructions for preparing the colors from M&Ms, Orange Kool-Aid, and food coloring.

The Science House



Analysis of anions in geological brines using ion chromatography  

SciTech Connect

Ion chromatographic procedures for the determination of the anions bromide, sulfate, nitrite, nitrate, phosphate, and iodide in brine samples have been developed and are described. The techniques have been applied to the analysis of natural brines, and geologic evaporites. Sample matrices varied over a range from 15,000 mg/L to 200,000 mg/L total halogens, nearly all of which is chloride. The analyzed anion concentrations ranged from less than 5 mg/L in the cases of nitrite, nitrate, and phosphate, to 20,000 mg/L in the case of sulfate. A technique for suppressing chloride and sulfate ions to facilitate the analysis of lower concentration anions is presented. Analysis times are typically less than 20 minutes for each procedure and the ion chromatographic results compare well with those obtained using more time consuming classical chemical analyses. 10 references, 14 figures.

Merrill, R.M.



Separation of vanadium isotopes by ion-exchange chromatography.  


Cation-exchange displacement chromatography of VO2+ was carried out for studying vanadium isotope effects in carboxylate ligand-exchange systems. The heavier isotope 51V was enriched in the carboxylate complex solution. The isotope separation coefficients epsilon(= alpha-1) for 50V/51V were 2.2 x 10(-4) and 2.4 x 10(-4) for citrate and lactate systems at 298 K, respectively. These values are much larger than those obtained in a previous study on the malate system. The existence of binuclear complexes of VO2+ may create the conditions for larger isotope fractionation. From the viewpoint of the process development of isotope separation, the heights equivalent to a theoretical plate of these processes were analyzed and found to be very small in each system due to the homogeneous, small and highly porous resin used. Citrate may be better than the other tested systems for the vanadium isotope separation. PMID:12641293

Zhang, Yong-Hong; Nomura, Masao; Aida, Masao; Fujii, Yasuhiko



Continuous separation of carbohydrates by ion-exchange chromatography  

SciTech Connect

A synthetic mixture of fructose, mannitol and sorbitol was continuously separated by a chromatographic method using a cation-exchange resin (Dowex 50W-X8) in its Ca{sup 2+}-form as the stationary phase. An annular chromatograph (AC) was used to achieve a continuous mode of operation. Distribution and mass transfer coefficients of the three substances as well as bed properties were obtained by batch chromatography. The separation was simulated mathematically in terms of an approximate linear chromatographic theory was applied to the modeling of the behavior of the continuous separations. The influence of rotation rate, column loading, eluent flow rate and feed concentration on the resolution of the individual peaks were investigated.

Wolfgang, J.; Prior, A. [Prior Technology, Goetzis (Australia); Bart, H.J.; Messenboeck, R.C. [Univ. Kaiserslautern (Germany); Byers, C.H. [Oak Ridge National Lab., TN (United States)




Technology Transfer Automated Retrieval System (TEKTRAN)

The ion chromatographic method for the quantification of phytate (InsP6) in foods was adapted for the analysis of roots and tubers. To maximize sensitivity, UV detection following post-column derivatization was compared with evaporative light scattering detection (ELSD). Detection limits for phyta...


Chromatographic properties of the ion-exclusion column IonPac ICE-AS6 and its application in environmental analysis, Part II: application in environmental analysis  


Biological processes, geochemical reactions, anthropogenic emissions, and transformation reactions of xenobiotics are responsible for the widespread occurrence of aliphatic carboxylic acids in the environment. To study the performance of the ion-exclusion chromatography column IonPac ICE-AS6 in the analysis of environmental and environmental-technical samples, organic acids are investigated in composting seepage, silage effluents, aqueous extracts of sewage sludge, molasses hydrolysate, and alkaline cellulose hydrolysates. With respect to the diverse sample matrix and composition, different chromatographic conditions are applied. It is possible to determine various volatile fatty acids, dicarboxylic acids, (poly)hydroxy acids, and keto acids as main and trace components in samples with very high and low dissolved organic carbon content. Low baseline noise allows the determination of malic and succinic acid in the concentration range of approximately 1 microM/L in the presence of higher concentrations of fully ionized compounds. The applicability of the column in environmental analysis may be limited by the poor retardation of strong organic acids, insufficient separation of some relevant substance combinations (i.e., citric and isocitric acid), and very strong hydrophobic interactions with straight-chain monocarboxylic acids containing four or more carbon atoms. PMID:11011725

Fischer; Kotalik; Kettrup



Extra-column dispersion of macromolecular solutes in aqueous-phase size-exclusion chromatography.  


A set of dextran standards was used to study the extra-column dispersion in conventional chromatographic equipment at a broad range of molecular weights, different mobile phase flow rates and connecting tube lengths and diameters. All known correlations for the tube dispersion at laminar flow, including those for short tubes, overestimated the values of the variance of the outlet concentration signal. The difference increased with the solute molecular weight and the flow rate. It was assumed that the discrepancy was due to the effect of natural convection invoked by the density differences of the injected dextran solutions and water. A suitable approximation of the relative band spreading was suggested in a form of a power function of the Reynolds and Schmidt numbers. A significant decrease of the dispersion was observed when the chromatography tubing was coiled into a circle. This decrease was successfully predicted combining the existing correlations for long coiled tubes and short straight tubes. PMID:15248423

Grznárová, G; Polakovic, M; Acai, P; Görner, T



Size-exclusion high-performance liquid chromatography in analysis of protein and peptide epitopes.  


Size-exclusion HPLC provides direct observation of antibody-antigen interactions in free solution without chemical modification of either component. HPLC data collection systems are now a routine resource in both academic and industrial research laboratories. Monoclonal antibodies are, in principle, homogeneous reagents whose interactions with epitope are suitable for unambiguous quantitative characterization. HPLC-based methods, therefore, have the potential to contribute significantly to efficient quantitative characterization of monoclonal antibodies in studies directed to the fundamental physiological roles of these molecules as well as to the optimized selection and quality control of these reagents in biotechnical applications such as represented by the immunodiagnostic industry. In many cases, HPLC-based methods may represent the simplest and most rapid approach for evaluation of relative epitope specificities and affinity/kinetic characteristics of interaction. PMID:2481206

Stevens, F J



Effect of Buffers on Aqueous Solute-Exclusion Zones around Ion-Exchange Resins  

PubMed Central

Interaction between charged surfaces in aqueous solution is a fundamental feature of colloid science. Theoretically, surface potential falls to half its value at a distance equal to a Debye length, which is typically on the order of tens to hundreds of nanometers. This potential prevents colloids from aggregating. On the other hand, long-range surface effects have been frequently reported. Here we report additional long-range effects. We find that charged latex particles in buffer solutions are uniformly excluded from several-hundred-micron-thick shells surrounding ion-exchange beads. Exclusion is observed whether the beads are charged similarly or oppositely to the particles. Hence, electrostatic interactions between bead and microsphere do not cause particle exclusion. Rather, exclusion may be the consequence of water molecules re-orienting to produce a more ordered structure, which then excludes the particles. PMID:19185312

Zheng, Jian-ming; Wexler, Adam



Analysis of fluid inclusion leachates from quartz by ion chromatography  

NASA Astrophysics Data System (ADS)

20 chemical species have been detected and quantified in standard solutions using a Dionex 2000i-SP ion Chromatograph. These species are (minimum detection limits in ppb in injected sample follow each species; anions and cations listed in order of increasing retention time): F - (14), CH 3COO - (12), HCOO - (4), Cl - (6), NO -2 (9), Br -? (19), NO -3(16), HPO 2-4 (28), SO 2-4 (26), C 2O 2-4 oxalate (250), I - (20), Li + (0.5), Na +(0.7), NH +4 (0.6), K + (1.6), Rb + (3.5), Cs + (5.9), Mg 2+ (5), Ca 2+ (15) and Sr 2+ (100). A technique has been developed to clean fluid inclusion-bearing samples and obtain fluid inclusion leachates by hand crushing ~1-2 g samples under leaching solutions in an agate mortar and then separating the leachates by vacuum filtration. High-efficiency ion removal from the crushed sample is required since gas Chromatographic H 2O analyses of sample splits have been used to calculate species concentrations in fluid inclusions. Three separate crushes using different leaching solutions are required for a complete analysis. Cleaning procedures have been established for all components involved in the crush/leach procedure, and a system blank has been obtained by crush/leach analysis of heat-treated Brazilian quartz. The contact time between the leachate and the component (i.e., agate mortar) has been established as an important control on blank levels. The technique has been applied to three samples from the Tanco granitic pegmatite: the analyses show both a 'pegmatitic' and a possibly external fluid component. A combined, single sample, gas and ion Chromatographic procedure has been developed to link directly the fluid inclusion volatile and leachate data.

Der Channer, D. M.; Spooner, E. T. C.



An Empirical Formula from Ion Exchange Chromatography and Colorimetry  

NASA Astrophysics Data System (ADS)

Experimental determination of the empirical formula for sodium salicylate, Nax(C7H5O3)y, using colorimetry and cation exchange. A Beer's Law plot is prepared for salicylate using 0.0050 M salicylic acid solution. Colorimetric analysis is performed on the salicylate ion in the form of an aqueous ferric complex, which is intensely violet-red, using a simple, inexpensive colorimeter constructed from readily available electronic parts and PVC pipe. Determination of sodium content is conducted using cation exchange, using simple re-usable exchange columns, followed by titration with OH-. The procedure is involved, yet has been conducted by high school chemistry students as a lab final.

Johnson, Steven D.



Structural Evolution of Polylactide Molecular Bottlebrushes: Kinetics Study by Size Exclusion Chromatography, Small Angle Neutron Scattering and Simulations  

SciTech Connect

Structural evolution from poly(lactide) (PLA) macromonomer to resultant PLA molecular bottlebrush during ring opening metathesis polymerization (ROMP) was investigated for the first time by combining size exclusion chromatography (SEC), small-angle neutron scattering (SANS) and coarse-grained molecular dynamics (CG-MD) simulations. Multiple aliquots were collected at various reaction times during ROMP, and subsequently analyzed by SEC and SANS. The two complementary techniques enable the understanding of systematic changes in conversion, molecular weight and dispersity as well as structural details of PLA molecular bottlebrushes. CG-MD simulation not only predicts the experimental observations, but it also provides further insight into the analysis and interpretation of data obtained in SEC and SANS experiments. We find that PLA molecular bottlebrushes undergo three conformational transitions with increasing conversion (i.e., increasing the backbone length): (1) from an elongated to a globular shape due to longer side chain at lower conversion, (2) from a globular to an elongated shape at intermediate conversion caused by excluded volume of PLA side chain, and (3) the saturation of contour length at higher conversion due to chain transfer reactions.

Pickel, Deanna L [ORNL; Kilbey, II, S Michael [ORNL; Uhrig, David [ORNL; Hong, Kunlun [ORNL; Carrillo, Jan-Michael Y [ORNL; Sumpter, Bobby G [ORNL; Ahn, Suk-Kyun [ORNL; Han, Youngkyu [ORNL; Kim, Dr. Tae-Hwan [Korea Atomic Energy Research Institute; Smith, Gregory Scott [ORNL; Do, Changwoo [ORNL



Development and validation of a simple and sensitive size-exclusion chromatography method for quantitative determination of heparin in pharmaceuticals.  


Heparin is widely used as an anticoagulant for the treatment and prevention of various thrombotic diseases. However, due to its high anionic charge, heterogeneity in size distribution and high polarity, its analysis is very challenging. In this paper, a novel method based on size-exclusion chromatography (SEC) for quantitative determination of intact heparin in pharmaceuticals is presented. Analyses were performed on a BioSep-SEC-S 2000 column with Larginine solution at pH 6.5 as mobile phase and UV detection at 210 nm. The proposed method was found to be selective, linear (R2 > 0.997) over the concentration range of 3.1 to 1222 ?g mL-1, with a limit of detection of 1.0 ?g mL-1. Intraday and inter-day precision were below 5.1 % and inaccuracy expressed as bias did not exceed 6.5 %. The reported method is simple, selective, sensitive, and requires no laborious sample preparation, which makes it appropriate for routine quantitative analysis of heparin in pharmaceuticals. PMID:25781703

Matanovi?, Maja Radivojša; Grabnarm, Iztok; Grabnar, Pegi Ahlin; Roškar, Robert



Electrophoresis and size-exclusion chromatography of humic substances extracted from detritus and soils of different geneses  

NASA Astrophysics Data System (ADS)

Electrophoresis in 10% polyacrylamide gel in the presence of denaturants and size-exclusion chromatography in Sephadex G-75 in 7 M urea were used for the comparative analysis of humic substances isolated from a typical chernozem, soddy-podzolic soil, and chestnut soil and from the easily decomposable organic matter (plant detritus) contained in these soils. After the electrophoresis, the gel with naturally colored bands of humic substances was further stained with a dye specific for proteins by immersing into a solution containing Coomassie Brilliant Blue R-250 and CuSO4. The electrophoretic and chromatographic analyses showed that humic substances from the soils and the corresponding detritus fractions significantly differed in the intensity of the natural color of the electrophoretic fractions, the molecular-weight distribution, and the color of the electrophoretic fractions colored by the protein-specific dye (which was first discovered in this study). The hypothesis of Tyurin and Aleksandrova suggesting that the transformation of humus sources (plant detritus) into humic substances proceeds in the direction from the high-molecular compounds to the low-molecular compounds was experimentally confirmed.

Trubetskaya, O. E.; Trubetskoi, O. A.; Borisov, B. A.; Ganzhara, N. F.



Revisiting size-exclusion chromatography for measuring structural changes in raw and pretreated mixed hardwoods and switchgrass.  


The study of the biomass porous structure and its role in defining the accessibility of cell-wall-degrading enzymes (CWDEs) to the substrate is very important for understanding the cellulase-cellulose reaction system. Specific pore volume and specific surface area are two important measures of accessibility and a variety of methods have been used to make these measurements. For this study a size exclusion chromatography system was developed to measure specific pore volume and specific surface areas for raw and pretreated mixed-hardwood and switchgrass. Polyethylene glycol (PEG) probes of known molecular diameter (1.8-13?nm) were allowed to diffuse into the pore structure of the various biomass substrate packed in the column and subsequently eluted to generate high resolution concentration measurements with excellent reproducibility. Replicate measurements of probe concentrations from this system consistently yielded coefficient of variance of less than 1.5%. Our results showed that particle size reduction had a smaller influence on the specific pore volume distribution of raw mixed-hardwoods, whereas for switchgrass the larger particles yielded a significantly lower estimate for the pore volume distribution compared to the smaller particles. Our results also clearly showed that our bi-phasic pretreatment yielded the largest increase in pore volume accessibility for mixed-hardwoods relative to switchgrass. From these results a pore size change mechanism was proposed that could explain the influence of size reduction and pretreatment on pore volume measurements. PMID:25212985

Yang, Dong; Parlange, Jean-Yves; Walker, Larry P



Characterization of small protein aggregates and oligomers using size exclusion chromatography with online detection by native electrospray ionization mass spectrometry.  


Self-association of proteins is important in a variety of processes ranging from acquisition of native quaternary structure (where the association is tightly controlled and proceeds in a highly ordered fashion) to aggregation and amyloidosis. The latter is frequently accompanied (or indeed triggered) by the loss of the native structure, but a clear understanding of the complex relationship between conformational changes and protein self-association/aggregation remains elusive due to the great difficulty in characterizing these complex and frequently heterogeneous species. In this study, size exclusion chromatography (SEC) was used in combination with online detection by native electrospray ionization mass spectrometry (ESI MS) to characterize a commercial protein sample (serum albumin) that forms small aggregates. Although noncovalent dimers and trimers of this protein are readily detected by native ESI MS alone, combination of SEC and ESI MS allows a distinction to be made between the oligomers present in solution and those formed during the ESI process (artifacts of ESI MS). Additionally, native ESI MS detection allows a partial loss of conformation integrity to be detected across all albumin species present in solution. Finally, ESI MS detection allows these analyses to be carried out readily even in the presence of other abundant proteins coeluting with albumin. Native ESI MS as an online detection method for SEC also enables meaningful characterization of species representing different quaternary organization of a recombinant glycoprotein human arylsulfatase A even when their rapid interconversion prevents their separation on the SEC time scale. PMID:25310183

Muneeruddin, Khaja; Thomas, John J; Salinas, Paul A; Kaltashov, Igor A



A hemagglutinin quantification method for development of an influenza pandemic vaccine using size exclusion high performance liquid chromatography.  


Single radial immunodiffusion (SRID) assay requires a reference antigen and an antibody to the hemagglutinin (HA) of an influenza vaccine. As it takes 2?3 months to develop the reference antigen, vaccine development is delayed in cases of an influenza pandemic. In the present study, the measurement of the HA content of influenza vaccines was assessed using size exclusion high performance liquid chromatography (SE?HPLC) for the rapid development of a pandemic vaccine. When the 2009 H1N1 reference antigen, pandemic 2009 H1N1 vaccine and 2010 seasonal influenza vaccines were analyzed by SE?HPLC, the HA of the reference antigen and vaccines was specifically separated. The presence and specificity of HA were evidenced with immunoprecipitation and ELISA assays. For the influenza vaccines, the chromatogram pattern and retention time of HA were similar among the antigen types (2009 H1N1, 2010 H3N2 and 2010 B). In addition, when SE?HPLC was applied, the ratio of HA chromatogram to peak area revealed a significant correlation with HA concentration for the reference antigen and vaccine. The result of the HA content calculation based on SE?HPLC exhibited 99.91?100% similarity, compared with that of SRID. These findings suggest that the measurement of peak area ratio/HA content using SE?HPLC may be a substitute for SRID and rapidly measure HA content to enable faster development of a vaccine during an influenza pandemic. PMID:25482872

Roh, Hang Sik; Song, Hye Min; Yun, Bo Reum; Kang, Hyun Kyung; Choi, Keum Suk; Park, Yun Ju; Kim, Dong Sub; Kim, Seung Hee; Mo, In Pil; An, Beum-Soo; Ahn, Chi Young



High-pressure size exclusion chromatography analysis of dissolved organic matter isolated by tangential-flow ultra filtration  

USGS Publications Warehouse

A 1,000-Dalton tangential-flow ultrafiltration (TFUF) membrane was used to isolate dissolved organic matter (DOM) from several freshwater environments. The TFUF unit used in this study was able to completely retain a polystyrene sulfonate 1,800-Dalton standard. Unaltered and TFUF-fractionated DOM molecular weights were assayed by high-pressure size exclusion chromatography (HPSEC). The weight-averaged molecular weights of the retentates were larger than those of the raw water samples, whereas the filtrates were all significantly smaller and approximately the same size or smaller than the manufacturer-specified pore size of the membrane. Moreover, at 280 nm the molar absorptivity of the DOM retained by the ultrafilter is significantly larger than the material in the filtrate. This observation suggests that most of the chromophoric components are associated with the higher molecular weight fraction of the DOM pool. Multivalent metals in the aqueous matrix also affected the molecular weights of the DOM molecules. Typically, proton-exchanged DOM retentates were smaller than untreated samples. This TFUF system appears to be an effective means of isolating aquatic DOM by size, but the ultimate size of the retentates may be affected by the presence of metals and by configurational properties unique to the DOM phase.

Everett, C.R.; Chin, Y.-P.; Aiken, G.R.



Use of ion chromatography–electrospray mass spectrometry for the determination of ionic compounds in agricultural chemicals  

Microsoft Academic Search

This paper reports the use of ion chromatography–electrospray mass spectrometry for the separation and structure elucidation of anionic compounds in a complex organophosphate matrix. Conventional HPLC with ion pairing reagents, pH adjustments or use of buffer solutions have limited compatibility with mass spectrometry, as the ion pairing reagents or buffers have to be volatile to be introduced into the mass

Sheher Bano Mohsin



Fabricating electrospun cellulose nanofibre adsorbents for ion-exchange chromatography.  


Protein separation is an integral step in biopharmaceutical manufacture with diffusion-limited packed bed chromatography remaining the default choice for industry. Rapid bind-elute separation using convective mass transfer media offers advantages in productivity by operating at high flowrates. Electrospun nanofibre adsorbents are a non-woven fibre matrix of high surface area and porosity previously investigated as a bioseparation medium. The effects of compression and bed layers, and subsequent heat treatment after electrospinning cellulose acetate nanofibres were investigated using diethylaminoethyl (DEAE) or carboxylate (COO) functionalisations. Transbed pressures were measured and compared by compression load, COO adsorbents were 30%, 70% and 90% higher than DEAE for compressions 1, 5 and 10MPa, respectively, which was attributed to the swelling effect of hydrophilic COO groups. Dynamic binding capacities (DBCs) at 10% breakthrough were measured between 2000 and 12,000CV/h (2s and 0.3s residence times) under normal binding conditions, and DBCs increased with reactant concentration from 4 to 12mgBSA/mL for DEAE and from 10 to 21mglysozyme/mL for COO adsorbents. Comparing capacities of compression loads applied after electrospinning showed that the lowest load tested, 1MPa, yielded the highest DBCs for DEAE and COO adsorbents at 20mgBSA/mL and 27mglysozyme/mL, respectively. At 1MPa, DBCs were the highest for the lowest flowrate tested but stabilised for flowrates above 2000CV/h. For compression loads of 5MPa and 10MPa, adsorbents recorded lower DBCs than 1MPa as a result of nanofibre packing and reduced surface area. Increasing the number of bed layers from 4 to 12 showed decreasing DBCs for both adsorbents. Tensile strengths were recorded to indicate the mechanical robustness of the adsorbent and be related to packing the nanofibre adsorbents in large scale configurations such as pleated cartridges. Compared with an uncompressed adsorbent, compressions of 1, 5 and 10MPa showed increases of 30%, 110% and 110%, respectively, for both functionalisations. The data presented show that capacity and mechanical strength can be balanced through compression after electrospinning and is particular to different functionalisations. This trade-off is critical to the development of nanofibre adsorbents into different packing configurations for application and scale up in bioseparation. PMID:25541092

Dods, Stewart R; Hardick, Oliver; Stevens, Bob; Bracewell, Daniel G



Determination of chlorine and bromine in automotive shredder residues by oxygen bomb and ion chromatography.  


An analytical procedure, oxygen bomb combustion-ion chromatography (IC), has been developed for the determination of total chlorine in Automotive Shredder Residues (ASR). Samples of these residues are fired under elevated oxygen pressure (30 atm) and the combustion products are transferred into a Na2CO3/NaHCO3 absorbent solution containing 1% of H2O2; the chlorine contents are then evaluated by ion chromatography. The use of the non-suppressed IC determination with a conductivity detector provides a rapid, sensitive and selective method for chlorine determination in ASR, allowing determinations of this heteroatom at levels below 1% in the presence of bromine and sulfur. Moreover, the proposed method allows the simultaneous determination of chlorine, bromine and sulfur which are potential environmental hazards. PMID:12152898

Cortés-Peña, M A; Pérez-Arribas, L V; León-González, M E; Polo-Díez, L M



Application of size exclusion chromatography with surfactant eluent to the study of polymer–surfactant interactions: oligomeric and micellar chromatographic effects  

Microsoft Academic Search

Complexation of sodium dodecyl sulphate (SDS) with a wide range of molecular weights of poly(ethylene glycol) (PEG) and poly(ethylene oxide) (PEO) has been studied by size exclusion chromatography using aqueous SDS eluent. A multi-angle laser light scattering detector and a differential refractometer were applied to give direct measurement of the molecular weight of complexes without reference to elution volume, since

Andrew P. Rodenhiser; Jan C. T. Kwak



Determination of molecular weight of polyethylene glycol using size-exclusion chromatography with multi-angle laser light scattering and acid–base titration  

Microsoft Academic Search

Size-exclusion chromatography with multi-angle laser light scattering (SEC-MALLS) and acid–base titration were used to determine the molecular weight of a polyethylene glycol with low molecular weight. All potential uncertainty factors for each measurement were evaluated using cause-effect diagrams. Weight analysis was applied to harmonize the two different measurement results. It was found that the main uncertainty sources of SEC-MALLS measurement

Guangwen Cheng; Xiaodong Fan; Guotao Liu; Yuyang Liu



Utilisation d'anticorps spécifiques d'une fraction obtenue par chromatographie d'exclusion pour une amélioration de la caractérisation sérologique de Rhizoctonia solani Kühn AG3  

Microsoft Academic Search

La purification d'un extrait mycélien soluble d'une souche deR. solani AG3 par chromatographie d'exclusion permet de recueillir une fraction antigénique. Une lapine est immunisée par voie intradermique. L'immunsérum titre 0,125 par la technique de double-diffusion en agarose. Différentes techniques sérologiques (immunodiffusion, électrotransfert suivi de révélation des fractions antigéniques, coloration immunoenzymatique du mycélium) sont appliquées à des souches deR. solani AG1,

Sylvie Le Coz-Gillet; Lucien Hingand



Determination of pyrethroid pesticide residues in fatty materials by solid-matrix dispersion partition, followed by mini-column size-exclusion chromatography  

Microsoft Academic Search

The method studied uses a combination of a solid-matrix dispersion partition (SMDP) followed by high-performance size-exclusion chromatography on a minicolumn (HPmSEC) of 7.8 mm I.D. for the separation of pyrethroid (PYR) residues from fatty material. The solid-matrix dispersion extraction is carried out by absorbing a fat solution onto an Extrelut-3 cartridge (filled with a macroporous diatomaceous material) and extracting the

Alfonso Di Muccio; Patrizia Pelosi; Danilo Attard Barbini; Tiziana Generali; Silvana Girolimetti; Patrizia Stefanelli; Antonio Leonelli; Graziella Amendola; Luciano Vergori



Improved separation of conjugated fatty acid methyl esters by silver ion-high-performance liquid chromatography  

Microsoft Academic Search

Operating from one to six silver ion-high-performance liquid chromatography (Ag+-HPLC) columns in series progressively improved the resolution of the methyl esters of conjugated linoleic acid (CLA) isomeric\\u000a mixtures from natural and commercial products. In natural products, the 8 trans, 10 cis-octadecadienoic (18?2) acid was resolved from the more abundant 7 trans, 9 cis-18?2, and the 10 trans, 12 cis-18?2 was

Najibullah Sehat; Rainer Rickert; Magdi M. Mossoba; John K. G. Kramer; Martin P. Yurawecz; John A. G. Roach; Richard O. Adlof; Kim M. Morehouse; Jan Fritsche; Klaus D. Eulitz; Hans Steinhart; Yuoh Ku



Hair analysis for nordiazepam and oxazepam by gas chromatography-negative-ion chemical ionization mass spectrometry  

Microsoft Academic Search

A procedure is presented for the identification of nordiazepam and its metabolite, oxazepam, in human hair. The method involves decontamination of hair with dichloromethane, incubation in phosphate buffer (pH 7.6) in the presence of deuterated internal standards, liquid-liquid extraction, derivatization with N,O-bis(trimethylsilyl)trifluoroacetamide plus 1% trimethylchlorosilane and gas chromatography-mass spectrometry using negative-ion chemical ionization with methane. Among thirty samples obtained from

Pascal Kintz; Vincent Cirimele; François Vayssette; Patrice Mangin



Investigating effects of sample pretreatment on protein stability using size-exclusion chromatography and high-resolution continuum source atomic absorption spectrometry.  


In this study, size-exclusion chromatography and high-resolution atomic absorption spectrometry methods have been developed and evaluated to test the stability of proteins during sample pretreatment. This especially includes different storage conditions but also adsorption before or even during the chromatographic process. For the development of the size exclusion method, a Biosep S3000 5 ?m column was used for investigating a series of representative model proteins, namely bovine serum albumin, ovalbumin, monoclonal immunoglobulin G antibody, and myoglobin. Ambient temperature storage was found to be harmful to all model proteins, whereas short-term storage up to 14 days could be done in an ordinary refrigerator. Freezing the protein solutions was always complicated and had to be evaluated for each protein in the corresponding solvent. To keep the proteins in their native state a gentle freezing temperature should be chosen, hence liquid nitrogen should be avoided. Furthermore, a high-resolution continuum source atomic absorption spectrometry method was developed to observe the adsorption of proteins on container material and chromatographic columns. Adsorption to any container led to a sample loss and lowered the recovery rates. During the pretreatment and high-performance size-exclusion chromatography, adsorption caused sample losses of up to 33%. PMID:24964383

Rakow, Tobias; El Deeb, Sami; Hahne, Thomas; El-Hady, Deia Abd; AlBishri, Hassan M; Wätzig, Hermann



Influence of soil type and extraction conditions on perchlorate analysis by ion chromatography.  


Perchlorate is a stable anion that has been introduced into the environment through activities related to its production and use as a solid rocket propellant. Perchlorate is thought to transport through soils without being adsorbed; thus, for determination of perchlorate in soil, samples are typically extracted with water prior to analysis. The completeness of extraction depends on perchlorate existing as a free ion within the soil matrix. In this study, perchlorate extraction efficiency was evaluated with five soil types under two different oxygen states. For each soil, 30% (w/w) slurries were prepared and equilibrated under either oxic or anoxic conditions prior to spiking with a stock solution of sodium perchlorate, and the slurries were then maintained for 1-week or 1-month. At the end of the exposure, slurries were centrifuged and separated into aqueous and soil phases. After phase separation, the soil was washed first with deionized water and then with 50mM NaOH, producing second and third aqueous phases, respectively. Perchlorate concentrations in the three aqueous phases were determined using ion chromatography. The results obtained from this study suggest that matrix interference and signal suppression due to high conductivity have greater effects upon observed perchlorate concentrations by ion chromatography than does perchlorate interaction with soil. Thus, a single water extraction is sufficient for quantitative determination of perchlorate in soil. PMID:17092539

MacMillan, Denise K; Dalton, Shana R; Bednar, Anthony J; Waisner, Scott A; Arora, Prem N



Method for the determination of dissolved chloride, nitrate, and sulfate in natural water using ion chromatography  

USGS Publications Warehouse

Ion chromatography was used for the determination of dissolved chloride, nitrate and sulfate in natural water where concentrations ranged from a detection limit of 0.02 milligrams per liter to 80 milligrams per liter for chloride, to 18 milligrams per liter for nitrate, and to 280 milligrams per liter for sulfate. Specific conductance was the mode of detection used. Three analytical sample size loops of 11, 61, and 250 microliters, were used to include the analytical ranges described. U.S. Geological Survey Standard Reference Water Samples were analyzed to test the precision and accuracy of the analyses.

Brinton, Terry I.; Antweiler, Ronald C.; Taylor, Howard E.



The glycolate and 2-phosphoglycolate content of tissues measured by ion chromatography coupled to mass spectrometry  

PubMed Central

Glycolate and 2-phosphoglycolate (PG) are 2-carbon monocarboxylic acids with ill-defined metabolic roles. Their concentrati ons have not yet been described in tissues apart from body fluids and erythrocytes. We describe the use of ion chromatography coupled with mass spectrometry (IC-MS) to quantify levels of glycolate and PG in tissue. Sample preparation and analysis can be performed within an hour. Low concentrations of glycolate (12 – 48 nmoles/g) and PG (4 – 17 nmoles/g) were detected in all tissues. The availability of this IC-MS assay will facilitate investigations of the origin, function, and metabolism of glycolate and PG in tissues. PMID:22093610

Knight, John; Hinsdale, Mark; Holmes, Ross



Ion Exchange Chromatography and Mass Spectrometric Methods for Analysis of Cadmium-Phytochelatin (II) Complexes  

PubMed Central

In this study, in vitro formed Cd-phytochelatin (PC2) complexes were characterized using ion exchange chromatography (IEC) and matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry. The ratio of both studied compounds as well as experimental conditions were optimized. The highest yield of the complex was observed under an applied concentration of 100 µg·mL?1 PC2 and 100 µg·mL?1 of CdCl2. The data obtained show that IEC in combination with MALDI-TOF is a reliable and fast method for the determination of these complexes. PMID:23538727

Merlos Rodrigo, Miguel Angel; Cernei, Natalia; Kominkova, Marketa; Zitka, Ondrej; Beklova, Miroslava; Zehnalek, Josef; Kizek, Rene; Adam, Vojtech



Insights Into Water-Soluble Organic Aerosol Sources From Carbon-13 Ratios of Size Exclusion Chromatography Fractions  

NASA Astrophysics Data System (ADS)

Many sources of organic aerosols have been identified and quantified, and much of this work has used individual (mosty water-insoluble) compounds as tracers of primary sources. However, most organic aerosol cannot be molecularly characterized, and the water-soluble organic carbon (WSOC) in many aerosols is thought to originate from gaseous precursors (i.e., it is secondary in nature). It can therefore be difficult to infer aerosol sources, particularly of background (i.e., aged) aerosols, and of the relatively high-MW component of aerosols. The stable isotope ratios (?13C) of organic aerosols have been used to distinguish between sources, with lighter values (-30‰ to -25‰) interpreted as having originated from fossil fuel combustion and C4 biogenic emission, and heavier values (-25‰ to - 20‰) indicating a marine or C3 biogenic source. Most published measurements were of either total suspended particulates or PM2.5, however, and it is unknown to what extent these fractions differ from submicron WSOC. We report ?13C for submicron WSOC collected at a variety of sites, ranging from marine to polluted to background continental. Bulk marine organic ?13C ranged from -30.4 to - 27.6‰, slightly lighter than previously published results. This could be due to the elimination of supermicron cellular material or other biogenic primary emissions from the sample. Continental WSOC ?13C ranged from -19.1 to -29.8‰, with heavier values (-19.8 ± 1.0‰) in Oklahoma and lighter values at Great Smoky Mountain National Park in Tennessee (-25.8 ± 2.6‰) and Illinois (-24.5 ± 1.0‰). This likely results from the greater proportional of C3 plant material in the Oklahoma samples. In addition to bulk samples, we used size exclusion chromatography (SEC) to report ?13C of organic aerosols as a function of hydrodynamic diameter. Variability and magnitude of hydrodynamic diameter was greatest at low SEC pH, indicative of the acidic character of submicron WSOC. Tennessee aerosols included neutral compounds not observed at other sites, and in general showed more variability in both hydrodynamic diameter and ?13C. This suggests that secondary formation processes were most active at this site.

Ruehl, C. R.; Chuang, P. Y.; McCarthy, M. D.



Size Exclusion Chromatography Studies of the Initial Self-Association Steps of Chicken Egg White Lysozyme Nucleation  

NASA Technical Reports Server (NTRS)

Nucleation is one of the least understood aspects of crystallogenesis. In the case of macromolecule nucleation, this understanding is further hampered by uncertainty over what precisely is being discussed. We define the process of solute self-association (aggregation, oligomerization, interaction, clustering, etc.) whereby n-mers (n > or = 2) having a crystallographic or nascent crystallographic arrangement leading to the critical nucleus reversibly form in the solution, to be part of the nucleation process. This reversible self-association process is a fundamental part of the nucleation process, and occurs as a function of the solute concentration. In the case of chicken egg white lysozyme, a considerable body of experimental evidence leads us to the conclusion that it also forms the crystal growth units. Size exclusion chromatography is a simple and direct method for determining the equilibrium constants for the self-association process. A Pharmacia FPLC system was used to provide accurate solution flow rates. The column, injection valve, and sample loop were all mounted within a temperature-controlled chamber. Chromatographically re-purified lysozyme was first dialyzed against the column equilibration buffer, with injection onto the column after several hours pre-incubation at the running temperature. Preliminary experiments, were carried out using a Toyopearl HW-50F column (1 x 50cm), equilibrated with 0.1 M sodium acetate, 5% sodium chloride, pH 4.6, at 15C. Protein concentrations from 0.1 to 4 mg/ml were employed (C(sub sat) = 1.2 mg/ml). The data from several different protein preparations consistently shows a progressively decreasing elution volume with increasing protein concentration, indicating that reversible self-association is occurring. The dotted line indicates the monomeric lysozyme elution volume. However, lysozyme interacts with the column matrix in these experiments, which complicates data analysis.Accordingly, we are testing silica-based HPLC columns in an effort to eliminate this problem and substantially reduce the column volume and experimental run time. The results and data analysis from these and subsequent experiments will be presented.

Ewing, Felecia; Donovan, David; Pusey, Marc



Portable, fully autonomous, ion chromatography system for on-site analyses.  


The basic operating principles of a portable, fully autonomous, ion chromatography system are described. The system affords the user the ability to collect and analyze samples continuously for 27 days, or about 1930 injections before needing any user intervention. Within the 13 kg system, is a fully computer controlled autosampling, chromatography and data acquisition system. An eluent reflux device (ERD), which integrates eluent suppression and generation in a single multi-chambered device, is used to minimize eluent consumption. During operation, about 1 ?L of water per minute is lost to waste while operating standard-bore chromatography at 0.5 mL min(-1) due to eluent refluxing. Over the course of 27 days, about 100mL of rinse water is consumed, effectively eliminating waste production. Data showing the reproducibility (below 1% relative standard deviation over 14 days) of the device is also presented. Chromatographic analyses of common anions (Cl(-), NO3(-), SO4(2-), PO4(3-)), is accomplished in under 15 min using a low backpressure guard column with ? 25 mM KOH isocratic elution. For detection, a small capacitively-coupled contactless conductivity detector (C4D) is employed, able to report analytes in the sub to low micromolar range. Preconcentration of the injected samples gives a 50-fold decrease in detection limits, primarily utilized for in-situ detection of phosphate (LOQ 10 ?g L(-1)). Field analyses are shown for multiple on-site analyses of stream water indifferent weather conditions. PMID:24913366

Elkin, Kyle R



Suppressed ion chromatography for monitoring chemical impurities in steam for geothermal power plants.  


A suppressed ion chromatography (IC) technique has been evaluated as a chemical monitoring tool for detecting major anions (F-, Cl-, NO3- and SO4(2-)) of condensed steam in geothermal power plants. It is shown that the suppressed IC technique provides a suitable means for preventing possible damage to generating equipment in the geothermal industry. An electrical conductivity detector (0.1 microS sensitivity) with an anion-exchange column (IonPac AS4A-SC), a micro-membrane suppressor (AMMS II), and an isocratic high-pressure pump system were successfully used for detecting low concentrations of inorganic anions. Method detection limits for the anions of interest were <0.184 mg/L. Details of the IC methodology as well as some experimental results obtained during its application for the chemical monitoring of geothermal steam pipes are also described. PMID:11999745

Santoyo, E; Verma, S P; Sandoval, F; Aparicio, A; García, R



Determination of anionic surfactants during wastewater recycling process by ion pair chromatography with suppressed conductivity detection  

NASA Technical Reports Server (NTRS)

A direct approach utilizing ion pairing reversed-phase chromatography coupled with suppressed conductivity detection was developed to monitor biodegradation of anionic surfactants during wastewater recycling through hydroponic plant growth systems and fixed-film bioreactors. Samples of hydroponic nutrient solution and bioreactor effluent with high concentrations (up to 120 mS electrical conductance) of inorganic ions can be analyzed without pretreatment or interference. The presence of non-ionic surfactants did not significantly affect the analysis. Dynamic linear ranges for tested surfactants [Igepon TC-42, ammonium lauryl sulfate, sodium laureth sulfate and sodium alkyl (C10-C16) ether sulfate] were 2 to approximately 500, 1 to approximately 500, 2.5 to approximately 550 and 3.0 to approximately 630 microg/ml, respectively.

Levine, L. H.; Judkins, J. E.; Garland, J. L.; Sager, J. C. (Principal Investigator)



The removal of uranium from acidic media using ion exchange and/or extraction chromatography  

SciTech Connect

The separation and purification of uranium from either nitric acid or hydrochloric acid media can be accomplished by using either solvent extraction or ion-exchange. Over the past two years at Los Alamos, emerging programs are focused on recapturing the expertise required to do limited, small-quantity processing of enriched uranium. During this period of time, we have been investigating ion-addition, waste stream polishing is associated with this effort in order to achieve more complete removal of uranium prior to recycle of the acid. Extraction chromatography has been demonstrated to further polish the uranium from both nitric and hydrochloric acid media thus allowing for a more complete recovery of the actinide material and creation of less waste during the processing steps.

FitzPatrick, J.R.; Schake, B.S.; Murphy, J.; Holmes, K; West, M.H.



Selected ion monitoring gas chromatography\\/mass spectrometry of 1,2-diacylglycerol tert -butyldimethylsilyl ethers derived from glycerophospholipids  

Microsoft Academic Search

Selected ion monitoring was used in conjunction with gas chromatography\\/mass spectrometry to analyzetert-butyldimethylsilyl ethers (tert-BDMS) of 1,2-diacyl-sn-glycerols derived from naturally occurring glycerophospholipids, including those ofEscherichia coli, soybean, egg yolks and porcine liver. First, the fatty acid composition of the unknown glycerophospholipid was determined\\u000a by gasliquid chromatography (GLC) and, based on that, the fatty acids (mostly >0.5 wt%) were selected for

Toshiaki Ohshima; Chiaki Koizumi



Plant lipidomics based on hydrophilic interaction chromatography coupled to ion trap time-of-flight mass spectrometry  

Microsoft Academic Search

Plants synthesize a wide range of hydrophobic compounds, generally known as lipids. Here, we report an application of liquid\\u000a chromatography ion trap time-of-flight mass spectrometry (LC-IT-TOF-MS) for plant lipidomics. Using hydrophilic interaction\\u000a chromatography (HILIC) for class separation, typical membrane lipids including glycerolipids, steryl glucosides and glucosylceramides,\\u000a and hydrophobic plant secondary metabolites such as saponins were analyzed simultaneously. By this method,

Yozo Okazaki; Yukiko Kamide; Masami Yokota Hirai; Kazuki Saito


Determination of indole-3-pyruvic acid levels in Arabidopsis thaliana by gas chromatography–selected ion monitoring-mass spectrometry  

Microsoft Academic Search

A rapid and simple method is described for the determination of indole-3-pyruvic acid (IPA) levels in Arabidopsis thaliana by gas chromatography–selected ion monitoring-mass spectrometry (GC–SIM-MS). The method includes derivatization of IPA with hydroxylamine in the crude extract, followed by ethyl acetate partitioning, solid-phase extraction with C18 resin, reversed-phase high-performance liquid chromatography (HPLC), and GC–SIM-MS. Three derivatizing reagents were tested; these

Yuen Yee Tam; Jennifer Normanly



Determination of perchlorate in infant formula by isotope dilution ion chromatography/tandem mass spectrometry  

PubMed Central

A sensitive and selective isotope dilution ion chromatography/tandem mass spectrometry (ID IC-MS/MS) method was developed and validated for the determination of perchlorate in infant formula. The perchlorate was extracted from infant formula by using 20 ml of methanol and 5 ml of 1% acetic acid. All samples were spiked with 18O4 isotope-labelled perchlorate internal standard prior to extraction. After purification on a graphitised carbon solid-phase extraction column, the extracts were injected into an ion chromatography system equipped with an Ionpac AS20 column for separation of perchlorate from other anions. The presence of perchlorate in samples was quantified by isotope dilution mass spectrometry. Analysis of both perchlorate and its isotope-labelled internal standard was carried out on a Waters Quattro Ultima triple quadrupole mass spectrometer operating in a multiple reaction monitoring (MRM) negative ionisation mode. The method was validated for linearity and range, accuracy, precision, sensitivity, and matrix effects. The limit of quantification (LOQ) was 0.4 ?g 1?1 for liquid infant formula and 0.95 ?g kg?1 for powdered infant formula. The recovery ranged from 94% to 110% with an average of 98%. This method was used to analyse 39 infant formula, and perchlorate concentrations ranging from

Wang, Z.; Lau, B.P.-Y.; Tague, B.; Sparling, M.; Forsyth, D.



Effect of injection matrix concentration on peak shape and separation efficiency in ion chromatography.  


