Electrochemically Reduced Graphene Oxide-Based Screen-Printed Electrodes for Total Tetracycline Determination by Adsorptive Transfer Stripping Differential Pulse Voltammetry.

Disposable electrochemically reduced graphene oxide-based (ERGO) screen-printed electrodes (SPE) were developed for the determination of total tetracyclines as a sample screening approach. To this end, a selective adsorption-detection approach relied on adsorptive transfer stripping differential pulse voltammetry (AdTDPV) was devised, where the high adsorption capacity and the electrochemical properties of ERGO were simultaneously exploited. The approach was very simple, fast (6 min.

A soft material for chromium speciation in water samples using a chemiluminescence automatic system.

A soft material formed by multiwall carbon nanotubes and 1-butyl-3-methyl imidazolium chloride was used as sorbent material to perform the chromium speciation in natural waters. This soft material was not yet used for the speciation of metals as chromium. Thus, a multicommutated flow system containing a minicolumn packed with the soft material was designed.

Flow-batch analysis of clenbuterol based on analyte extraction on molecularly imprinted polymers coupled to an in-system chromogenic reaction. Application to human urine and milk substitute samples.

A fully automated spectrophotometric method based on flow-batch analysis has been developed for the determination of clenbuterol including an on-line solid phase extraction using a molecularly imprinted polymer (MIP) as the sorbent. The molecularly imprinted solid phase extraction (MISPE) procedure allowed analyte extraction from complex matrices at low concentration levels and with high selectivity towards the analyte. The MISPE procedure was performed using a commercial MIP cartridge that was introduced into a guard column holder and integrated in the analyzer system.

A simple and new reverse liquid-liquid microextraction for the automated spectrometric determination of doxycycline in chicken fat.

This work presents a new, simple and inexpensive reverse liquid-liquid microextraction of doxycycline (DOC) from chicken fat. In this just 13min extraction methodology, acidulated water, as extraction solvent (400µL), was used. A monochannel flow injection system was designed for the spectrometric determination of the analyte (ʎ=344nm).

Ionic liquid mediated extraction, assisted by ultrasound energy, of available/mobilizable metals from sediment samples.

A new extraction method for metals from sediment samples was developed. In this procedure, the chelating agent EDTA was combined with a minimal amount of the ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate (Bmim[BF]), assisted by ultrasound energy. The available analytes -Cd, Cr, Cu, Ni, Pb and Zn- were extracted under optimal conditions for a 12.

In-line coupled single drop liquid-liquid-liquid microextraction with capillary electrophoresis for determining fluoroquinolones in water samples.

A simple in-line single drop liquid-liquid-liquid microextraction (SD-LLLME) coupled with CE for the determination of two fluoroquinolones was developed. The method is capable to quantify trace amount of analytes in water samples and to improve the sensitivity of CE detection. For the SD-LLLME, a thin layer of organic phase was used to separate a drop of 0.

Capillary electrophoresis to determine entrapment efficiency of a nanostructured lipid carrier loaded with piroxicam.

A simple and fast capillary electrophoresis method has been developed to determine the amount of piroxicam loaded in a drug delivery system based on nanostructured lipid carriers (NLCs). The entrapment efficiency of the nanostructured lipid carrier was estimated by measuring the concentration of drug not entrapped in a suspension of NLC. The influence of different parameters on migration times, peak symmetry, efficiency and resolution was studied; these parameters included the pH of the electrophoretic buffer solution and the applied voltage.

Application of a fully integrated photodegradation-detection flow-batch analysis system with an on-line preconcentration step for the determination of metsulfuron methyl in water samples.

This work presents the development of a fully automated flow-batch analysis (FBA) system as a new approach for on-line preconcentration, photodegradation and fluorescence detection in a lab-constructed mixing chamber that was designed to perform these processes without sample dispersion. The system positions the mixing chamber into the detection system and varies the instrumental parameters according to the required photodegradation conditions. The developed FBA system is simple and easily coupled with any sample pretreatment without altering the configuration.

