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Papers by Beata Polak
Molecules, Feb 17, 2022
This article is an open access article distributed under the terms and conditions of the Creative... more This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY
Journal of analytical methods in chemistry, 2016
The new mode of two-dimensional gradient thin layer chromatography (MGD-2D TLC) has been presente... more The new mode of two-dimensional gradient thin layer chromatography (MGD-2D TLC) has been presented. Short distance development of sample in the first dimension leads to formation of the preconcentrated narrow zones. They are consecutively separated in the second dimension with the mobile phase gradient in several steps of development until the eluent reaches the further end of the chromatographic plate. The use of the above-mentioned technique allows isolating and then identifying the compounds of various polarity from the multicomponent mixture. The practical application of two-dimensional gradient thin layer chromatography has been performed for isolation of the two plant (Juniperus and Thymus) oils components as the examples of test mixtures. The experiments have been carried out with the use of silica gel plates as well as a normal phase condition. The results of solute separation with isocratic one-dimensional thin layer chromatography system have been compared with those of twodimensional gradient system. It has been observed that application of the latter mode leads to almost triplicated number of zones in comparison with the former one. It is purposeful to apply the proposed mode to control the purity of the dominant component or components of the mixture.
Journal of Chromatography A, May 1, 2011
Theoretical backgrounds, development, examples of separations, constructional details and princip... more Theoretical backgrounds, development, examples of separations, constructional details and principle of action of devices of pressurized planar electrochromatography (PPEC) are presented. Development of the mode is described in respect of operating variables (composition of the mobile phase, pressure exerted on adsorbent layer, mobile phase flow velocity, temperature of separating system, etc.) influencing separation efficiency (kinetic performance, repeatability, separation time). Advantages of PPEC such as high kinetic performance, short separation time and different separation selectivities, especially relative to conventional thin-layer chromatography, are described. Examples of two-dimensional separations are demonstrated to show high separation potential of the mode when combined with conventional thin-layer chromatography (TLC). The PPEC mode is in infancy stage of development, so its challenges are presented as well.
Current Issues in Pharmacy and Medical Sciences
In this work, analysis of some drugs used in the treatment of neurodegenerative disorders (sulpir... more In this work, analysis of some drugs used in the treatment of neurodegenerative disorders (sulpiride, olanzapine, carbamazepine, trazodone, clomipramine, and pridinol) was achieved through micellar electrokinetic chromatography (MEKC). The effect of surfactant (sodium dodecylsulphate), acetonitrile, and buffer pH and concentration on the solute retention was also investigated. Successful separation of all compound mixtures was obtained. The method was applied for the quantitative analysis of investigated compounds, and the LOD and LOQ were determined. The LOD values were in the range from 0.0127 mg/mL for clomipramine, to 0.1398 mg/mL for pridinol, while LOQ were in the range 0.0384 mg/mL for clomipramine, to 0.4237 for pridinol. The mode was also applied for the determination of investigated solutes in pharmaceutical prescriptions.
Current Issues in Pharmacy and Medical Sciences
Separation of some isoquinoline alkaloids (narcotine, chelidonine, dihydrocodeine, cinchonine, be... more Separation of some isoquinoline alkaloids (narcotine, chelidonine, dihydrocodeine, cinchonine, berberine, cinchonidine, papaverine, apomorphine) has been investigated with pressurized planar electrochromatography (PPEC) and high-performance thin-layer chromatography (HPTLC) in reversed-phase systems. The mobile phase consisted of acetonitrile and aqueous buffer (disodium phosphate and citric acid). The influence of the mobile phase buffer pH on migration distance (PPEC) and retardation factor (HPTLC) of the solutes has been investigated and compared. The results show different separation selectivity in both PPEC and HPTLC systems especially at pH range of buffer solution of the mobile phase that facilitates ionization of the solutes investigated.
