Search results for "Reproducibility"
showing 10 items of 1976 documents
Selective and sentivive method based on capillary liquid chromatography with in-tube solid phase microextraction for determination of monochloramine …
2015
Abstract Due to the difficulties of working with chloramines, a critical examination of monochloramine standard preparation has been performed in order to select the best synthesis conditions. The analyte has been determined by in-tube solid phase extraction coupled to capillary liquid chromatography with UV detection (IT-SPME Capillary LC DAD). Potential factors affecting the response of monochloramine such as the pH of mobile phase and the volume of sample processed by IT-SPME Capillary LC DAD have been investigated and optimized. According to the results of the study, 0.1 mL or 4.0 mL of sample at neutral pH were loaded in the chromatographic system. A sensitive and selective method has …
Sensitive determination of methylenedioxylated amphetamines by liquid chromatography.
2001
Different strategies for the liquid chromatographic determination of methylenedioxylated amphetamines were evaluated: separation and detection of underivatized analytes by (i) UV or (ii) fluorescence, (iii) derivatization with 3,5-dinitrobenzoyl chloride followed by separation and UV detection of the derivatives formed and (iv) derivatization with 9-fluorenylmethyl chloroformate (FMOC) and subsequent separation and fluorimetric detection of the derivatives. The compounds tested were 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyethylamphetamine (MDE). On the basis of these studies, a new procedure for the chromatographic determination of…
Derivatization techniques for automated chromatographic analysis of amphetamine usingo-phthaldialdehyde: A comparative study
2000
The potential of different chromatographic systems for automated, on-line analysis of amphetamine in biological fluids is illustrated. The various systems integrate analyte purification and enrichment, separation, derivatization in different derivatization modes witho-phthaldialdehyde (OPA) and N-acetyl-L-cysteine (NAC), and fluorimetric detection. The reliability of the systems has been tested by analysing urine and plasma samples containing amphetamine in the 0.1–20.0 μg mL−1 range. Pre, on and post-column derivatization strategies are compared in terms of their instrumental requirements, selectivity, sensitivity, linearity and reproducibility.
Automated trace enrichment for screening and/or determination of primary, secondary and tertiary amphetamines in biological samples by liquid chromat…
1999
A rapid and simple liquid chromatographic method for the automated determination of amphetamines in biological fluids was developed. The proposed procedure is based on the injection of 250 microL of sample into a 20 x 2.1 mm id precolumn (packed with a 30 microns Hypersil C18 stationary phase) for enrichment and purification of the analytes. Next, the analytes are transferred to a 5 microns LiChrospher 100 RP18, 125 x 4 mm id analytical column for their separation under reversed-phase conditions. Water was used to eliminate the matrix components from the precolumn and a 0.2 M phosphate buffer (pH 3) containing 2% triethylamine was the mobile phase for the resolution of the amphetamines. The…
Photo-induced chemiluminescence determination of the pesticide Buminafos by a Multicommutation flow-analysis assembly
2008
Abstract The preliminary experiments in this paper deal with the photo-induced chemiluminescent behaviour of Buminafos family, after the experimental screening tests and several of them resulted positive, the herbicide Buminafos was selected to develop a new analytical method. The determination of Buminafos was performed with the aid of a Multicommutation (a solenoid valve set) assembly. The method involves the on-line photo-degradation of the analyte (stopped flow, 5 s) with the selected suitable medium (0.05% hydrogen peroxide) and its subsequent chemiluminescent oxidation by the potassium permanganate. Sample solution alternated segments with the photo-degradation medium; and, after the …
Spectrophotometric determination of mercury(II) and silver(I) with copper(II) and diethyldithiocarbamate in the presence of triton X-100
1986
Abstract Procedures for the determination of mercury and silver by displacement of diethyldithiocarbamate (DDTC) from its copper complex in the presence of 1% Triton X-100, and measurement of the decrease in the Cu(DDTC) 2 absorbance, are described. The use of the surfactant avoids the need for an extraction step. Reproducibility within 1% and detection limits of 0.25 ppm Hg(II) and 0.45 ppm Ag(I) have been obtained, and linear calibration ranges up to 13 ppm Hg(II) and 15 ppm Ag(I). In the presence of 0.1 M EDTA very good selectivity is achieved.
Photo-induced chemiluminescence-based determination of diphenamid by using a multicommuted flow system
2007
This manuscript deals with the application of molecular connectivity calculations to predict the photo-induced chemiluminescent behaviour of the family of herbicides grouped as amides. Several compounds of this group were theoretically studied by means of a general discriminant equation formerly obtained, being 18 of them (plus eight from the chloroacetanilide sub-group) predicted with a high probability as photo-induced chemiluminescent. Empirical confirmation of the chemiluminometric behaviour was performed with some few commercially available amide herbicides. On the basis of these results, a new multicommutation-photo-chemiluminescent method is proposed for the determination of the diph…
Automated determination of amisulpride by liquid chromatography with column switching and spectrophotometric detection.
2003
A fully automated chromatographic method including on-line blood serum or plasma clean-up, isocratic high-performance liquid chromatography (HPLC) and spectrophotometric detection was developed for quantitative analysis of the new antipsychotic drug amisulpride. After injection of serum or plasma onto the HPLC system and clean-up on a pre-column (10x4.0 mm I.D.) filled with Silica CN 20 micrometer (pore size 10 nm) by an eluent consisting of 8% acetonitrile in deionized water, the chromatographic separation was performed on Lichrospher CN (5 micrometer; 250x4.6 mm I.D.) by an eluent consisting of 50% acetonitrile and 50% aqueous potassium phosphate buffer (0.008 M, pH 6.4). The UV detector …
Multimycotoxin LC-MS/MS Analysis in Tea Beverages after Dispersive Liquid-Liquid Microextraction (DLLME).
2017
The aim of the present study was to develop a multimycotoxin liquid chromatography tandem mass spectrometry (LC-MS/MS) method with a dispersive liquid-liquid microextraction procedure (DLLME) for the analysis of AFs, 3aDON, 15aDON, NIV, HT-2, T-2, ZEA, OTA, ENNs, and BEA in tea beverages and to evaluate their mycotoxin contents. The proposed method was characterized in terms of linearity, limits of detection (LODs), limits of quantification (LOQs), recoveries, repeatability (intraday precision), reproducibility (interday precision), and matrix effects to check suitability. The results show LODs in the range of 0.05-10 μg/L, LOQs in the range of 0.2-33 μg/L, and recoveries in the range of 65…
Simultaneous homogeneous immunoassay of phenytoin and phenobarbital using a Nafion-loaded carbon paste electrode and two redox cationic labels
1997
Abstract The dual-analyte homogeneous immunoassay of two antiepileptic drugs was carried out simultaneously at physiological pH by square-wave voltammetry at a Nafion-loaded carbon paste electrode. Phenobarbital (PB) and phenytoin (DPH) were labeled by a cobaltocenium salt (Cc+) and a ferroceneammonium salt (N+Fc), respectively, and the corresponding standard redox potentials were −1.05 V and 0.26 V. Detection limits of 0.25 and 0.2 μM were achieved for PB-Cc+ and DPH-N+Fc (S/N = 3) after a 5-minute accumulation step, with linear responses over the 0.25–5 and 0.2–5 μM ranges, respectively. The relative standard deviation was evaluated to be ≥ 11% for 1 μM of each labeled drug. The separate,…