Determination of fluoroquinolones in bovine milk samples using a pipette-tip SPE step based on multiwalled carbon nanotubes prior to CE separation.

A simple CE-UV method was developed for the simultaneous determination of ciprofloxacin, norfloxacin, and ofloxacin in milk samples. The optimum separation was obtained using a 20 mM ammonium dihydrogenphosphate solution with 2 mM cetyltrimethylammonium bromide at pH 3.0 as the BGE.

Synthesis and characterization of hybrid-magnetic nanoparticles and their application for removal of arsenic from groundwater.

Multiwall carbon nanotubes (MWCNTs) were oxidized with different agents and a characterization study was carried out. Then, hybrid-magnetic nanoparticles (HMNPs) were synthesized as iron oxide supported on the selected multiwalled carbon nanotubes (MWCNTs-Fe₃O₄) obtained from MWCNTs oxidized with HNO3. The HMNPs characterization revealed the presence of iron oxide as magnetite onto the MWCNTs surfaces.

Determination of sulfonylureas in cereal samples with electrophoretic method using ionic liquid with dispersed carbon nanotubes as electrophoretic buffer.

A capillary electrophoresis method to determine four sulfonylureas in grain samples was developed using 10mM of 1-butyl-3-methyl imidazolium tetrafluoroborate (bminBF4) as electrophoretic buffer solution. 2mgL(-1) of Surfactant Coated-Single Wall-Carbon Nanotubes (SC-SWCNTs) was added to the buffer solution to improve the resolution. In this way, the separation of nicosulfuron, ethoxysulfuron, sulfometuron methyl and chlorsulfuron was carried out in 16min without using organic solvents.

Quantification of uncertainty in mercury wastewater analysis at different concentration levels and using information from proficiency test with a limited number of participants.

Measurement uncertainty is one of the most required parameters of analytical quality in environmental decision-making. Several approaches have been reported for estimating uncertainty in analytical measurements. The use of proficiency test (PT) is an alternative, not only for assessing the performance of individual analytical laboratories, but also for estimating the concordance of an analytical method and their measurement uncertainties.

Micellar nanotubes dispersed electrokinetic chromatography for the simultaneous determination of antibiotics in bovine milk.

A method to determine four antibiotics for veterinary use (ciprofloxacin, enrofloxacin, florfenicol, and chloramphenicol) of different families (fluoroquinolones and amphenicols) in bovine milk was developed. The determination of the analytes was carried out using micellar electrokinetic capillary chromatography (MEKC) with a common sodium borate-SDS buffer solution containing single-walled carbon nanotubes (SWCNTs). In this way, a great improvement in the electrophoretic resolution and the separation efficiency was achieved compared to MEKC.

Simultaneous determination of hydroquinone, resorcinol, phenol, m-cresol and p-cresol in untreated air samples using spectrofluorimetry and a custom multiple linear regression-successive projection algorithm.

In this study, a novel, simple, and efficient spectrofluorimetric method to determine directly and simultaneously five phenolic compounds (hydroquinone, resorcinol, phenol, m-cresol and p-cresol) in air samples is presented. For this purpose, variable selection by the successive projections algorithm (SPA) is used in order to obtain simple multiple linear regression (MLR) models based on a small subset of wavelengths. For comparison, partial least square (PLS) regression is also employed in full-spectrum.

A simple and fast method for chlorsulfuron and metsulfuron methyl determination in water samples using multiwalled carbon nanotubes (MWCNTs) and capillary electrophoresis.

A new method to determine metsulfuron methyl (MSM) and chlorsulfuron (CS) in different water samples was developed. It consists in a solid phase extraction (SPE) procedure using multiwalled carbon nanotubes (MWCNTs) as sorbent material in combination with capillary zone electrophoretic determination. To carry out the pre-concentration step, a simple flow injection system was developed and optimized.

Successive projections algorithm applied to spectral data for the simultaneous determination of flavour enhancers.

