2008
VVCE-0070-07, APVV
Establishment of centre of excelence of (bio)separation methods based on principles of principles of electroseparations, liquid chromatography and mass spectrometry, Dušan Kaniansky, 2008 - 2011
APVV-0595-07
Development of novel combined high performance liquid chromatography methods focused to characterization and analysis of environmental biopolymers, Milan Hutta, 2008-2010
VEGA 1/0430/08
Study and development of analytical methods for determination, pre-concentration and speciation of eco-toxicologically important elements in environmental samples - Mária Žemberyová, 2008 - 2010
VEGA 1/4474/07
On-line and off-line combination of liquid chromatography methods for analysis and characterization of natural envirobiopolymers - humic substances and lignins - Róbert Góra
VEGA 1/3558/06
Combinations of capillary electrophoresis techniques for multidimensional separations of multi-component mixtures of low-molecular and high-molecular substances - Dušan Kaniansky, 2006 - 2008
This project contributes, especially, for new approaches to chiral separation of enantiomers as based on the combination ITP-CZE-DAD supported for the analyses of bio-samples. A significant contribution, as directed to the use of suitable electrolyte solutions, covered for various electroseparation techniques. One of the application trends is reflecting for drinking water analysis as documented by the results of advanced analytical methods. An original preparative electroseparation system based on capillary isotachophoresis as intended to the separation and fractionation of multicomponent mixtures was developed.
VEGA 1/3562/06
Miniaturized integrated analytical systems for (ultra)trace analysis based on electro-separations on a chip with coupled-columns - Marián Masár, 2006 - 2008
The project dealt with implementation of capillary electrophoresis (CE) on miniaturized analytical systems (chips) for (ultra)trace analysis. From CE techniques, zone electrophoresis (ZE), isotachophoresis (ITP) and their on-line combinations (ITP-ITP, ITP-ZE and ZE-ZE) were implemented on CC chip. Significant results were obtained using a new principle of bubble formation suppression in the separation system on the chip. New approaches for effective suppression of the analytes adsorption on the chip walls were studied. CC chip operated in a regime with extremely large sample volume was found as an effective mean for reaching more favorable cLOD for trace analytes present in multicomponent matrices. Significant results were also obtained in pre-column sample pretreatment based on membrane extraction.
VEGA 1/3583/06
Combinations of liquid chromatography methods and electro-separation methods for multi-component trace analysis of ionogenic substances in complex samples - Milan Hutta, 2006 - 2008
The project was intended to the development of combined analytical techniques on the basis of liquid chromatography and electro-separation methods devoted to trace and/or ultra-trace analysis of ionogenic compounds present in complex natural samples. Aided study of orthogonality of these combined techniques and testing of compatibility of used separation media from the point of view of multi-component mixtures of selected analytes was done beside the development of techniques of by sample on-column pumping large-volume injection of selected ionogenic substances (pesticides) and further development of "solid sample injection" technique in column-switching HPLC.
VEGA 1/03563/06
On-line and off-line combinations of liquid chromatography methods and methods of atomic spectrometry for trace analysis and speciation of organometallic substances in biological and environmental samples - Radoslav Halko, 2006 - 2008
The project was focused on the study of applicability of mobile phases used in HPLC for the need of effective combining of liquid chromatography methods and methods of molecular or atomic spectrometry (AAS). Another aim was the design and development of a proper interface for these combinations. Application of off line combination of HPLC and molecular spectroscopy or AAS methods, respectively, was used systematically for such problems solving as are problems of determination of copper in human urine at trace concentration levels. Knowledge gained from HPLC and molecular spectrometry or AAS off-line combination study was be utilized for construction of on-line interface for their coupling.
PRIF UK 4/2008
Evaluation of on-line combination of capillary zone electrophoresis with isotachophoresis in a two-dimensional mode for the separation of multi-component samples - Miroslava Halašiová, 2008
The aim of presented grant was to study basic possibilities 2D approach of on-line combination of ITP and CZE in anionic mode by using of model sample, which contain 50-60 organic UV absorbing model analytes. In comparison with common ITP-CZE approach to evaluate elimination of risk overlap by decreasing number of analytes present in CZE stage. One of the main task was to found appropriate separation condition, effective discrete spacers and their concentration to reach total number of resoluted peaks as height as possible.
