Investigation of the electrochemical properties of edoxaban using glassy carbon and boron-doped diamond electrodes and development of an eco-friendly and cost effective voltammetric method for its determination.

In this study, the highly risky drug Edoxaban (EDX), which can threaten life and cause bleeding, was electro analytically evaluated. The electrochemical behavior of EDX was investigated using glassy carbon electrode (GCE) and boron-doped diamond electrode (BDDE). In this study, for the first time, a simple, rapid, sensitive, and selective voltammetric technique was developed by using different electrodes for the electrochemical characterization and detection of EDX. The optimized voltammetric technique showed anodic signals of EDX at +1.09 V and +1.08 V on GCE and BDDE, respectively, in BR (pH 5.0) solution. The developed voltammetric method provided a very good analytical working range for EDX in BR (pH 5.0) solution on GCE and BDDE, covering concentration ranges from 1.84 µM to 12.88 µM and from 3.68 µM to 14.72 µM, respectively. The limits of detection for EDX on GCE and BDDE under these experimental conditions were calculated as 0.24 µM and 0.57 µM, respectively. The developed voltammetric methods on both electrodes were successfully applied to urine and tablet samples. Additionally, the obtained voltammetric results were compared with UV-Vis spectroscopy results.

Fluorescence Properties and Electrochemical Behavior of Some Schiff Bases Derived from N-Aminopyrimidine.

A series of Schiff bases (L 1 , L 2 and L 3) were prepared by refluxing aromatic aldehydes with N-Aminopyrimidine derivatives in methanol and ethanol. The structures of synthesized compounds were characterized by FTIR, (1)H NMR, (13)C NMR and microanalysis. The electrochemical behaviors of the Schiff base ligands were also discussed. Moreover, the evaluation of absorption and emission properties of the structures were carried out in five different solvents. The products show visible absorption maxima in the range of 304-576 nm, and emission maxima from 636 to 736 nm in all solvents tested.

First electrochemical investigation and determination of non-steroidal anti-inflammatory drug etofenamate using disposable pencil graphite electrode with voltammetric techniques.

In this study, the electrochemical properties of etofenamate, an active ingredient belonging to the non-steroidal anti-inflammatory drug group, were investigated using cyclic voltammetry (CV) and square wave voltammetry (SW) techniques on a disposable pencil graphite electrode (PGE). With the CV technique, reversible voltammetric waves of around +0.470 V and irreversible voltammetric waves of around +1.02 V were produced on the PGE. An environmentally friendly, selective and highly sensitive SW voltammetric method was developed using disposable PGE. This voltammetric method gave very good analytical working range on PGE in PBS (pH = 3.0) medium at concentrations ranging from 0.017 µM to 0.306 µM. The LOD value of this analytical method in PBS (pH = 3.0) medium was calculated as 0.0011 µM (0.406 µg L-1). The developed voltammetric method was successfully applied to urine and drug samples. The results of the voltammetric method were compared with the results of the spectrophotometric method. The results were found to be compatible with each other.

Voltammetric studies and spectroscopic investigations of the interaction of an anticancer drug bevacizumab-DNA and analytical applications of disposable pencil graphite sensor.

A sensitive, simple, fast electrochemical biosensor for the DNA interaction of bevacizumab (BEVA), which is used as a targeted drug in cancer treatment, was developed using the differential pulse voltammetry (DPV) technique with pencil graphite electrode (PGE). In the work, PGE was electrochemically activated in a supporting electrolyte medium of +1.4 V/60 s (PBS pH 3.0). Surface characterization of PGE was carried out by SEM, EDX, EIS, and CV techniques. Determination and electrochemical properties of BEVA were examined with CV and DPV techniques. BEVA gave a distinct analytical signal on the PGE surface at a potential of +0.90 V (vs. Ag/AgCl). In the procedure proposed in this study, BEVA gave a linear response on PGE in PBS (pH 3.0 containing 0.02 M NaCl) (0.1 mg mL-1 - 0.7 mg mL-1) with LOD and LOQ values of 0.026 mg mL-1 and 0.086 µg mL-1, respectively. BEVA was reacted with 20 µg mL-1 DNA in PBS for 150 s and analytical peak signals for adenine and guanine bases were evaluated. The interaction between BEVA-DNA was supported by UV-Vis. Absorption spectrometry and the binding constant was determined as 7.3 × 104.

