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In the present work, we have included for the first time diamond nanoparticles (DNPs) in a sol-gel matrix derived from (3-mercaptopropyl)-trimethoxysilane (MPTS) in order to improve electron transfer in a lactate oxidase (LOx) based electrochemical biosensing platform. Firstly, an exhaustive AFM study, including topographical, surface potential (KFM) and capacitance gradient (CG) measurements, of each step involved in the biosensing platform development was performed. The platform is based on gold electrodes (Au) modified with the sol-gel matrix (Au/MPTS) in which diamond nanoparticles (Au/MPTS/DNPs) and lactate oxidase (Au/MPTS/DNPs/LOx) have been included. For the sake of comparison, we have also characterized a gold electrode directly modified with DNPs (Au/DNPs). Secondly, the electrochemical behavior of a redox mediator (hydroxymethyl-ferrocene, HMF) was evaluated at the platforms mentioned above. The response of Au/MPTS/DNPs/LOx towards lactate was obtained. A linear concentration range from 0.053 mM to 1.6 mM, a sensitivity of 2.6 muA mM-1 and a detection limit of 16 muM were obtained. These analytical properties are comparable to other biosensors, presenting also as advantages that DNPs are inexpensive, environment-friendly and easy-handled nanomaterials. Finally, the developed biosensor was applied for lactate determination in wine samples.

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Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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Matrix materials, such as sol-gels and polymers derivatives to contain a redox active material can be used to form electrodes and probes suitable for use in pH meters and other analyte sensing devices.

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Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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We investigate the Faradaic currents of ferrocene species at an electrode-membrane-electrode system. The membrane electrodes system is fabricated by physical sputtering of conductive metal on both sides of a nanoporous alumina membrane. The metal coatings function as working electrodes by connection to a bipotentiostat and reference/counter electrodes in the sample solution. Collection and shielding efficiency studies are carried out at this membrane electrodes system to measure mobility values of charged ferrocene species within nanochannels of alumina membrane. Results indicated high selective electrode response of up to 16 times for positively charged (dimethylaminomethyl)ferrocene (FcN), and neutral ferrocenemethanol (FcMeOH), compared to the negatively charged ferrocenecarboxylic acid (FcCOOH) when the receiver electrode was maintained at negative potentials of 0.5-1.0 V relative to the feed electrode. This is a report on the use of an electrode-membrane-electrode system to achieve selective response towards differently charged redox species, under the condition of high electrolyte concentration (0.1 M, pH 7.0 phosphate buffer).

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Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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Suitably blocked carbohydrates containing free thio 4, amino 5, and hydroxyl 10,19 nucleophilic functionalities have been treated with (a) ferrocenecarbonyl chlorides 2 and 3. (b) N,N-dimethylaminomethylferrocene methiodide 12, and (c) ferrocenyl tosylate 16 to form the ferrocenyl sugar derivatives 6,7,8,9,11,13,14,15 and 20.Direct conjugation of a free, water-soluble sugar to ferrocene was achieved by the formation of a Schiff’s base between glucosamine hydrochloride 25 and ferrocene carboxaldehyde 24.The synthesis of ferrocenyl sugars using bridging group technology is exemplified by the conjugation of the thio sugar 4 to ferrocene via the versatile coupling reagent cyanuric chloride 21 to form the s-triazine compound 23.These products have been studied by 1H nmr spectroscopy: chemical shifts, coupling constants, and proton spin-lattice relaxation measurements.

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Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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Mononuclear Zr complexes CpZrCl2{eta5-C 5H4(CH2)nCH=CH2} (n = 1, 2, 3) undergo intermolecular metathesis of the vinyl group catalyzed by a Ru complex to produce dinuclear complexes with bridging ligands, (CpZrCl 2)2 {mu-eta5-eta5-C 5H4(CH2)nC5H 4}. Hydrogenation of the products catalyzed by Pd/C affords complexes with a flexible polymethylene chain that bridges two Cp2ZrCl 2 groups. A dinuclear complex with a bridging bisfluorenyl ligand, (CpZrCl2)2(mu-eta5,eta5-C 13H8CH2CH=CHCH2C13H 8), is also obtained from the metathesis of a mononuclear Zr complex with the allylfluorenyl ligand. X-ray crystallography of (CpZrCl 2)2(mu-eta5,eta5-C 13H8CH2CH=CHCH2C13H 8) revealed the molecular structure with a trans-C=C double bond and the two Zr centers situated at different sides of the bridging bisfluorenyl ligand. Cross metathesis reaction of CpZrCl2{eta5-C 5H4(CH2)2CH=CH2} and ferrocenylmethyl acrylate produces the Zr/Fe dinuclear complex CpZrCl 2{mu-eta5,eta5-C5H 4(CH2)2-CH=CHCOOCH2C 5H4}FeCp. The dinuclear complexes catalyze polymerization of ethylene and propylene in the presence of MAO (methylaluminoxane). The activity of the Zr/Zr dinuclear complexes for ethylene polymerization is higher than that of the mononuclear precursors. The length and flexibility of the bridging group of the biscyclopentadienyl ligand also influence the catalytic activity.

