Journal of Chromatography A (J Chrom)

Publisher: Elsevier

Journal description

The Journal of Chromatography A publishes papers on all aspects of separation science including chromatography, electrochromatography, electrophoresis, hyphenated and other multi-dimensional techniques, sample preparation as well as detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with chromatographic and electrophoretic theory, instrumental developments and their analytical and preparative applications. Section A covers all areas except biomedical sciences and biomedical applications of separation science, which are published in section B: Biomedical Sciences and Applications. Electronic version.

Current impact factor: 4.26

Impact Factor Rankings

2015 Impact Factor Available summer 2015
2013 / 2014 Impact Factor 4.258
2012 Impact Factor 4.612
2011 Impact Factor 4.531
2010 Impact Factor 4.194
2009 Impact Factor 4.101
2008 Impact Factor 3.756
2007 Impact Factor 3.641
2006 Impact Factor 3.554
2005 Impact Factor 3.096
2004 Impact Factor 3.359
2003 Impact Factor 2.922
2002 Impact Factor 3.098
2001 Impact Factor 2.793
2000 Impact Factor 2.551
1999 Impact Factor 2.52
1998 Impact Factor 2.321
1997 Impact Factor 2.697
1996 Impact Factor 2.457
1995 Impact Factor 2.296
1994 Impact Factor 2.523

Impact factor over time

Impact factor
Year

Additional details

5-year impact 0.00
Cited half-life 7.10
Immediacy index 0.65
Eigenfactor 0.11
Article influence 0.81
Website Journal of Chromatography A website
ISSN 1873-3778

Publisher details

Elsevier

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    • Deposit due to Funding Body, Institutional and Governmental policy or mandate only allowed where separate agreement between repository and the publisher exists.
    • Permitted deposit due to Funding Body, Institutional and Governmental policy or mandate, may be required to comply with embargo periods of 12 months to 48 months .
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    • Publisher's version/PDF cannot be used
    • Articles in some journals can be made Open Access on payment of additional charge
    • NIH Authors articles will be submitted to PubMed Central after 12 months
    • Publisher last contacted on 18/10/2013
  • Classification
    ​ green