Chromatographia, 2006
The enantiomers of some amino acids have been separated on commercial chiral TLC plates in revers... more The enantiomers of some amino acids have been separated on commercial chiral TLC plates in reversed-phase mode. The effect of the pH* of the aqueous-organic mobile phase on the retention and mobility of the enantiomers and on selectivity was investigated. It was shown that for most of the amino acids investigated the highest enantioselectivity was obtained at pH* 3-4 or 6-7. The drift and disturbance of the baseline on the chromatograms were also much smaller at pH* 3-4 and 6-7.
Current Issues in Pharmacy and Medical Sciences
Eight drugs blocking beta-adrenergic receptors activity (acebutolol, alprenolol, atenolol, oxpren... more Eight drugs blocking beta-adrenergic receptors activity (acebutolol, alprenolol, atenolol, oxprenolol, labetalol, metoprolol, propranolol and sotalol) were investigated through the use of the thin-layer technique with its mobile phase containing surfactant. Assessment of the effect of surfactant presence and 1-propanol concentration in the mobile phase on the retention and separation of investigated solutes was then carried out wherein the effect of the surfactant concentration on the zone shape properties (asymmetry and tailing coefficient) was investigated. The method was applied for the quantitative analysis of the chosen solutes, and the LOD and LOQ values of chosen were determined. These were as follows: acebutolol – 1.11 and 3.36 μg/spot, metoprolol 1.45 μg/spot, 4.4 μg/spot. The chosen system is environmentally friendly due to using silica gel plates and only 5% of propanol in water.
Chromatographia, 1993
Equations for the final R F values for mobile phase gradient development and gradient multiple de... more Equations for the final R F values for mobile phase gradient development and gradient multiple development are presented. Computer simulations of gradient development for both modes of thin-layer chromatography are discussed for the preliminary optimization of gradient programs.
Applications, Theory and Instrumentation, 2011
In conventional thin layer chromatography (TLC), the movement of the mobile phase is driven by ca... more In conventional thin layer chromatography (TLC), the movement of the mobile phase is driven by capillary forces; in overpressured-layer chromatography (OPLC), by external pressure; and in rotational planar chromatography (RPC), by centrifugal force. Two main ...
Molecules
This article is an open access article distributed under the terms and conditions of the Creative... more This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY
Molecules
Solvent front position extraction procedure was used to prepare biological samples containing sel... more Solvent front position extraction procedure was used to prepare biological samples containing selected antihypertensive drugs (ramipril, lercanidipine, indapamide, valsartan, hydrochlorothiazide, perindopril, and nebivolol). Substances separated from the biological matrix components (bovine serum albumin) were quantified by means of liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Sample preparation process was performed with the use of a prototype horizontal chamber with a moving pipette driven by a 3D printer mechanism enabling a controlled eluent flow velocity. Application of this device was advantageous for simultaneous preparation of several samples for further quantitative analysis, with a synchronized reduction of manual operations and solvent consumption. Quantitative results obtained for the majority of the investigated antihypertensive drugs in a complex biological matrix were satisfactory. The values of the %RSD were around 5% for six of the seven s...
Molecules, 2021
The aim of this study was to conduct a histochemical analysis to localize lipids, terpenes, essen... more The aim of this study was to conduct a histochemical analysis to localize lipids, terpenes, essential oil, and iridoids in the trichomes of the L. album subsp. album corolla. Morphometric examinations of individual trichome types were performed. Light and scanning electron microscopy techniques were used to show the micromorphology and localization of lipophilic compounds and iridoids in secretory trichomes with the use of histochemical tests. Additionally, the content of essential oil and its components were determined using gas chromatography-mass spectrometry (GC-MS). Qualitative analyses of triterpenes carried out using high-performance thin-layer chromatography (HPTLC) coupled with densitometric detection, and the iridoid content expressed as aucubin was examined with spectrophotometric techniques. We showed the presence of iridoids and different lipophilic compounds in papillae and glandular and non-glandular trichomes. On average, the flowers of L. album subsp. album yielded ...