Electrochemical evaluation of nivolumab used in cancer treatment with differential pulse voltammetry: A novel approach with single-use pencil graphite electrode.

OBJECTIVES: Nivolumab is used in a treatment called immunotherapy, which helps the immune system cells to attack cancer cells. The electrochemical properties and quantification of this drug were performed using single-use pencil tips. EVIDENCE ACQUISITION: Here, a selective voltammetric method for the determination and electrochemical characterization of Nivolumab used in cancer therapy was developed for the first time using a disposable pencil electrode by cyclic voltammetry and differential pulse voltammetry techniques. Nivolumab exhibited an anodic signal at +0.879 V (vs. Ag/AgCl) in PBS (pH 3.0, 0.02 M NaCl) medium. RESULTS: This procedure showed a linear response in phosphate buffer solutions (pH 3.0, 0.02 M NaCl) media within the concentration range of 0.01 mg mL-1 to 0.07 mg mL-1 and limit of detection and the limit of quantification values were determined to be 2.49 µg mL-1 and 8.30 µg mL-1, respectively. CONCLUSIONS: The developed method offers an important analytical approach for the detection and characterization of NIVO. Precisely measuring and monitoring the levels of such drugs in real sample analyses or biological samples is critical for evaluating response to treatment, optimizing treatment strategies. Therefore, the method was applied to real sample analyses. Voltammetric results developed using PG electrode were compared with UV-Vis results. It has been determined that the results obtained are compatible with each other.

Firstly electrochemical investigetions and determination of anticoagulant drug edoxaban at single-use pencil graphite electrode: an eco-friendly and cost effective voltammetric method.

OBJECTIVES: The anticoagulant drug edoxaban has a blood thinning mechanism of action. In this study, a pencil graphite electrode was electrochemically activated at + 1.4 V for 60 s. in a Britton-Robinson (pH 9.0) supporting electrolyte solution. EVIDENCE ACQUISITION: A simple, fast, and sensitive electrochemical procedure was developed using cyclic voltammetry and square wave voltammetry techniques. It was observed that edoxaban gave a good oxidation signal with cyclic voltammetry technique at a potential of + 0.98 V (vs. Ag/AgCl). RESULTS: This procedure showed a linear response in a Britton-Robinson (pH 9.0) media within the concentration range of 0.2-1.8 µM and limit of detection (LOD) and the limit of quantification (LOQ) values were determined to be 0.073 µM (0.133 µg mL-1) and 0.243 µM (0.443 µg mL-1), respectively. CONCLUSION: The method developed in this study was successfully applied to drug and urine samples. The developed voltammetric method was highly selective and gave satisfactory recovery results in urine and pharmaceutical samples. The results of the voltammetric method were compared with the spectroscopic method and it was determined that the results were compatible.

The effect of Plantago major Linnaeus on serum total sialic acid, lipid-bound sialic acid, some trace elements and minerals after administration of 7,12-dimethylbenz(a)anthracene in rats.

The present study was designed to evaluate the effect of Plantago major Linnaeus (PM) extract on serum total sialic acid (TSA), lipid-bound sialic acid (LSA), some trace elements (copper (Cu), zinc (Zn) and iron) and mineral levels (magnesium, calcium and sodium) in Wistar albino rat administrated 7,12-dimethylbenz(a)anthracene (DMBA). Rats were divided into three equal groups (n = 6). Group I comprised the control group, group II was treated with DMBA (100 mg/kg, single dose) and group III was treated with DMBA (100 mg/kg single dose) and aqueous extract of PM 100 mg/kg/day for 60 days. After 60 days, statistical analyses showed that TSA and LSA levels in DMBA and DMBA + PM groups were significantly higher compared to the control group (TSA: p < 0.01, p < 0.05; LSA: p < 0.05, p < 0.05, respectively). Serum Zn levels were decreased in subjects treated with DMBA (p < 0.01) and DMBA + PM (p < 0.05) compared to the control group values. Serum Cu levels were increased in DMBA group and PM-treated group compared to the control group values. The results of this investigation showed that the levels of TSA and LSA changed significantly, which are sensitive markers for detecting the toxic effects of DMBA. On the other hand, observed decline in Zn levels in rats from DMBA + PM group might be due to decreased generation of free radicals and oxidative stress. Results from this study suggest that PM may be partially effective in preventing carcinogenesis initiated by environmental carcinogen DMBA.