Publications in this journal

  • [Show abstract] [Hide abstract]
    ABSTRACT: Analytical scale supercritical fluid chromatography (SFC) is largely a sub-discipline of high performance liquid chromatography (HPLC), in that most of the hardware and software can be used for either technique. The aspects that separate the 2 techniques stem from the use of carbon dioxide (CO2) as the main component of the mobile phase in SFC. The high compressibility and low viscosity of CO2 mean that pumps, and autosamplers designed for HPLC either need to be modified or an alternate means of dealing with compressibility needs to be found. The inclusion of a back pressure regulator and a high pressure flow cell for any UV-Vis detector are also necessary. Details of the various approaches, problems and solutions are described. Characteristics, such as adiabatic vs. isothermal compressibility, thermal gradients, and refractive index issues are dealt with in detail. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.062
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    ABSTRACT: An efficient and target-oriented sample enrichment method was established to increase the content of the minor alkaloids in crude extract by using the corresponding two-phase solvent system applied in pH-zone-refining counter-current chromatography. The enrichment and separation of seven minor indole alkaloids from Uncaria rhynchophylla (Miq.) Miq. ex Havil(UR) were selected as an example to show the advantage of this method. An optimized two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (3:7:1:9, v/v) was used in this study, where triethylamine (TEA) as the retainer and hydrochloric acid (HCl) as the eluter were added at the equimolar of 10mM. Crude alkaloids of UR dissolved in the corresponding upper phase (containing 10mM TEA) were extracted twice with lower phase (containing 10mM TEA) and lower phase (containing 10mM HCl), respectively, the second lower phase extract was subjected to pH-zone-refining CCC separation after alkalization and desalination. Finally, from 10g of crude alkaloids, 4g of refined alkaloids was obtained and the total content of seven target indole alkaloids was increased from 4.64% to 15.78%. Seven indole alkaloids, including 54mg isocorynoxeine, 21mg corynoxeine, 46mg isorhynchophylline, 35mg rhynchophylline, 65mg hirsutine, 51mg hirsuteine and 27mg geissoschizine methylether were all simultaneously separated from 2.5g of refined alkaloids, with the purity of 86.4%, 97.5%, 90.3%, 92.1%, 98.5%, 92.3%, and 92.8%, respectively. The total content and purities of the seven minor indole alkaloids were tested by HPLC and their chemical structures were elucidated by ESI-HRMS and (1)H NMR. Copyright © 2015. Published by Elsevier B.V.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.066
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    ABSTRACT: Nanomaterials are of great interest for the development of electrochemical sensors. Multi-walled carbon nanotubes and graphene were used to modify the working electrode surface of different screen-printed carbon electrodes (SPCE) with the aim of improving the sensitivity of the SPCE and comparing it with the conventional glassy carbon electrode. To assay the usability of these sensors, a HPLC methodology with amperometric detection was developed to analyze several phytochelatins in plants of Hordeum vulgare and Glycine max treated with Hg(II) or Cd(II) giving detection limits in the low μmolL(-1) range. Phytochelatins are low molecular weight peptides with the general structure γ-(Glu-Cys)n-Gly (n=2-5) which are synthesized in plants in the presence of heavy metal ions. These compounds can chelate heavy metal ions by the formation of complexes which, are transported to the vacuoles, where the toxicity is not threatening. For this reason phytochelatins are essential in the detoxification of heavy metal ions in plants. The developed HPLC method uses a mobile phase of 1% of formic acid in water with KNO3 or NaCl (pH=2.00) and 1% of formic acid in acetonitrile. Electrochemical detection at different carbon-based electrodes was used. Among the sensors tested, the conventional glassy carbon electrode offers the best sensitivity although modification improves the sensitivity of the SPCE. Glutathione and several isoforms of phytochelatin two were found in plant extracts of both studied species. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.057
  • Nikola Vaňková, Jelle De Vos, Eva Tyteca, Gert Desmet, Tony Edge, Lenka Česlová, Petr Česla, Sebastiaan Eeltink
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    ABSTRACT: The effect of gradient steepness on the kinetic performance limits and peak compression effects has been assessed in gradient mode for the separation of phenol derivatives using columns packed with 2.6μm core-shell particles. The effect of mobile-phase velocity on peak capacity was measured on a column with fixed length while maintaining the retention factor at the moment of elution and the peak-compression factor constant. Next, the performance limits were determined at the maximum system pressure of 100MPa while varying the gradient steepness. For the separation of small molecules applying a linear gradient with a broad span, the best performance limits in terms of peak capacity and analysis time were obtained applying a gradient-time-to-column-dead-time (tG/t0) ratio of 12. The magnitude of the peak-compression factor was assessed by comparing the isocratic performance with that in gradient mode applying different gradient times. Therefore, the retention factors for different analytes were determined in gradient mode and the mobile-phase composition in isocratic mode was tuned such that the difference in retention factor was smaller than 2%. Peak-compression factors were quantitatively determined between 0.95 and 0.65 depending on gradient steepness and the gradient retention factor. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.061