Croatica Chemica Acta, 2010
The chromatographic behavior of newly obtained derivatives of thiosemicarbazide and 1,2,4- triazo... more The chromatographic behavior of newly obtained derivatives of thiosemicarbazide and 1,2,4- triazoline-5-thione was determined. The lipophilicity was confirmed by the use of the Reversed Phase Thin-Layer Chromatography (RP-TLC) method. For both groups of solutes the lipophilicity depended on the substituents. All obtained compounds were tested for their antimycotic activity. The strongest antitu- berculosis activity was observed for 4-(2-iodophenyl)-1-(pyridine-4-ylacetyl)thiosemicarbazide 4 and 4- phenyl-3-(pyridine-4-ylmethyl)-1,2,4-triazoline-5-thione 27.
Scientific Reports
The separation of some water- and fat-soluble vitamins via micellar systems of reversed-phase hig... more The separation of some water- and fat-soluble vitamins via micellar systems of reversed-phase high-performance thin-layer chromatography (HPTLC) and pressurized planar electrochromatography (PPEC) was subjected to research. Hence, the influence of the mobile phase composition (surfactant and acetonitrile concentration, eluent buffer pH) on the migration distances and zone separation of some vitamins (thiamine, riboflavin, niacin, pyridoxine, cyanocobalamin, folic acid, ergocalciferol and α-tocopherol) was investigated. Our results indicated that the applied technique has an impact on the solute order. Comparing the system capacity of HPLC and PPEC (measured as height of the theoretical plate) for the mobile phase systems with and without surfactant shows differences, especially for fat-soluble vitamin. The variances and reproducibilities (% RDS) values of the vitamin are less in PPEC than in TLC. Moreover, the migration distances of water-soluble vitamins are longer than fat-soluble...
Thin Layer Chromatography in Chiral Separations and Analysis
Current Analytical Chemistry
Journal of Chromatography A
Molecules, Feb 17, 2022
This article is an open access article distributed under the terms and conditions of the Creative... more This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY
Journal of analytical methods in chemistry, 2016
The new mode of two-dimensional gradient thin layer chromatography (MGD-2D TLC) has been presente... more The new mode of two-dimensional gradient thin layer chromatography (MGD-2D TLC) has been presented. Short distance development of sample in the first dimension leads to formation of the preconcentrated narrow zones. They are consecutively separated in the second dimension with the mobile phase gradient in several steps of development until the eluent reaches the further end of the chromatographic plate. The use of the above-mentioned technique allows isolating and then identifying the compounds of various polarity from the multicomponent mixture. The practical application of two-dimensional gradient thin layer chromatography has been performed for isolation of the two plant (Juniperus and Thymus) oils components as the examples of test mixtures. The experiments have been carried out with the use of silica gel plates as well as a normal phase condition. The results of solute separation with isocratic one-dimensional thin layer chromatography system have been compared with those of twodimensional gradient system. It has been observed that application of the latter mode leads to almost triplicated number of zones in comparison with the former one. It is purposeful to apply the proposed mode to control the purity of the dominant component or components of the mixture.
Journal of Chromatography A, May 1, 2011
Theoretical backgrounds, development, examples of separations, constructional details and princip... more Theoretical backgrounds, development, examples of separations, constructional details and principle of action of devices of pressurized planar electrochromatography (PPEC) are presented. Development of the mode is described in respect of operating variables (composition of the mobile phase, pressure exerted on adsorbent layer, mobile phase flow velocity, temperature of separating system, etc.) influencing separation efficiency (kinetic performance, repeatability, separation time). Advantages of PPEC such as high kinetic performance, short separation time and different separation selectivities, especially relative to conventional thin-layer chromatography, are described. Examples of two-dimensional separations are demonstrated to show high separation potential of the mode when combined with conventional thin-layer chromatography (TLC). The PPEC mode is in infancy stage of development, so its challenges are presented as well.
