Sinteza i karakterizacija facijalnog i meridijalnog izomera uns-cis-(etilendiamin-N,N’-di-3-propionato)(S-arginin)kobalt(III)-hlorida dihidrata

Both theoretically possible geometrical isomers, facial and meridional, of uns-cis-(ethylenediamine-N,N'-di-3-propionato)(S-arginine)cobalt(III) chloride dihydrate were prepared by the reaction of sodium uns-cis-(ethylenediamine-N,N'-di-3-propionato)(carbonato)cobaltate(III) with S-arginine at 75 degreesC. The complexes were isolated chromatographically and characterized by elemental analysis as well as electron absorption and infrared spectroscopy.Oba teorijski moguća geometrjiska izomera, facijalni i meridijalni uns-cis-(etilendiamin- N,N’-di-3-propionato)(S-arginin)-kobalt(III)-hlorida dihidrata su dobijena reakcijom natrijum-uns-cis-(etilendiamin-N,N'-di-3-propionato)karbonatokobaltata(III) sa S-argininom na temperaturi 75 ºC. Kompleksi su izolovani hromatografski i okarakterisani elementarnom analizom, elektronskom apsorpcionom i infracrvenom spektroskopijom

Synthesis and crystal structure of trans-dichloro(1,3-propylenediamine-N,N '-diacetato)platinum(IV) monohydrate

The trans-geometrical isomer of the first Pt(IV) complex with the tetradentate ligand 1,3-propylenediamine-N,N'-diacetate ion (pdda) was prepared by a direct synthesis from potassium hexachloroplatinate(IV) and pdda in the presence of lithium hydroxide. The crystal structure of trans-[Pt(pdda)Cl-2] (.) H2O complex has been determined. The Pt(IV) ion has a distorted octahedral coordination due to intramolecular N-(HCl)-Cl-... interactions

Preparation and characterization of cobalt(III) complexes with sarcosine and some tetradentate ligands of the edda type

Meridional geometrical isomers of cobalt(III) complexes with sarcosine (N-methylglycine) and tetradentate ligands edda (ethylenediamine-N, N ' -diacetate ion), eddp (ethylenediamine-N, N ' -di-3-propionate ion) and 1,3-pdda (1, 3-propylenediamine-N,N ' -diacetate ion) have been prepared. The edda and eddp cobalt(III) complexes were made by the reaction of sarcosine and sodium ethylenediamine-N, N ' -diacetato(carbonato)cobaltate(III), and sodium uns-cis-(ethylenediamine-N,, N ' -di-3-propionato)(carbonato)cobaltate(III) dihydrate, respectively. The previously synthesized pdda-cobalt(III) complex with sarcosine was obtained by a new route by direct synthesis of cobalt(II) chloride hexahydrate with sarcosine and 1,3-pdda in the presents of lead(IV) oxide. Complexes were isolated chromatographically and characterized by elemental analysis, electron absorption spectra, infrared spectra and H-1 NMR spectroscopy

Synthesis and crystal structure of s-cis-(ethylenediamine-N,N '-diacetato)cobalt(III) complex with N,N-dimethylglycine

The s-cis-geometrical isomer of the cobalt(III) complex with N,N-dimethylglycine (dmgly) and the tetradentate ligand ethylenediamine-N,N'-diacetate ion (edda) was prepared by a direct synthesis from cobalt(II) chloride hexahydrate, N,N-dimethylglycine and edda in the presence of lead(IV) oxide. The complex has been isolated chromatographically and characterized by elemental analyses, electron absorption spectra, infrared spectra and X-ray diffraction analysis

Activity of some platinum(II/IV) complexes with edda-type ligands against human adenocarcinoma HeLa cells

Cisplatin analogues, cis-dichloro(ethylenediamine-N,N'-di-3-propanoic acid)platinum(II) (1) and cis-iodo(ethylenediamine-N,N'-di-3-propanoic acid) platinum(II) (2), as well as trans-dichloro(ethylenediamine-N,N'-di-3-propanoato)platinum(IV) (3), trans-dibromo(ethylenediamine-N,N'-di-3-propanoato)platinum(IV) (4), trans-dichloro(propylenediamine-N,N'-diacetato)platinum(IV) (5) and trans-dibromo(propylenediamine-N,N'-diacetato)platinum(IV) (6), -([Pt(H(2)eddp)Cl(2)], [Pt(Heddp)I], trans-[Pt(eddp)Cl(2)], trans-[Pt(eddp)Br(2)], trans-[Pt(pdda)Cl(2)] and trans-[Pt(pdda)Br(2)], respectively) were used to assess antitumor selectivity against human adenocarcinoma HeLa cells. The results show that different oxidation states of platinum, different halide ligands, chelating aminocarboxylato and diamine backbones have similar effects with edda-type ligands and activity is lower than for cisplatin

Activity of some platinum(II/IV) complexes with O,O-n-butyl-and O,O-n-pentyl-ethylenediamine-N,N '-di-3-propanoate and halogeno ligands against HeLa and K562 cell lines and human PBMC