From analytical point of view is very important repeatability of 2D experiments. According to fact, that analytes were separated in ITP and CZE stage on the base of effective mobilities, emphasis were put on tools, which can influence the effective mobility. We want to create the model, which can be applicated in separation of real multicomponent samples (for example urine, serum).
UK/13/2008
Determination of environmentally important markers of quality of drinking waters by chip electrophoresis in accordance with regulation of Ministry of Health of Slovak Republic Nr. 354/2006 - Milan Luc, 2008
This project was aimed at simultaneous determination of major cationic constituents (ammonium, calcium, magnesium, sodium and potassium) in drinking waters by capillary zone electrophoresis in a column-coupling (CC) chip. Under prefered conditions (suppressed electroosmotic and hydrodynamic flow), the CZE separations were carried out in a propionate background electrolyte at pH = 3.2 containing a surface modifier of the chip channels' walls triethylentetramine (TETA) and a complexing agent 18-crown-6-ether (at 35 mmol/l concentration) to reach complete resolution of studied cations. The concentration limits of detection estimated for the studied cations ranged from 4.9 to 11.5 µg/l. A short total analysis time (ca. 300s) and dynamic range over two orders of magnitude (25-4000 µg/l) were reached using contact conductivity detection. RSD values of migration times and peak areas of model analytes and real sample did not exceed the 5% except the case of small concentration 50 µg/l. Sample pre-treatment was realized only through dilution and degassing of drinking waters.
UK/206/2008
Analysis and identification of drugs and their metabolites in complex matrices by combinatation of electrophoretic and chromatographic techniques with mass spectrometry - Andrea Sta?ová, 2008
The work is dealing with analysis of biologically important compounds in complex matrices using off-line combination of electrophoretic separation techniques with mass spectrometric selective detection and UPLC/MS combination. Busereline was chosen as model analyte and urine as complex matrix. Urine spiked with busereline was analyzed by DI-MS and UPLC/MS. Both techniques can detect and identify busereline in complex biological matrix without any sample pretreatment but analysis time is favoring DI-MS. The fractions, catched by using preparative ITP with the help of discrete spacers, were finally analyzed by DI-MS. It was shown that pITP performed before DI-MS analysis can significantly simplify complex matrix, and, due to its concentration power, pITP can consequently decrease the concentration limit of detection. Concentration of busereline in urine samples was in our work relatively high (10 mg/L) but from the ion intensities obtained in MS as well as MS/MS analyses it is clear that this concentration level could be several orders of magnitude lower for reliable detection and identification of busereline in urine by MS detection.
UK/324/2008
Development and application of solid phase extraction for vanadium and chromium preconcentration and speciation in water samples by electrothermal atomic absorption spektrometry - Lenka Machá?ková, 2008
The determination of vanadium and chromium species is of great importance in understanding the biological and their physiological functions as well as their potential toxicity. In this project, the effective solid phase extraction methods were developed and used for the preconcentration and determination of vanadium (V) and chromium (VI) coupled with electrothermal and flame AAS detection, respectively. Solid phase extraction using Chromabond® NH2 columns was used for the selective preconcentration of vanadium (V) as its chelate with Alizarin Red S and chromium (VI) ions. Present methods were applied successfully to the analysis of trace concentrations of vanadium (V) and chromium (VI) in real water samples. Moreover, the method for direct determination of vanadium in the different types of natural waters by ETAAS with Zeeman background correction with application of ascorbic acid and ammonium nitrate as the matrix modifier was developed.
2007
VEGA 1/4474/07
On-line and off-line combination of liquid chromatography methods for analysis and characterization of natural envirobiopolymers - humic substances and lignins - Róbert Góra
VEGA 1/3558/06
Combinations of capillary electrophoresis techniques for multidimensional separations of multi-component mixtures of low-molecular and high-molecular substances - Dušan Kaniansky, 2006 - 2008
VEGA 1/3562/06
Miniaturized integrated analytical systems for (ultra)trace analysis based on electro-separations on a chip with coupled-columns - Marián Masár, 2006 - 2008
VEGA 1/3583/06
Combinations of liquid chromatography methods and electro-separation methods for multi-component trace analysis of ionogenic substances in complex samples - Milan Hutta, 2006 - 2008
VEGA 1/03563/06
On-line and off-line combinations of liquid chromatography methods and methods of atomic spectrometry for trace analysis and speciation of organometallic substances in biological and environmental samples - Radoslav Halko, 2006 - 2008
VEGA 1/2466/05
Study and development of new analytical methods for elemental speciation and pre-concentration in environmental samples - Mária Žemberyová, 2005-2007
Study and elaboration of analytical procedures for on-line elemental speciation and preconcentration of the elements in water samples for the determination by the atomic spectrometry and chromatography techniques was conducted. Trace inorganic speciation of As, Sb and Cr in water samples in regard of differention of oxidation states, using SPE preconcentration of the species was done. Study of the determination of bioavailable and specific forms using recommended single and sequential procedures and elaboration of new procedures by which the fractionation of the organic matter is also possible.
