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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

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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.

2

Determination of the lipophilicity of selected isoquinoline alkaloids by RP-TLC

Waksmundzka-Hajnos M., Matosiuk D., Petruczynik A., Kijkowska-Murak U.

Acta Chromatographica

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2008

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Vol. 20, no. 4

563-573

EN

Nine alkaloids were chromatographed by reversed phase (RP) TLC on RP-18 with aqueous acetone or aqueous dioxane mobile phases. A variety of mobile phase additives (ammonia, diethylamine (DEA), tetrabutylammonium chloride (TBA-Cl)) were used to suppress ionization of the alkaloids and/or reduce ionic interactions with surface silanol groups. Ion-pair (IP) RP-TLC was also performed with aqueous acetone mobile phases and reagents such as pentane sulphonic acid (PSA), octane sulphonic acid (OSA), or di-(2-ethylhexyl)orthophosphoric acid (HDEHP) as mobile phase additives. In these systems retention of the alkaloids was determined using mobile phases with different modifier concentrations. Relationships between R M and modifier concentration were sought. A linear semilogarithmic equation was fitted to experimental data and used to obtain lipophilicity values R MW ( R M for pure water), the slope ( S ), and φ 0 , the intercept with the x -axis. The retention of standards with known lipophilicity log P was then determined using the chromatographic systems described above and R MW values were calculated. From these experimental data equations relating log P and R MW were created for each system separately and these equations were used to estimate log P exp values for the alkaloids. log P exp , slope ( S ), and φ 0 values obtained by use of different TLC systems were also correlated.

3

Synthesis and Crystal Structure of Hydrogenated Pyrazino[2,1-a]isoquinoline Derivatives

Zawadzka A., Leniewski A., Maurin J. K., Wojtasiewicz K., Siwicka A., Czarnocki Z.

Polish Journal of Chemistry

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2003

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Vol. 77 / nr 5

565-576

EN

Areview of the experimental as well as of the theoretical studies, performed on the area of the infrared spectroscopy of hydrogen bonded molecular crystals, is given. Discussion of some physical phenomena is presented, responsible for basic spectral effects registered in the infrared spectra, as breaking of vibrational dipole selection rules in the IR spectra, linear dichroic as well as temperature effects, observed in the frequency range of the proton stretching vibrations. Also some newly recognized H/D isotopic effects for hydrogen bonded systems are presented, deduced from a quantitative analysis of the polarized spectra in the IR, namely the so called isotopic "self-organization" effects and the "long-range" H/D isotopic effects.