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1

Application of mobile phases containing ionic liquid for the analysis of selected psychotropic drugs by HPLC–DAD and HPLC–MS

Petruczynik A., Wróblewski K., Waksmundzka-Hajnos M.

Acta Chromatographica

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2019

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Vol. 31, no. 4

255--261

EN

In reversed-phase liquid chromatography, in case of the absence of additives, cationic basic compounds give rise to asymmetrical and broad peaks as a result of interactions of analyte cations with residual free silanols on silica-based stationary phases. Ionic liquids, added to the mobile phase, have been suggested as alternatives to amines to block the activity of free silanols. The different parameters affecting the retention behavior, symmetry of peak, system efficiency, and separation selectivity of selected psychotropic drugs, especially the effect of concentration of ionic liquid, kind and concentration of organic modifiers of mobile phases, and kind of stationary phases were investigated. The most selective and efficient systems are used for separations of psychotropic drug standards' mixture and for determination of selected psychotropic drugs in human serum.

2

Techniki sprzężone i miniaturyzacja gwarancją rozwoju chemii analitycznej

Waksmundzka-Hajnos M., Garniewska A.

Laboratorium - Przegląd Ogólnopolski

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2018

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nr 2

12--13

PL

Rozmowa z prof. dr hab. n. farm. Moniką Waksmundzką-Hajnos, kierownik Zakładu Chemii Nieorganicznej Uniwersytetu Medycznego w Lublinie, przewodniczącą Komitetu Organizacyjnego X Polskiej Konferencji Chemii Analitycznej odbywającej się pod hasłem „Od chemii wszystko się zaczyna”.

3

Determination of vortioxetine in human serum and saliva samples by HPLC–DAD and HPLC–MS

Wróblewski K., Petruczynik A., Buszewski B., Szultka-Młyńska M., Karakuła-Juchnowicz H., Waksmundzka-Hajnos M.

Acta Chromatographica

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2017

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Vol. 29, no. 3

325--344

EN

Vortioxetine is a new drug against major depressive disorder with high affinity for a range of different serotonergic targets in the central nervous system. Therapeutic drug monitoring is an important tool for the clinical management of patients receiving a pharmacotherapy, particularly in psychiatry. For this reason, determination of drug concentration in biological fluids is important for a rational dosage of drugs. Rapid and reliable analytical assays are also required to detect and identify drugs of toxicological importance. For analysis of vortioxetine by high-performance liquid chromatography (HPLC), no procedures for its determination in saliva have been reported and there are only a few ones for its determination in serum. A sensitive and selective highperformance liquid chromatography with diode array detector (HPLC-DAD) or mass spectrometer (HPLC-MS) method was developed for the fast quantification of vortioxetine in human saliva and serum. The determination was performed on a Synergi Polar RP column in isocratic mode under the optimal mobile phase containing 70% methanol, 20% acetate buffer at pH 3.5, 10% double distilled water, and 0.025 M L−1 diethylamine.

4

Determination of selected antiepileptic drugs in mouse brain homogenates by HPLC—DAD

Wróblewski K., Petruczynik A., Radzik I., Czuczwar S. J., Waksmundzka-Hajnos M.

Acta Chromatographica

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2017

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Vol. 29, no. 2

219--234

EN

Three independent reversed phase high-performance liquid chromatography (HPLC) procedures with diode array detection (DAD) for the analysis of carbamazepine (CBZ), topiramate (TPM), and valproic acid (VPA) have been developed in order to determine drug penetration of the blood—brain barrier. Determination of CBZ was performed on C18 column with mobile phases containing methanol (55%, v/v), acetate buffer at pH 3.5 (20%, v/v), double distilled water (25%, v/v), and 0.025 M L−1 diethylamine (DEA). The mobile phase containing acetonitrile and water (8:2, v/v) or acetonitrile and phosphate—citrate buffer at pH 2.6 (1:1), respectively, for analysis of VPA and TPM was applied. Quantification of carbamazepine was performed at 285 nm without extraction procedure before the analysis. Determination of topiramate and valproic acid was performed using precolumn derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl). FMOC-Cl is a suitable agent, which reacts with both primary and secondary amines and also with acidic groups. Topiramate was determined at 263 nm and valproic acid at 300 nm. The proposed procedures are simple, not time-consuming, and suitable for the determination of investigated compounds in mouse brain homogenates.