Electrochemical evaluation of the desloratadine at bismuth film electrode in the presence of cationic surfactant: Highly sensitive determination in pharmaceuticals and human urine by Linear sweep-cathodic stripping voltammetry.

In this study, the electrochemical properties of desloratadine, which is in the second generation antihistamines group, were determined by bismuth film electrode (BiFE) in aqueous and aqueous/surfactant solutions. This compound gave an irreversible and diffusion-controlled reduction peak at about -1.65 V by cyclic voltammetry. It was found that the addition of cationic surfactants (cetyltrimethylammonium bromide (CTAB) increased the reduction current signal of desloratadine, while anionic (sodium dodecylsulfate (SDS) and nonionic (Tween 80) surfactants were found to have an adverse effect. Using linear sweep-cathodic stripping voltammetry, the analytical signal showed a linear correlation with a concentration of 0.1 to 4 µM in 0.04 M Britton-Robinson solution (pH = 8.0) in the presence of 5 mM CTAB, while the detection limit was calculated to be 11.70 nM (3.64 µgL-1). This method has been successfully applied for the quantitation of desloratadine in pharmaceutical and urine samples without the need for any separation.

Simultaneous Electrochemical Evaluation of Ascorbic Acid, Epinephrine and Uric Acid at Disposable Pencil Graphite Electrode: Highly Sensitive Determination in Pharmaceuticals and Biological Liquids by Differential Pulse Voltammetry.

AIM AND OBJECTIVE: As is known, AA, EP and UA can also coexist in biological fluids. Therefore, the determination of the levels of these compounds in biological fluids is extremely important both for the diagnosis and treatment of the related diseases. In the presence of many interfering substances in biological fluids such as blood and urine samples, it is very important that these compounds can be selectively analyzed. MATERIALS AND METHODS: All electrochemical experiments were performed using an Autolab PGSTAT 128N potentiostat. Before beginning the electrochemical measurements, the PGE was activated. The electrochemical pretreatment of PG was exercised by anodically +1.40 V for 60 s. Then, measurements were performed with CV (-0.4 V to 1.2 V) and DPV (-0.2 V to 0.7 V) for single and simultaneous voltammetric behaviour of AA, EP, and UA in the electrochemical method. RESULTS: The anodic peak potentials of AA and UA were observed at about +0.32 V and +0.62 V, respectively. On the other hand, for EP, while anodic peak potential was observed at about +0.53 V, in the reverse scan, cathodic peak potentials were observed at about +0.41 V and +0.007 V. The reduction peak observed at +0.3 V with the oxidation peak observed at +0.53 V are the reversible peaks. In the method developed for the electrochemical simultaneous determination of AA, EP and UA using PGE with DPV technique in BR buffer solution (pH 4.0), the anodic peak potentials are sufficiently separated from each other. CONCLUSION: A voltammetric method was developed for the simultaneous determination of AA, EP and UA with PGE for the first time. Here, the most important thing is that the simultaneous determination of AA, EP and UA was successfully achieved with that targeted voltammetric method which was sensitive, low-cost, practical and well-repeated; and that these were proven to be selectively applicable in pharmaceutical products and biological liquids.

Graphene/Nafion composite film modified glassy carbon electrode for simultaneous determination of paracetamol, aspirin and caffeine in pharmaceutical formulations.

A graphene-Nafion composite film was fabricated on the glassy carbon electrode (GR-NF/GCE), and used for simultaneous determination of paracetamol (PAR), aspirin (ASA) and caffeine (CAF). The electrochemical behaviors of PAR, ASA and CAF were investigated by cyclic voltammetry and square-wave adsorptive anodic stripping voltammetry. By using stripping one for simultaneous determination of PAR, ASA and CAF, their electrochemical oxidation peaks appeared at +0.64, 1.04 and 1.44V, and good linear current responses were obtained with the detection limits of 18ngmL(-1) (1.2×10(-9)M), 11.7ngmL(-1) (6.5×10(-8)M) and 7.3ngmL(-1) (3.8×10(-8)M), respectively. Finally, the proposed electrochemical sensor was successfully applied for quantifying PAR, ASA and CAF in commercial tablet formulations.

Synthesis and characterization of 1,2-bis(2-(5-bromo-2-hydroxybenzilidenamino)-4-chlorophenoxy)ethane and its metal complexes: an experimental, theoretical, electrochemical, antioxidant and antibacterial study.