Current Issues in Pharmacy and Medical Sciences
In this work, analysis of some drugs used in the treatment of neurodegenerative disorders (sulpir... more In this work, analysis of some drugs used in the treatment of neurodegenerative disorders (sulpiride, olanzapine, carbamazepine, trazodone, clomipramine, and pridinol) was achieved through micellar electrokinetic chromatography (MEKC). The effect of surfactant (sodium dodecylsulphate), acetonitrile, and buffer pH and concentration on the solute retention was also investigated. Successful separation of all compound mixtures was obtained. The method was applied for the quantitative analysis of investigated compounds, and the LOD and LOQ were determined. The LOD values were in the range from 0.0127 mg/mL for clomipramine, to 0.1398 mg/mL for pridinol, while LOQ were in the range 0.0384 mg/mL for clomipramine, to 0.4237 for pridinol. The mode was also applied for the determination of investigated solutes in pharmaceutical prescriptions.
Current Issues in Pharmacy and Medical Sciences
Separation of some isoquinoline alkaloids (narcotine, chelidonine, dihydrocodeine, cinchonine, be... more Separation of some isoquinoline alkaloids (narcotine, chelidonine, dihydrocodeine, cinchonine, berberine, cinchonidine, papaverine, apomorphine) has been investigated with pressurized planar electrochromatography (PPEC) and high-performance thin-layer chromatography (HPTLC) in reversed-phase systems. The mobile phase consisted of acetonitrile and aqueous buffer (disodium phosphate and citric acid). The influence of the mobile phase buffer pH on migration distance (PPEC) and retardation factor (HPTLC) of the solutes has been investigated and compared. The results show different separation selectivity in both PPEC and HPTLC systems especially at pH range of buffer solution of the mobile phase that facilitates ionization of the solutes investigated.
Chromatographia, 2006
The enantiomers of some amino acids have been separated on commercial chiral TLC plates in revers... more The enantiomers of some amino acids have been separated on commercial chiral TLC plates in reversed-phase mode. The effect of the pH* of the aqueous-organic mobile phase on the retention and mobility of the enantiomers and on selectivity was investigated. It was shown that for most of the amino acids investigated the highest enantioselectivity was obtained at pH* 3-4 or 6-7. The drift and disturbance of the baseline on the chromatograms were also much smaller at pH* 3-4 and 6-7.
Current Issues in Pharmacy and Medical Sciences
Eight drugs blocking beta-adrenergic receptors activity (acebutolol, alprenolol, atenolol, oxpren... more Eight drugs blocking beta-adrenergic receptors activity (acebutolol, alprenolol, atenolol, oxprenolol, labetalol, metoprolol, propranolol and sotalol) were investigated through the use of the thin-layer technique with its mobile phase containing surfactant. Assessment of the effect of surfactant presence and 1-propanol concentration in the mobile phase on the retention and separation of investigated solutes was then carried out wherein the effect of the surfactant concentration on the zone shape properties (asymmetry and tailing coefficient) was investigated. The method was applied for the quantitative analysis of the chosen solutes, and the LOD and LOQ values of chosen were determined. These were as follows: acebutolol – 1.11 and 3.36 μg/spot, metoprolol 1.45 μg/spot, 4.4 μg/spot. The chosen system is environmentally friendly due to using silica gel plates and only 5% of propanol in water.
Chromatographia, 1993
Equations for the final R F values for mobile phase gradient development and gradient multiple de... more Equations for the final R F values for mobile phase gradient development and gradient multiple development are presented. Computer simulations of gradient development for both modes of thin-layer chromatography are discussed for the preliminary optimization of gradient programs.
Applications, Theory and Instrumentation, 2011
In conventional thin layer chromatography (TLC), the movement of the mobile phase is driven by ca... more In conventional thin layer chromatography (TLC), the movement of the mobile phase is driven by capillary forces; in overpressured-layer chromatography (OPLC), by external pressure; and in rotational planar chromatography (RPC), by centrifugal force. Two main ...
