Chromatographia (CHROMATOGRAPHIA )

Publisher: Springer Verlag


The ever increasing demands on the analyst make the rapid communication of new techniques and developments in the field of analytical chemistry of prime importance. CHROMATOGRAPHIA has been fulfilling this function for chromatography since it was first founded in 1968. During the intervening years, however, the journal has itself evolved to meet the challenges of changing times and demands. Thus, the composition of the Editorial Board is reviewed at regular intervals so as to reflect shifts in interest and the establishment of centres of excellence in countries that have not previously been active in the field. Publishing policy, including the number of papers and the format, are subject to continuous appraisal.

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    Chromatographia (Online)
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Springer Verlag

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Publications in this journal

  • [Show abstract] [Hide abstract]
    ABSTRACT: The present study deals with the preconcentration and determination of toxic metal ions using p-tetranitrocalix[4]arene (3) appended silica-based new HPLC column. The synthesized material was characterized using Fourier transform infrared and scanning electron microscopy techniques. The sorption characteristics of the HPLC column were investigated for three toxic metals (Cd2+, Hg2+ and Pb2+) in column agreement. The experiments were performed in five steps that were monitored using a UV–visible diode-array detector. However, all the HPLC experimental results were reconfirmed by using atomic absorption spectrophotometer. The effect of concentration on the sorption efficiency of the column was evaluated for all the three metals and the data obtained were investigated using Langmuir, Freundlich and Dubinin–Redushkevich (D–R) sorption isotherms. The value of coefficient of determination (R 2), i.e. 0.99, suggested that the Freundlich sorption isotherm was found to be the best-fit model for all the three toxic metal ions, whereas, mean free energy was calculated from the D–R isotherm as 5.3, 5.7, and 5.8 kJ/mol for Pb2+, Cd2+, and Hg2+, respectively; suggesting that physical electrostatic force is involved in the sorption process. The developed method was validated for system efficiency, accuracy, and precision.
    Chromatographia 08/2014; 76(15-16).
  • Chromatographia 08/2014;
  • Chromatographia 04/2014;
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    ABSTRACT: A novel microporous membrane/solvent microextraction (MPMSME) approach was developed in which a piece of microporous filter membrane was used as not only extraction solvent holder but also solid phase extraction unit. Subsequently, high-performance liquid chromatography with an UV detector was conducted. The wide exchange surface and very little organic solvent consumption made this sample pretreatment technology very interesting. The cinnamic acid derivatives were used as model analytes to evaluate the procedure. Parameters that affect the MPMSME such as type of extraction solvent, membrane area (or volumes of extraction solvent), aqueous phase pH, ionic strength, extraction stirring rate, extraction time, and sample volume were investigated and optimized. The enrichment factor (EF) of analyte was defined in MPMSME. Under the optimized conditions, the EFs of cinnamic acid derivatives were 43–144. Good linearities were obtained from 4 to 4,000 ng mL−1 for all the analytes with regression coefficients of between 0.9956 and 0.9977; the limits of quantification were below 0.4 ng mL−1, and satisfactory recoveries (93–106 %) and precisions (0.37–13 %) were also achieved. The experimental results showed that the method was simple, rapid, practical, and effective for preconcentration and determination of the cinnamic acid derivatives in rhizoma typhonii.
    Chromatographia 04/2014; 77(7-8).
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    ABSTRACT: Liquid chromatography–ion trap mass spectrometry was employed to investigate the metabolism of linarin in rats. Identification and structural elucidation of the metabolites were performed by comparing the differences in molecular masses, retention times, and full scan MSn spectra between linarin and its metabolites. Six metabolites (acacetin, apigenin, acacetin glucuronide, apigenin glucuronide, acacetin sulfate, apigenin sulfate) were detected in rat urine after oral administration of linarin at the dose of 50 mg kg−1. Furthermore, a selective and sensitive liquid chromatography–triple quadruple mass spectrometry assay was developed and validated for the simultaneous determination of linarin and acacetin (the major metabolite of linarin) in rat urine. Chromatographic separation was carried out on a C18 column, and mass spectrometric detection was performed using a triple-quadrupole mass spectrometer coupled with an electrospray ionization source in the positive ion mode. Quantitation of linarin and acacetin was performed using selected reaction monitoring of precursor–product ion transitions at m/z 593 → 285 for linarin, 285 → 242 for acacetin, and 303 → 153 for hesperitin (internal standard), respectively. The assay exhibited good linearity (r > 0.9900) for both linarin and acacetin. The intra- and inter-day precisions were <13.4 % and the accuracy was between −8.1 and 3.1 %. The method was successfully applied to the urinary excretion study of linarin in rats after oral administration of linarin.
    Chromatographia 03/2014; 77(7):571-579.
  • Chromatographia 02/2014; 77(xx):xxx-xxx.
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    ABSTRACT: A rapid, convenient and reliable method for microextraction in packed syringe (MEPS) of the loop diuretic furosemide (FUR) in urine along with high-per-formance liquid chromatography (HPLC) was developed. A nanocomposite based on silver nanoparticles/polyaniline (Ag-NPs/PANI) was synthesized and used as the MEPS packing material. This nanocomposite was prepared con-veniently using interfacial polymerization without the need for any templates or functional dopants. The feasibility of the synthesized nanocomposites was examined by isolation of FUR from diluted urine samples. After extraction, the analyte was desorbed by 200lL of methanol. It was then dried and the residue was dissolved in 30lL of methanol and an aliquot of 25lL was, finally, injected into the HPLC system. Important parameters influencing the extraction and desorption processes were optimized and 25 cycles of draw–eject gave maximum peak area, when desorption was performed. The linearity was studied by preconcentration of 5 mL of diluted urine sample spiked with a standard solution of FUR in the concentration range of 15–750lgL -1 . The coefficient of determination was satisfactory (r 2[0.99) and the relative standard deviation (RSD %) value under the optimized condition was 8.8 %. The limit of detection and limit of quantification were 7 and 15lgL -1 , respectively.
