A validated high-performance thin-layer chromatography method for the simultaneous estimation of berberine,berbamine, palmatine,magnoflorine and jatrorrhizine from Berberis aristata

JPC – Journal of Planar Chromatography – Modern TLC - Berberis aristata DC., well known as ‘Indian barberry’ or ‘tree turmeric’, (Berberidaceae) is a medicinal...     

Chemoprofiling and Solamargine Estimation from a Few Solanum Species Used as ‘Brihati’ and Its Market Samples Using a Validated High-Performance Thin-Layer Chromatography Method

JPC – Journal of Planar Chromatography – Modern TLC - An ingredient of ‘Dasamoola’ and ‘Laghupanchamoola’ group of drugs, the source of ‘Brihati’ has...     

HPTLC Method for Chemical Standardization of Sida Species and Estimation of the Alkaloid Ephedrine

JPC – Journal of Planar Chromatography – Modern TLC - The roots of Sida cordifolia, known as ‘Bala’ in the Ayurvedic system of medicine, are used to treat a variety of...     

Densitometric Determination of Taurine and l-Lysine Hydrochloride in an Energy Drink and in Multi-Vitamin Syrup,and Validation of the Method

JPC – Journal of Planar Chromatography – Modern TLC - A simple and rapid densitometric method has been developed for determination of taurine and lysine in ‘energy drinks’...     

A Fast Isolation Method for Glycyrrhizic Acid,the Bioactive Marker of Glycyrrhiza glabra,and Its Quantitative Evaluation in Some Single and Multiherbal Formulations Using High-Performance Thin-Layer Chromatography

JPC – Journal of Planar Chromatography – Modern TLC - Glycyrrhizic acid, the major metabolite of Glycyrrhiza glabra, is a ‘Hot Molecule’ in view of its sweet tasting...     

On the Way to Optoionics

Based on the recent finding of significant ion conduction enhancement in iodide perovskites upon illumination, the potential of an emerging field ‘opto-ionics’ – that we define in parallelism to ‘opto-electronics’ – is explored. We emphasize that the major prerequisite is the identification of appropriate stable materials which can act as light-tunable electrolytes, permeation membranes, or electrodes. In this way, classic, but light-tunable electrochemical devices would be in reach. We also touch upon related issues such as sensing, switching, and catalysis, in which light effects on ionic charge carriers are also expected to be important.     

Der ‘Push-Pull’-Effekt von ‘Push-Pull’-Oligoacetylenen. Eine 13C-NMR-Untersuchung

The ‘Push-Poll’ Effect of ‘Push-Pull’ Oligoacetylenes. A ¹³C-NMR Investigation According to ¹³C-chemicaI shifts of ‘push-pull’ oligoacetylenes 1 – 4 , the ‘push-pull’ effect (i.e. π delocalization induced by ‘push-pull’ substituents) rapidly decays in this series. To correct for other than π -charge-density effects, Δδ values of symmetrically placed C-atoms of the oligoacetylene chain are discussed. Stereoelectronic resteffects (SER) of the substituents on terminal C-atoms of PP-ketones 1a – 3a and PP -esters 1b – 4b are estimated from the residual Δδ of the asymptotes of Fig. 3. Fig. 4 convincingly shows that Δδ values are dramatically decreasing with increasing number n of acetylene units between the push and pull substituents. Assignment problems of ‘push-pull’ triacetylenes 3 have been solved by ¹³C labelling of the CO group of 3a .     

Use of HPTLC to Establish the Chemotype of a Parasitic Plant,Dendrophthoe falcata (Linn. f.) Etting. (Loranthaceae), Growing on Different Substrates

JPC – Journal of Planar Chromatography – Modern TLC - Dendrophthoe falcata (Linn. f.) Etting. is a stem parasite commonly known as ‘Vanda’ in the Ayurvedic system of...     

Influence of the Axial Alkyl Ligand on the Reduction Potential of Alkylcob(III)alamins and Alkylcob(III)yrinates

The irreversible-reduction potentials of 26 alkylcob(III)alamins (RCbl^III 1a – z ) and 26 alkylcob(III)yrinates (R‘Cby’^III; 2a – z ) (E_p 1a – z and E_p 2a – z , resp.) have been measured in situ by single-scan voltammetry of hydroxocob(III)alamin hydrochloride (vitamin B_12b- HCl; 1 ) or heptamethyl cob(II)yrinate perchlorate (ClO₄‘Cby’^II; 2 ) in presence of the corresponding alkyl halides (RX; 3a – z ) in DMF. The reduction potentials of alkylcobalt complexes exhibiting half-life times as short as a few seconds become measurable by this technique. Thermodynamic cycles prove that the observed reduction potentials are closely related to the standard reduction potentials E°(R? Co^III + e^??R? + Co^I). Electron-withdrawing groups and/or an increased degree of substitution at the Co-bound C-atom in RCbl^III and, R‘Cby’^III shift E_p( 1a – z ) and E_p ( 2a – z ) towards positive potentials. Linear correlations have been found between E_p( 1a – z ) (E_p( 2a – z )) of RCbl^III (R‘Cby’^III) and the pK_a of RH (or the Taft σ*- or the Hammett σ-values of R) within each class of R, i. e. MeCbl^III (Me‘Cby’^III), primary RCbl^III (R‘Cby’^III) and secondary RCbl^III (R‘Cby’^III). The correlations allow to distinguish between electronic effects of the Co-bound alkyl residues and their steric interactions with the corrin side chains. The correlations have further been used to visualize the light-induced formal insertion of an olefin into the Co, C-bond of an alkylcobalamin (Scheme 2, 1a → 1u ), a key step in the vitamin-B₁₂-catalized C, C-bond formation.     

Qualitative and Quantitative Standardization of Myrica esculenta Buch.-Ham. Stem Bark by Use of HPTLC

JPC – Journal of Planar Chromatography – Modern TLC - Bark of Myrica esculenta Buch.-Ham., commonly known as ‘Kaphal’ in indigenous systems of medicine, is used for...     

Two-Stage Fractionation of a Mixture of Pesticides by Micropreparative TLC and HPLC

JPC – Journal of Planar Chromatography – Modern TLC - A ten-component mixture of pesticides was applied to the edge of the layer in ‘frontal + elution’ mode for preliminary...     

Estimation of Guggulsterones E and Z in Solid Dosage Forms Containing Commiphora mukul,Hook

JPC – Journal of Planar Chromatography – Modern TLC - The oleo-gum-resin known as ‘guggul’, obtained from the plant Commiphora mukul, Hook (family Burseraceae), is widely...     

Modern TLC: A Key Technique for Identification and Quality Control of Botanicals and Dietary Supplements

JPC – Journal of Planar Chromatography – Modern TLC - Thin-layer chromatography (TLC) is generally regarded as a common analytical technique. Everybody ‘knows’ it and it is...     

Orbital Correspondence Analysis in Maximum Symmetry

A method is described in which the ‘allowed’ course of a reaction is determined by means of an analysis – within the symmetry point group common to reactants and products – of their molecular orbitals and of the distortions that occur along the reaction path connecting them. The procedure, and its relation to and advantages over conventional correlation methods, is illustrated with a few very well known reactions: Cyclization of hexatriene, the ‘photochemical Diels-Alder reaction’ and the stepwise and concerted [2+2]-cycloadditions.     

Definitive Proof for the Operation of Isotopically Sensitive Branching (‘Metabolic Switching’) in FeI-Mediated C?H Bond Activation in the Gas Phase Short Communication

Rigorous regio- and stereospecific labeling experiments are performed to demonstrate the operation of the previously suggested operation of ‘isotopically sensitive branching’ in Fe^I-mediated C? H bond activation. For the hexane-1,6-diol/Fe⁺-complex, it is shown that dehydrogenation involves specifically the central C(3)/C(4) position, and the study of the stereospecifically labeled D ,L - and meso-[3,4-D₂]-isotompomers 1e and 1f demonstrates that dehydrogenation proceedes via two competing pathways (i.e. ‘anti’- vs. ‘syn’-route). The contribution of these routes to the product formation is – due to a kinetic isotope effect – controlled by the relative configuration at the labeled positions C(3)/C(4). For the D ,L -form 1e , we estimate a ratio of 49:1 in favor of the ‘anti’-route; due to an isotope effect, this ratio drops to 4.3:1 for the meso-form 1f .     

Die Reaktion von 1-Halogeno-1-Lithiocyclopropanen mit CuCl2: Konkurrenz zwischen ‘Carben-Dimerisierung’ und oxidativer Kupplung

The Reaction of 1-Halogeno-1-lithiocyclopropanes with CuCl₂: Competition between ‘Carbene Dimerization’ and Oxidative Coupling The 1-chloro-1-lithiocyclopropanes 2a – d react at low temperature with CuCl₂ to give diastereoisomeric mixtures of oxidative-coupling products 5a – d and of ‘carbene dimers’ 6a–d . The relative amount of 5a – d increases with CuCl₂ concentration and reaction time. Diastereoselectivity of the reaction seems to be low, and separation as well as spectroscopic structure assignment of single diastereoselectivity of the reaction seems to be low, and separation as well as spectroscopic structure assignment of single diastereoisomers are difficult. The conformational behavior of 1,1′-dichloro-1,1′-bi(cyclopropyls) 5c and 5d is discussed. Contrary to 2a – d , 1-bromo-1-lithiocyclopropanes normally react with CuCl₂ to give ‘carbene dimers’ 6 and no coupling products 5 . So far the only exception is 1-bromo-1-lithio-2-phenylcyclopropane 2e which in the presence of CuCl₂ gives some percents of coupling products 5e besides carbene dimers 6b as main products. An X-ray structure analysis of the predominant diastereoisomer 5e was performed.     

Molecular modeling of 8-methoxy quinolone analogues by using quantitative structure activity relationship

Quantitative structure activity relationship (QSAR) studies on a series of 8-methoxy quinolone are found to correlate well with steric parameters and electronic parameter. The results are critically discussed on the basis of regression data, Pogliani factor Q and cross validation technique. The results are found to be useful in discussing the mechanism of drug – receptor interaction. Steric parameter ‘Mr’ and electronic parameter ‘Pz’ gives the best model.     

Synthesis and Cytotoxicity Studies of New (Dimethylamino)‐Functionalised and 7‐Azaindole‐Substituted ‘Titanocene’ Anticancer Agents (7‐Azaindole=1H‐Pyrrolo[2,3‐b]pyridine)

From the carbolithiation of 1‐(cyclopenta‐2,4‐dien‐1‐ylidene)‐N,N‐dimethylmethanamine (=6‐(dimethylamino)fulvene; 3 ) and different lithiated azaindoles 2 (1‐methyl‐7‐azaindol‐2‐yl, 1‐[(diethylamino)methyl]‐7‐azaindol‐2‐yl, and 1‐(methoxymethyl)‐7‐azaindol‐2‐yl), the corresponding lithium cyclopentadienide intermediates 4a – 4c were formed (7‐azaindole=1H‐pyrrolo[2,3‐b]pyridine). The latter underwent a transmetallation reaction with TiCl₄ resulting in the (dimethylamino)‐functionalised ‘titanocenes’ 5a – 5c . When the ‘titanocenes’ 5a – 5c were tested against LLC‐PK cells, the IC₅₀ values obtained were of 8.8, 12, and 87 μM , respectively. The most cytotoxic ‘titanocene’, 5a , with an IC₅₀ value of 8.8 μM is nearly as cytotoxic as cis‐platin, which showed an IC₅₀ value of 3.3 μM when tested on the epithelial pig kidney LLC‐PK cell line, and ca. 200 times better than ‘titanocene dichloride’ itself.     

Synthesis of 1,2,3‐Triazole Analogues of Lincomycin

In search for new antibiotics we replaced the amide moiety of lincomycin 1 by a 1,2,3‐triazole ring. The 1,2,3‐triazoles 10a – 10k were obtained as single regioisomers by ‘click reaction’ of azide 5 with the alkyne 9k , derived from propyl hygric acid, and the alkyl, aryl, or cycloalkyl alkynes ribosomes 9a – 9j . The new analogues proved inactive towards wild‐type and A2058G mutant.     

The ‘t‐Amino Effect’ of ortho‐Nitroso Amines. Synthesis of 2,6‐Diaminoadenine Derivatives from 6‐(Dialkylamino)‐5‐nitrosopyrimidines

The ‘t‐amino effect’ of amino‐nitroso compounds was documented by preparing the (dialkylamino)‐nitroso pyrimidines 4 – 18 , and cyclising them under thermal conditions in high yields to the purine derivatives 19 – 32 . The reactivity of the amino‐nitroso‐pyrimidines, particularly of 17 derived from diethyl iminodiacetate, and of 19 , derived from 1‐phenylimidazolidine, correlates with the stability of the intermediate azomethine ylide. Thermolysis of the amino‐nitroso‐pyrimidines 34 – 37 , possessing dialkylamino substituents at C(4) and C(6), proceeded by protiodenitrosation, leading to 38 – 41 .