Unsymmetrical Mesoporphyrinic Complexes of Copper (II) and Zinc (II). Microwave-Assisted Synthesis, Spectral Characterization and Cytotoxicity Evaluation

New unsymmetrical mesoporphyrinic complexes, namely 5-(4-hydroxyphenyl)-10,15,20–tris-(4-carboxymethylphenyl)–21,23-Zn(II)-porphine and 5-(4-hydroxyphenyl)-10,15,20–tris-(4-carboxymethylphenyl)–21,23-Cu(II)-porphine, were synthesized using a microwave irradiation method. The structures of the porphyrinic complexes were confirmed using FT-IR, UV–Vis, EPR and NMR spectral data. The spectral absorption and emission properties of the porphyrinic complexes were studied in organic solvents of different polarities and the influence of solvent polarity on the wavelengths of the absorbance and fluorescence band maxima is described. The cytotoxicity evaluation of the porphyrinic complexes was performed on human colon adenocarcinoma cell line HT29 for different doses and incubation times. The obtained result indicates a lack of or low toxicity for both compounds, thus recommending them for further testing in light activation protocols

Microwave Assisted Digestion of Heroin Street Samples for Trace Metals Analysis by Inductively Coupled Plasma Mass Spectrometry

The present paper describes the development of a microwave acid digestion procedure for street heroin samples in order to achieve sample dissolution prior the determination of major and trace elements employing inductively coupled plasma mass spectrometry (ICPMS

Investigation of Uncertainty Contributions for Elemental Analysis of Sesized Street Heroin by ICPMS

The aim of the study was the identification and quantification of uncertainty sources associated with heroin elemental analysis by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) following sample dissolution through microwave assisted acid digestion. The percentage contribution of each source to the relative combined uncertainty was also calculated. The "bottom-up" approach The main objective of quantitative analysis is to obtain the most reliable analytical results, which must reflect unambiguously true and clear values of sample composition As measurement uncertainty estimation is considered an important part of the method validation procedure, the list of guidelines and works dedicated to this topic is getting longer every year. Previous studies about uncertainty determination in drugs of abuse analysis referred mostly to chromatographic techniques such as GC-FID [4], GC-MS [5,6] HPLC The level of inorganic impurities in seized drugs was also investigated In what method validation and, particularly, measurement uncertainty estimation are concerned, there is a gap in the area of illicit drug elemental analysis by Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Our study aimed to evaluate the uncertainty related to determination of metal content in seized heroin by ICP-MS. The contribution of each uncertainty source was investigated in order to identify solutions for the improvement of the combined measurement uncertainty. Experimental part Reagents and calibration standards Acid digestion of the samples was carried out with a mixture of nitric acid (60% volume concentration of HNO 3 * email: [email protected]; Tel.: +40742285994 ultrapure , Merck) and hydrogen peroxide (30% volume concentration of H 2 O 2 p.a., Fluka). Multi-element calibration Standard 3 (Ag, Al, As, Ba, Be, Bi, Ca, Cd, Co, Cr, Cs, Cu, Fe, Ga, In, K, Li, Mg, Mn, Na, Ni, Pb, Rb, Se, Sr, Ti, V, U, Zn, for each 10 μg/mL) and Yttrium solution (1000 μg/mL) from Perkin Elmer were employed for calibration of the instrument and internal standardization respectively. Single element standard solutions (Al, Co, Cu, Mg, for each 1000 μg/mL) were used for the fortification of blank and sample solutions. All solutions were prepared or diluted with double deionized water (specific resistance 18.2 MΩcm -1 ) from a Milli-Q Millipore water purification system. Preparation of standard solutions Standard solutions were prepared just before analysis through a serial dilution method ( Sample preparation Heroin samples were weighed using a CP224S-0CE Sartorius electronic analytical balance and a microwave oven decomposition system (Multiwave 3000 with Rotor 8SXQ80, Anton Paar GmbH, Graz) was involved for samples microwave assisted acid digestion following a particular procedure described in our prior published work [16]

Microwave Synthesis Under Solvent-Free Conditions and Spectral Studies of Some Mesoporphyrinic Complexes

A series of A<sub>3</sub>B and A<sub>4</sub> type mesoporphyrinic complexes were synthesized with superior yields using microwave irradiation under solvent-free conditions. The structures of the complexes were confirmed using elemental analysis, FT-IR, UV-Vis, EPR and NMR spectral data. The influence of environmental polarity on spectral properties of the mesoporphyrinic complexes was investigated. The obtained results indicate that the shape of absorption and fluorescence spectra does not depend on the solvent polarity under the experimental conditions used. The small shifts of the absorption and emission maximums that occur by increasing of solvent polarity reflects the physical<strong> </strong>interaction between the porphyrinic substituents and the solvent molecules

Spectroscopic Behavior of Some A3B Type Tetrapyrrolic Complexes in Several Organic Solvents and Micellar Media

The paper presents spectral studies of some unsymmetrical A3B tetrapyrrolic, porphyrin-type complexes with Cu(II) and Zn(II) in different solvents and micellar media aimed at estimating their properties in connection with the living cell. The results indicate that the position of the absorption and emission peaks is mostly influenced by the central metal ion and less by the environmental polarity or the peripheric substituents of the porphyrinic core. The comparison between the overall absorption and emission spectra of the compounds in methanol or cyclohexane vs. direct and reverse Triton X micellar systems, respectively, suggests for all compounds the localization at the interface between the polyethylene oxide chains and the tert-octyl-phenyl etheric residue of the Triton X-100 molecules. These findings could be important when testing the compounds embedded in liposomes or other delivery systems to the targeted cell

Synthesis, Spectral Analysis and Preliminary in Vitro Evaluation of Some Tetrapyrrolic Complexes with 3d Metal Ions

In this paper, two tetrapyrrolic complexes, Zn(II)-5-(3-hydroxyphenyl)-10,15,20-tris-(4-acetoxy-3-methoxyphenyl)porphyrin and Cu(II)-5-(3-hydroxyphenyl)-10,15,20-tris-(4-acetoxy-3-methoxyphenyl)porphyrin were synthesized, and characterized from a spectral and biological point of view. The study provided data concerning the behavior of identical external substituents vs. two different core insertions. Some of the properties of the proposed tetrapyrrolic structures were highlighted, having photodynamic therapy of cancer as a targeted biomedical application. Elemental analysis, NMR, FTIR and UV-Vis data in various solvents were provided. A preliminary in vitro study on normal and cancer cultured cells was carried out for biocompatibility assessment in dark conditions. The preliminary in vitro study performed on human peripheral mononuclear cells exposed to tetrapyrrolic compounds (2 µM) showed that the proposed compounds had a convenient cytotoxic profile on human normal peripheral blood mononuclear cells under dark conditions. Meanwhile, the investigated compounds reduced the number of metabolically active breast tumor MCF-7 cells, with the exception of Zn(II) complex-containing a symmetrical ligand. Accordingly, preliminary in vitro data suggest that the proposed tetrapyrrolic compounds are good candidates for PDT, as they limit tumor expansion even under dark conditions, whilst sparing normal cells