  • Nándor Lambert, Attila Felinger
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    ABSTRACT: We have studied the chromatographic behavior of the homologous series of alkylbenzenes (ranging from octylbenzene to octadecylbenzene) on the same C18 reversed-phase column in supercritical fluid chromatography (SFC) and reversed phase liquid chromatography (RPLC) at various experimental conditions, such as different eluent compositions, flow-rates, and mobile phase densities. The first and the second moments of the peaks were used to estimate the overall mass-transfer processes in both chromatographic modes using the stochastic model of chromatography. The results confirm that in SFC - as the density of the mobile phase is influenced by the flow-rate - there is a broader variation of mass-transfer properties than in liquid chromatography. As expected, the optimum mobile phase velocity is higher in SFC, but there is no real difference in the minimum value of plate height, i.e. in the optimum efficiency. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.056
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    ABSTRACT: The main goal of this work was to optimize the SPME sampling method for measuring microbial volatile organic compounds (MVOCs) emitted by active molds that may deteriorate historical objects. A series of artificially aged model materials that resemble those found in historical objects was prepared and evaluated after exposure to four different types of fungi. The investigated pairs consisted of: Alternaria alternata on silk, Aspergillus niger on parchment, Chaetomium globosum on paper and wool, and Cladosporium herbarum on paper. First of all, a selection of the most efficient SPME fibers was carried out as there are six different types of fibers commercially available. It was important to find a fiber that absorbs the biggest number and the highest amount of MVOCs. The results allowed establishing and selecting the DVB/CAR/PDMS fiber as the most effective SPME fiber for this kind of an analysis. Another task was to optimize the time of MVOCs extraction on the fiber. It was recognized that a time between 12 and 24h is adequate for absorbing a high enough amount of MVOCs. In the last step the temperature of MVOCs desorption in the GC injection port was optimized. It was found that desorption at a temperature of 250°C allowed obtaining chromatograms with the highest abundances of compounds. To the best of our knowledge this work constitutes the first attempt of the SPME method optimization for sampling MVOCs emitted by molds growing on historical objects. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.059
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    ABSTRACT: Pentacyclic triterpenes are gaining interest due to their beneficial health effects, as anti-inflammatory, anti-diabetic and anti-tumoral, among others. In this study, an analytical LC-MS method was developed for the simultaneous determination of maslinic, oleanolic and ursolic acids along with erythrodiol and uvaol, which are the main triterpenic compounds present in the fruits and leaves of Olea europaea L. A Zorbax Eclipse PAH column at 30°C with mobile phase of water (17%) and methanol (83%) at 0.8mL/min conformed the optimal chromatographic conditions that allowed the separation of the compounds of interest, two pairs of which are isomers differing only in the position of one methyl group (oleanolic-ursolic and erythrodiol-uvaol). The ionization was performed in an APCI source at 450°C programmed in negative mode for the triterpenic acids, and in positive for the alcohols. An ion trap (LC-IT-MS) and a triple quadrupole (LC-QqQ-MS) were assessed for maximal sensitivity that was achieved with LC-QqQ-MS. The LODs of triterpenic acids were lower than 1nM, whereas for erythrodiol and uvaol were 4.5 and 7.5nM, respectively. The method was linear for the five analytes in the range of concentrations from 0.005 to 15μM with correlation coefficients exceeding 0.99. The precision and accuracy were ≤9.90% and ≤9.57%, respectively. The applicability of the validated method was assessed in the analysis of the pentacyclic triterpenes in Marfil table olives, after the optimization of the extraction procedure. The developed method constitutes the first step for future studies of triterpenic compounds present in foods that would allow establishing their effects on human health. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.064
