New Spectrophotometric Methods for Estimation of Diosmin in Pharmaceutical Formulations Using Batch and FIA Systems

A new attempt is made to determine diosmin (DIO) in its pure form and in dietary supplements by using spectrophotometric flow injection analysis (FIA) assay method conjugated with batch method. The analysis was achieved depending on the oxidative coupling reaction with N, N-dimethyl-p-phenylenediamine (DMPD) to form a green dye which is measured at wavelength of 677 nm. The tested methods were found to be economical, delicate, precise and sturdy. The validation variables of the batch and FIA methods gave linearity in the determination range of DIO (1-35) μg/mL and (5-120) μg/mL demonstrated calibration graphs with linearity coefficient values of r2 =0.9989 and r2 =0.9991, respectively. Limits of quantitation (LOQ) values were found to be (0.8463 and 1.022) μg/mL, while limits of detection (LOD) were (0.2539 and 0.3067) µg/mL for the two methods, respectively. The precision for the developed methods denoted by relative standard deviation (RSD %), were 0.386 and 0.55 %, while the accuracy based on recovery values (Rec %) were 100.273 and 100.24, respectively. The relative error (RE %) was less than 1% for the batch method and (1.1%) for the FIA method. The values of these parameters were observed to fall within the specified accepted limits; therefore, the tested methods seem to be adequate for the analysis of DIO in pharmaceutical preparations.

Analytical Pervaporation: A Key Technique in the Enological Laboratory

This paper reviews the use of analytical pervaporation (defined as the integration of 2 different analytical separation principles, evaporation and gas diffusion, in a single micromodule) coupled to flow-injection manifolds for the determination of analytes of interest in enology; the review discusses the advantages that these techniques can provide in wine analytical laboratories. Special attention is given to methods that enable the determination of either of 2 volatile analytes, or of one volatile analyte and one nonvolatile analyte by taking advantage of the versatility of the designed approaches. In a comparison of these methods with the official and/or standard methods, the results showed good agreement. In addition, the new methods offer improvements in linear determination range, quantitation limit, precision, rapidity, and potential for full automation. Thus, this review demonstrates that although the old technologies used in wine analytical laboratories may be supported by official and standard methods, they should be replaced by properly validated, new, and automated technologies.

Determination of Zinc in Serum, Blood, and Ultrafiltrate Fluid from Patients on Hemofiltration by Graphite Furnace/Atomic Absorption Spectroscopy or Flow Injection Analysis/Atomic Absorption Spectroscopy

Two methods were optimized for the determination of zinc in samples of blood, serum, and ultrafiltrate fluid from patients with chronic renal impairment undergoing hemofiltration. In the first procedure, after acid digestion of the samples, Zn in blood and serum is determined by a system coupled to flow injection analysis and atomic absorption spectros-copy. The method is rapid, automated, simple, needs small amounts of sample, and has acceptable analytical characteristics. The analytical characteristics obtained were as follows: determination range of method, 0.05-2.0 ppm of Zn; precision as coefficient of variation (CV), 5.3%; recovery, 95-105%; and detection limit (DL), 0.02 ppm. The second method is optimized for ultrafiltrate fluid because the sensitivity of the first procedure is not suitable for the levels of Zn (ppb or ng/mL) in these samples. The technique chosen was atomic absorption spectroscopy with electrothermal atomization in a graphite furnace. The analytical characteristics obtained were as follows: determination range of method, 0.3-2.0 ppb Zn; CV, 5.7%; recovery, 93-107%; and DL, 0.12 ppb. The methods were used to determine zinc in samples of blood, serum, and ultrafiltrate fluid from 5 patients with chronic renal impairment undergoing hemofiltration to discover whether there were significant differences in the zinc contents of blood, serum, and ultrafiltrate fluid after the hemofiltration process. An analysis of variance of the experimental data obtained from a randomly selected group of 5 patients showed that zinc concentrations in the ultrafiltrate fluid, venous blood, and venous serum do not vary during hemofiltration (p < 0.05), whereas in arterial blood and serum, the time factor has a significant effect.

Development and evaluation of an immunoenzymometric assay for the chicken progesterone receptor

ABSTRACT A specific and sensitive immunoenzymometric assay (IEMA) was developed for measuring the quantity of chicken progesterone receptor (PR) in tissue cytosol. The assay uses two monoclonal antibodies to the PR. One is used to capture the PR. The second (labelled with biotin) reacts first with the captured receptor and subsequently with avidin-labelled horseradish peroxidase to provide an enzymatic end-point. The method has a determination range from 0·3 to 60 pmol/l. Intra- and interassay coefficients of variation were 3·7% and 9·0% respectively. The assay can be performed with equal results as a rapid (3 h) or an overnight procedure. The IEMA is convenient, especially for signal measurement and the calculation of results. No ultracentrifugation of samples is needed, since the IEMA can be performed on low-speed cytosol samples. Assay results correlated well (r = 0·927) with those obtained by the conventional ligand-binding assay used in our laboratory. Similar results were obtained with the IEMA and the ligand-binding assay after exposure of cytosol samples to increased temperatures: at 20 °C the PR remained stable for the 4-h period examined, whereas at 37 °C almost complete degradation of the PR was observed in 30 min. Being more than 100 times as sensitive as the ligand-binding assay, the IEMA enabled the quantification of PR for the first time in such tissues as the bursa and small intestine even of immature animals. Journal of Endocrinology (1991) 129, 189–196