    Chromatographia 01/2014;
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    ABSTRACT: quantitative structure-retention relationship (QSRR) approach and gradient retention modeling based on isocratic retention data is developed and presented in this paper. Such an integrated approach removes the general QSRR limitation of highly predefined application conditions (i.e., QSRR are generally applicable only under the conditions used during model development) and allows the prediction of retentions over a wide range of different elution conditions (practically for any isocratic or gradient elution profile). At the same time, it retains the ability to predict retention of components unknown to the model, i.e., the components that have not been used in modeling. Ion-exchange chromatography (IC) analysis of carbohydrates was selected as modeling environment. Three regression techniques were applied and compared during QSRR modeling, namely: stepwise multiple linear regression, partial least squares (PLS), and uninformative variable elimination–PLS regression. The obtained prediction results of the best QSRR model (root-meansquare error of prediction = 22.69 %) were similar to those found in the literature. The upgrade from QSRR to the integrated model did not diminish the predictive ability of the model, indicating an excellent potential of the developed methodology not only in IC but also in chromatography in general.
    Chromatographia 01/2014;
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    ABSTRACT: Biomarkers in amniotic fluid (AF) include both non-modified and phosphorylated proteins and can be used in the diagnosis of pregnancy-associated pathologic conditions. In this work, an integrated LC-MS method for selective, sensitive and reproducible analysis of phosphorylation in proteins has been applied to AF. Online digestion of (phospho) proteins was coupled with the selective enrichment on a TiO2 trap, and separated by RPLC-MSn of both normal and phosphorylated produced peptides. First, an AF-pooled sample was analyzed and a general map of contained proteins and biomarkers was derived in a single run. Then, individual AF samples were analyzed with a downscaled platform with improved sensitivity. On purpose, a trypsin-based CIMA (R) minidisk was used for online digestion of AF. The obtained protein profile was highly consistent with the one obtained with traditional off-line digestions. Moreover, the use of a specific phospho-enrichment tool followed by LTQ-Orbitrap, enhanced the confidence in the determination of protein phosphorylation state and phosphorylation sites. The phosphorylation sites of IGFBP-1 and osteopontin present in the AF of two individual samples were monitored with a total of 24 and 17 phosphopeptides, respectively, encoding for 12 putative novel phosphorylation sites in addition to known sites.
    Chromatographia 01/2014; 77(1-2):39-50.
  • Chromatographia 01/2014;
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    ABSTRACT: Liposoluble vitamins are widely analyzed due to their significant antioxidant activity. Quantification by liquid or gas chromatography is often time consuming and requires sample treatments prior to the analysis. Supercritical fluid chromatography (SFC), especially with the developments of new commercial systems, is nowadays considered as a credible alternative to standard chromatography. It provides a reduced acquisition time as well as sensitivity similar to that of liquid chromatography. To illustrate the new capabilities of SFC, six organic compounds related to the vitamin A family, all-trans-retinal, all-trans-retinol, all-trans-retinoic acid, retinyl propionate, retinyl acetate, and all-trans-retinyl palmitate, were analyzed and quantified. The choice of the column chemistry, co-solvent, the linearity and reproducibility of the method, and the matrix effect are discussed in detail. Best separation was finally obtained using a diphenyl column, with an excellent linearity over three orders of magnitude and limits of quantification in the low picomole range. Finally, the method was used for the quantification of retinyl palmitate in a pharmaceutical product with minimal sample preparation.
    Chromatographia 12/2013; 76(17-18):1097-1105.
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    ABSTRACT: A method based on capillary electrophoresis with amperometric detection (CE–AD) was developed for the determination of amifostine (a cytoprotective agent, WR2721) and 2-(3-aminopropylamino)ethanethiol) (WR1065, the active metabolite of WR2721) in rat plasma. The contents of WR1065 and amifostine were determined by measuring WR1065 in deproteinized rat plasma using CE–AD before and after it was incubated at 37 °C for 4 h in acidic solution, respectively. During the incubation, amifostine was quantitatively converted to WR1065. In addition, cysteine and uric acid in rat plasma were also determined simultaneously. The detection electrode was a 500 μm diameter platinum disc electrode at a detection potential of +1.0 V (vs. saturated calomel electrode). The analytes can be well separated within 9 min in a 50-cm-long fused-silica capillary at a separation voltage of 18 kV in a 100 mM phosphate buffer (pH 7.5). The relation between peak current and analyte concentration was linear over about 3 orders of magnitude with the limits of quantification (S/N = 3) ranging from 0.60 to 1.40 μM. The method has been validated. Satisfactory within-day and between-day precisions were obtained with relative standard deviations of ≤4.9 and ≤5.1 % for WR1065 and ≤5.0 and ≤5.3 % for amifostine, respectively. The within-day and between-day accuracy was in the range of 98.6–102.3 % and 95.7–97.2 % for WR1065 and 97.5–98.6 and 95.3–97.1 % for amifostine, respectively.
    Chromatographia 12/2013; 76(23-24).

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