Spectrophotometric method for estimation of alkaloids precipitable with Dragendorff's reagent in plant materials

A rapid, easy, and simple spectrophotometric method was developed for the estimation of total alkaloids precipitated by Dragendorff's reagent (DR) in plant materials. It is based on the formation of yellow bismuth complex in nitric acid medium with thiourea. The yellow-colored complex formed obeys Lambert-Beer's law in the concentration range of 0.06-50 microg/mL with lambdamax at 435 nm. Using this method, the alkaloidal percentage of certain alkaloids (ajamalicine, papaverine, cinchonine, piperine, berberine) and some plant materials containing alkaloids (Berberis aristata, Solanum nigrum, and Piper longum) were determined. The method was compared with other methods. It can be used for routine analysis of commercial samples by industries dealing with herbal drugs for standardization of plant materials containing alkaloids and for alkaloid-containing pharmaceutical products.     

Spectrophotometric method for determination parts per million levels of cyclohexylamine in water

UV-vis spectrophotometric method for the analysis of cyclohexylamine (CHA) in aqueous medium in the range of 0.3-20 ppm was developed by coupling CHA with sodium 1,2-naphthaquinone-4-sulphonate (NQS). At 470 nm a calibration slope of 0.028 OD ppm(-1) was observed. Minimum detection limit was 0.3 ppm with standard deviation of 0.1 ppm. Reagent concentration and solution pH for the analysis are optimised by studying its effect on absorbance at 470 nm. The method was applied to analyse CHA for evaluating the performance of ion exchange resin used in condensate purification plant (CPP) of power station where, CHA is used as all volatile treatment (AVT) reagent to inhibit steam generator (SG) corrosion. Structure of the adduct formed by coupling CHA with NQS is elucidated using NMR ((1)H and (13)C) and IR spectra, CHN analysis and mole ratio variation method.     

Partitioning of polystyrene between incompatible phases and distributional effects in the system polystyrene–polybutadiene–toluene

The average molecular weights and the molecular weight distributions of polystyrene (PS) in the conjugate incompatible phases of the ternary system of PS and polybutadiene with toluene as solvent were studied at 23°C. Gelpermeation chromatography, with ultraviolet and differential refractive index detectors, was used for analyzing the compositions of the conjugate phases and for obtaining the molecular weight averages of PS in the phases. Both narrow and broad molecular weight distribution (MWD) polymer samples were used. The effect of broad MWD polymers is seen as one of narrowing the shape of the binodal, thus effectively increasing the compatible region. The molecular weight averages of PS in the two conjugate phases do not vary significantly in the case of the narrow MWD PS sample while for broad MWD samples the average molecular weight of PS is found to be higher in the PS-rich phase than in the polybutadiene-rich phase for tie lines closer to the plait point indicating a partitioning or redistribution of the molecular weight species of PS between the incompatible phases.     

Organo-lithiation and halogen metal exchange reactions in organic synthesis-an anomolous aromatic substitution via halogen-metal exchange

Synthesis via organo-lithium compounds is reviewed. An anomalous aromatic substitution via halogen-metal exchange is described. Here, the substitution does not occur at the position where the halogen was present; but at an alternate position. A mechanism is advanced, in which the halogen-metal exchange is proposed as being faster than the hydrogen(acidic)-metal exchange.     

Unrestricted Hartree-Fock calculations of spin densities with orthogonalized atomic orbitals: Proton and 13C hyperfine splittings in some pi hydrocarbon radicals

The spin density distribution in a few hydrocarbon radicals has been calculated using orthogonalized atomic orbitals in the Unrestricted Hartree-Fock formalism of Amos and Snyder and including certain more important two-electron hybrid and exchange integrals and all the core-resonance integrals. Our calculated spin densities for the cation and anion radicals of alternant hydrocarbons, which are now different due to the breakdown of the pairing theorem, are, in general, of the right relative order so that even the simple McConnell type of relation can account partly for the observed differences in the proton splittings between cations and anions. The proton splittings for position 2 of naphthalene and anthracene radical ions are correctly predicted, thus clearing up the well-known cation-anion anomaly for this position. Comparative calculations have been made to show that the spin density results are worsened with the neglect of the integrals of the type mentioned before. An empirical analysis correlating the observed ¹³C splittings and the spin density results over a non-orthogonal basis set shows that the available ¹³C splittings in alternant hydrocarbon radical ions can be explained with a set of sigma-pi parameters which are consistent with the theory. It is shown that even though the spin densities in cations and anions may be different, these can lead to similar ¹³C splittings.     

Utilization of CS2 as a source of C1 synthetic units for the preparation of bis(alkylthio)methanes and alkyl dithioformates

Double insertion of CS2 into two Ru-H bonds of [(dppm)2Ru(H)2] (dppm = Ph2PCH2PPh2) affords the methanedithiolate complex [(dppm)2Ru(eta2-S2CH2)]. The methanedithiolate moiety has been functionalized using 2 equiv of RX resulting in bis(alkylthio)methane derivatives [(dppm)2Ru(RSCH2SR)][X]2. The bis(alkylthio)methane complex loses the bis(alkylthio)methane moiety under very mild conditions and in turn affords the [(dppm)2RuX2] complex from which the starting dihydride [(dppm)2Ru(H)2] has been regenerated via reaction with KOH/EtOH. On the other hand, insertion of CS2 into one Ru-H bond of [(dppe)2Ru(H)2] (dppe = Ph2PCH2CH2PPh2) followed by functionalization using RX results in alkyl dithioformate complex trans-[(dppe)2Ru(H)(SC(SR)H)][X]. In this case also, the alkyl dithioformate moiety gets eliminated under very mild conditions to afford the [(dppe)2Ru(H)(X)] derivative from which the starting dihydride has been regenerated via reaction with NaBH4. The reactions presented here constitute utilization of CS2 as a C1 synthetic source for the generation of useful organic compounds.     

Magnetic properties of Gd1−xThxFe2 and Gd1−xCexFe2

Saturation magnetization, magnetization vs temperature, Curie temperatures, and lattice parameters are presented for the ternary alloys Gd_1?xTh_xFe₂ and Gd_1?xCe_xFe₂. Quadrivalent Th and Ce were introduced into the lattice in an effort to induce ferromagnetic GdFe coupling. Experiment showed that the antiferromagnetic GdFe coupling in GdFe₂ is preserved in the ternaries. The Fe moment and Curie temperature decrease as the Gd content of the sample is decreased. This is ascribed to electron transfer from Th or Ce to the Fe d shell. Failure to achieve ferromagnetic coupling is ascribed to electron capture by iron, which prevents a rise in electron concentration as Gd is replaced by Ce or Th.     

Laser Micropatterning of Polylactide Microspheres into Neuronal-Glial Coculture for the Study of Axonal Regeneration

250,000 Americans suffer from spinal cord injury caused by vehicular, work, and sports related accidents^[1]. After injury to the spinal cord, axons do not have the capability of regenerating across the lesioned site. To understand the mechanisms of axon regeneration and to identify a better method of regeneration, a new technique for mimicking and studying the in vivo cellular environment is needed. To meet this goal, we have developed a laser cell micropatterning system that uses a weakly focused laser beam to pattern both biological cells and nonbiological particles for the study of various cell-cell-polymer interactions. Using this system, we have successfully copatterned neurons, glial cells, and polymer microspheres into a viable matrix. These copatterns allow us to study the effects nerve growth factor has, when released from a degradable polymer microsphere, on a single neuron within a specific arrangement of multiple cell types.