Molecules
This article is an open access article distributed under the terms and conditions of the Creative... more This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY
Molecules
Solvent front position extraction procedure was used to prepare biological samples containing sel... more Solvent front position extraction procedure was used to prepare biological samples containing selected antihypertensive drugs (ramipril, lercanidipine, indapamide, valsartan, hydrochlorothiazide, perindopril, and nebivolol). Substances separated from the biological matrix components (bovine serum albumin) were quantified by means of liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Sample preparation process was performed with the use of a prototype horizontal chamber with a moving pipette driven by a 3D printer mechanism enabling a controlled eluent flow velocity. Application of this device was advantageous for simultaneous preparation of several samples for further quantitative analysis, with a synchronized reduction of manual operations and solvent consumption. Quantitative results obtained for the majority of the investigated antihypertensive drugs in a complex biological matrix were satisfactory. The values of the %RSD were around 5% for six of the seven s...
Molecules, 2021
The aim of this study was to conduct a histochemical analysis to localize lipids, terpenes, essen... more The aim of this study was to conduct a histochemical analysis to localize lipids, terpenes, essential oil, and iridoids in the trichomes of the L. album subsp. album corolla. Morphometric examinations of individual trichome types were performed. Light and scanning electron microscopy techniques were used to show the micromorphology and localization of lipophilic compounds and iridoids in secretory trichomes with the use of histochemical tests. Additionally, the content of essential oil and its components were determined using gas chromatography-mass spectrometry (GC-MS). Qualitative analyses of triterpenes carried out using high-performance thin-layer chromatography (HPTLC) coupled with densitometric detection, and the iridoid content expressed as aucubin was examined with spectrophotometric techniques. We showed the presence of iridoids and different lipophilic compounds in papillae and glandular and non-glandular trichomes. On average, the flowers of L. album subsp. album yielded ...
Croatica Chemica Acta, 2010
The chromatographic behavior of newly obtained derivatives of thiosemicarbazide and 1,2,4- triazo... more The chromatographic behavior of newly obtained derivatives of thiosemicarbazide and 1,2,4- triazoline-5-thione was determined. The lipophilicity was confirmed by the use of the Reversed Phase Thin-Layer Chromatography (RP-TLC) method. For both groups of solutes the lipophilicity depended on the substituents. All obtained compounds were tested for their antimycotic activity. The strongest antitu- berculosis activity was observed for 4-(2-iodophenyl)-1-(pyridine-4-ylacetyl)thiosemicarbazide 4 and 4- phenyl-3-(pyridine-4-ylmethyl)-1,2,4-triazoline-5-thione 27.
Scientific Reports
The separation of some water- and fat-soluble vitamins via micellar systems of reversed-phase hig... more The separation of some water- and fat-soluble vitamins via micellar systems of reversed-phase high-performance thin-layer chromatography (HPTLC) and pressurized planar electrochromatography (PPEC) was subjected to research. Hence, the influence of the mobile phase composition (surfactant and acetonitrile concentration, eluent buffer pH) on the migration distances and zone separation of some vitamins (thiamine, riboflavin, niacin, pyridoxine, cyanocobalamin, folic acid, ergocalciferol and α-tocopherol) was investigated. Our results indicated that the applied technique has an impact on the solute order. Comparing the system capacity of HPLC and PPEC (measured as height of the theoretical plate) for the mobile phase systems with and without surfactant shows differences, especially for fat-soluble vitamin. The variances and reproducibilities (% RDS) values of the vitamin are less in PPEC than in TLC. Moreover, the migration distances of water-soluble vitamins are longer than fat-soluble...
Thin Layer Chromatography in Chiral Separations and Analysis
Current Analytical Chemistry
Journal of Chromatography A