A Polydimethylsiloxane Rod Extraction-Based Method for the Determination of Pharmaceuticals and Triclosan by Liquid Chromatography in Water Samples.

A new analytical method for the determination of naproxen, ketoprofen, diclofenac, carbamazepine, and triclosan (TCS) in water samples by liquid chromatography is developed and validated. The method is based on the extraction of the analytes by a polydimethylsiloxane (PDMS) rod. The different parameters affecting extraction, such as the addition of salt, pH, initial volume, extraction and elution times and elution solvent, as well as the application of sonication, are studied. The results showed that the detection limits are all in the 0.1-0.3 µg L-1 range except for carbamazepine (6 µg L-1) with relative standard deviations in the range of 0.4%-9.7%. The method developed, which was validated by analysing spiked surface water samples at 10, 25 and 75 µg L-1 gave recoveries of between 84.8% and 111.2%. In the case of carbamazepine, a recovery of 99.1% was obtained at 75 µg L-1. The main advantage of the developed method is that allows high performance liquid chromatography-diode array detection, which is widely available in non-specialised laboratories, to be applied for pharmaceuticals and TCS determination in surface waters after performing a preconcentration/clean-up step with PDMS rods as it has been shown by analysing real water samples.

Fluorescent BODIPY-Anionic Boron Cluster Conjugates as Potential Agents for Cell Tracking.

A series of novel fluorescent BODIPY-anionic boron cluster conjugates bearing [B12H12]2- (5, 6), [3,3'-Co(1,2-C2B9H11)2]- (7, 8), and [3,3'-Fe(1,2-C2B9H11)2]- (9) anions have been readily synthesized from meso-(4-hydroxyphenyl)-4,4-difluoro-4-bora-3 a,4 a-diaza- s-indacene (BODIPY 4), and their structure and photoluminescence properties have been assessed. Linking anionic boron clusters to the BODIPY (4) does not alter significantly the luminescent properties of the final fluorophores, showing all of them similar emission fluorescent quantum yields (3-6%). Moreover, the cytotoxicity and cellular uptake of compounds 5-9 have been analyzed in vitro at different concentrations of B (5, 50, and 100 µg B/mL) using HeLa cells. At the lowest concentration, none of the compounds shows cytotoxicity and they are successfully internalized by the cells, especially compounds 7 and 8, which exhibit a strong cytoplasmic stain indicating an excellent internalization efficiency. To the best of our knowledge, these are the first BODIPY-anionic boron cluster conjugates developed as fluorescent dyes aiming at prospective biomedical applications. Furthermore, the cellular permeability of the starting BODIPY (4) was improved after the functionalization with boron clusters. The exceptional cellular uptake and intracellular boron release, together with the fluorescent and biocompatibility properties, make compounds 7 and 8 good candidates for in vitro cell tracking.

Antioxidant and α-amylase inhibitory activities of extract and isolates from Zygogynum pancheri subsp. arrhantum.

One new sesquiterpenoid (5R(*),8R(*),9R(*),10R(*))-cinnamolide (8), and seven known compounds, 5-hydroxy-7-methoxyflavonone (1), 8-hydroxy-3-(4'-hydroxyphenyl)-6,7-(2″,2″-dimethylchromene)-tetralone (2), 8-hydroxy-3-(3',4'-dihydroxyphenyl)-6,7-(2″,2″-dimethylchromene)-tetralone (3), 1ß-E-O-p-methoxycinnamoyl-bemadienolide (4), 1ß-O-(E-cinnamoyl)-6α-hydroxy-9-epi-polygodial (5), 1ß-O-(E-cinnamoyl)-6α-hydroxypolygodial (6), and 1ß-O-E-cinnamoylpolygodial (7) were isolated from the ethyl acetate extract of barks of Zygogynum pancheri subsp. arrhantum (Winteraceae). The structures of these molecules were assigned predominantly based on spectral data. The structure of compound 8 was confirmed by X-ray crystallographic analysis. Compounds 2 and 3 exhibited significant antioxidant activity, whereas compounds 1 and 4-7 showed significant α-amylase inhibitory activity.

The interpenetrated three-dimensional framework of a new mixed lithium/ammonium perchlorate grown in a gel medium.

Mixed lithium/ammonium perchlorate, Li(0.41)(NH4)(0.59)ClO4, has been prepared by gel diffusion using agar agar gel as the medium of growth at ambient temperature. The Cl and mixed Li/N atoms are located on the 4a (½, ½, ½) and 4b (½, 0, ») special positions, respectively, in the space group I42d. The structure features a twofold interpenetrated three-dimensional entanglement architecture, in which single three-dimensional networks are constructed from tetrahedral coordination based on [-(ClO4)-(Li/NH4)-(ClO4)-]∞ diamondoid arrays. A comparison of the crystal structures of Li(0.41)(NH4)(0.59)ClO4, LiClO4·3H2O, LiClO4 and NH4ClO4 is given.

The solid solution (Fe0.81Al0.19)(H2PO4)3 with a strong hydrogen bond.

