HPLC monitored synthesis of R2NCH2 substituted benzene derivatives used as (C,N)-ligands for organometallic compounds

2-(Diethylaminomethyl)phenyl bromide and 1,3-bis(dimethylaminomethyl)-benzene, useful ligands for the synthesis of hypervalent organometallic compounds, were prepared and characterized by NMR (¹H, ¹³C, 2D experiments) spectroscopy. Their synthesis was monitored by the HPLC method. The compounds were eluted on a Nucleosil 120 Si column (5 μm, 25×0.4 cm) with n-hexane at room temperature using a 1.0 ml/min flow-rate. The maximum values of absorbance for the studied compounds, excepting the diethylamine, were located in a narrow range around 212 nm, the wavelength used for their UV detection. The diethylamine was detected at 190 nm. The calibration curves are straight lines with correlation factors r>0.995. The HPLC data are in good agreement with those provided by NMR spectroscopy.     

HPTLC Quantification of Some Flavonoids in Extracts of Satureja hortensis L. Obtained by Use of Different Techniques

JPC – Journal of Planar Chromatography – Modern TLC - A study of quantitative analysis of some flavonoids in Satureja hortensis L. extracts is presented. The HPTLC analyses were...     

HPTLC Analysis of Thymol in Extracts of Satureja hortensis L. Obtained by Different Techniques

JPC – Journal of Planar Chromatography – Modern TLC - The separation and quantitative analysis of thymol in Satureja hortensis L. extracts is reported. The extracts were obtained by...     

Phytochemistry and Biological Activities of Iris Species Growing in Iraqi Kurdistan and Phenolic Constituents of the Traditional Plant Iris postii

A dozen Iris species (Iridaceae) are considered traditional remedies in Kurdistan, especially for treating inflammations. Phytochemical studies are still scarce. The information reported in the literature about Iris species growing in Kurdistan has been summarized in the first part of this paper, although, except for Iris persica, investigations have been performed on vegetal samples collected in countries different from Kurdistan. In the second part of the work, we have investigated, for the first time, the contents of the methanolic extracts of Iris postii aerial parts and rhizomes that were collected in Kurdistan. Both extracts exhibited a significant dose-dependent free radical scavenging and total antioxidant activities, comparable to those of ascorbic acid. Medium-pressure liquid chromatographic separations of the two extracts afforded l-tryptophan, androsin, isovitexin, swertisin, and 2″-O-α-l-rhamnopyranosyl swertisin from the aerial parts, whereas ε-viniferin, trans-resveratrol 3,4′-O-di-β-d-glucopyranoside, and isotectorigenin were isolated from the rhizomes. This is the first finding of the last three metabolites from an Iris species. The various remarkable biological activities of isolated compounds scientifically sustain the traditional use of I. postii as a medicinal plant.     

ORGANOBISMUTH HOMOCYCLES (RBi)n AND HETEROCYCLES (RBiS)2

The homocycles (RBi)_n (n = 3–5) react with MeC₅ H₄Mn(CO)₂(thf) (thf = tetrahydrofuran) or Fe₂(CO)₉ to give Bi₂[Mn(CO)₂MeC₅ H₄]₃ (1) or Bi₂Fe₃(CO)₉ (3). Reaction of R₄Bi₂ (R = Me₃SiCH₂) with Fe₂(CO)₉ in toluene gives R₂Bi₂Fe₂(CO)₈ (4) and R₄Bi₂Fe(CO)₄ (5). The heterocycles (RBiS)₂(R = 2-(Me₂NCH₂)C₆ H₄ (6), 2, 6-(Me₂NCH₂)₂ C₆ H₄ (7) are formed by reaction of the corresponding dihalides RBiCl₂ with Na₂S. The reaction of (RBiS)₂(R = 2-(Me₂NCH₂)C₆ H₄) with W(CO)₅(thf) leads to (RBiS)₂[W(CO)₅]₂ (8).     

Performance of density‐functional tight‐binding models in describing hydrogen‐bonded anionic‐water clusters

Density‐functional tight‐binding (DFTB) models are computationally efficient approximations to density‐functional theory that have been shown to predict reliable structural and energetic properties for various systems. In this work, the reliability and accuracy of the self‐consistent‐charge DFTB model and its recent extension(s) in predicting the structures, binding energies, charge distributions, and vibrational frequencies of small water clusters containing polyatomic anions of the Hofmeister series (carbonate, sulfate, hydrogen phosphate, acetate, nitrate, perchlorate, and thiocyanate) have been carefully and systematically evaluated on the basis of high‐level ab initio quantum‐chemistry [MP2/aug‐cc‐pVTZ and CCSD(T)/aug‐cc‐pVQZ] reference data. Comparison with available experimental data has also been made for further validation. The self‐consistent‐charge DFTB model, and even more so its recent extensions, are shown to properly account for the structural properties, energetics, intermolecular polarization, and spectral signature of hydrogen‐bonding in anionic water clusters at a fraction of the computational cost of ab initio quantum‐chemistry methods. This makes DFTB models candidates of choice for investigating much larger systems such as seeded water droplets, their structural properties, formation thermodynamics, and infrared spectra. © 2014 Wiley Periodicals, Inc.     