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Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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Organometallic Ru(II)-cymene complexes linked to ferrocene (Fc) via nitrogen heterocycles have been synthesized and studied as cytotoxic agents. These compounds are analogues of Ru(II)-arene piano-stool anticancer complexes such as RAPTA-C. The Ru center was coordinated by pyridine, imidazole, and piperidine with 0-, 1-, or 2-carbon bridges to Fc to give six bimetallic, dinuclear compounds, and the properties of these complexes were compared with their non-Fc-functionalized parent compounds. Crystal structures for five of the compounds, their Ru-cymene parent compounds, and an unusual trinuclear compound were determined. Cyclic voltammetry was used to determine the formal MIII/II potentials of each metal center of the Ru-cymene-Fc complexes, with distinct one-electron waves observed in each case. The Fc-functionalized complexes were found to exhibit good cytotoxicity against HT29 human colon adenocarcinoma cells, whereas the parent compounds were inactive. Similarly, antibacterial activity from the Ru-cymene-Fc compounds was observed against Bacillus subtilis, but not from the unfunctionalized complexes. In both cases, the IC50 values correlated quantitatively with the Fc+/0 reduction potentials. This is consistent with more facile oxidation to give ferrocenium, and subsequent generation of toxic reactive oxygen species, leading to greater cytotoxicity. The antioxidant properties of the complexes were quantified by a 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging assay. EC50 values indicate that linking of the Ru and Fc centers promotes antioxidant activity.

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Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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The rapid and accurate determination of specific circulating biomarkers at different molecular levels with non- or minimally invasive methods constitutes a major challenge to improve the breast cancer outcomes and life quality of patients. In this field, electrochemical biosensors have demonstrated to be promising alternatives against more complex conventional strategies to perform fast, accurate and on-site determination of circulating biomarkers at low concentrations in minimally treated body fluids. In this article, after discussing briefly the relevance and current challenges associated with the determination of breast cancer circulating biomarkers, an updated overview of the electrochemical affinity biosensing strategies emerged in the last 5 years for this purpose is provided highlighting the great potentiality of these methodologies. After critically discussing the most interesting features of the electrochemical strategies reported so far for the single or multiplexed determination of such biomarkers with demonstrated applicability in liquid biopsy analysis, existing challenges still to be addressed and future directions in this field will be pointed out.

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Iron Catalysis in Organic Synthesis | Chemical Reviews,
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Herein we describe a simple approach for fabrication of microring electrodes by electroless plating a thin layer of gold on polycarbonate (PC) rods. First, the PC rod was exposed to UV light to generate carboxyl groups on the surface. After amination of the surface carboxyl groups by ethylenediamine, the rod was sequentially immersed in HAuCl4 and NaBH4 solutions to form a layer of gold nanoparticles. These gold nanoparticles then functioned as the catalytically active centers for electroless plating thin gold film on the PC rod surface. Finally, the rod surface was thoroughly covered by an insulating glue and fresh microring surface could be obtained easily by laterally cutting with a knife. The electrochemical behavior of thus prepared microring electrodes were characterized by cyclic voltammetry in hydroxymethylferrocene and H2SO4. The whole fabrication process is simple and economic, which can be carried out in ordinary laboratories. In addition, the results of electrocatalytic oxygen reduction demonstrated that the proposed microelectrode could be used as an alternative electrode materials for electrocatalysis and electroanalysis.

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Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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New ferrocenylalkylimidazolium salts [Fc(CH2)n(C3H3N2)R]X- were synthesised through the incorporation of green chemistry principles of atom economy and when feasible under solvent-free conditions. The products comprise a series of salts all characterised by the ferrocenyl moiety with variations in the length of the linker alkyl chain (n), the size of the imidazolium alkyl substituent (R) or the electronic nature of the counter-ion (X-). The dependence of the physical and electronic properties of the salts on the three main structural variants was studied. It was found that variation in the steric size of the R group has the most profound influence on the melting points of the ionic liquids. The compounds were fully characterised by IR, 1H and 13C NMR, MS and melting point determinations.

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Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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A new chiral ferrocene-labelled tyrosine PNA monomer 1 has been synthesised in good yield in both racemic and enantiomerically pure forms. It is suitable for insertion in various positions of PNA oligomers, a possibility that has been preliminarily demonstrated by synthesising the dimer 16. Moreover, in view of possible applications to nucleic acid detection, a preliminary voltammetric investigation on the electrochemical activity of monomer 1 and its synthetic precursors has been carried out in DMF. It appears that, despite the bulkiness of the PNA monomer backbone, its insertion on the ferrocene group only moderately lowers the latter’s diffusion coefficients and peak currents, thus affording voltammetric detection limits in the order of 10-6-10 -7 M.

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Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion