ABSTRACT
A novel stepwise injection fluorometric method for the determination of epinephrine in human urine has been developed. In the current study, the stepwise injection analysis (SWIA) was successfully combined with on-line in-syringe cloud point extraction (CPE) and fluorometric detection. The procedure was based on the epinephrine derivatization in the presence of o-phenylenediamine followed by the preconcentration stage based on the CPE with the nonionic surfactant Triton X-114. After the phase separation into a syringe of the flow system, the micellar phase containing the epinephrine derivative was transported to a fluorometric detector. The excitation and emission wavelengths were set at 447 nm and 550 nm, respectively. The conditions of epinephrine derivatization and CPE have been studied. The calibration plot constructed using the developed procedure was linear in the range of 1·10(-11)-5·10(-7) mol L(-1). The limit of detection, calculated as 3 σ of a blank test (n = 10), was found to be 3·10(-12) mol L(-1). The proposed method was successfully applied for the determination of epinephrine in human urine samples.
Subject(s)
Epinephrine/urine , Fluorometry/methods , Calibration , Chromatography, High Pressure Liquid , Humans , MicellesABSTRACT
We suggest a novel approach for classification of flow analysis methods according to the conditions under which the mass transfer processes and chemical reactions take place in the flow mode: dispersion-convection flow methods and forced-convection flow methods. The first group includes continuous flow analysis, flow injection analysis, all injection analysis, sequential injection analysis, sequential injection chromatography, cross injection analysis, multi-commutated flow analysis, multi-syringe flow injection analysis, multi-pumping flow systems, loop flow analysis, and simultaneous injection effective mixing flow analysis. The second group includes segmented flow analysis, zone fluidics, flow batch analysis, sequential injection analysis with a mixing chamber, stepwise injection analysis, and multi-commutated stepwise injection analysis. The offered classification allows systematizing a large number of flow analysis methods. Recent developments and applications of dispersion-convection flow methods and forced-convection flow methods are presented.
Subject(s)
Flow Injection Analysis/classification , Flow Injection Analysis/methods , Flow Injection Analysis/instrumentationABSTRACT
The simple and easy performed automated method for the IR determination of petroleum products (PP) in water using extraction-chromatographic cartridges has been developed. The method assumes two stages: on-site extraction of PP during a sampling by using extraction-chromatographic cartridges and subsequent determination of the extracted PP using sequential injection analysis (SIA) with IR detection. The appropriate experimental conditions for extraction of the dissolved in water PP and for automated SIA procedure were investigated. The calibration plot constructed using the developed procedure was linear in the range of 3-200 µg L(-1). The limit of detection (LOD), calculated from a blank test based on 3σ was 1 µg L(-1). The sample volume was 1L. The system throughput was found to be 12 h(-1).
ABSTRACT
An automation of the extraction of analytes from solid samples into the aqueous phase based on multicommutated stepwise injection analysis concept has been suggested. The feasibility of the approach has been demonstrated by determination of ascorbic acid as model analyte. The method includes automated extraction of ascorbic acid from solid sample into borate buffer solution pH 8 in mixing chamber during vigorous mixing by nitrogen stream, and subsequent detection by capillary zone electrophoresis at 254 nm. The method has a linear range of 0.1-5.0 mg g(-1) for ascorbic acid with the LOD of 0.03 mg g(-1). The sample throughput was 7 h(-1). This method was applied for determination of ascorbic acid in various medicinal plants and food samples.