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    ABSTRACT: Carbohydrates in herbs are a relatively untapped source of new drugs and health beneficial ingredients. Their analysis has been developed as a novel aspect in quality control and herbal glycomics. In this study, glycome of Astragalus membranaceus was decoded based on optimized pressurized liquid extraction (PLE), microwave-assisted acidic hydrolysis (MAAH) and comprehensive chromatographic approaches. Twelve saccharides including sucrose, galacturonic acid, mannitol, fructose, rhamnose, ribose, arabinose, fucose, xylose, mannose, glucose and galactose were quantitatively analyzed by GC-MS and HPLC-CAD (charged aerosol detectors). Different columns, including Prevail Carbohydrate ES, XBridge Amide and CARBOSep CHO-820 CA for HPLC-CAD analysis, were compared for evaluation of oligosaccharides. The polysaccharides in water extract of Astragalus membranaceus were characterized by high performance size exclusive chromatography (HPSEC) combined with multiple angle light scattering detection (MALSD) and refractive index detection (RID). The results showed that A. membranaceus contained more than 108.5mgg(-1) free sucrose and small amounts of glucose 9.6-26.0mgg(-1) and fructose 8.7-22.9mgg(-1). While its polymeric carbohydrates were composed of glucose 71.0-162.3mgg(-1), galacturonic acid 52.0-113.4mgg(-1), arabinose 22.8-54.4mgg(-1) and small amounts of galactose, rhamnose, xylose and mannose. CARBOSep CHO-820 CA showed its potential in simultaneously analyzing oligosaccharides and uronic acid, especially only the environment-friendly water mobile phase was used. HPSEC-MALSD-RID showed that there were three different molecular weight distributions of polysaccharides in A. membranaceus and the average molecular weight were 21901.1, 2038.5, and 353.4kDa. Hierarchical clustering analysis and principal component analysis demonstrated that A. membranaceus from different regions showed variations both in free and polymeric carbohydrates, which indicated that carbohydrates should be evaluated for the proper quality control of A. membranaceus. Rha, Ara, Xyl, Man and Gal were found to be the main elements for quality evaluation of polymeric carbohydrates in A. membranaceus by factor analysis. The strategy for decoding the glycome based on chromatographic approaches including GC-MS, HPLC-CAD and HPSEC-MALSD-RID after pressurized liquid extraction and microwave-assisted hydrolysis could be applied for carbohydrates profiling in herbs and beneficial for their quality control. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.058
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    ABSTRACT: Given the importance of short and medium chain free fatty acids (FFAs) in several fields, this study sought to improve the extraction efficiency of the solid-phase microextraction (SPME) of FFAs by evaluating salting out agents that appear promising for this application. The salts ammonium sulfate ((NH4)2SO4) and sodium dihydrogen phosphate (NaH2PO4) were tried on their own and in combination (3.7/1), in four different total amounts, as salting out agents in the headspace-SPME-gas chromatographic (HS-SPME-GC) analysis of the FFAs from acetic acid (C2) to decanoic acid (C10). Their performance in a model system of an aqueous standard mixture of FFAs at a pH of 3.5 was compared to that of the more commonly used sodium chloride (NaCl) and sodium sulfate (Na2SO4). All of the salts and salt systems evaluated, in proper amount, gave improved results compared to NaCl (saturated), which instead gave interesting results only for the least volatile FFAs C8 and C10. For C2-C6, the salt system that gave the best results compared to NaCl was (NH4)2SO4/NaH2PO4, in the highest of the four amounts evaluated, with factor increases between 1.2 and 4.1-fold, and NaH2PO4, between 1.0 and 4.3-fold. The SPME extraction efficiency given by the mixture (NH4)2SO4/NaH2PO4 was also assessed on biological and food samples, confirming that overall it performed better than NaCl. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.051
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    ABSTRACT: This study combines solid phase extraction (SPE) using 96-well plates with column-switching technology to construct a rapid and high-throughput method for the simultaneous extraction and non-targeted analysis of small molecules metabolome and lipidome based on ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry. This study first investigated the columns and analytical conditions for small molecules metabolome and lipidome, separated by an HSS T3 and BEH C18 columns, respectively. Next, the loading capacity and actuation duration of SPE were further optimized. Subsequently, SPE and column switching were used together to rapidly and comprehensively analyze the biological samples. The experimental results showed that the new analytical procedure had good precision and maintained sample stability (RSD<15%). The method was then satisfactorily applied to more widely analyze the small molecules metabolome and lipidome to test the throughput. The resulting method represents a new analytical approach for biological samples, and a highly useful tool for researches in metabolomics and lipidomics. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.048
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    ABSTRACT: Volatile compounds are responsible for most of the sensory qualities of virgin olive oil and they are synthesized when enzymes and substrates come together as olive fruit is crushed during the industrial process to obtain the oil. Here we have studied the variability among the major volatile compounds in virgin olive oil prepared from the progeny of a cross of Picual and Arbequina olive cultivars (Olea europaea L.). The volatile compounds were isolated by SPME, and analyzed by HRGC-MS and HRGC-FID. Most of the volatile compounds found in the progeny's oil are produced by the enzymes in the so-called lipoxygenase pathway, and they may be clustered into different groups according to their chain length and polyunsaturated fatty acid origin (linoleic and linolenic acids). In addition, a group of compounds derived from amino acid metabolism and two terpenes also contributed significantly to the volatile fraction, some of which had significant odor values in most of the genotypes evaluated. The volatile compound content of the progeny was very varied, widely transgressing the progenitor levels, suggesting that in breeding programs it might be more effective to consider a larger number of individuals within the same cross than using different crosses with fewer individuals. Multivariate analysis allowed genotypes with particularly interesting volatile compositions to be identified and their flavor quality deduced. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.055