5

Micro-2D-TLC separation of phenolics in some species of mint and their fingerprints on diol bonded polar stationary phase

Hawrył M. A., Niemiec M., Słomka K., Waksmundzka-Hajnos M., Szymczak G.

Acta Chromatographica

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2016

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Vol. 28, no. 1

119--127

EN

Micro thin- layer chromatography in two dimensional (2D-mTLC) mode in normal and reversed phase systems by use of diol bonded stationary phase was applied to make fingerprints of 11 species of Mentha genus and two finished pharmaceutical products. Nonaqueous eluents (propan-2-ol or ethyl acetate dissolved in n-heptane) were used in normal phase systems. Mixtures of acetonitrile with water were used in reversed phase chromatographic systems. Optimization of one dimensional systems was performed by determining of RF vs. composition of mobile phases dependencies for standards occurring in various species of Mentha. Most selective eluents were chosen to optimize two-dimensional systems by creating RF in normal-phase (NP) systems vs. RF in reversed-phase (RP) systems correlations. 2D-mTLC on diol polar bonded stationary phase were optimized to separate phenolic compounds and make fingerprints of examined plant materials and this method was never applied earlier in the chromatographic analysis.

6

A Comparison of Antioxidant, Antibacterial, and Anticancer Activity of the Selected Thyme Species by Means of Hierarchical Clustering and Principal Component Analysis

Orłowska M., Pytlakowska K., Mrozek-Wilczkiewicz A., Musioł R., Waksmundzka-Hajnos M., Sajewicz M., Kowalska T.

Acta Chromatographica

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2016

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Vol. 28, no. 2

207--221

EN

In this study, six numerical data sets are presented valid for eighteen thyme (Thymus L.) species and characterizing three biological properties of these herbs, i.e., antioxidant, antibacterial, and anticancer activity. Four data sets characterize antioxidant properties, one data set characterizes antibacterial property, and one data set characterizes anticancer activity. Antioxidant properties were measured with two free radical standards (DPPH and ABTS), two free radical scavenger standards (trolox and gallic acid), and three analytical techniques (EPR spectroscopy, ultraviolet–visible [UV–vis] spectrophotometry, and the dot blot test with bioautographic detection). Antibacterial activity was tested upon the Gram-positive Bacillus subtilis (ATCC 6633) strain, and anticancer activity was evaluated upon the human colon adenocarcinoma cells (HCT116). It was found out that the thyme extracts characterize with all three biological activities (yet with anticancer activity not very strongly pronounced) and that in quantitative terms, each activity strongly depends on the thyme species considered. An ultimate goal of this study was to investigate if any quantitatively confirmed correlation exists among these three biological activities, which might point out to a common mechanism of their action. To this effect, six sets of numerical data underwent hierarchical clustering and Principal Component Analysis. Based on the results obtained, no quantitative correlation was established among antioxidant, antibacterial, and anticancer activity of the thyme species, which seems indicative of different molecular mechanisms of these three actions.

7

Comparison of Matrix Solid-Phase Dispersion and Liquid—Solid Extraction Methods Followed by Solid-Phase Extraction in the Analysis of Selected Furanocoumarins from Pimpinella Roots by HPLC—DAD

Oniszczuk A., Waksmundzka-Hajnos M., Podgórski R., Nowak R., Żukiewicz-Sobczak W., Blicharski T.

Acta Chromatographica

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2015

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Vol. 27, no. 4

687--696

EN

The use of matrix solid-phase dispersion (MSPD) was tested to extract some coumarins (umbelliferone, xanthotoxin, isopimpinellin, bergapten, and pimpinellin) from Pimpinella roots. The method was compared with liquid—solid extraction methods (LSE) such as accelerated solvent extraction (ASE), ultrasound-assisted extraction (USAE) and Soxhlet extraction followed by solid-phase extraction (SPE). Several methanol concentrations and temperature conditions were examined during the liquid—solid extraction techniques. The analysis was performed by high-performance liquid chromatography with diode array detector (HPLC—DAD). MSPD extracted furanocoumarins with satisfactory recoveries ranging from 91.65% to 97.55% and relative standard deviations lower than 5,0415%. The results presented in the paper reveal that MSPD is an efficient, fast, simple and easy-to-perform method suitable for the isolation of furanocoumarins from herbs.

