Search results for "mines"
showing 10 items of 2609 documents
Chemiluminometric photo-induced determination of Strychnine in a Multicommutation flow assembly
2007
This paper deals on the determination of Strychnine, a potent and dangerous pesticide and the analytical procedure is based on the photo-induced chemiluminescence of the pesticide by means of the Multicommutation continuous-flow methodology. Small segments of the pesticide solution were sequentially alternated with segments of the solution for adjusting the suitable medium for the photodegradation. The required time of UV irradiation was obtained by stopped-flow during 150 s; then, the resulting solution formed alternated segments with the oxidizing solution containing 5 × 10−3 mol l−1 Ce(IV) in 0.6 mol l−1 nitric acid. The calibration range, from 2 μg l−1 to 50 mg l−1, resulted in a linear…
Application of ACC method to synchronous luminiscence: determination of alpha-tocopherol and alpha-tocopheryl acetate in beverages.
2001
A new method based on the Q parameter, that permits the determination of the C(compound A)/C(compound B) ratio without preparing calibration graphs of the two compounds, is proposed. This method has been applied to signals obtained by synchronous luminiscence. Simultaneous determination of alpha-tocopherol and alpha-tocopheryl acetate in beverages using synchronous fluorescence has been carried out. To isolate the compounds from samples, liquid extraction with n-hexane as the organic phase was employed. The presence of interferences was tested using the apparent content curves (ACC) method and the C(alpha-tocopherol)/C(alpha-tocopheryl acetate) ratio was calculated using the Q parameter. Th…
Enhanced flow-injection–chemiluminometric determination of sulphonamides by on-line photochemical reaction
2003
Abstract The viability of the tandem photochemical reaction-chemiluminescence detection has been studied for an heterogeneous group of sulphonamides (sulphamethoxazole, sulphadiazine, sulphamerazine, sulphamethoxypyridazine, sulphacetamide, sulphadimidine, sulphanilamide, sulphathiazole and sulphaguanidine) using sulphamethoxazole (whose chemiluminescent behaviour has not been previously reported) as a test substance. The ‘on-line’ photochemical-reaction of sulphonamides provides an enhancing influence on the chemiluminometric response of the drugs during their oxidation by potassium permanganate in sulphuric acid medium (sulphamethoxazole, sulphacetamide, sulphadimidine and sulphanilamide …
A chemiluminescence flow-based procedure for determination of carbaryl in natural waters exploiting multicommutation and enzymatic reaction
2007
A chemiluminescence procedure for the determination of carbaryl in natural waters using acetylcholinesterase and choline oxidase is described. The flow system designed to implement multicommutation approach controlled by microcomputer comprised five solenoid valves, two columns with immobilized enzymes on controlled pore glass beads and chemiluminometric flow cell. In the best experimental conditions a linear response ranging from 25 to 700 µg L-1 carbaryl was obtained. Water samples were spiked with carbaryl in order to access the accuracy and recoveries between 95 and 101% were obtained for a concentration level ranging from 25 to 100 µg L-1 carbaryl. Detection limit and variation coeffic…
Quantification of Imidacloprid in Honeybees: Development of a Chemiluminescent ELISA
2010
A Chemiluminescente Enzyme-Linked Immuno-Sorbent Assay (CL-ELISA) for determination and quantification of the fungicide imidacloprid in honeybees was developed in an indirect competitive format. The assay was optimized by determining: the optimal coating conjugate concentration and anti-imidacloprid antiserum dilution, the effect of the incubation time on the competitive step, the tolerance to organic solvents. The IC50 and the limit of detection (LOD) values were 14.8 ng mL-1 and 0.11 ng mL -1, respectively, similar to those of colorimetric ELISA with a calibration range of 0.1 – 2600 ng mL-1. Cross reactivity of some related compounds such as three imidacloprid metabolites, 6-chloro nicot…
Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry Analysis of Carbosulfan, Carbofuran, 3-Hydroxycarbofuran, and Other Metabolites in …
2007
The potential of liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QqTOF-MS) to identify and confirm carbosulfan and seven of its main metabolites (carbofuran, 3-hydroxycarbofuran, 3-ketocarbofuran, 3-hydroxy-7-phenol carbofuran, 3-keto-7-phenolcarbofuran, 7-phenolcarbofuran, dibutylamine) at trace levels from food is explored for the first time. The analytical method developed consists of pressurized liquid extraction (PLE) and LC-QqTOF-MS in positive ion mode, which attains unequivocal identification and quantification of the studied compounds in food, at levels well below of those of concern (0.05 mg/kg for the sum of carbosulfan, carbofuran, and 3-hydroxycarbofuran).…
In-tube solid-phase microextraction and liquid chromatography using a monolithic column for the selective determination of residual ethylenediamine i…
2009
The selective determination of the diamine ethylenediamine (EDA) in the presence of a higher amount of residual dimethylamine in cationic polymers has been developed. The strategy uses both a solution derivatization with a selective agent of primary amines such as o-phthaldialdehyde-N-acetyl-L-cysteine (OPA-NAC) and an in-tube solid-phase microextraction (IT-SPME) coupled to liquid chromatography (LC). A 70 cm long, 0.32 mm internal diameter, and 3 microm thick commercially available capillary column coated with 95% polydimethylsiloxane and 5% polydiphenylsiloxane was employed to replace the injection loop of a Rheodyne injection valve. A volume of 1 mL of derivatized sample was passed thro…
Automated on-line in-tube solid-phase microextraction-assisted derivatization coupled to liquid chromatography for quantifying residual dimethylamine…
2008
Abstract A method for the analysis of dimethylamine (DMA) by automated in-tube solid-phase microextraction (IT-SPME)-supported chemical derivatization coupled with high-performance liquid chromatography was developed. Extraction, derivatization and desorption were studied by using a capillary coated with 95% polydimethylsiloxane and 5% polydiphenylsiloxane. Solution derivatization and automated IT-SPME derivatization using 9-fluorenylmethyl chloroformate (FMOC) were compared. The proposed procedure provided adequate linearity, accuracy and precision in the 0.2–2.0 μg/mL concentration interval, and the limit of detection (LOD) was 50 ng/mL. The main advantages of the proposed procedure are: …
New Reusable Solid Biosensor with Covalent Immobilization of the Horseradish Peroxidase Enzyme: In Situ Liberation Studies of Hydrogen Peroxide by Po…
2019
Herein, we reported a chemiluminescent biosensor based on the covalent immobilization of the horseradish peroxidase (HRP) enzyme on a polydimethylsiloxane (PDMS) support to quantify in situ hydrogen peroxide (H2O2). The chemiluminescent reaction based on the use of luminol as an oxidizable substrate, with HRP as the catalyst, has been used in order to quantify H2O2 as the oxidizing agent. The performance of the proposed biosensor has been demonstrated to determine H2O2 liberated by cells in a culture medium and for evaluating the delivery of H2O2 from denture cleaner tablets, as examples of application. For both analyses, the results indicated that the biosensor is cost-effective, sensitive…
Derivatization of tertiary amphetamines with 9-fluorenylmethyl chloroformate for liquid chromatography: determination of N-methylephedrine.
2000
The fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) was evaluated for the derivatization of tertiary amphetamines prior to liquid chromatographic analysis. Conditions for the derivatization were investigated, including the reaction time, the derivatization reagent concentration and the pH, using N-methylephedrine as a model compound. On the basis of these studies, a method for the quantification of N-methylephedrine is presented. The method involves derivatization with FMOC at ambient temperature and separation of the derivatives formed on a LiChrospher C18, 5 μm, 125 × 4 mm id column using acetonitrile–water gradient elution. The proposed procedure shows good linearity, accuracy…