A new Schiff base ligand was synthesized by reaction of 5-bromosalicylaldehyde with 1,2-bis(4-chloro-2-aminophenoxy)ethane. Then the Schiff base complexes were synthesized by the reaction of metal salts and the novel Schiff base. The molar conductivity properties of the complexes were studied and found out that the complexes are nonelectrolytes. The structures of the ligand and its metal complexes were characterized by elemental analysis, FT-IR, UV-VIS, magnetic susceptibility measurements, molar conductivity measurements, and thermal gravimetric analysis. In addition antioxidant, theoretical NMR studies and cyclic voltammetry of the complexes were done. Two methods namely metal chelating activity and diphenylpicrylhydrazyl (DPPH) radical scavenging method were used to determine the antioxidant activity, and antibacterial properties of the compounds were also studied.

Synthesis, characterization and experimental, theoretical, electrochemical, antioxidant and antibacterial study of a new Schiff base and its complexes.

A new Schiff base ligand was synthesized by reaction of salicylaldehyde with 1,6-bis(4-chloro-2-aminophenoxy)hexane. Then the Schiff base complexes were synthesized by metal salts and the Schiff base. The metal to ligand ratio of metal complexes was found to be 1:1. The Cu(II) complex is proposed to be square planar and the Co(II), Ni(II), Mn(II) and Zn(II) complexes are proposed to be tetrahedral geometry. The Ti(III) and V(III) complexes are proposed to be a capped octahedron in which a seventh ligand has been added to triangular face. The complexes are non-electrolytes as shown by their molar conductivities (ΛM). The structure of metal complexes is proposed from elemental analysis, FT-IR, UV-vis, magnetic susceptibility measurements, molar conductivity measurements, Mass Spectra and thermal gravimetric analysis. In addition antimicrobial and antioxidant studies, cyclic voltammetry of the complexes, theoretical 1H NMR and HOMO-LUMO energy calculations of the new di-functional ligand were done.

Protective effect of Hypericum perforatum L. on serum and hair trace elements in rats 7,12-dimethylbenz[a]anthracene-induced oxidative stress.

The study was designed to assess the effect of Hypericum perforatum L. (H.P) on serum and hair trace elements and mineral levels, oral administration of 7,12-dimethylbenz[a]anthracene (DMBA) induced oxidative stress in Sprague-Dawley female rats. Analysis of the trace element has been carried out using atomic absorption spectrophotometer method at end of 60th day. It has been found out that the DMBA group contained statistically lower Zn and Cr compared to the control group (p<0.01) and (p<0.05), Cu, Mg and Na contained higher than control group (p<0.05), (p<0.05) and (p<0.05). In DMBA+H.P group, Zn higher and Na lower than DMBA group (p<0.05), (p<0.05), in hair samples Cd, K and Zn contained lower DMBA compared to the control group (p<0.05), (p<0.05) and (p<0.05). In group DMBA+H.P, Cd was higher than DMBA group and Cr lowered accordance with control group (p<0.05). The present study demonstrated significantly positive and beneficial effect of H.P on the concentration levels of Zn and Na in serum, also on Cd levels in hair between DMBA and DMBA+H.P groups.

Determination of 7,12-dimethylbenz[a]anthracene in orally treated rats by high-performance liquid chromatography and transfer stripping voltammetry.

A number of polycyclic aromatic hydrocarbons (PAHs) have been shown to be toxicants, and induce carcinogenic and immunotoxic effects. As a model PAH agent, 7,12-dimethylbenz[a]anthracene (DMBA) was the strongest one tested in terms of its biological activities and biotransformation. A new and simple high-performance liquid chromatographic (HPLC) method with diode-array detection at 290 nm was developed and validated for monitoring of DMBA in different matrices (serum, liver and kidney) of rats orally treated with DMBA. Furthermore, the applicability of adsorptive transfer stripping voltammetry (AdTSV) on the pencil-lead graphite electrode to these samples was illustrated using our previously reported data for bulk aqueous solutions of DMBA. HPLC and AdTSV methods, which were compatible with each other, allowed DMBA to be detected down to the levels of 3.82x10-9 M (0.98 ppb) and 6.73x10-9 M (1.73 ppb), respectively. Olive oil solutions of DMBA in dose 50 mg/kg were orally administered. 60 days after a single dose of DMBA, its concentrations in these biological samples from rats were measured by means of both methods. Because of rapid biotransformation, DMBA could not be detected in serum. Only low levels of the compounds were deposited unchanged in kidney whereas its levels were considerably higher in liver. These methods were also applied to the assay whether there is an influence of the intake of aqueous extracts of Hypericum Perforatum L. plant on the parent DMBA levels accumulated in rat tissues.