Hypervalent organobismuth(iii) carbonate, chalcogenides and halides with the pendant arm ligands 2-(Me2NCH2)C6H4 and 2,6-(Me2NCH2)2C6H3

R2BiOH (1) [R = 2-(Me2NCH2)C6H4] and (R2Bi)2O (2) are formed by hydrolysis of R2BiCl with KOH. Single crystals of were obtained by air oxidation of (R2Bi)2. The reaction of R2BiCl and Na2CO3 leads to (R2Bi)2CO3 (3). 3 is also formed by the absorption of CO2 from the air in solutions of 1 or 2 in diethyl ether or toluene. (R2Bi)2S (4) is obtained from R2BiCl and Na2S or from (R2Bi)2 and S8. Exchange reactions between R2BiCl and KBr or NaI give R2BiX [X = Br (5), I (6)]. The reaction of RBiCl2 (7) with Na2S and [W(CO)5(THF)] gives cyclo-(RBiS)2[W(CO)5]2 (8). cyclo-(R'BiS)2 (9) [R' = 2,6-(Me2NCH2)2C6H3] is formed by reaction of R'BiCl2 and Na2S. The structures of were determined by single-crystal X-ray diffraction.     

Cobalt(III) dimethylglyoximates containing selenourea and an unusual diselenourea ligand: Synthesis and structures

The complexes [Co(DH)₂(Seu) _y (Se-Seu) _z ]₂X · mSolv (DH is the dimethylglyoxime monoanion, Seu is selenourea, and X is [TiF₆]²⁻, [ZrF₆]²⁻) were obtained from the system CoX · 6H₂O-DH₂-Seu in DMF-MeOH or MeOH-H₂O and examined by UV, IR, and NMR spectroscopy and X-ray diffraction. Unexpectedly, the ligand Se-Seu (the oxidized form of selenourea) was detected on the axial coordinate, partially replacing selenourea. The complexes were formulated as [Co(DH)₂(Seu)_1.75(Se-Seu)_0.25]₂[TiF₆] · H₂O (I) and [Co(DH)₂(Seu)(Se-Seu)]₂[ZrF₆] · 3H₂O (II). The complex cations in I and II have trans-octahedral structures. Their crystal structures are made up of the complex Co³⁺ cations and the outer-sphere MF₆²⁻ anions (M = Ti(IV) (I) and Zr(IV) (II)) held together by electrostatic interactions and hydrogen bonds; water of crystallization is also involved in hydrogen bonding.     

High-Performance Thin-Layer Chromatographic Quantification of Myristicin and Linalool from Leaf Extracts of Microwave-Irradiated Parsley,Dill, and Celery

JPC – Journal of Planar Chromatography – Modern TLC - The aim of the present work was to establish a proper high-performance thin-layer chromatographic (HPTLC) method for the...     

Determination of some frequently used antibiotics in waste waters using solid phase extraction followed by high performance liquid chromatography with diode array and mass spectrometry detection

This study is focused on the determination of some important antibiotics from different classes in waste water samples using solid phase extraction followed by high performance liquid chromatography with two detectors, diode array and mass spectrometer in positive ionisation mode. The investigated antibiotics include three penicillins (amoxicillin, ampicillin, penicillin G), two cephalosporins (ceftazidime, ceftriaxone), and two tetracyclines (tetracycline, doxycycline). The studied antibiotics were extracted from waste water samples using hydrophilic-lipophilic balanced cartridges. The extraction of antibiotics from water matrices was tested at several pH values. The best recoveries were obtained at pH 3 and 7 respectively. Depending on the nature of antibiotic, the limits of detection and quantification were obtained in the range of 0.07–0.92 µg mL^?1 and 0.21–2.77 µg mL^?1 respectively. Influent and effluent waste water samples were collected from a Waste Water Treatment Plant from Romania in order to detect the studied antibiotics. The antibiotics detected in the influent waste water samples were ceftriaxone (334 µg L^?1), tetracycline (146 µg L^?1) and doxycycline (110 µg L^?1). In effluent waste water samples no target antibiotics were detected.