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    ABSTRACT: We demonstrate improved power of Iatroscan thin layer chromatography/flame ionization detection (TLC-FID) technique for analysis of complex marine lipid mixture by developing protocol for the separation and analysis of glycolipids including sulfoquinovosyldiacylglycerols (SQDG), monogalactosyldiacylglycerols (MGDG) and digalactosyldiacylglycerols (DGDG). We have modified the common protocol used so far for the analysis of lipid classes by replacing the elution step which uses pure acetone for the elution of acetone mobile polar lipids, with the elution step containing chloroform-acetone (72:28, v:v) for separation of MGDG and DGDG. To separate SQDG from the complex lipid matrix we introduced solvent mixture acetone-chloroform-methanol-formic acid (33:33:33:0.6, v:v:v:v). Quantification of glycolipid classes was performed after calibration with glycolipid standards for the masses between 0.2 and 2.7-5.0μg. With this new protocol we have successfully separated three glycolipids from the complex particulate lipid mixture of the seawater samples. Such an approach extends the power of existing protocol for the analysis of lipids which altogether ensure detection and quantification of 18 lipid classes what was demonstrated on seawater samples. This enables to gain a very broad system overview of the particularly complex environments as are seas, oceans and freshwaters. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.047
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    ABSTRACT: A newly designed molecularly imprinted polymer (MIP) material was developed and successfully used as recognition element for enantioselective recognition by microchip electrophoresis. In this work, molecularly imprinted polymers were facilely prepared employing Fe3O4 nanoparticles (NPs) as the supporting substrate and norepinephrine as the functional monomer in the presence of template molecule in a weak alkaline solution. After extracting the embedded template molecules, the produced imprinted Fe3O4@polynorepinephrine (MIP-Fe3O4@PNE) NPs have cavities complementary to three dimensional shape of template molecules favoring high binding capacity and magnetism property for easy manipulation. The MIP-Fe3O4@PNE NPs prepared with l-tryptophan, l-valine, l-threonine, Gly-l-Phe, S-(-)-ofloxacin or S-(-)-binaphthol as template molecules were packed in the polydimethylsiloxane microchannel via magnetic field as novel stationary phase to successful enantioseparation of corresponding target analysts. The MIP-Fe3O4@PNE NPs-based microchip electrophoresis system exhibited strong recognition ability, excellent high-performance, admirable reproducibility and stability, which provided a powerful protocol for separation enantiomers within a short analytical time and opened up an avenue for multiplex chiral compound assay in various systems. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.052
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    ABSTRACT: In the present work, the phlorotannin composition of different Sargassum muticum samples collected at different locations along the North Atlantic coasts as well as the bioactivities related to these components were investigated. After pressurized liquid extraction, the samples collected at the extreme locations of a latitudinal gradient from Portugal and Norway, were found to be the richest on total phenols and, particularly, on phlorotannins, containing up to 148.97 and 5.12mg phloroglucinol equivalents g(-1), respectively. The extracts obtained from these locations were further purified and chemically characterized using a modified HILIC×RP-DAD-MS/MS method. The application of this methodology allowed the tentative identification of a great variability of phlorotannins with different degrees of polymerization (from 3 to 11) and structures, determined for the first time in S. muticum. The most-abundant phlorotannins on these samples were fuhalols, hydroxyfuhalols and phlorethols, showing also particularities and important differences depending on the geographical location. Afterwards, the antiproliferative activity of these extracts against HT-29 adenocarcinoma colon cancer cells was studied. Results revealed that the richest S. muticum samples in terms of total phlorotannins, i.e., those from Norway, presented the highest activity, showing a good cytotoxic potential at concentrations in the medium micromolar range. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.053