8

Simultaneous HPLC determination of pomolic, ursolic and euscaphic/tormentic acids in roots and rhizomes of various Potentilla species

Jóźwiak A., Jóźwiak G., Waksmundzka-Hajnos M.

Acta Chromatographica

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2014

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Vol. 26, no. 1

97--110

EN

A reversed-phase high-performance liquid chromatography diode array detector (HPLC-DAD) method was developed for the separation of triterpene acids and their determination in crude extracts of Potentilla species. Symmetry octadecylsilyl silica (ODS) column with acetonitrile and water with phosphoric acid (pH = 2.5) as the mobile phase was used in the described HPLC system. The column temperature was at 20 °C, the flow rate was 0.8 mL/min. The detection wavelength was 210 nm. For quantitative purposes, the linear dependencies of analyte concentration and peak surface area were obtained with regression coefficient values 0.9983 < r2 < 0.9995. For euscaphic acid, calibration was performed in the range of 0.07–0.525; 0.7–2.1 mg/mL, for pomolic acid in the range of 0.019–0.171; 0.209–0.665 mg/mL, for ursolic acid in the range of 0.2–1.375–3.3 mg/mL. The observed recovery of triterpene acids was from 95.3% to 103.1%. The observed values of RSD were well within the generally acceptable limit of no more than 5%. This method was successfully applied to quantify pomolic acid (PA), ursolic acid (UA) and the sum of euscaphic (EA) and tormentic acids (TA) (expressed as euscaphic acid) in roots and rhizomes of 15 various Potentilla species and 2 subspecies (i.e., P. atrosanguinea, P. recta).

9

Determination of some psychotropic drugs in human plasma by HPTLC

Wróblewski K., Petruczynik A., Waksmundzka-Hajnos M.

Acta Chromatographica

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2014

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Vol. 26, no. 2

297--307

EN

Psychotropic drugs: desipramine, olanzapine and mitrazapine were chromatographed on cyanopropyl-silica and Diol-silica thin layers using various nonaqueous and aqueous eluents.The best results were obtained with addition of ammonia to nonaqueous eluent on both adsorbents. On the basis of the optimization, systems for extraction from human plasma and quantitative determination of investigated drugs were selected.RP18 encaped SPE columns conditioned and pre-eluted with acetonitrile:water:ammonium buffer at pH 8.6 (5:5:2) and eluted with methanol:water (9:1) containing 2% acetic acid were used for sample preparation with high recoveries of all investigated drugs. Diol and CN plates with mixture of 15% methanol in diisopropyl ether + 1% ammonia were used for quantitative analysis by a calibration curve method.

10

Influence of sample preparation methods on the quantitation of selected tropane alkaloids from herb of Datura innoxia mill. by HPTLC

Oniszczuk A., Waksmundzka-Hajnos M., Gadzikowska M., Podgórski R., Oniszczuk T.

Acta Chromatographica

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2013

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Vol. 25, no. 3

545--554

EN

The aim of our paper was the examination of various procedures of extraction and purification methods on the yield of atropine and scopolamine in Datura innoxia extracts determined by high-performance thin-layer chromatography (HPTLC). In our experiments, the following extraction methods were used: percolation, ultrasound-assisted extraction (USAE) at various temperatures, and microwave-assisted extraction (MASE). The highest extraction yields of atropine and scopolamine were obtained by ultrasound-assisted extraction method and aqueous acetic acid or aqueous tartaric acid used as extractants. Crude extracts of D. innoxia herb were purified by use of various methods: solid-phase extraction-strong cation exchanger (SPE-SCX), SPE-C18, and liquid-liquid extraction (LLE). The best results of purification with satisfactory %RSD values were obtained by liquid-liquid extraction by use of dichloromethane from aqueous crude alkaloid extract alkalized to pH 12. HPTLC was performed on pre-coated plates Kieselgel 60 F254 in horizontal DS chambers by use of mobile phase: methanol-acetone-aqueous ammonia (5:4.5:0.5). The alkaloids’ content was determined in extracts by use of calibration curve method for atropine and scopolamine. Calibration curves were linear in range of 3.0–30 μg for scopolamine (R = 0.9980) and 2.6–26 μg for atropine (R = 0.9923). Limits of detection (LOD) and limits of quantification (LOQ) were 1.12 μg and 3.42 μg per spot for scopolamine and 0.89 μg and 2.82 μg per spot for atropine.

