Development and validation of an HPLC stability-indicating method for identification and assay of elemental iron(II) in pharmaceutical drug products using reversed-phase HPLC

Ferrous sulfate tablets are a supplementary iron source for people who suffer from iron deficiency anemia. A simple, fast, and QC-friendly HPLC method was developed and validated to determine elemental iron in ferrous sulfate drug products. A TSK-GEL Super octadecylsilyl column (50 x 4.6 mm id, 2 microm particle size) with a mobile phase consisting of 0.06 M methanesulfonic acid in water-acetonitrile (40 + 60, v/v) and UV detection at 282 nm were used for this method. Separation of the elemental iron peak from the matrix was achieved within 5 min. This method was successfully validated according to International Conference on Harmonization guidelines, and shown to be stability-indicating for the shelf-life samples of ferrous sulfate tablets, as well as selective for the analyte of interest.     

Silver(I) and copper(I) complexes supported by fully fluorinated 1,3,5-triazapentadienyl ligands

Synthesis of the perfluorinated 1,3,5-triazapentadiene [N{(CF(3))C(C(6)F(5))N}(2)]H and the use of its conjugate base as a supporting ligand for the isolation of silver(i) and copper(i) complexes are reported. Some of the related chemistry involving [N{(C(3)F(7))C(C(6)F(5))N}(2)](-) (that has bulkier -C(3)F(7) groups on the 1,3,5-triazapentadienyl ligand backbone) is also presented. X-ray crystallographic data show a wide variety of structures ranging from intermolecular, hydrogen-bonded chain structure for [N{(CF(3))C(C(6)F(5))N}(2)]H with a twisted W-shaped N(3)C(2) core, monomeric [N{(CF(3))C(C(6)F(5))N}(2)]Ag(CN(t)Bu)(2) and [N{(C(3)F(7))C(C(6)F(5))N}(2)]Ag(CN(t)Bu)(2) where the κ(1)-bonded triazapentadienyl ligand bonding to the metal fragment via the central nitrogen atom, monomeric [N{(CF(3))C(C(6)F(5))N}(2)]Ag(PPh(3))(2) and [N{(C(3)F(7))C(C(6)F(5))N}(2)]Ag(PPh(3))(2) that feature κ(1)-bonded triazapentadienyl ligand bonding to the metal fragment via one of the terminal nitrogen atoms, to that of the monomeric [N{(CF(3))C(C(6)F(5))N}(2)]Cu(CN(t)Bu)(2) containing a κ(2)-bonded triazapentadienyl ligand and a U-shaped NCNCN ligand backbone. The isocyanide adducts show relatively high ν(CN) values in the IR spectra.     

Vanishing viscosity with short wave-long wave interactions for multi-D scalar conservation laws

We consider a system coupling a multidimensional semilinear Schrödinger equation and a multidimensional nonlinear scalar conservation law with viscosity, which is motivated by a model of short wave-long wave interaction introduced by Benney (1977). We prove the global existence and uniqueness of the solution of the Cauchy problem for this system. We also prove the convergence of the whole sequence of solutions when the viscosity ε and the interaction parameter α approach zero so that α=o(ε1/2). We also indicate how to extend these results to more general systems which couple multidimensional semilinear systems of Schrödinger equations with multidimensional nonlinear systems of scalar conservation laws mildly coupled.     

Hysteresis effects under CIR interest rates

Most decision making research in real options focuses on revenue uncertainty assuming discount rates remain constant. However, for many decisions revenue or cost streams are relatively static and investment is driven by interest rate uncertainty, for example the decision to invest in durable machinery and equipment. Using interest rate models from Cox et al. (1985b), we generalize the work of Ingersoll and Ross (1992) in two ways. Firstly, we include real options on perpetuities (in addition to zero coupon cash flows). Secondly, we incorporate abandonment or disinvestment as well as investment options, and thus model interest rate hysteresis (parallel to revenue uncertainty in Dixit (1989a)). Under stochastic interest rates, economic hysteresis is found to be significant, even for small sunk costs.     