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    ABSTRACT: Preservation of ionic species within Antarctic ice yields a unique proxy record of the Earth's climate history. Studies have been focused until now on two proxies: the ionic components of sea salt aerosol and methanesulfonic acid. Measurement of the all of the major ionic species in ice core samples is typically carried out by ion chromatography. Former methods, whilst providing suitable detection limits, have been based upon off-column preconcentration techniques, requiring larger sample volumes, with potential for sample contamination and/or carryover. Here, a new capillary ion chromatography based analytical method has been developed for quantitative analysis of limited volume Antarctic ice core samples. The developed analytical protocol applies capillary ion chromatography (with suppressed conductivity detection) and direct on-column sample injection and focusing, thus eliminating the requirement for off-column sample preconcentration. This limits the total sample volume needed to 300μL per analysis, allowing for triplicate sample analysis with <1mL of sample. This new approach provides a reliable and robust analytical method for the simultaneous determination of organic and inorganic anions, including fluoride, methanesulfonate, chloride, sulfate and nitrate anions. Application to composite ice-core samples is demonstrated, with coupling of the capillary ion chromatograph to high resolution mass spectrometry used to confirm the presence and purity of the observed methanesulfonate peak. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.034
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    ABSTRACT: Concentration of blood catecholamines (CAs) is linked to a host of cardiovascular diseases, including hypertension and stenocardia. The matrix interferences and low concentration require tedious sample pretreatment methods before quantitative analysis by the gold standard method of high-performance liquid chromatography-electrochemical detector (HPLC-ECD). Solid phase extraction (SPE) has been widely used as the pretreatment technique. Here, a facile polymeric ionic liquid (PIL)-diphenylboric acid (DPBA)-packed capillary column was prepared to selectively extract dopamine (DA), noradrenaline (NE) and epinephrine (E) prior to their quantitative analysis by a fast separation in HPLC-ECD method, while microdialysis sampling method was applied to get the analysis sample. Parameters that influenced desorption efficiency, such as pH, salt concentration, acetonitrile content and wash time, were examined and optimized. The proposed method, combining microdialysis sampling technique, SPE and HPLC-ECD system, was successfully applied to detect CAs in rat blood microdialysate with high sensitivity and selectivity in small sample volumes (5-40μl) and a short analysis time (8min), yielding good reproducibility (RSD 6.5-7.7%) and spiked recovery (91-104.4%). Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.040
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    ABSTRACT: On-column focusing or preconcentration is a well-known approach to increase concentration sensitivity by generating transient conditions during the injection that result in high solute retention. Preconcentration results from two phenomena: (1) solutes are retained as they enter the column. Their velocities are k'-dependent and lower than the mobile phase velocity and (2) zones are compressed due to the step-gradient resulting from the higher elution strength mobile phase passing through the solute zones. Several workers have derived the result that the ratio of the eluted zone width (in time) to the injected time width is the ratio k2/k1, where k1 is the retention factor of a solute in the sample solvent and k2 is the retention factor in the mobile phase (isocratic). Mills et al. proposed a different factor. To date, neither of the models has been adequately tested. The goal of this work was to evaluate quantitatively these two models. We used n-alkyl esters of p-hydroxybenzoic acid (parabens) as solutes. By making large injections to create obvious volume overload, we could measure accurately the ratio of widths (eluted/injected) over a range of values of k1 and k2. The Mills et al. model does not fit the data. The data are in general agreement with the factor k2/k1, but focusing is about 10% better than the prediction. We attribute the extra focusing to the fact that the second, compression, phenomenon provides a narrower zone than that expected for the passage of a step gradient through the zone. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.038
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    ABSTRACT: A novel dispersive micro-solid-phase extraction (DMSPE) method using ultramicro chitosan as an adsorbent was proposed for the analysis of flavonols in Flos Sophorae tea, with detection by ultra-high performance liquid chromatography. Various parameters affecting the extraction recovery, including the concentration and viscosity of chitosan, extraction time and the pH of the sample solution were investigated and optimized. The optimized conditions were found to be 0.4μg/mL of sorbent, pH of 7, an extraction time of 1.0min and 100μL of methanol as the elution solvent. The DMSPE method showed excellent linearity (r(2)>0.99) with pre-concentration factor values ranging from 23 to 77-fold. The limits of detection and quantification were 0.22-0.36ng/mL and 0.72-1.21ng/mL, respectively. This method was successfully applied to the analysis of flavonols in Flos Sophorae tea samples, and their recoveries were in the range of 95.2-102.4%. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 07/2015; DOI:10.1016/j.chroma.2015.07.041