New screen-printed sensor with a boron-doped diamond working electrode (SP/BDDE) was fabricated using a large-area linear antenna microwave chemical deposition vapor system (LA-MWCVD) with a novel precursor composition. It combines the advantages of disposable printed sensors, such as tailored design, low cost, and easy mass production, with excellent electrochemical properties of BDDE, including a wide available potential window, low background currents, chemical resistance, and resistance to passivation. The newly prepared SP/BDDEs were characterized by scanning electron microscopy (SEM) and Raman spectroscopy. Their electrochemical properties were investigated by cyclic voltammetry and electrochemical impedance spectroscopy using inner sphere ([Fe(CN)6]4-/3-) and outer sphere ([Ru(NH3)6]2+/3+) redox probes. Moreover, the applicability of these new sensors was verified by analysis of the anti-inflammatory drug lornoxicam in model and pharmaceutical samples. Using optimized differential pulse voltammetry in Britton-Robinson buffer of pH 3, detection limits for lornoxicam were 9 × 10-8 mol L-1. The oxidation mechanism of lornoxicam was investigated using bulk electrolysis and online electrochemical cell with mass spectrometry; nine distinct reaction steps and corresponding products and intermediates were identified.
- MeSH
- bor * chemie MeSH
- elektrody MeSH
- elektrolýza * MeSH
- oxidace-redukce MeSH
- Ramanova spektroskopie MeSH
- Publikační typ
- časopisecké články MeSH
The review describes fentanyl and its analogs as new synthetic opioids and the possibilities of their identification and determination using electrochemical methods (e.g., voltammetry, potentiometry, electrochemiluminescence) and electrochemical methods combined with various separation methods. The review also covers the analysis of new synthetic opioids, their parent compounds, and corresponding metabolites in body fluids, such as urine, blood, serum, and plasma, necessary for a fast and accurate diagnosis of intoxication. Identifying and quantifying these addictive and illicit substances and their metabolites is necessary for clinical, toxicological, and forensic purposes. As a reaction to the growing number of new synthetic opioid intoxications and increasing fatalities observed over the past ten years, we provide thorough background for developing new biosensors, screen-printed electrodes, or other point-of-care devices.
- MeSH
- fentanyl * MeSH
- opioidní analgetika * MeSH
- Publikační typ
- časopisecké články MeSH
- přehledy MeSH
The performances of ionic liquid (1-hexyl-3-methylimidazolium-bis(trifluoromethylsulfonyl)imide, IL/CPE) and iron phthalocyanine (IP/CPE) modified carbon paste electrodes in electroanalytical determinations of rutin were evaluated and compared to the performance of unmodified carbon paste electrode (CPE). Cyclic voltammetry (CV), differential pulse voltammetry (DPV), differential pulse adsorptive stripping voltammetry (DPAdSV), and amperometry were used for rutin analysis. The best current responses of rutin were obtained at pH 4.0 for all tested techniques. IL/CPE electrode was found to perform best with DPAdSV technique, where a detection limit (LOD) as low as 5 nmol L(-1) of rutin was found. On the other hand, IP/CPE showed itself to be an optimum choice for DPV technique, where LOD of 80 nmol L(-1) was obtained. Analytical applicability of newly prepared electrodes was demonstrated on determination of rutin in the model samples and the extracts of buckwheat seeds. To find an optimum method for buckwheat seeds extraction, a boiling water extraction (BWE), Soxhlet extraction (SE), pressurized solvent extraction (PSE), and supercritical fluid extraction (SFE) were tested.
- MeSH
- elektrochemie metody MeSH
- elektrody MeSH
- Fagopyrum chemie MeSH
- molekulární struktura MeSH
- rutin chemie MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
Derivatives of quinoxalin-2-one are interesting compounds with potential pharmacological activity. From this point of view, understanding of their electrochemical behavior is of great importance. In the present paper, a mechanism of electrochemical reduction of quinoxalin-2-one derivatives at mercury dropping electrode was proposed. Pyrazine ring was found to be the main electroactive center undergoing a pH-dependent two-electron reduction process. The molecule protonization of nitrogen in the position 4 precedes the electron acceptance forming a semiquinone radical intermediate which is relatively stable in acidic solutions. Its further reduction is manifested by separated current signal. A positive mesomeric effect of the nonprotonized amino group in the position 7 of the derivative III accelerates the semiquinone reduction yielding a single current wave. The suggested reaction mechanism was verified by means of direct current polarography, differential pulse, cyclic and elimination voltammetry, and coulometry with subsequent GC/MS analysis. The understanding of the mechanism was applied in developing of analytical method for the determination of the studied compounds.
A simple, fast and sensitive HPLC method employing dual-channel coulometric detection for the determination of repaglinide in human plasma is presented. The assay involved extraction of repaglinide by ethyl acetate and isocratic reversed-phase liquid chromatography with dual-channel coulometric detection. The mobile phase composition was 50mM disodium hydrogen phosphate/acetonitrile (60:40, v/v), pH of the mobile phase 7.5 set up with phosphoric acid. For all analyses, the first cell working potential was +380mV, the second was +750mV (vs. Pd/H(2)). Calibration curve was linear over the concentration range of 5-500nmolL(-1). Rosiglitazone was used as an internal standard. The limit of detection (LOD) was established at 2.8nmolL(-1), and the lower limit of quantification (LLOQ) at 8.5nmolL(-1). The developed method was applied to human plasma samples spiked with repaglinide at therapeutical concentrations. It was confirmed that the method is suitable for pharmacokinetic studies or therapeutic monitoring.
- MeSH
- elektrochemické techniky metody MeSH
- hypoglykemika krev chemie MeSH
- karbamáty krev chemie MeSH
- kolorimetrie metody MeSH
- koncentrace vodíkových iontů MeSH
- lidé MeSH
- lineární modely MeSH
- piperidiny krev chemie MeSH
- reprodukovatelnost výsledků MeSH
- senzitivita a specificita MeSH
- thiazolidindiony analýza MeSH
- vysokoúčinná kapalinová chromatografie metody MeSH
- Check Tag
- lidé MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
A method for the separation of six selected antihyperglycemic (antidiabetic) drugs (tolbutamide, gliclazide, glimepiride, glibenclamide, repaglinide, and glipizide) was developed with use of micellar electrokinetic chromatography. Two non-ionic poly(ethylene glycol)-based surfactants Genapol X-080 and Triton X-114 (reduced) were studied as neutral pseudostationary phases. High alkaline pH 10.0 was used to obtain negative charges of separated antidiabetic drugs and non-ionic surfactants were employed for selectivity alteration. Both non-ionic surfactants provided good selectivity at concentration 0.2% (v/v) in sodium borate buffer and the separation of six drugs was obtained within 5min. An on-line preconcentration method based on reversed electrode polarity switching was employed for the determination of antihyperglycemic drugs in blood serum after acetonitrile protein precipitation. The limits of detection ranged from 20.8nmolL(-1) for tolbutamide to 6.5nmolL(-1) for glibenclamide, respectively.
- MeSH
- chromatografie MeSH
- hypoglykemika analýza krev MeSH
- lidé MeSH
- polyethylenglykoly chemie MeSH
- povrchově aktivní látky chemie MeSH
- senzitivita a specificita MeSH
- Check Tag
- lidé MeSH
- Publikační typ
- hodnotící studie MeSH
- práce podpořená grantem MeSH