Optimization of a validated stability‐indicating RP‐LC method for the determination of fulvestrant from polymeric based nanoparticle systems,drugs and biological samples

Fulvestrant is used for the treatment of hormone receptor‐positive metastatic breast cancer in postmenopausal women with disease progression following anti‐estrogen therapy. Several reversed‐phase columns with variable silica materials, diameters, lengths, etc., were tested for the optimization study. A good chromatographic separation was achieved using a Waters X‐Terra RP₁₈ column (250 × 4.6 mm i.d. × 5 µm) and a mobile phase, consisting of a mixture of acetonitrile–water (65:35; v/v) containing phosphoric acid (0.1%). The separation was carried out 40°C with detection at 215 nm.The calibration curves were linear over the concentration range between 1.0–300 and 1.0–200 µg/mL for standard solutions and biological media, respectively. The proposed method is accurate and reproducible. Forced degradation studies were also realized. This fully validated method allows the direct determination of fulvestrant in dosage form and biological samples. The average recovery of the added fulvestrant amount in the samples was between 98.22 and104.03%. The proposed method was also applied for the determination of fulvestrant from the polymeric‐based nanoparticle systems. No interference from using polymers and other excipients was observed in in vitro drug release studies. Therefore an incorporation efficiency of fulvestrant‐loaded nanoparticle could be determined accurately and specifically. Copyright © 2014 John Wiley & Sons, Ltd.     

A parallel monolithic algorithm for the numerical simulation of large‐scale fluid structure interaction problems

A novel parallel monolithic algorithm has been developed for the numerical simulation of large‐scale fluid structure interaction problems. The governing incompressible Navier–Stokes equations for the fluid domain are discretized using the arbitrary Lagrangian–Eulerian formulation‐based side‐centered unstructured finite volume method. The deformation of the solid domain is governed by the constitutive laws for the nonlinear Saint Venant–Kirchhoff material, and the classical Galerkin finite element method is used to discretize the governing equations in a Lagrangian frame. A special attention is given to construct an algorithm with exact total fluid volume conservation while obeying both the global and the local discrete geometric conservation law. The resulting large‐scale algebraic nonlinear equations are multiplied with an upper triangular right preconditioner that results in a scaled discrete Laplacian instead of a zero block in the original system. Then, a one‐level restricted additive Schwarz preconditioner with a block‐incomplete factorization within each partitioned sub‐domains is utilized for the modified system. The accuracy and performance of the proposed algorithm are verified for the several benchmark problems including a pressure pulse in a flexible circular tube, a flag interacting with an incompressible viscous flow, and so on. John Wiley & Sons, Ltd.     

Na3[BN2] and Na2K[BN2]: A Known and a Novel Alkali Metal Dinitridoborate Obtained via Mild Thermal Dehydrogenation

Na₃[BN₂] and Na₂K[BN₂] were obtained as white polycrystalline powders from the reaction of the respective binary mixtures NaNH₂:NaBH₄ and NaNH₂:KBH₄ in molar ratio 2:1 at 873 K and 683 K, respectively, in an argon stream. According to the results of thermal analysis measurements, both compounds are thermally stable only up to 954 K (Na₃[BN₂]) and 712 K (Na₂K[BN₂]), respectively, decomposing under evolution of alkali metal and nitrogen to yield hexagonal BN as final residue, which was identified from powder patterns. The crystal structure of Na₃[BN₂] {β‐Li₃[BN₂] type; P2₁/c (No. 14); Z = 4} was confirmed and the unit cell parameters redetermined: a = 5.724(1) Å, b = 7.944(1) Å, c = 7.893(1) Å, β = 111.31(1)°. According to X‐ray powder data, Na₂K[BN₂] crystallizes isotypic to Na₂KCuO₂ in the tetragonal space group I4/mmm (No. 139) with a = 4.2359(1) Å, c = 10.3014(2) Å and Z = 2. The crystal structure of Na₂K[BN₂] is composed of linear [N–B–N]^3– anions centering elongated M₁₄ rhombic dodecahedra, which are formed by 8 sodium and 6 potassium atoms. The [BN₂]@Na_8/4K_6/6 polyhedra are stacked along [001] and condensed via common tetragonal faces to generate a space‐filling 3D arrangement. The B–N bond lengths for the strictly linear [N–B–N]^3– units are 1.357(4) Å. Vibrational spectra of the title compounds were measured and analyzed based on D_∞h symmetry of the relevant [N–B–N]^3– groups taking into account the site symmetry effects for Na₃[BN₂]. Both the wavenumbers, as well as the calculated valence force constants f(B–N) = 7.29 N · cm^–1 (Na₃[BN₂]) and 7.33 N · cm^–1 (Na₂K[BN₂]), respectively, are in good agreement with those of the known alkali and alkaline earth dinitridoborates.     

