Journal of Chromatography A (J Chrom )

Publisher: Elsevier


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.

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    • Publisher last contacted on 18/10/2013
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Publications in this journal

  • [Show abstract] [Hide abstract]
    ABSTRACT: Evaluation of a several fluorine-containing stationary phases for the chromatographic separation of fluorine-containing pharmaceuticals from their corresponding desfluoro analogs revealed a number of perfluoroaryl and perfluoroalky stationary phases that afford good separations. These fluorous stationary phases exhibit greater retention for the fluorine-containing compounds relative to the H-containing analogs, consistent with a fluorophilic retention mechanism. While both perfluoroalkyl and perfluoroaryl stationary phases afford adequate resolution, the perfluoroaryl columns generally exhibit superior separation factor (α) and peak efficiency (N), resulting in faster baseline separations, with the Hypersil Gold PFP and Poroshell 120 PFP columns providing the best overall performance for the test group studied. Copyright © 2014 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 01/2015; 1380:45-54.
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    ABSTRACT: In the present study, 12-tungstophosphoric (PW) acid as heteropoly acid, supported on silica-coated γ-Fe2O3 nanoparticles (NPs) was used as a new fiber coating for solid-phase microextraction (SPME). The γ-Fe2O3@SiO2-PW nanocomposite with high surface area was synthesized and characterized by SEM, FT-IR. The prepared nanocomposite was immobilized on a stainless steel wire for fabrication of the SPME fiber. The fiber was evaluated for the extraction of some phenolic compounds (PCs) from the water sample in combination with gas chromatography-mass spectrometry (GC-MS). A one-at-the-time optimization strategy was applied for optimizing the important extraction parameters such as extraction temperature, extraction time, ionic strength, stirring rate, pH, and desorption temperature and time. In optimum conditions, the repeatability for one fiber (n = 3), expressed as relative standard deviation (R.S.D. %), was between 4.8% and 9.6% for the test compounds. The detection limits for the studied compounds were between 0.004–0.05 pg mL−1. The developed method offers the advantage of being simple to use, with shorter analysis time, lower cost of equipment, thermal stability of fiber and high relative recovery in comparison to conventional methods of analysis.
    Journal of Chromatography A 01/2015;
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    ABSTRACT: The present study investigated the practical use of modern ultra-high performance liquid chromatography (UHPLC) separation techniques for drug metabolite profiling, aiming to develop a widely applicable, high-throughput, easy-to-use chromatographic method, with a high chromatographic resolution to accommodate simultaneous qualitative and quantitative analysis of small-molecule drugs and metabolites in biological matrices. To this end, first the UHPLC system volume and variance were evaluated. Then, a mixture of 17 drugs and various metabolites (molecular mass of 151-749Da, logP of -1.04 to 6.7), was injected on six sub-2μm particle columns. Five newest generation core shell technology columns were compared and tested against one column packed with porous particles. Two aqueous (pH 2.7 and 6.8) and two organic mobile phases were evaluated, first with the same flow and temperature and subsequently at each column's individual limit of temperature and pressure. The results demonstrated that pre-column dead volume had negligible influence on the peak capacity and shape. In contrast, a decrease in post-column volume of 57% resulted in a substantial (47%) increase in median peak capacity and significantly improved peak shape. When the various combinations of stationary and mobile phases were used at the same flow rate (0.5mL/min) and temperature (45°C), limited differences were observed between the median peak capacities, with a maximum of 26%. At higher flow though (up to 0.9mL/min), a maximum difference of almost 40% in median peak capacity was found between columns. The finally selected combination of solid-core particle column and mobile phase composition was chosen for its selectivity, peak capacity, wide applicability and peak shape. The developed method was applied to rat hepatocyte samples incubated with the drug buspirone and demonstrated to provide a similar chromatographic resolution, but a 6 times higher signal-to-noise ratio than a more traditional UHPLC metabolite profiling method using a fully porous particle packed column, within one third of the analysis time. In conclusion, a widely applicable, selective and fast chromatographic method was developed that can be applied to perform drug metabolite profiling in the timeframe of a quantitative analysis. It is envisioned that this method will in future be used for simultaneous qualitative and quantitative analysis and can therefore be considered a first important step in the Quan/Qual workflow. Copyright © 2014 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 12/2014; 1374:122-133.