11

Application of hydrophilic interaction chromatography in phytochemical analysis

Petruczynik A., Waksmundzka-Hajnos M.

Acta Chromatographica

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2013

|

Vol. 25, no. 1

1--25

EN

Hydrophilic interaction chromatography (HILIC) is a liquid chromatography technique when a polar stationary phases - silica or polar bonded phases and aqueous mobile phase containing amount of a less polar solvent (often acetonitrile) is applied. HILIC is important for the separation of highly polar substances including biologically active compounds, such as drugs, amino acids, peptides, proteins, nucleosides, neurotransmitters, etc. HILIC is also the appropriate method for analysis of plant extract polar components such as carbohydrates, amino acids, peptides, phenolic acids, flavonoids and some alkaloids. Plant extracts are usually multicomponent mixtures of compounds of wide polarity range, which often cannot be analyzed by use of a single separation and detection method because of the high chemical diversity. Good results are obtained by use of coupled method, e.g., reversed-phase liquid chromatography (RP-LC) and HILIC mode separation. The elution order in HILIC is usually opposite to that in RP separations. This orthogonality determines one of the advantages of HILIC - the possibility of creating multidimensional separations. An important feature of HILIC is the improved sensitivity with electrospray mass spectrometry. This is significant for the analysis of components existing in small concentration in multicomponent mixtures. The high acetonitrile content also gives additional advantage of HILIC - faster separations due to the lower viscosity of HILIC eluents compared to standard RP ones. The presented review deals with the optimization of HILIC separations and application of the method for analysis of plant extracts components.

12

Wpływ rodzaju i parametrów ekstrakcji na wydajność izolacji wybranych furanokumaryn z owoców gorysza wyniosłego (Peucedanum verticillare)

Waksmundzka-Hajnos M., Oniszczuk A., Podgórski R.

Camera Separatoria

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2012

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Vol. 4, No. 1

83--91

PL

Analiza materiału roślinnego jest ważnym zadaniem w poszukiwaniu roślin o działaniu farmakologicznym a także w standaryzacji leków roślinnych. Celem każdego procesu ekstrakcji jest szybka i skuteczna izolacja związków z matrycy przy użyciu minimalnej ilości rozpuszczalnika. Celem przedstawionej pracy był wybór optymalnych warunków do analizy materiału roślinnego oraz zbadanie wpływu metody ekstrakcji na wydajność izolacji niektórych furanokumaryn z owoców gorysza wyniosłego. Furanokumaryny mają istotne zastosowanie w lecznictwie. Są między innymi wykorzystywane w terapii bielactwa i łuszczycy oraz leczeniu skórnego T-komórkowego chłoniaka z erytmodermią. Zastosowano następujące metody ekstrakcyjne: wyczerpująca ekstrakcja w aparacie Soxhleta, ekstrakcja wspomagana ultradźwiękami w temperaturze 20 i 60◦C oraz ekstrakcja wspomagana mikrofalami w układzie otwartym i zamkniętym. Analiza została przeprowadzona metodą wysokosprawnej chromatografii cieczowej z detektorem UV/VIS. Wyniki wskazują, że najwyższą wydajność imperatoryny uzyskano w wyniku ekstrakcji ultradźwiękowej 60◦C, natomiast metodą najskuteczniejszą do izolacji umbeliferonu okazała się ekstrakcja mikrofalowa w układzie zamkniętym.