Synthesis,characterization, and antioxidant and anticholinesterase activities of pyrazolo derivatives

Twenty-four pyrazolo derivatives (1–4)(a-f) were synthesized and characterized by FTIR, ¹H, and ¹³C NMR (Nuclear Magnetic Resonance), and elemental analysis. The synthesized compounds were also investigated for their antioxidant and anticholinesterase activities. The compounds (3–4)(a-f) carrying morpholine ring were more active than the piperidinyl containing compounds (1–2)(a-f) in both activities. The compound 4f showed higher activity in both assays as compared with the others. Additionally, the anticholinesterase activity test provided higher values than the galantamine in the BChE assay. Therefore, compound 4f can be used as anticholinesterase agent and/or anticholinesterase assay standard.     

Isolation,Characterization, and Medicinal Potential of Polysaccharides of Morchella esculenta

Mushroom polysaccharides are active medicinal compounds that possess immune-modulatory and anticancer properties. Currently, the mushroom polysaccharides krestin, lentinan, and polysaccharopeptides are used as anticancer drugs. They are an unexplored source of natural products with huge potential in both the medicinal and nutraceutical industries. The northern parts of Pakistan have a rich biodiversity of mushrooms that grow during different seasons of the year. Here we selected an edible Morchella esculenta (true morels) of the Ascomycota group for polysaccharide isolation and characterization. Polysaccharopeptides and polysaccharides from this mushroom were isolated using the green chemistry, hot water treatment method. Fourier transform infrared spectroscopy revealed the sugar nature and possible beta-glucan type structure of these polysaccharides. Antioxidant assays showed that the deproteinized polysaccharides have moderate free radical scavenging activity. These isolated polysaccharides exhibited good acetylcholinesterase (AChE) and butyryl cholinesterase (BChE) inhibition activities. Therefore, these polysaccharides may be valuable for the treatment of Alzheimer’s and Parkinson’s diseases. Further bioassays are needed to discover the true potential of M. esculenta polysaccharides for medicinal purposes.     

Electrochemical technologies coupled with biological treatments

When possible, the bioprocesses should be implemented to treat wastewater for their cost-effectiveness. However, many effluents are composed of biorecalcitrant organic pollutants, especially in industrial wastewaters. Advanced physico-chemical treatments are therefore needed to deal with these pollution levels. Electrochemical processes could be cost-effective solutions. However, the energy required to reach complete mineralization is often high. One promising combination would be to combine electrochemical processes that can remove xenobiotic compounds from effluent with biotechnologies that are able to mineralize the biodegradable fraction. Therefore, this review presents the most recent articles dealing with this combination, by mainly focusing on electrochemical advanced oxidation processes that demonstrated to have high removal efficiency for organic biorecalcitrant compounds. Additional and imperative information about the treatment strategy and the engineering aspects for the upscaling approach are also given.     

Synthesis,structure and in vitro anticancer activity of ruthenium(II) and platinum(II) complexes with chiral aminophosphine ligands

Transition Metal Chemistry - (R)-[Ru(η6-p-MeC6H4iPr)Cl2{Ph2PNHCH(CH3)(C6H4-4-F)}] (1) and cis-(R,R)-[PtCl2{Ph2PNHCH(CH3)(C6H4-4-F)}2] (2) have been obtained by the reaction of the chiral...