In HPLC, injection of solvents that differ from the eluent can result in peak broadening due to solvent strength mismatch or viscous fingering. Broadened, distorted or even split analyte peaks may result. Past studies of this injection-induced peak distortion in reversed phase (RPLC) and hydrophilic interaction (HILIC) liquid chromatography have led to the conclusion that the sample should be injected in the eluent or a weaker solvent. However, there have been no studies of injection-induced peak distortion in ion chromatography (IC). To address this, injection-induced effects were studied for six inorganic anions (F-, Cl-, NO2-, Br-, NO3- and SO4(2-)) on a Dionex AS23 IC column using a HCO3-/CO3(2-) eluent. The VanMiddlesworth-Dorsey injection sensitivity parameter (s) showed that IC of anions has much greater tolerance to the injection matrix (HCO3-/CO3(2-) herein) mismatch than RPLC or HILIC. Even when the injection contained a ten-fold greater concentration of HCO3-/CO3(2-) than the eluent, the peak shapes and separation efficiencies of six analyte ions did not change significantly. At more than ten-fold greater matrix concentrations, analyte anions that elute near the system peak of the matrix were distorted, and in the extreme cases exhibited a small secondary peak on the analyte peak front. These studies better guide the degree of dilution needed prior to IC analysis of anions. PMID:25456596

Zhang, Ya; Lucy, Charles A



Computer-assisted multi-segment gradient optimization in ion chromatography.  


This study reports simulation and optimization of ion chromatography separations using multi-segment gradient elution. First, an analytical expression for the gradient retention factor under these complex elution profiles was derived. This allows a rapid retention time prediction calculations under different gradient conditions, during computer-assisted method development. Next, these analytical expressions were implemented in an in-house written Matlab(®) routine that searches for the optimal (multi-segment) gradient conditions, either via a four-segment grid search or via the recently proposed one-segment-per-component search, in which the slope is adjusted after the elution of each individual component. Evaluation of the retention time simulation and optimization approaches was performed on a mixture of 18 inorganic anions and different subsets with varying number of compounds. The two considered multi-segment gradient optimization searches resulted in similar proposed gradient profiles, and corresponding chromatograms. Moreover, the resultant chromatograms were clearly superior to the chromatograms obtained from the best simple linear gradient profiles, found via a fine grid search. The proposed approach is useful for automated method development in ion chromatography in which complex elution profiles are often used to increase the separation power. PMID:25596760

Tyteca, Eva; Park, Soo Hyun; Shellie, Robert A; Haddad, Paul R; Desmet, Gert



Quantitation of diethylene glycol and its metabolites by gas chromatography mass spectrometry or ion chromatography mass spectrometry in rat and human biological samples.  


The misuse of the commonly used chemical diethylene glycol (DEG) has lead to many poisonings worldwide. Methods were developed for analysis of DEG and its potential metabolites; ethylene glycol, glycolic acid, oxalic acid, diglycolic acid and hydroxyethoxy acetic acid in human urine, serum and cerebrospinal fluid samples, collected following a DEG-associated poisoning in the Republic of Panama during 2006. In addition, methods were developed for rat blood, urine, kidney and liver tissue to support toxicokinetic analysis during the conduct of DEG acute toxicity studies in the rat. Sample analysis was conducted using two techniques; ion chromatography with suppressed conductivity and negative ion electrospray ionization with MS detection or with gas chromatography using electron impact ionization or methane negative chemical ionization with MS detection. Stable-isotope-labeled analogs of each analyte were employed as quantitative internal standards in the assays. PMID:24668490

Perala, Adam W; Filary, Mark J; Bartels, Michael J; McMartin, Kenneth E



[Simultaneous analysis of iodate, iodide, bromate and bromide by ion chromatography with ultraviolet detection].  


An analytical method of ion chromatography with ultraviolet detection has been developed and applied for the simultaneous determination of iodate, iodide, bromate and bromide. The separation was performed on a quaternary ammonium type anion exchange column with citric acid and acetonitrile as mobile phase. The effects of the detection wavelength, the kind and concentration of the mobile phase and other parameters on separation and detection of the four ions were investigated. The retention rules were studied and the chromatographic conditions were optimized. Under the conditions of 210 nm as detection wavelength, 0.9 mL/min as flow rate, 40 degrees C as column temperature, and 1.0 mmol/L citric acid-acetonitrile (85:15, v/ v; pH 5.0) as mobile phase, the four ions were completely separated and the system peaks and other common anions didn't interfere with the determination. The detection limits of the four ions (S/N = 3) were 0.07-0.16 mg/L. The relative standard deviations of the retention times and peak areas obtained by determining samples five times continuously were below 1%. The spiked recoveries of the four anions were from 98.0% to 102%. This method has been successfully used to determine ionic liquids synthesized by chemistry laboratory and underground water samples. The results were accurate and reliable. PMID:24984472

Li, Meng; Yu, Hong; Zheng, Xiurong



Evaluation and Quantitation of Intact Wax Esters of Human Meibum by Gas-Liquid Chromatography-Ion Trap Mass Spectrometry  

PubMed Central

Purpose. Wax esters (WE) of human meibum are one of the largest group of meibomian lipids. Their complete characterization on the level of individual intact lipid species has not been completed yet. We obtained detailed structural information on previously uncharacterized meibomian WE. Methods. Intact WE were separated and analyzed by means of high-temperature capillary gas-liquid chromatography (GLC) in combination with low voltage (30 eV) electron ionization ion trap mass spectrometry (ITMS). 3D (mass-to-charge ratio [m/z] versus lipid sample weight versus signal intensity) calibration plots were used for quantitation of WE. Results. We demonstrated that GLC-ITMS was suitable for analyzing unpooled/underivatized WE collected from 14 individual donors. More than 100 of saturated and unsaturated WE (SWE and UWE, respectively) were detected. On average, UWE represented about 82% of the total WE pool. About 90% of UWE were based on oleic acid, while less than 10% were based on palmitoleic acid. The amounts of poly-UWE were <3% of their mono-UWA counterparts. SWE were based primarily on C16–C18 fatty acids (FA) in overall molar ratios of 22:65:13. A pool of C16:0-FA was comprised of a 20:80 (mol/mol) mixture of straight chain and iso-branched isomers, while the corresponding ratio for C18:0-FA was 43:57. Interestingly, C17:0-FA was almost exclusively branched, with anteiso- and iso-isomers found in a ratio of 93:7. Conclusions. GLC-ITMS can be used successfully to analyze more than 100 individual species of meibomian WE, which were shown to comprise 41 ± 8% (wt/wt) of meibum, which made them the largest group of lipids in meibum. PMID:22531701

Butovich, Igor A.; Arciniega, Juan C.; Lu, Hua; Molai, Mike



Determination of trace sulfides in turbid waters by gas dialysis/ion chromatography  

SciTech Connect

The accuracy of the methylene blue colorimetric procedure for the determination of sulfide in environmental waters and waste waters is influenced by turbidity interferences even after application of recommended pretreatment techniques. The direct analysis of sulfide by ion chromatography (IC), without sample pretreatment, is complicated by field preservation of samples with zinc ion (or equivalent). A continuous-flow procedure has been developed that converts the acid-extractable sulfide to H/sub 2/S, which is separated from the sample matrix by a gas dialysis membrane and then trapped in a dilute sodium hydroxide solution. A portion of this solution is injected into the ion chromatograph for analysis with an electrochemical detector. Detection limits as low as 1.9 ng/mL have been obtained. Good agreement was found between the gas dialysis/IC and methylene blue methods for nonturbid standards. The addition of ascorbic acid as an antioxidant is required to obtain adequate recoveries from spiked tap and well waters.

Goodwin, L.R.; Francom, D.; Urso, A.; Dieken, F.P.



Determination of sulfur anions in spent oil shale leachates by ion chromatography  

SciTech Connect

The leaching and transport of chemical constituents from spent oil shale disposal areas is an area of environmental concern at the present time. Sulfur-containing compounds are prevalent in spent oil shales and have the potential to leach into aqueous systems surrounding disposal sites. Computer modeling has been used in recent years to predict the transport of species in an aqueous environment. The quality of model predictions, however, depends on the validation steps taken in comparing model predictions with laboratory data on ion speciation. Further, the quality of the validation step depends on the reliability of laboratory methods in generating ion speciation data. The purpose of this study was to develop methods to separate and quantify sulfur-containing anions in spent oil shale leachates by suppressed ion chromatography. The anions studied were S{sup 2{minus}} (sulfide), SO{sup 2{minus}}{sub 3} (sulfite), SO{sup 2{minus}}{sub 4} (sulfate), SCN{sup {minus}} (thiocyanate), S{sub 2}O{sup 2{minus}}{sub 3} (thiosulfate), and S{sub 4}O{sup 2{minus}}{sub 6} (tetrathionate). After the separations were developed, a series of method-challenging experiments were performed to test the reliability of the methods and assure the development of an analytically sound product. 24 refs., 7 figs., 5 tabs.

Niss, N.D.



Rapid screening for the detection and differentiation of ?-hydroxybutyrate using ion chromatography.  


The analysis of gamma-hydroxybutyric acid (GHB) is problematic because it is hygroscopic, it lacks a good UV chromophore, and it undergoes heat-induced cyclization. This paper presents a new method utilizing ion-exchange chromatography (IC) with conductivity detection. The simple sample preparation, rapid analysis time, and inorganic anion detection capabilities are all advantages over the current methods. The detection of inorganic salts (formed during GHB synthesis) gives insight into the synthetic route utilized and can aid in drug seizure comparison. The developed method has a detection limit for GHB anions of 0.57 mg/L and chloride of 0.22 mg/L. A comparison of this technique with a current gas chromatography-mass spectrometry technique is presented, and a t-test found that the two methods' results are not statistically different at the 99.9% confidence level demonstrating the merits of this fast, simple, and informative IC method as a routine screening tool. PMID:21790598

Hughes, Rachel R; Walker, G Stewart



Determination of hexavalent chromium in cosmetic products by ion chromatography and postcolumn derivatization.  


Chromium hydroxide green [Cr(2)O(OH)(4)] and chromium oxide green (Cr(2)O(3)) are colouring agents for use in cosmetic products. These colourants may contain chromium (VI), which cause skin allergies through percutaneous adsorption on the skin. Eye shadow is a representative cosmetic product in which significant colourants are used. We analysed the chromium (VI) in the eye shadows by ion chromatography and post column derivatization. We optimize conditions of chromium (VI) analysis in eye shadows. During the pretreatment procedure, there are no exchange of chromium (III) to chromium (VI). This method has a limit of quantification for chromium (VI) of 1.0 microg l(-1), recovery rate of 100 +/- 3% and analysis time less than 10 min. This result is 300 times more sensitive than the high-performance liquid chromatography method. We applied the optimized method to analyse 22 eye shadows and 6 colouring agents. 2 out of 22 of the products contained more than 5 mg l(-1). In our previous work, 5 mg l(-1) of Cr represented a threshold level. There was much more Cr(VI) in the colouring agents. The Cr(VI) in one of the colouring agents was 97.6 mg l(-1). PMID:16689807

Kang, Eun Kyung; Lee, Somi; Park, Jin-Hee; Joo, Kyung-Mi; Jeong, Hye-Jin; Chang, Ih Seop



Determination of glyphosate and phosphate in water by ion chromatography—inductively coupled plasma mass spectrometry detection  

Microsoft Academic Search

Quantitative determination of trace glyphosate and phosphate in waters was achieved by coupling ion chromatography (IC) separation with inductively coupled plasma mass spectrometry (ICP–MS) detection. The separation of glyphosate and phosphate on a polymer anion-exchange column (Dionex IonPac AS16, 4.0mm×250mm) was obtained by eluting them with 20mM citric acid at 0.50mLmin?1, and the analytes were detected directly and selectively by

Zhong-Xian Guo; Qiantao Cai; Zhaoguang Yang



Rapid quantitative method for total brominated vegetable oil in soft drinks using ion chromatography.  


A simple, quantitative and rapid method for total brominated vegetable oil (BVO) using ion chromatography (IC) with suppressed conductivity detection was developed and successfully applied to soft drinks with results expressed as inorganic bromide anion. The procedure involves extraction of BVO with diethyl ether and treatment with zinc dust in a solution of acetic acid, giving recoveries ranging between 92.5 and 98.5%. The calibration curves obtained were linear with correlation coefficients (r²) of 0.998, a coefficient of variation (CV) of less than 5% and limit of detection (LOD) and limit of quantification (LOQ) of 250 and 750?µg?l?¹, respectively. The method was successfully applied to the determination of BVO in several commercial soft drinks which were found to contain BVO in the range 1.8-14.510?mg?l?¹. The method has less sources of error compared to previously published methods. PMID:22725649

Yousef, Ashraf A; Abbas, Alaa B; Badawi, Bassam Sh; Al-Jowhar, Wafaa Y; Zain, Esam A; El-Mufti, Seham A



Effect of modulator sorption on gradient shape in ion-exchange chromatography  

NASA Technical Reports Server (NTRS)

Mobile phase additives, or modulators, are used in gradient elution chromatography to facilitate separation and reduce separation time. The modulators are usually assumed to be linearly adsorbed or unadsorbed. Here, the consequences of nonlinear modulator adsorption are examined for ion-exchange gradient elution through a series of simulations. Even when the buffer salt is identical to the modulator salt, gradient deformation is observed; the extent of deformation increases as the volume of the feed is increased. When the modulator salt is different from the buffer salt, unusual effects are observed, and the chromatograms are quite different from those predicted by classical gradient elution theory. In particular, local increases in the buffer concentration are found between feed bands, and serve to improve the separation. These effects become more pronounced as the feed volume increases, and could therefore prove valuable in preparative applications.

Velayudhan, A.; Ladisch, M. R.; Mitchell, C. A. (Principal Investigator)



Chloride determination by ion chromatography in petroleum coke after digestion by microwave-induced combustion.  


Microwave-induced combustion was applied to petroleum coke digestion in closed vessels for further chloride determination by ion chromatography. Samples were pressed as pellets and placed on a quartz holder. Combustion was performed using oxygen pressure of 2 MPa and 50 microl of 6 moll(-1) NH(4)NO(3) as aid for ignition. Recoveries from 97 to 102% were obtained for all studied absorbing solutions (water, H(2)O(2), Na(2)CO(3) or (NH(4))(2)CO(3)). Accuracy was evaluated using certified reference materials with agreement better than 98% using water as absorbing solution with reflux step. The limit of quantification was 3.8 microg g(-1). PMID:18996537

Pereira, Juliana S F; Diehl, Liange O; Duarte, Fábio A; Santos, Maria F P; Guimarães, Regina C L; Dressler, Valderi L; Flores, Erico M M



Detection of phosphorus oxyanions in synthetic geothermal water using ion chromatography-mass spectrometry techniques.  


Recent developments in microbiology suggest that reduced inorganic phosphorus oxyanions, including hypophosphite and phosphite, may be present in nature. These studies have inspired the development of specific and sensitive methods that detect phosphorus oxyanions in natural water. This paper will discuss a new technique that couples suppressed conductivity ion chromatography (Dionex AS17 analytical column and potassium hydroxide eluent) with electrospray mass spectrometry (IC/MS) with limits of detection nearly 200 times lower than those reported using suppressed conductivity detection. The technique was optimized for the detection of hypophosphite, phosphite, and phosphate in a synthetic geothermal water matrix. Samples were pre-treated with silver and sulfonic acid cartridges, and injection loop sizes as large as 800microl were employed to enhance instrument sensitivity. All peaks were clearly resolved, and calibrations were linear with estimated 3sigma limits of detection of 0.011, 0.0020, and 0.029microM for hypophosphite, phosphite, and phosphate, respectively. PMID:16185702

Ivey, Michelle M; Foster, Krishna L



Determination of fluorinated quinolone antibacterials by ion chromatography with fluorescence detection*  

PubMed Central

For preparing fluorinated quinolone antibiotic medicine locally used in stomatology, simultaneous determination of norfloxacin, ciprofloxacin, and enoxacin was carried out by multiphase ion chromatography with fluorescence detection. Quinolone antibiotics were separated by Dionex OmniPac PAX-500 column with an eluent of 15 mmol/L H2SO4 and 35% methanol (v/v) at a flow-rate of 1.0 ml/min and detected with fluorescence with excitation and emission wave lengths of 347 nm and 420 nm respectively. The detection limits (S/N=3) of norfloxacin, ciprofloxacin and enoxacin were 50, 105 and 80 ng/ml respectively. The relative standard deviations of retention time, peak area and peak height were less than 1.1% and good linear relationship resulted. The developed method was applied to pharmaceutical formulations and biological fluids. PMID:17542056

Zhang, Yan-zhen; Zhang, Zheng-yi; Zhou, Yan-chun; Liu, Li; Zhu, Yan



Rapid measurement of free cyanide in liquor by ion chromatography with pulsed amperometric detection.  


This study investigated the measurement of free cyanide in liquor by ion chromatography coupled with pulsed amperometric detection (IC-PAD). Eluent concentration, interferent evaluation and method performance were discussed. Results show that free cyanide in liquor can be rapidly determined by the optimised IC-PAD method. A sample requires only 1:100 dilution and simple filtration before being subjected to IC-PAD. The linear range is 1-5000 ?g/L with an R value of 0.9998. The detection limit is 1 ?g/L for a 25 ?L injection loop. The overall relative standard deviation (RSD) of the method is less than 5%, and the recovery range is from 98.1% to 105.0%. This study has been proven significant and may have potential applications in liquors analysis. PMID:25442607

Wu, Wenlin; Xiao, Quanwei; Zhang, Ping; Ye, Mei; Wan, Yuping; Liang, Hengxing



Isotope effects of neodymium in different ligands exchange systems studied by ion exchange displacement chromatography.  


The isotope effects of neodymium in Nd-glycolate ligand exchange system were studied by using ion exchange chromatography. The separation coefficients of neodymium isotopes, ?'s, were calculated from the observed isotopic ratios at the front and rear boundaries of the neodymium adsorption band. The values of separation coefficients of neodymium isotopes, ?'s, for the Nd-glycolate ligand exchange system were compared with those of Nd-malate and Nd-citrate, which indicated that the isotope effects of neodymium as studied by the three ligands takes the following direction Malate > Citrate > Glycolate. This order agrees with the number of available sites for complexation of each ligand. The values of the plate height, HETP of Nd in Nd-ligand exchange systems were also calculated. PMID:25685410

Ismail, Ibrahim; Fawzy, Ahmed S; Ahmad, Mohammad I; Aly, Hisham F; Nomura, Masao; Fujii, Yasuhiko




SciTech Connect

Ion Chromatography (IC) is routinely used at the Savannah River National Laboratory (SRNL) for sample analysis and characterization. Results from IC analysis are valued in corrosion control maintenance and measurement programs, remediation waste process control, soil and ground water measurement, nuclear materials processing, and various other research and development programs. Presented in this report are analytical methods developed on a DIONEX ICS3000 Reagent Free Ion Chromatography (RFIC) system located in AD at SRNL. This IC system contains two independent analysis channels comprising of a mobile phase generator, a pump, stationary phase columns, a suppressor and a conductivity detector. One channel is dedicated to anion analysis using Potassium Hydroxide (KOH) as the mobile phase while a second channel is configured for cation analysis using Methanesulfonic Acid (MSA) as the mobile phase. Both channels share an autosampler and the peak analysis software, Chromeleon{reg_sign} v.6.8. Instrument configuration is modified from the manufacturer for radiological service. Listed within this report are Dionex ICS3000 parameters and results for the analysis of routine anions and cations. Additional method parameters and discussion are presented on the analysis of Acetate (CH{sub 3}COO{sup -}) and Iodate (IO{sub 3}{sup -}). Previous IC analysis instruments at AD have been based upon carbonate/bicarbonate buffer mobile phase chemistry. This report represents a transition to hydroxide as a mobile phase eluent. The hydroxide eluent offers a lower baseline conductivity, which allows for greater sample dilution and/or lower detection limits. Also the hydroxide mobile phase and column set has a significant separation of the phosphate peak from the nitrate and sulfate peaks vs. the carbonate/bicarbonate mobile phase and column set, an advantage for the industrial waste analyzed at SRNL.

Wiedenman, B.; White, T.



Scaled-up separation of cellobiohydrolase1 from a cellulase mixture by ion-exchange chromatography.  


Enzymatic hydrolysis of cellulose often involves cellulases produced by Trichoderma reesei, of which cellobiohydrolase1 (CBH1) is the most abundant (about 60% of total cellulases) and plays an important role in the hydrolysis of crystalline cellulose. A method for separating sufficient quantities from the bulk cellulase cocktail is highly desirable for many studies, such as those that aim to characterize binding and hydrolysis kinetics of CBH1. In this work, CBH1 was separated from other Spezyme CP cellulases by ion-exchange chromatography using an efficient modification of a smaller scale process. The ion-exchange column was connected to a vacuum manifold system to provide a steady flow through parallel columns and thus achieve scale-up for enzyme separation. With five 5-mL columns running in parallel, about 55 mg of CBH1 was separated from 145 mg of Spezyme CP in a single separation. Step elution was used to replace the continuous gradient used at smaller scale. The purified CBH1 was collected in the fraction eluted with a buffer containing 0.33 M salt and showed comparable purity and activity as the enzyme purified by a fast protein liquid chromatography system. The stability of separated CBH1 was studied for up to 2 days and good thermal stability was observed. Separated CBH1 also showed both high adsorption to bacterial microcrystalline cellulose with ~4 ?mol/g maximum adsorption and a K(a) of 5.55 ± 2.34 ?M(-1) , and good hydrolytic activity based on atomic force microscopy observations that show a reduction in fiber height. PMID:21905272

Ye, Zhuoliang; Lane, Andrew N; Willing, Gerold A; Berson, R Eric



Simultaneous and sensitive analysis of aliphatic carboxylic acids by ion-chromatography using on-line complexation with copper(II) ion.  


A new approach to ion chromatography is proposed to improve the UV detection of aliphatic carboxylic acids separated by anion-exchange chromatography. When copper(II) ion added to the mobile phase, it forms complexes with carboxylic acids that can be detected at 240 nm. The absorbance was found to increase with increasing copper(II) ion concentration. The retention times of ?-hydroxy acids were also found to depend on the copper(II) ion concentration. Addition of acetonitrile to the mobile phase improved the separation of aliphatic carboxylic acids. The detection limits of the examined carboxylic acids (formate, glycolate, acetate, lactate, propionate, 3-hydroxypropionate, n-butyrate, isobutyrate, n-valerate, isovalerate, n-caproate) calculated at S/N=3 ranged from 0.06 to 3 ?M. The detector signal was linear over three orders of magnitude of carboxylic acid concentration. The proposed method was successfully applied to analyze aliphatic carboxylic acids in rainwater and bread. PMID:25523885

Kemmei, Tomoko; Kodama, Shuji; Yamamoto, Atsushi; Inoue, Yoshinori; Hayakawa, Kazuichi



Determination of trace levels of haloacetic acids and perchlorate in drinking water by ion chromatography with direct injection  

Microsoft Academic Search

Disinfection by products of haloacetic acids and perchlorate pose significant health risks, even at low ?g\\/l levels in drinking water. A new method for the simultaneous determination of nine haloacetic acids (HAAs) and perchlorate as well as some common anions in one run with ion chromatography was developed. The HAAs tested included mono-, di-, trichloroacetic acids, mono, di-, tribromoacetic acids,

Yongjian Liu; Shifen Mou



Chemical Speciation Analysis of Sports Drinks by Acid-Base Titrimetry and Ion Chromatography: A Challenging Beverage Formulation Project  

ERIC Educational Resources Information Center

Students have standardized a sodium hydroxide solution and analyzed commercially available sports drinks by titrimetric analysis of the triprotic citric acid, dihydrogen phosphate, and dihydrogen citrate and by ion chromatography for chloride, total phosphate and citrate. These experiments are interesting examples of analyzing real-world food and…

Drossman, Howard



Determination of Methylamines and Trimethylamine-N-oxide in particulate matter by non-suppressed ion chromatography  

Technology Transfer Automated Retrieval System (TEKTRAN)

An ion chromatography method with non-suppressed conductivity detection was developed for the simultaneous determination of methylamines (methylamine, dimethylamine, trimethylamine) and trimethylamine-N-oxide in particulate matter air samples. The analytes were well separated by means of cation-exch...



EPA Science Inventory

Bromate is a disinfection byproduct in drinking water which is formed during the ozonation of source water containing bromide. This paper described the analysis of bromate via ion chromatography-inductively coupled plasma mass spectrometry. The separation of bromate from interfer...


Purification of hemoglobin by ion exchange chromatography in flow-through mode with PEG as an escort.  


Development of hemoglobin-based blood substitutes requires production of highly purified hemoglobin. Process of hemoglobin purification by ion exchange chromatography in flow-through mode was researched and optimized. Three kinds of media including, QMA Spherosil LS (Biosepra, France) and Q Sepharose Big Beads (Amersham Bioscience, Sweden), and an anion exchange membrane column, Mustang Q (PALL, USA) were investigated and compared. Adding polyethylene glycol (PEG) as an escort in ion exchange chromatography improved the purity and recovery, and the recovery in the chromatography was increased from 75 to 95%. The mechanism of PEG effects on chromatography was discussed. The optimal chromatography step, in combination with hypotonic dilution hemolyzing and membrane separation, formed an integrated hemoglobin purification process. The total recovery in the process was 87.6%. The activity of hemoglobin was well preserved: P50 23.2 mmHg, and Hill coefficient 2.31. The product appeared as a single band in SDS-PAGE, and GF-HPLC showed only one peak. The purity of the prepared hemoglobin was more than 99.9%. The optimized process is time saving and suitable for large-scale preparation of hemoglobin to provide materials for further preparation of blood substitutes. PMID:15274429

Lu, Xiuling; Zhao, Dongxu; Su, Zhiguo



On the propensity of lignin to associate: A size exclusion chromatography study with lignin derivatives isolated from different plant species  

Microsoft Academic Search

Despite evidence that lignin associates under both aqueous and organic media, the magnitude and nature of the underlying driving forces are still a matter of discussion. The present paper addresses this issue by examining both solution properties and size exclusion behaviour of lignins isolated from five different species of softwoods, as well as from the angiosperms Eucalyptus globulus and wheat

Anderson Guerra; Armindo R. Gaspar; Sofía Contreras; Lucian A. Lucia; Claudia Crestini; Dimitris S. Argyropoulos




Technology Transfer Automated Retrieval System (TEKTRAN)

A high performance size exclusion chromatographic method utilizing an evaporative light scattering detector was developed to separate and quantify galacturonic acid (GA) oligomers. Values of k for GA monomer ranged from 0.16 in water to 0.67 in 100 mM acetic acid. In 40 mM acetic acid calibration ...


Separation of amaranthine-type betacyanins by ion-pair high-speed countercurrent chromatography.  


Betacyanins, red-violet plant pigments, were fractionated by ion-pair high-speed countercurrent chromatography (IP-HSCCC) from leaves extract of Iresine lindenii Van Houtte, an ornamental plant of the family Amaranthaceae. An HSCCC solvent system consisting of TBME-1-BuOH-ACN-H2O (1:3:1:5, v/v/v/v) was applied using ion-pair forming heptafluorobutyric acid (HFBA). Significantly different elution profiles of betacyanin diastereomeric pairs (derivatives based on betanidin and isobetanidin) observed in the HSCCC in comparison to HPLC systems indicate a complementarity of both techniques' fractionation capabilities. The numerous diastereomeric pairs can be selectively separated from each other using the HSCCC system simplifying the pigment purification process. Apart from the three well known highly abundant pigments (amaranthine, betanin and iresinin I) together with their isoforms, three new acylated (feruloylated and sinapoylated) betacyanins as well as known pigment hylocerenin (previously isolated from cacti fruits) were characterized in the plant for the first time and they are new for the whole Amaranthaceae family. PMID:24767836

Jerz, Gerold; Gebers, Nadine; Szot, Dominika; Szaleniec, Maciej; Winterhalter, Peter; Wybraniec, Slawomir



LC-IMS-MS Feature Finder: Detecting Multidimensional Liquid Chromatography, Ion Mobility, and Mass Spectrometry Features in Complex Datasets  

SciTech Connect

We introduce a command line software application LC-IMS-MS Feature Finder that searches for molecular ion signatures in multidimensional liquid chromatography-ion mobility spectrometry-mass spectrometry (LC-IMS-MS) data by clustering deisotoped peaks with similar monoisotopic mass, charge state, LC elution time, and ion mobility drift time values. The software application includes an algorithm for detecting and quantifying co-eluting chemical species, including species that exist in multiple conformations that may have been separated in the IMS dimension.

Crowell, Kevin L.; Slysz, Gordon W.; Baker, Erin Shammel; Lamarche, Brian L.; Monroe, Matthew E.; Ibrahim, Yehia M.; Payne, Samuel H.; Anderson, Gordon A.; Smith, Richard D.



Quality control considerations for size exclusion chromatography with online ICP-MS: a powerful tool for evaluating the size dependence of metal-organic matter complexation  

PubMed Central

Size exclusion chromatography (SEC), which separates molecules based on molecular volume, can be coupled with online inductively coupled plasma mass spectrometry (ICP-MS) to explore size-dependent metal-natural organic matter (NOM) complexation. To make effective use of this analytical dual detector system, the operator should be mindful of quality control measures. Al, Cr, Fe, Se, and Sn all exhibited columnless attenuation, which indicated unintended interactions with system components. Based on signal-to-noise ratio and peak reproducibility between duplicate analyses of environmental samples, consistent peak time and height were observed for Mg, Cl, Mn, Cu, Br, and Pb. Al, V, Fe, Co, Ni, Zn, Se, Cd, Sn, and Sb were less consistent overall, but produced consistent measurements in select samples. Ultrafiltering and centrifuging produced similar peak distributions, but glass fiber filtration produced more high molecular weight peaks. Storage in glass also produced more high molecular weight peaks than did plastic bottles. PMID:23416600

McKenzie, Erica R.; Young, Thomas M.



A comparison between SDS-PAGE and size exclusion chromatography as analytical methods for determining product composition in protein conjugation reactions.  


Horseradish peroxidase (HRP) was conjugated with bovine serum albumin (BSA) or human alpha(1)-proteinase inhibitor (alpha(1)-PI). The enzyme was maleimidylated using N-succinimidyl 4-(N-maleimidomethyl)cyclohexane-1-carboxylate (SMCC) and then allowed to react with thiolated BSA or reduced alpha(1)-PI. The conjugation products were analysed both by SDS-PAGE and size exclusion chromatography (SEC) on Sephadex G200. The two methods of evaluating conjugative processes were compared with respect to information provided in relation to the behaviour of the products in solution. The results showed that neither SDS-PAGE nor SEC alone provides sufficient information about conjugate structure. The basic conjugate units observed in electrophoresis tend to form dimeric or higher-order aggregates under gel chromatographic conditions. PMID:12376019

Tacal, Ozden; Ozer, Inci



Conductivity detection for molecular mass estimation of per-O-sulfonated glycosaminoglycans separated by high-performance size-exclusion chromatography.  


Chemically per-O-sulfonated polysaccharides, including glycosaminoglycans (GAGs) and hyaluronan oligosaccharides were analyzed using high-performance size-exclusion chromatography (HPSEC) with suppressed conductivity detection. The results were compared to those obtained by gel filtration HPLC using UV detection or fluorescence detection after the post-column reaction with 2-cyanoacetamide in strong alkaline solution. Analysis was performed on a TSKgel G3000SWXL HPSEC column in 5 mM boric acid (pH 7.0 adjusted by 10 mM NaOH). The use of conductivity detection, in the absence of any derivatization and under isocratic conditions gave a limit of detection in the picogram range. Preliminary studies suggest that this approach may be particularly useful in examining sulfonated polysaccharides and oligosaccharides having no UV chromophore, such as those prepared from O-sulfonated fucans and galactans isolated from algae. PMID:12141565

Chaidedgumjorn, Amornrut; Suzuki, Atsushi; Toyoda, Hidenao; Toida, Toshihiko; Imanari, Toshio; Linhardt, Robert J



Chromatography Theory  

NSDL National Science Digital Library

This site contains standard definitions related to chromatography similar to treatments found in analytical chemistry textbooks. It introduces the beginning student to Liquid Chromatography concepts relevant to biochemistry and includes a good example of choosing a mobile phase pH for a protein separation based on ion exchange.


Characterization and quantitative amino acids analysis of analgesic peptides in cinobufacini injection by size exclusion chromatography, matrix-assisted laser desorption/ionization time of flight mass spectrometry and gas chromatography mass spectrometry.  


Cinobufacini injection that comes from the water extract of Bufo bufo gargarizans Cantor skin is widely used for cancer treatment in China. Peptide is one of its major types of constituents, however the biological effects and content of this injection are little reported. In present study, the analgesic effect of peptides was determined and evaluated by in-vivo models. To characterize and quantitatively analyze these peptides, a reliable and efficient method combining size exclusion chromatography and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry with amino acid analysis was developed. The peptides presented as a series of analogs with similar molecular weights mostly ranging from 2 to 8 kDa. The amino acid analysis by gas chromatography mass spectrometry (GC-MS) was developed to determine both free and combined amino acids (FAA and CAA) in cinobufacini injection. This method achieved good linearity (R(2) , 0.9909-0.9999) and low limit of detection and quantification. FAA and CAA samples were efficiently analyzed by modified Phenomenex EZ: faast procedure. For the sample analysis, the method showed good repeatability (relative standard deviation, RSD???10%). For most FAA and CAA the mean recoveries were >80% with RSD <10%. The GC-MS based method is useful for quality assurance of both FAA and CAA in cinobufacini injection. PMID:24924921

Wu, Xu; Si, Nan; Bo, Gao; Hu, Hao; Yang, Jian; Bian, Baolin; Zhao, Hai Yu; Wang, Hongjie



Highly sensitive determination of dialkyl phosphinate acids in environmental samples by ion chromatography tandem mass spectrometry.  


Dialkyl phosphinate acids (DPAs) are the hydrolysates of aluminum dialkyl phosphinates (ADPs), one class of emerging phosphorus flame retardants since brominated flame retardants have been gradually phased out in recent years. It has been found that once dissolved in water, ADPs are completely hydrolyzed and exist as DPAs. However, there is no report on the determination of DPAs in environmental water samples. For the first time, we developed a method for the analysis of trace DPAs and ADPs in different environmental samples, including waters, soils and sediments. In this proposed method, MAX cartridges were employed for the purification, and ion chromatography (IC) tandem mass spectrometry (MS) method with large volume injection (200?L) and postcolumn addition of methanol and NH3·H2O were employed for the determination of DPAs and ADPs. The matrix effects were <16% for water samples and <25% for soil/sediment samples, which were greatly improved in comparison to the liquid chromatography (LC) tandem MS determination. Determined at three fortified levels of 0.02?g/L, 0.2?g/L and 1.0?g/L, the mean recoveries were from 75.8% to 110.2%, with an acceptable coefficient of variation (3.3-20%, n=6) for water samples. The limits of the method were 3.5-9.3ng/L for DPAs in environmental water samples, and 0.06-0.09?g/kg for DPAs and ADPs in soil and sediment samples. For soil and sediment samples, results determined by the present IC-MS method were in good agreement with that determined by LC-MS in our previous study. PMID:25836050

Niu, Yu-Min; Liang, Yong; Liu, Ji-Yan; Liu, Jing-Fu



Determination of trace anions in liquefied petroleum gas using liquid absorption and electrokinetic migration for enrichment followed by ion chromatography.  


A simple sample enrichment technique, electrokinetic migration enrichment in single phase using a designed device, coupled with ion chromatography is presented for the determination of four anions (H(2)PO(4)(-), Cl(-), NO(3)(-), and SO(4)(2-)) in liquefied petroleum gas by liquid adsorption. The electrokinetic migration enrichment is based on the phenomenon of ion electrokinetic migration to the opposite electrode. When the anions migrated to the anode in a smaller volume chamber under the electric field, the concentration was realized. The main parameters affecting enrichment efficiency of applied voltage and enrichment time were investigated. The ion chromatography condition for anions separation was also studied. Under the optimal electrokinetic migration enrichment and ion chromatography conditions, the four anions were detected simultaneously with good linear relationship (r(2) = 0.9908-0.9968) and high precisions (less than 5% of the relative standard deviations of peak areas). The limits of detection of anions (S/N of 3) were in the range of 8-600 ?g L(-1). The enrichment factors of the four anions ranged from 3.1 to 5.8. The established method was successfully applied to the analysis of the trace anions in liquefied petroleum gas by liquid adsorption with satisfactory results. The advantages of this method are simple operation and low cost. PMID:22733518

Li, Meilan; Yang, Jianmin; Li, Hai-Fang; Lin, Jin-Ming



Energy transduction in the thermophilic anaerobic bacterium Clostridium fervidus is exclusively coupled to sodium ions.  

PubMed Central

The thermophilic, peptidolytic, anaerobic bacterium Clostridium fervidus is unable to generate a pH gradient in the range of 5.5-8.0, which limits growth of the organism to a narrow pH range (6.3-7.7). A significant membrane potential (delta psi approximately -60 mV) and chemical gradient of Na+ (-Z delta pNa approximately -60 mV) are formed in the presence of metabolizable substrates. Energy-dependent Na+ efflux is inhibited by the Na+/H+ ionophore monensin but is stimulated by uncouplers, suggesting that the Na+ gradient is formed by a primary pumping mechanism rather than by secondary Na+/H+ antiport. This primary sodium pump was found to be an ATPase that has been characterized in inside-out membrane vesicles and in proteoliposomes in which solubilized ATPase was reconstituted. The enzyme is stimulated by Na+, resistant to vanadate, and sensitive to nitrate, which is indicative of an F/V-type Na(+)-ATPase. In the proteoliposomes Na+ accumulation depends on the presence of ATP, is inhibited by the ATPase inhibitor nitrate, and is completely prevented by the ionophore monensin but is stimulated by protonophores and valinomycin. These and previous observations, which indicated that secondary amino acid transport uses solely Na+ as coupling ion, demonstrate that energy transduction at the membrane in C. fervidus is exclusively dependent on a Na+ cycle. Images Fig. 2 PMID:8367451

Speelmans, G; Poolman, B; Abee, T; Konings, W N



Ion chromatography to detect salts in stone structures and to assess salt removal methods  

NASA Astrophysics Data System (ADS)

Stone - and in general all materials- from built heritage is very often damaged by salt crystallisation processes. Such processes usually derive into a loss of material compactness, as salts - given specific conditions and parameters- crystallize inside the material pores, exerting a pressure against the material pore walls higher than what they can resist - similar to the effect of liquid water when converts to solid water or ice-, thus breaking and disrupting the material by generating fissures and increasing the pore volume ratio, loosing its initial cohesion. When these deterioration processes take place inside a structure, salts - from different sources: material itself, restoration materials, from the ground, etc.- may come up to the stone surface - either temporarily or in permanently-, from beneath it, as efflorescences, depending mainly on the microclimatic conditions of the environment and the salts source. Efflorescences can be analysed and their nature identified (e.g. by means of X ray diffraction, in which the mineralogical composition of the salt is obtained), which can be, general, of aid not only for restoration but for preventive conservation measures. But what we do not know a priori when only characterising salt compounds- is the extent of the damage due to the presence of salts inside a structure (sub- and cryptoefflorescences). In this work we present a procedure in which the depth of the salt content can be measured, and its nature identified, based on the use of the ion chromatography technique. This technique allows identifying the existing ions in a specific sample, both anions and cations. The procedure consists of drilling (with a drilling core ranging from 5 to 8 mm in diameter, therefore causing the minimum damage to the material) in a same point at different depths from the surface and several depths from the bottom. The samples obtained are analysed and the ion content determined, qualitative and quantitatively. By means of a thorough previous inspection, we can select the most representative points by a drilling net - as minimum as possible- and make some profiles of the inner salt content of a structure. Moreover, this procedure is not only reliable for determining the nature and extent of salts damage, but to assess the efficacy of salts removal methods in cultural heritage. Here we present two case studies from relevant buildings of the Spanish cultural heritage in which this procedure was performed with successful and useful results, in both terms of understanding what types of salts were decaying the stones structures, and also whether the salts removal methods that were planned in the restoration project were efficient or not. It should be remarked that even ion chromatography is not a non destructive technique (can be considered as a minimally destructive one due to the few quantity it is needed for the analysis), the information it can provide is so useful that should not be ruled out from the beginning, depending of each specific case.

Alvarez de Buergo, M.; Lopez-Arce, P.; Fort, R.



Determination of alkanolamines in cattails (Typha latifolia) utilizing electrospray ionization with selected reaction monitoring and ion-exchange chromatography.  


Selected reaction monitoring (SRM) with electrospray ionization was used as a specific detection technique for the analysis of alkanolamines in plant tissue extracts. Ion-exchange chromatography was used as the method of separation. Quantification was based on monitoring the loss of either H2O or 2(H2O) from the protonated molecule [M+H]+. The method provided increased selectivity for all analytes and better detection limits for three of the six analytes investigated compared with an earlier method using selected ion monitoring with liquid chromatography. Instrumental detection limits ranged from 6-300 pg injected for monoethanolamine (MEA), monoisopropanolamine (MIPA), diethanolamine (DEA), methyldiethanolamine (MDEA), diisopropanolamine (DIPA), and triethanolamine (TEA). Method robustness and selectivity were demonstrated by the determination of DIPA and a known transformation product MIPA in over 35 plant extract samples derived from a laboratory study of plant uptake mechanisms. PMID:15282789

Peru, Kerry M; Headley, John V; Doucette, William J



Separation of uremic toxins from urine with resorcinarene-based ion chromatography columns.  


People with chronic kidney disease suffer from uremic toxins which accumulate in their bodies. Detection and quantification of uremic toxins help diagnose kidney problems and start patient care. The aim of this research was to seek a new method to assist this diagnosis by trace level detection and separation of guanidine containing uremic toxins in water and urine. To detect and quantify the uremic toxins, new stationary phases for ion chromatography (IC) columns based on glutamic acid functionalized resorcinarenes bound to divinylbenzene macroporous resin were prepared. The new column packing material afforded separation of the five compounds: guanidinoacetic acid, guanidine, methylguanidine, creatinine, and guanidinobenzoic acid in 30min. Peak resolutions ranged from 7.6 to 1.3. Gradient elutions at ambient temperature with methanesulfonic acid (MSA) solution as eluent resulted in detection levels in water from 10 to 47ppb and in synthetic urine from 28 to 180ppb. Limits of quantification for the analytes using pulsed amperometric detection were 30-160ppb in water and 93-590ppb in urine. Trace levels of creatinine (1ppm) were detected in the urine of a healthy individual using the columns. PMID:25537175

Panahi, Tayyebeh; Weaver, Douglas J; Lamb, John D; Harrison, Roger G



Fabrication of electrolytic cell for online post-column electrochemical derivatization in ion chromatography.  