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    ABSTRACT: Poly(glycidyl methacrylate-co-ethylene dimethacrylate) (poly(GMA-co-EDMA)) is most frequently used as parent monolith to obtain stationary phases with a variety of surface chemistries for liquid chromatography and capillary electrochromatography. Functionalization is performed by opening the accessible 2,3-epoxypropyl groups of the monolith with a suitable reagent. The number of 2,3-epoxypropyl groups which are accessible before and after the functionalization reaction, and the grafting yield, are important parameters, required both to optimize functionalization and to interpret the chromatographic performance of functionalized monoliths. In this work, a method capable of providing this information for parent and functionalized poly(GMA-co-EDMA) monoliths prepared both in silica capillaries and in other supports is proposed. First, sulfuric acid and lithium aluminium hydride (LiAlH4) are sequentially used to release the 2,3-epoxypropyl groups as glycerol, which is subsequently determined by GC. About 6.0mmol of 2,3-epoxypropyl groups per gram of monolith was found in this work for the parent monoliths prepared in silica capillaries using UV-initiation. The monoliths were also functionalized using ammonia (NH3), diethylamine (DEA) and epinephrine, and the amount of residual 2,3-epoxypropyl groups, and hence the functionalization yield, were established by also measuring the GC peak of glycerol. The amounts of 2,3-epoxypropyl groups and the derivatization yields were established with RSDs of 1.7 and 3.4%, respectively. The proposed method was also applied to the characterization of poly(GMA-co-EDMA) monoliths prepared in glass vials. Significant differences with respect to those prepared in 100μm I.D. silica capillaries were evidenced. Copyright © 2014 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 12/2014;
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    ABSTRACT: A method for the determination of parabens in human urine and serum by capillary liquid chromatography (cLC) with UV-Vis and mass spectrometry (MS) detection using methacrylate ester-based monolithic columns has been developed. The influence of composition of polymerization mixture was studied. The optimum monolith was obtained with butyl methacrylate monomer at 60/40% (wt/wt) butyl methacrylate/ethylene dimethacrylate ratio and 50wt% porogens (composed of 36wt% of 1,4-butanediol, 54wt% 1-propanol and 10wt% water). Baseline resolution of analytes was achieved through a mobile phase of acetonitrile/water in gradient elution mode. Additionally, dispersive liquid-liquid microextraction (DLLME) was combined with both cLC-UV-Vis and cLC-MS to achieve the determination of parabens in human urine and serum samples with very low limits of detection. Satisfactory intra- and inter-day repeatabilities were obtained in UV-Vis and MS detection, although the latter provided lower detection limits (up to 300-fold) than the UV-Vis detection. Recoveries for the target analytes from spiked biological samples ranged from 95.2% to 106.7%. The proposed methodology for the ultra-low determination of parabens in human urine and serum samples is simple and fast, the consumption of reagents is very low, and very small samples can be analyzed. Copyright © 2014 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 12/2014;
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    ABSTRACT: Single-hole hollow molecularly imprinted microspheres (h-MIMs) were prepared by hard template method and applied to extract six triazine pesticides in cereal samples, followed by HPLC-MS/MS detection. The synthesis mechanism of the h-MIMs has been studied. The h-MIMs exhibited bigger specific surface area and much higher binding capacity than the molecularly imprinted polymers prepared by precipitation polymerization (p-MIPs) and surface polymerization (s-MIPs). Besides, the adsorption rate of h-MIMs to prometryn was significantly higher than that of p-MIPs and s-MIPs. Owing to the hollow structure of the h-MIMs, more binding cavities were located on the inner and outer surfaces of the h-MIMs, which could facilitate the removal of template molecules from the polymers and the rebinding of the target molecules to the polymers. Under the optimal conditions, the detection limits of triazines are in the range of 0.08-0.16ngg(-1). At the spiked level (5ngg(-1)), the recoveries of triazines are in the range of 81±4% to 96±4%. The proposed method was successfully applied to determine six triazines in five cereal samples. Atrazine was found in two rice samples and a wheat sample with the contents of 5.1, 6.7 and 5.6ngg(-1), respectively. Ametryn and prometryn were found in a maize sample with the contents of 7.6 and 7.3ngg(-1), respectively. Copyright © 2014 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 12/2014; 1376:26-34.