A novel variable selection strategy for multiple lineal regression (MLR), the successive projections algorithm (SPA), was applied to spectrophotometric data (190-320 nm) for the simultaneous determination of monosodium glutamate (MSG), guanosine-5'-monophosphate (GMP) and inosine-5'-monophosphate (IMP) in dehydrated broths samples. This selection method uses simple operations in a vector space to minimize variable collinearity and has become an interesting variable selection strategy for multivariate calibration. In this work, nine, six and four wavelengths for MSG, GMP and IMP, respectively, were selected to construct calibrations models in order to solve successfully the serious spectral overlapping in samples containing these analytes.

A new automated approach to determine monosodium glutamate in dehydrated broths by using the flow-batch methodology.

The advantages of the flow-batch methodology were exploited to implement a simple system with nephelometric detection for the determination of monosodium glutamate (MSG) in food samples. The method is based on the inhibitory effect of the MSG over the crystallization of L-lysine in an isopropanol/acetone mixture. The calibration curve was prepared on-line.

Determination of phenol, resorcinol and hydroquinone in air samples by synchronous fluorescence using partial least-squares (PLS).

The determination of phenolic compounds is of great importance owing to their high toxicity. Some of them are present in tobacco smoke and it is important for their monitoring in air of closed room. A simple, rapid and sensitive method was developed for simultaneous determination of hydroquinone, resorcinol and phenol in this kind of samples.

Enzymatic reverse FIA method for total phenols determination in urine samples.

A reverse flow injection spectrophotometric enzymatic method is proposed to quantify total phenols in urine samples. The polyphenol oxidase (PPO; EC 1.14.

Evaluation of complex spectral-pH three-way arrays by modified bilinear least-squares: determination of four different dyes in interfering systems.

This article reports on the first application of a modified version of the bilinear least-squares model to absorbance-pH second-order data recorded for complex samples. The latter are composed of fruit drink powders, where four different analytes and additional background components occur. The analytes are the common juice colorants tartrazine, yellow sunset, allura red and indigo carmine.

Screening and analytical confirmation of sulfonamide residues in milk by capillary electrophoresis-mass spectrometry.

A new methodology is proposed to automate the monitoring of sulfonamide residues in milk samples. It combines a screening unit for the total amount of sulfonamide with capillary electrophoresis-mass spectrometry (CE-MS) equipment for processing the samples containing a detectable level of sulfonamide. The screening unit consists of continuous-flow system (CFS) to precipitate the proteins connected on-line to the CE-MS equipment, in which a common characteristic ion of all sulfonamides was monitored with the MS detector by flushing the sample through the capillary.

New method for the determination of benzoic and sorbic acids in commercial orange juices based on second-order spectrophotometric data generated by a pH gradient flow injection technique.

Two widely employed antimicrobials, benzoic and sorbic acids, were simultaneously determined in commercial orange juices employing a combination of a flow injection system with pH gradient generation, diode array spectrophotometric detection, and chemometric processing of the recorded second-order data. Parallel factor analysis and multivariate curve resolution-alternating least-squares were used for obtaining the spectral profiles of sample components and concentration profiles as a function of pH, including provisions for managing rank-deficient data sets. An appropriately designed calibration with a nine-sample set of binary mixtures of standards, coupled to the use of the second-order advantage offered by the applied chemometric techniques, allowed quantitation of the analytes in synthetic test samples and also in commercial orange juices, even in the presence of unmodeled interferents (with relative prediction errors of 8.

Flow injection analysis: Rayleigh light scattering technique for total protein determination.

A novel flow injection analysis (FIA) method with Rayleigh light scattering (RLS) detection was developed for the determination of total protein concentrations. This method is based on the weak intensity of RLS of bromothymol blue (BB) (3',3"-dibromothymolsulfonephthalein) which can be enhanced by the addition of protein in weakly acidic solution. A common spectrofluorimeter was used as a detector.