An electrolytic cell (EC), composed of two ruthenium-plated titanium electrodes separated by cation-exchange membranes, was fabricated and evaluated for online postcolumn derivatization in ion chromatography (IC). Folic acid (FA) and methotrexate (MTX) were preliminarily used as prototype analytes to test the performance of EC. After separation by an anion exchange column, FA and MTX, which emit very weak fluorescence when excited, were electrochemically oxidized online in the anode chamber of the EC. The compounds with strong fluorescence, which are oxidation products, were detected by the fluorescence detector. The phosphate buffer solution (100 mM KH(2)PO(4)) served as an optimal eluent for anion exchange chromatographic separation and a suitable supporting electrolyte for electro-oxidation, leading to ideal compatibility between IC separation and the postcolumn electrochemical derivatization. For the presently proposed method, the linear ranges were from 0.01 mg L(-1) to 5 mg L(-1) for both FA and MTX. The detection limits of FA and MTX were 1.8 and 2.1 ?g L(-1), and the relative standard deviations (RSD, n=7) were 2.9% and 3.6%, respectively. The method was applied for the simultaneous determination of FA and MTX in the plasma of patients being treated for rheumatoid arthritis. The determination of MTX in the urine of the patients of diffuse large B cell lymphoma was also demonstrated. PMID:22713918

Wu, Shuchao; Xu, Wei; Yang, Bingcheng; Ye, Mingli; Zhang, Peimin; Shen-Tu, Chao; Zhu, Yan



Anionic Forensic Signatures for Sample Matching of Potassium Cyanide Using High Performance Ion Chromatography and Chemometrics  

SciTech Connect

Potassium cyanide, a known poison, was used a model compound to determine the feasibility of using anionic impurities as a forensic signature for matching KCN samples back to their source. In this study, portions of eight KCN stocks originating from four countries were separately dissolved in water and analyzed by high performance ion chromatography (HPIC) using an anion exchange column and conductivity detection. Sixty KCN aqueous samples were produced from the eight stocks and analyzed for 11anionic impurities. Hierarchal cluster analysis and principal component analysis were used to demonstrate that KCN samples cluster according to source based on the concentrations of their anionic impurities. The F-ratio method and degree-of-class separation (DCS) were used for feature selection on a training set of KCN samples in order to optimize sample clustering. The optimal subset of anions needed for sample classification was determined to be sulfate, oxalate, phosphate, and an unknown anion named unk5. Using K-nearest neighbors (KNN) and the optimal subset of anions, KCN test samples from different KCN stocks were correctly determined to be manufactured in the United States. In addition, KCN samples from stocks manufactured in Belgium, Germany, and the Czech Republic were all correctly matched back to their original stocks because each stock had a unique anionic impurity profile. The application of the F-ratio method and DCS for feature selection improved the accuracy and confidence of sample classification by KNN.

Fraga, Carlos G.; Farmer, Orville T.; Carman, April J.



Mixing characteristics of mixers in flow analysis. Application to two-dimensional detection in ion chromatography.  


Three mixer designs, a back-flow tee mixer (BT), an end-blocked membrane tee mixer (EMT), and a tubular membrane mixer (TM), were fabricated and compared to three commercially available mixers, Visco-Jet Micro mixer (VJM) and HS binary tee mixer with 2 and 10 ?L volume (HS-2 and HS-10) mixing cartridges. Internal volumes ranged from 8.3 to 20.3 ?L. Performance characteristics were evaluated by the Villermaux-Dushman reaction, noise in baseline conductance upon mixing an electrolyte solution with water, and dispersion/relative dispersion of an injected solute. No single characteristic would uniquely qualify a particular device. In typical postcolumn use when a small reagent flow is added to a principal flow stream using a low-pulsation high-end chromatographic pump, with the worst of these mixers, imperfect mixing accounted for 99.6% of the observed noise. EMT, BT, and TM with asymmetric inlets provided better mixing performances relative to VJM, HS-2, and HS-10 with symmetric inlet ports, especially when the secondary liquid flow rate was much lower than the principal stream-flow rate. Dispersion per unit residence time was singularly large for HS-2. Based on its mixing efficiency and small dispersion, the BT design was found to be the best for practicing postcolumn reaction. As an illustrative application, this was then used to introduce electrogenerated LiOH in a suppressed ion chromatography system to perform sensitive detection of weak acids in a second dimension. PMID:25426864

Liao, Hongzhu; Dasgupta, Purnendu K; Srinivasan, Kannan; Liu, Yan



Determination of sulfur species in oil shale waste waters by ion chromatography  

SciTech Connect

Ion chromatography was evaluated for analysis of sulfur (S) species in oil shale waste waters. Chromatographic separation of S/sub 2/O/sub 3//sup 2 -/ and SCN/sup -/, the effect of high salt concentration on the elution of SO/sub 4//sup 2 -/, and the inherent instability of S species in the samples are discussed. Several sulfur-oxide anions, including S/sub 2/O/sub 4//sup 2 -/, S/sub 2/O/sub 5//sup 2 -/, S/sub 2/O/sub 6//sup 2 -/, and S/sub 2/O/sub 7//sup 2 -/ were unstable when added to solution, forming SO/sub 3//sup 2 -/, SO/sub 4//sup 2 -/. However the method proved applicable to determination of SO/sub 3//sup 2 -/, SO/sub 4//sup 2 -/, S/sub 2/O/sub 3//sup 2 -/ and SCN/sup -/ in oil shale retort water and from retorted shale in both laboratory and field studies.

McFadden, K. M.; Garland, T. R.




SciTech Connect

The Process Science Analytical Laboratory (PSAL) at the Savannah River National Laboratory was requested by the Defense Waste Processing Facility (DWPF) to develop and demonstrate an Ion Chromatography (IC) method for the analysis of glycolate, in addition to eight other anions (fluoride, formate, chloride, nitrite, nitrate, sulfate, oxalate and phosphate) in Sludge Receipt and Adjustment Tank (SRAT) and Slurry Mix Evaporator (SME) samples. The method will be used to analyze anions for samples generated from the Alternate Reductant Demonstrations to be performed for the DWPF at the Aiken County Technology Laboratory (ACTL). The method is specific to the characterization of anions in the simulant flowsheet work. Additional work will be needed for the analyses of anions in radiological samples by Analytical Development (AD) and DWPF. The documentation of the development and demonstration of the method fulfills the third requirement in the TTQAP, SRNL-RP-2010-00105, 'Task Technical and Quality Assurance Plan for Glycolic-Formic Acid Flowsheet Development, Definition and Demonstrations Tasks 1-3'.

Best, D.



Laboratory robotics -- An automated tool for preparing ion chromatography calibration standards  

SciTech Connect

This paper describes the use of a laboratory robot as an automated tool for preparing multi-level calibration standards for On-Line Ion Chromatography (IC) Systems. The robot is designed for preparation of up to six levels of standards, with each level containing up to eleven ionic species in aqueous solution. The robot is required to add the standards` constituents as both a liquid and solid additions and to keep a record of exactly what goes into making up every standard. Utilizing a laboratory robot to prepare calibration standards provides significant benefits to the testing environment. These benefits include: accurate and precise calibration standards in individually capped containers with preparation traceability; automated and unattended multi-specie preparation for both anion and cation analytical channels; the ability to free up a test operator from a repetitive routine and re-apply those efforts to test operations; The robot uses a single channel IC to analyze each prepared standard for specie content and concentration. Those results are later used as a measure of quality control. System requirements and configurations, robotic operations, manpower requirements, analytical verification, accuracy and precision of prepared solutions, and robotic downtime are discussed in detail.

Chadwick, J.L.



Preparation of polyaniline modified electrode in novel ionic liquid and its application in ion chromatography.  


In this work, a promising electrochemical detector has been fabricated by immersing a glass carbon electrode (GCE) in aniline containing novel ionic liquid and scanning between -1.0 and 1.0 V for 40 cycles, and was used in ion chromatography (IC) system. The morphology of the modified electrode surface was characterized by scanning electron microscope (SEM). The polyaniline (PANI) film showed excellent electrocatalytic activity than bare GCE and provided enhanced selectivity and stability for the detection of ascorbic acid (AA). Separated by IC with phosphate buffer solution (pH = 5.2) as eluent, AA could be determined by the PANI/GCE successfully at the working potential of 0.3 V. The retention time of AA was approximately 5.75 min, and the peak shape of AA was satisfactory. The calibration curve of AA was linear (r > 0.99), in the range between 0.05 mg/L and 1000 mg/L and the detection limit was 23.41 ?g/L (S/N = 3). The proposed method was successfully applied in the detection of AA in four beverage samples. The recoveries of AA in these samples were from 92.32% to 110.57%. PMID:21859535

Dandan, Ren; Xu, Jingang; Lingling, Xi; Yan, Zhu



Determination of alendronate in pharmaceutical dosage formulations by ion chromatography with conductivity detection.  


A method was developed and validated for the direct determination in pharmaceutical dosage formulations of alendronate, a non-chromophoric compound. It is based on the use of single-column ion chromatography with conductivity detection that obviates the need for the tedious chemical derivatization procedures that are required for UV and fluorescence detection. Diluted samples of 0.05 mg/ml were chromatographed directly on a Waters IC-Pak HR anion-exchange column or a Dionex OmniPac PAX-100 column with dilute nitric acid as the mobile phase followed by conductivity detection. The method was validated and shown to be precise, accurate and specific for the assay of alendronate in intravenous (i.v.) solution and tablet formulations. The ruggedness of the assay was studied by generating data from four different instruments. Also established was the equivalence between this method and a previously reported high-performance liquid chromatographic method with 9-fluorenylmethyl chloroformate derivatization and UV detection. Application of the method to the determination of alendronate in i.v. and tablet formulations is presented and the performances of the Waters IC-Pak HR and Dionex OmniPac columns are discussed. PMID:1400839

Tsai, E W; Ip, D P; Brooks, M A



Anionic forensic signatures for sample matching of potassium cyanide using high performance ion chromatography and chemometrics.  


Potassium cyanide was used as a model toxicant to determine the feasibility of using anionic impurities as a forensic signature for matching cyanide salts back to their source. In this study, portions of eight KCN stocks originating from four countries were separately dissolved in water and analyzed by high performance ion chromatography (HPIC) using an anion exchange column and conductivity detection. Sixty KCN aqueous samples were produced from the eight stocks and analyzed for 11 anionic impurities. Hierarchal cluster analysis and principal component analysis were used to demonstrate that KCN samples cluster according to source based on the concentrations of their anionic impurities. The Fisher-ratio method and degree-of-class separation (DCS) were used for feature selection on a training set of KCN samples in order to optimize sample clustering. The optimal subset of anions needed for sample classification was determined to be sulfate, oxalate, phosphate, and an unknown anion named unk5. Using K-nearest neighbors (KNN) and the optimal subset of anions, KCN test samples from different KCN stocks were correctly determined to be manufactured in the United States. In addition, KCN samples from stocks manufactured in Belgium, Germany, and the Czech Republic were all correctly matched back to their original stocks because each stock had a unique anionic impurity profile. The application of the Fisher-ratio method and DCS for feature selection improved the accuracy and confidence of sample classification by KNN. PMID:21215851

Fraga, Carlos G; Farmer, Orville T; Carman, April J



Quantitative Silver Ion Thin Layer Chromatography of Triacylglycerols from Sunflower Oils Differing in the Level of Linoleic Acid  

Microsoft Academic Search

Eight samples of sunflower oil with different linoleic acid contents (9–63{%}) were subjected to a triacylglycerol (TAG) analysis by silver-ion thin-layer chromatography with densitometric quantification. In spite of this substantial change in the fatty acid composition, the relative content of the component TAG classes in the sum of polyunsaturated triacylglycerols remains constant. Thus, a characteristic fingerprint of sunflower oil TAG

Ilko Marekov; Roumyana Tarandjiiska; Svetlana Momchilova; Boryana Nikolova-Damyanova



The determination of 63 Ni and 99 T c in class C waste by ion chromatography and scintillation detection  

Microsoft Academic Search

A procedure using high performance ion chromatography coupled with on-line scintillation counting and described for the determination\\u000a of nickel-63 and technecium-99 radioisotopes in irradiated stainless steel. Commercially available chromatograph équipment,\\u000a columns and online scintillation detectors were used. The method provides detection limits for63Ni and99Tc within the range needed the determination of these radioisotopes in class “C” waste streams at our

C. D. Morgan; S. M. Frank; C. D. Monghan; A. P. Maddison



Identification and dating of the fountain pen ink entries on documents by ion-pairing high-performance liquid chromatography  

Microsoft Academic Search

A novel approach for the identification and dating of the fountain pen ink entries on paper has been established by ion-pairing high-performance liquid chromatography (IP-HPLC). Twelve black and six red fountain inks have been collected, and their ink entries have been prepared by drawing lines on paper. The chromatographic conditions for separation of their dye components after extraction with solvents

Xiang-Feng Wang; Jing Yu; Meng-Xia Xie; Ya-Tong Yao; Jie Han



Effect of suppressor current intensity on the determination of glyphosate and aminomethylphosphonic acid by suppressed conductivity ion chromatography  

Microsoft Academic Search

This paper presents the application of ion chromatography with electrolytic eluent generation and mobile phase suppression for the direct conductimetric detection of glyphosate and its degradation product aminomethylphosphonic acid (AMPA). The compounds were separated on a Dionex AS18 anion exchange column with a 12–40mM KOH step gradient from 9 to 9.5min. The effect of the suppressor current intensity on the

Ioannis K. Dimitrakopoulos; Nikolaos S. Thomaidis; Nikolaos C. Megoulas; Michael A. Koupparis



Condensation nucleation light scattering detection with ion chromatography for direct determination of glyphosate and its metabolite in water  

Microsoft Academic Search

An ion chromatography–condensation nucleation light scattering detection (IC–CNLSD) method was successfully used to directly analyze glyphosate, a polar pesticide, and aminomethylphosaphonic acid, the major metabolite of glyphosate, in water without need of pre-treatment or derivatization. CNLSD gave a LOD of 53 ng\\/ml for glyphosate, which is much lower than the maximum contaminant level of 700 ng\\/ml for drinking water issued

Jing You; John A. Koropchak



Analysis of fatty acid mono- and diacylglycerol positional isomers by silver ion high-performance liquid chromatography  

Microsoft Academic Search

Mono- and diacylglycerol positional isomer pairs were separated (as acetates) by silver ion high-performance liquid chromatography on a commercially available column using an isocratic solvent system of 1.2% (v\\/v) acetonitrile in hexane and flame ionization detection. The acetate derivative(s) from the 1- and 2-monoacylglycerols and 1,2- and 1,3-diacylglycerols were prepared by acetic anhydride-pyridine. Conversion of the thermodynamically less stable 2-mono-

Richard O. Adlof



Adsorption of peptides and small proteins with control access polymer permeation to affinity binding sites. Part I: Polymer permeation-immobilized metal ion affinity chromatography separation adsorbents with polyethylene glycol and immobilized metal ions.  


Despite the many efforts to develop efficient protein purification techniques, the isolation of peptides and small proteins on a larger than analytical scale remains a significant challenge. Recovery of small biomolecules from diluted complex biological mixtures, such as human serum, employing porous adsorbents is a difficult task mainly due to the presence of concentrated large biomolecules that can add undesired effects in the system such as blocking of adsorbent pores, impairing diffusion of small molecules, or competition for adsorption sites. Adsorption and size exclusion chromatography (AdSEC) controlled access media, using polyethylene glycol (PEG) as a semi-permeable barrier on a polysaccharide matrix, have been developed and explored in this work to overcome such effects and to preferentially adsorb small molecules while rejecting large ones. In the first part of this work, adsorption studies were performed with small peptides and proteins from synthetic mixtures using controlled access polymer permeation adsorption (CAPPA) media created by effectively grafting PEG on an immobilized metal affinity chromatography (IMAC) agarose resin, where chelating agents and immobilized metal ions were used as the primary affinity binding sites. Synthetic mixtures consisted of bovine serum albumin (BSA) with small proteins, peptides, amino acids (such as histidine or Val?-Angiotensin III), and small molecules-spiked human serum. The synthesized hybrid adsorbent consisted of agarose beads modified with iminodiacetic (IDA) groups, loaded with immobilized Cu(II) ions, and PEG. These CAPPA media with grafted PEG on the interior and exterior surfaces of the agarose matrix were effective in rejecting high molecular weight proteins. Different PEG grafting densities and PEG of different molecular weight were tested to determine their effect in rejecting and controlling adsorbent permeation properties. Low grafting density of high molecular weight PEG was found to be as effective as high grafting density of low molecular weight PEG in the rejecting properties of the semi-permeable synthesized media. PMID:22281505

González-Ortega, Omar; Porath, Jerker; Guzmán, Roberto




Technology Transfer Automated Retrieval System (TEKTRAN)

Eleven B-lactams antibiotics were analyzed in fortified and incurred beef kidney tissue using high-performance liquid chromatography/selective reaction monitoring/tandem ion trap mass spectrometry. The analytes included: deacetylcephapirin, amoxicillin, cephapirin, desfuroylceftiofur cysteine disul...



EPA Science Inventory

In this presentation the analytical instrumentation and procedures necessary to qualitatively and quantitatively determine low levels of perchlorate (ClO4-) in drinking waters using ion chromatography with electrolytic conductivity suppression, electrospray ionization mass spec...



EPA Science Inventory

This method is applicable to the identification and quantitation of perchlorate in raw and finished drinking waters. The approach used is ion chromatography with suppressed conductivity and electrospray ionization mass spectrometry (IC-ESI/MS)...


A Volatile Organic Analyzer for Space Station - Description and evaluation of a gas chromatography/ion mobility spectrometer  

NASA Technical Reports Server (NTRS)

An on-board Volatile Organic Analyzer (VOA), an essential component of the Environmental Health System (EHS) air-quality monitoring strategy, is described. The strategy is aimed at warning the crew and ground personnel if volatile compounds exceed safe exposure limits. The VOA uses a combination of gas chromatography (GC) and ion-mobility spectrometry (IMS) for environmental monitoring and analysis. It is concluded that the VOA dual-mode detection capability and the ion mobilities in the drift region are unique features that can assist in the resolution of coeluting GC peaks. The VOA is capable of accurately identifying and quantifying target compounds in a complex mixture.

Limero, Thomas; Brokenshire, John; Cumming, Colin; Overton, ED; Carney, Ken; Cross, Jay; Eiceman, Gary; James, John



Confirmatory method for sulfonamide residues in animal tissues by gas chromatography and pulsed positive ion-negative ion-chemical ionization mass spectrometry.  


A confirmatory method has been developed for determination of 13 sulfonamides in edible tissues. The assay involves extraction from a solution resulting from a screening procedure by liquid chromatography and subsequent derivatization. Sulfachloropyridazine (SCP), sulfadiazine (SDA), sulfadimethoxine (SDM), sulfamethazine (SMZ), sulfamerazine (SME), sulfamethoxazole (SMX), sulfamethoxypyridazine (SMP), sulfapyridine (SPR), sulfaquinoxaline (SQX), and sulfathiazole (STA) were detected as the N1-methyl-N4-trifluoroacetyl derivatives, sulfaguanidine (SGU) as the same derivative after cyclization by hexafluoroacetylacetone, and sulfacetamide (SAC) as the methyl derivative. These sulfonamides were detected by gas chromatography and pulsed positive ion-negative ion-chemical ionization mass spectrometry with methane as the reactant gas, whereas sulfanilamide (SAA) was determined as the methyl derivative by electron-impact ionization. PMID:8241826

Mooser, A E; Koch, H



[Determination of principal components and related substances in adenosine disodium triphosphate preparation by ion chromatography].  


A new method was developed for the determination of adenosine disodium triphos- phate (ATP-Na2 ) and its related substances in ATP-Na2 preparation by ion chromatography (IC). The sample was diluted with ultrapure water and filtrated by 0.22 ?m polyether sulfone filter membrance, and then analyzed by IC directly without any more pretreatment. The analysis was performed on a Dionex IonPac AS11-HC column (250 mm x 4 mm) and a guard column Ion-Pac AG11-HC (50 mm x 4 mm). A KOH eluent generator cartridge was used for gradient elution at the flow rate of 1.0 mL/min. The detection was performed by a Dionex suppressed (Dionex AERS 500 4-mm) conductivity detector. The injection volume was 10 ?L. The assay was quantitatively completed by external standard method and the related substances were calculated with correction factors. The linear ranges of the method for ATP-Na2, adenosine disodium diphosphate (ADP-Na2) and adenosine disodium monophosphate (AMP-Na2) were 0.000 146-1.83 g/L (r = 0.9997), 0.000484-1.51 g/L (r = 0.9996) and 0.000426-0.804 g/L (r = 0.9999), respectively. The average recoveries of ATP-Na2 were 96.50%, 96.57% and 96.77% at three spiked levels. The limits of quantitation (S/N = 10) of ATP-Na2, ADP-Na2 and AMP-Na2 were 1.5 ng, 4.8 ng, 4.3 ng, and the limits of detection (S/N = 3) were 0.58 ng, 1.21 ng, 1.28 ng, respectively. The results demonstrated that the system has the advantages of high sensitivity, facile automation and simple sample pretreatment. The method is suitable for the quality control of adenosine disodium triphosphate preparations. PMID:25764665

Shan, Guangzhi; Zong, Yanping; Wang, Xiao; Lu, Jinghua



Simultaneous determination of dimethylamine, trimethylamine and trimethylamine- n-oxide in aquatic products extracts by ion chromatography with non-suppressed conductivity detection  

Microsoft Academic Search

An ion chromatography method with non-suppressed conductivity detection was developed for the simultaneous determination of dimethylamine (DMA), trimethylamine (TMA) and trimethylamine-n-oxide (TMAO) in aquatic products. They were separated by means of cation-exchange chromatography using a 3.0mmol\\/L methanesulfonic acid solution as eluent and an IonPac CS17 column (250mm×4mm i.d.) as the separation column. Detection limits of dimethylamine, trimethylamine and trimethylamine-n-oxide were

Feng Li; Hong-ying Liu; Chang-hu Xue; Xue-qian Xin; Jie Xu; Yao-guang Chang; Yong Xue; Li-ang Yin



Principles and Methods Chromatography  

E-print Network

Edition AC 18-1022-29 Principles and Methods Affinity Chromatography #12;Antibody Purification-1142-75 Protein Purification Handbook 18-1132-29 Ion Exchange Chromatography Principles and Methods 18-1114-21 Affinity Chromatography Principles and Methods 18-1022-29 Hydrophobic Interaction Chromatography Principles

Lebendiker, Mario


Evaluation of the Botanical Authenticity and Phytochemical Profile of Black Cohosh Products by High-Performance Liquid Chromatography with Selected Ion Monitoring Liquid Chromatography–Mass Spectrometry  

PubMed Central

Black cohosh (Actaea racemosa L., syn. Cimicifuga racemosa L.) has become increasingly popular as a dietary supplement in the United States for the treatment of symptoms related to menopause, but the botanical authenticity of most products containing black cohosh has not been evaluated, nor is manufacturing highly regulated in the United States. In this study, 11 black cohosh products were analyzed for triterpene glycosides, phenolic constituents, and formononetin by high-performance liquid chromatography–photodiode array detection and a new selected ion monitoring liquid chromatography–mass spectrometry method. Three of the 11 products were found to contain the marker compound cimifugin and not cimiracemoside C, thereby indicating that these plants contain Asian Actaea instead of black cohosh. One product contained both black cohosh and an Asian Actaea species. For the products containing only black cohosh, there was significant product-to-product variability in the amounts of the selected triterpene glycosides and phenolic constituents, and as expected, no formononetin was detected. PMID:16637680

Jiang, Bei; Kronenberg, Fredi; Nuntanakorn, Paiboon; Qiu, Ming-Hua; Kennelly, Edward J.



A size exclusion-reversed phase two dimensional-liquid chromatography methodology for stability and small molecule related species in antibody drug conjugates.  


Antibody drug conjugates (ADCs) are complex therapeutic agents combining the specific targeting properties of antibodies and highly potent cytotoxic small molecule drugs to selectively eliminate tumor cells while limiting the toxicity to normal healthy tissues. One unique critical quality attribute of ADCs is the content of unconjugated small molecule drug present from either incomplete conjugation or degradation of the ADC. In this work, size exclusion chromatography (SEC) was coupled with reversed-phase (RP) HPLC in an online 2-dimensional chromatography format for identification and quantitation of unconjugated small molecule drugs and related small molecule impurities in ADC samples directly without sample preparation. The SEC method in the 1st dimension not only separated the small molecule impurities from the intact ADC, but also provided information about the size variants (monomer, dimer, aggregates, etc.) of the ADC. The small molecule peak from the SEC was trapped and sent to a RP-HPLC in the 2nd dimension to further separate and quantify the different small molecule impurities present in the ADC sample. This SEC-RP 2D-LC method demonstrated excellent precision (%RSD<2.0), linearity (r(2)=0.9999), sensitivity (LOQ of 0.05?g/mL of free drug in ADC sample) and accuracy (95-105% recovery of spiked samples). The 2D-LC method was further utilized to study the stability of an ADC drug product at different temperatures and pHs. Both small molecule degradation products and aggregation of the conjugate were observed in the stability samples and the degradation pathways of the ADC were investigated. This 2D-LC method offers a powerful tool for ADC characterization and provides valuable information for conjugation and formulation development. PMID:25818558

Li, Yi; Gu, Christine; Gruenhagen, Jason; Zhang, Kelly; Yehl, Peter; Chetwyn, Nik P; Medley, Colin D



Characterization of fatty acid and triacylglycerol composition in animal fats using silver-ion and non-aqueous reversed-phase high-performance liquid chromatography\\/mass spectrometry and gas chromatography\\/flame ionization detection  

Microsoft Academic Search

Fatty acid (FA) and triacylglycerol (TG) composition of natural oils and fats intake in the diet has a strong influence on the human health and chronic diseases. In this work, non-aqueous reversed-phase (NARP) and silver-ion high-performance liquid chromatography with atmospheric pressure chemical ionization mass spectrometry detection and gas chromatography with flame-ionization detection (GC\\/FID) and mass spectrometry detection are used for

Miroslav Lísa; Kate?ina Netušilová; Lukáš Fran?k; Hana Dvo?áková; Vladimír Vrkoslav; Michal Hol?apek



Ion Trace Detection Algorithm to Extract Pure Ion Chromatograms to Improve Untargeted Peak Detection Quality for Liquid Chromatography/Time-of-Flight Mass Spectrometry-Based Metabolomics Data.  


Able to detect known and unknown metabolites, untargeted metabolomics has shown great potential in identifying novel biomarkers. However, elucidating all possible liquid chromatography/time-of-flight mass spectrometry (LC/TOF-MS) ion signals in a complex biological sample remains challenging since many ions are not the products of metabolites. Methods of reducing ions not related to metabolites or simply directly detecting metabolite related (pure) ions are important. In this work, we describe PITracer, a novel algorithm that accurately detects the pure ions of a LC/TOF-MS profile to extract pure ion chromatograms and detect chromatographic peaks. PITracer estimates the relative mass difference tolerance of ions and calibrates the mass over charge (m/z) values for peak detection algorithms with an additional option to further mass correction with respect to a user-specified metabolite. PITracer was evaluated using two data sets containing 373 human metabolite standards, including 5 saturated standards considered to be split peaks resultant from huge m/z fluctuation, and 12 urine samples spiked with 50 forensic drugs of varying concentrations. Analysis of these data sets show that PITracer correctly outperformed existing state-of-art algorithm and extracted the pure ion chromatograms of the 5 saturated standards without generating split peaks and detected the forensic drugs with high recall, precision, and F-score and small mass error. PMID:25622715

Wang, San-Yuan; Kuo, Ching-Hua; Tseng, Yufeng J



A volatile organic analyzer for Space Station: Description and evaluation of a gas chromatography/ ion mobility  

NASA Technical Reports Server (NTRS)

A Volatile Organic Analyzer (VOA) is being developed as an essential component of the Space Station's Environmental Health System (EHS) air quality monitoring strategy to provide warning to the crew and ground personnel if volatile organic compounds exceed established exposure limits. The short duration of most Shuttle flights and the relative simplicity of the contaminant removal mechanism have lessened the concern about crew exposure to air contaminants on the Shuttle. However, the longer missions associated with the Space Station, the complex air revitalization system and the proposed number of experiments have led to a desire for real-time monitoring of the contaminants in the Space Station atmosphere. Achieving the performance requirements established for the VOA within the Space Station resource (e.g., power, weight) allocations led to a novel approach that joined a gas chromatograph (GC) to an ion mobility spectrometer (IMS). The authors of this paper will discuss the rational for selecting the GC/IMS technology as opposed to the more established gas chromatography/mass spectrometry (GC/MS) for the foundation of the VOA. The data presented from preliminary evaluations will demonstrate the versatile capability of the GC/IMS to analyze the major contaminants expected in the Space Station atmosphere. The favorable GC/IMS characteristics illustrated in this paper included excellent sensitivity, dual-mode operation for selective detection, and mobility drift times to distinguish co-eluting GC peaks. Preliminary studies have shown that the GC/IMS technology can meet surpass the performance requirements of the Space Station VOA.

Limero, Thomas F.; James, John T.



Comprehensive and reproducible phosphopeptide enrichment using iron immobilized metal ion affinity chromatography (Fe-IMAC) columns.  


Advances in phosphopeptide enrichment methods enable the identification of thousands of phosphopeptides from complex samples. Current offline enrichment approaches using TiO(2), Ti, and Fe immobilized metal ion affinity chromatography (IMAC) material in batch or microtip format are widely used, but they suffer from irreproducibility and compromised selectivity. To address these shortcomings, we revisited the merits of performing phosphopeptide enrichment in an HPLC column format. We found that Fe-IMAC columns enabled the selective, comprehensive, and reproducible enrichment of phosphopeptides out of complex lysates. Column enrichment did not suffer from bead-to-sample ratio issues and scaled linearly from 100 ?g to 5 mg of digest. Direct measurements on an Orbitrap Velos mass spectrometer identified >7500 unique phosphopeptides with 90% selectivity and good quantitative reproducibility (median cv of 15%). The number of unique phosphopeptides could be increased to more than 14,000 when the IMAC eluate was subjected to a subsequent hydrophilic strong anion exchange separation. Fe-IMAC columns outperformed Ti-IMAC and TiO(2) in batch or tip mode in terms of phosphopeptide identification and intensity. Permutation enrichments of flow-throughs showed that all materials largely bound the same phosphopeptide species, independent of physicochemical characteristics. However, binding capacity and elution efficiency did profoundly differ among the enrichment materials and formats. As a result, the often quoted orthogonality of the materials has to be called into question. Our results strongly suggest that insufficient capacity, inefficient elution, and the stochastic nature of data-dependent acquisition in mass spectrometry are the causes of the experimentally observed complementarity. The Fe-IMAC enrichment workflow using an HPLC format developed here enables rapid and comprehensive phosphoproteome analysis that can be applied to a wide range of biological systems. PMID:25394399

Ruprecht, Benjamin; Koch, Heiner; Medard, Guillaume; Mundt, Max; Kuster, Bernhard; Lemeer, Simone



An Interface for Sensitive Analysis of Monoamine Neurotransmitters by Ion-Pair Chromatography–ESI-MS with Continuous On-Line Elimination of Ion-Pair Reagents  

PubMed Central

A challenge in coupling ion-pair chromatography (IPC) on-line with electrospray ionization-mass spectrometry (ESI-MS) is that the nonvolatile ion-pair reagent (e.g., alkyl sulfate for amines or tetrabutylammonium for carboxylic acids) in the mobile phase suppresses the ESI-MS signals in the gas phase and their accumulation can clog the MS sampling interface. Consequently, IPC–ESI-MS is conducted either with a volatile ion-pair reagent, which could compromise the analyte separation efficiency, or with a downstream ion-exchange column to rid the ion-pair reagents of the mobile phase. In the latter approach, the limited capacity of ion-exchange columns requires frequent off-line column regeneration, which affects the separation throughput and prohibits long separations from being performed. A dual-valve, dual-ion exchange column interface of IPC–ESI-MS is designed for undisrupted separations and simultaneous column regeneration. Owing to the efficacy in removing the ion-pair reagent, the detection of eluents of monoamine neurotransmitters by an ion trap MS results in the limits of detection of 0.03 ?M for dopamine or DA and 0.01 ?M for 5-hydroxytryptamine or 5-HT. These values are lower than those obtained with ion trap MS of similar sensitivity when combined with the use of specialized chromatographic columns or sample preconcentration. Excellent reproducibility was attained with repeatedly regenerated ion-exchange columns (RSD = 4–6%) for an extended period of time (RSD < 6% for six days). DA and 5-HT in rat straital extracts were analyzed and our data demonstrate that interferences inherent in the tissues and the ion-pair reagent have been successfully eliminated. This simple interface should be readily amenable to the separation and MS analysis of other types of polar compounds in complex sample media. PMID:23767971

Shi, Shuyun; Zhao, Binqing; Yagnik, Gargey; Zhou, Feimeng



LC-IMS-MS Feature Finder: detecting multidimensional liquid chromatography, ion mobility and mass spectrometry features in complex datasets  

PubMed Central

Motivation: The addition of ion mobility spectrometry to liquid chromatography-mass spectrometry experiments requires new, or updated, software tools to facilitate data processing. Results: We introduce a command line software application LC-IMS-MS Feature Finder that searches for molecular ion signatures in multidimensional liquid chromatography-ion mobility spectrometry-mass spectrometry (LC-IMS-MS) data by clustering deisotoped peaks with similar monoisotopic mass, charge state, LC elution time and ion mobility drift time values. The software application includes an algorithm for detecting and quantifying co-eluting chemical species, including species that exist in multiple conformations that may have been separated in the IMS dimension. Availability: LC-IMS-MS Feature Finder is available as a command-line tool for download at The Microsoft.NET Framework 4.0 is required to run the software. All other dependencies are included with the software package. Usage of this software is limited to non-profit research to use (see README). Contact: Supplementary information: Supplementary data are available at Bioinformatics online. PMID:24008421

Crowell, Kevin L.; Slysz, Gordon W.; Baker, Erin S.; LaMarche, Brian L.; Monroe, Matthew E.; Ibrahim, Yehia M.; Payne, Samuel H.; Anderson, Gordon A.; Smith, Richard D.



Multielemental speciation analysis of fungi porcini (Boletus edulis) mushroom by size exclusion liquid chromatography with sequential on-line UV-ICP-MS detection.  


An analytical methodology to determine the molecular weight (MW) distribution patterns of several elements among different compounds present in commonly consumed edible mushrooms is presented in this work. A hyphenated technique based on size exclusion liquid chromatography (SEC) coupled on-line to UV and inductively coupled plasma mass spectrometry (ICP-MS) detection was used. The association of the elements to high and low MW fractions was confirmed with sequential detection by UV and ICP-MS. Separation of the fractions was performed by injecting a 100 microL sample volume to a Superdex 75 column. The effect of different mobile phases on the separation was evaluated. Additionally, three different extraction conditions including 0.05 mol L(-1) NaOH, 0.05 mol L(-1) HCl, and hot water at 60 degrees C were applied to extract the elemental species from the mushroom samples. Significant differences were observed in the chromatograms depending on the extraction conditions utilized. Optimization of the experimental variables involved in the SEC-UV-ICP-MS coupling was carried out. The method was applied to investigate the fractionation patterns of Bi, Co, Cu, Fe, I, Mo, Ni, Se, and Zn in fungi porcini (Boletus edulis) mushroom. The results obtained in this work indicate an important association of most of the elements to high MW fractions. PMID:14995139

Wuilloud, Rodolfo G; Kannamkumarath, Sasi S; Caruso, Joseph A



Study of pH effects on the evolution of properties of brown-water natural organic matter as revealed by size-exclusion chromatography during photocatalytic degradation.  


This study shows the effect of pH on the photocatalytic degradation of natural organic matter (NOM). The experiments were carried out in batch reactor (a solar UV-light simulator) with Degussa P-25 titanium dioxide (TiO2). The NOM degradation was followed by size-exclusion chromatography for dissolved organic carbon (DOC), ultraviolet absorption and fluorescence-detection (SEC-DOC, SEC-UV254 and SEC-Fl254/450). Changes in pH values affected the adsorption of NOM onto TiO2, but did not affect the photodegradation sequence of NOM. For high or low pH values, the degradation of the NOM preferentially removed the larger molecular size fraction in comparison to the middle and small molecular size fractions, resulting in the relative increase of these smaller fractions. This sequence of NOM degradation leads to the evolution of the formation potential for disinfection by-products (DBPs). Specifically, the trihalomethanes and halogenated organic compounds formation potential (THMF and AOXFP) decreased steadily. PMID:22209274

Valencia, Sergio; Marín, Juan; Velásquez, Jorge; Restrepo, Gloria; Frimmel, Fritz H



Evaluations of the TiO2/simulated solar UV degradations of XAD fractions of natural organic matter from a bog lake using size-exclusion chromatography.  


This work reports on the changes in compositions of humic acids (HAs) and fulvic acids (FAs) during photocatalytic degradation. The HAs and FAs were obtained from the XAD-resin fractionation of natural-organic matter (NOM) from a bog lake (Lake Hohloh, Black Forest, Germany). Degussa P-25 titanium dioxide (TiO2) in a suspension and a solar UV simulator (batch reactor) were used in the experiments. The photocatalytic degradation of the HAs and FAs were monitored using size-exclusion chromatography (SEC) equipped with dissolved organic carbon (DOC) and ultraviolet (UV254) detection (SEC-DOC and SEC-UV254) and UV-Vis spectrophotometry. The evolutions of the photocatalytic degradations of the HA and FA fractions were selective. The photocatalytic degradation started with the degradations of high molecular weight compounds with relatively high UV254 absorbances in the HA and FA fractions to yield low molecular weight compounds showing less specific UV254 absorbances. Observance of the same tendency for the original NOM from Lake Hohloh indicates that these XAD-fractions still having complex compound mixtures. However, the larger molecular weight fractions of the FAs showed higher preferential adsorptions onto TiO2, which caused their faster degradation rates. Furthermore, FAs showed a greater reduction of the total THM formation potential (TTHMFP) and the organic halogen compounds adsorbable on activated carbon formation potential (AOXFP), in comparison with the HAs. PMID:23863374

Valencia, Sergio; Marín, Juan M; Restrepo, Gloria; Frimmel, Fritz H



An Ultra-Trace Analysis Technique for SF6 Using Gas Chromatography with Negative Ion Chemical Ionization Mass Spectrometry.  


Sulfur hexafluoride (SF6) is widely used as a tracer gas because of its detectability at low concentrations. This attribute of SF6 allows the quantification of both small-scale flows, such as leakage, and large-scale flows, such as atmospheric currents. SF6's high detection sensitivity also facilitates greater usage efficiency and lower operating cost for tracer deployments by reducing quantity requirements. The detectability of SF6 is produced by its high molecular electronegativity. This property provides a high potential for negative ion formation through electron capture thus naturally translating to selective detection using negative ion chemical ionization mass spectrometry (NCI-MS). This paper investigates the potential of using gas chromatography (GC) with NCI-MS for the detection of SF6. The experimental parameters for an ultra-trace SF6 detection method utilizing minimal customizations of the analytical instrument are detailed. A method for the detection of parts per trillion (ppt) level concentrations of SF6 for the purpose of underground ventilation tracer gas analysis was successfully developed in this study. The method utilized a Shimadzu gas chromatography with negative ion chemical ionization mass spectrometry system equipped with an Agilent J&W HP-porous layer open tubular column coated with an alumina oxide (Al2O3) S column. The method detection limit (MDL) analysis as defined by the Environmental Protection Agency of the tracer data showed the method MDL to be 5.2 ppt. PMID:25452581

Jong, Edmund C; Macek, Paul V; Perera, Inoka E; Luxbacher, Kray D; McNair, Harold M



Analysis of di-n-butylphthalate biotransformation in cattle by liquid chromatography/ion trap mass spectrometry/mass spectrometry.  


The nature of products of contamination intake were investigated in cattle dosed with [14C]di-n-butylphthalate (DBP). Radio-labelled metabolites were extracted from bile, faeces, plasma and urine onto solid-phase media, fractionated by ion-exchange chromatography, separated by reverse phase HPLC and analysed by negative ion atmospheric pressure chemical ionization mass spectrometry(n) (LCQ, Finnigan). All matrices contained a common major metabolite [deprotonated molecular ion (M-H)- m/z 221] which coeluted with and had an identical daughter ion spectrum to reference monobutylphthalate (MBP). MBP was metabolised to a beta-glucuronidase sensitive compound (M-H)- m/z 397 whose spectrum contained daughter ions (m/z 175 and 221) consistent with the parent glucuronide. A further three beta-glucuronidase resistant radio-labelled metabolites were also produced (M-H- m/z 165, 193 and 237); comparison of daughter ion spectra with those of reference MBP and phthalic acid indicated identity with phthalic acid, monoethylphthalate (MEP) and monohydroxybutylphthalate (MHBP) respectively. The presence of a benzoate daughter ion (m/z 121) in all spectra was indicative of side chain biotransformation. Both MBP and MEP contained a phthalate daughter ion (m/z 165) indicating loss of a butyl and ethyl side chain respectively. A daughter ion of m/z 89 derived from the side chain provided evidence that the third metabolite was MHBP. Incubation of DBP with isolated bovine hepatocytes produced the same metabolites and provided relatively clean samples for LC/MSn analysis. Detection of these DBP metabolites in meat or dairy food products will provide evidence for environmental exposure and biotransformation in vivo, whereas the presence of the parent compound would suggest contamination during food processing and packaging. PMID:9768498

Coldham, N G; Dave, M; Sauer, M J




SciTech Connect

Radiological characterization and monitoring is an important component of environmental management activities throughout the Department of Energy complex. Gamma-ray spectroscopy is the technology most often used for the detection of radionuclides. However, radionuclides which cannot easily be detected by gamma-ray spectroscopy, such as pure beta emitters and transuranics, pose special problems because their quantification generally requires labor intensive radiochemical separations procedures that are time consuming and impractical for field applications. This project focused on a technology for measuring transuranics and pure beta emitters relatively quickly and has the potential of being field deployable. The technology combines ion exchange liquid chromatography and on-line alpha/beta pulse shape discriminating scintillation counting to produce simultaneous alpha and beta chromatograms. The basic instrumentation upon which the project was based was purchased in the early 1990's. In its original commercial form, the instrumentation was capable of separating select activation/fission products in ionic forms from relatively pure aqueous samples. We subsequently developed the capability of separating and detecting actinides (thorium, uranium, neptunium, plutonium, americium, and curium) in less than 30 minutes (Reboul, 1993) and realized that the potential time savings over traditional radiochemical methods for isolating some of these radionuclides was significant. However, at that time, the technique had only been used for radionuclide concentrations that were considerably above environmental levels and for aqueous samples of relatively high chemical purity. For the technique to be useful in environmental applications, development work was needed in lowering detection limits; to be useful in applications involving non-aqueous matrices such as soils and sludges or complex aqueous matrices such as those encountered in waste samples, development work was needed in sample preparation and processing. The general goal of this project was to address the issues mentioned above, and in so doing transform an interesting laboratory technique of limited applicability into a robust field instrument suitable for environmental restoration and waste management applications. The project consisted of the following tasks: (1) development of a low background, flow-cell detector, (2) identification of sample chemical and radiological interferences, (3) development of protocols for processing waste and/or environmental samples, and (4) integration and testing of the prototype system. The scope of work associated with these tasks has been completed and the report for Tasks 1-3 was submitted previously. Presented here are the results for Task 4.