UK/116/2007
Determination of halogenacetic acids in drinking water by extraction sample pretreatment and electrophoretic chip - Roman Žurek
The project was focused to the development of new analytical methods designed around miniaturized chip-based format for determination of cancerogenic substances - halogenacetic acids (HAAC) in drinking waters. Techniques of capillary electrophoresis (CZE, ITP) with conductimetric detection were evaluated for the purpose and resulted in both less expensive and faster methods of HAAC determination in comparison to most of recently used methods.
UK/222/2007
The use of micellar systems in liquid chromatography for separation of substances on columns with monolithic stationary phases. - Radoslav Halko
This project was aimed at the study of the utilization micellar systems as components of mobile phases in liquid chromatography. The monolithic stationary phase is used. This stationary phase is able to eliminate disadvantageous impact to loss of separation efficiency, which is observed with the classical reverse-phase analytical columns.
UK/259/2007
On-line and off-line combination of liquid chromatography methods for analysis and characterization of natural enviropolymers - humic substances and lignins.- Róbert Góra
RP-HPLC using stepwise gradients of dimethylformamide (DMF) in buffered aqueous mobile phase and a wide-pore (30nm) octadecylsilica column has been aplied to the analysis of soil, peat and air particulate humic and humic-like substances (HSs), as-well-as lignin in order to demonstrate the usefullness of the approach for their characterization even at trace concentration level. Tandem combination of spectrophotometric (DAD) and fluorimetric detection was used to get more detailed information on chromatographic behaviour of humic substances and lignins, respectively.
UK/122/2007
Analysis and identification of peptides in complex matrices by electrophoretic techniques devised for combination with mass spectrometry - Andrea Sta?ová
2006
VEGA 1/3558/06
Combinations of capillary electrophoresis techniques for multidimensional separations of multi-component mixtures of low-molecular and high-molecular substances - Dušan Kaniansky, 2006 - 2008
VEGA 1/3562/06
Miniaturized integrated analytical systems for (ultra)trace analysis based on electro-separations on a chip with coupled-columns - Marián Masár, 2006 - 2008
VEGA 1/3583/06
Combinations of liquid chromatography methods and electro-separation methods for multi-component trace analysis of ionogenic substances in complex samples - Milan Hutta, 2006 - 2008
VEGA 1/03563/06
On-line and off-line combinations of liquid chromatography methods and methods of atomic spectrometry for trace analysis and speciation of organometallic substances in biological and environmental samples - Radoslav Halko, 2006 - 2008
VEGA 1/2466/05
Study and development of new analytical methods for elemental speciation and pre-concentration in environmental samples - Mária Žemberyová, 2005-2007
DAAD 13/2004
Development and study of New Analytical Methods for elemental speciation and preconcentration of metals in environmental samples, Institute of Chemistry, Department of Instrumental Analytics, University Duisburg-Essen, Germany - Mária Žemberyová, 2005-2006
Elaboration and study of new analytical procedures for preconcentration and speciation of Be, Mo, V and Cr in water samples for the determination by atomic spectrometry methods. Inorganic speciation of Mo, V, Cr in water samples in regard to differentiaton of oxidation states, using SPE preconcentration of the species. Study of the determination of bioavailable and specific forms using recommended (BCR) single and sequential procedures.
