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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.
EN
The relative lipophilicity, R M0 , and specific hydrophobic surface area of eleven 3-hydroxy-1,2-benzoisoxazoles substituted in the benzene ring (two isomeric fluoro, three isomeric chloro, three isomeric bromo and dibromo derivatives, and a nitro derivative) have been studied by reversed-phase thin layer chromatography (RP-TLC) on silica gel RP-C18 plates with methanol-water mixtures as mobile phases. Linear correlation between the volume fraction of methanol and R M values over a limited range was established with high correlation coefficients ( r > 0.99). Lipophilicity R M0 was compared with computed partition coefficients IAlogP, A logP s , clogP, milogP, logP KOWIN , and xlogP. The best correlation ( r > 0.9) was found between R M0 and logP KOWIN and xlogP values. Principal-components analysis (PCA) was also used to compare R M0 values with computed partition coefficients. The chromatographic behaviour of 3-hydroxy-1,2-benzisoxazoles was compared with that of their bioisosteric analogues 1,2-benzisot-iazolonoles. Experimental R M0 values for both groups of compounds were in accor-dance with the equation R M0 aR M0 +b(r> 0.9).
EN
The lipophilicity R M0 and log P TLC of thirteen novel, potentially biologically active, 12 H -quino[3,4- b] [1,4] benzothiazinium salts have been determined by reversed-phase thin-layer chromatography using RP-18 silica plates and methanol-aqueous Tris buffer solution mixtures as mobile phases. R M values of the compounds were linearly dependent on methanol concentration; extrapolation of these to 0% methanol gave the lipophilicity R M0 . log P TLC was obtained from R M0 by use of a calibration curve obtained for five standards of known experimental lipophilicity (log P). Lipophilicity log P calcd for the thirteen quinobenzothiazines was calculated by use of nine software products. The values determined were discussed in terms of structure-lipophilicity relationships. The results indicate that chromatographic lipophilicity R M0 can be used as a measure of the lipophilicity of the azaphenothiazine derivatives investigated.
4
Content available remote Determination of the lipophilicity of selected isoquinoline alkaloids by RP-TLC
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.
5
Content available remote RP-HPLC and RP-TLC in the analysis of flavonoids
EN
Effect of mobile phase composition on the separation of flavonoids from five major classes (catechins, flavonols, flavanones, flavones and anthocyam'dins) has been investigated on RP-18 TLC plates. Water-acetonitrile mixtures and trifl no ro acetic acid in waier-acetoni-trile mixtures have been used as the mobile phases. An RP-HPLC system for these compounds has also been developed. Interferences from vitamins and methyixanthines in the new RP-HPLC system have been investigated. Flavonoids were determined in fruit, vegetables, wine, tea and urine samples.
PL
Rozdzielano flawonoidy z pięciu gtównych klas (katechiny, flawony. flawanony, flawonole i antocyjanidyny) metodą chromatografii cienkowarstwowej na płytkach RP-18, stosując jako fazę ruchomąmieszaniny wody i acetonitrylu z dodatkiem kwasu trifluorooctowego. Dla tej samej grupy flawonoidów opracowano układ RP-HPLC. W opracowanym układzie badano wpływ interferencji ze strony witamin i metyłoksantyn. Oznaczono zawartość flawonoidów w próbkach: owoców, warzyw, win, herbat i w moczu.
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