Single crystals of the solid solution iron aluminium tris(dihydrogenphosphate), (Fe(0.81)Al(0.19))(H(2)PO(4))(3), have been prepared under hydrothermal conditions. The compound is a new monoclinic variety (gamma-form) of iron aluminium phosphate (Fe,Al)(H(2)PO(4))(3). The structure is based on a two-dimensional framework of distorted corner-sharing MO(6) (M = Fe, Al) polyhedra sharing corners with PO(4) tetrahedra. Strong hydrogen bonds between the OH groups of the H(2)PO(4) tetrahedra and the O atoms help to consolidate the crystal structure.

Redetermination of K(4)[Bi(2)Cl(10)]·4H(2)O.

In comparison with the previous refinement of tetra-potassium di-µ-chlorido-bis-[tetra-chloridobismuthate(III)] tetra-hydrate [Volkova, Udovenko, Levin & Shevchenko (1983). Koord. Khim.9, 356-360], the current redetermination reveals anisotropic displacement parameters for all non-H atoms, localization of the H atoms, and higher precision of lattice parameters and inter-atomic distances. The crystal structure is built up of edge-sharing [Bi(2)Cl(10)](4-) double octa-hedra with the bridging Cl atoms situated on a mirror plane, three K(+) counter-cations (two of which are on mirror planes), and two water mol-ecules that are solely coordinated to the K(+) cations. These building units are linked into a three-dimensional network structure. Additional O-H⋯Cl hydrogen bonds between the water mol-ecules and the complex anions stabilize this arrangement.

N-Methyl-isosalsoline from Hammada scoparia.

THE TITLE COMPOUND (SYSTEMATIC NAME: 1,2-dimethyl-6-meth-oxy-1,2,3,4-tetra-hydro-isoquinolin-7-ol), C(12)H(17)NO(2), is a major alkaloid isolated from Hammada scoparia leaves. It belongs to the isoquinoline family and it was characterized by NMR spectroscopy and X-ray crystallographic techniques. The absolute configuration could not be reliably determined. An intermolecular O-H⋯N hydrogen bond is present in the crystal structure.

N-(Hydroxymethyl)ibogaine.

THE TITLE COMPOUND (SYSTEMATIC NAME: 16-hydroxy-methyl-12-methoxy-ibogamine), C(21)H(28)N(2)O(2), was prepared by reaction of ibogaine with a formaldehyde-acetic acid solution (pH = 4). The crystal structure of this new product, belonging to the iboga indole family, is stabilized by an inter-molecular O-H⋯N hydrogen bond. The identity of the compound was confirmed by one- and two-dimensional NMR spectroscopic techniques.

Ethyl 6-amino-5-cyano-4-isopropyl-2-methyl-4H-pyran-3-carboxyl-ate.

In the title compound, C(13)H(18)N(2)O(3), the two H atoms of the NH(2) group are engaged in hydrogen bonding with the N atom of the cyano group and with one O atom of the ethoxy-carbonyl group, building a chain parallel to the [100] direction. The N-H⋯N hydrogen bonds assemble the mol-ecules around inversion centres, forming dimers with an R(2) (2)(12) graph-set motif.

[Yb(H(2)O)(8)][Cd(3)Cl(9)(H(2)O)].6H(2)O.

The title compound, namely octaaquaytterbium(III) aquanonachlorotricadmate(II) hexahydrate, [Yb(H(2)O)(8)][Cd(3)Cl(9)(H(2)O)].6H(2)O, was prepared by evaporation at 278 K from an aqueous solution of the ternary system YbCl(3)-CdCl(2)-H(2)O and was characterized by elemental chemical analysis and by X-ray powder and single-crystal diffraction studies. The crystal structure can be viewed as being built from layers of double chains of CdCl(6) and CdCl(5)(H(2)O) octahedra separated by antiprismatic [Yb(H(2)O)(8)](3+) cations. The stabilization of the structure is ensured by O-H.O and O-H.Cl hydrogen bonds. A comparison with the structures of SrCd(2)Cl(6).8H(2)O and CeCd(4)Cl(11).13H(2)O is presented.

Lead bismuth calcium sodium phosphate: Pb4.6Bi0.4Ca2.6Na2.4(PO4)6.

The title compound, lead bismuth calcium sodium phosphate, Pb(4.6)Bi(0.4)Ca(2.6)Na(2.4)(PO(4))(6) crystallizes in the apatite structure type, with vacancies in sites 2a or 2b that are normally occupied by anions. The fact that the Bi and Pb ions are mainly localized in the 6h sites confirms the electron lone-pair influence on the apatite structure.

Strontium hexabromodicadmate(II) octahydrate.

The ternary system SrBr(2)-CdBr(2)-H(2)O was investigated at room temperature. The title phase, SrCd(2)Br(6) x 8H(2)O, has been isolated from this system and its structure determined by single-crystal X-ray diffraction. The structure consists of infinite double chains of CdBr(6) octahedra and chains of Sr(H(2)O)(9) polyhedra packed along the b axis. The interaction between these two isolated chains occurs through O-H.O and O-H...Br hydrogen bonds. The structure is compared with that of SrCd(2)Cl(6) x 8H(2)O.