UK/277/2006
RP-HPLC analysis and characterization of lignins isolated from various woods by Klason method - Róbert Góra, 2006
RP HPLC using stepwise gradients of N, N-dimethylformamide (DMF) in a phosphate buffered (pH 3.00) aqueous mobile phase and a wide-pore (30nm) octadecylsilica column has been aplied to the analysis of a variety of lignins - organocell lignin, dioxane lignin, Björkman lignin and Klason lignins from both softwoods and hardwoods, respectively, in order to demonstrate the usefullness of the approach for their characterization. Tandem combination of spectrophotometric (DAD) and fluorimetric detection was used to get more detailed information on chromatographic behaviour of lignins. The results showed that ten-step gradient can induce distinct features of lignins and humic substances. Combination of good solvating properties of DMF for lignins together with wide pore RP sorbent improves surface interactions of the analytes and suppresses influence of size exclusion effects. Thus it provides reproducibility of characterization profiles and robustness of the method. Calculated reproducibility of retention time of selected peaks was 0.46 % RSD. Repeatability of the data within one week (set of 7 data) was 1.1%RSD. These data are representative also for the other well-shaped peaks of analysed substances.
UK/156/2006
Chip with conductivity detection based highly-precise isotachophoretic determinations of ionogenic substances in biopharmaceutical products - Mária Drusková, 2006
UK/166/2006
Two-dimensional separations combining on-line capillary isotachophoresis with capillary zone electrophoresis- Vladimíra Jánošová, 2006
2005
VEGA 1/2466/05
Study and development of new analytical methods for elemental speciation and pre-concentration in environmental samples - Mária Žemberyová, 2005-2007
VEGA 1/0087/03
Miniaturised electroseparation techniques for trace analysis of ionogenic compounds and biopolymers present in complex ionic matrices - Dušan Kaniansky, 2003-2005
The most important contributions that deal with the use of driving electrodes as designed for the electroseparations on chips (original results as documented by an EU patent). An original electrophoretic technique is based on a combination of electrophoresis-zone technique on a column-switching electrophoresis chip. Significant results that dealt with the electroseparation of proteins on the chips (an original combination of the chip with a conductivity detector as intended for the separation of proteins). A new approach to the separation of proteins based on a combination of isotachophoresis with zone electrophoresis on a column-switching chip was elaborated. A significant contribution, as directed to the use of suitable electrolyte solutions, developed for the various electroseparation techniques. One of the application trends, in the electrophoresis chips, is focused on food analysis as documented by original contributions. An original preparative electroseparation system based on capillary isotachophoresis as intended for the separation and fractionation of proteins was elaborated.
VEGA 1/0061/03
Study of the oxidation in chemical processing of wood through new methods of separation and analysis - Principal Investigator: Svetozár Katuščák, Co-investigators: Dušan Kaniansky and Milan Hutta, 2003-2005
Oxidation processes play a key role in many technologies connected with the processing of the most important renewable raw material - wood. Processes include bleaching, de-lignification, ageing, combustion, recycling and processing of wastes. Improvements in our knowledge on the course of oxidation reactions and products in the chemical processing of wood is limited by the multi-component and complex character of the products of lignin oxidation, cellulose and lingo-cellulose materials (LCM). We propose to attain new information on the course of oxidation, delignification and bleaching through utilizing effective new separation methods in combination with multi-detecting systems. The aim of the project is to utilize previous achievements in the techniques of miniaturized analytical systems (lab-on-a-chip concept), new monolithic HPLC columns, imunosorbents, AAS and tandem multi-detector systems, for improving the analytical characterization of the reaction products. A better understanding of LCM oxidation and new information should be achieved supporting better control of the oxidation processes, better utilization of multi-component oxidants and catalysts in wood processing and subsequently further improvement of the environmental quality of technologies and properties of the final products.
VEGA 1/0070/03
New chromatographic methods of sampling and on-line analysis of chiral pollutants in air, water and soil - Milan Hutta, 2003-2005
New methods for the characterization and analysis of humic substances in soil and air dust particles were devised and published based on the proper use of a combination of step gradient, wide-pore octadecylsilica and solubilization power of dimethylformamide in a chromatographic system of HPLC with UV-VIS (DAD) and fluorescence detection. A study of the influence of co-sampled polen particles on various parameters of a new HPLC method for the determination of air humic-like substances (HULIS) was done. For diagnostic purposes a fast (3 min) HPLC method of analysis of urine porphyrins (including their positional isomers) at ultratrace (ng/l) level using monolithic column was designed and published. Interactions between analyte and the soil matrix were studied and on this basis a new approach to large-volume injection (20 ml and more) of soil extracts in RP-HPLC was devised, published and applied to the detection of pesticides (including chiral pyrethroids) at trace levels.