R. A. Fjeld; T.A. DeVol; J.D. Leyba



The evaluation of novel microwave-induced plasma sources and the inductively-coupled plasma for element specific detection for capillary supercritical fluid chromatography and ion chromatography  

SciTech Connect

This dissertation involved two aspects of the development of plasma atomic emission detectors for chromatography. Four novel microwave cavities/devices were investigated to establish the positive features and limitations of each. The enhanced Beenakker cavity (EBC) was determined to be easiest to operate and tune. An annular helium plasma was produced in a concentric torch in the EBC, and 5 ppm phosphorus was detected in aqueous solutions introduced into the 85 W plasma by means of an ultrasonic nebulizer/desolvator. The annular plasma produces more efficient analyte excitation than a filament type of plasma, and had minimal contact with the torch walls, resulting in much lower silicon emission. Gaseous and supercritical fluid carbon dioxide were introduced into the helium plasmas in the EBC and the stripline cavity. The molecular background increased significantly due to CO and CO{sup +} systems, however, the increase in C{sub 2} molecular bands was not significant. A large analytically useful window exists in the background spectrum of the plasmas in the EBC and SLC with CO{sub 2} added from a capillary supercritical fluid chromatograph (SFC). The inductively coupled plasma (ICP) was interfaced to a capillary SFC. The argon plasma was optimized for Si(I) 251.6 nm emission to detect separated organosilicon compounds selectively. The linear dynamic concentration range for octamethylcyclotetra-siloxane was 10{sup 2}, with a detection limit of 5.8 ng Si injected. The relative standard deviations of the peak heights for repetitive injections were typically 1-5%. The effects of the CO{sub 2} pressure on the plasma stability and sensitivity, and upon the spectral background are presented. An ICP was also used as an element specific detector for ion chromatography. An analytical method is presented for the determination of Didronel (1-hydroxyethylidene-l,l-disodium diphosphonate, HEDP), in standard solutions and tablet dosage formulations.

Forbes, K.A.



Estimation of atmospheric inorganic water-soluble particulate matter in Muharraq Island, Bahrain, (Arabian Gulf), by ion chromatography  

NASA Astrophysics Data System (ADS)

Inorganic particulate matter was sampled weekly during the period, from March to August of 1996 at eight different sites on Muharraq Island at height of ˜8 m above the ground level. Muharraq is the second most populated of the islands in the country (after the Bahrain island), but in terms of population per square kilometer, it is the most densely populated. Deposited aerosols were chemically analysed by ion chromatography and a comparison was made between these sites. The results were in good correlation with the meteorological and surface features of Bahrain.

Ali-Mohamed, Ahmed Y.; Ali, Hussain A. N.


The quantitation of triazolam in postmortem blood by gas chromatography/negative ion chemical ionization mass spectrometry.  


A specific and sensitive assay has been developed to quantitate triazolam in postmortem blood using 2H6-triazolam as an internal standard. Triazolam is isolated from whole blood by adsorption on an Amberlite XAD-2 resin and subsequent elution with an organic solvent. The extract is analyzed by gas chromatography/mass spectometry using selected ion monitoring (GC/MS/SIM) in the negative chemical ionization mode (Cl-). The procedure is presently being used in case work and the results from 36 cases are presented. PMID:3807323

Koves, G; Wells, J



Determination of methylmercury in waters using sodium tetraphenylaborate derivatization/solvent extraction and gas chromatography-ion trap mass spectrometry  

SciTech Connect

An analytical approach involving aqueous-phase derivatization followed by gas chromatography/ion trap mass spectrometry (GC/ITMS) for the determination of methylmercury in waters is described. The aqueous-phase derivatization is based on the formation of a more hydrophobic compound between MeHg{sup +} and BPh{sub 4}{sup -}, i.e., MeHgPh, which is extractable into dichloromethane. The detection limit of the method for MeHg is 1 ng/mL for Hg when 100 ml water was analyzed. Recoveries from standard addition to tap water, lake water are 96 {+-} 8% and 92 {+-} 8%, respectively.

Guanglin Hu; Wang Xiaoru; Wang Yiru [Xiamen Univ. (China)] [and others



Use of gas chromatography-ion trap tandem mass spectrometry for the detection and characterization of microorganisms in complex samples  

Microsoft Academic Search

Gas chromatography-mass spectrometry (GC-MS) can be applied to detect and characterize microorganisms in clinical and environmental\\u000a samples, and microbial contaminants in biotechnological production cultures. With this approach, unique microbial monomeric\\u000a compounds, known as chemical markers, are used as analytes. In the present article, two GC-MS-based techniques, viz. GC-ion\\u000a trap tandem MS (GC-MS-MS) and conventional quadrupole GC-MS used in the selected

Lennart Larsson; Anita Saraf



An improved thin-layer chromatography/mass spectrometry coupling using a surface sampling probe electrospray ion trap system  

SciTech Connect

A combined surface sampling probe/electrospray emitter coupled with an ion trap mass spectrometer was used for the direct read out of unmodified reversed-phase C18 thin-layer chromatography (TLC) plates. The operation of the surface sampling electrospray ionization interface in positive and negative ionization modes was demonstrated through the direct analysis of TLC plates on which a commercial test mix comprised of four dye compounds viz., rhodamine B, fluorescein, naphthol blue black, and fast green FCF, and an extract of the caffeine-containing plant Ilex vomitoria, were spotted and developed. Acquisition of full-scan mass spectra and automated collection of MS/MS product ion spectra while scanning a development lane along the surface of a TLC plate demonstrated the advantages of using an ion trap in this combination. Details of the sampling system, benefits of analyzing a developed lane in both positive ion and negative ion modes, levels of detection while surface scanning, surface scan speed effects, and the utility of three-dimensional data display, are also discussed.

Ford, Michael J [ORNL; Van Berkel, Gary J [ORNL



Ion-exchange chromatography: basic principles and application to the partial purification of soluble mammalian prolyl oligopeptidase.  


Ion-exchange chromatography (IEC) allows for the separation of ionizable molecules on the basis of differences in charge properties. Its large sample-handling capacity, broad applicability (particularly to proteins and enzymes), moderate cost, powerful resolving ability, and ease of scale-up and automation have led to it becoming one of the most versatile and widely used of all liquid chromatography (LC) techniques. In this chapter, we review the basic principles of IEC, as well as the broader criteria for selecting IEC conditions. By way of further illustration, we outline protocols necessary to partially purify a serine peptidase from bovine whole brain cytosolic fraction, covering crude tissue extract preparation through to partial purification of the target enzyme using anion-exchange chromatography. Protocols for assaying total protein and enzyme activity in both pre- and post-IEC fractions are also described. The target serine peptidase, prolyl oligopeptidase (POP, EC3.4.21.26), is an 80-kDa enzyme with endopeptidase activity towards peptide substrates of ?30 amino acids. POP is a ubiquitous post-proline cleaving enzyme with particularly high expression levels in the mammalian brain, where it participates in the metabolism of neuroactive peptides and peptide-like hormones (e.g. thyroliberin, gonadotropin-releasing hormone). PMID:20978968

Cummins, Philip M; Dowling, Oonagh; O'Connor, Brendan F




Microsoft Academic Search

SUMMARY The equilibrium distribution coefficients (p-value) of D-arabinose between the water in sulfonate ion-exchange resin and the external aqueous solution vary with the nature of the five alkali metal counterions studied. The strongest exclusion (lowest p -value) is found in the Li+ resin and the least exclusion (highest p -value) in the Cs+ resin. The p-value decreases with the increasing



Two-dimensional separation of ionic species by hyphenation of capillary ion chromatography × capillary electrophoresis-mass spectrometry.  


The separation of complex mixtures such as biological or environmental samples requires high peak capacities, which cannot be established with a single separation technique. Therefore, multidimensional systems are in demand. In this work, we present the hyphenation of the two most important (orthogonal) techniques in ion analysis, namely, ion chromatography (IC) and capillary electrophoresis (CE), in combination with mass spectrometry. A modulator was developed ensuring a well-controlled coupling of IC and CE separations. Proof-of-concept measurements were performed using a model system consisting of nucleotides and cyclic nucleotides. The data are presented in a multidimensional contour plot. Analyte stacking in the CE separation could be exploited on the basis of the fact that the suppressed IC effluent is pure water. PMID:25708415

Beutner, Andrea; Kochmann, Sven; Mark, Jonas Josef Peter; Matysik, Frank-Michael



Hollow fiber flow field-flow fractionation and size-exclusion chromatography with MALS detection: A complementary approach in biopharmaceutical industry.  


Monoclonal antibodies (mAbs) are promising reagents both for the manufacture of drug substances and for their employment as a drug themselves, but to be approved for utilization, according to FDA recommendations and WHO guidelines, they have to undergo verifications regarding their purity, stability and percentage of aggregates. Moreover, stability tests of lots have to be performed in order to verify molecular size distribution over time and lot-to-lot consistency. Recent works in literature have highlighted the need for suitable, sensitive and reliable complementary analytical techniques for the characterization of mAbs and quantification of aggregates. Size-exclusion chromatography (SEC) is the reference technique in the biopharmaceutical industry for its robustness, high performance and simple use; however it presents some limitations especially toward the separation and detection of aggregates with high molecular weight. On the other hand, flow field-flow fractionation (F4) in its miniaturized version (hollow fiber flow field-flow fractionation, HF5) shows comparable performances with interesting additional advantages: a broad size range, gentle separation mechanism with low dilution factor and higher sensitivity. To propose HF5 as a complementary technique for evaluating aggregates' content in mAbs samples, a comparative study of both SEC and HF5 performances has been made. In this work, SEC and HF5 were coupled with UV and multi-angle light scattering detection and employed first in separating standard samples of proteins mixture used as a sample model. Then, a screening of mobile phases and an evaluation of separation performances was performed on a therapeutic mAbs formulation, demonstrating the complementarities between SEC and HF5 and their possible use as a separative platform approach for the characterization and quality control of protein drugs. PMID:25468501

Marassi, V; Roda, B; Zattoni, A; Tanase, M; Reschiglian, P



Self-association of long-acting insulin analogues studied by size exclusion chromatography coupled to multi-angle light scattering.  


Two structurally very different insulin analogues analysed here, belong to a class of analogues of which two have been reported to have a protracted action through self-assembly to high molar mass in subcutis. The process of self-association of insulin analogues Lys(B29) (N(?)?-carboxyheptadecanoyl) des(B30) human insulin and Lys(B29) (N(?)-lithocholyl) des(B30) human insulin was investigated using size exclusion chromatography (SEC) in connection with multi-angle light-scattering. Self-assembly to high molar mass was obtained by exchanging the formulation containing phenolic preservatives with an isotonic eluent during SEC. It was shown that increasing amounts of zinc in the formulations of the two analogues increased the size of the self assemblies formed during gel filtration. The addition of 0.2 mM phenol to the elution buffer slowed down the self-association process of zinc containing formulations and shed light on the initial association process. The results indicated that a dihexamer is a possible building block during self-association of Lys(B29) (N(?)?-carboxyheptadecanoyl) des(B30) human insulin. Surprisingly, in the absence of zinc the two analogues behaved very differently. Lys(B29) (N(?)?-carboxyheptadecanoyl) des(B30) human insulin was in equilibrium between oligomers smaller than a hexamer, whereas Lys(B29) (N(?)-lithocholyl) des(B30) human insulin self-associated and formed even larger complexes than in the presence of zinc. PMID:21937288

Jensen, Malene H; Wahlund, Per-Olof; Jacobsen, Jes K; Vestergaard, Bente; van de Weert, Marco; Havelund, Svend



Branched polymers characterized by comprehensive two-dimensional separations with fully orthogonal mechanisms: molecular-topology fractionation×size-exclusion chromatography.  


Polymer separations under non-conventional conditions have been explored to obtain a separation of long-chain branched polymers from linear polymers with identical hydrodynamic size. In separation media with flow-through channels of the same order as the size of the analyte molecules in solution, the separation and the elution order of polymers are strongly affected by the flow rate. At low flow rates, the largest polymers are eluted last. At high flow rates, they are eluted first. By tuning the channel size and flow rate, conditions can be found where separation becomes independent of molar mass or size of linear polymers. Long-chain branched polymers did experience lower migration rates under these conditions and can be separated from linear polymers. This type of separation is referred to as molecular-topology fractionation (MTF) at critical conditions. Separation by comprehensive two-dimensional molecular-topology fractionation and size-exclusion chromatography (MTF×SEC) was used to study the retention characteristics of MTF. Branching selectivity was demonstrated for three- and four-arm "star" polystyrenes of 3-5×10(6)g/mol molar mass. Baseline separation could be obtained between linear polymer, Y-shaped molecules, and X-shaped molecules in a single experiment at constant flow rate. For randomly branched polymers, the branching selectivity inevitably results in an envelope of peaks, because it is not possible to fully resolve the huge numbers of different branched and linear polymers of varying molar mass. It was concluded that MTF involves partial deformation of polymer coils in solution. The increased coil density and resistance to deformation can explain the different retention behavior of branched molecules. PMID:25282310

Edam, Rob; Mes, Edwin P C; Meunier, David M; Van Damme, Freddy A; Schoenmakers, Peter J



How does roasting affect the antioxidants of a coffee brew? Exploring the antioxidant capacity of coffee via on-line antioxidant assays coupled with size exclusion chromatography.  


During coffee roasting major changes occur in coffee bean composition. Among others dark coloured melanoidins are formed, which are high molecular weight Maillard reaction products. A new approach is presented here to monitor the influence of roasting conditions on the antioxidant capacity of melanoidins and chlorogenic acids (CGAs) in a coffee brew. Validated Folin-Ciocalteu (FC) and ABTS assays were used as on-line antioxidant assays coupled (post-column) with high performance size-exclusion chromatography (HPSEC). HPSEC enabled the separation of melanoidins from CGAs and the determination of the antioxidant capacity of each fraction, within a total elution time of 25 min. Besides the on-line assay measurements, both assays were also applied off-line with flow injection analysis (FIA). The maximum antioxidant capacity was determined to be at a light-to-medium roast degree, measured with both ABTS-FIA and FC-FIA assays as well as on-line ABTS assay. With FC on-line assay the maximum was found to be at a very light roast degree. Based on the peak areas obtained with the new coupled technique the roasting effects on the variability of melanoidin and CGA contents in coffee brews were studied. The majority of melanoidins are already formed in the early stage of the roasting process and the relative contribution of melanoidins to the total antioxidant capacity increases towards darker roasts, mainly because CGAs degrade during roasting. A new parameter, the ratio of melanoidin to CGA peak area, was introduced as a possible predictor of the roast degree. PMID:23592006

Smrke, Samo; Opitz, Sebastian E W; Vovk, Irena; Yeretzian, Chahan



Textural characterization of native and n-alky-bonded silica monoliths by mercury intrusion/extrusion, inverse size exclusion chromatography and nitrogen adsorption.  


Native and n-alkyl-bonded (n-octadecyl) monolithic silica rods with mesopores in the range between 10 and 25 nm and macropores in the range between 1.8 and 6.0 microm were examined by mercury intrusion/extrusion, inverse size exclusion chromatography (ISEC) and nitrogen sorption. Our results reveal very good agreement for the mesopore size distribution obtained from nitrogen adsorption (in combination with an advanced NLDFT analysis) and ISEC. Our studies highlight the importance of mercury porosimetry for the assessment of the macropore size distribution and show that mercury porosimetry is the only method which allows obtaining a combined and comprehensive structural characterization of macroporous/mesoporous silica monoliths. Our data clearly confirm that mercury porosimetry hysteresis and entrapment have different origin, and indicate the intrinsic nature of mercury porosimetry hysteresis in these silica monoliths. Within this context some silica monoliths show the remarkable result of no entrapment of mercury after extrusion from the mesopore system (i.e. for the first intrusion/extrusion cycle). The results of a systematic study of the mercury intrusion/extrusion behavior into native silica monoliths and monoliths with bonded n-alkyl groups reveals that the macro (through) pore structure, which controls the mass transfer to and from the mesopores, here mainly controls the entrapment behavior. Our data suggest that mercury intrusion/extrusion porosimetry does not only allow to obtain a comprehensive pore structure analysis, but can also serve as a tool to estimate the mass transport properties of silica monoliths to be employed in liquid-phase separation processes. PMID:18423477

Thommes, M; Skudas, R; Unger, K K; Lubda, D



A direct microassay for serum retinol (vitamin A alcohol) by using size-exclusion high-pressure liquid chromatography with fluorescence detection.  


Serum retinol (bound to plasma retinol-binding protein, RBP) can be determined by direct injection of as little as 20 microliter of serum or plasma by using size-exclusion high-pressure liquid chromatography (SE-HPLC) with fluorescence detection. Toyo Soda TSK G-3000SW columns (0.75 X 7.5-cm guard column plus 0.75 X 30-cm analytical column) were eluted with 0.2 M NaCl/0.01 M phosphate buffer (pH 6.8) at 1 ml/min, with detection at 280 nm for protein elution. Fluorescence of the retinol-RBP complex was monitored with excitation at 334 nm (interference filter) and emission at 425 nm (long-pass filter). The retinol-RBP complex eluted as two peaks, the holo-RBP-transthyretin complex (apparent molecular weight 70,000) and holo-RBP (apparent molecular weight 9000). Identities of these peaks were established by immunodiffusion assay of the proteins and by extraction and analysis of retinol. Nonideal interactions with the column packing seem to be responsible for the low apparent molecular weight of holo-RBP. The first peak predominated when large volumes of serum (100 to 250 microliters) were injected, and the second when small volumes (5 to 50 microliters) were analyzed. The integrated area of the two fluorescence peaks due to retinol bound to RBP was proportional to the volume of a serum sample injected over the range 5 to 250 microliters.(ABSTRACT TRUNCATED AT 250 WORDS) PMID:3407933

Furr, H C; Olson, J A



Simultaneous speciation of selenoproteins and selenometabolites in plasma and serum by dual size exclusion-affinity chromatography with online isotope dilution inductively coupled plasma mass spectrometry.  


A method for the simultaneous speciation of selenoproteins and selenometabolites in mouse plasma has been developed based on in series two-dimensional size exclusion and affinity high-performance liquid chromatography (2D/SE-AF-HPLC), using two columns of each type, and hyphenation to inductively coupled plasma-(quadrupole) mass spectrometry (ICP-QMS). The method allows the quantitative determination of selenoprotein P (SeP), extracellular glutathione peroxidase (eGPx), selenoalbumin (SeAlb), and selenometabolites in mouse plasma using species-unspecific isotope dilution (SUID). The 2D chromatographic separation is proposed to remove typical spectral interferences in plasma from chloride and bromide on (77)Se ((40)Ar(37)Cl) and (82)Se ((81)Br(1)H). In addition, the approach increases chromatographic resolution allowing the separation of eGPx from Se metabolites of low molecular mass. The method is robust, reliable, and fast with a typical chromatographic runtime less than 20 min. Precision in terms of relative standard deviation (n?=?5) is in the order of 4 %, and detection limits are in the range of 0.2 to 1.0 ng Se g(-1). Method accuracy for determination of total protein bound to Se was assessed by analyzing human serum reference material (BCR-637) certified for total Se content, and latterly applied to mouse plasma (Mus musculus). In summary, a reliable speciation method for the analysis of eGPx, selenometabolites, SeP, and SeAlb in plasma/serum samples is proposed for the first time and is applicable to the evaluation of Se status in human in clinical studies and other mammals for environmental or toxicological assessment. PMID:24535684

García-Sevillano, M A; García-Barrera, T; Gómez-Ariza, J L



Determination of metal--EDTA complexes in soil solution and plant xylem by ion chromatography-electrospray mass spectrometry.  


An ion chromatography-electrospray mass spectrometry (IC-MS) method was developed to quantify the metal complexes of ethylenediaminetetraacetic acid (EDTA) in soil solution and plant xylem exudate. Suitable separation of the metal-EDTA complexes was achieved on a Dionex AS5 column using 2 mM Na2CO3 as the eluant. However, satisfactory detection by eluant suppressed IC-MS, in either the positive or negative ion detection mode, could not be attained. A new eluant that still attained suitable separation and produced ionic species that could be detected by MS in the negative ion mode was developed. The eluant consisted of 2.5 mM (NH4)2CO3, 9.7 mM NH4OH, and 4% (v/v) methanol and had a pH 9.9. Even though eluant suppressed IC-MS degraded detection limits by a factor of 4 over the nonsuppressed system, using the retention time and not the m/z (mass-to-charge ratio) of the intact chelate for identification, the latter allowed the metal complexes to be detected intact and was optimized for the analysis of environmental samples. The number of metal-EDTA species that could be detected was limited by the eluant used for ion chromatography (i.e. only those complexes that were stable at high pH), with metal-EDTA complexes of Al, Cd, Cu, Co, Mn, Ni, Pb, and Zn being adequately resolved. Iron(III), Ca, MgEDTA, and EDTA itself were not detected. Detection limits for the various complexes ranged from 0.1 to 1 microM. PMID:11432569

Collins, R N; Onisko, B C; McLaughlin, M J; Merrington, G



Online spectrophotometric determination of Fe(II) and Fe(III) by flow injection combined with low pressure ion chromatography.  


A simple and new low pressure ion chromatography combined with flow injection spectrophotometric procedure for determining Fe(II) and Fe(III) was established. It is based on the selective adsorption of low pressure ion chromatography column to Fe(II) and Fe(III), the online reduction reaction of Fe(III) and the reaction of Fe(II) in sodium acetate with phenanthroline, resulting in an intense orange complex with a suitable absorption at 515nm. Various chemical (such as the concentration of colour reagent, eluant and reductive agent) and instrumental parameters (reaction coil length, reductive coil length and wavelength) were studied and were optimized. Under the optimum conditions calibration graph of Fe(II)/Fe(III) was linear in the Fe(II)/Fe(III) range of 0.040-1.0mg/L. The detection limit of Fe(III) and Fe(II) was respectively 3.09 and 1.55?g/L, the relative standard deviation (n=10) of Fe(II) and Fe(III) 1.89% and 1.90% for 0.5mg/L of Fe(II) and Fe(III) respectively. About 2.5 samples in 1h can be analyzed. The interfering effects of various chemical species were studied. The method was successfully applied in the determination of water samples. PMID:25523043

Chen, Shujuan; Li, Nan; Zhang, Xinshen; Yang, Dongjing; Jiang, Heimei



Direct separation and detection of biogenic amines by ion-pair liquid chromatography with chemiluminescent nitrogen detector.  


Analysis of biogenic amines is critical to pharmaceutical and food industry due to their biological importance. For many years, the determination of biogenic amines has relied on high performance liquid chromatography (HPLC) coupling with pre-, on-, or post-column derivatization procedures to enable UV or fluorescent detections. In this study, 14 biogenic amines were separated on a Phenomenex Luna Phenyl-Hexyl column by an ion-pair liquid chromatography method using perfluorocarboxylic acids as ion-pair reagents and detected by a chemiluminescent nitrogen detector (CLND). This direct separation and detection HPLC method eliminated the time consuming and cumbersome derivatization procedures. Compared with HPLC-UV (post-column derivatization with ninhydrin) and HPLC-charged aerosol detector (CAD) methods, this HPLC-CLND technique provided narrower peaks, better baselines, and improved separations and detections. Excellent linearity was acquired by CLND for each of the 14 biogenic amines ranging from less than 1 ng to about 1000 ng (on-column weights). The relative response factors determined by this LC-CLND method were proportional to the numbers of nitrogen atoms in each compound, which has been the characteristic of the equimolar determinations by CLND. In addition, a number of samples including beer, dairy beverage, herb tea, and vinegar were analyzed by the LC-CLND method with satisfactory precision and accuracy. PMID:21665217

Sun, Jingshun; Guo, Hong-Xun; Semin, David; Cheetham, Janet




EPA Science Inventory

The choice of gas chromatography (GC) detectors has expanded rapidly. The necessity for mass spectrometric (MS) characterization of GC effluents stems from the complexity of the matrices associated with environmental samples. There are currently several MS types being used in con...


Confirmation of clorsulon residues in cattle kidney by capillary gas chromatography-negative-ion chemical-ionization mass spectrometry.  


A confirmatory assay for residues of the anthelmintic agent clorsulon [4-amino-6-(trichloroethenyl)-1,3-benzenedisulfonamide] in cattle kidney tissue has been developed. The assay involves isolation of a drug-containing fraction by solvent extraction, methylation of the analyte, and fused-silica capillary column gas chromatography-negative-ion chemical-ionization mass spectrometry of the pentamethyl derivative of clorsulon. The intensities of four negative ions [m/z 406 and 408 (trichloro species) and m/z 413 and 415 (dichloro species)] are monitored. Confirmation of the presence of drug in an analyte requires that all four ions appear at the appropriate retention time with their intensity ratios within 10-15% of those arising from analysis of the reference standard, methylated clorsulon; the lower limit of detection is 3 ppb. Quantification of the drug is based on the intensity of the m/z 406 ion. Identification and quantification of residues by the gas chromatographic-mass spectrometric assay gave results in good agreement with those obtained with an electron-capture gas chromatographic assay. PMID:3654857

Wehner, T A; Wood, J S; Walker, R; Downing, G V; Vandenheuvel, W J



Novel algorithm for simultaneous component detection and pseudo-molecular ion characterization in liquid chromatography-mass spectrometry.  


Resolving components and determining their pseudo-molecular ions (PMIs) are crucial steps in identifying complex herbal mixtures by liquid chromatography-mass spectrometry. To tackle such labor-intensive steps, we present here a novel algorithm for simultaneous detection of components and their PMIs. Our method consists of three steps: (1) obtaining a simplified dataset containing only mono-isotopic masses by removal of background noise and isotopic cluster ions based on the isotopic distribution model derived from all the reported natural compounds in dictionary of natural products; (2) stepwise resolving and removing all features of the highest abundant component from current simplified dataset and calculating PMI of each component according to an adduct-ion model, in which all non-fragment ions in a mass spectrum are considered as PMI plus one or several neutral species; (3) visual classification of detected components by principal component analysis (PCA) to exclude possible non-natural compounds (such as pharmaceutical excipients). This algorithm has been successfully applied to a standard mixture and three herbal extract/preparations. It indicated that our algorithm could detect components' features as a whole and report their PMI with an accuracy of more than 98%. Furthermore, components originated from excipients/contaminants could be easily separated from those natural components in the bi-plots of PCA. PMID:25467485

Zhang, Yufeng; Wang, Xiaoan; Wo, Siukwan; Ho, Hingman; Han, Quanbin; Fan, Xiaohui; Zuo, Zhong



Analysis of Underivatized Amino Acids in Geological Samples Using Ion-Pairing Liquid Chromatography and Electrospray Tandem Mass Spectrometry  

NASA Astrophysics Data System (ADS)

The capability of detecting biomarkers, such as amino acids, in chemically complex field samples is essential to establishing the knowledge required to search for chemical signatures of life in future planetary explorations. However, due to the complexities of in situ investigations, it is important to establish a new analytical scheme that utilizes a minimal amount of sample preparation. This paper reports the feasibility of a novel and sensitive technique, which has been established to quantitate amino acids in terrestrial crust samples directly without derivatization using volatile ion-pairing liquid chromatography and tandem mass spectrometry equipped with an electrospray ionization source. Adequate separation of 20 underivatized amino acids was achieved on a C18 capillary column within 26 min with nonafluoropentanoic acid (NFPA) as ion-pairing reagent. Each amino acid was identified from its retention time as well as from its characteristic parent-to-daughter ion transition. Using tandem mass spectrometry as a detection technique allows co-elution of some amino acids, as it is more specific than traditional spectrophotometric methods. In the present study, terrestrial samples collected from 3 different locations were analyzed for their water-extractable free amino acid contents, following the removal of metal and organic interferences via ion exchange procedures. This is the first time that amino acids in geological samples were directly determined quantitatively without complicated derivatization steps. Depending on the amino acid, the detection limits varied from 0.02 to 5.7 pmol with the use of a 1 ?l sample injection loop.

Liu, De-Ling; Beegle, Luther W.; Kanik, Isik



Liquid chromatography and ion trap mass spectrometry for simultaneous and multiclass analysis of antimicrobial residues in feed water.  


This work firstly reported the development of liquid chromatography coupled to an ion trap mass spectrometer (LC-MS ion trap) for the simultaneous determination of nitrofurans (e.g. nitrofurazone (NFZ), nitrofurantoin (NFT), furazolidone (FZD) and furaltadone (FTD)), nitroimidazoles (e.g. metronidazole (MNZ), ronidazole (RNZ) and dimetridazole (DMZ)) and chloramphenicol (CAP) in feed water. Isotope-labeled internal standards for the corresponding target analytes were employed to prevent matrix effects that might lead to signal suppression/enhancement. High performance liquid chromatography (HPLC) analysis was performed on a Prodigy ODS-3 column, 2.0mm×150mm, 5?m with a guard cartridge at a flow rate of 0.2mL/min, column oven temperature of 40°C, and an injection volume of 10?L. Solid phase extraction (SPE) procedures, factors affecting HPLC separation (e.g. buffer pH and concentrations) and mass spectrometry (MS) parameters were optimized. After an off-line SPE by the OASIS HLB cartridges (with an enrichment factor of 400), the eight antimicrobial agents were separated in 18min using a gradient elution of acetonitrile in acidified water (pH 5.0). MS detection was by an ion trap MS coupled with electrospray ionization (ESI) in tandem mass spectrometry mode (MS/MS) using the nebulizer gas at 35psi, drying gas at 9L/min and drying temperature of 325°C. Method linearity was good (r(2)=0.979-0.999) with acceptable precision (% RSDs=3.4-26.6%) and accuracy (%recovery=88.4-110.1%). Very low limits of detection (LOD) and quantitation (LOQ) were achieved in ranges of 0.002-0.06?g/L and 0.005-0.25?g/L, respectively. The established method is successfully employed by the Department of Livestock Development of Thailand for the monitoring of the drug residues in feed waterbecause of its convenience, reliability and high sensitivity. PMID:24321758

Ardsoongnearn, Chusak; Boonbanlu, Ongart; Kittijaruwattana, Sunan; Suntornsuk, Leena



Separation of lead-203 from cyclotron-bombarded thallium targets by ion-exchange chromatography.  


A simple method is presented for the separation of lead-203 from copper-backed thallium cyclotron targets. The procedure involves cation-exchange chromatography in hydrochloric acid and hydrochloric acid-acetone mixtures. Further purification involves anion-exchange chromatography in nitric acid-hydrobromic acid mixtures. A cation-exchange column containing 3.0 g of resin can handle as much as 15 g of thallium and 160 mg of copper. An anion-exchange column containing 3.0 g of resin can separate lead from up to 200 mg of thallium and 10 mg of copper. Separations are extremely sharp and less than 0.1 mug of thallium and less than 0.1 mug of copper remain in the lead-203 fraction. PMID:18963189

van der Walt, T N; Strelow, F W; Haasbroek, F J



Analysis of methylisothiazolones by ion pair high-performance liquid chromatography after pre-column derivatisation  

Microsoft Academic Search

Summary 2-Methyl-3(2H)-isothiazolone resp. 5-chloro-2-methyl-3(2H)-isothiazolone were isolated from a commercial methylisothiazolone formulation (Kathon CG) by flash chromatography and subsequently converted into the respectiveß-thio-substituted acrylamide derivative with the help of the nucleophilic reagent hydrogensulfite. UV spectra and absorption characteristics, for both the derivates as well as the original methylisothiazolones are given and represented in comparison. The derivatives differ clearly in their absorption

Reinhard Matissek; Regine Nagorka; Ingrid Wengatz; Jeannette Rohde



Capability measurement of size-exclusion chromatography with a light-scattering detection method in a stability study of bevacizumab using the process capability indices.  


In this study, we investigated if the size-exclusion chromatography coupled with light-scattering and refractive index detection (SEC/LS/RI) method is fitted for its intended purpose and checked if the analytical method is able to provide enough conforming results. For this, the process capability indices Cp, Cpk, and Cpm were computed. The traditional X-chart and moving range (MR) chart were used by the same analyst to monitor the equipment in the laboratory over a 1-year period. For this, a bovine serum albumin (BSA) sample (0.3 mg mL(-1)) with a nominal Mw of 66.4 kDa was analyzed each working day. The results confirmed that the analytical method is in-control and stable. To determine whether the given process meets the present capability requirement and runs under the desired quality conditions, the Pearn and Shu (2003) method based on the lower confidence bound C on Cpm was used. The estimator Cpm was 1.81, and the lower confidence bound C was 1.40. We therefore conclude that the true value of the method capability Cpm is no less than 1.40 with a 95% level of confidence. This result indicates that the method is satisfactory and no stringent precision control is required. The usefulness of this method was applied in the characterization of bevacizumab commercial pharmaceutical preparations stored under different conditions that lead to aggregation. In this case, the computed Cpm index was 0.98 (0.70, 1.26), which indicates that the method does not comply with the specification limits and needs to be revised. The quality improvement effort should: (1) reduce the uncertainty in the absolute Mw determination; (2) either move the process mean closer to the target value or reduce the process variation, i.e. improve the method accuracy (?-T) and precision (?(2)). On this point, the Bayesian posterior distribution of the mean and standard deviation pointed out the need to control the precision but specially accuracy in order to reduce the overall uncertainty of analytical method and thus, the method is capable. PMID:24786652

Oliva, Alexis; Llabrés, Matías; Fariña, José B



Generic detection of basic taxoids in wood of European Yew (Taxus baccata) by liquid chromatography-ion trap mass spectrometry.  


The occurrence of the cardiotoxin taxine (comprising taxine B and several other basic taxoids) in leaves of Taxus baccata L. (European yew) is well known and has led to public concerns about the safety of eating or drinking from utensils crafted from the wood of this poisonous species. The occurrence of basic taxoids in the heartwood of T. baccata had not been examined in detail, although the bark is known to contain 2'?-deacetoxyaustrospicatine. Initial examination of heartwood extracts for 2'?-deacetoxyaustrospicatine by liquid chromatography-mass spectrometry (LC-MS) revealed the presence of this basic taxoid at about 0.0007% dry weight, using a standard isolated from bark. Analyses for taxine B, however, proved negative at the extract concentration analysed. Observing other basic taxoids within the heartwood extracts was facilitated by developing generic LC-MS methods that utilised a fragment arising from the N-containing acyl group of basic taxoids as a reporter ion. Of the various MS strategies available on a hybrid ion trap-orbitrap instrument that allowed observation of this reporter ion, combining all-ion collisions with high resolution ion filtering by the orbitrap was most effective, both in terms of the number of basic taxoids detected and sensitivity. Numerous basic taxoids, in addition to 2'?-deacetoxyaustrospicatine, were revealed by this method in heartwood extracts of T. baccata. Red wine readily extracted the basic taxoids from heartwood while coffee extracted them less efficiently. Contamination with basic taxoids could also be detected in soft cheese that had been spread onto wood. The generic LC-MS method for detecting basic taxoids complements specific methods for detecting taxine B when investigating yew poisoning cases in which the analysis of complex extracts may be required or taxine B has not been detected. PMID:23314400

Kite, Geoffrey C; Rowe, Emily R; Veitch, Nigel C; Turner, Jill E; Dauncey, Elizabeth A



Characterization of triglycerides in vegetable oils by silver-ion packed-column supercritical fluid chromatography coupled to mass spectroscopy with atmospheric pressure chemical ionization and coordination ion spray  

Microsoft Academic Search

Characterization of triglycerides in vegetable oils was achieved by silver-ion packed-column supercritical fluid chromatography (SI-pSFC) with mass spectrometric detection. Hyphenation was made using commercially available liquid chromatography–mass spectrometry (LC–MS) interfaces without any modification. A make-up fluid was delivered through a T-piece placed before or after the SFC restrictor by means of a high pressure pump. Atmospheric pressure chemical ionization (APCI)

P. Sandra; A. Medvedovici; Y. Zhao; F. David



Immobilized palladium(II) ion affinity chromatography for recovery of recombinant proteins with peptide tags containing histidine and cysteine.  


Fusion of peptide-based tags to recombinant proteins is currently one of the most used tools for protein production. Also, immobilized metal ion affinity chromatography (IMAC) has a huge application in protein purification, especially in research labs. The combination of expression systems of recombinant tagged proteins with this robust chromatographic system has become an efficient and rapid tool to produce milligram-range amounts of proteins. IMAC-Ni(II) columns have become the natural partners of 6xHis-tagged proteins. The Ni(II) ion is considered as the best compromise of selectivity and affinity for purification of a recombinant His-tagged protein. The palladium(II) ion is also able to bind to side chains of amino acids and form ternary complexes with iminodiacetic acid and free amino acids and other sulfur-containing molecules. In this work, we evaluated two different cysteine- and histidine-containing six amino acid tags linked to the N-terminal group of green fluorescent protein (GFP) and studied the adsorption and elution conditions using novel eluents. Both cysteine-containing tagged GFPs were able to bind to IMAC-Pd(II) matrices and eluted successfully using a low concentration of thiourea solution. The IMAC-Ni(II) system reaches less than 20% recovery of the cysteine-containing tagged GFP from a crude homogenate of recombinant Escherichia coli, meanwhile the IMAC-Pd(II) yields a recovery of 45% with a purification factor of 13. Copyright © 2014 John Wiley & Sons, Ltd. PMID:25277090

Kikot, Pamela; Polat, Aise; Achilli, Estefania; Fernandez Lahore, Marcelo; Grasselli, Mariano



Purification of a lectin from M. rubra leaves using immobilized metal ion affinity chromatography and its characterization.  


Lectins represent a heterogeneous group of proteins/glycoproteins with unique carbohydrate specificity, with wide range of biomedical applications. The multi-step purification protocols generally used for purification of lectin result in a significant reduction in the final yield and activity. In the present study, Morus rubra lectin (MRL) was purified to homogeneity from the leaves using a single-step immobilized metal ion affinity chromatography (IMAC) procedure. The approximate molecular weight of purified MRL resolved as a single band on SDS-PAGE was 52 kDa. Final percentage yield of purified lectin by IMAC was calculated as 74.7 %. Purified MRL was specific to three sugars, galactose, D-galactosamine and N-acetyl-D-galactosamine, and rendered haemagglutination (HA) activity towards different human blood group RBCs. MRL showed stability over a wide range of temperature (up to 80 °C) and pH (4-11). Chelation of the lectin with EDTA did not alter HA which indicates that metal ion is not required for activity. In the presence of Fe(2+), Ca(2+), Zn(2+), Ni(2+), Mn(2+), Na(+) and K(+), HA activity was reduced to 50 %, whereas the presence of trivalent metal ions (Fe3(+) and Al(3+)) and Cu(2+) did not affect the activity. In the presence of Mg(2+) and Hg(2+), only 25 % of HA activity remained. PMID:23070714

Sureshkumar, Thavamani; Priya, Sulochana



Diagnostic ion filtering to characterize ginseng saponins by rapid liquid chromatography with time-of-flight mass spectrometry.  


As one of the most commonly used medicinal plants, ginseng has been an attractive model herb for study. A wide range of analytical methods has been used to characterize its constituents. However, less effort has been devoted to the rare ginseng saponins, especially their isomers and sugar linkages. In this study, we used segmental monitoring and diagnostic ion filtering to characterize ginseng saponins by rapid liquid chromatography with time-of-flight mass spectrometry (LC-TOF-MS). By using selected diagnostic ions, specific groups of ginseng saponins were readily extracted from the complicated matrix. 20(R) and 20(S) stereo-saponins were differentiated using the peak abundance ratio of [M-H(2)O+H](+) to [M-2H(2)O+H](+). The fragmentation behavior of ginsenosides was first reported in negative ion mode by MS/MS with high-energy collision-induced dissociation, producing rules to determine sugar numbers, positions and linkages. Using the rules, we identified and compared the nontarget ginseng saponin profiling of raw and steamed American ginseng roots and berries. We characterized 70 saponins in the samples. Our strategy can be extended to screen and characterize other rare ginseng saponins and their metabolites. PMID:22349142

Qi, Lian-Wen; Wang, Huai-You; Zhang, Hui; Wang, Chong-Zhi; Li, Ping; Yuan, Chun-Su



Metabolomic analysis via reversed-phase ion-pairing liquid chromatography coupled to a stand alone orbitrap mass spectrometer  

PubMed Central

We present a liquid chromatography-mass spectrometry (LC-MS) method that capitalizes on the mass-resolving power of the orbitrap to enable sensitive and specific measurement of known and unanticipated metabolites in parallel, with a focus on water soluble species involved in core metabolism. The reversed phase LC method, with a cycle time 25 min, involves a water-methanol gradient on a C18 column with tributylamine as the ion pairing agent. The MS portion involves full scans from 85 – 800 m/z at 1 Hz and 100,000 resolution in negative ion mode on a stand alone orbitrap (“Exactive”). The median limit of detection, across 80 metabolite standards, was 5 ng/mL with linear range typically ? 100-fold. For both standards and a cellular extract from Saccharomyces cerevisiae (Baker’s yeast), the median inter-run relative standard deviation in peak intensity was 8%. In yeast exact, we detected 137 known compounds, whose 13C-labeling patterns could also be tracked to probe metabolic flux. In yeast engineered to lack a gene of unknown function (YKL215C), we observed accumulation of an ion of m/z 128.0351, which we subsequently confirmed to be oxoproline, resulting in annotation of YKL215C as an oxoprolinase. These examples demonstrate the suitability of the present method for quantitative metabolomics, fluxomics, and discovery metabolite profiling. PMID:20349993

Lu, Wenyun; Clasquin, Michelle F.; Melamud, Eugene; Amador-Noguez, Daniel; Caudy, Amy A.; Rabinowitz, Joshua D.



A solid phase extraction-ion chromatography with conductivity detection procedure for determining cationic surfactants in surface water samples.  


A new analytical procedure for the simultaneous determination of individual cationic surfactants (alkyl benzyl dimethyl ammonium chlorides) in surface water samples has been developed. We describe this methodology for the first time: it involves the application of solid phase extraction (SPE-for sample preparation) coupled with ion chromatography-conductivity detection (IC-CD-for the final determination). Mean recoveries of analytes between 79% and 93%, and overall method quantification limits in the range from 0.0018 to 0.038 ?g/mL for surface water and CRM samples were achieved. The methodology was applied to the determination of individual alkyl benzyl quaternary ammonium compounds in environmental samples (reservoir water) and enables their presence in such types of waters to be confirmed. In addition, it is a simpler, less time-consuming, labour-intensive, avoiding use of toxic chloroform and significantly less expensive methodology than previously described approaches (liquid-liquid extraction coupled with liquid chromatography-mass spectrometry). PMID:24148395

Olkowska, Ewa; Polkowska, ?aneta; Namie?nik, Jacek



Detection of anionic energetic material residues in enhanced fingermarks on porous and non-porous surfaces using ion chromatography.  