This paper reports on syntheses and characterization of chlorotribromo(O,O-n-butyl-ethylenediamine-N,N'-di-3-propanoate)platinum(IV) [II], dichlorodiiodo(O,O-ii-butyl-ethylenediamine-N,N'-di-3-propanoate)platinum(IV) [III], and dichloro(O,O-n-butyl-ethylenediamine-N,N'-di-3-propanoate)platinum(II) [V] complexes, with the formulae [Pt(dbeddp)Br3Cl], [Pt(dbeddp)Cl2I2] and [Pt(dbeddp)Cl-2], respectively. The complexes were characterized by elemental analysis, infrared, H-1 and C-13 NMR spectroscopy and electrospray mass spectrometry. In the aim to assess the selectivity in the antitumor action of these complexes, as well, as tetrachloro(O,O-n-butyl-ethylenediamine-N,N'-di-3-propanoate)platinum(IV) [I] and tetrachloro(O,O-n-pentyl-ethylenediamine-N,N'-di-3-propanoate)platinum(IV) [IV], the antiproliferative action of these compounds was determined to human adenocarcinoma HeLa cells, to human myelogenous leukemia K562 cells and to normal immunocompetent cells, i.e., on human peripheral blood mononuclear PBMC cells. (C) 2004 Elsevier Inc. All rights reserved

Syntheses and activity of some platinum(IV) complexes with N-methyl derivate of glycine and halogeno ligands against HeLa, K562 cell lines and human PBMC

Four platinum(IV) complexes, trans,trans-dichlorobis(N,N-dimethylglycinato)platinum(IV), trans,trans-[Pt(dmgly)(2)Cl-2] (1) and trans.trans-dibromobis(N,N'-dimethylglycinato)platinum(IV), trans,trans-[Pt(dmgly)(2)Br-2] (2), as well as, trans,trans-dichlorobis(N-methylglycinato)platinum(IV), trans,trans-[Pt(sar)(2)Cl-2] (3) and trans,trans-dibromobis(N-methylglycinato)platinum(IV), trans,trans-[Pt(sar)(2)Br-2] (4) (with configuration index for all complexes OC-6-14), were synthesized and characterized by elemental analysis, infrared and H-1 NMR spectroscopy. In the aim to assess the selectivity in the antitumor action of these complexes, the antiproliferative action of these compounds was determined to human adenocarcinoma HeLa cells; to human myelogenous leukemia K562 cells and to normal immunocompetent cells; i.e., on human PBMC. The details of the crystal structure synthesized trans,trans-[Pt(sar)(2)Br-2] complex were also reported here. In the crystal structure of trans, trans-[Pt(sar)(2)Br-2] the Pt(IV) ion had a deformed octahedral coordination with both N-methylglycinates and bromides bonded trans to one another and with the NPt-Br bond angles of 84.1(4) and 95.9(4)degrees. The trans, trans-[Pt(sar)(2)Br-2] complex molecules form 2D-layers with multiple N-H (...) O and C-H (...) O hydrogen bonds. (c) 2005 Elsevier B.V. All rights reserved

Benzo[a]pyrene, benz[a]anthracene, benzo[b]fluoranthene and chrysene in smoked meat and smoked meat products - validation of the method

Polycyclic aromatic hydrocarbons (PAHs) are products of the incomplete combustion or pyrolysis of organic material and they are among the most harmful compounds. During process of meat smoking, wood combustion is one of the most important sources of PAH compounds, which can be adsorbed by the surface of meat. The EFSA (European Food Safety Authority) Panel on Contaminants in the Food Chain (CONTAM Panel) recommended to the member states of European Union to use the sum of benzo[a] pyrene (BaP), benz[a] anthracene (BaA), benzo[b] fluoranthene (BbF) and chrysene (CHR), (PAH4 compounds), as a marker for the occurrence and impact of carcinogenic PAHs in food, instead of benzo[a]pyrene. The maximum content of BaP and sum of all four compounds (PAH4) has been established by European Commission Regulation No. 835/2011. For smoked foods, from 1st September 2014, the maximum BaP content was lowered to 2 mu g/kg, while the content of PAH4 is allowed to 12 mu g/kg. The new maximum residue limits (MRL) both for BaP and sum of PAH4 compounds in smoked meat and meat products were defined by the legislation of Serbia, as well, and it is in accordance with EU regulation. The aim of this paper was the validation of the method for identification and determination of benzo[a] pyrene, chrysene, benz[a] anthracene and benzo[b] fluoranthene in smoked meat and smoked meat products. Accelerated solvent extraction (ASE) was used for extraction of lipids and lipophilic compounds. Solid Phase Extraction (SPE) was used in order to remove lipids from analysed samples. High-performance liquid chromatographic with fluorescence detection (HPLC-FL) was applied for identification and quantification of PAH4 compounds. Fluorescence detector operated at excitation/emission wavelength 275/385 nm for BaA and CHR, 256/446 nm for BbF and 260/410 nm for BaP, respectively. On the base of experimental results, it is possible to conclude as follows: The in-house validation procedure of the method meets all criteria (applicability, specificity, repeatability, reproducibility, recovery, LOD and LOQ) set out by EU Regulation No. 836/2011. The method is suitable for operative control of PAH4 content in smoked meat products