Development and validation of HPLC method for simultaneous estimation of piperine and guggulsterones in compound Unani formulation (tablets) and a nanoreservoir system

An attempt has been made to develop and validate a simultaneous HPLC method for novel approach of drug release via oil‐in‐water (o/w) nanoemulsion formulation and Habb‐e‐Khardal Unani tablet containing piperine and guggul sterones E and Z as main ingredients. Nanoemulsion was prepared by titration method using sefsol‐218 as an oily phase, cremophor‐EL as a surfactant, transcutol as a co‐surfactant and distilled water as an aqueous phase. The formulation was optimized on the basis of thermodynamic stability and dispersibilty test. The nanoformulation was evaluated for particle size, surface morphology, electrical conductivity and viscosity determination. The in vitro dissolution was carried out by dialysis bag method. Drugs were quantified using an HPLC method developed in‐house with a C₁₈ column as stationary phase and acetonitrile and water as mobile phase at λ_max of 240 nm. The optimized formulation showed higher drug release, lower droplet size and less viscosity as compared with the conventional Habb‐e‐Khardal Unani tablet. The present study illustrated the potential of nanoemulsion dosage form in improving biopharmaceutic performance of piperine and guggul sterone. The HPLC method was also found to be quite sufficient for the routine quality control of formulations containing piperine and guggul sterone E and Z as ingredients and also for in vitro drug release studies. Copyright © 2011 John Wiley & Sons, Ltd.     

Simultaneous quantification of five marker compounds of Betula utilis stem bark using a validated high-performance thin-layer chromatography method

A sensitive, selective and robust densitometric high-performance thin-layer chromatographic method was developed and validated for five marker compounds, namely betulin, lupeol, oleanolic acid, 3-acetyloleanolic acid and β-sitosterol, known for their various therapeutic activities. The marker compounds have been isolated from the stem bark of Betula utilis, well characterized by the spectral analysis, and their simultaneous quantitative determination carried out by high-performance thin-layer chromatography (HPTLC) method. The resolution of marker compounds was carried out on silica-gel 60 plates, using n-hexane:ethyl acetate (8:2 v/v) as the mobile phase. The HPTLC densitometry was performed at 500-nm wavelength after the post chromatographic derivatization with ceric ammonium sulfate reagent. The optimized method provided good linear relation (r>0.9960) for all the investigated analytes. The method is simple, and reproducible, which may be applied for quantitative analysis of the above-mentioned marker compounds.     

Recent trends in chiral separations on immobilized polysaccharides CSPs

Polysaccharide CSPs are recognized widely in chiral chromatography but the introduction of immobilized phases (Chiralpak IA, Chiralpak IB and Chiralpak IC columns) is a remarkable achievement. The immobilized CSPs can be used with organic, normal and reversed phase modes; even with prohibited solvents too (tetrahydrofuran, chlorofom, dichloromethane, acetone, 1,4-dioxane, ethylacetate, and certain other ethers). Their susceptibilities to work with a wide range of solvents have increased the range of applications including chiral recognition mechanisms. Besides, these are also useful for monitoring the progress of stereo-specific reactions; normally need prohibited solvents. The present review describes the various aspects of commercial available immobilized chiral columns. Attempts have been made to discuss immobilized polysaccharides CSPs, immobilized vs coated CSPs, comparison of immobilized CSPs, method development, optimization, chiral recognition mechanism and applications. The chiral recognition capabilities of commercial columns were in the order of Chiralpak IA > Chiralpak IB > Chiralpak IC columns; but complimentary to each other. Of course, these CSPs are not fully developed and need more advancements and applications. Definitely, the future of immobilized CSPs is quite better. Hopefully, in the coming years they will be the choice of the chromatographers for chiral separations in liquid chromatography.     

Photodynamic effect in near-IR light by a photocytotoxic iron(III) cellular imaging agent

A red light for cancer cells: an iron(III) complex (1, see picture) that contains an anthracenyl fluorophore moiety and a catecholate ligand is a potent, metal-based PDT agent that efficiently photocleaves DNA in near-infrared light, has significant nuclear uptake, and high photocytotoxicity in red light by an apoptotic pathway in HeLa and MCF-7 cancer cells.     