The ability to link criminal activity and identity using validated analytical approaches can be of great value to forensic scientists. Herein, the factors affecting the recovery and detection of inorganic and organic energetic material residues within chemically or physically enhanced fingermarks on paper and glass substrates are presented using micro-bore anion exchange chromatography with suppressed conductivity detection. Fingermarks on both surfaces were enhanced using aluminium powder or ninhydrin after spiking with model test mixtures or through contact with black-powder substitutes. A quantitative study of the effects of environmental/method interferences, the sweat matrix, the surface and the enhancement technique on the relative anion recovery of forensically relevant species is presented. It is shown that the analytical method could detect target analytes at the nanogram level even within excesses of enhancement reagents and their reaction products when using solid phase extraction and/or microfiltration. To our knowledge, this work demonstrates for the first time that ion chromatography can detect anions in energetic materials within fingermarks on two very different surfaces, after operational enhancement techniques commonly used by forensic scientists and police have been applied. PMID:23890630

Love, Catherine; Gilchrist, Elizabeth; Smith, Norman; Barron, Leon



Liquid chromatography–ion trap tandem mass spectrometry for the characterization of polypeptide antibiotics of the colistin series in commercial samples  

Microsoft Academic Search

A selective reversed-phase liquid chromatography–tandem mass spectrometry method is described for the characterization of related substances in the colistin complex. Mass spectral data were acquired on an LCQ ion trap mass spectrometer equipped with an electrospray ionization probe operated in the positive ion mode. The main advantage of this technique is the characterization of novel related substances without time-consuming isolation

Cindy Govaerts; Jennifer Orwa; Ann Van Schepdael; Eugène Roets; Jos Hoogmartens



Nano TiO 2-based preconcentration for the speciation analysis of inorganic selenium by using ion chromatography with conductivity detection  

Microsoft Academic Search

A simple, sensitive, and cost-effective analytical method was developed for the speciation analysis of inorganic selenium by combining a nano-TiO2 preconcentration with an ion chromatography-conductivity detection (IC-CD) system. The experimental conditions for the simultaneous adsorption and desorption of Se(IV) and Se(VI) were carefully investigated. Under the established optimum condition, the Se(IV) and Se(VI) ions could been simultaneously adsorbed onto the

Shuxia Xu; Maoli Zheng; Xinfeng Zhang; Junlong Zhang; Yong-Ill Lee


Separation and Detection of Some Phenoxyacid Herbicides and Plant Growth Regulators by Ion-Pair Reversed-Phase Thin-Layer Chromatography  

Microsoft Academic Search

Separation and detection of phenoxyacid herbicides such as 4-chlorophenoxyacetic, 2,4-dichlorophenoxyacetic, phenoxyacetic, 2,4,5-trichlorophenoxyacetic, trichloroacetic acids and plant growth regulators such as benzoic, cinnamic, gallic, indole-3-acetic, indole-3-propionic, ?-naphthaleneacetic, ?-naphthalenaecetic, ?-naphthoxyacetic acids have been made by ion-pair reversed-phase thin-layer chromatography on calcium sulphate coating impregnated with an ion-pair reagent cetrimide and different oils such as coconut oil, olive oil, paraffin oil and silicon

H. S. Rathore; I. Ali; S. R. Sharma; S. K. Saxena



Preparation of Fluorescein Isothiocyanate-Labeled ?-Globulin by Dialysis, Gel Filtration, and Ion-Exchange Chromatography in Combination  

PubMed Central

Dedmon, Robert E. (Presbyterian-St. Luke's Hospital, Chicago, Ill.), Albert W. Holmes, and Friedrich Deinhardt. Preparation of fluorescein isothiocyanate-labeled ?-globulin by dialysis, gel filtration, and ion-exchange chromatography in combination. J. Bacteriol. 89:734–739. 1965.—Antiviral immune ?-globulins isolated from rabbit and guinea pig sera were labeled through dialysis membranes with fluorescein isothiocyanate and purified in several ways to eliminate nonspecific staining. Gel filtration of the conjugate with Sephadex G-25 coarse beads followed by column fractionation with diethylaminoethyl-Sephadex yielded consistently highly specific staining materials. Fluorescein-protein ratios varied between 1.0 and 4.0. This technique has proved to be simple and reliable, and is less time-consuming than previous techniques. PMID:14273654

Dedmon, Robert E.; Holmes, Albert W.; Deinhardt, Friedrich



Analysis of polyphenolic antioxidants from the fruits of three pouteria species by selected ion monitoring liquid chromatography-mass spectrometry.  


Pouteria campechiana, Pouteria sapota, and Pouteria viridis are tropical plants in the Sapotaceae family that bear edible fruits. The fresh fruits of these three Pouteria species were each extracted, and activity-guided fractionations were performed to identify the antioxidant constituents. Seven polyphenolic antioxidants, gallic acid (1), (+)-gallocatechin (2), (+)-catechin (3), (-)-epicatechin (4), dihydromyricetin (5), (+)-catechin-3-O-gallate (6), and myricitrin (7), were isolated and identified. Extracts of the three Pouteria fruits were analyzed by a selected ion monitoring liquid chromatography-mass spectrometry method to quantify their polyphenolic antioxidants. The highest level of the seven measured polyphenols was found in P. sapota, the second highest in P. viridis, and the lowest in P. campechiana. The levels of the seven polyphenols corresponded with the results of the 1,1-diphenyl-2-picrylhydrazyl assay, by which P. sapota had the highest antioxidant activity, P. viridis the second highest, and P. campechiana the lowest. PMID:15366835

Ma, Jun; Yang, Hui; Basile, Margaret J; Kennelly, Edward J



Retention study of some cation-type compounds using bile acid sodium salts as ion pairing agents in liquid chromatography.  


The possibility of forming ion-pairs between bile acids (sodium taurocholate, sodium taurodeoxycholate and sodium taurochenodeoxycholate) and different compounds (pralidoxime, obidoxime and pyridostigmine) having a cationic character has been studied in reversed-phase liquid chromatography (RP-LC). This study can be useful in understanding the role of bile acids in the transport of ionic species through hydrophobic membrane. The present study focused on the influence of mobile phase composition on the retention parameters of chosen compounds (percentage of acetonitrile, pH of aqueous component or ionic strength). For constant concentration of bile acids in aqueous component of mobile phase the functional dependencies between the logarithm of the retention factor (k) and the methanol content in the mobile phase followed a binomial pattern (U-shaped), with a minimum positioned within the interval 70-85% methanol. PMID:20960581

Radulescu, Medeea; Voicu, Victor; Medvedovici, Andrei; David, Victor



Validation of a gas chromatography—Ion trap tandem mass spectrometry for simultaneous analyse of cocaine and its metabolites in saliva  

Microsoft Academic Search

Cocaine (COC) is one of the most widely used drugs of abuse. Therefore numerous procedures are published in the literature to propose an analysis of this substance and related compounds in different matrixes. In the same way, the authors have described, in a previous work, the simultaneous analysis of COC and three of its metabolites in hair by gas chromatography–ion-trap

Emmanuelle Cognard; Stéphane Bouchonnet; Christian Staub




EPA Science Inventory

The objective of this research was to evaluate, in the laboratory, the potential of gas chromatography/ion mobility spectrometry (GC/IMS) for monitoring vinyl chloride and other organic compounds in air samples in the field. It was determined that GC/IMS has the potential to dire...


Profiling the indole alkaloids in yohimbe bark with ultra-performance liquid chromatography coupled with ion mobility quadrupole time-of-flight mass spectrometry  

Technology Transfer Automated Retrieval System (TEKTRAN)

An ultra-high performance liquid chromatography-ion mobility- quadrupole time-of-flight mass spectrometry (UHPLC-IM-QTOF-MS) method was developed for profiling the indole alkaloids in yohimbe bark. Many indole alkaloids with the yohimbine core structure, plus methylated, oxidized, and reduced speci...


Ligand-Exchange Chromatography of Aromatic Amines on Resin-Bound Cobalt Ion  

Microsoft Academic Search

The use of cobalt metal for the selective separation of aromatic amines is completed with a chemically bonded diamine and glyoxime functional groups onto Lycopodium clavatum. Oximes and amines are excellent complexing agents for transition metal ions. Cobalt(II) metal ions can easily be immobilized on bis-diami-noethyl-glyoximated sporopollenin (bDAEG-sporopollenin). The ligand-exchange behavior of modified Lycopodium clavatum with respect to aromatic amines

Erol Pehlivan; Ufuk S. Vural; Ahmet Ayar; Salih Yildiz



Ion size effects at ionic exclusion from dielectric interfaces and slit nanopores  

E-print Network

A previously developed field-theoretic model [R.D. Coalson et al., J. Chem. Phys. 102, 4584 (1995)] that treats core collisions and Coulomb interactions on the same footing is investigated in order to understand ion size effects on the partition of neutral and charged particles at planar interfaces and the ionic selectivity of slit nanopores. We introduce a variational scheme that can go beyond the mean-field (MF) regime and couple in a consistent way pore modified core interactions, steric effects, electrostatic solvation and image-charge forces, and surface charge induced electrostatic potential. We show that in the dilute limit, the MF and the variational theories agree well with MC simulation results, in contrast to a recent RPA method. The partition of charged Yukawa particles at a neutral dielectric interface (e.g air-water or protein-water interface) is investigated. It is shown that as a result of the competition between core collisions that push the ions towards the surface, and repulsive solvation and image forces that exclude them from the interface, a concentration peak of finite size ions sets in close to the dielectric interface. We also characterize the role played by the ion size on the ionic selectivity of neutral slit nanopores. We show that the complex interplay between electrostatic forces, excluded volume effects induced by core collisions and steric effects leads to an unexpected reversal in the ionic selectivity of the pore with varying pore size: while large pores exhibits a higher conductivity for large ions, narrow pores exclude large ions more efficiently than small ones.

Sahin Buyukdagli; C. V. Achim; T. Ala-Nissila



Characterization of diacylglycerol isomers in edible oils using gas chromatography-ion trap electron ionization mass spectrometry.  


Verifying the authenticity of edible oils is of international concern. A new quality control standard for olive oil has been proposed that relates the ratio of 1,2-diacylglycerol (DAG) to 1,3-DAG to sensory aspects of olive oil. DAGs and their isomers are difficult to quantitate and characterize by Flame Ionization Gas Chromatography (GC-FID) due to the lack of suitable standards. Mass detectors offer the advantage of providing structural detail to the eluding DAG(s), thus removing ambiguity to the identification of both resolved and unresolved DAGs in GC chromatograms. In this study, a GC Electron Ionization Mass Spectrometry (GC-EI-MS) method was developed to determine the fatty acid composition and molecular structure of trimethylsilyl (TMS) derivatized DAGs present in edible oils. Twenty-two species of DAG isomers were identified in refined coconut oil and unrefined olive oil utilizing signature fragment ions, [M-15](+), [M-89](+), [M-RCO2](+), [RCO2+58](+) and [M-RCO2CH2](+). The [M-RCO2CH2](+) ion is considered the key diagnostic ion to distinguish between DAG positional isomers. MS/MS spectra of [M-RCO2](+) and [M-15](+) ions obtained from commercial standards containing both 1,2- and 1,3-DAG isomers were used as a model system to confirm the identification of DAG isomers in natural products. Furthermore, a number of reaction mechanisms are proposed to explain the formation of the most abundant mass fragments of DAGs and their isomers. PMID:23880469

Zhu, Hanjiang; Clegg, Michael S; Shoemaker, Charles F; Wang, Selina C



Analysis of underivatized amino acids in geological samples using ion-pairing liquid chromatography and electrospray tandem mass spectrometry.  


The capability of detecting biomarkers, such as amino acids, in chemically complex field samples is essential to establishing the knowledge required to search for chemical signatures of life in future planetary explorations. However, due to the complexities of in situ investigations, it is important to establish a new analytical scheme that utilizes a minimal amount of sample preparation. This paper reports the feasibility of a novel and sensitive technique, which has been established to quantitate amino acids in terrestrial crust samples directly without derivatization using volatile ion-pairing liquid chromatography and tandem mass spectrometry equipped with an electrospray ionization source. Adequate separation of 20 underivatized amino acids was achieved on a C(18) capillary column within 26 min with nonafluoropentanoic acid (NFPA) as ion-pairing reagent. Each amino acid was identified from its retention time as well as from its characteristic parent-to-daughter ion transition. Using tandem mass spectrometry as a detection technique allows co-elution of some amino acids, as it is more specific than traditional spectrophotometric methods. In the present study, terrestrial samples collected from 3 different locations were analyzed for their water-extractable free amino acid contents, following the removal of metal and organic interferences via ion exchange procedures. This is the first time that amino acids in geological samples were directly determined quantitatively without complicated derivatization steps. Depending on the amino acid, the detection limits varied from 0.02 to 5.7 pmol with the use of a 1 microl sample injection loop. PMID:18393689

Liu, De-Ling; Beegle, Luther W; Kanik, Isik



Exclusive processes in electron-ion collisions in the dipole formalism  

SciTech Connect

We compare the predictions of two saturation models for production of vector mesons and of photons in electron-ion collisions. The models considered are the b-CGC and the rcBK. The calculations were made in the kinematical range of the LHeC and of the future eRHIC.

Cazaroto, E. R.; Navarra, F. S. [Instituto de Fisica, Universidade de Sao Paulo, C.P. 66318, 05314-970 Sao Paulo, SP (Brazil); Carvalho, F. [Departamento de Ciencias Exatas e da Terra, Universidade Federal de Sao Paulo, Campus Diadema, Rua Prof. Artur Riedel, 275, Jd. Eldorado, 09972-270 Diadema, SP (Brazil); Goncalves, V. P. [Instituto de Fisica e Matematica, Universidade Federal de Pelotas, Caixa Postal 354, 96010-900 Pelotas, RS (Brazil)




EPA Science Inventory

Determination of carboxylic acids using non-suppressed conductivity and UV detections is described. he background conductance of I-octanesulfonic acid, hexane sulfonic acid and sulfuric acid at varying concentrations was determined. sing 0.2 MM I-octanesulfonic acid as a mobile p...



EPA Science Inventory

Determination of carboxylic acids using non-suppressed conductivity and UV detections is described. The background conductance of 1-octanesulfonic acid, hexane sulfonic acid and sulfuric acid at varying concentrations was determined. Using 0.2 mM 1-octanesulfonic acid as a mobile...


Ion exchange chromatography and radioimmunoassay procedure for measuring opioid peptides and substance P  

SciTech Connect

The measurements of peptides of the enkephalin, dynorphin and substance P systems is complicated by the number of possible precursor fragments and degradation products that might cross-react with the antisera. By using an ion-exchanger step before radioimmunoassay one can reduce the possibility that observed peptide levels are due to precursors or metabolites. The ion-exchanger method runs with good recovery and its main advantage is that many samples can be run in parallel. The recovery from the ion-exchanger was similar using two different homogenizing media, whereas the measured endogenous levels of (Met) and (Leu)enkephalin were 3-4 fold higher with 1M acetic acid than when a 1:1 MeOH/HCl mixture was used for tissue extraction.

Bergstroem, L.; Christensson, I.; Folkesson, R.; Stenstroem, B.; Terenius, L.



Determination of scopolamine in human serum by gas chromatography-ion trap tandem mass spectrometry.  


The objective of this study was to develop a very sensitive and selective method for the determination of scopolamine in serum with a rapid and simple sample preparation. A capillary column gas chromatographic-ion trap tandem mass spectrometric technique has been applied. Scopolamine and the internal standard mexiletine were extracted from serum samples and cleaned up by using a single step liquid-liquid extraction. Derivatization was carried out using 2,2,2-trifluoro-N-methyl-N-trimethylsilylacetamide. The mass spectrometer was operated with positive ions in the selected reaction mode with chemical ionisation using methane. The sum of peak height of two daughter ions was used for quantification. The detection limit was 50 pg/ml in serum. PMID:8844418

Oertel, R; Richter, K; Ebert, U; Kirch, W



Ligand-exchange chromatography of aromatic amines on resin-bound cobalt ion  

SciTech Connect

The use of cobalt metal for the selective separation of aromatic amines is completed with a chemically bonded diamine and glyoxime functional groups onto Lycopodium clavatum. Oximes and amines are excellent complexing agents for transition metal ions. Cobalt(II) metal ions can easily be immobilized on bis-diaminoethyl-glyoximated sporopollenin (bDAEG-sporopollenin). The ligand-exchange behavior of modified Lycopodium clavatum with respect to aromatic amines was investigated. This will permit the evaluation of bDAEG-sporopollenin ligand exchangers for their utilization as sorbents in the recovery, pollution control, and elimination of amines from wastewater.

Pehlivan, E.; Vural, U.S.; Ayar, A.; Yildiz, S. [Selcuk Univ., Konya (Turkey)



Phenolic profile characterization of chemlali olive stones by liquid chromatography-ion trap mass spectrometry.  


Aqueous methanol extracts of Chemlali olive stones were analyzed by reverse phase high-performance liquid chromatography (HPLC) with diode array detection and mass spectrometry [LC-MS/MS]. Oleoside, oleoside 11-methyl ester, nuezhenide, oleoside 11-methyloleoside, nuezhenide 11-methyloleoside, oleuropein, and glycosides of tryosol and hydroxytyrosol glycosides were identified in stones of Chemali olives. The antioxidant activity observed for the extract of the olive stones (IC50 = 13.84 ?g/mL, TEAC = 0.436 mM) may be due to the high content of phenolic compounds, of which the main compounds are nuezhenide (325.78 mg/100g), methoxy derivative of nuezhenide (132.46 mg/100g), and nuezhenide-11-methyloleoside (82.91 mg/100g). These results suggest the use of olive stones as sources of natural antioxidants. PMID:25650173

Ben Mansour, Amir; Porter, Elaine A; Kite, Geoffrey C; Simmonds, Monique S J; Abdelhedi, Ridha; Bouaziz, Mohamed



Simultaneous characterization of pyrrolizidine alkaloids and N-oxides in Gynura segetum by liquid chromatography/ion trap mass spectrometry.  


Gynura segetum (Lour.) Merr. (Jusanqi) is a traditional herbal product used for hemostasis and detumescence in Chinese folk medicine. However, its hepatic toxicity should not be ignored. In this study, pyrrolizidine alkaloids (PAs) and their corresponding N-oxides (PANOs) were extracted from the whole plant of G. segetum and analyzed by high-performance liquid chromatography coupled to ion trap mass spectrometry (ITMS). Identification of eluted peaks as PANOs was indicated by virtue of their MS and MS(n) analysis, in addition to the [M+H](+) adduct ion, characteristically showed a significant (usually 100% abundance) dimer adduct [2M+H](+) that is not observed in the MS of the parent PAs. A total of 20 compounds were identified or tentatively characterized based on their mass spectra and possible biosynthetic pathways, of which three PAs and one PANO, namely seneciphylline, senecionine, seneciphylline and seneciphyllinine N-oxide, were unequivocally characterized, while other PAs and PANOs were tentatively assigned. Sixteen constituents were reported for the first time from G. segetum and tetrahydrosenecionine has not been previously reported as a natural product. Our results are the first comprehensive analysis of PAs and PANOs in G. segetum constituents and will be helpful for the quality control of the herb of G. segetum and its related preparations. PMID:19072862

Qi, Xueyong; Wu, Bin; Cheng, Yiyu; Qu, Haibin



Ion chromatography-mass spectrometry: a review of recent technologies and applications in forensic and environmental explosives analysis.  


The development and application of ion chromatography (IC) coupled to mass spectrometry (MS) is discussed herein for the quantitative determination of low-order explosives-related ionic species in environmental and forensic sample types. Issues relating to environmental explosives contamination and the need for more confirmatory IC-MS based applications in forensic science are examined. In particular, the compatibility of a range of IC separation modes with MS detection is summarised along with the analytical challenges that have been overcome to facilitate determinations at the ng-?g L(-1) level. Observed trends in coupling IC to inductively coupled plasma and electrospray ionisation mass spectrometry form a particular focus. This review also includes a discussion of the relative performance of reported IC-MS methods in comparison to orthogonal ion separation-based, spectrometric and spectroscopic approaches to confirmatory detection of low-order explosives. Finally, some promising areas for future research are highlighted and discussed with respect to potential IC-MS applications. PMID:24331039

Barron, Leon; Gilchrist, Elizabeth



[Study of chemical kinetics between pyrroloquinoline quinine and D-serine in body by ion-pair liquid chromatography].  


As a new neurotransmitter present in the glial cells, D-serine (DSer) plays an important role in central nervous system diseases. Pyrroloquinoline quinine (PQQ) can promote the production of the nerve growth factor and has a protective effect on nerve injuries. The chemical kinetics of PQQ and DSer was studied by determining the free contents of PQQ using ion-pair liquid chromatography (LC), so it can provide important information for the mechanisms of PQQ in the regulation of neurotransmitter. The PQQ and the production of the incubation were separated on an Amethyst C18-P column using tetrabutylammonium bromide as ion-pair reagent. The average recoveries were between 94.2% and 99.3%, and the relative standard deviations were between 1.05% and 2.03%. The average rate constants (K) of PQQ with DSer were 0.032, 0.07 and 0.17 h(-1) at 25, 37 and 50 degrees C, respectively. The average activation energy (E(a)) was 54.7 kJ/mol. The values of half life (t1/2) were 22.0, 9.8 and 3.99 h at 25, 37 and 50 degrees C, respectively. The results showed that PQQ can regulate the balance of DSer in the brain. The method is simple and reliable. PMID:22679836

Zhou, Xingqin; Qin, Xiaofeng; Zhang, Jiankang; Cao, Guoxian



Identification and separation of saxitoxins using hydrophilic interaction liquid chromatography coupled to traveling wave ion mobility-mass spectrometry.  


The aim of this work was to develop a reliable and efficient analytical method to characterise and differentiate saxitoxin analogues (STX), including sulphated (gonyautoxins, GTX) and non-sulphated analogues. For this purpose, hydrophilic interaction liquid chromatography (HILIC) was used to separate sulphated analogues. We also resorted to ion mobility spectrometry to differentiate the STX analogues because this technique adds a new dimension of separation based on ion gas phase conformation. Positive and negative ionisation modes were used for gonyautoxins while positive ionisation mode was used for non-sulphated analogues. Subsequently, the coupling of these three complementary techniques, HILIC-IM-MS, permitted the separation and identification of STX analogues; isomer differentiation was achieved in HILIC dimension while non-sulphated analogues were separated in the IM-MS dimension. Additional structural characteristics concerning the conformation of STXs could be obtained using IM-MS measurements. Thus, the collision cross sections (CCS) of STXs are reported for the first time in the positive ionisation mode. These experimental CCSs correlated well with the calculated CCS values using the trajectory method. PMID:25601690

Poyer, Salomé; Loutelier-Bourhis, Corinne; Coadou, Gaël; Mondeguer, Florence; Enche, Julien; Bossée, Anne; Hess, Philipp; Afonso, Carlos



Identification of novel isomeric pectic oligosaccharides using hydrophilic interaction chromatography coupled to traveling-wave ion mobility mass spectrometry.  


Separation and characterization of complex mixtures of pectic oligosaccharides still remains challenging and often requires the use of multiple analytical techniques, especially when isomeric structures are present. In this work, it is demonstrated that the coupling of hydrophilic interaction chromatography (HILIC) to traveling-wave ion mobility mass spectrometry (TWIMMS) enabled the simultaneous separation and characterization of complex mixtures of various isomeric pectic oligosaccharides. Labeling of oligosaccharides with 3-aminoquinoline (3-AQ) improved MS-ionization efficiency of the oligosaccharides and reduced the complexity of the product ion mass spectra, without losing resolution of the HILIC separation. In addition, labeling enabled quantification of oligosaccharides on molar basis using in-line fluorescence detection. Isomeric structures were distinguished using TWIMMS. The 3-AQ-HILIC-TWIMMS method was used to characterize a series of isomeric sugar beet rhamnogalacturonan I derived oligosaccharides carrying a glucuronic acid substituent. Thereby, some novel structural features were identified for the first time: glucuronic acid was attached to O-3 or to O-2 of galacturonic acid residues and a single galacturonic acid residue within an oligomer could contain both an acetyl group and a glucuronic acid substituent. PMID:25647688

Leijdekkers, Antonius G M; Huang, Jie-Hong; Bakx, Edwin J; Gruppen, Harry; Schols, Henk A



Analysis of water from the Space Shuttle and Mir Space Station by ion chromatography and capillary electrophoresis  

NASA Technical Reports Server (NTRS)

Drinking water and condensate samples collected from the US Space Shuttle and the Russian Mir Space Station are analyzed routinely at the NASA-Johnson Space Center as part of an ongoing effort to verify water quality and monitor the environment of the spacecraft. Water quality monitoring is particularly important for the Mir water supply because approximately half of the water consumed is recovered from humidity condensate. Drinking water on Shuttle is derived from the fuel cells. Because there is little equipment on board the spacecraft for monitoring the water quality, samples collected by the crew are transported to Earth on Shuttle or Soyuz vehicles, and analyzed exhaustively. As part of the test battery, anions and cations are measured by ion chromatography, and carboxylates and amines by capillary electrophoresis. Analytical data from Shuttle water samples collected before and after several missions, and Mir condensate and potable recovered water samples representing several recent missions are presented and discussed. Results show that Shuttle water is of distilled quality, and Mir recovered water contains various levels of minerals imparted during the recovery processes as designed. Organic ions are rarely detected in potable water samples, but were present in humidity condensate samples.

Orta, D.; Mudgett, P. D.; Ding, L.; Drybread, M.; Schultz, J. R.; Sauer, R. L.



A comprehensive method for lipid profiling by liquid chromatography-ion cyclotron resonance mass spectrometry[S  

PubMed Central

This work aims to combine chromatographic retention, high mass resolution and accuracy, MS/MS spectra, and a package for automated identification and quantitation of lipid species in one platform for lipidomic analysis. The instrumental setup elaborated comprises reversed-phase HPLC coupled to a Fourier transform ion cyclotron resonance mass spectrometer (LTQ-FT), and Lipid Data Analyzer (LDA) software. Data analysis for lipid species quantification in this platform is based on retention time, mass resolution of 200,000, and mass accuracy below 2 ppm. In addition, automatically generated MS/MS spectra provide structural information at molecular level. This LC/MS technology allows analyzing complex biological samples in a quantitative manner as shown here paradigmatically for murine lipid droplets having a huge surplus of triacylglycerol species. Chromatographic preseparation of the bulk lipid class alleviates the problem of ion suppression of lipid species from other classes. Extension of 1D to 2D chromatography is possible, yet time consuming. The platform affords unambiguous detection of lipid species as low as 0.1‰ within major lipid classes. Taken together, a novel lipidomic LC/MS platform based on chromatographic retention, high mass resolution and accuracy, MS/MS analysis, and quantitation software enables analysis of complex samples as demonstrated for lipid droplets. PMID:21960706

Fauland, Alexander; Köfeler, Harald; Trötzmüller, Martin; Knopf, Astrid; Hartler, Jürgen; Eberl, Anita; Chitraju, Chandramohan; Lankmayr, Ernst; Spener, Friedrich



Development Of Ion Chromatography Methods To Support Testing Of The Glycolic Acid Reductant Flowsheet In The Defense Waste Processing Facility  

SciTech Connect

Ion Chromatography (IC) is the principal analytical method used to support studies of Sludge Reciept and Adjustment Tank (SRAT) chemistry at DWPF. A series of prior analytical ''Round Robin'' (RR) studies included both supernate and sludge samples from SRAT simulant, previously reported as memos, are tabulated in this report.2,3 From these studies it was determined to standardize IC column size to 4 mm diameter, eliminating the capillary column from use. As a follow on test, the DWPF laboratory, the PSAL laboratory, and the AD laboratory participated in the current analytical RR to determine a suite of anions in SRAT simulant by IC, results also are tabulated in this report. The particular goal was to confirm the laboratories ability to measure and quantitate glycolate ion. The target was + or - 20% inter-lab agreement of the analyte averages for the RR. Each of the three laboratories analyzed a batch of 12 samples. For each laboratory, the percent relative standard deviation (%RSD) of the averages on nitrate, glycolate, and oxalate, was 10% or less. The three laboratories all met the goal of 20% relative agreement for nitrate and glycolate. For oxalate, the PSAL laboratory reported an average value that was 20% higher than the average values reported by the DWPF laboratory and the AD laboratory. Because of this wider window of agreement, it was concluded to continue the practice of an additional acid digestion for total oxalate measurement. It should also be noted that large amounts of glycolate in the SRAT samples will have an impact on detection limits of near eluting peaks, namely Fluoride and Formate. A suite of scoping experiments are presented in the report to identify and isolate other potential interlaboratory disceprancies. Specific ion chromatography inter-laboratory method conditions and differences are tabulated. Most differences were minor but there are some temperature control equipment differences that are significant leading to a recommendation of a heated jacket for analytical columns that are remoted for use in radiohoods. A suggested method improvement would be to implement column temperture control at a temperature slightly above ambient to avoid peak shifting due to temperature fluctuations. Temperature control in this manner would improve short and longer term peak retention time stability. An unknown peak was observed during the analysis of glycolic acid and SRAT simulant. The unknown peak was determined to best match diglycolic acid. The development of a method for acetate is summaraized, and no significant amount of acetate was observed in the SRAT products tested. In addition, an alternative Gas Chromatograph (GC) method for glycolate is summarized.

Wiedenman, B. J.; White, T. L.; Mahannah, R. N.; Best, D. R.; Stone, M. E.; Click, D. R.; Lambert, D. P.; Coleman, C. J.




EPA Science Inventory

Bromate is a disinfection by-product in drinking water, formed during the ozonation of source water containing bromide. An inductively coupled plasma mass spectrometer is combined with an ion chromatograph for the analysis of bromate in drinking waters. Three chromatographic colu...



EPA Science Inventory

A standardized method for the analysis of perchlorate in plants was developed, based on dry weight, and applied to the analysis of plant organs, foodstuffs, and plant products. The procedure greatly reduced the ionic interferences in water extracts of plant materials. Ion chro...


[Simultaneous determination of chlormequat chloride and mepiquat chloride in plants by mobile phase ion chromatography].  


Ion-pair reagent was used as mobile phase for the simultaneous separation of chlormequat chloride and mepiquat chloride in plants. The rapid separation was performed on a Dionex IonPac NG1 guard column and a Dionex IonPac NS1 analytical column using 1.0 mL/min of the eluent mixture of 1.00 mmol/L nonafluoropentanoic acid (as ion-pair reagent) and 7% acetonitrile, and the detection was achieved by a suppressed conductivity detector. The method provided good resolution of the analyte peaks without any interference. The detection limits of chlormequat chloride and mepiquat chloride were 0.154 6 mg/L and 0.171 4 mg/L, respectively. The linear calibration curves were obtained in the range of 1 - 100 mg/L. The mean recoveries in the ranges of 96.06% - 104.6% for chlormequat chloride and 98.53% - 103.7% for mepiquat chloride were obtained in real samples. The method requires only simple sample preparation and the technique is suitable for routine quality control analysis. PMID:21657055

Zhou, Xu; Xu, Jingang; Chen, Zhidong; Zhu, Yan



Method for Characterization of Low Molecular Weight Organic Acids in Atmospheric Aerosols Using Ion Chromatography Mass  

E-print Network

Method for Characterization of Low Molecular Weight Organic Acids in Atmospheric Aerosols Using Ion in the atmosphere is usually divided by the analysis of organic carbon, black (also called elemental) carbon, mecha- nisms of formation, and the ability to model their fate and transport. The composition

Dickerson, Russell R.


Miniaturized GC/MS instrumentation for in situ measurements: micro gas chromatography coupled with miniature quadrupole array and paul ion trap mass spectrometers  

NASA Technical Reports Server (NTRS)

Miniaturized chemical instrumentation is needed for in situ measurements in planetary exploration and other spaceflight applications where factors such as reduction in payload requirements and enhanced robustness are important. In response to this need, we are 'continuing to develop miniaturized GC/MS instrumentation which combines chemical separations by gas chromatography (GC) with mass spectrometry (MS) to provide positive identification of chemical compounds in complex mixtures of gases, such as those found in the International Space Station's cabin atmosphere. Our design approach utilizes micro gas chromatography components coupled with either a miniature quadrupole mass spectrometer array (QMSA) or compact, high-resolution Paul ion trap.

Holland, P.; Chutjian, A.; Darrach, M.; Orient, O.



Determination of glyphosate and phosphate in water by ion chromatography--inductively coupled plasma mass spectrometry detection.  


Quantitative determination of trace glyphosate and phosphate in waters was achieved by coupling ion chromatography (IC) separation with inductively coupled plasma mass spectrometry (ICP-MS) detection. The separation of glyphosate and phosphate on a polymer anion-exchange column (Dionex IonPac AS16, 4.0 mm x 250 mm) was obtained by eluting them with 20 mM citric acid at 0.50 mL min(-1), and the analytes were detected directly and selectively by ICP-MS at m/z = 31. Parameters affecting their chromatographic behaviors and ICP-MS characteristics were systematically examined. Based on a 500-microL sample injection volume, the detection limits were 0.7 microgL(-1) for both glyphosate and phosphate, and the calibrations were linear up to 400 microgL(-1). Polyphosphates, aminomethylphosphonic acid (the major metabolite of glyphosate), non-polar and other polar phosphorus-containing pesticides showed different chromatographic behaviors from the analytes of interest and therefore did not interference. The determination was also interference free from the matrix anions (nitrate, nitrite, sulphate, chloride, etc.) and metallic ions. The analysis of certified reference material, drinking water, reservoir water and Newater yielded satisfactory results with spiked recoveries of 97.1-107.0% and relative standard deviations of < or = 7.4% (n = 3). Compared to other reported methods for glyphosate and phosphate, the developed IC-ICP-MS method is sensitive and simple, and does not require any chemical derivatization, sample preconcentration and mobile phase conductivity suppression. PMID:16185703

Guo, Zhong-Xian; Cai, Qiantao; Yang, Zhaoguang



The analysis of aqueous mixtures using liquid chromatography-electrospray mass spectrometry  

SciTech Connect

The focus of this dissertation is the use of chromatographic methods coupled with electrospray mass spectrometry (ES-MS) for the determination of both organic and inorganic compounds in aqueous solutions. The combination of liquid chromatography (LC) methods and ES-MS offers one of the foremost methods for determining compounds in complex aqueous solutions. In this work, LC-ES-MS methods are devised using ion exclusion chromatography, reversed phase chromatography, and ion exchange chromatography, as well as capillary electrophoresis (CE). For an aqueous sample, these LC-ES-MS and CE-ES-MS techniques require no sample preparation or analyte derivatization, which makes it possible to observe a wide variety of analytes as they exist in solution. The majority of this work focuses on the use of LC-ES-MS for the determination of unknown products and intermediates formed during electrochemical incineration (ECI), an experimental waste remediation process. This report contains a general introduction to the project and the general conclusions. Four chapters have been removed for separate processing. Titles are: Chapter 2: Determination of small carboxylic acids by ion exclusion chromatography with electrospray mass spectrometry; Chapter 3: Electrochemical incineration of benzoquinone in aqueous media using a quaternary metal oxide electrode in the absence of a soluble supporting electrolyte; Chapter 4: The determination of electrochemical incineration products of 4-chlorophenol by liquid chromatography-electrospray mass spectrometry; and Chapter 5: Determination of small carboxylic acids by capillary electrophoresis with electrospray mass spectrometry.

Johnson, S.



Potential effects of surface water components on actinide determinations conducted by ion chromatography.  


An elution program for separating actinides (thorium, uranium, neptunium, plutonium, americium, and curium) on low hydrophobicity ion exchange columns was evaluated for solutions spiked with actinides and common surface water components. Potential interferences from dissolved ions (Na+, K+, Ca2+, Cl-, and SO(4)2-), humic acid, and radium were investigated. Sulfate levels greater than 0.25 mumol interfered with separation of americium, curium, and plutonium. Humic acid levels above 100 micrograms produced distinct widening of actinide peaks and reduced actinide recoveries. These interferences limit the range of useful sample volumes and create a need for sample pretreatment procedures. No interferences were produced by 0.025 to 2.5 mumol Ca2+, 0.045 to 4.5 mumol Na+, 0.015 to 1.5 mumol K+, and 0.025 to 4.5 mumol Cl-. In the absence of interferences, the program effectively separated radium from the actinides. PMID:7883573

Reboul, S H; Fjeld, R A



Determination of ammonium in a buddingtonite sample by ion-chromatography  

USGS Publications Warehouse

An ion-chromatographic method for the direct determination of ammonium, potassium, and sodium in geologic materials is described. Samples are decomposed with a mixture of hydrofluoric and hydrochloric acids in a sealed polycarbonate bottle heated in a microwave oven. The ion-chromatograph separates the cations and determines them by conductivity measurement. The ammonium concentrations thus determined have been verified by use of an ammonia-specific electrode. A total of 32 analyses of ammonium salts by both techniques showed an average error of -4%, with a relative standard deviation (RSD) of 6%. The ammonium concentrations found in a buddingtonite sample had an RSD of 2.2% and their mean agreed with that obtained by the Kjeldahl method. By use of the prescribed dilution of the sample, detection limits of 0.1% can be achieved for all three cations. ?? 1986.

Klock, P.R.; Lamothe, P.J.



Efficient separation of acetate and formate by ion chromatography: application to air samples in a cultural heritage environment.  


A method for the separation of acetate and formate anions by ion chromatography has been optimized under various measurement conditions (e.g. the composition of the mobile phase, and the flow rate of the eluent). For this purpose, two different analytical columns were examined: the IonPac AS14 (250 mm x 4 mm i.d.; designed mostly for the separation of inorganic anions) and the Allsep A-2 (150 mm x 4.6 mm i.d.; designed for the separation of low-molecular mass organic acids). However, nearly baseline separation of acetate and formate has been found on each column using the following conditions: (i) IonPac AS14 column and 2.0 mM Na2B4O7 solution as an eluent with a flow rate of 1.0 ml/min, or (ii) Allsep A-2 column and an eluent containing a mixture of 1.2 mM Na2CO3 plus 1.5 mM NaHCO3 with a flow rate of 1.3 ml/min. Additionally, the separation of fluoride from acetate and formate on both columns was studied. On the IonPac AS14 column it was possible to separate all three investigated anions. However, on the Allsep A-2 column, when the concentration of fluoride was comparable to, or higher than acetate, it was impossible to achieve good separation of these two anions, even using the optimized elution procedure. Therefore, the measurements of real samples were carried out with the use of IonPac AS14 column. The concentrations of acetate and formate have been determined in the air samples of the Cathedral of Cologne (Germany), after sampling the corresponding acids by passive diffusion tubes. Average concentrations of 122 and 9 microg/m(3) for acetic and formic acids were found, respectively, inside the Cathedral and in a depot with medieval stained glass panels. PMID:18371901

Kontozova-Deutsch, Velichka; Krata, Agnieszka; Deutsch, Felix; Bencs, László; Van Grieken, René



Improved determination of tributyl phosphate degradation products (mono- and dibutyl phosphates) by ion chromatography.  


Tributyl phosphate (TBP) is a very important compound in the nuclear industry, particularly in the area of nuclear fuel reprocessing. This compound is used in the PUREX (plutonium and uranium refining extraction) process which consists of the extraction of uranium and plutonium from an aqueous nitric acid phase, for the purpose of recycling. But TBP may be degraded to dibutyl phosphate (DBP) and monobutyl phosphate (MBP) by dealkylation of one or two butoxy groups, respectively. We have compared and evaluated the capacity of two resins manufactured by Dionex (AS11 and AS5A) in the separation and measurement of these two degradation products. AS11 generates two interferences: nitrite/DBP and carbonate/MBP. The first one is the most serious. So, we have developed a method for oxidising nitrite ions to nitrate ions which have no trouble over the measurement. The second resin tested, AS5A, allows a very efficient separation between DBP and NO2- ions and a good separation between MBP and CO3(2-) in comparison with the AS11. The detection limits for the AS5A column are 0.13 microM for MBP and 0.71 microM for DBP (injection loop=50 microl). PMID:11453010

Dodi, A; Verda, G



Negative ion chemical ionization gas chromatography/mass spectrometry of valproic acid metabolites.  


A negative ion chemical ionization (NICI) gas chromatographic/mass spectrometric method is described for the identification of 15 valproic acid (VPA) metabolites as their pentafluorobenzyl derivatives. Samples analyzed were serum, urine and saliva taken from a volunteer on VPA at steady state and also given selected doses of (2H6)VPA. Metabolite peaks were identified by comparison to synthetic standards. All the metabolites, like the parent drug, produced abundant [M - 181]- ions, except 3-keto VPA, which gave an [M - 181 - CO2]- ion. Using the NICI method, two new VPA metabolites were identified. One of these metabolites was characterized as 4'-keto-2-ene VPA by synthesis, while the second one appeared to be a positional isomer of 4'-keto-2-ene VPA. The sensitivity of the method was also sufficient to detect metabolites of VPA in saliva. The ratio of the levels of (Z)-2-ene VPA to (E)-2-ene VPA was much greater in saliva than in serum, suggesting stereoselective plasma protein binding or transport of these two metabolites. The lower limit of detection for the quantification of VPA in serum or saliva was 2 ng ml-1. PMID:2508808

Kassahun, K; Burton, R; Abbott, F S



[Analysis of toxaphene and its eight congeners in sediment and fish tissue by gas chromatography-negative ion mass spectrometry].  


Toxaphene quantification incorporating gas chromatography/negative chemical ionization mass spectrometry (GC/NCI-MS) offers improved sensitivity and specificity. The U. S. Environmental Protection Agency (USEPA) recently released a GC/NCI-MS method (Method 8276) for the measurement of technical toxaphene and eight specific congeners (Hx-Sed, Hp-Sed, P26, P41, P40, P44, P50 and P62). However, there is still lack of a practical and complete analytical method including sample extraction, clean up, instrumental analysis, and data analysis. The goal of this work was to develop a ready-to-use method for the quantification of total toxaphene and the eight congeners. Sediment and salmon fish tissue were selected as sample matrices and extracted with methylene chloride using an accelerated solvent extraction system. The sample extracts were cleaned up with active copper powder or gel permeation chromatography, and finally silica/alumina combination column. Separation was performed on a DB-XLB column. GC/NCI-MS was operated under selected ion monitoring mode with an identical set of confirmation and quantitation ions for total toxaphene and the eight congeners. Oxygen reaction of polychlorinated biphenyls (PCB) was monitored by PCB204, an internal calibration standard, and the reaction level was kept below 1%. Average relative response factors were used in quantitation. Quantitation of total toxaphene employed the sum of all detectable (S/N > or = 3) 6-C1 to 10-Cl homolog peak areas, while the individual congeners were quantified followed the standard procedures for single analytes. Multi-point calibration solutions ranged from 0. 5 (5 for P62) to 500 microg/L for the individual congeners, and 50 to 500 microg/L for technical toxaphene, with the lowest calibration levels as lower limits of quantitation. Average congener recovery was (90.8 +/- 17.4)% (n =10) in spiked sediment with relative standard deviations of 5.4% - 12.8% (n =10), underscoring an excellently accurate and precise method. The method was applied to analyze sediment and fish tissue sample. PMID:24164036

Lao, Wenjian



Dioxin analysis by gas chromatography-Fourier transform ion cyclotron resonance mass spectrometry (GC-FTICRMS)  

Microsoft Academic Search

The feasibility of utilizing a gas chromatograph-tandem quadrupole-Fourier transform ion cyclotron resonance mass spectrometer\\u000a (GC-MS\\/MS-FTICRMS) to analyze chlorinated-dioxins\\/furans (CDDs\\/CDFs) and mixed halogenated dioxins\\/furans (HDDs\\/HDFs) was\\u000a investigated by operating the system in the GC-FTICRMS mode. CDDs\\/CDFs and mixed HDDs\\/HDFs could be analyzed at 50,000 to\\u000a 100,000 resolving power (RP) on the capillary gas Chromatographic time scale. Initial experiments demonstrated that 1

Vince Y. Taguchi; Robert J. Nieckarz; Ray E. Clement; Stefan Krolik; Robert Williams



Semiautomated pH gradient ion-exchange chromatography of monoclonal antibody charge variants.  


A new approach using a chromatography system equipped with isocratic pumps and an electrolytic eluent generator (EG) is introduced, replacing external pH gradient delivery using conventional gradient systems, in which bottled buffers with preadjusted pH are mixed using a gradient pump. The EG is capable of generating high purity base or acid required for online preparation of the buffer at the point of use, utilizing deionized water as the only carrier stream. Typically, the buffer was generated from online titration of a reagent composed of low molecular weight amines. The reagent was delivered isocratically into a static mixing tee, where it was titrated to the required pH with electrolytically generated base or acid. The required pH gradient was thus conveniently generated by electrically controlling the concentration of titrant. Also, since the pH was adjusted at the point of use, this approach offered enhanced throughput in terms of eluent preparation time and labor, and with a more reproducible pH profile. The performance of the system was demonstrated by running pH gradients ranging from pH 8.2 to 10.9 on a polymer monolith cation-exchange column for high throughput profiling of charge heterogeneity of intact, basic therapeutic monoclonal antibodies. A high degree of flexibility in modulating the key parameters of the pH gradient, including the buffer concentration, the pH gradient slope and the operating pH range was demonstrated. This enabled fine-tuning of the separation conditions for each individual antibody in order to enhance the chromatographic resolution. PMID:25199803

Talebi, Mohammad; Shellie, Robert A; Hilder, Emily F; Lacher, Nathan A; Haddad, Paul R



Mixed-bed ion exchange chromatography employing a salt-free pH gradient for improved sensitivity and compatibility in MudPIT.  


