Simultaneous determination of propranolol and pindolol by synchronous spectrofluorimetry

A completely automated method to determine the most common parameters in cured meat products is proposed. The approach to full automation is based on the coupling of a robotic station for development of preliminary operations (namely weighing of the sample, grinding, leaching, filtration and transport to the aspiration zone) and a continuous unsegmented manifold for derivatisation and spectrophotometric monitoring of the reaction coloured products. This assembly works in an unattended fashion thus eliminating the bottleneck produced by the determination of these parameters in routine laboratories. The good agreement between results obtained by the proposed method and those from conventional methods for target analytes confirms its excellent performance and usefulness.     

Sensitive spectrophotometric determination of vanadium with hydrogen peroxide and 2-(5-chloro-2-pyridylazo)-5-dimethylaminophenol after extraction with N-benzoyl-N-phenylhydroxylamine

A selective and precise spectrophotometric determination of vanadium(V) is performed after preceding extraction with N-benzoyl-N-phenylhydroxylamine (BPHA). The color is developed in a water-ethanol solution with hydrogen peroxide and 2-(5-chloro-2-pyridylazo)-5-dimethylaminophenol (5-Cl-DMPAP). The molar absorptivity at 588 nm is (6.57 ± 0.05) × 10⁴ L mol^–1 cm^–1 at pH 2.1. The method permits the determination of vanadium (V) at trace levels in the presence of large amounts of other ions. It is applied to the determination of vanadium in aluminium (analytical reagent grade) and in human hair. High accuracy and precision is obtained.     

Analytical method for assessing exposure of greenhouse applicators to procymidone by gas chromatography and whole body dosimetry

Summary An analytical method for the determination of the potential and actual exposure of agricultural workers to procymidone has been developed. The methodology is based on the whole body technique, using Tyvek Pro-Tech and Sontara as sampling media, and uses hexane extraction, GC-ECD analysis and GC-MSD confirmation. The validation of the analytical method has been carried out incorporating the matrix of coverall in all steps when calculating parameters such as retention time window, limits of detection and quantification, linear ranges and precision. A field sampling strategy has also been developed and the method has been applied to the evaluation of the potential and actual dermal exposure of an applicator and an assistant in normal working conditions.     

Application of several modified peak purity assays to real complex multicomponent mixtures by high-performance liquid chromatography with diode-array detection.

Simple to use interactive self-modelling mixture analysis (SIMPLISMA), orthogonal projection (OPA) and Needle Search (NS) approaches have been applied to the determination of a number of compounds present in a complex multicomponent system. None of these three approaches succeeded completely when they were tested using the whole data matrix. When OPA and NS were applied to three simpler submatrices, obtained by dividing the total data matrix, and where a smaller number of compounds were present, better performance was achieved.     

The chromatographic quantification of hydrophobicity using micellar mobile phases

Summary In micellar liquid chromatography (MLC), the hydrophobicity of a compound is the predominant factor in its retention and interaction with micelles. A non-linear empirical model can describe the dependence between the retention factor (logk) in MLC and the logarithm of partition coefficients octanol-water (logP). An algorithm based on such a model has been used to makelogP predictions. Retention data for series of neutral compounds eluted with different mobile phases and alkyl-bonded stationary phases have been used to test the predictive ability of the algorithm. The results of this approach are compared with those obtained from automatic computational software packages.     

Flow-injection spectrofluorimetric determination of ethylenethiourea

A flow-injection configuration is proposed for the fluorimetric determination of ethylenethiourea. The procedure is based on the inhibitory effect of ethylenethiourea on the oxidation of thiamine to thiochrome by mercury(II). A linear calibration graph was obtained between 0.1 and 2.0 μg mL^–1, with a sampling rate of 40 samples per hour and a relative standard deviation of about 1.11%. The usefulness of the method was tested for the determination of ethylenethiourea residues in water, milk, potatoes, pear, grape and apple. Received: 26 January 1998 / Revised: 6 April 1998 / Accepted: 9 April 1998     

New diterpenoids extractives of Maytenus dispermus

The light petroleum extract of Maytenus dispermus has been shown to contain, in addition to pristimerin and maytenone, three new diterpenes: Maytenoquinone (1), 12-methoxytotarol (dispermol), and 12-hydroxy-7-oxototarol (dispermone), together with the known compounds: sugiol and β-sitosterol.     

Extraction of the (C4H9)4N+Co(II)SCN− ion-pair in chloroform and in isoamyl alcohol: Spectrophotometric determination of cobalt

When excesses of ammonium thiocyanate and tetrabutylammonium chloride are added to a cobalt(II) solution, a water-insoluble ion-pair is formed; this compound is soluble in chloroform, isoamyl alcohol, and other solvents. The variables which affect the extractions by these two solvents are studied in order to obtain the optimal conditions and two alternative extraction procedures are proposed. Thus, the separation of cobalt as a previous step for its spectrophotometric determination is studied.