Determination of Cd and Pb in fuel ethanol by filter furnace electrothermal atomic absorption spectrometry

A method was developed for quantification of Cd and Pb in ethanol fuel by filter furnace atomic absorption spectrometry. Filter furnace was used to eliminate the need for chemical modification, to stabilize volatile analytes and to allow the application of short pyrolysis step. The determinations in samples were carried out against calibration solutions prepared in ethanol. Recovery tests were made in seven commercial ethanol fuel samples with values between 90 and 120%. Limits of detection were 0.1 µg L-1 for Cd and 0.3 µg L-1 for Pb. Certified water samples (APS 1071, APS 1033, NIST 1643d, NIST 1640) were also used to evaluate accuracy and recoveries from 86.8% to115% were obtained

Pre-concentration of rosuvastatin using solid-phase extraction in a molecularly imprinted polymer and analytical application in water supply

In this work, it is shown the development and validation of innovative analytical methodology based on solid-phase extraction (SPE) with molecularly imprinted polymers (MIP) as a sorbent associated to UV–Vis spectroscopy to isolate and quantify, respectively, rosuvastatin (RSV) in water samples. For this purpose, porogenic solvent in MIP synthesis and SPE extraction parameters for MIP and non-imprinted polymers (NIP) were evaluated univariately for comparison purposes. The sorptive capacity and characterization studies by infrared spectroscopy and atomic force microscopy showed difference between MIP and NIP. The selectivity study of the MIP–RSVagainst other statins (simvastatin and atorvastatin) showed that the synthesized MIP can also be applied as a solid phase for isolation and quantitative pre-concentration of RSVand atorvastatin. The conjugation of SPE and UV–Vis spectroscopy in the determination of RSV in aqueous matrices led to large factor of pre-concentration (125 times), limit of detection (LOD) of 3 μg L−1, limit of quantification (LOQ) of 10 μg L−1, precision of 2.87% (n = 10), and accuracy of 83.1% (n = 4)

Voltammetric determination of sibutramine in beverages and in pharmaceutical formulations

A simple and sensitive method has been proposed for the determination of sibutramine-HCl in energy drinks, green tea and pharmaceutical formulations using differential pulse voltammetry performed on a hanging mercury drop electrode. In the chosen experimental condition (Mcllvaine pH 4.0 buffer, 50 mV pulse amplitude and 40 mV s-1 scan velocity), sibutramine-HCl presented a reversible behavior and a peak maximum at -80 mV. Detection limit was 0.4 mg L-1 and the working linear range extended up to 33.3 mg L-1 (r = 0.99). Analysis of real and fortified samples enabled recoveries between 91 and 102%. The electroanalytical method was compared with a HPLC method which indicated it accuracy

Synchronous scanning phosphorimetry for the selective determination of chrysene: a metrological study

Room-temperature phosphorimetry was used to quantify trace levels of chrysene in sugar-cane spirits and in fish bile. A selective phosphorescence enhancer (AgNO3) and synchronous scanning allowed the detection of ng amounts of chrysene. Accuracy (113 ± 17%) and selectivity was evaluated using the CRM-NIST-1647d - Priority Pollutant Polycyclic Aromatic Hydrocarbons in acetonitrile. Analysis of sugar-cane spirit samples enabled recovery of 108 ± 18% which agreed with the one achieved using HPLC. Method's uncertainty was equivalent to 3.4 ng of the analyte, however, the analyte pre-concentration (SPE) improved sensibility and minimized the relative uncertainty. Characterization and homogeneity studies in fish bile were also performed

Determination of trifloxystrobin in soy grape juice and natural water by photoinduced fluorescence and high-performance liquid chromatography

A fluorescent (340/380 nm) photochemical product, identified at m/z 206 by mass spectrometry was obtained by photo-derivatization (15 s ultraviolet exposure) in water/acetonitrile 10/90 v/v. The photoproduct was used for indirect determination of trifloxystrobin in water and soy grape juice by high-performance liquid chromatography and fluorescence detection. Separation was made under isocratic conditions (acetonitrile/water 70/30% v/v, at 1.0 mL min-1 and 35 °C) with trifloxystrobin photo-derivative eluting at 3.2 min. The influence of ultraviolet exposure was evaluated in short and long terms with photoproduct showing stability up to 120 min after 15 s of ultraviolet exposure. The limit of detection was 57 µg L-1 in water (87-109% recoveries). For soy grape juice, dispersive liquid-liquid micro-extraction was used to clean up and for pre-concentration (limit of detection of 9.5 µg kg-1 and 93-101% recoveries) attending to the maximum residue limits for citrus juices established by regulatory agencies. Potential interference by triazoles was evaluated

Direct determination of chlorine in the glycerin by-product of biodiesel production: A green approach using energy dispersive X-ray fluorescence spectrometry

Glycerin, by-product of biodiesel, is produced in large amounts and it contains several contaminants, including chorine (due to the neutralization stage using HCl). When using this glycerin as biomass to produce energy, the presence of alkaline chlorides may lead to the formation of corrosive fumes at high temperatures. In this sense, the knowledge of chloride content is important in order to decide the fate of this raw by-product. The direct spectrometric determination of chlorine is an analytical challenge. In this context, energy-dispersive X-ray fluorescence spectrometry provided direct and accurate determination, relying on external calibration based on sample dilution and matrix matching with mixture of pure glycerin and water and using NaCl as the analytical (primary) standard. Method limit of quantification was 50 mg kg−1, with analytical curve up to 1000 mg kg−1 (R2 = 0.9992), and repeatability below 5% were found to be adequate for such application in such highly salty samples (original concentrations at mg g−1). In addition to sample directly analysis, without any previous treatment but homogenization and dilution, not requiring chemical derivatization and the not using of toxic reagents are in consonance to the analytical green chemistry requirements, allowing direct analysis of sample with no chemical derivatization with toxic reagents