Chemiluminescence determination of amikacin based on the inhibition of the luminol reaction catalyzed by copper.

A simple and sensitive method has been proposed for the amikacin sulphate determination. It is based on the inhibition of the chemiluminescence (CL) emission generated from the oxidation of luminol in alkaline medium by H2O2 catalyzed by Cu(II), due to the interaction caused by amikacin, which forms a robust complex with the catalyst. The optimization of the experimental and instrumental variables affecting this CL inhibition effect has been carried out using statistical models, based on the application of two-level full factorial and Box-Behnken designs. The performance characteristics of the proposed method have been established, showing that the method is efficient to determine amikacin sulphate in the linear range of 9.89-20 mg/L with a detection limit of 2.97 mg/L. It has been successfully applied to the amikacin sulphate determination in pharmaceutical formulations.

Determination of albumin in biological fluids by flow injection analysis using the peroxyoxalate chemiluminescent system in micellar medium.

A new sensitive analytical procedure for the determination of albumin is presented, based on the participation of a fluorescent derivative of the protein in the peroxyoxalate chemiluminescent system using imidazole as a catalyst. The chemiluminescent emission is detected in a flow injection analysis (FIA) system, employing micellar medium as carrier, whereas the derivatisation reaction is carried out off-line using fluorescamine as a label. The optimisation of the operational and chemical variables of the method such as concentration of reagents, flow-rates, injection volume, etc., involves the use of experimental designs, including Draper-Lin small composite design, scarcely used in analytical chemistry. The performance characteristics were established and a detection limit of about 0.1 fmol of albumin was obtained. The method has been validated and satisfactorily applied to the determination of albumin in human serum and urine.

A first and straightforward approach to detection limits for narrow-bore HPLC and CE.

Two methodologies have been proposed for a simple statistical estimation of the detection limits in microbore-HPLC and CE techniques. Due to the impossibility to measure the blank, by using the extrapolated or approximated expressions it is possible to obtain a straightforward approach of the detection limits from the study of the residuals of the calibration data set, avoiding tedious treatment of the signals. The utility of these expressions has been checked on the data from an experimental microbore HPLC system.

Method for the Quantitative Determination of 1-Naphthaleneacetic Acid in Spiked Canned Pineapple Samples by Micelle-Stabilized Room Temperature Phosphorescence.

This paper presents a convenient method for the determination of 1-naphthaleneacetic acid (NAA) plant growth regulator in spiked canned pineapple samples by micellar-stabilized room temperature phosphorescence with sodium dodecyl sulfate as a micellar medium, thallium nitrate as an external heavy atom, and sodium sulfite as an oxygen scavenger. A multivariate optimization approach using the type of central composite blocked cube-star design was carried out. The analytical curve of NAA gives a linear dynamic range of 70-500 ng mL(-)(1) with a detection limit of 21 ng mL(-)(1) and precision of 2.37% (n = 7). A mean recovery value of 98.6% was obtained for 250 ng mL(-)(1) NAA in the pineapple samples.

Derivative spectrophotometric resolution of mixtures of the food colourants Tartrazine, Amaranth and Curcumin in a micellar medium.

A study of the absorption spectra of the food colourants Tartrazine (E-102), Amaranth (E-123) and Curcumin (E-100) in various organic solvents and pH media, have been carried out. In addition, the spectral behaviour in aqueous micellar systems of anionic, cationic and non-ionic surfactants, as well as beta-cyclodextrin, was investigated. Analytical methods are proposed for the determination of the three dyes in mixtures without any prior separation step, by the application of the derivative technique to the normal absorption spectra, based on the use of cetyltrimethylammonium bromide (CTAB) in 0.1 M NaOH, over the concentration range 2-50 mug ml(-1). The methods are applied for determining the three dyes in commercial food products.

Spectrofluorimetric determination of boron in soils, plants and natural waters with Alizarin Red S.

A simple and sensitive spectrofluorimetric method for the determination of boron with Alizarin Red S is described. The fluorescence intensity of the complex formed in aqueous solution develops immediately and heating is not required. The excitation and emission wavelengths are 465 and 615 nm, respectively. The detection limit is 7.2 ng cm-3. A study was made of the influence of several ions as potential interferents. The method was applied satisfactorily to the determination of boron in soils, plants and natural waters.