In proteomics, comprehensive analysis of peptides mixtures necessitates multiple dimensions of separation prior to mass spectrometry analysis to reduce sample complexity and increase the dynamic range of analysis. The main goal of this work was to improve the performance of (online) multidimensional protein identification technology (MudPIT) in terms of sensitivity, compatibility and recovery. The method employs weak anion and strong cation mixed-bed ion exchange chromatography (ACE) in the first separation dimension and reversed phase chromatography (RP) in the second separation dimension (Motoyama Anal. Chem 2007, 79, 3623-34.). We demonstrated that the chromatographic behavior of peptides in ACE chromatography depends on both the WAX/SCX mixing ratio as the ionic strength of the mobile phase system. This property allowed us to replace the conventional salt gradient by a (discontinuous) salt-free, pH gradient. First dimensional separation of peptides was accomplished with mixtures of aqueous formic acid and dimethylsulfoxide with increasing concentrations. The overall performance of this mobile phase system was found comparable to ammonium acetate buffers in application to ACE chromatography, but clearly outperformed strong cation exchange for use in first dimensional peptide separation. The dramatically improved compatibility between (salt-free) ion exchange chromatography and reversed phase chromatography-mass spectrometry allowed us to downscale the dimensions of the RP analytical column down to 25 ?m i.d. for an additional 2- to 3-fold improvement in performance compared to current technology. The achieved levels of sensitivity, orthogonality, and compatibility demonstrates the potential of salt-free ACE MudPIT for the ultrasensitive, multidimensional analysis of very modest amounts of sample material. PMID:23772827

Mommen, Geert P M; Meiring, Hugo D; Heck, Albert J R; de Jong, Ad P J M



Determination of sulfonic acids and alkylsulfates by ion chromatography in water.  


A fast ion chromatographic method with suppressed conductivity detection has been developed for the simultaneous determination of methane-, ethane-, 1-propane-, 1-butane-, 1-pentane-, 1-hexane-, 1-heptane-, 1-octane-, 1-nonane-, 1-decane-, 1-dodecane-, dodecylbenzene-, p-toluene-, benzenesulfonic acids, octylsulfate and dodecylsulfate in water samples. Due to the high number of analytes and their heterogeneity, the effect of the mobile phase parameters (NaOH, CH(3)OH and CH(3)CN concentration) on the retention factors has been studied in detail, so achieving, for the first time, the separation among 15 of these analytes by a gradient elution. Detection limits included within 0.06-0.16 microM have been obtained. Interferences from Cl(-), NO(3)(-) and SO(4)(2-), possible anions present in water samples, have been considered and a SPE procedure has been developed for analytes enrichment and matrix removal in a seawater sample. This is the first application of an ion-exchange chromatographic method to a seawater sample for this kind of analytes. PMID:18585139

Bruzzoniti, Maria Concetta; De Carlo, Rosa Maria; Sarzanini, Corrado



Determination of methylmercury in human blood using capillary gas chromatography and selected-ion monitoring.  


A capillary gas chromatographic method, using selected-ion monitoring in the electron-impact mode, was developed for the analysis of methylmercury (MeHg) in human blood. The samples, spiked with the internal standard propylmercury bromide (PropHgBr), were, after addition of sodium bromide and cupric sulfate, extracted with toluene. The organic phase was extracted with an ethanol-water solution of sodium thiosulfate. After addition of sodium bromide solution, the ethanol-water phase was extracted with toluene. Methylated derivatives (MeHgCH2Br and PropHgCH2Br) were formed by the addition of a diethyl ether solution of diazomethane. The chromatographic properties of the derivatives were much better than those of the non-methylated compounds. The m/z 215 fragment of MeHgCH2Br and the molecular ion m/z 338 of PropHgCH2Br were monitored. The calibration graphs, with a linear correlation coefficient of 0.992 (n = 12) in the 1-5 micrograms/l concentration range, passed through the origin. The detection limit for MeHg in human blood was ca. 0.5 microgram/l. Analysis of spiked blood samples at concentrations of about 2 and 10 micrograms/l gave a relative standard deviation of 4.2 and 5.5%, respectively (n = 10). PMID:1564105

Brunmark, P; Skarping, G; Schütz, A



Potential of ion chromatography coupled to isotope ratio mass spectrometry via a liquid interface for beverages authentication.  


New tools for the determination of characteristic parameters for food authentication are requested to prevent food adulteration from which health concerns, unfair competition could follow. A new coupling in the area of compound-specific carbon 13 isotope ratio (?(13)C) analysis was developed to simultaneously quantify ?(13)C values of sugars and organic acids. The coupling of ion chromatography (IC) together with isotope ratio mass spectrometry (IRMS) can be achieved using a liquid interface allowing a chemical oxidation (co) of organic matter. Synthetic solutions containing 1 polyol (glycerol), 3 carbohydrates (sucrose, glucose and fructose) and 12 organic acids (gluconic, lactic, malic, tartaric, oxalic, fumaric, citric and isocitric) were used to optimize chromatographic conditions (concentration gradient and 3 types of column) and the studied isotopic range (-32.28 to -10.65‰) corresponds to the values found in food products. Optimum chromatographic conditions are found using an IonPac AS15, an elution flow rate of 0.3mLmin(-1) and a linear concentration gradient from 2 to 76mM (rate 21mMmin(-1)). Comparison between ?(13)C value individually obtained for each compound with the coupling IRMS and elemental analyzer, EA-IRMS, and the ones measured on the mixture of compounds by IC-co-IRMS does not reveal any isotope fractionation. Thus, under these experimental conditions, IC-co-IRMS results are accurate and reproducible. This new coupling was tested on two food matrices, an orange juice and a sweet wine. Some optimization is necessary as the concentration range between sugars and organic acids is too large: an increase in the filament intensity of the IRMS is necessary to simultaneously detect the two compound families. These first attempts confirm the good results obtained on synthetic solutions and the strong potential of the coupling IC-co-IRMS in food authentication area. PMID:24267317

Guyon, Francois; Gaillard, Laetitia; Brault, Audrey; Gaultier, Nicolas; Salagoïty, Marie-Hélène; Médina, Bernard



Fragment profiling of low molecular weight heparins using reversed phase ion pair liquid chromatography-electrospray mass spectrometry.  


Low molecular weight heparins (LMWHs) are linear and highly charged carbohydrate polymers prepared by chemical or enzymatic depolymerization of heparin. Compared to unfractionated heparin (UFH), LMWHs are prevalently used as clinical anticoagulant drugs due to their lower side effects and better bioavailability. The work presented herein provides a rapid and powerful fragment mapping method for structural characterization of LMWHs. The chain fragments of two types of LMWHs, enoxaparin and nadroparin, were generated by controlled enzymatic digestion with each of heparinase I (Hep I, Enzyme Commission (EC) #, heparinase II (Hep II, no EC # assigned) and heparinase III (Hep III, EC # Reversed phase ion pair high performance liquid chromatography (RPIP-HPLC) coupled with electrospray ion trap time-of-flight mass spectrometry (ESI-IT-TOF-MS) was used to profile the oligosaccharide chains ranging from disaccharides to decasaccharides. A database containing all theoretical structural compositions was established to assist the mass spectra interpretation. The six digests derived by three enzymes from two types of LMWHs exhibited distinguishable fingerprinting patterns. And a total of 94 enoxaparin fragments and 109 nadroparin fragments were detected and identified. Besides the common LMWH oligosaccharides, many components containing characteristic LMWH structures such as saturated l-idopyranosuronic acid, 2,5-anhydro-d-mannitol, 1,6-anhydro-d-aminopyranose, as well as odd number oligosaccharides were also revealed. Quantitative comparison of major components derived from innovator and generic nadroparin products was presented. This approach to profile LMWHs' fragments offers a highly reproducible, high resolution and information-rich tool for evaluating the quality of this category of anticoagulant drugs or comparing structural similarities among samples from various sources. PMID:25701653

Xu, Xiaohui; Li, Daoyuan; Chi, Lequan; Du, Xuzhao; Bai, Xue; Chi, Lianli



Comprehensive identification of walnut polyphenols by liquid chromatography coupled to linear ion trap-Orbitrap mass spectrometry.  


Epidemiologic studies and clinical trials have demonstrated consistent benefits of walnut consumption on coronary heart disease risk and other chronic diseases. Walnuts (Juglans regia L.) have been described previously as a rich source of polyphenols with a broad array of different structures. However, an accurate screening of its complete phenolic profile is still lacking. In the present work, liquid chromatography coupled with electrospray ionization hybrid linear trap quadrupole-Orbitrap mass spectrometry (LC-LTQ-Orbitrap) was applied for a comprehensive identification of phenolic compounds in walnuts. A total of 120 compounds, including hydrolysable and condensed tannins, flavonoids and phenolic acids were identified or tentatively identified on the base of their retention times, accurate mass measurements and subsequent mass fragmentation data, or by comparing with reference substances and literature. The peak area of each signal in mass chromatograms was used to provide semiquantitative information for comparison purposes. The most abundant ions were observed for ellagitannins, ellagic acid and its derivatives. Furthermore, the high-resolution MS analysis revealed the presence of eight polyphenols that have never been reported in walnuts: stenophyllanin C, malabathrin A, eucalbanin A, cornusiin B, heterophylliin E, pterocarinin B, reginin A and alienanin B. PMID:24444946

Regueiro, Jorge; Sánchez-González, Claudia; Vallverdú-Queralt, Anna; Simal-Gándara, Jesús; Lamuela-Raventós, Rosa; Izquierdo-Pulido, Maria



Multiple applications of ion chromatography oligosaccharide fingerprint profiles to solve a variety of sugar and sugar-biofuel industry problems.  


Sugar crops contain a broad variety of carbohydrates used for human consumption and the production of biofuels and bioproducts. Ion chromatography with integrated pulsed amperometric detection (IC-IPAD) can be used to simultaneously detect mono-, di-, and oligosaccharides, oligosaccharide isomers, mannitol, and ethanol in complex matrices from sugar crops. By utilizing a strong NaOH/NaOAc gradient method over 45 min, oligosaccharides of at least 2-12 dp can be detected. Fingerprint IC oligosaccharide profiles are extremely selective, sensitive, and reliable and can detect deterioration product metabolites from as low as 100 colony-forming units/mL lactic acid bacteria. The IC fingerprints can also be used to (i) monitor freeze deterioration, (ii) optimize harvesting methods and cut-to-crush times, (iii) differentiate between white refined sugar from sugar cane and from sugar beets, (iv) verify the activities of carbohydrate enzymes, (v) select yeasts for ethanol fermentations, and (vi) isolate and diagnose infections and processing problems in sugar factories. PMID:25708094

Eggleston, Gillian; Borges, Eduardo



Electro-driven extraction of inorganic anions from water samples and water miscible organic solvents and analysis by ion chromatography.  


A simple electromembrane extraction (EME) procedure combined with ion chromatography (IC) was developed to quantify inorganic anions in different pure water samples and water miscible organic solvents. The parameters affecting extraction performance, such as supported liquid membrane (SLM) solvent, extraction time, pH of donor and acceptor solutions, and extraction voltage were optimized. The optimized EME conditions were as follows: 1-heptanol was used as the SLM solvent, the extraction time was 10 min, pHs of the acceptor and donor solutions were 10 and 7, respectively, and the extraction voltage was 15 V. The mobile phase used for IC was a combination of 1.8 mM sodium carbonate and 1.7 mM sodium bicarbonate. Under these optimized conditions, all anions had enrichment factors ranging from 67 to 117 with RSDs between 7.3 and 13.5% (n = 5). Good linearity values ranging from 2 to 1200 ng/mL with coefficients of determination (R(2) ) between 0.987 and 0.999 were obtained. The LODs of the EME-IC method ranged from 0.6 to 7.5 ng/mL. The developed method was applied to different samples to evaluate the feasibility of the method for real applications. PMID:24788937

Nojavan, Saeed; Bidarmanesh, Tina; Memarzadeh, Farkhondeh; Chalavi, Soheila



Selective removal of carbon dioxide contained in the effluent from ion chromatography suppressors using a new non-vacuum device.  


In this paper, a new CO2 gas removal device optimized to selectively remove CO2 gas contained in the effluent from suppressors used in ion chromatography (IC) under non-vacuum conditions is described. This device consists of a closed vessel equipped with gas permeable tubing (GPT) and a CO2 adsorbent. During operation, the CO2 adsorbent adsorbs CO2 gas in the vessel, creating CO2 partial pressure difference between the inside of the GPT and the vessel. The CO2 gas contained in the effluent being pumped into the GPT is selectively removed from the effluent based on the diffusion of the CO2 associated with the CO2 partial pressure difference. The purpose of this study is to optimize the IC operating conditions with the aim of selectively removing HCO3(-) (CO3(2-)) contained in the effluent and reducing the electrical conductivity of the effluent under non-vacuum conditions. The electrical conductivity of the effluent and the signal intensity of the water dip is decreased by approximately 25?S/cm (from 30 to 5?S/cm) and by approximately twentieth, respectively, using the optimized CO2 remover. In addition, the anion detection limit achieved in IC instruments with a CO2 remover is on the order of a few ppb. PMID:25817478

Masunaga, Hiroto; Higo, Yuji; Ishii, Mizuo; Maruyama, Noboru; Yamazaki, Shigeo



Derivatization Ion Chromatography for the Determination of Monoethanolamine in Presence of Hydrazine in PHWR Steam-Water Circuits  

PubMed Central

A simple, rapid and accurate method for the determination of monoethanolamine (MEA) in PHWR steam-water circuits has been developed. MEA is added in the feed water to provide protection against corrosion while hydrazine is added to scavenge dissolved oxygen. The quantitative determination of MEA in presence of hydrazine was accomplished using derivatization ion chromatography with conductometric detection in nonsuppressed mode. A Metrosep cation 1-2 analytical column and a Metrosep cartridge were used for cation separation. A mixture of 4?mM tartaric acid, 20% acetone and 0.05?mM HNO3 was used as eluent. Acetone in the mobile phase leads to the formation of different derivatives with MEA and hydrazine. The interferences due Na+ and NH4?+ were eliminated by adopting a simple pretreatment procedure employing OnGuard-H cartridge. The limit of detection limit of MEA was 0.1??g?mL?1 and the relative standard deviation was 2% for the overall method. The recovery of MEA added was in the range 95%–102%. The method was applied to the determination of MEA in steam generator water samples. PMID:21785596

D., Ayushi; Sengupta, Arijit; Kumar, Sangita D.; Kumbhar, A. G.; Venkateswaran, G.



Analysis of terpenoids from hemlock (Tsuga) species by solid-phase microextraction/gas chromatography/ion-trap mass spectrometry.  


A sampling method for determining the volatile terpenoid composition from single needles of seven Tsuga species was developed using headspace solid-phase microextraction (SPME). A reproducible sampling method for the volatile components was generated by examination of sample storage, method of needle cutting, and headspace sampling duration. Following SPME collection of the volatile compounds from the seven Tsuga species, gas chromatography/ion-trap mass spectrometry was used to identify 51 terpenoids present in the needle headspace. A semiquantitative method was devised to express individual terpenoid amounts as a percentage of all of the identified peaks in the chromatogram. The semiquantitative results permitted facile interspecies comparison using principal component analysis. Two components were able to account for 90% of the variance and were interpreted as a "species" component and a "resistance/susceptibility" component. Three interspecies groupings were evident from the principal component analysis: (1) Tsuga canadensis and Tsuga caroliniana; (2) Tsuga chinesnsis, Tsuga diversifolia, Tsuga heterophylla, and Tsuga sieboldii; and (3) Tsuga mertensiana. The finding that T. mertensiana was grouped alone and far removed from the other species adds to the morphological evidence that this species should be segregated from other Tsuga. PMID:12670144

Lagalante, Anthony F; Montgomery, Michael E



Stability of plasma gamma-hydroxybutyrate determined by gas chromatography-positive ion chemical ionization-mass spectrometry.  


An effective method for the determination of gamma-hydroxybutyric acid (GHB) in human plasma is described that utilizes a simple liquid-liquid extraction procedure and gas chromatography-positive ion chemical ionization-mass spectrometry (GC-PCI-MS). The method has been used to study the stability of plasma GHB under several storage conditions. Following the extraction with acetonitrile, GHB and deuterated GHB (GHB-d(6)) were derivatized with N,O-bis[trimethylsilyl] trifluoroacetamide (BSFTA). After the separation on a capillary GC column, the derivatives were ionized with ammonia reagent gas and analyzed by MS. The lower limit of quantitation in 100 microL of plasma was 2.5 microg/mL, over a range from 2.5 to 250 microg/mL. The coefficients of variation did not exceed 3.9% and the mean measured concentrations did not deviate more than 8% from the target for both intra- and interassay precision and accuracy. Plasma GHB was found to be stable at -20 degrees C for up to 9 months, at room temperature for 48 h, and after 3 freeze/thaw cycles. It was also found to be stable in processed samples stored at room temperature for 5 days and for 15 days at -20 degrees C. PMID:14606997

Chen, Meng; Andrenyak, David M; Moody, David E; Foltz, Rodger L



[Determination of benomyl, carbendazim and thiabendazole in apple juice concentrate using solid-phase extraction coupled with ion exchange chromatography].  


A method was developed for the determination of benomyl, carbendazim and thiabendazole in apple juice concentrate by solid-phase extraction coupled with ion exchange chromatography (IEC). The sample was diluted with water, and then benomyl was degradated completely to carbendazim at 80 degrees C, and purified by an SCX solid-phase extraction column. Liquid chromatographic analysis was performed on the instrument of Agilent 1200 series equipped with a diode-array detector and autosampler. The column was LC-SCX (25 cm x 4.6 mm, 5 microm). The mobile phase was 0.1 mol/L KH2PO4 (pH 2.5)-acetonitrile (70:30, v/v) with a flow rate of 1.0 mL/min. The presented method showed good linear relationship with good precision and accuracy at the range of 0.02 - 2.0 mg/L for carbendazim and thiabendazole. The detection limits were 0. 004 mg/kg for carbendazim and thiabendazole. The method was characterized with acceptable sensitivity to meet the requirements for monitoring these pesticides in apple juice concentrate. PMID:19160754

He, Qiang; Kong, Xianghong; Zhao, Jie; Li, Jianhua; Yue, Aishan; Zhang, Ying



Molecular differentiation of ischemic and valvular heart disease by liquid chromatography/fourier transform ion cyclotron resonance mass spectrometry.  


Proteomic patterns of myocardial tissue in different etiologies of heart failure were investigated using a direct analytical approach with High Performance Liquid Chromatography (HPLC)/Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (FT-ICR MS). Right atrial appendages from 20 patients, 10 with hemodynamically significant isolated aortic valve disease and 10 with symptomatic coronary artery disease were collected during elective cardiac surgery. After preparation of tissue samples and tryptic digestion of proteins, the peptide mixture was HPLC-separated and on-line analyzed by electrospray FT-ICR MS. Data obtained from HPLC / FT-ICR MS runs were compared for classification. To extract the classification features, the selection of best individual features was applied and the "nearest mean classifier" was used for the classification of test samples and the sample projection onto classification patterns. The pattern distribution characteristics of aortic and coronary diseases were clearly different. No interference between samples of both disease categories was registered, even if the distribution of unsupervised classified test samples were closer. Samples representing aortic valve disease showed a closer accumulation pattern of spots compared to the samples representing coronary disease, which indicated a more specific protein classification. Through selective identification of specific peptides and protein patterns with FTMS, valvular and coronary heart disease is for the first time clearly distinguished at molecular level. The described methodology could also be feasible in search for specific biomarkers in plasma or serum for diagnostic purposes. PMID:16820333

Baykut, Doan; Grapow, M; Bergquist, M; Amirkhani, A; Ivonin, I; Reineke, D; Grussenmeyer, T; Hakansson, P; Zerkowski, H-R; Baykut, G; Bergquist, J



Simultaneous determination of Cr(III)-EDTA and Cr(VI) by ion interaction chromatography using a C18 column.  


The simultaneous determination of Cr(III) and Cr(VI) by ion interaction chromatography has been investigated. The mobile phase consisted of a 5 mM octylammonium orthophosphate at pH 4.0 with 35% (v/v) MeOH. The Nucleosil-100, C18 (5 microm, 250 x 4.6 mm) was used as the separating column and the component was detected at 200 nm. The separation of Cr(III) and Cr(VI) was based on anionic interaction. Since the Cr(III) did not exist as an anionic form like the Cr(VI) (Cr2O7(2-)) presented at the optimum condition, Cr(II) was firstly reacted with EDTA (1:40 mole ratio) to form the anionic complex prior to injecting into the chromatographic system. The characteristics of the method for separation of Cr(III)-EDTA and Cr(VI) were satisfactory. The wide linear range (0.3-50.0 mg l(-1)) was achieved. The repeatabilities (%R.S.D.) calculated from peak areas were 0.49% and 0.14%, detection limit (signal to noise ratio of 3) of 0.02 mg l(-1) and 0.3 mg l(-1) were obtained and the average of percent recoveries were found to be 98.5% and 99.6% for Cr(III) and Cr(VI), respectively. PMID:15909532

Threeprom, Jirasak; Purachaka, Sumalee; Potipan, Lamfa



Determination of arsenic speciation in sulfidic waters by Ion Chromatography Hydride-Generation Atomic Fluorescence Spectrometry (IC-HG-AFS).  


A method for the analysis of arsenic species in aqueous sulfide samples is presented. The method uses an ion chromatography system connected with a Hydride-Generation Atomic Fluorescence Spectrometer (IC-HG-AFS). With this method inorganic As(III) and As(V) species in water samples can be analyzed, including arsenite (HnAs(III)O3(n-3)), thioarsenite (HnAs(III)S3(n-3)), arsenate (HnAs(V)O4(n-3)), monothioarsenate (HnAs(V)SO3(n-3)), dithioarsenate (HnAs(V)S2O2(n-3)), trithioarsenate (HnAs(V)S3O(n-3)) and tetrathioarsenate (HnAs(V)S4(n-3)). The peak identification and retention times were determined based on standard analysis of the various arsenic compounds. The analytical detection limit was ~1-3 µg L(-1) (LOD), depending on the quality of the baseline. This low detection limit makes this method also applicable to discriminate between waters meeting the drinking water standard of max. 10 µg L(-1) As, and waters that do not meet this standard. The new method was successfully applied for on-site determination of arsenic species in natural sulfidic waters, in which seven species were unambiguously identified. PMID:25059187

Keller, Nicole S; Stefánsson, Andri; Sigfússon, Bergur



Automated determination of bromide in waters by ion chromatography with an amperometric detector  

USGS Publications Warehouse

An automated ion chromatograph, including a program controller, an automatic sampler, an integrator, and an amperometric detector, was used to develop a procedure for the determination of bromide in rain water and many ground waters. Approximately 10 min is required to obtain a chromatogram. The detection limit for bromide is 0.01 mg l-1 and the relative standard deivation is <5% for bromide concentrations between 0.05 and 0.5 mg l-1. Chloride interferes if the chloride-to-bromide ratio is greater than 1 000:1 for a range of 0.01-0.1 mg l-1 bromide; similarly, chloride interferes in the 0.1-1.0 mg l-1 range if the ratio is greater than 5 000:1. In the latter case, a maximum of 2 000 mg l-1 of chloride can be tolerated. Recoveries of known concentrations of bromide added to several samples, ranged from 97 to 110%. ?? 1983.

Pyen, G.S.; Erdmann, D.E.



Simultaneous determination of serum cations, anions and uremic toxins by ion chromatography using an immobilized enzyme.  


A procedure is described for the analysis of serum cations and uremic toxins by simultaneous conductivity (CD) and ultraviolet (UV) photometric detection and using phosphoric acid as the eluent. In addition, studies were made on the determination of urea in serum using immobilized urease, and on the simultaneous determination of cationic and anionic compounds. The ammonium ion produced from urea by immobilized urease was determined by CD. No significant differences in amounts were found between the present method and conventional colorimetric methods. There was no significant reduction in immobilized urease activity after two months of continuous use. Simultaneous analysis of cationic and anionic compounds in serum was performed by switching valves in order to change the eluents and to change the channel to the analytical column. No marked base-line variation was observed and satisfactory recovery of anions was achieved. PMID:4086536

Shintani, H; Ube, S



Ultrafiltration by a compacted clay membrane-II. Sodium ion exclusion at various ionic strengths  

USGS Publications Warehouse

Several recent laboratory studies and field investigations have indicated that shales and compacted clay minerals behave as semipermeable membranes. One of the properties of semipermeable membranes is to retard or prevent the passage of charged ionic species through the membrane pores while allowing relatively free movement of uncharged species. This phenomenon is termed salt filtering, reverse osmosis, or ultrafiltration. This paper shows how one can proceed from the ion exchange capacity of clay minerals and, by means of Donnan membrane equilibrium concept and the Teorell-Meyer-Siever theory, develop a theory to explain why and to what extent ultrafiltration occurs when solutions of known concentration are forced to flow through a clay membrane. Reasonable agreement between theory and laboratory results were found. The concentration of the ultrafiltrate was always greater than predicted because of uncertainty in values of some parameters in the equations. Ultrafiltration phenomena may be responsible for the formation of some subsurface brines and mineral deposits. The effect should also be taken into consideration in any proposal for subsurface waste emplacement in an environment containing large quantities of clay minerals. ?? 1973.

Hanshaw, B.B.; Coplen, T.B.



Determination of trace concentrations of bromate in municipal and bottled drinking waters using a hydroxide-selective column with ion chromatography  

Microsoft Academic Search

The International Agency for Research on Cancer determined that bromate is a potential human carcinogen, even at low ?g\\/l levels in drinking water. Bromate is commonly produced from the ozonation of source water containing naturally occurring bromide. Traditionally, trace concentrations of bromate and other oxyhalides in environmental waters have been determined by anion exchange chromatography with an IonPac AS9-HC column

Brian M. De Borba; Jeff S. Rohrer; Chris A. Pohl; Charanjit Saini



Regioisomeric analysis of triacylglycerols using silver-ion liquid chromatography–atmospheric pressure chemical ionization mass spectrometry: Comparison of five different mass analyzers  

Microsoft Academic Search

Silver-ion high-performance liquid chromatography (HPLC) coupled to atmospheric pressure chemical ionization mass spectrometry (APCI-MS) is used for the regioisomeric analysis of triacylglycerols (TGs). Standard mixtures of TG regioisomers are prepared by the randomization reaction from 8 mono-acid TG standards (tripalmitin, tristearin, triarachidin, triolein, trielaidin, trilinolein, trilinolenin and tri-gamma-linolenin). In total, 32 different regioisomeric doublets and 11 triplets are synthesized, separated

Michal Hol?apek; Hana Dvo?áková; Miroslav Lísa; Ana Jimenéz Girón; Pat Sandra; Josef Cva?ka



Stability studies of propoxur herbicide in environmental water samples by liquid chromatography–atmospheric pressure chemical ionization ion-trap mass spectrometry  

Microsoft Academic Search

Liquid chromatography–atmospheric pressure ionization ion-trap mass spectrometry has been investigated for the analysis of polar pesticides in water. The degradation behavior of propoxur, selected as a model pesticide belonging to the N-methylcarbamate group, in various aqueous matrices (Milli-Q water, drinking water, rain water, seawater and river water) was investigated. Two interfaces of atmospheric pressure ionization, atmospheric pressure chemical ionization (APCI)

Lei Sun; Hian Kee Lee



Multidimensional separations of complex peptide mixtures: a combined high-performance liquid chromatography\\/ion mobility\\/time-of-flight mass spectrometry approach  

Microsoft Academic Search

High-performance liquid chromatography (HPLC) has been combined with high-resolution ion mobility separations and time-of-flight mass spectrometry (MS) for the analysis of complex biomolecular mixtures such as those that arise upon tryptic digestion of protein mixtures. In this approach, components in a mixture are separated using reversed phase HPLC. As mixtures of peptides exit the column, they are electrosprayed into an

Stephen J. Valentine; Manoj Kulchania; Catherine A. Srebalus Barnes; David E. Clemmer



[Determination of antioxidants butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in cosmetics by gas chromatography-mass spectrometry selected ion method].  


A new method for the determination of butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in cosmetics by gas chromatography-mass spectrometry selected ion storage (SIS) method was developed. The BHA and BHT in samples were extracted by methanol. The m/z 165 and m/z 205 were the monitoring ion for BHA and BHT respectively. The detection limits of BHA and BHT in samples were 2.5 micrograms/g and 0.5 microgram/g, respectively. The method is simple, rapid and accurate. PMID:12541980

Zhang, Wei-Ya; Wu, Cai-Ying; Wang, Cheng-Yun; Yang, Zuo-Jun; Liu, Li



Measurement of gas-phase ammonia and amines in air by collection onto an ion exchange resin and analysis by ion chromatography  

NASA Astrophysics Data System (ADS)

Ammonia and amines are common trace gases in the atmosphere and have a variety of both biogenic and anthropogenic sources, with a major contribution coming from agricultural sites. In addition to their malodorous nature, both ammonia and amines have been shown to enhance particle formation from acids such as nitric, sulfuric and methanesulfonic acids, which has implications for visibility, human health and climate. A key component of quantifying the effects of these species on particle formation is accurate gas-phase measurements in both laboratory and field studies. However, these species are notoriously difficult to measure as they are readily taken up on surfaces, including onto glass surfaces from aqueous solution as established in the present studies. We describe here a novel technique for measuring gas-phase ammonia and amines that involves uptake onto a weak cation exchange resin followed by extraction and analysis using ion chromatography. Two variants - one for parts per billion concentrations in air and the second with lower (parts per trillion) detection limits - are described. The latter involves the use of a custom-designed high-pressure cartridge to hold the resin for in-line extraction. These methods avoid the use of sampling lines, which can lead to significant inlet losses of these compounds. They also have the advantages of being relatively simple and inexpensive. The applicability of this technique to ambient air is demonstrated in measurements made near a cattle farm in Chino, CA.

Dawson, M. L.; Perraud, V.; Gomez, A.; Arquero, K. D.; Ezell, M. J.; Finlayson-Pitts, B. J.



Measurement of gas-phase ammonia and amines in air by collection onto an ion exchange resin and analysis by ion chromatography  

NASA Astrophysics Data System (ADS)

Ammonia and amines are common trace gases in the atmosphere and have a variety of both biogenic and anthropogenic sources, with a major contribution coming from agricultural sites. In addition to their malodorous nature, both ammonia and amines have been shown to enhance particle formation from acids such as nitric, sulfuric and methanesulfonic acids, which has implications for visibility, human health and climate. A key component of quantifying the effects of these species on particle formation is accurate gas-phase measurements in both laboratory and field studies. However, these species are notoriously difficult to measure as they are readily taken up on surfaces, including onto glass surfaces from aqueous solution as established in the present studies. We describe here a novel technique for measuring gas-phase ammonia and amines that involves uptake onto a weak cation exchange resin followed by extraction and analysis using ion chromatography. Two variants, one for ppb concentrations in air and the second with lower (ppt) detection limits, are described. The latter involves the use of a custom-designed high-pressure cartridge to hold the resin for in-line extraction. These methods avoid the use of sampling lines, which can lead to significant inlet losses of these compounds. They also have the advantages of being relatively simple and inexpensive. The applicability of this technique to ambient air is demonstrated in measurements made near a cattle farm in Chino, CA.

Dawson, M. L.; Perraud, V.; Gomez, A.; Arquero, K. D.; Ezell, M. J.; Finlayson-Pitts, B. J.



Optimisation of ion trap parameters for the quantification of chlormequat by liquid chromatography/mass spectrometry and the application in the analysis of pear extracts.  


Optimisation of the activation parameters for ion trap mass spectrometric analysis of the chlormequat cation using simplex optimisation enabled the product ion (m/z 58) response to be improved 1000-fold. A comparison of the sensitivity of the optimised ion trap mass spectrometer with that of a triple quadrupole mass spectrometer for liquid chromatography/tandem mass spectrometry (LC/MS/MS) showed that similar limits of detection (LODs) could be achieved. For the MS/MS transition of the (35)Cl precursor to the most abundant product, LODs were 0.8 ng cation mL(-1) (0.004 mg cation kg(-1) pear equivalent) and 1.0 ng cation mL(-1) (0.005 mg cation kg(-1) pear equivalent) on the triple quadrupole and ion trap instrument, respectively. PMID:10623939

Evans, C S; Startin, J R; Goodall, D M; Keely, B J



Speciation of arsenic in different types of nuts by ion chromatography-inductively coupled plasma mass spectrometry.  


In this work the quantitative determination and analytical speciation of arsenic were undertaken in different types of nuts, randomly purchased from local markets. The hardness of the whole nuts and high lipid content made the preparation of this material difficult for analysis. The lack of sample homogeneity caused irreproducible results. To improve the precision of analysis, arsenic was determined separately in nut oil and in the defatted sample. The lipids were extracted from the ground sample with the two portions of a mixture of chloroform and methanol (2:1). The defatted material was dried and ground again, yielding a fine powder. The nut oil was obtained by combining the two organic extracts and by evaporating the solvents. The two nut fractions were microwave digested, and total arsenic was determined by inductively coupled plasma mass spectrometry (ICP-MS). The results obtained for oils from different types of nuts showed element concentration in the range 2.9-16.9 ng g(-)(1). Lower levels of arsenic were found in defatted material (<0.1 ng g(-)(1) with the exception of Brazil nuts purchased with and without shells, 3.0 and 2.8 ng g(-)(1) respectively). For speciation analysis of arsenic in nut oils, elemental species were extracted from 2 g of oil with 12 mL of chloroform/methanol (2:1) and 8 mL of deionized water. The aqueous layer, containing polar arsenic species, was evaporated and the residue dissolved and analyzed by ion chromatography-ICP-MS. The anion exchange chromatography enabled separation of As(III), dimethylarsinic acid (DMAs(V)), monomethylarsonic acid (MMAs(V)), and As(V) within 8 min. Several types of nuts were analyzed, including walnuts, Brazil nuts, almonds, cashews, pine nuts, peanuts, pistachio nuts, and sunflower seeds. The recovery for the speciation procedure was in the range 72.7-90.6%. The primary species found in the oil extracts were As(III) and As(V). The arsenic concentration levels in these two species were 0.7-12.7 and 0.5-4.3 ng g(-)(1), respectively. The contribution of As in DMAs(V) ranged from 0.1 +/- 0.1 ng g(-)(1) in walnuts to 1.3 +/- 0.3 ng g(-)(1) in pine nuts. MMAs(V) was not detected in almonds, peanuts, pine nuts, sunflower seeds, or walnuts, and the highest concentration was found in pistachio nuts (0.5 +/- 0.2 ng g(-)(1)). PMID:15030196

Kannamkumarath, Sasi S; Wróbel, Kazimierz; Wróbel, Katarzyna; Caruso, Joseph A



Chromatography Theory and Modes  

NSDL National Science Digital Library

This site is an introductory lecture in outline form about chromatography. It appears directed toward biochemical separations. The coverage is broad but not deep. Discussions of counter-current separations, gel permeation, and ion exchange are accompanied by some mention of partition, paper, and gas chromatography. Useful illustrations are also included.


Simultaneous determination of total nitrogen and total phosphorus in environmental waters using alkaline persulfate digestion and ion chromatography.  


An ion chromatography (IC) method was developed for the simultaneous determination of total nitrogen and total phosphorus after alkaline persulfate digestion. This study takes advantage of advances in construction of high-resolution, high-capacity anion-exchange columns that can better tolerate the matrices typically encountered when a determination of total nitrogen and total phosphorous is required. Here, we used an electrolytically generated hydroxide eluent combined with a high-capacity, hydroxide-selective, anion-exchange column for the determination of total nitrogen (as nitrate-N) and total phosphorus (as phosphate-P) in environmental samples by IC. This method yielded LODs for nitrate-N and phosphate-P of 1.0 and 1.3 ?g/L, respectively. The LOQs determined for these analytes were 3.4 and 4.2 ?g/L, respectively. Due to the dilution factor required and the blank nitrate-N concentration after the persulfate digestion, the quantification limits increased for nitrate-N and phosphate-P to 171 and 63 ?g/L, respectively. The suitability of the method was evaluated by determining the nitrogen and phosphorus concentrations from known concentrations of organic-containing nitrogen and phosphorus compounds. In addition, environmental samples consisting of six different wastewaters and 48 reservoir samples were evaluated for total nitrogen and phosphorus. The recoveries of nitrogen and phosphorus from the organic-containing compounds ranged from 93.1 to 100.1% and 85.2 to 97.1%, respectively. In addition, good correlation between results obtained by the colorimetric method and IC was also observed. The linearity, accuracy, and evaluation of potential interferences for determining TN and TP will be discussed. PMID:25441080

De Borba, Brian M; Jack, Richard F; Rohrer, Jeffrey S; Wirt, Joan; Wang, Dongmei



Simultaneous determination of aliskiren and hydrochlorothiazide in tablets and spiked human urine by ion-pair liquid chromatography.  


An alternative method for analysis of aliskiren (ALI) and hydrochlorothiazde (HCT) in combined dosage forms by ion-pair reversed phase high performance liquid chromatography was developed and validated. The pharmaceutical preparations were analyzed using a C18 column (250 mm x 4.6 mm, 3 microm) with a mobile phase consisting of 25% methanol, 50% sodium monobasic phosphate aqueous solution containing 6 mM tetrabutylammonium bromide and 25% water at pH 7.2. Isocratic analysis was performed at a flow rate of 1 mL/min and a column temperature of 30 degrees C under direct UV detection at 210 nm. Paracetamol was used as internal standard. The validation was performed according to the ICH guidelines. The proposed method was linear over the concentration range of 0.250 to 60 and 0.1 to 10 microg/mL for ALI and HCT, respectively. The limits of detection and quantitation (LOD and LOQ) were 0.075 and 0.198 microg/mL, respectively, for ALI and 0.04 and 0.062 microg/mL, respectively, for HCT. The method proved to be specific, sensitive, precise and accurate with mean recovery values of 101.1 +/- 0.32% and 100.9 +/- 0.41% for ALI and HCT, respectively. The method robustness was evaluated by means of an experimental design. The proposed method was applied successfully to spiked human urine samples with mean recoveries of 98.8 +/- 0.36% and 98.1 +/- 0.21% for ALI and HCT, respectively. PMID:24400438

Belal, F; Walash, M; El-Enany, N; Zayed, S



Quality evaluation of extracted ion chromatograms and chromatographic peaks in liquid chromatography/mass spectrometry-based metabolomics data  

PubMed Central

Background Extracted ion chromatogram (EIC) extraction and chromatographic peak detection are two important processing procedures in liquid chromatography/mass spectrometry (LC/MS)-based metabolomics data analysis. Most commonly, the LC/MS technique employs electrospray ionization as the ionization method. The EICs from LC/MS data are often noisy and contain high background signals. Furthermore, the chromatographic peak quality varies with respect to its location in the chromatogram and most peaks have zigzag shapes. Therefore, there is a critical need to develop effective metrics for quality evaluation of EICs and chromatographic peaks in LC/MS based metabolomics data analysis. Results We investigated a comprehensive set of potential quality evaluation metrics for extracted EICs and detected chromatographic peaks. Specifically, for EIC quality evaluation, we analyzed the mass chromatographic quality index (MCQ index) and propose a novel quality evaluation metric, the EIC-related global zigzag index, which is based on an EIC's first order derivatives. For chromatographic peak quality evaluation, we analyzed and compared six metrics: sharpness, Gaussian similarity, signal-to-noise ratio, peak significance level, triangle peak area similarity ratio and the local peak-related local zigzag index. Conclusions Although the MCQ index is suited for selecting and aligning analyte components, it cannot fairly evaluate EICs with high background signals or those containing only a single peak. Our proposed EIC related global zigzag index is robust enough to evaluate EIC qualities in both scenarios. Of the six peak quality evaluation metrics, the sharpness, peak significance level, and zigzag index outperform the others due to the zigzag nature of LC/MS chromatographic peaks. Furthermore, using several peak quality metrics in combination is more efficient than individual metrics in peak quality evaluation. PMID:25350128



Analysis of 19-nortestosterone residue in animal tissues by ion-trap gas chromatography-tandem mass spectrometry*  

PubMed Central

A rapid sample treatment procedure for the gas chromatography-tandem mass spectrometry (GC-MS) determination of 19-nortestosterone (19-NT) in animal tissues has been developed. In our optimized procedures, enzymatic hydrolysis with ?-glucuronidase from Escherichia coli was performed in an acetate buffer (pH 5.2, 0.2 mol/L). Next, the homogenate was mixed with methanol and heated at 60 °C for 15 min, then placed in an ice-bath at ?18 °C for 2 h. After liquid-liquid extraction with n-hexane, the analytes were subjected to a normal-phase solid phase extraction (SPE) C18 cartridge for clean-up. The dried organic extracts were derivatized with heptafluorobutyric anhydride (HFBA), and then the products were injected into GC-MS. Using electron impact mass spectrometry (EI-MS) with positive chemical ionization (PCI), four diagnostic ions (m/z 666, 453, 318, and 306) were determined. A standard calibration curve over the concentration range of 1–20 ng/g was reached, with Y=467 084X?68 354 (R 2=0.999 7) for 19-NT, and the detection limit was 0.3 ng. When applied to spiked samples collected from bovine and ovine, the recoveries ranged from 63% to 101% with relative standard deviation (RSD) between 2.7% and 8.9%. The procedure is a highly efficient, sensitive, and more economical method which offers considerable potential to resolve cases of suspected nandrolone doping in husbandry animals. PMID:21634039

Jiang, Jin-qing; Zhang, Lei; Li, Guang-ling; Zhang, Hai-tang; Yang, Xue-feng; Liu, Jun-wei; Li, Ren-feng; Wang, Zi-liang; Wang, Jian-hua



Chemometric Analysis of Gas Chromatography – Mass Spectrometry Data using Fast Retention Time Alignment via a Total Ion Current Shift Function  

SciTech Connect

A critical comparison of methods for correcting severely retention time shifted gas chromatography-mass spectrometry (GC-MS) data is presented. The method reported herein is an adaptation to the Piecewise Alignment Algorithm to quickly align severely shifted one-dimensional (1D) total ion current (TIC) data, then applying these shifts to broadly align all mass channels throughout the separation, referred to as a TIC shift function (SF). The maximum shift varied from (-) 5 s in the beginning of the chromatographic separation to (+) 20 s toward the end of the separation, equivalent to a maximum shift of over 5 peak widths. Implementing the TIC shift function (TIC SF) prior to Fisher Ratio (F-Ratio) feature selection and then principal component analysis (PCA) was found to be a viable approach to classify complex chromatograms, that in this study were obtained from GC-MS separations of three gasoline samples serving as complex test mixtures, referred to as types C, M and S. The reported alignment algorithm via the TIC SF approach corrects for large dynamic shifting in the data as well as subtle peak-to-peak shifts. The benefits of the overall TIC SF alignment and feature selection approach were quantified using the degree-of-class separation (DCS) metric of the PCA scores plots using the type C and M samples, since they were the most similar, and thus the most challenging samples to properly classify. The DCS values showed an increase from an initial value of essentially zero for the unaligned GC-TIC data to a value of 7.9 following alignment; however, the DCS was unchanged by feature selection using F-Ratios for the GC-TIC data. The full mass spectral data provided an increase to a final DCS of 13.7 after alignment and two-dimensional (2D) F-Ratio feature selection.

Nadeau, Jeremy S.; Wright, Bob W.; Synovec, Robert E.