DAAD 13/2004
Development and study of New Analytical Methods for elemental speciation and preconcentration of metals in environmental samples, Institute of Chemistry, Department of Instrumental Analytics, University Duisburg-Essen, Germany - Mária Žemberyová, 2005-2006
Elaboration and study of new analytical procedures for preconcentration and speciation of Be, Mo, V and Cr in water samples for the determination by atomic spectrometry methods. Inorganic speciation of Mo, V, Cr in water samples in regard to differentiaton of oxidation states, using SPE preconcentration of the species. Study of the determination of bioavailable and specific forms using recommended (BCR) single and sequential procedures.
UK/266/2005
HPLC large volume injection of pesticides - Zoltán Hajdú, 2005
In this work we compared two approaches to injection of a sample in HPLC (large volume injection LVI and a "normal" volume injection directly onto the analytical column). The advantages and disadvantages of LVI HPLC applied to analysis of pyrethroid insecticides were evaluated. The method of direct LVI onto HPLC analytical column is applicable for the analysis of pyrethroides at low concentration levels. With the injection of 10 ml of soil extract of pyrethroids we were able to determine kadethrin with a concentration of 62,7 ng/ml, cypermethrin 56 ng/ml, trans - permethrin 37 ng/ml and cis - permethrin 13 ng/ml, contrary to injection of 50 l which abled determination of kadethrin with a concentration of 4 g/ml, cypermethrin 6 g/ml , trans - permethrin 5.87 g/ml and cis - permethrin 2 g/ml. The analysis was highly acceptable in spite of the fact that the sorption of these compounds to soil is significant.
UK/263/2005
New on-line chromatografic methods for pretreatment and detection of environmental samples and their speciation - Radoslav Halko, 2005
UK 307/2005
Preparative capillary isotachophoresis as a sample pretreatment technique in the analysis of cytosol - Róbert Bodor, 2005
The project deals with the use of preparative capillary isotachophoresis (pITP), operating in discontinuous fractionation mode, to the pretreatment of multi-component biosample - cytosol of mycobacterium smegmatis (MSmeg) before their analysis by other analytical methods. Preparative ITP was used in two sample pretreatment modes: 1) the isolation of trace analyte from the sample; 2) the fractionation of the sample into a certain number of fractions.The fractions of the samples obtained by preparative ITP were monitored by capillary isotachophoresis, by on-line combination of capillary zone electrophoresis with isotachophoresis (ITP-CZE) and by planar gel electrophoresis (SDS-PAGE). The off-line combination of the preparative ITP with other electrophoretic methods (ITP-CZE, planar gel electrophoresis) shows that pre-treatment of samples by pITP can be effective in better general separations of the proteinic samples. The results obtained in SDS-PAGE experiments shows that ITP offers orthogonal separating conditions to the molecular size based on separation of proteins by SDS-PAGE.
UK 265/2005
Two-dimensional electroseparations on the chip for trace analysis of ionogenic compounds in ionogenic matrices - Marián Masár, 2005
This work deals with the determination of chloride, sulfate and nitrate in drinking water by zone electrophoresis (ZE) on a column-coupling (CC) chip with conductivity detection. A low pH of the carrier electrolyte used in ZE separations suppressed potential disturbances of the co-migrating constituents, e.g., some inorganic anions and organic acids. The required differences in the effective mobilities of the analytes were reached by combining the ionic strength effect of bis-tris propane and a host-guest complex forming equilibria with ?-cyclodextrin or an association equilibria with 3-(N,N-dimethyldodecyl-ammonio)propane sulfonate. Under our working conditions, studied analytes were detected at a concentration of 100 ?g/l. Total analysis time below 450 s and a working range for chloride and sulfate up to 60 mg/l and for nitrate of up to 20 mg/l can be achieved via this method without sample dilution. Filtration and degassing were the only sample pre-treatment procedures. The use of an internal standard enabled an easy chip-to-chip and equipment-to-equipment transfer of the employed analytical method.
UK 103/2005
Direct Analysis of Solid Environmental Samples by Electrothermal Atomic Absorption Spectrometry - Ingrid Hagarová, 2005
From analytical techniques, electrothermal atomic absorption spectrometry (ETAAS) has been shown to be the most attractive technique for the direct analysis of solid samples. There are two well-established procedures for the direct analysis of solids by ETAAS, namely slurry sampling and solid sampling. The aim of this project was to develop simple and reliable procedures for direct determination of beryllium, molybdenum and vanadium in solid environmental samples (soils, sedimets, sludges) by slurry sampling ETAAS and solid sampling ETAAS.
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