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The derivatization and analysis of anticancer pharmaceuticals in the presence of tricyclic antidepressants by gas chromatography

Haliński Ł., Śmigiel D., Czerwicka M., Paszkiewicz M., Kumirska J., Stepnowski P.

Acta Chromatographica

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2014

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Vol. 26, no. 3

473--484

EN

The evaluation of several derivatization procedures for the gas chromatographic analysis of selected anticancer pharmaceuticals (cyclophosphamide, iphosphamide, flutamide, chlorambucil, and melphalan) in the presence of tricyclic antidepressants was carried out. Among the methods, concerning trimethylsilylation, tert-butyldimethylsilylation, and methylation, the most useful was methylation using (trimethylsilyl)diazomethane (TMSD), which is a safe alternative for the common reaction with diazomethane. Most of the anticancer drugs were unstable during derivatization using silylating agents, while antidepressants were stable in all tested conditions. Melphalan was the only compound, for which the results of all tested procedures were not satisfying. The TMSD-based procedure was validated, giving the results possibly suitable for the screening purposes in contaminated environmental samples.

2

Spektrometria mas - uniwersalna technika analityczna

Czerwicka M., Kumirska J., Stepnowski P.

Laboratorium - Przegląd Ogólnopolski

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2012

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nr 5-6

20--22

PL

Spektrometria mas jest jedną z najpopularniejszych technik analitycznych. Umożliwia ona analizę jakościową i ilościową zarówno prostych związków, jak i wysokocząsteczkowych biomolekuł, a dzięki połączeniu spektrometrii mas z technikami chromatograficznymi także analizę skomplikowanych mieszanin. Najważniejsze aspekty tej techniki zostaną zaprezentowane w niniejszej pracy.

EN

Mass spectrometry is one of the most popular analytical technique. It enables quantitative and qualitative analyses of both simple compounds and high-molecular biomolecules. By means of combination of mass spectrometry with chromatographic techniques also analysis of the complicated mixtures is possible. The most important aspects of this technique will be presented in this article.

3

Współczesne metody ekstrakcji, izolacji i analizy metabolitów wtórnych roślin

Haliński Ł. P., Czerwicka M., Stepnowski P.

LAB Laboratoria, Aparatura, Badania

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2010

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R. 15, nr 6

16-21

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Chemical Structure of the Salmonella Anatum (O:3,10) O-antigen

Gajdus J., Kaczyński Z., Czerwicka M., Dziadziuszko H., Szafranek J.

Polish Journal of Chemistry

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2008

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Vol. 82, nr 7

1393-1393

EN

An O-specific polysaccharide containing D-galactose, D-mannose and L-rhamnose was obtained by mild acid hydrolysis of the lipopolysaccharide of the Salmonella Anatum bacterium. The structure of the polymeric O-antigen was studied by composition analysis and by 1D and 2D, 1H and 13C NMR spectroscopy. The repeating unit of the polymer was identified as a linear trisaccharide with the structure shown below, in which the galactose residue was partially O-ac ety lat ed at C-6; this was re spon si ble for the mol e cule’s structural heterogeneity. → 3)-D-Galp-(1𔾺)-D-Manp-(1𔾸)-alfa-L-Rhap-(1→ 6 OAc (75%).

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Repeating Unit Structure of Enterobacter sakazakii ZORB A 741 O-Polysaccharide

Szafranek J., Czerwicka M., Kumirska J., Paszkiewicz M., Łojkowska E.

Polish Journal of Chemistry

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2005

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Vol. 79 / nr 2

287-295

EN

The O-specific polysaccharide from Enterobacter sakazakii cell was isolated and structurally characterized. Lipopolysaccharide (LPS) was obtained from cell mass by hot phenol- water extraction procedure. Mild acid hydrolysis followed by gel filtration provided pure O-antigen (OPS). Two-stage sugar analysis detected tyvelose, rhamnose and galactose in the molar ratio of 1:1:2, and their linkages were established by means of methylation analysis. Sugar configurations, D or L, were determined by gas-liquid chromatography on an achiral liquid phase for (S)-(+)-2-butyl glycosides. D configuration was determined for galactose and 3,6-dideoxy-mannose (tyvelose), but L for rhamnose. Repeating unit structure was deduced by analysis of 1H and 13C NMR spectra. 1H and 13C NMR resonances have been assigned by homonuclear (COSY, TOCSY) and heteronuclear (HSQC, HMBC) correlations spectra. Anomeric configurations were determined from anomeric proton chemical shifts and 3JH1-H2 and JC-H coupling constants. Sugar sequences were established from comparisons of specific carbon chemical shifts with those in literature, two-dimensional nuclear Overhauser effect spectroscopy (NOESY), and heteronuclear multiple-bond correlation experiments (HMBC). The repeating unit structure of Enterobacter sakazakii was found to be as: alfa-Tyvp _2 _3)-alfa-L-Rhap-(1--3)-alfa-D-Galp-(1_3)-alfa-D-Galp-(1_ _6 O-Ac

6

Structure of the Polysaccharide O-Antigen of Salmonella Aberdeen (O : 11)

Szafranek J., Kaczyńska M., Kaczyński Z., Gajdus J., Czerwicka M., Dziadziuszko H., Głośnicka R.

Polish Journal of Chemistry

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2003

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Vol. 77 / nr 9

1135-1140

EN

O-specific polysaccharide (OPS) of Salmonella Aberdeen was obtained from bacterial cell mass by water-phenol extraction procedure of lipopolysaccharide (LPS) followed by its mild acid hydrolysis and gel filtration of soluble carbohydrate material. Rhamnose, galactose, N-acetyl-glucosamine and mannose were detected and their linkages were established. Sugar configurations, D or L, were determined for (S)-(+)-2-butyl glycosides on an achiral capillary column. The structure of OPS was determined by analysis of spectra of 1H and 13C NMR and homonuclear and heteronuclear correlations spectra. Anomeric configurations were tentatively assigned by chromium trioxide oxidation and later proved by anomeric proton chemical shifts, H1-H2 coupling constants and proton coupled 13C spectra. Sugar sequences were established from comparisons of specific carbon shifts with those from literature, two-dimensional nuclear Overhauser effect spectroscopy (NOESY) and heteronuclear multiple-bond correlation experiments (HMBC). The repeating unit of S. Aberdeen OPS has the structure: _3)-_-D-GlcpNAc-(1_3)-[ _-D-Manp-(1_4)-]_-D-Galp-(1_4)-_-L-Rhap-(1_