Multiresidue analysis of 50 pesticides in grape, pomegranate, and mango by gas chromatography-ion trap mass spectrometry.  


A selective and sensitive multiresidue analysis method is reported for simultaneous determination of 50 pesticides of different chemical classes in three commercially important fruits of different nature viz. grape, pomegranate, and mango. The sample preparation method involves extraction of a 10 g sample with 10 mL of ethyl acetate; cleanup by dispersive solid phase extraction with primary secondary amine (PSA, 25 mg) for grape and PSA + graphitized carbon black (25 + 5 mg) for pomegranate and mango; and determination by gas chromatography-ion trap mass spectrometry through multiple reaction monitoring (MRM). Sample preparation under acidified (pH 4) and cold (<4 degrees C) conditions, use of PTV-large volume injection (20 microL) through multibaffled liner and chromatographic separation on a short 10 m VF-5MS capillary column gave a satisfactory response for all of the analytes including relatively unstable compounds such as captan, captafol, folpet, endrine, and iprodione within 31.8 min. The limit of quantification (LOQ) of most of the compounds was

Savant, Rahul H; Banerjee, Kaushik; Utture, Sagar C; Patil, Sangram H; Dasgupta, Soma; Ghaste, Manoj S; Adsule, Pandurang G



Quantitative analysis of trimethobenzamide hydrochloride by ion-pair column chromatography and semiquantitative analysis of 3,4,5-trimethoxybenzoic acid by thin-layer chromatography.  


An ion-pair column chromatographic/UV spectrophotometric method for assaying trimethobenzamide hydrochloride in capsules and injections is presented, as well as a method for the detection of 3,4,5- trimethoxybenzoic acid in trimethobenzamide hydrochloride bulk drug and dosage forms. Results obtained by the USP XX, Pharmacopeial Forum, and ion-pair column assay procedures are compared, and results of a collaborative study of the proposed assay and impurity detection methods are presented. PMID:6726641

Naviasky, H



Characterization of molecular mass ranges of two coal tar distillate fractions (creosote and anthracene oils) and aromatic standards by LD-MS, GC-MS, probe-MS and size-exclusion chromatography  

SciTech Connect

Laser-desorption mass spectrometry (LD-MS) method development was undertaken to improve estimates of mass ranges for complex hydrocarbon mixtures. A creosote oil, an anthracene oil, and a mixture of known polynuclear aromatic hydrocarbon (PAH) compounds were examined. The formation of cluster ions was possible without overloading the detector system. These multimer ions overlapped with higher-mass ion signals from the sample. However, careful balancing of sample concentration, laser power, total ion current, and delayed ion extraction appears to show high-mass materials without generating high-mass multimer (artifact) ions. It is possible to suppress the formation of cluster ions by keeping low target concentrations and, consequently, low gas phase concentrations formed by the laser pulse. The principal method used in this work was the fractionation of samples by planar chromatography followed by successive LD-MS analysis of the separated fractions directly from the chromatographic plates. This method separated the more abundant small molecules from the less abundant large molecules to permit the generation of their mass spectra independently, as well as reducing the concentration of sample by spreading over the PC-plate. The technique demonstrably suppressed multimer formation and greatly improved the reproducibility of the spectra. Results showed the presence of molecule ions in the ranges m/z 1000-2000 for the anthracene oil sample and m/z 600-1500 for the creosote oil sample, tailing off to m/z about 5,000. The creosote oil contained significantly less of this high-mass material than the anthracene oil sample, and in both cases, high-mass material was only present in low quantities. The method outlined in the paper appears directly applicable to the characterization of heavier coal and petroleum derived fractions. 44 refs., 14 figs., 3 tabs.

T.J. Morgan; A. George; P. A'lvarez; M. Millan; A.A. Herod; R. Kandiyoti [Imperial College London, London (United Kingdom). Department of Chemical Engineering



Simultaneous ionization and analysis of 84 anabolic androgenic steroids in human urine using liquid chromatography-silver ion coordination ionspray/triple-quadrupole mass spectrometry.  


Metal ion coordination ionspray (M(+) CIS) ionization is a powerful technique to enhance ionization efficiency and sensitivity. In this study, we developed and validated an analytical method for simultaneous ionization and analysis of 84 anabolic androgenic steroids (65 exogenous and 19 endogenous) using liquid chromatography-silver ion coordination ionspray/triple-quadrupole mass spectrometry (LC-Ag(+) CIS/MS/MS). The concentrations of silver ions and organic solvents have been optimized to increase the amount of silver ion coordinated complexes. A combination of 25??M of silver ions and methanol showed the best sensitivity. The validation results showed the intra- (0.8-9.2%) and inter-day (2.5-14.9%) precisions, limits of detection (0.0005-5.0?ng/mL), and matrix effect (71.8-100.3%) for the screening analysis. No significant ion suppression was observed. In addition, this method was successfully applied to analysis of positive samples from suspected abusers and useful for the detection of the trace levels of anabolic steroids in human urine samples. PMID:25382000

Kim, So-Hee; Cha, Eun-Ju; Lee, Kang Mi; Kim, Ho Jun; Kwon, Oh-Seung; Lee, Jaeick



Investigation of isomeric flavanol structures in black tea thearubigins using ultraperformance liquid chromatography coupled to hybrid quadrupole/ion mobility/time of flight mass spectrometry.  


Ultra performance liquid chromatography (UPLC) when coupled to ion mobility (IMS)/orthogonal acceleration time of flight mass spectrometry is a suitable technique for analyzing complex mixtures such as the black tea thearubigins. With the aid of this advanced instrumental analysis, we were able to separate and identify different isomeric components in the complex mixture which could previously not be differentiated by a conventional high performance liquid chromatography/tandem mass spectrometry. In this study, the difference between isomeric structures theasinensins, proanthocyanidins B-type and rutin (quercetin-3O-rutinoside) were studied, and these are present abundantly in many botanical sources. The differentiation between these structures was accomplished according to their acquired mobility drift times differing from the traditional investigations in mass spectrometry, where calculation of theoretical collisional cross sections allowed assignment of the individual isomeric structures. The present work demonstrates UPLC-IMS-MS as an efficient technology for isolating and separating isobaric and isomeric structures existing in complex mixtures discriminating between them according to their characteristic fragment ions and mobility drift times. Therefore, a rational assignment of isomeric structures in many phenolic secondary metabolites based on the ion mobility data might be useful in mass spectrometry-based structure analysis in the future. PMID:25395124

Yassin, Ghada H; Grun, Christian; Koek, Jean H; Assaf, Khaleel I; Kuhnert, Nikolai



Effect of suppressor current intensity on the determination of glyphosate and aminomethylphosphonic acid by suppressed conductivity ion chromatography.  


This paper presents the application of ion chromatography with electrolytic eluent generation and mobile phase suppression for the direct conductimetric detection of glyphosate and its degradation product aminomethylphosphonic acid (AMPA). The compounds were separated on a Dionex AS18 anion exchange column with a 12-40 mM KOH step gradient from 9 to 9.5 min. The effect of the suppressor current intensity on the electrostatic interaction of these amphoteric compounds with the suppressor cation exchange membranes was evaluated. A suppressor current gradient technique was proposed for the limitation of peak broadening and baseline noise, in order to improve method sensitivity and detectability. It was observed that residual sample carbonates co-eluted with AMPA when a large injection loop was installed for the low level determination of both compounds in natural waters. For this reason, glyphosate was isocratically eluted using 33 mM KOH in order to decrease analysis time within 10 min and a column clean up step using 100 mM KOH was used to ensure retention time reproducibility. The developed method was applied to the analysis of drinking and natural water and it was further successfully applied to orange samples with slight modifications. Instrumental LOD for glyphosate was 0.24 microg/L, while method LOD was 0.54 microg/L for spring waters and 0.01 mg/kg for oranges using a 1000 microL direct loop injection of the sample. Intra-day and inter-day precision (as %RSD) for water samples was 4.6% and 12% at a spiking level of 2 microg/L, and the recovery ranged from 64% to 88% depending on sample conductivity. For orange samples, the inter-day precision was 1.4% at a spiking level of 4.4 mg/kg, while overall recovery was 103%. The developed method is direct, fast, sensitive and relatively inexpensive, and could be used as an ideal fast screening tool for the monitoring of glyphosate residues in water and fruit samples. PMID:20399436

Dimitrakopoulos, Ioannis K; Thomaidis, Nikolaos S; Megoulas, Nikolaos C; Koupparis, Michael A



Solidphase extraction–high-performance liquid chromatography–ion trap mass spectrometry for analysis of trace concentrations of macrolide antibiotics in natural and waste water matrices  

Microsoft Academic Search

A method using solid-phase extraction (SPE) combined with high-performance liquid chromatography–ion trap tandem mass spectrometry (LC–MS–MS) has been developed for determination of trace concentrations of erythromycin-H2O (ETM-H2O), roxithromycin (RTM) and tylosin (TLS) in natural and waste water matrices. These macrolides (MLs) were extracted from water samples using Oasis HLB cartridges, and the average recovery was 93.6±8.6, 92.1±10.0, and 94.3±8.9% for

S. Yang; K. H. Carlson



Determination of trace labile copper in environmental waters by magnetic nanoparticle solid phase extraction and high-performance chelation ion chromatography.  


Cobalt magnetic nanoparticles surface functionalised with iminodiacetic acid were evaluated as a nano-particulate solid phase extraction absorbent for copper ions (Cu(2+)) from environmental water samples. Using an external magnetic field, the collector nanoparticles could be separated from the aqueous phase, and adsorbed ions simply decomplexed using dilute HNO3. Effects of pH, buffer concentration, sample and sorbent volume, extraction equilibrium time, and interfering ion concentration on extraction efficiency were investigated. Optimal conditions were then applied to the extraction of Cu(2+) ions from natural water samples, prior to their quantitation using high-performance chelation ion chromatography. The limits of detection (LOD) of the combined extraction and chromatographic method were ~0.1 ng ml(-1), based upon a 100-fold preconcentration factor (chromatographic performance; LOD=9.2 ng ml(-1) Cu(2+)), analytical linear range from 20 to 5000 ng mL(-1), and relative standard deviations=4.9% (c=1000 ng ml(-1), n=7). Accuracy and precision of the combined approach was verified using a certified reference standard estuarine water sample (SLEW-2) and comparison of sample determinations with sector field inductively coupled plasma mass spectrometry. Recoveries from the addition of Cu(2+) to impacted estuarine and rain water samples were 103.5% and 108.5%, respectively. Coastal seawater samples, both with and without prior UV irradiation and dissolved organic matter removal were also investigated using the new methodology. The effect of DOM concentration on copper availability was demonstrated. PMID:25640140

Wei, Z; Sandron, S; Townsend, A T; Nesterenko, P N; Paull, B



Reversed-phase ion-pair high-performance liquid chromatography of mercaptoacetate and N-acetylcysteine after derivatization with N-(1-pyrene)maleimide and N-(7-dimethylamino-4-methyl-3-coumarinyl)maleimide.  


We have developed a high-performance liquid chromatographic system capable of resolving mercaptoacetate and N-acetylcysteine as their N-(1-pyrene)maleimide (PM) and N-(7-dimethylamino-4-methyl-3-coumarinyl)maleimide (DACM) derivatives. Good resolution was obtained by ion pairing with tetramethylammonium hydroxide and chromatography on reversed phase. The detection limits for the thiols were about 50 fmol as their DACM derivatives and about 400 fmol as their PM derivatives. The method is illustrated by chromatography of urinary thiols which indicates that the derivatization and chromatography procedures should be well applicable in bioanalytical work. PMID:7096475

Kågedal, B; Källberg, M



Liquid chromatography tandem mass spectrometry with ion trap and triple quadrupole analyzers for determination of thyreostatic drugs in urine and muscle tissue.  


Liquid chromatography tandem mass spectrometry methods were developed and validated to screen for and confirm residues of the thyreostatic drugs: tapazole, thiouracil, methylthiouracil, propylthiouracil, and phenylthiouracil in bovine and porcine urine and muscle tissues using dimethylthiouracil as internal standard. Thyreostats were extracted from urine samples with diethyl ether after derivatisation with 3-iodobenzylbromide in basic medium (pH 8.0) and analyzed by gradient elution on a Nucleosil C18 column with ion trap mass spectrometry detection using an electrospray source and triple quadrupole MS detection with turbo spray source. Thyreostats were extracted from muscle tissue with methanol, the denaturation of matrix protein was performed and then the same steps as for the urine samples were carried out. The methods were validated in accordance with the Commission Decision 2002/657/EC. Good thyreostats recoveries were obtained (from 82% to 117%) as well as acceptable within-lab reproducibility. The values of the decision limit CC? and the detection capability CC? of five thyreostatic drugs are found to be below the recommended concentration set at 10 ?g L(-1) (kg(-1)). The results of the validation demonstrate that liquid chromatography mass spectrometry with ion trap detection does not meet the criteria for confirmation for some thyreostats and therefore was applied for screening purpose only. PMID:21742128

Wozniak, Barbara; Zuchowska, Iwona Matraszek; Zmudzki, Jan; Jedziniak, Piotr; Korycinska, Beata; Sielska, Katarzyna; Witek, Sebastian; Klopot, Alicja



Residues from low-order energetic materials: the comparative performance of a range of sampling approaches prior to analysis by ion chromatography.  


A quantitative study of common forensic evidence collection devices for the recovery of low-explosive residues from non-porous glass and plastic is presented herein. Swabbing materials including cotton, rayon, Nomex(®) (poly(isophthaloylchloride/m-phenylenediamine)), Teflon/Teflon-coated fibreglass (polytetrafluoroethylene) and adhesive-coated tapes were used to collect known quantities of up to 14 forensically relevant inorganic and organic anion and cation species from both surfaces. Analysis was performed using two validated ion chromatography methods. This study revealed that all swabs and surfaces contributed highly variable levels of interfering ionic species and that swabbing materials showed variance in the quantities and total number of analytes recovered from both surfaces. Teflon and Nomex(®) materials demonstrated the most promise due to their ability to collect and release analytes into simple extraction solvents as well as displaying relatively low endogenous interference. In parallel, the ability to extract residue directly from both surfaces via the addition of a suitable extraction solvent was investigated instead of swabbing. This work highlights that direct solvent extraction from a surface should be considered as an alternative approach, especially for small areas or objects. To the best of our knowledge, this work represents the most comprehensive study of the efficiencies of sample collection technologies for low-explosive residues prior to analysis by ion chromatography. PMID:24314502

Szomborg, Katarzyna; Jongekrijg, Fleur; Gilchrist, Elizabeth; Webb, Tony; Wood, Dan; Barron, Leon



Characteristic fragmentation patterns of the trimethylsilyl and trimethylsilyl-oxime derivatives of various saccharides as obtained by gas chromatography coupled to ion-trap mass spectrometry.  


The fragmentation patterns of selected glycosidic linkage containing non-reducing (methylmannoside, methylgalactoside, lactitol, sucrose, trehalose, raffinose, erlose, melezitose) and reducing saccharides (maltose, cellobiose, lactose, melibiose, palatinose, primeverose, rutinose) have been compared as their trimethylsilyl and as their trimethylsilyl-oxime derivatives. Fragmentation characteristics of the glycosidic linkage containing trimethylsilyl-oxime derivatives have been investigated at the first time: these spectra are not available in the official libraries (NIST, Wiley). Applying gas chromatography-ion trap mass spectrometry, informative fragments of high masses with high intensities have been obtained. Results confirmed characteristic differences between the simple trimethylsilyl derivative providing non-reducing glycosides and the trimethylsilyl, syn and antioxime species. Fragmentation starts at the glycosidic linkage resulting in the case of the non-reducing di- and trisaccharides in two, identical fragments of ring structure, with the abundant selective fragment ion at m/z=361. In the case of reducing disaccharides fragmentation provides two different moieties: one moiety of ring structure at m/z=361, and one of the open chain trimethylsilyl-oxime moiety with two special fragment ions at m/z=361 and at m/z=538. These fragmentation patterns proved to be independent on the position of the glycosidic linkage. Distribution of the selective fragment ions, obtained from their total ion current elutions, was evaluated on a quantitative basis, expressed in percentages of the total of ions formed. Reproducibility in the formation of these selective fragment ions, depending on their amount to be fragmented, proved to be proper for identification and quantitation purposes, equally. On this basis, in addition to the authentic ones, also two reducing disaccharides (primeverose and rutinose), as authentic compounds not available on the market, were identified and quantified in natural matrices. PMID:18061601

Füzfai, Zs; Boldizsár, I; Molnár-Perl, I



Chromatography Nomenclature and Definitions  

NSDL National Science Digital Library

This website gives the International Union of Pure and Applied Chemistry approved definitions in the field of chromatography. It is critical for students to appreciate the importance of using standardized nomenclature and definitions. Sections of the site include general terminology, terms related to the chromatographic system, terms related to the chromatographic process and the theory of chromatography, terms related to detection, ion exchange, liquid-liquid distribution (solvent extraction) and other related subjects.


Quantitation of Phenol Levels in Oil of Wintergreen Using Gas Chromatography-Mass Spectrometry with Selected Ion Monitoring  

ERIC Educational Resources Information Center

Industrial application of gas chromatography-mass spectrometry (GC-MS) analysis is a powerful technique that could be used to elucidate components of a complex mixture while offering the benefits of high-precision quantitative analysis. The natural wintergreen oil is examined for its phenol concentration to determine the level of refining…

Sobel, Robert M.; Ballantine, David S.; Ryzhov, Victor



Particle beam liquid chromatography/mass spectrometry with negative ion chemical ionization for the confirmation of ivermectin residue in bovine milk and liver.  


Particle beam liquid chromatography/mass spectrometry (LC/MS) using negative ion chemical ionization was applied to the analysis of ivermectin residue in bovine milk and liver. Samples were prepared by liquid/liquid extraction followed by alumina B solid-phase extraction clean-up. On-line LC/MS of extracts was carried out on a C-18 bonded silica column. Signals were observed from on-column injections of 4 ng dihydro-avermectin B1a (H2B1a) in extracts equivalent to 2 ml milk or 0.3 g liver. The specificity required for a regulatory confirmation procedure was achieved by monitoring the H2B1a molecular ion and four fragment ions. Ion chromatogram peak areas were at least three times greater than control samples integrated over the same time window. Coeluting matrix compounds enhanced the response and altered the abundance pattern of H2B1a. To compensate for this matrix effect, control milk extracts were spiked with H2B1a standard and used for the abundance matching for the abundance matching requirement of regulatory confirmation. PMID:8461342

Heller, D N; Schenck, F J



Determination of lipoic acid, Trolox methyl ether and tocopherols in human plasma by liquid-chromatography and ion-trap tandem mass spectrometry.  


A method for the simultaneous determination of lipoic acid and/or Trolox methyl ether, along with ?-, ?- and ?-tocopherol was developed using liquid chromatography-tandem mass spectrometry with negative electrospray ionization (HPLC-ESI-MS/MS) in an ion-trap mass spectrometer. Detection and quantification were accomplished by a multiple reaction monitoring method, using specific transitions from precursor ion to product ion for each analyte. Chromatographic separation was achieved in a 12?min run using a C(18) -bonded phase and methanol-aqueous ammonium acetate elution gradient. Linear correlations of the chromatographic peak area (r.u. × s(-1) ) to the injected amount (ng) gave the slope values (r.u. × s(-1) ?×?ng(-1) ) 2.34?×?10(4) for ?-tocopherol, 5.05?×?10(4) for ?-tocopherol, 1.27?×?10(5) for ?-tocopherol, 8.86?×?10(5) for lipoic acid and 1.23?×?10(5) for Trolox methyl ether. The lower limit of quantification ranged between 0.02 and 1.22?ng for Trolox methyl ether and lipoic acid. MS(3) experiments of ?- and ?-tocopherol suggest ion-radical reactions and dependence of the tocopherol fragmentation pattern on the phenolic ring methylation degree. The method is shown to be applicable to measurement of these metabolites in human serum after extraction. PMID:22222855

Montero, Olimpio; Ramírez, María; Sánchez-Guijo, Alberto; González, Constancio



Effect of humic acid on absorption-release processes in the bottom sediments-Yenisei river water system as studied by dual-column ion chromatography and ?-ray spectrometry  

Microsoft Academic Search

The effect of humic acid on absorption-release processes in the bottom sediments-Yenisei river water system was studied by\\u000a dual-column ion chromatography and ?-ray spectrometry. With the use of ion chromatography, it was found that processes related\\u000a to the absorption of SO\\u000a 4\\u000a 2?\\u000a and Cl? anions by a solid phase with the release of NO\\u000a 3\\u000a ?\\u000a , PO\\u000a 4

L. G. Bondareva; O. P. Kalyakina; A. Ya. Bolsunovskii



High-performance liquid chromatography with paired ion electrospray ionization (PIESI) tandem mass spectrometry for the highly sensitive determination of acidic pesticides in water.  


A novel method based on the paired ion electrospray ionization (PIESI) mass spectrometry has been developed for determination of acidic pesticides at ultratrace levels in surface and ground waters. The proposed approach provides greatly enhanced sensitivity for acidic pesticides and overcomes the drawbacks of the less sensitive negative ion mode ESI-MS. The limits of detection (LODs) of 19 acidic pesticides were evaluated with four types of dicationic ion-pairing reagent (IPR) in both single ion monitoring (SIM) and selected reaction monitoring (SRM) mode. The LOD of 19 pesticides obtained with the use the optimal dicationic ion-pairing reagent ranged from 0.6pg to 19pg, indicating the superior sensitivity provided by this method. The transition pathways for different pesticide-IPR complexes during the collision induced dissociation (CID) were identified. To evaluate and eliminate any matrix effects and further decrease the detection limits, off-line solid-phase extraction (SPE) was performed for DI water and a river water matrix spiked with 2000ng L(-1) and 20ng L(-1) pesticides standards respectively, which showed an average percent recovery of 93%. The chromatographic separation of the acidic pesticides was conducted by high-performance liquid chromatography (HPLC) using a C18 column (250mm×2.1mm) in the reversed phase mode using linear gradient elution. The optimized HPLC-PIESI-MS/MS method was utilized for determination of acidic pesticide at ng L(-1) level in stream/pond water samples. This experimental approach is 1-3 orders of magnitude more sensitive for these analytes than other reported methods performed in the negative ion mode. PMID:23910961

Xu, Chengdong; Armstrong, Daniel W



Analysis of sugars and sugar polyols in atmospheric aerosols by chloride attachment in liquid chromatography/negative ion electrospray mass spectrometry.  


Sugars and sugar polyols are relatively abundant groups of water-soluble constituents in atmospheric aerosols. This paper describes a method that uses liquid chromatography-mass spectrometry (LC-MS) to analyze sugars and sugar polyols in atmospheric aerosols, ranging from C3 sugar alcohols to trisaccharides. Postcolumn addition of chloroform in acetonitrile was found to greatly enhance ionization of these compounds by forming chloride adduct ions in the negative-ion mode using electrospray ionization. A gradient elution program starting at 5%:95% H20/acetonitrile and ending at 30%:70% H2O/acetonitrile provides baseline separations of the sugars and sugar polyols on an amino-based carbohydrate column. The detection limits based on quantification of [M + 35Cl]- adduct ions were in the order of 0.1 microM. By eliminating the need for derivatization, this LC-MS based method provides a simpler alternative method to the commonly used and more laborious gas-chromatography based methods. It also has an additional advantage of being able to quantify trisaccharide sugars. The method was applied to analyze 30 ambient samples of fine particulate matter collected at a site away from urban centers in Hong Kong. The sugar compounds positively identified and detected in the ambient samples included four sugar alcohols (glycerol, erythritol, xylitol, and mannitol), three monosacchride sugars (xylose, fructose, and glucose), two disaccharides (sucrose, trehalose), two trisaccharides (melezitose, raffinose), and one anhydrosugar (levoglucosan). The sum of these sugar and sugar polyol compounds ranged from 38 to 1316 ng m(-3), accounting for an average of 1.3% organic carbon mass. Through the use of a principal component analysis of the ambient measurements, the mono- to trisactharide sugars and C3-C5 sugar polyols were identified to be mainly associated with soil/soil microbiota while the anhydrosugar (levoglucosan) was associated with biomass burning. PMID:17438800

Wan, Eric C H; Yu, Jian Zhen



Rapid Purification of Recombinant Green Fluorescent Protein Using the Hydrophobic Properties of an HPLC Size-Exclusion Column  

Microsoft Academic Search

The green fluorescent protein (GFP) of the jelly fish Aequoria victoria was cloned into an Escherichia coli cell line that is a methionine auxotroph. The recombinant GFP (rGFP) was isolated from the cells and purified using a simple procedure consisting of only two chromatographic steps: size-exclusion chromatography and ion-exchange HPLC. Due to the hydrophobic nature of the protein, the surface

J. R. Deschamps; C. E. Miller; K. B. Ward



Simultaneous qualitative and quantitative determination of phenolic compounds in Aloe barbadensis Mill by liquid chromatography-mass spectrometry-ion trap-time-of-flight and high performance liquid chromatography-diode array detector.  


An effective and comprehensive method was developed for the simultaneous analysis of phenolic compounds in the dried exudate of Aloe barbadensis Mill by liquid chromatography-mass spectrometry-ion trap-time-of-flight (LCMS-IT-TOF) and high performance liquid chromatography-diode array detector (HPLC-DAD). Qualitative analysis of all the compounds presented in A. barbadensis Mill was performed on LCMS-IT-TOF, and the diagnostic fragmentation patterns of different types of phenolic compounds (chromones, phenyl pyrones, naphthalene derivative, anthrones and anthraquinones) were discussed on the basis of ESI-IT-TOF MS of components in A. barbadensis Mill and eleven authentic standards. Under the optimal HPLC-DAD chromatographic conditions, quantification of 11 typical phenolic compounds in 15 batches of A. barbadensis Mill was achieved on an Agilent TC-C18 column using gradient elution with a solvent system of methanol and water at a flow rate of 1.0mLmin(-1) and detected at 230nm. All calibration curves exhibited good linear relationship (r(2)>0.9991). The relative standard deviation values for intraday precision were less than 2% with accuracies between 98.21% and 104.57%. The recoveries of the eleven analytes ranged from 97.53 to 105.00% with RSDs less than 2%. This is the first simultaneous characterization and quantitative determination of multiple phenolic compounds in A. barbadensis Mill from locally grown cultivars in China by LCMS-IT-TOF and HPLC-DAD, which can be applied to standardize the quality of A. barbadensis Mill and the future design of nutraceutical and cosmetic preparations. PMID:23542732

Wu, Xiaofang; Ding, Wenjing; Zhong, Jiasheng; Wan, Jinzhi; Xie, Zhiyong



ORIGINAL PAPER Development of a methodology utilizing gas chromatography  

E-print Network

ORIGINAL PAPER Development of a methodology utilizing gas chromatography ion-trap tandem mass chromatography coupled with an ion-trap tandem mass spectrometry detection system (IT-MS/MS) was developed. Four

Mazumder, Asit


[Screening and confirmation of 24 hormones in cosmetics by ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry].  


A method of ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (UPLC-LTQ/Orbitrap MS) was established to screen and confirm 24 hormones in cosmetics. Various cosmetic samples were extracted with methanol. The extract was loaded onto a Waters ACQUITY UPLC BEH C18 column (50 mm x 2.1 mm, 1.7 microm) using a gradient elution of acetonitrile/water containing 0.1% (v/v) formic acid for the separation. The accurate mass of quasi-molecular ion was acquired by full scanning of electrostatic field orbitrap. The rapid screening was carried out by the accurate mass of quasi-molecular ion. The confirmation analysis for targeted compounds was performed with the retention time and qualitative fragments obtained by data dependent scan mode. Under the optimal conditions, the 24 hormones were routinely detected with mass accuracy error below 3 x 10(-6) (3 ppm), and good linearities were obtained in their respective linear ranges with correlation coefficients higher than 0.99. The LODs (S/N = 3) of the 24 compounds were < or = 10 microg/kg, which can meet the requirements for the actual screening of cosmetic samples. The developed method was applied to screen the hormones in 50 cosmetic samples. The results demonstrate that the method is a useful tool for the rapid screening and identification of the hormones in cosmetics. PMID:25185307

Li, Zhaoyong; Wang, Fengmei; Niu, Zengyuan; Luo, Xin; Zhang, Gang; Chen, Junhui



Ion chromatography/inductively coupled plasma mass spectrometry for simultaneous determination of glyphosate, glufosinate, fosamine and ethephon at nanogram levels in water.  


This paper describes the first approach that simultaneously quantifies four polar, water-soluble organophosphorus herbicides, i.e., glyphosate, glufosinate, fosamine and ethephon, at nanogram levels in environmental waters. The target herbicides were separated completely by ion chromatography (IC) on a polymer anion-exchange column, Dionex IonPac AS16 (4.0 mm x 250 mm), with 30 mM citric acid flowing at 0.70 mL min(-1) as the eluent. On-line inductively coupled plasma mass spectrometry (ICP-MS) using a quadrupole mass spectrometer was employed as a sensitive and selective detector of the effluents. Various parameters affecting the separation and detection were systematically examined and optimized. Detection limits of the herbicides achieved with the proposed IC/ICP-MS method were 1.1-1.4 microg L(-1) (as compound) based on a 500-microL sample injection. Matrix anions, metal ions, phosphate, polyphosphates, non-polar and other polar organophosphorus pesticides showed no interference. The developed method was validated using reservoir water, treated water and NEWater samples spiked at the level of 10-25 microg L(-1) with satisfactory recoveries (95-109%). It is applicable to the simultaneous determination of microg L(-1) concentrations of the herbicides in polluted water. PMID:17443488

Guo, Zhong-Xian; Cai, Qiantao; Yang, Zhaoguang



Organic solvent and temperature-enhanced ion chromatography-high resolution mass spectrometry for the determination of low molecular weight organic and inorganic anions.  


There has recently been increased interest in coupling ion chromatography (IC) to high resolution mass spectrometry (HRMS) to enable highly sensitive and selective analysis. Herein, the first comprehensive study focusing on the direct coupling of suppressed IC to HRMS without the need for post-suppressor organic solvent modification is presented. Chromatographic selectivity and added HRMS sensitivity offered by organic solvent-modified IC eluents on a modern hyper-crosslinked polymeric anion-exchange resin (IonPac AS18) are shown using isocratic eluents containing 5-50mM hydroxide with 0-80% methanol or acetonitrile for a range of low molecular weight anions (<165Da). Comprehensive experiments on IC thermodynamics over a temperature range between 20-45°C with the eluent containing up to 60% of acetonitrile or methanol revealed markedly different retention behaviour and selectivity for the selected analytes on the same polymer based ion-exchange resin. Optimised sensitivity with HRMS was achieved with as low as 30-40% organic eluent content. Analytical performance characteristics are presented and compared with other IC-MS based works. This study also presents the first application of IC-HRMS to forensic detection of trace low-order anionic explosive residues in latent human fingermarks. PMID:25732588

Gilchrist, Elizabeth S; Nesterenko, Pavel N; Smith, Norman W; Barron, Leon P



Mass Spectrometry Parameters Optimization for the 46 Multiclass Pesticides Determination in Strawberries with Gas Chromatography Ion-Trap Tandem Mass Spectrometry  

NASA Astrophysics Data System (ADS)

Multiclass analysis method was optimized in order to analyze pesticides traces by gas chromatography with ion-trap and tandem mass spectrometry (GC-MS/MS). The influence of some analytical parameters on pesticide signal response was explored. Five ion trap mass spectrometry (IT-MS) operating parameters, including isolation time (IT), excitation voltage (EV), excitation time (ET), maximum excitation energy or " q" value (q), and isolation mass window (IMW) were numerically tested in order to maximize the instrument analytical signal response. For this, multiple linear regression was used in data analysis to evaluate the influence of the five parameters on the analytical response in the ion trap mass spectrometer and to predict its response. The assessment of the five parameters based on the regression equations substantially increased the sensitivity of IT-MS/MS in the MS/MS mode. The results obtained show that for most of the pesticides, these parameters have a strong influence on both signal response and detection limit. Using the optimized method, a multiclass pesticide analysis was performed for 46 pesticides in a strawberry matrix. Levels higher than the limit established for strawberries by the European Union were found in some samples.

Fernandes, Virgínia C.; Vera, Jose L.; Domingues, Valentina F.; Silva, Luís M. S.; Mateus, Nuno; Delerue-Matos, Cristina



Automated Gain Control and Internal Calibration With External Ion Accumulation Capillary liquid chromatography-electrospray ionization-fourier transform ion cyclotron resonance.  

SciTech Connect

When combined with capillary LC separations, Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (ESI-FTICR MS) has increasingly been applied for advanced characterization of proteolytic digests. Incorporation of external (to the ICR cell) ion accumulation multipoles with FTICR for ion pre selection and accumulation has enhanced the dynamic range, sensitivity and duty cycle of measurements. However, the highly variable ion production rate from an LC separation can result in overfilling of the external trap, resulting in m/z discrimination and fragmentation of peptide ions. An excessive space charge trapped in the ICR cell causes significant shifts in the detected ion cyclotron frequencies, reducing the achievable mass measurement accuracy (MMA) for protein identification. To eliminate m/z discrimination in the external ion trap, further increase the duty cycle and improve MMA, we developed a capability for data-dependent adjustment of ion accumulation times in the course of an LC separation, referred to as Automated Gain Control (AGC), in combination with low kinetic energy gated ion trapping and internal calibration using a dual-channel electrodynamic ion funnel. The system was initially evaluated in the analysis of a 0.5 mg/mL tryptic digest of bovine serum albumin. The implementation of LC/ESI/AGC/FTICR with internal calibration gave rise to a {approx} 10-fold increase in the number of identified tryptic peptides within mass measurement accuracy of 2 ppm as compared to that detected during the conventional LC/FTICR run with a fixed ion accumulation time and external calibration.




Hydrophilic interaction vs ion pair liquid chromatography for the determination of streptomycin and dihydrostreptomycin residues in milk based on mass spectrometric detection.  


Streptomycin (STR) and dihydrostreptomycin (DHSTR) are two of the most common aminoglycoside antibiotics used in veterinary medicine. The physicochemical properties of both substances, make their determination challenging. In the present study the development of methods based on ion-pair chromatography (IPC) and on hydrophilic interaction chromatography (HILIC), for the determination of the above mentioned aminoglycosides in the range of 100-1000 ?g L(-1) is described. The two methods were validated according to EU requirements for residues in food. The recoveries for the IPC method were 69.3% and 56.5% of STR and DHSTR, respectively, and for HILIC method 85.5% and 72.3%, respectively. The intra- and inter-day precision, studied at 100, 200 and 300 ?g kg?¹ levels in milk samples, gave %RSD ? 13 for both methods. LOQs for the HILIC method were 14 ?g kg?¹ for both analytes and for the IPC method were 109 and 31 ?g kg?¹, for STR and DHSTR, respectively. The sensitivity of the HILIC method is 80 and 210 times greater than that of the ICP method, for STR and DHSTR, respectively. PMID:20546761

Gremilogianni, Aikaterini M; Megoulas, Nikolaos C; Koupparis, Michael A



Separation and determination of metallocyanide complexes of Fe(II), Ni(II) and Co(III) by ion-interaction chromatography with membrane suppressed conductivity detection applied to analysis of oil refinery streams (sour water)  

Microsoft Academic Search

A separation and determination method for the analysis of cyanometallic complexes of Fe(II), Ni(II) and Co(III) was developed to be applied to the analysis of petroleum refinery streams (sour water). Ion-interaction chromatography was used employing an analytical column IonPac NS1 10?m and a chromatographic system ICS 2500 equipped with a membrane conductivity suppression ASRS ultra 4mm, both supplied by Dionex

Renata Souza e Silva; Maria de Fátima Batista de Carvalho; Ricardo Erthal Santelli



Evaluation of on-line high-performance size-exclusion chromatography, differential refractometry, and multi-angle laser light scattering analysis for the monitoring of the oligomeric state of human immunodeficiency virus vaccine protein antigen.  


Chiron has developed a novel mutant form of the human immunodeficiency virus (HIV) envelop protein, o-gp140, that is currently entering Human Phase 1 clinical trials for testing as a prophylactic HIV vaccine. The o-gp140 protein is oligomeric and the quaternary structure is thought to play an important role in its activity as an antigen. As o-gpl40 proceeds through the clinical trial process and prior to marketing approval, analytical methods that are able to demonstrate manufacturing consistency with respect to degree of oligomerization will need to be developed and validated. On-line high-performance size-exclusion chromatography, differential refractometry, and multi-angle laser light scattering analysis (HPSEC-RI-MALLS), a method commonly used to obtain the molar mass of macromolecules based on the Rayleigh-Gans-Debye approximation, was evaluated for this purpose. The results obtained demonstrated intra- and inter-day precisions to be 0.9 and 3.6% R.S.D., respectively. Accuracy was found to be equal to, or better than, 11% when comparing the known molar masses of test proteins to that of the molar masses determined by the method. Additionally, the method compared favorably to orthogonal native polyacrylamide gel electrophoresis and ultracentrifugation analyses. R-factor analysis was used to demonstrate that HPSEC-RI-MALLS is capable of discriminating compositional differences between o-gpl40 test lots. Based on the data presented, HPSEC-RI-MALLS may be a suitable manufacturing control method. PMID:15317413

Barackman, John; Prado, Isaias; Karunatilake, Chulani; Furuya, Kenji



A speciation methodology to study the contributions of humic-like and fulvic-like acids to the mobilization of metals from compost using size exclusion chromatography-ultraviolet absorption-inductively coupled plasma mass spectrometry and deconvolution analysis.  


High performance size-exclusion chromatography (HP-SEC) with UV absorption for organic matter detection and inductively coupled plasma mass spectrometry (ICP-MS) for elemental detection have been used to study the mobilization of metals from compost as a function of pH and the molecular mass of their complexes with dissolved organic matter (DOM). Due to its heterogeneous nature, organic matter mobilized from compost shows a continuous distribution of molecular masses in the range studied (up to 80kDa). In order to differentiate between the contribution of humic and fulvic acids (FA) to the organic matter mobilized in the pH range 5-10, their UV absorption chromatographic profiles have been deconvoluted with respect to the adjusted gaussian profiles of the humic and fulvic acids isolated from compost. Results show a preponderant contribution of fulvic acids at low pH values and an increasing percentage of humic acids (HA) mobilized at basic pH (up to 49% of total DOM at pH 10). A similar deconvolution procedure has been applied to the ICP-MS chromatograms of selected metals (Co, Cu, Pb and Bi). In general, both fulvic and humic acids contribute to the mobilization of divalent transition metals, such as copper or cobalt, whereas bismuth or lead are preferably associated to humic acids. Non-humic substances (HS) also contribute to the mobilization of cations, especially at acidic pHs. These conclusions have been extended to different elements based on deconvolution analysis results at pH 7. PMID:18068764

Laborda, Francisco; Bolea, Eduardo; Górriz, María P; Martín-Ruiz, María P; Ruiz-Beguería, Sergio; Castillo, Juan R



In vitro evaluation of total venom-antivenin immune complex formation and binding parameters relevant to antivenin protection against venom toxicity and lethality based on size-exclusion high-performance liquid chromatography.  


Total venom-antivenin immune complex formation and binding parameters relevant to antivenin protection against venom toxicity and lethality can be evaluated using size-exclusion high-performance liquid chromatography (SE-HPLC). Simple integration of regions within SE-HPLC elution profiles was used to compare binding characteristics of Crotalidae Polyvalent Immune Fab (Ovine) antivenin (FabAV) and Crotalus atrox (western diamondback rattlesnake; C. atrox), C. varidis varidis (prairie rattlesnake; C. v. v.), Agkistrodon contortrix contortrix (southern copperhead; A. c. c.), and A. piscivorus leukostoma (western cottonmouth; A. p. l.) venom. Areas associated with bound venom and antivenin ({Area(bnd)}) were evaluated using a logistic dose-response equation to estimate EC(50) and {Area(bnd)}(max). The relative magnitudes of EC(50), which inversely reflect venom-antivenin binding affinity, were C. atrox > C. v. v. > A. c. c. > A. p. l. Less than 50% of FabAV appeared to be reactive with each of the venoms based on {Area(bnd)}(max). Data was also consistent with FabAV binding to multiple sites on polyvalent antigens within the venoms. Evaluation of immune complex formation using SE-HPLC was compared to neutralization of phospholipase A(2) (PLA(2)) activity of C. atrox, A. c. c., and A. p. l. venom by FabAV as reported in the literature. Maximum neutralization of PLA(2) activity occurred, in general, prior to maximum immune complex formation. Venom-antivenin binding at EC(50) determined via SE-HPLC appeared to be greater than binding associated with neutralization of venom lethality in mice based on LD(50) and ED(50) reported by others. SE-HPLC analysis of venom-antivenin binding could provide a priori information, relevant to reducing the use of animals in evaluating antivenin protection against venom-induced toxicity and lethality. PMID:21392522

Sanny, Charles G



Molecular size and mass distributions of native starches using complementary separation methods: asymmetrical flow field flow fractionation (A4F) and hydrodynamic and size exclusion chromatography (HDC-SEC).  


Starch consists of a mixture of two ?-glucans built mainly upon ?-(1,4) linkages: amylose, an essentially linear polymer, and amylopectin, a branched polymer containing 5-6% of ?-(1,6) linkages. The aim of the present work was to analyze the structural properties of native starches displaying different amylose-to-amylopectin ratios and arising from different botanical sources, using asymmetrical flow field flow fractionation (A4F) and a combination of hydrodynamic and size-exclusion chromatography (HDC-SEC) coupled with multiangle laser light scattering, online quasi-elastic light scattering, and differential refractive index techniques. The procedure, based upon dimethyl sulfoxide pretreatment and then solubilization in water, generates a representative injected sample without altering the initial degree of polymerization. The amylopectin weight-average molar masses and radii of gyration were around 1.0 × 10(8)-4.8 × 10(8) g mol(-1) and 110-267 nm, respectively. For each starch sample, the hydrodynamic radius (R(H)) distributions and the molar mass distributions obtained from the two fractionation systems coupled with light scattering techniques were analyzed. The size determination scales were extended by means of R(H) calibration curves. HDC-SEC and A4F data could be matched. However, A4F enabled a better separation of amylopectins and therefore an enhanced structural characterization of the starches. The two advantages of this experimental approach are (1) it can directly obtain distributions as a function of both molar mass and size, while taking account of sample heterogeneity, and (2) it is possible to compare the results obtained using the different techniques through the direct application of R(H) distributions. PMID:20878394

Rolland-Sabaté, Agnès; Guilois, Sophie; Jaillais, Benoît; Colonna, Paul



Rapid screening and identification of multi-class substances of very high concern in textiles using liquid chromatography-hybrid linear ion trap orbitrap mass spectrometry.  


A new analytical method was established and validated for the analysis of 19 substances of very high concern (SVHCs) in textiles, including phthalic acid esters (PAEs), organotins (OTs), perfluorochemicals (PFCs) and flame retardants (FRs). After ultrasonic extraction in methanol, the textile samples were analyzed by high performance liquid chromatography-hybrid linear ion trap Orbitrap high resolution mass spectrometry (HPLC-LTQ/Orbitrap). The values of LOQ were in the range of 2-200mg/kg. Recoveries at two levels (at the LOQ and at half the limit of regulation) ranged from 68% to 120%, and the repeatability was lower than 13%. This method was successfully applied to the screening of SVHCs in commercial textile samples and is useful for the fast screening of various SVHCs. PMID:25698382

Zhang, Li; Luo, Xin; Niu, Zengyuan; Ye, Xiwen; Tang, Zhixu; Yao, Peng



Study on the photocatalytic degradation of methyl orange in water using Ag/ZnO as catalyst by liquid chromatography electrospray ionization ion-trap mass spectrometry.  