Long range energy transfer in conjugated polymer sequential bilayers

Steady-state and time-resolved photoluminescence have been used to investigate the optical properties of bilayer and blend films made from poly(9,9-dioctyl-fluorene-2,7-diyl) (PFO) and poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene] (MEH PPV). Energy transfer has been observed in both systems. From steady-state photoluminescence measurements, the energy transfer was characterized by the effective enhancement of the MEH PPV emission intensity after exciting the donor states. Relatively faster decays for the PFO donor emission have been observed in the blends as well as in the bilayer structures, confirming effective energy transfer in both structures. In contrast to the bilayers, the time decay of the acceptor emission in the blends presents a long decay component, which was assigned to the exciplex formation in these samples. For the blends the acceptor emission is in fact a composition of exciplex and MEH PPV emissions, the later being due to Fo?rster energy transfer from PFO. In the bilayers, the exciplex is not observed and temperature dependence photoluminescence measurements show that exciton migration has no significant contribution to the energy transfer. The efficiency and very long range of the energy transfer in the bilayers is explained assuming a surface-surface interaction geometry where the donor/acceptor distances involved are much longer than the common Fo?rster radius.     

Cationic gold carbonyl complex on a phosphine support

A cationic gold carbonyl complex has been synthesized and characterized using several techniques including X-ray crystallography. [(Mes(3)P)Au(CO)][SbF(6)] (Mes = 2,4,6-Me(3)C(6)H(2)) has a linear, two-coordinate gold atom. This compound displays the CO stretching frequency at 2185 cm(-1). The (13)C NMR signal of the gold-bound (13)CO appears as a doublet centered at δ 182.6 ((2)J(C,P) = 115 Hz). A computational study shows that the Au-CO bond consists of electrostatic attraction, Au ← CO donation, and significant Au → CO π-back-bonding components. Polarization of the CO bond caused by the electrostatic effect of the cationic gold center is mainly responsible for the large blue shift in the CO stretching frequency.     

Formation of cinnoline derivatives by a gold(I)-catalyzed hydroarylation of N-propargyl-N′-arylhydrazines

A study concerning the gold(I)-catalyzed hydroarylation of N-propargyl-N′-arylhydrazinecarboxylic acid methyl esters is described. The use of the gold complex [XPhosAu(NCCH₃)SbF₆] as the catalyst in refluxing nitromethane allows the generally rapid and efficient synthesis of a range of functionalized 4-exo-methylene-1,2-dihydrocinnolines.     

On/off luminescence vapochromic selective sensing of benzene and its methylated derivatives by a trinuclear silver(I) pyrazolate sensor

{[3,5-(CF(3))(2)Pz]Ag}(3) (1) films exhibit selective/reversible sensing of small-organic-molecule (SAM) vapors, which readily switch-on bright-green (benzene or toluene) or bright-blue (mesitylene) luminescence that switches-off upon vapor removal. Vapors of electron-deficient SAMs or non-aromatic solvents did not attain luminescence switching and were not adsorbed.     

Trypanocidal activity of oxoaporphine and pyrimidine-β-carboline alkaloids from the branches of Annona foetida Mart. (Annonaceae)

Phytochemical investigation of the branches of Annona foetida Mart. led to isolation from the CH(2)Cl(2) extract of four alkaloids: Atherospermidine (1), described for the first time in this species, liriodenine (2), O-methylmoschatoline (3), and annomontine (4). Their chemical structures were established on the basis of spectroscopic data from IR, MS, NMR (1D and 2D), and comparison with the literature. Compounds 2-4 showed potent trypanocidal effect when evaluated against epimastigote and trypomastigote forms of Trypanosoma cruzi.     

Geometry of plane curves

In this paper we obtain, for a class of plane curves, extensions of the well-known relation of inflection points, double points and bitangencies established by Fabricius-Bjerre for closed curves.