Voltammetric behavior of benzo[a]pyrene at boron-doped diamond electrode: a study of its determination by adsorptive transfer stripping voltammetry based on the enhancement effect of anionic surfactant, sodium dodecylsulfate.

Benzo[a]pyrene (BaP), a member of the polycyclic aromatic hydrocarbon (PAH) class, is one of the most potent PAH carcinogens. The electrochemical oxidation of BaP was first studied by cyclic voltammetry at the boron-doped diamond electrode in non-aqueous solvent (dimethylsulphoxide with lithium perchlorate). The compound was irreversibly oxidized in a single step at high positive potential, resulting in the well-resolved formation of a couple with a reduction and re-oxidation wave at much lower potentials. Special attention was given to the use of adsorptive stripping voltammetry together with a medium exchange procedure in aqueous and aqueous/surfactant solutions over the pH range of 2.0-8.0. The technique in aqueous solutions had little value in practice because of too small oxidation peak current. This problem was solved when surfactants were added into the sample solution, by which the oxidation peak currents of BaP were found enhanced dramatically. The employed surfactants were sodium dodecylsulfate (anionic, SDS), cetyltrimethylammonium bromide (cationic, CTAB) and Tween 80 (non-ionic). Using square-wave stripping mode, the compound yielded a well-defined voltammetric response in Britton-Robinson buffer, pH 2.0 containing 2.5×10(-4)M SDS at +1.07 V (vs. Ag/AgCl) (after 120s accumulation at +0.10 V). The process could be used to determine BaP in the concentration range of 16-200 nM (4.04-50.46 ng mL(-1)), with a detection limit of 2.86 nM (0.72 ng mL(-1)). This method was also applied to determine BaP in model water sample prepared by adding its different concentrations into tap water.

Plantago major protective effects on antioxidant status after administration of 7,12-Dimethylbenz(a)anthracene in rats.

AIM: The present study was designed to evaluate effects of Plantago major extract on oxidative status in Wistar albino rats administrated 7,12-dimethylbenz(a)anthracene (DMBA). METHODS: Rats were divided into three equal groups of 6 animals each: Group 1 controls, group 2 treated with DMBA (100 mg/kg, single dose) and group 3 receiving the DMBA and the aqueous extract at 100 mg/kg/d for 60 days. RESULTS: Significant decrease in catalase (P < 0.05), carbonic anhydrase (p ≤ 0.01), reduced glutathione (GSH) (P < 0.01) and total protein (P < 0.01) values was observed in the DMBA group compared with the healthy controls and DMBA + Plantago major groups. CONCLUSION: The results suggest preventive effects of Plantago major on DMBA induced oxidative damage in Wistar albino rats that might be due to decreased free radical generation.

Colorimetric and atomic absorption spectrometric determination of mucolytic drug ambroxol through ion-pair formation with iron and thiocyanate.

Colorimetric and atomic absorption spectrometric methods have been developed for the determination of mucolytic drug Ambroxol. These procedures depend upon the reaction of iron(III) metal ion with the drug in the presence of thiocyanate ion to form stable ion-pair complex which extractable chloroform. The red-coloured complex was determined either colorimetrically at 510 nm or by indirect atomic absorption spectrometry (AAS) via the determination of the iron content in the formed complex. The optimum experimental conditions for pH, concentrations of Fe(3+) and SCN(-), shaking time, phase ratio, and the number of extractions were determined. Under the proposed conditions, linearity was obeyed in the concentration ranges 4.1x10(-6) - 5.7x10(-5) M (1.7-23.6 µg mL(-1)) using both methods, with detection limits of 4.6x10(-7) M (0.19 µg mL(-1)) for colorimetry and 1.1x10(-6) M (0.46 µg mL(-1)) for AAS. The proposed methods were applied for the determination of Ambroxol in tablet dosage forms. The results obtained were statistically analyzed and compared with those obtained by applying the high-performance liquid chromatographic method with diode-array detection.