EN

Analysis of plant material is an important task in chemotaxonomical investigations, particularly, in search of plants with pharmacological activity or in standardisation of plant drugs. The goal of every extraction process is rapid and effective isolation of compounds from a matrix by use of minimum amount of solvent. The aim of this paper was the choice of optimal condi-tions for the analysis of plant material and effect of extraction method on the yield of some furanocoumarins from Peucedanum verticillare fruits. Furanocoumarins have important uses in human medicine and exhibit toxicity against a wide range of organisms. This group of com-pounds reveal pharmacological activity. They are important drugs in vitiligo and psoriaris therapy and are also used in therapy erythrodermic variants of cutaneous T-cell lymphoma and chronic graft-versus-host disease. The following extraction methods were used in our experiments: exhaustive extraction in Soxh-let apparatus, ultrasound- assisted solvent extraction (USAE) at 20 and 60◦C as well as micro-wave-assisted solvent extraction in open and closed system (MASE). Target compounds analysis was performed by high performance liquid chromatography with UV/VIS detector. The results indicated that, the highest yield of imperatorin can be obtained by ultrasonification at 60◦C, while microwave-assisted solvent extraction in closed system is very efficient in the extraction of umbelliferone.

13

Determination of the lipophilicity of some new thiosemicarbaside derivatives by reversed-phase thin-layer chromatography

Hawrył A., Kuśmierz E., Pisarczyk P., Wujec M., Waksmundzka-Hajnos M.

Acta Chromatographica

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2012

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Vol. 24, no. 2

271--290

EN

In this study, the chromatographic behavior of a newly synthesized series of 1,4-disubstituted thiosemicarbazide derivatives and products of their dehydrocyclization is presented. These compounds have been subjected to this study because they exhibit antimicrobial activity. The compounds have been chromatographed on RP-18 and on cyano-bonded silica chromatographic phases with eluents containing water and an organic modifier (methanol, dioxane, acetone, acetonitrile or tetrahydrofuran) of various concentrations. Statistically proved linear relationships between the retention parameter (RM) and the concentration of organic modifier in the mobile phase allow the extrapolation procedure to obtain RM0 for investigated compounds. The correlations between both the values of the intercept (RM0 ) and the slope (S) from the linear equation, taken as a measure of the lipophilicity, were calculated. The experimentally established parameters of lipophilicity (RM0 ) were compared with the log P values calculated by use of four different software packages. The values of the correlation coefficients of these relationships are higher for the cyanopropyl phase than for RP-18. Moreover, in this work the influences of different mobile phase modifiers and adsorbent layers on experimentally obtained lipophilicity parameters were analyzed and compared. Generally, the best correlations were obtained for systems with the cyanopropyl-bonded stationary phase in comparison with RP-18.

14

Profesor Andrzej Waksmundzki 1910-1998

Waksmundzka-Hajnos M.

Analityka : nauka i praktyka

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2011

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nr 1

74-79

15

Exploration of the possibility of combined HS-GC-MS and 13C NMR spectroscopic investigation of the composition of the essential oils of selected sage (Salvia) species

Sajewicz M., Matlengiewicz M., Rzepa J., Wojtal Ł., Hajnos M., Waksmundzka-Hajnos M., Kowalska T.

Acta Chromatographica

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2011

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Vol. 23, no. 1

181--190

EN

The objective of this study was to explore the possibility of combining headspace gas chromatography with mass spectrometric detection (HS-GC-MS) and 13C NMR spectroscopy to enhance the detectability of components of the essential oils of medicinal plants of the Salvia genus. Preliminary investigations were performed with two sage species, Salvia lavandulifolia and Salvia triloba, known for particularly abundant yields of their respective essential oils. By use of HS-GC-MS, characteristic fingerprints of the volatile fractions were obtained for plant species from two different vegetation seasons (2007 and 2008). Partial identification of the components of these volatile fractions was performed, and comparison of the chromatographic fingerprints confirmed seasonal fingerprint similarity within the same species. Preliminary 13C NMR measurements resulted in well shaped spectra with an abundance of regularly distributed signals. This suggested the possibility of using 13C NMR spectroscopy in phytochemical research, in parallel with HS-GC-MS, to enhance the detectability of volatile components of plant species belonging to this genus.

