Electrocatalytic materials play a crucial role in the development of technologies for hydrogen production (hydrogen evolution reaction) from renewable and sustainable energy resources. Among these materials, nickel sulfides are promising catalysts due to their activity, stability, and cost-effectiveness. However, while the performance of nickel sulfides is linearly correlated to the crystalline structure, synthesis of single crystalline phases of nickel sulfides with controlled morphology is not trivial. In the face of this challenge, we report a simple and selective method to synthesize different phases and morphologies of nickel sulfide with superior electrocatalytic activities, by combining microwave energy and a solvothermal method.
Mononuclear and binuclear Ru II /arene/triphenylphosphine complexes with p-substituted benzoic acid derivatives were prepared and characterized. These monocationic complexes of type [Ru(η 6-p-cymene)(PPh 3)L] (L = benzoic acid (1), p-hydroxybenzoic acid (2), p-nitrobenzoic acid (3) and terephthalic acid (4)) were characterized using various techniques, such as nuclear magnetic resonance (NMR) and matrix-assisted laser desorption/ionization-time of flight (MALDI-TOF) mass spectrometry, and the crystal structure of 1, 3 and 4 were determined by X-ray diffraction analysis. The cytotoxicity of the complexes was evaluated, in vitro, against tumorigenic [MDA-MB-231, MCF-7 (breast), A549 (lung) and DU-145 (prostate)] and non-tumorigenic [MCF-10A (breast), MRC-5 (lung) and PNT-2 (prostate)] cells. The binuclear complex (4) was inactive due to its low solubility. Complexes 1, 2 and 3 showed similar cytotoxicity, however, complex 1 presented better selectivity index against MDA-MB-231 than compounds 2 and 3. Cellular ruthenium absorption was explored by inductively coupled plasma mass spectrometry (ICP-MS) analyzing the whole cells and the culture medium. Complementary studies showed that complex 1 inhibited colony formation, induced morphology changes in cells and promoted cell cycle arrest in the Sub-G1 phase for the MDA-MB-231 cells.
Upon exploration of the chemistry of the combination
of ruthenium/arene
with anthraquinone alizarin (L), three new complexes with the general
formulas [Ru(L)Cl(η6-p-cymene)]
(C1), [Ru(L)(η6-p-cymene)(PPh3)]PF6 (C2), and [Ru(L)(η6-p-cymene)(PEt3)]PF6 (C3) were synthesized and characterized using spectroscopic
techniques (mass, IR, and 1D and 2D NMR), molar conductivity, elemental
analysis, and X-ray diffraction. Complex C1 exhibited
fluorescence, such as free alizarin, while in C2 and C3, the emission was probably quenched by monophosphines and
the crystallographic data showed that hydrophobic interactions are
predominant in intermolecular contacts. The cytotoxicity of the complexes
was evaluated in the MDA-MB-231 (triple-negative breast cancer), MCF-7
(breast cancer), and A549 (lung) tumor cell lines and MCF-10A (breast)
and MRC-5 (lung) nontumor cell lines. Complexes C1 and C2 were more selective to the breast tumor cell lines, and C2 was the most cytotoxic (IC50 = 6.5 μM
for MDA-MB-231). In addition, compound C1 performs a
covalent interaction with DNA, while C2 and C3 present only weak interactions; however, internalization studies
by flow cytometry and confocal microscopy showed that complex C1 does not accumulate in viable MDA-MB-231 cells and is detected
in the cytoplasm only after cell permeabilization. Investigations
of the mechanism of action of the complexes indicate that C2 promotes cell cycle arrest in the Sub-G1 phase in MDA-MB-231,
inhibits its colony formation, and has a possible antimetastatic action,
impeding cell migration in the wound-healing experiment (13% of wound
healing in 24 h). The in vivo toxicological experiments
with zebrafish indicate that C1 and C3 exhibit
the most zebrafish embryo developmental toxicity (inhibition of spontaneous
movements and heartbeats), while C2, the most promising
anticancer drug in the in vitro preclinical tests,
revealed the lowest toxicity in in vivo preclinical
screening.
We have synthesized and characterized three new ruthenium(II) diphosphine complexes containing an acylthiourea ligand, with the general formula [Ru(DPEPhos)(O,S)(bipy)]PF6, where DPEPhos = bis(2-(diphenylphosphino)phenyl)ether, bipy = 2,2’-bipyridine, O,S = N,N-dimethyl-N’-(benzoyl)thiourea (1),...
Background:
Breast cancer is one of the most common types among women. Its incidence progressively
increases with age, especially after age 50. Platinum compounds are not efficient in the treatment of breast cancer,
highlighting the use of other metals for the development of new chemotherapeutic agents.
Objective:
This paper aims to obtain three new ruthenium compounds that incorporate sulfur amino acids in their
structures and to investigate their cytotoxic activity in breast tumor cell lines.
Methods:
Complexes with general formula [Ru(AA)(dppb)(bipy)] (complexes 1 and 2) or [Ru(AA)(dppb)(bipy)]PF6
(complex 3), where AA = L-cysteinate (1), D-penicillaminate (2), and L-deoxyalliinate (3), dppb = 1,4-
bis(diphenylphosphino)butane and 2,2´-bipyridine, were obtained from the cis-[RuCl2(dppb)(bipy)] precursor. The
cytotoxicity of the complexes on MDA-MB-231 (triple negative human breast cancer); MCF-7 (double positive human
breast cancer) and V79 (hamster lung fibroblast) were performed by the MTT (4,5-dimethylthiazol-2-yl-2,5-
diphenyltetrazolium bromide) method. The control agent was the cisplatin, which is a commercially available drug for
cancer treatment.
Results:
In complexes (1) and (2), the ligands are coordinated to the metal center by nitrogen and sulfur atoms, while in
complex (3) coordination is through the oxygen and nitrogen atoms. These suggestions are based on the infrared and
31P1H NMR data. For complexes (1) and (2), their X-ray structures were determined confirming this suggestion. The
three complexes are stable in a mixture of DMSO (80 %) and biological medium (20 %) for at least 48 h and presented
cytotoxicity against the MDA-MB-231 and MCF-7 tumor cells with reasonable selectivity indexes.
Conclusion:
Our work demonstrated that ruthenium complexes containing sulfur amino acids, bipyridines and
bisphosphines showed cytotoxicity against the MDA-MB-231 and MCF-7 cancer cell lines, in vitro, and that they interact
weakly with the DNA (Deoxyribonucleic Acid) and the HSA (Human Serum Albumin) biomolecules.
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