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    ABSTRACT: Phosphine (PH3), sulfuryl fluoride (SO2F2) and methyl bromide (CH3Br) are highly toxic chemical substances commonly used for fumigation, i.e., pest control with gaseous pesticides. Residues of fumigation agents constitute a health risk for workers affected, and therefore accurate methods for air sampling and analysis are needed. In this study, three commercial adsorbent tubes; Carbosieve SIII™, Air Toxics™ and Tenax TA™, were evaluated for sampling these highly volatile chemicals in air and their subsequent analysis by thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). The breakthrough volume (BTV) of each fumigant was experimentally determined on the different adsorbents at concentrations at or above their permissible exposure limits, using a method based on frontal chromatography of generated fumigant atmospheres. Carbosieve SIII™, a molecular sieve possessing a very high specific area, proved to be a better adsorbent than both Air Toxics™ and Tenax TA™, resulting in at least a 4-fold increase of the BTV50%. BTV50% for Carbosieve SIII™ at 20°C was measured as 4.7L/g, 5.5L/g and 126L/g for phosphine, sulfuryl fluoride and methyl bromide, respectively, implying safe sampling volumes of 1.9L, 2.2L and 50L, respectively, for a commercial tube packed with 800mg Carbosieve SIII™. The temperature dependence of BTV was strong for Carbosieve SIII™, showing a reduction of 3-5%/°C in breakthrough volume within the range -20 to 40°C. Furthermore, although Carbosieve SIII™ reportedly has a higher affinity for water than most other adsorbents, relative humidity had only a moderate influence on the retention capacity of phosphine. Overall, the applicability of Carbosieve SIII™ adsorbent sampling in combination with TD-GC-MS analysis was demonstrated for highly volatile fumigants. Copyright © 2014 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 12/2014; 1375:17-26.
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    ABSTRACT: Environmentally relevant organophosphate (OP) triester flame retardants are known to degrade to OP diester phosphoric acids. In this study, a quantitatively sensitive method was developed for OP diesters in biological samples of varying complexity, bovine serum, chicken egg homogenate and pork liver. Fortified with 1ng or 10ng each of the six OP diester and six OP triester standards, samples were extracted by accelerated solvent extraction that completely separated OP diesters and triesters. OP diester fractions were cleaned up using weak anion exchange solid phase extraction and eluted with high ionic strength ammonium acetate buffer. Optimal analysis of chlorinated OP diesters was via decamethonium hydroxide dicationic reagent derivatization and by LC-ESI(+)-MS/MS, and for all non-chlorinated OP diesters by non-derivatized LC-ESI(-)-MS/MS. Except for derivatization LC-ESI(+)-MS/MS analysis of liver, at the 10ng spiking level for the three matrices, recovery efficiencies, matrix effects and method limits of quantification (MLOQs) of OP diesters ranged from 55-116%, 92-119%, and 0.02-0.31ng/g wet weight (ww) respectively. Plasma samples of n=6 herring gulls (2010, Chantry Is., Laurentian Great Lakes) contained triphenyl phosphate and tris(1-3-dichloro-2-propyl) phosphate ranging from 1.3 to 4.0ng/g ww and <MLOQ to 0.41ng/g ww respectively. The OP diesters bis(1,3-dichloro-2-propyl) phosphate, bis-(2-butoxyethyl) phosphate and di(2-ethylhexyl) phosphate ranged from 0.7 to 3.5ng/g ww, 0.08 to 29.4ng/g ww and <MLOQ to 0.18ng/g ww respectively, and thus OP triester to diester metabolism occurs in exposed wild herring gulls. Crown Copyright © 2014. Published by Elsevier B.V. All rights reserved.
    Journal of Chromatography A 11/2014;
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    ABSTRACT: An online preconcentration approach was developed allowing the injection of very high volumes of biological samples, thereby greatly increasing sensitivity while maintaining LC resolution. The approach was applied to the analysis of radioactive samples from both in vitro and in vivo metabolism studies where typically the concentration of radioactivity given is often limited, while sample volume is usually not. The described online preconcentration approach reduces sample preparation and, therefore, also the risk for degradation and recovery issues often seen with offline preconcentration methods. In addition to facilitating the identification and profiling of low level metabolites within a sample, the described approach also provides robust quantitative analysis of samples derived from a range of biological matrices. The application of this approach is illustrated on real life samples from different matrices and containing drugs and metabolites with a wide variety in polarity, more specifically the analysis of extracts derived from an in vitro hepatocyte incubation, 36mL of blood/acetonitrile (1/1, v/v; 28dpm/mL) and 72mL of urine/methanol (9/1, v/v; 208dpm/mL). Copyright © 2014 Elsevier B.V. All rights reserved.
    Journal of Chromatography A 11/2014; 1372C:102-109.