A nanocrystal catalyst Ag/ZnO was successfully synthesized using a simple solvothermal method in this study. This catalyst was characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results showed that this catalyst was composed of metallic Ag and ZnO. The photodegradation of methyl orange (MO) was investigated in aqueous suspension containing Ag/ZnO catalyst under UV irradiation. Liquid chromatography coupled with electrospray ionization ion-trap mass spectrometry was applied to the analysis of the samples coming from the photocatalytic degradation of MO. The experimental results showed that there were four intermediates existing in the photocatalytic reaction. MO could be mineralized in the Ag/ZnO suspension after 60 min illumination. PMID:18430584

Chen, Tianwen; Zheng, Yuanhui; Lin, Jin-Ming; Chen, Guonan



Analysis of sample of highly water-soluble Th-symmetric fullerenehexamalonic acid C66(COOH)12 by ion-chromatography and capillary electrophoresis.  


Ion chromatography (IC) was used to establish isomer purity of the highly water-soluble sample of fullerenehexamalonic acid, Th-symmetric hexakis-adduct C66(COOH)12. Sharp and symmetric peaks were obtained by IC using 1.0 M potassium hydroxide as eluent and applying gradient elution program. The identity of the two largest peaks in the chromatogram was assigned to Th-C66(COOH)12 and C66H(COOH)11. The developed IC procedure can be used for the semi-quantitative determination of the extent of the partial decarboxylation of the sample. As an alternative analytical technique, a CE procedure was introduced and its performance against IC was compared for this particular case. PMID:17888933

Cerar, Janez; Pompe, Matevz; Gucek, Marjan; Cerkovnik, Janez; Skerjanc, Joze



Direct chemical-analysis of uv laser-ablation products of organic polymers by using selective ion monitoring mode in gas-chromatography mass-spectrometry  

USGS Publications Warehouse

Trace quantities of laser ablated organic polymers were analyzed by using commercial capillary column gas chromatography/mass spectrometry; the instrument was modified so that the laser ablation products could be introduced into the capillary column directly and the constituents of each peak in the chromatogram were identified by using a mass spectrometer. The present study takes advantage of the selective ion monitoring mode for significantly improving the sensitivity of the mass spectrometer as a detector, which is critical in analyzing the trace quantities and confirming the presence or absence of the species of interest in laser ablated polymers. The initial composition of the laser ablated polymers was obtained by using an electron impact reflectron time-of-flight mass spectrometer and the possible structure of the fragments observed in the spectra was proposed based on the structure of the polymers.

Choi, Y.; Lee, H.W.; Fountain, S.T.; Lubman, D.M.



Determination of gamma-hydroxybutyric acid (GHB) in plasma and urine by headspace solid-phase microextraction and gas chromatography/positive ion chemical ionization mass spectrometry.  


A new method for the qualitative and quantitative analysis of gamma-hydroxybutyric acid (GHB) in plasma and urine samples is described. It involves the conversion of GHB to gamma-butyrolactone (GBL), its subsequent headspace solid-phase microextraction (SPME), and detection by gas chromatography/positive ion chemical ionization mass spectrometry (GC/PICI-MS), using D(6)-GBL as internal standard. The assay is linear over a plasma GHB range of 1-100 microg/mL (n = 5, r = 0.999) and a urine GHB range of 5-150 microg/mL (n = 5, r = 0. 998). Relative intra- and inter-assay standard deviations, determined for plasma and urine samples at 5 and 50 microg/mL, are all below 5%. The method is simple, specific and reasonably fast. It may be applied for clinical and forensic toxicology as well as for purposes of therapeutic drug monitoring. PMID:11114057

Frison, G; Tedeschi, L; Maietti, S; Ferrara, S D



Determination of testosterone in plasma from men by gas chromatography/mass spectrometry, with high-resolution selected-ion monitoring and metastable peak monitoring  

SciTech Connect

Highly specific methods are described for determining testosterone in plasma or serum from men. Extract fractions obtained by selective isolation procedures are converted to tert-butyldimethylsilyl (TBDMS) oximes/TBDMS ethers or methyl oximes/TBDMS ethers and analyzed by gas chromatography/mass spectrometry in the high-resolution selected-ion monitoring or metastable peak-monitoring modes. (2H3)Testosterone and unlabeled 17-epitestosterone are used as the respective internal standards. When we applied the two procedures to analysis of samples of pooled plasma and serum used for external quality assessment of routine assays, the results agreed well. Interlaboratory values for mean concentrations obtained by routine immunoassays (y) consistently exceeded values obtained by our technique (x), although the values closely correlated (r . 0.997; y . 1.008x + 0.564 nmol/L).

Finlay, E.M.; Gaskell, S.J.



Nano-fabricated size exclusion chromatograph  

NASA Technical Reports Server (NTRS)

This paper describes the development of a nano-fabricated size exclusion chromatograph (nSEC) based on the principle that molecules traveling through amicrocolumn containing nano-fabricated features will have characteristic elution times that directly correlate to molecular weight. Compared to conventional size exclusion chromatography, the nSEC offers greater control over the size exclusion process; mass fabrication; integration of the separation column with associated valves, pumps, and detectors; and dramatic reductions in instrument mass and power requirements.

Svehla, D.; Feldman, S.; Feldman, J.; Grunthaner, F.; Shakkottai, P.; Castillo, L. del; White, V.



Chromatography Theory  

NSDL National Science Digital Library

James Hardy has produced a number of presentation-style lecture modules for analytical chemistry. This is a very good module that covers the introductory theory of chromatography. The material includes information on chromatography along with plate and kinetic theories. It is a colorful and well planned presentation of the introduction to chromatography that could be used as the basis for lectures on chromatography at the introductory analytical chemistry or instrumental analysis level.


Affinity Chromatography  

NSDL National Science Digital Library

This is an experiment showing the application of affinity chromatography to the separation of albumin from horse serum. A brief introduction of affinity chromatography and how it is being used in this specific experiment is given. This appears to be a good experiment to show the advantages of affinity chromatography in separating specific proteins from a complex matrix and would be useful in a biochemistry course or a course that is specifically looking at differing types of chromatography.

DiResta, Dan


Neuere Chromatographie  

NASA Astrophysics Data System (ADS)

Besides high-performance liquid chromatography (HPLC) which is now a well-established and currently used technique, several emerging methods for the isolation and separation of natural products are receiving considerable attention. Centrifugal thin-layer chromatography is a very rapid technique, but limited in resolution. Of special interest are the recently developed support-free liquid-liquid chromatography methods such as droplet counter-current chromatography (DCCC) and rotation locular counter-current chromatography (RLCC). This latter method was applied to the separation of the enantiomers of (±)-norephedrine.

Hostettmann, K.



Structural modifications of dicationic acetylcholinesterase reactivators studied under ion-pairing mechanism in reversed-phase liquid chromatography.  


A study focused on the chromatographic behavior of several acetylcholinesterase reactivators under ion-pairing mechanism is reported. Among these reactivators, dicationic oximes and carbamoyl-based pyridinium congeners were studied, which form ion pairs with alkylsulfonate anions. This mechanism was studied for some major experimental parameters, such as the chain length of the ion-pairing agent added to the aqueous phase, its concentration, temperature, and nature of the organic modifier from mobile phase. Retention data showed one or two possibilities of forming ion pairs and the tautomerism of the studied reactivators, for different pH values of the aqueous component. Double sigmoid shapes were obtained for the studied compounds for the dependence between retention factor and pH, indicating the possibility of one or two tautomeric equilibria: at pH close to 7 these compounds are not stable as dicationic species and they participate in the retention process as nitroso forms, which are not able to form ion pairs with alkylsulfonates. The dependences of the retention factor on the organic modifier content from mobile phase were linear. Two complementary theoretical models were used to explain the functional dependences for the retention data on the experimental parameters. PMID:25141798

Radulescu, Medeea; Kuca, Kamil; Musilek, Kamil; David, Victor



Confirmation of avermectin residues in food matrices with negative-ion atmospheric pressure chemical ionization liquid chromatography/mass spectrometry.  


A multi-residue LC/MS method has been developed to confirm avermectin drug residues in several food matrices. Ivermectin (IVR), doramectin (DOR), eprinomectin (EPR) and moxidectin (MOX) are confirmed using atmospheric pressure chemical ionization (APCI) with negative ion detection and selected ion monitoring of three to four ions for each compound. The drug residues are extracted from tissue or milk using previously published procedures. IVR and DOR are confirmed at 20 ppb levels in fortified salmon muscle; IVR is also confirmed in tissue from salmon dosed with the drug. Residues of DOR, IVR, and EPR are confirmed in fortified milk at the 20 ppb level and in fortified beef liver at 40 ppb. Residues of MOX can also be confirmed in these matrices, but at slightly higher levels (40-80 ppb). PMID:10204245

Turnipseed, S B; Roybal, J E; Rupp, H S; Gonzales, S A; Pfenning, A P; Hurlbut, J A



Transfer RNA chromatography on reversed phase five: effect of cadmium ion on a queuine-type tRNA  

SciTech Connect

A sensitive method is described that detects an alteration in the structure of tRNA that is caused by cadmium but not by magnesium or zinc ions. The chromatographic system, RPC-5, separates Drosophila tyrosyl-tRNA into two fractions. These two isoacceptors differ by a single position in the anticodon where either a guanosine or queuine residues. Cadmium ions apparently interact with the tRNA and prevent the chromatographic separation. This is the first instance where cadmium is shown to cause a selective change in nucleic acid structure. The RPC-5 system seems to be uniquely useful in detecting such a change. 17 references, 2 figures.

Jacobson, K.B.; Lee, E.H.



Transfer RNA chromatography on reversed phase five: effect of cadmium ion on a queuine-type tRNA  

SciTech Connect

A sensitive method is described that detects an alteration in the structure of tRNA that is caused by cadmium but not by magnesium or zinc ions. The chromatographic system, RPC-5, separates Drosophila tyrosyl-tRNA into two fractions. These two isoacceptors differ by a single position in the anticodon where either a guanosine or queuine resides. Cadmium ions apparently interact with the tRNA and prevent the chromatographic separation. This is the first instance where cadmium is shown to cause a selective change in nucleic acid structure. The RPC-5 system seems to be uniquely useful in detecting such a change. 17 references, 2 figures.

Jacobson, K.B.; Lee, E.H.



The simultaneous determination of active ingredients in cough-cold mixtures by isocratic reversed-phase ion-pair high-performance liquid chromatography.  


A simple, rapid and accurate method for the simultaneous determination of active ingredients in cough-cold mixtures using isocratic reversed-phase ion-pair high-performance liquid chromatography has been developed. It involves the use of an octadecylsilane column as the stationary phase with methanol, water, tetrahydrofuran, phosphoric acid mixtures as mobile phase including sodium dioctylsulphosuccinate as the ion-pair agent. The pH of the mobile phase was adjusted to 4.6 by means of phosphoric acid and ammonium hydroxide solutions. The proposed method involves the simple dilution of the samples with the mobile phase and the addition of metoclopramide hydrochloride as the internal standard. The active ingredients under investigation were chlorpheniramine, codeine, diphenhydramine, ephedrine, ethylmorphine, phenylephrine, phenylpropanolamine and pholcodine, which exist as various combinations in cough-cold mixtures. The optimum composition of the mobile phase and the optimum flow rate were determined and are reported. The method was applied to the determination of active ingredients in seven commercially available cough-cold mixtures. PMID:2577452

Lau, O W; Chan, K; Lau, Y K; Wong, W C



Analysis of permethrin isomers in composite diet samples by molecularly imprinted solid-phase extraction and isotope dilution gas chromatography-ion trap mass spectrometry.  


Determination of an individual's aggregate dietary ingestion of pesticides entails analysis of a difficult sample matrix. Permethrin-specific molecularly imprinted polymer (MIP) solid-phase extraction cartridges were developed for use as a sample preparation technique for a composite food matrix. Vortexing with acetonitrile and centrifugation were found to provide optimal extraction of the permethrin isomers from the composite foods. The acetonitrile (with 1% acetic acid) was mostly evaporated and the analytes reconstituted in 90:10 water/acetonitrile in preparation for molecularly imprinted solid-phase extraction. Permethrin elution was accomplished with acetonitrile and sample extracts were analyzed by isotope dilution gas chromatography-ion trap mass spectrometry. Quantitation of product ions provided definitive identification of the pesticide isomers. The final method parameters were tested with fortified composite food samples of varying fat content (1%, 5%, and 10%) and recoveries ranged from 99.3% to 126%. Vegetable samples with incurred pesticide levels were also analyzed with the given method and recoveries were acceptable (81.0-95.7%). Method detection limits were demonstrated in the low ppb range. Finally, the applicability of the MIP stationary phase to extract other pyrethroids, specifically cyfluthrin and cypermethrin, was also investigated. PMID:19393156

Vonderheide, Anne P; Boyd, Brian; Ryberg, Anna; Yilmaz, Ecevit; Hieber, Thomas E; Kauffman, Peter E; Garris, Sherry T; Morgan, Jeffrey N



Ion pair-based dispersive liquid-liquid microextraction followed by high performance liquid chromatography as a new method for determining five folate derivatives in foodstuffs.  


A novel technique for simultaneous determination of five folate derivatives in various food matrices was developed by ion pair-based dispersive liquid-liquid microextraction (IP-DLLME) combined with high-performance liquid chromatography (HPLC). In the proposed method, N-methyl-N,N-dioctyloctan-1-ammonium chloride (aliquat-336) was used as an ion-pair reagent. Effective variables of microextraction process were optimized. Under optimum conditions, the method yielded a linear calibration curve ranging from 1-200ngg(-1) with correlation coefficients (r(2)) higher than 0.98. The relative standard deviation for the seven analyses was 5.2-7.4%. Enrichment factors for the five folates ranged between 108-135. Limits of detection were 2-4.1ngg(-1). A comparison of this method with other methods described that the new proposed method is rapid and accurate, and gives very good enrichment factors and detection limits for determining five folate derivatives. The newly developed method was successfully applied for the determination of five folate derivatives in wheat flour, egg yolk and orange juice samples. PMID:25770603

Nojavan, Yones; Kamankesh, Marzieh; Shahraz, Farzaneh; Hashemi, Maryam; Mohammadi, Abdorreza



Determination of trace levels of herbicides and their degradation products in surface and ground waters by gas chromatography/ion-trap mass spectrometry  

USGS Publications Warehouse

A rapid, specific and highly sensitive method is described for the determination of several commonly used herbicides and their degradation products in surface and ground waters by using gas chromatography/ion-trap mass spectrometry. The compounds included atrazine, and its degradation products desethylatrazine and desisopropylatrazine; Simazine; Cyanazine; Metolachlor; and alachlor and its degradation products, 2-chloro-2', 6'-diethylacetanilide, 2-hydroxy-2', 6'-diethylacetanilide and 2,6-diethylaniline. The method was applied to surface-water samples collected from 16 different stations along the lower Mississippi River and its major tributaries, and ground-water samples beneath a cornfield in central Nebraska. Average recovery of a surrogate herbicide, terbuthylazine, was greater than 99%. Recoveries of the compounds of interest from river water spiked at environmental levels are also presented. Full-scan mass spectra of these compounds were obtained on 1 ng or less of analyte. Data were collected in the full-scan acquisition mode. Quantitation was based on a single characteristic ion for each compound. The detection limit was 60 pg with a signal-to-noise ratio of greater than 10:1.

Pereira, W.E.; Rostad, C.E.; Leiker, T.J.



Dispersive solid phase extraction combined with ion-pair ultra high-performance liquid chromatography tandem mass spectrometry for quantification of nucleotides in Lactococcus lactis.  


Analysis of intracellular metabolites in bacteria is of utmost importance for systems biology and at the same time analytically challenging due to the large difference in concentrations, multiple negative charges, and high polarity of these compounds. To challenge this, a method based on dispersive solid phase extraction with charcoal and subsequent analysis with ion-pair liquid chromatography coupled with electrospray ionization tandem mass spectrometry was established for quantification of intracellular pools of the 28 most important nucleotides. The method can handle extracts where cells leak during the quenching. Using a Phenyl-Hexyl column and tributylamine as volatile ion-pair reagent, sufficient retention and separation was achieved for mono-, di-, and triphosphorylated nucleotides. Stable isotope labeled nucleotides were used as internal standards for some analytes. The method was validated by determination of the recovery, matrix effects, accuracy, linearity, and limit of detection based on spiking of medium blank as well as standard addition to quenched Lactococcus lactis samples. For standard addition experiments, the isotope-labeled standards needed to be added in similar or higher concentrations as the analytes. L. lactis samples had an energy charge of 0.97 ± 0.001 which was consistent with literature, whereas some differences were observed compared with legacy data based on ³³P labeling. PMID:23747533

Magdenoska, Olivera; Martinussen, Jan; Thykaer, Jette; Nielsen, Kristian Fog



Liquid phase microextraction-ion exchange-high performance thin layer chromatography for the preconcentration, separation, and determination of plasticizers in aqueous samples.  


Liquid phase microextraction combined with ion-exchange-high performance thin layer chromatography has been developed for analysis of four plasticizers in aqueous samples. After their preconcentration by liquid phase microextraction, fast separation on thin layers of inorganic ion-exchanger stannic silicate has been developed using a mixture of toluene + ethyl acetate (10:1, v/v) as mobile phase. Consequently, densitometric quantitative determination of the plasticizers has been made at ? = 280 nm in reflection-absorption mode by Camag TLC scanner-3. The effects of type and volume of extraction solvent, stirring rate, extraction time, and ionic strength in the microextraction method have been also evaluated and optimized. The results show that the proposed method provides enhanced accuracy, linear range, LOD, and LOQ, and is very effective for analyzing the target compounds in water samples. Under the optimized conditions, preconcentration factor of 149-279 and extraction efficiency of 31-59% have been obtained. Repeatability (5.67-7.26%) and intermediate precision (6.21-8.17%) were in acceptable range. The relative recovery obtained for each analyte in different water samples was higher than 82.3% at three fortification levels with RSD <7.9%. PMID:23526645

Faraji, Hakim; Mirzaie, Afshin; Waqif-Husain, Syed



Monitoring of phosphorus oxide ion for analytical speciation of phosphite and phosphate in transgenic plants by high-performance liquid chromatography-inductively coupled plasma mass spectrometry.  


Large amounts of phosphate fertilizers utilized in agriculture and their relatively poor efficiency are of high ecological and economic concern. Therefore, transgenic plants capable of metabolizing phosphite are being engineered. In support of this biotechnological task, analytical speciation of phosphorus in biological tissues is required. In this study, plant extracts were analyzed by liquid chromatography-inductively coupled plasma mass spectrometry at m/z of elemental phosphorus and phosphorus oxide ions. Using polymeric-based anion exchange column and millimolar concentration of nitric acid in potassium phthalate mobile phase (pH 2.5), phosphite and phosphate ions were baseline resolved with retention times 6.95 ± 0.03 and 7.90 ± 0.03 min and with a total chromatographic run time 10 min. The detection limits were 1.58 and 1.74 ?g P L(-1) at m/z 47, as compared to 2.18 and 2.04 ?g P L(-1) at m/z 31, respectively. The results obtained in real world samples for the two detection modes were in good agreement, yet signal acquisition at m/z 47 enabled better precision without collision/reaction cell (RSD below 2%) as compared to RSD around 4% obtained at m/z 31 using He-pressurized cell (3.5 mL min(-1)). PMID:23782169

Torres Elguera, Julio Cesar; Yañez Barrientos, Eunice; Wrobel, Katarzyna; Wrobel, Kazimierz



Solid-phase extraction and residue determination of glyphosate in apple by ion-pairing reverse-phase liquid chromatography with pre-column derivatization.  


A new method for glyphosate residue determination in apple has been developed. A SPE cartridge was used to clean up the samples before derivatization. Glyphosate was derivatized with 4-chloro-3,5-dinitrobenzotrifluoride (CNBF) and quantified by reverse ion-pair liquid chromatography using cetyltrimethylammonium bromide (CTAB) as ion-pair reagent. In pH 9.5 H(3)BO(3)-Na(2)B(4)O(7) medium, the reaction of glyphosate with CNBF was complete after 30 min at 60 degrees C. The stability of the derivative on exposure to light at room temperature in methanol-water was demonstrated. The labeled glyphosate was separated on a Kromasil C(18) column (250 x 4.6 mm, 5 microm) at room temperature and UV detection was applied at 360 nm. Separation was achieved within 15 min in gradient elution mode. The correlation coefficient for the method was 0.9998 at concentrations ranging from 0.1 to 50 microg/g. The calculated recoveries for glyphosate in apple were from 86.00 to 99.55%, and the relative standard deviations (n = 6) were from 1.43 to 6.32. The limit of detection was 0.01 microg/g for glyphosate in apple. PMID:19551741

Qian, Kun; Tang, Tao; Shi, Tianyu; Li, Pingliang; Li, Jianqiang; Cao, Yongsong



Quantiative determination of sulfonated aliphatic and aromatic surfactants in sewage sludge by ion-pair/supercritical fluid extraction and derivatization gas chromatography/mass spectrometry  

SciTech Connect

Secondary alkanesulfonate (SAS) and linear alkylbenzene-sulfonate (LAS) surfactants were quantitatively (> 90%) extracted from sewage sludges as their tetrabutylammonium ion pairs using 400 atm of supercritical CO[sub 2] for 5 min of static extraction followed by 10 min of dynamic extraction at 80[degrees]C. Ion pairs of SAS and LAS quantitatively formed butyl esters in the injection port of the gas chromatograph and were determined by gas chromatography/mass spectrometry without class fractionation of the sewage sludge extracts. Concentrations of SAS and LAS in sludges from five different sewage treatment plants ranged from 0.27 to 0.80 g/kg of dry sewage sludge and from 3.83 to 7.51 g/kg, respectively. Good reproducibility was achieved with RSDs of typically 5% for replicate extractions and analyses. Homologue and isomer distributions of SAS in sewage sludge indicated an enrichment of the more hydrophobic components in sewage sludge during sewage treatment. 25 refs., 5 figs., 5 tabs.

Field, J.A.; Field, T.M.; Giger, W. (Swiss Federal Inst. for Water Resources and Water Pollution Control, Duebendorf (Switzerland)); Miller, D.J.; Hawthorne, S.B. (Univ. of North Dakota, Grand Forks (United States))



An integrated analytical approach using ion chromatography, PIXE and electron microscopy to point out the differences in composition of PM10 individual particles  

NASA Astrophysics Data System (ADS)

This study presents a part of a project aiming at characterizing the PM10 composition in the Venice area with detailed chemical analyses using various techniques. The concentrations of six major inorganic ions (Cl-, NO3-, SO42-, Na+, NH4+, Mg2+) and 19 elements (Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Br, Pb) were quantified using ion chromatography and PIXE, respectively. The masses of PM10 daily samples and their chemical contents were studied in relationship to micro-meteorological parameters to select a few of them characterized by very different chemical profiles. Four samples from the whole period were categorized as representative of i) clean days; ii) sea spray generation events; iii) high contribution of mineral dust and iv) heavy pollution events. Individual particle analyses of the samples were also performed by SEM-EDS microscopy. Six different classes of particles were identified (mineral particles, chlorides, sulfates, elemental and organic carbon compounds, metals and biological particles) and an estimation of their abundance yielded a significant relationship between the chemical content and composition in individual particles of PM10. Further information was also obtained on PM10 source contributions, morphology, mineralogy and mixed state of particles demonstrating the importance of combining different analytical approaches.

Masiol, Mauro; Ceccato, Daniele; Squizzato, Stefania; Carturan, Sara; Pavoni, Bruno



[Determination of fosetyl-aluminium by ion-pair reversed phase-high performance liquid chromatography with evaporative light scattering detection].  


Ion-pair reversed phase-high performance liquid chromatography (RP-HPLC) with evaporative light scattering detection (ELSD) has been established for the analysis of fosetyl-aluminium and relevant impurities in technical or formulated substance. The method was achieved on a Symmetry Shield RP18 column by using n-butylamine as ion-pairing agent. The mobile phase was methanol-redistilled water containing 0.5% n-butylamine which was adjusted pH 5.0 with acetic acid (8:92, v/v) and the flow rate was set at 0.8 mL/min. The active ingredient fosetyl-aluminium was successfully separated from relevant impurities under the conditions. The calibration curve was linear in the range of 100-1200 mg/L. The average recoveries of two fortification levels (100 mg/L and 1000 mg/L) were 100.58% and 99.53%, and the relative standard deviations (RSDs) were 0.62% and 0.49%, respectively. The method is rapid, simple and accurate which provides another new and reliable means for the analysis of fosetyl-aluminium in its technical or formulated substance. PMID:20352944

Fan, Zhixian; Jia, Shumin; Ding, Ning; Zhao, Wenying; Wang, Shujuan



Thiophilic-interaction chromatography of enzymatically active tissue prostate-specific antigen T-PSA) and its modulation by zinc ions  

PubMed Central

Prostate-specific antigen (PSA) is a serine protease secreted both by normal prostate glandular epithelia cells and prostate cancer cells. We explored “thiophilic-interaction chromatography” (TIC) to isolate tissue prostate-specific antigen (T-PSA) from fresh human prostate cancer tissue harvested by radical prostatectomy for the purpose to characterize T-PSA for its enzymatic activity and sensitivity to zinc ions. We have shown, for the first time, that T-PSA has strong affinity for the thiophilic gel (T-gel). The average recovery of T-PSA from T-gel is over 87%. The presence of PSA in the column eluate was confirmed by ELISA and SDS/PAGE. Western blot developed with monoclonal antibody to PSA revealed that T-PSA was predominantly in the “free” form having a molecular weight of 33kDA. Furthermore, T-PSA was found to be enzymatically active. T-PSA was found to be less enzymatically active as compared to seminal plasma PSA. The inhibition of enzymatic activity of both f-PSA and T PSA over a wide range of concentrations of Zn2+ ions (10 nM to 50 ?M) was comparable. In contrast, the enzymatic activity of chymotrypsin, another serine-protease, was affected differently. At higher concentrations of Zn2+ (10 ?M and higher) the enzymatic activity of chymotrypsin was inhibited, whereas, at lower concentrations of Zn2+ (5 ?M and lower), the enzymatic activity was enhanced. PMID:18083072

Satheesh Babu, A. K.; Vijayalakshmi, M. A.; Smith, Gary J.; Chadha, Kailash C.



Quantitative Phosphoproteome Analysis of Lysophosphatidic Acid Induced Chemotaxis applying Dual-step ¹?O Labeling Coupled with Immobilized Metal-ion Affinity Chromatography  

SciTech Connect

Reversible protein phosphorylation is a central cellular regulatory mechanism in modulating protein activity and propagating signals within cellular pathways and networks. Development of more effective methods for the simultaneous identification of phosphorylation sites and quantification of temporal changes in protein phosphorylation could provide important insights into molecular signaling mechanisms in a variety of different cellular processes. Here we present an integrated quantitative phosphoproteomics approach and its applications for comparative analysis of Cos-7 cells in response to lysophosphatidic acid (LPA) gradient stimulation. The approach combines trypsin-catalyzed 16O/18O labeling plus 16O/18O-methanol esterification labeling for quantitation, a macro- Immobilized Metal-ion Affinity Chromatography trap for phosphopeptide enrichment, and a monolithic capillary column with integrated electrospray emitter. LC separation and MS/MS is followed by neutral loss-dependent MS/MS/MS for phosphopeptide identification using a linear ion trap (LTQ)-FT mass spectrometer and complementary searching algorithms for interpreting MS/MS spectra. Protein phosphorylation involved in various signaling pathways of cell migration were identified and quantified, such as mitogen-activated protein kinase 1, dual-specificity mitogen-activated protein kinase kinase 2, and dual-specificity tyrosine-phosphorylation regulated kinase 1b, and a number of Rho GTPase-activating proteins. These results demonstrate the efficiency of this quantitative phosphoproteomics approach and its application for rapid discovery of phosphorylation events associated with gradient sensing and cell chemotaxis.

Ding, Shi-Jian; Wang, Yingchun; Jacobs, Jon M.; Qian, Weijun; Yang, Feng; Tolmachev, Aleksey V.; Du, Xiuxia; Wang, Wei; Moore, Ronald J.; Monroe, Matthew E.; Purvine, Samuel O.; Waters, Katrina M.; Heibeck, Tyler H.; Adkins, Joshua N.; Camp, David G.; Klemke, Richard L.; Smith, Richard D.



The rapid and direct determination of ATP-ase activity by ion exchange chromatography and the application to the activity of heat shock protein-90  

PubMed Central

Adenosine nucleotides are involved as substrates or co-factors in several biochemical reactions, catalyzed by enzymes, which modulate energy production, signal transduction and cell proliferation. We here report the development and optimization of an ion exchange liquid chromatography (LC) method for the determination of ATP, ADP and AMP. This method is specifically aimed at the determination of the ATP-ase activity of human heat shock protein 90 (Hsp90), a molecular chaperone that has emerged as target enzyme in cancer therapy. Separation of the three nucleotides was achieved in a 15-min run by using a disk shaped monolithic ethylene diamine stationary phase of small dimensions (2×6 mm i.d.), under a three-solvent gradient elution mode and UV detection at 256 nm. The described direct LC method resulted highly specific as a consequence of the baseline separation of the three adenosine nucleotides and could be applied to the determination of the enzymatic activity of ADP/ATP generating or consuming enzymes (such as kinases). Furthermore, comparison of the LOD and LOQ values of the LC method with those obtained with the malachite green assay, which is one of the most used indirect screening methodologies for ATP-ase activity, showed that the LC method has a similar range of application without presenting the drawbacks related to contamination by inorganic phosphate ions and glycerol, which are present in Hsp90 commercial samples. PMID:22497853

Bartolini, Manuela; Wainer, Irving W.; Bertucci, Carlo; Andrisano, Vincenza



On-line pretreatment and determination of Pb, Cu and Cd at the microgram l-1 level in drinking water by chelation ion chromatography.  


A novel, highly sensitive method for the simultaneous separation and determination of lead, copper, cadmium and other transition metals in drinking water was achieved by on-line sample pretreatment of chelation ion chromatography. Manganese, which coeluted with cadmium, was oxidized to permanganate by ammonium persulfate before injection. Permanganate, with bulk quantity of alkali, alkaline earth metals, iron and aluminum, was eliminated by pyrophosphoric acid-ammonium acetate buffer solution (pH 5.5), while retaining heavy and transition metals on a selective chelating resin (MetPac CC-1 column). Then, they were disabsorbed and transferred to a sulfonated cation exchanger (TMC-1 column). Finally, the concentrated trace metals were separated on a bifunctional ion-exchange column (CS5A) by a concentration gradient of oxalic acid and sodium nitrate eluents, coupled with post-column spectrophotometric detection with 2-[(5-bromo-2-pyridyl)azo]-5-diethylaminophenol (5-Br-PADAP) at 560 nm. The separation and color-development conditions were optimized. The detection limits for the method (signal-to-noise ratio = 3:1) were at or below the microgram l-1 level. The results of drinking water analyses were satisfactory. PMID:9561765

Lu, H; Mou, S; Yan, Y; Tong, S; Riviello, J M



Separation of penicillin and its major degradation products by ion-pair reversed-phase high-pressure liquid chromatography.  


An ion-pair reversed-phase high-pressure liquid chromatographic technique capable of separating penicillin and its major degradation products within 8 min was developed. The influence of pH, counterion concentration, buffer concentration, and organic modifier content was studied and the observed behavior of the compounds during the chromatographic process was discussed. PMID:6279818

Ghebre-Sellassie, I; Hem, S L; Knevel, A M



Comprehensive Two-Dimensional Separation of Hydroxylated Polybrominated Diphenyl Ethers by Ultra-Performance Liquid Chromatography Coupled with Ion Mobility-Mass Spectrometry  

NASA Astrophysics Data System (ADS)

A comprehensive two-dimensional system coupling ultra-performance liquid chromatography (UPLC) and ion mobility-mass spectrometry (IM-MS) has been applied for the separation and analysis of hydroxylated polybrominated diphenyl ethers (OH-PBDEs). A complex mixture containing 23 OH-PBDE congeners ranging from hydroxylated monobromodiphenyl ether (OH-monoBDE) to hydroxylated octabromodiphenyl ether (OH-octaBDE) was satisfactorily separated within 16 min of analysis time. The first-dimensional reversed-phase UPLC was performed on a sub-2 ?m BEH C18 chromatographic column using acetonitrile-water gradient elution program with a flow rate ramp. It enabled excellent chromatographic separation for both between-class and within-class OH-PBDEs based on their differences in hydrophobicity. Following the pre-ionization resolution in the first dimension, the second-dimensional IM-MS employed a hybrid electrospray quadrupole ion mobility time-of-flight mass spectrometer and added an extra post-ionization separation for between-class OH-PBDE congeners on account of their relative mobility disparity during a very short period of 8.80 ms. The orthogonality of the developed two-dimensional system was evaluated with the correlation coefficient of 0.9665 and peak spreading angle of 14.87°. The peak capacity of the system was calculated to be approximately 2 and 15 times higher than that of the two dimensions used alone, respectively. The two-dimensional separation plane also contributed to the removal of background interference ions and the enhanced confidence in the characterization of OH-PBDEs of interest.

Ma, Qiang; Wang, Chao; Bai, Hua; Xi, Hai-Wei; Xi, Guang-Cheng; Ren, Xiao-Min; Yang, Yu; Guo, Liang-Hong



Qualitative Metabolome Analysis of Human Cerebrospinal Fluid by 13C-/12C-Isotope Dansylation Labeling Combined with Liquid Chromatography Fourier Transform Ion Cyclotron Resonance Mass Spectrometry  

NASA Astrophysics Data System (ADS)

Metabolome analysis of human cerebrospinal fluid (CSF) is challenging because of low abundance of metabolites present in a small volume of sample. We describe and apply a sensitive isotope labeling LC-MS technique for qualitative analysis of the CSF metabolome. After a CSF sample is divided into two aliquots, they are labeled by 13C-dansyl and 12C-dansyl chloride, respectively. The differentially labeled aliquots are then mixed and subjected to LC-MS using Fourier-transform ion cyclotron resonance mass spectrometry (FTICR MS). Dansylation offers significant improvement in the performance of chromatography separation and detection sensitivity. Moreover, peaks detected in the mass spectra can be readily analyzed for ion pair recognition and database search based on accurate mass and/or retention time information. It is shown that about 14,000 features can be detected in a 25-min LC-FTICR MS run of a dansyl-labeled CSF sample, from which about 500 metabolites can be profiled. Results from four CSF samples are compared to gauge the detectability of metabolites by this method. About 261 metabolites are commonly detected in replicate runs of four samples. In total, 1132 unique metabolite ion pairs are detected and 347 pairs (31%) matched with at least one metabolite in the Human Metabolome Database. We also report a dansylation library of 220 standard compounds and, using this library, about 85 metabolites can be positively identified. Among them, 21 metabolites have never been reported to be associated with CSF. These results illustrate that the dansylation LC-FTICR MS method can be used to analyze the CSF metabolome in a more comprehensive manner.

Guo, Kevin; Bamforth, Fiona; Li, Liang



Isolation of ?-linolenic acid biohydrogenation products by combined silver ion solid phase extraction and semi-preparative high performance liquid chromatography.  


Polyunsaturated fatty acids typically found in cattle feed include linoleic (LA) and ?-linolenic acid (ALA). In the rumen, microbes metabolize these resulting in the formation of biohydrogenation products (BHP), which can be incorporated into meat and milk. Bioactivities of LA-BHP, including conjugated linoleic acid (cis (c) 9,trans (t) 11-18:2 and t10,c12-18:2) and trans fatty acid isomers (t9-, t10- and t11-18:1) have been investigated, but effects of several BHP unique to ALA have not been extensively studied, and most ALA-BHP are not commercially available. The objective of the present research was to develop methods to purify and collect ALA-BHP using silver ion (Ag(+)) chromatography in sufficient quantities to allow for convenient bioactivity testing in cell culture. Fatty acid methyl esters (FAME) were prepared from perirenal adipose tissue from a cow enriched with ALA-BHP by feeding flaxseed. These were applied to Ag(+)-solid phase extraction, and eluted with hexane with increasing quantities of acetone (1, 2, 10, 20%) or acetonitrile (2%) to pre-fractionate FAME based on degree of unsaturation and double bond configuration. Fractions were collected, concentrated and applied to semi-preparative Ag(+)-high performance liquid chromatography (HPLC) for the isolation and collection of purified isomers, which was accomplished using isocratic elutions with hexane containing differing amounts of acetonitrile (from 0.015 to 0.075%). Purified trans-18:1 isomers collected ranged in purity from 88 to 99%. Purity of the ALA-BHP dienes collected, including c9,t13-18:2, t11,c15-18:2 and t10,c15-18:2, exceeded 90%, while purification of other dienes may require the use of other complementary procedures (e.g. reverse phase HPLC). PMID:25579113

Turner, T D; Meadus, W J; Mapiye, C; Vahmani, P; López-Campos, Ó; Duff, P; Rolland, D C; Church, J S; Dugan, M E R



Determination of the molecular weight of low-molecular-weight heparins by using high-pressure size exclusion chromatography on line with a triple detector array and conventional methods.  


The evaluation of weight average molecular weight (Mw) and molecular weight distribution represents one of the most controversial aspects concerning the characterization of low molecular weight heparins (LMWHs). As the most commonly used method for the measurement of such parameters is high performance size exclusion chromatography (HP-SEC), the soundness of results mainly depends on the appropriate calibration of the chromatographic columns used. With the aim of meeting the requirement of proper Mw standards for LMWHs, in the present work the determination of molecular weight parameters (Mw and Mn) by HP-SEC combined with a triple detector array (TDA) was performed. The HP-SEC/TDA technique permits the evaluation of polymeric samples by exploiting the combined and simultaneous action of three on-line detectors: light scattering detectors (LALLS/RALLS); refractometer and viscometer. Three commercial LMWH samples, enoxaparin, tinzaparin and dalteparin, a ?-ray depolymerized heparin (?-Hep) and its chromatographic fractions, and a synthetic pentasaccharide were analysed by HP-SEC/TDA. The same samples were analysed also with a conventional HP-SEC method employing refractive index (RI) and UV detectors and two different chromatographic column set, silica gel and polymeric gel columns. In both chromatographic systems, two different calibration curves were built up by using (i) ?-Hep chromatographic fractions and the corresponding Mw parameters obtained via HP-SEC/TDA; (ii) the whole ?-Hep preparation with broad Mw dispersion and the corresponding cumulative distribution function calculated via HP-SEC/TDA. In addition, also a chromatographic column calibration according to European Pharmacopoeia indication was built up. By comparing all the obtained results, some important differences among Mw and size distribution values of the three LMWHs were found with the five different calibration methods and with HP-SEC/TDA method. In particular, the detection of the lower molecular weight components turned out to be the most critical aspect. Whereas HP-SEC/TDA may underestimate species under 2 KDa when present in low concentration, other methods appeared to emphasize their content. PMID:25808152

Bisio, Antonella; Mantegazza, Alessandra; Vecchietti, Davide; Bensi, Donata; Coppa, Alessia; Torri, Giangiacomo; Bertini, Sabrina



Separation and direct detection of heavy lanthanides using new ion-exchange chromatography: fast Fourier transform continuous cyclic voltammetry system  

Microsoft Academic Search

In this study, possibilities of heavy lanthanides (Ho3+, Er3+, Tm3+, Yb3+, and Lu3+) separation on Nucleosil 100-5-SA, an ion-exchange column, was investigated. Separation of lanthanides was carried out using\\u000a an isocratic program of ?-hydroxyisobutyric acid (HIBA) eluent. Fast Fourier transform continuous cyclic voltammetry (FFT-CCV)\\u000a at a gold microelectrode was used as the detection method. Simplicity, high precision and accuracy, time

Mohammad Reza Pourjavid; Parviz Norouzi; Hamid Rashedi; Mohammad Reza Ganjali



Express analysis of explosives, chemical warfare agents and drugs with multicapillary column gas chromatography and ion mobility increment spectrometry  

Microsoft Academic Search

Description of a gas chromatograph designed for express analysis of explosives (2,4-dinitrotoluene, 2,4,6-trinitrotoluene, pentaerythritol tetranitrate), chemical warfare agents (mustard gas, lewisite, sarin) and drugs (heroin, cocaine hydrochloride, crack) is given. The devices comprises a multicapillary chromatographic column and an ion mobility increment spectrometer (MCC–IMIS). The main analytical characteristics of an IMIS (estimated detection limit (DL), linear dynamic range (LDR), speed

Igor A. Buryakov



Isolation of Pu-isotopes from environmental samples using ion chromatography for accelerator mass spectrometry and alpha spectrometry.  


A radiochemical method for the isolation of plutonium-isotopes from environmental samples, based on the use of specific extraction chromatography resins for actinides (TEVA), Eichrom Industries, Inc.), has been set up in our laboratory and optimised for their posterior determination by alpha spectrometry (AS) or accelerator mass spectrometry (AMS). The proposed radiochemical method has replaced in our lab a well-established one based on the use of a relatively un-specific anion-exchange resin (AG) 1X8, Bio-rad Laboratories, Inc.), because it is clearly less time consuming, reduces the amounts and molarities of acid wastes produced, and reproducibly gives high radiochemical yields. In order to check the reliability of the proposed radiochemical method for the determination of plutonium-isotopes in different environmental matrixes, twin aliquots of a set of samples were prepared with TEVA and with AG 1X8 resins and measured by AS. Some samples prepared with TEVA resins were measured as well by AMS. As it is shown in the text, there is a comfortable agreement between AS and AMS, which adequately validates the method. PMID:18082656

Chamizo, E; Jiménez-Ramos, M C; Wacker, L; Vioque, I; Calleja, A; García-León, M; García-Tenorio, R



Micellar liquid chromatography  

NASA Astrophysics Data System (ADS)

Background and possibilities of practical applications of micellar liquid chromatography (MLC) are considered. Various retention models in MLC, the effects of the nature and concentration of surfactants and organic modifiers, pH, temperature and ionic strength on the MLC efficiency and selectivity are discussed. The advantages and limitations of MLC are demonstrated. The performance of MLC is critically evaluated in relationship to the reversed-phase HPLC and ion-pair chromatography. The potential of application of MLC for the analysis of pharmaceuticals including that in biological fluids and separation of inorganic anions, transition metal cations, metal chelates and heteropoly compounds is described. The bibliography includes 146 references.

Basova, Elena M.; Ivanov, Vadim M.; Shpigun, Oleg A.



Analysis of perfluorinated compounds in biota by microextraction with tetrahydrofuran and liquid chromatography/ion isolation-based ion-trap mass spectrometry.  


An analytical method combining both a simple, fast and efficient solvent microextraction and a sensitive and selective monitoring mode, based on ion isolation ion-trap mass spectrometry (MS), was developed for analysis of perfluorinated compounds (PFCs) in biota. The method involved the vortex-shaking of 0.2g of tissue sample and 800microL of tetrahydrofuran (THF):water (75:25, v/v) for 7min, subsequent centrifugation for 13min and direct quantitation of PFCs in the extract against solvent-based calibration curves. Selection of solvent composition was based on Hildebrand solubility parameters and their components (i.e. dispersion, dipole-dipole and hydrogen bonding forces). Recoveries in samples for PFCs with hydrocarbon chain lengths between C(4) and C(14) ranged from 85 to 111%, with relative standard deviations between 1 and 11%. The ion isolation monitoring mode, proposed for the first time for ion-trap-MS quantitation, proved to be effective in avoiding space-charge effects caused