Solvent‐assisted anionic ring opening polymerization of glycidol: Toward medium and high molecular weight hyperbranched polyglycerols

Hyperbranched polyglycerols (HPGs) are globular structures with a large number of functionalizable hydroxyl groups and have excellent in vitro and in vivo biocompatibility profiles comparable to polyethylene glycol. This work introduces a facile method for the synthesis of medium molecular weights (M_ws) (50–300 kDa) HPGs, which has been difficult to synthesize with low polydispersity, with the assistance of solvents by ring opening polymerization. The influence of different solvents (1,4‐dioxane, tetrahydropyran (THP), ethylene glycol diethyl ether (EGDE) and decane), solvent to glycidol ratio, concentration of glycidol and the time of polymerization on M_w and polydispersity of HPGs has been studied. The M_w and polydispersity of HPGs are significantly affected by the nature of the polymerization phase (homogeneous or heterogeneous) and chemical structure of the solvent. The differences in the solvation of the potassium cations and change in the nucleophilicity of the alkoxide anion in various solvents may be responsible for the changes in M_w and PDI of the HPG. The M_w of the HPG decreases in the order 1,4‐dioxane > THP > EGDE >decane. The microstructure, solution and thermal properties of the HPG do not depend on the nature of solvent. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2013, 51, 2614–2621     

Radiobiokinetic evaluation of domestic cold kits

Domestically produced diagnostic cold kits, viz. glucoheptonate (GH), diisopropyliminodiacetic acid (DISIDA), dimercaptosuccinic acid (DMSA), diethylenetriamine-pentaacetic acid (DTPA), methylenediphosphonate (MDP) and Sn-colloid were labeled with^99mTc and their in-vivo distribution in experimental animals (rats) was evaluated prior to use in humans for diagnostic scanning. The biodistribution pattern was found in accordance with the latest guidelines of the International Atomic Energy Agency (IAEA), which serve as a standard for small scale producers.     

Enantio- and Diastereoselective Oxidation of N-Alkylimines Using Chiral α-Bromonitriles and Hydrogen Peroxide System

Chiral α-bromonitriles were prepared with good chemical and optical yields starting from natural α-amino acids by dehydrating the corresponding α-bromoamides with thionyl chloride. The combined system α-bromonitriles/hydrogen peroxide was examined for the enantio- and diastereoselective oxidation of N-alkylimines in basic media at room temperature. The oxidation of N-tertiobutylarylimines leads to optically active oxaziridines with moderate enantiomeric excess. However, the oxidation of (S)-1-phenylethylarylimines affords the corresponding oxaziridines with good diasteromeric excess up to 97/3 as proved by gaseous-phase chromatography.     

Synthesis and antimycobacterial activity of some beta-carboline alkaloids

In view of the attributed medicinal properties of beta-carboline alkaloids, some new O-acyl derivatives of beta-carboline alkaloid--harmol, were prepared and tested for possible antimycobacterial activity against Mycobacterium tuberculosis H37Rv.     

ITSTUDIES ON THE EFFECT OF UREA ON THE COMPATIBILITY OF PMMA/PVC MIXTURES IN DMF BY A DILUTE- SOLUTION VISCOMETRY METHOD

The interaction between poly(methymethacrylate) (PMMA) and poly(vinyl chloride) (PVC) has been studied indilute urea solutions of dimethylformamide (DMF) at 28℃ using a dilute solution viscometry method. The results show thatthe polymer mixtures are compatible in DMF solution in the absence of urea. The influence of urea addition on the degree ofcompatibility of the polymer mixtures has been studied in terms of the compatibility parameters (△b_m and △[η]_m). It wasfound that the compatibility of the polymer mixtures is decreased with increasing urea addition, passing through a minimumat 0.5 M urea.     

Apparent Solubility of Ibuprofen in Dimethyl Dodecyl Ammonium-Propane Sulfonate, DDAPS, Micelles, DDAPS/Butanol Mixtures and in Oil-in-Water Microemulsions Stabilized by DDAPS

Solubility of drugs in aqueous media is a real issue for scientists and a lot of work is going on to resolve the issue. The same is the case for ibuprofen, which is a derivative of propionic acid, belongs to the NSAIDs family and has low solubility in pure water. Therefore, its solubility has been investigated in dimethyl dodecyl ammonium-propane sulfonate, DDAPS, micellar solution, DDAPS/butanol mixtures and in various (hexane, decane and tetradecane) oil-in-water microemulsions to find out a suitable vehicle. The aggregation number, size and flow ability of micelles and microemulsions were estimated using refractive index, viscosity and light scattering measurements. It has been observed that these microemulsions have a higher ability to solubilize ibuprofen than DDAPS/butanol mixtures or DDAPS micelles.