Electrochemical HPLC Determination of Piperazine Antihistamine Drugs Employing a Spark-Generated Nickel Oxide Nanoparticle-Modified Carbon Fiber Microelectrode.

In this work, we demonstrate a sensitive high-performance liquid chromatography (HPLC) method for the determination of piperazine antihistamine drugs employing innovative electrochemical detection based on a spark-generated nickel oxide nanoparticle-modified carbon fiber microelectrode built into a miniaturized electrochemical detector. The direct carbon fiber-to-nickel plate electrode spark discharge, carried at 0.8 kV DC, with the nickel electrode connected to the negative pole of the high-voltage power supply, provides extremely fast (1 s) in situ tailoring of the carbon fiber microelectrode surface by nickel oxide nanoparticles.

Copper nanowire coated carbon fibers as efficient substrates for detecting designer drugs using SERS.

Miniature Surface Enhanced Raman Scattering (SERS) sensors were fabricated by coating the carbon fiber microelectrodes with copper nanowires. The coating procedure, based on anodizing the copper wire in ultrapure water followed by cathodic deposition of the anode-derived material onto carbon fiber electrodes, provides a "clean" copper nanowire network. The developed miniature (10µm in diameter and 2mm in length) and nanoscopically rough SERS substrates are applicable in drug sensing, as shown by the detection and resolving of a range of seized designer drugs in trace amounts (microliter volumes of 10-10M solutions).

A comparison of electrochemically pre-treated and spark-platinized carbon fiber microelectrode. Measurement of 8-oxo-7,8-dihydro-2'-deoxyguanosine in human urine and plasma.

A novel method of carbon fiber microelectrode activation using spark discharge was demonstrated and compared to conventional electrochemical pretreatment by potential cycling. The spark discharge was performed at 800 V between the microelectrode connected to positive pole of the power supply and platinum counter electrode. Spark discharge led both to trimming of the fiber tip into conical shape and to the modification of carbon fiber microelectrode with platinum, as proven by scanning electron microscopy and electron dispersive X-ray spectroscopy.

HPLC-ED of low-molecular weight brominated phenols and tetrabromobisphenol A using pretreated carbon fiber microelectrode.

Electrochemically pretreated carbon fiber microelectrode was used to develop a simple, fast and sensitive HPLC-ECD method for the determination of brominated phenols. In addition to simple mono-, di- and tri-bromophenols (4-bromophenol, 2,4-dibromophenol, 2,6-dibromophenol, 2,4,6-tri-bromophenol) the possibility of electrochemical detection of 3,3',5,5'-tetrabromobisphenol A in oxidation mode is reported for the first time. The isocratic separation was achieved within 14 min using ternary mobile phase consisting of 50mM-phosphate buffer (pH 3.

Electrochemical behavior of quinoxalin-2-one derivatives at mercury electrodes and its analytical use.

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.

Electrochemically pretreated carbon microfiber electrodes as sensitive HPLC-EC detectors.

The paper focuses on the analysis and detection of electroactive compounds using high-performance liquid chromatography (HPLC) combined with electrochemical detection (EC). The fabrication and utilization of electrochemically treated carbon fiber microelectrodes (CFMs) as highly sensitive amperometric detectors in HPLC are described. The applied pretreatment procedure is beneficial for analytical characteristics of the sensor as demonstrated by analysis of the model set of phenolic acids.

Electrochemical oxidation of berberine and mass spectrometric identification of its oxidation products.

Electrochemical oxidation of the isoquinoline alkaloid berberine in aqueous medium was studied by cyclic and differential pulse voltammetry at a glassy carbon electrode (GCE). Two anodic peaks of the quaternary form of berberine were observed at +1.2V and +1.

High-performance liquid chromatographic method with amperometric detection employing boron-doped diamond electrode for the determination of sildenafil, vardenafil and their main metabolites in plasma.

A simple, fast and sensitive HPLC method with electrochemical detection employing boron-doped diamond electrode (BDD) for the determination of sildenafil (Viagra™), vardenafil (Levitra™) and their main metabolites, N-desmethyl sildenafil and N-desethyl vardenafil in human plasma is presented. The assay involved drug extraction by tert-butyl methyl ether and isocratic reversed-phase liquid chromatography with amperometric detection. Complete separation of all analytes was achieved within 12 min.

Electrochemical characterization of repaglinide and its determination in human plasma using liquid chromatography with dual-channel coulometric detection.

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.

Determination of antihyperglycemic drugs in nanomolar concentration levels by micellar electrokinetic chromatography with non-ionic surfactant.

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.

Capillary electrophoresis-based nanoscale assays for monitoring ecto-5'-nucleotidase activity and inhibition in preparations of recombinant enzyme and melanoma cell membranes.

Powerful capillary electrophoresis (CE) methods were developed for monitoring the reaction of ecto-5'-nucleotidase (ecto-5'-NT, CD73), a (patho)biochemically important enzyme that hydrolyzes nucleoside-5'-monophosphates to the corresponding nucleosides. The enzymatic reaction was performed either before injection into the capillary (method A) or directly within the capillary (method B). In method A, separation of substrates and products was achieved within 8 min using an eCAP fused-silica capillary (20 cm effective length, 75 microM i.

HPLC analysis of rosmarinic acid in feed enriched with aerial parts of Prunella vulgaris and its metabolites in pig plasma using dual-channel coulometric detection.

This paper describes a sensitive isocratic HPLC/ECD method developed for the determination of rosmarinic acid (RA) in plant material, animal feed, and pig plasma. The plasma sample preparation only includes protein precipitation and adjustment of the pH. The applicability of the method was tested on plasma samples of pigs that were exposed to a 91-day oral intake of RA via feed enriched by aerial parts of Prunella vulgaris.

The biological and chemical variability of yacon.

This paper focuses on the biological and chemical variability of four yacon (Smallanthus sonchifolius) accessions cultivated under field conditions. Significant variations in tuber shape, weight, content of oligofructans, as well as in leaf isozymes, phenolics, and relative DNA contents were found. Accessions 6 and 88 were the most productive (up to 3.

Dimethylfumarate inhibits tumor-necrosis-factor-induced CD62E expression in an NF-kappa B-dependent manner.

Fumaric acid esters are thought to improve psoriasis by altering leukocyte, keratinocyte, and/or endothelial functions. To determine specificity, kinetics, and molecular mechanisms of different fumaric acid esters in their ability to inhibit endothelial cell activation, we analyzed CD62E and CD54 expression in endothelial cells in vivo and in vitro. In lesional skin of psoriatic patients, oral fumaric acid ester treatment resulted in a marked reduction of CD62E but not CD54 expression on dermal microvessels.

Methamphetamine--properties and analytical methods of enantiomer determination.

Methamphetamine is one of the most frequently abused drugs of today. Due to its stereogenic center, it can exist as single enantiomer. Like many other chiral compounds, methamamphetamine enantiomers exhibit different pharmacological effects on living organisms.