16

Chromatografia cienkowarstwowa jako technika kontroli jakości surowców roślinnych

Cieśla Ł., Waksmundzka-Hajnos M.

Analityka : nauka i praktyka

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2010

|

nr 2

54-58

PL

Ocena ilościowa składu surowca jest nieodłącznym elementem badania surowców farmakognostycznych, gdyż odpowiednia ilość określonych ciał czynnych zapewnia wartość leczniczą danego surowca.

17

RP-HPTLC determination of the lipophilicity of some new derivatives of thiosemicarbazide and 1,2,4-triazole of sulphanylacetic acid

Hawrył A., Popiołek Ł, Dobosz M., Pikuła E, Waksmundzka-Hajnos M.

Acta Chromatographica

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2010

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Vol. 22, no. 1

37--55

EN

Some new derivatives of thiosemicarbazide and the 1,2,4-triazole of sulphanylacetic acid have been chromatographed on RP-18 HPTLC plates with mobile phases containing water and an organic modifier (methanol, dioxane, acetone, 2-propanol, or tetrahydrofuran). Relationships between solute retention and modifier concentration were described by Snyder’s linear equation. The equation was used to determine R M 0 values, by extrapolation, and the S values denoting the slopes of the relationship between linear retention and mobile phase concentration; both values characterize the lipophilicity of the substances. Calculated values of R M 0 were correlated with log P values for the drugs investigated by use of the software HyperChem. Correlations between intercept ( R M 0 ) and slope ( S ) from the linear equations were also calculated. The effects of different mobile phase modifiers on experimentally obtained lipophilicity were also analysed and compared.

18

Effect of the vapour phase on the TLC separation of tropane alkaloids

Gadzikowska M., Jóźwiak G. W., Waksmundzka-Hajnos M.

Acta Chromatographica

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2010

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Vol. 22, no. 4

515--525

EN

The effect of conditioning the silica layer by mobile phase vapour or ammonia vapour on the retention of alkaloids eluted with non-aqueous mobile phases was examined. The effect of vapour phase composition on system efficiency, peak symmetry, and separation selectivity were also investigated. The most effective and selective systems were used for separation of the alkaloid fraction of Datura innoxia.

19

Effect of the vapour phase on the separation of isoquinoline alkaloids by thin-layer chromatography

Petruczynik A., Śliwka K., Waksmundzka-Hajnos M.

Acta Chromatographica

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2010

|

Vol. 22, no. 3

391--404

EN

The effect of conditioning of the silica layer by mobile phase vapour, diethylamine vapour and its aqueous and methanolic solutions, and ammonia vapour on the retention of alkaloids eluted with multicomponent non-aqueous mobile phases was examined. Effect of conditioning time and vapour phase composition on system efficiency and peak symmetry was investigated, as also was the effect of vapour phase composition on separation selectivity. The most effective and selective systems were used for separation of the alkaloid fraction from Fumaria officinalis.

20

Multidimensional TLC procedure for separation of complex natural mixtures spanning a wide polarity range; Application for fingerprint construction and for investigation of systematic relationships within the Peucedanum genus

Cieśla Ł., Skalicka-Woźniak K., Hajnos M., Hawrył M., Waksmundzka-Hajnos M.

Acta Chromatographica

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2009

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Vol. 21, no. 4

641--657

EN

Identification of closely related plant species is not a trivial task, and is often difficult on the basis of morphological or anatomical features. To differentiate among analyzed species, a chromatographic fingerprint is usually constructed. This is not easy for very complex samples, however, especially those containing substances spanning a wide polarity range. In such circumstances more than one fingerprint is constructed, e.g. one for polar and the other for apolar constituents. In this paper a new method has been used for resolution of a mixture of 17 coumarins and flavonoids and, subsequently, construction of a fingerprint of closely related species belonging to the Peucedanum genus. This is the first time multidimensional planar chromatography has been applied for such purpose. Distinctive fingerprints are produced for every analyzed plant species, without the need to construct two fingerprints and without the application of more sophisticated multidimensional methods (e.g. hyphenation of HPLC and TLC, HPLC-MS, etc).