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Flow injection analysis with in-line solid phase extraction for the spectrophotometric determination of sulfonated and unsulfonated Quinoline Yellow in Cologne.

An integrated solid-phase spectrophotometry/ FIA method is proposed for the determination of the synthetic colorant matter Quinoline Yellow (QYWS) in the presence of its unsulfonated derivative QYSS. The procedure is based on the retention and preconcentration of the low level QYSS on a C-18 silica gel minicolumn, followed by sequential measurement of its absorbance at lambda = 410 nm after its elution with methanol. The applicable concentration range, the detection limit and the relative standard deviation were the following: for QYWS, from 0.10 to 30.0 mg L(-1); 0.013 mg L(-1); and 0.6%; and for QYSS, between 10 and 1.000 microg L(-1); 2 microg L(-1); and 1.3%, respectively. The method was applied to the determination of small amounts of QYSS present in QYWS in Colognes. Percentages of recovery between 98% and 99% were obtained in all instances. The method was also satisfactorily applied to the determination of these compounds in samples of commercial Colognes comparing the results for QYWS with those offered by an HPLC reference method and also validating the results chemometrically.

Journal Article↗

A flow injection analysis system involving immobilized NADH oxidase in column form for clinical analysis.

A highly sensitive FIA system for chemiluminometric determination of reduced coenzyme, NADH, was developed, using immobilized NADH oxidase from Brevibacterium ammoniagenes. The enzyme catalyzed the oxidation of NADH generating hydrogen peroxide which emitted chemiluminescence when mixed with luminol and potassium ferricyanide. The immobilized enzyme reactor was a mini-column, measuring 1 or 2 mm in inner diameter and 20 mm in length, and the sample volume was only 1 microliter per assay, with a feeding speed of one sample per min and a lowest detection limit of 10 pmol NADH. A FIA system was also developed for the determination of magnesium in human serum, using an enzyme column reactor with simultaneously coimmobilized hexokinase, D-glucose-6-phosphate dehydrogenase, and NADH oxidase. The performance of the system was as satisfactory as a routine colorimetric assay, but with much higher sensitivity.

Colorimetry↗

Enzymatic determination of ethanol in saliva by flow injection analysis.

Enzymatic photometric and fluorimetric methods are proposed for the determination of ethanol in saliva with determinative ranges of 2.5-15.0 mug ml(-1) and 1.0-20.0 mug ml(-1) respectively, i.e. covering the legal ranges after 1 : 100 dilution. A comparison between the ethanol content in saliva, breath and blood has been carried out on 12 individuals; the determination in saliva has been shown to be a good option.

Journal Article↗

Rapid-scan hydrodynamic voltammetry and cyclic voltammetry of pharmaceuticals in flow injection analysis conditions.

An on-line rapid-scan electrochemical detector is described for HPLC and FIA systems. Its practical use in qualitative analysis is demonstrated for 19 drug substances. The detector can be operated to record convection/diffusion-controlled (S-shaped), or diffusion-controlled (peak-shaped) voltammograms. In the latter mode, on-line cyclic voltammetry measurements are possible. The cell can also be used as an amperometric detector for conventional, microbore and micro-LC methods. Detection limits are of the order of 10 pg (conventional and microbore HPLC), or at the sub-picogram level (micro-LC). For scanning work, drugs can be analysed at mg l-1 levels in an FIA setup.

Caffeic Acids↗

Chromatography, flow injection analysis and electrophoresis in computer-assisted comparative biochemistry: its application and possibilities in clinical research. Preliminary studies on Crohn's disease.

A computer-assisted multicomponent analytical system, developed for comparative biochemical studies, was used for a clinical study of Crohn's disease in which 73 subjects, of comparable age and sex distribution, were considered: 40 with Crohn's disease, 16 with ulcerative colitis and 17 healthy volunteers as controls. Blood samples (5 ml) were taken to recover plasma and red cells. After extraction and fractionation of low- and high-molecular weight substances, the samples were analysed by ion-exchange chromatography and electrophoresis. The contents of amino acids, sugars, polyamines and proteins in the plasma and the red cells from the three groups of individuals were compared using statistical (means, variance, principal components analysis) and graphical profile methods. The first results indicate that the content of red cells, in comparison with plasma, allows the best differentiation of the three groups of subjects considered. In particular, the amino acids (Asp, Thr, Ser, Glu, Gly, Ala and Leu), the polyamines (spermidine and spermine) and glucose, show the most significant differences. The methodology followed and the results obtained, together with possible uses of this computer-assisted multicomponent analytical system in problems concerning clinical research, are discussed.

Adult↗