Determination of trace amounts of carbaryl in water by solid-phase laser-induced fluorescence.

A quick and very sensitive method is proposed for the determination of the insecticide carbaryl, following transformation in 1-naphthol, using solid-phase fluorescence excited by a pulsed nitrogen laser and detected with a charge-coupled device. Carbaryl is hydrolized in an alkaline medium resulting in 1-naphthol. This hydrolysis product is fixed on QAE Sephadex A-25 gel at pH 11.20. The fluorescence of the gel, packed in a 1 mm silica cell, was measured directly using a solid-surface attachment. The detection limit obtained was 1.8 ng. A recovery study was carried out on several types of water samples to check the efficiency of the method. The results obtained are compared with data published in a previous paper where the LS-50 spectrofluorimeter was used. The detection and quantification limits are improved here by an order of magnitude.

Determination of warfarin at trace-levels in water by solid-phase spectrofluorimetry.

A new selective and sensitive spectrofluorimetric method for the determination of warfarin at trace levels (0.2-50.0 ng/ml) in water is proposed. Warfarin is fixed on Sephadex QAE A-25 gel (at pH = 7.0) and its fluorescence is measured directly in the solid-phase using a 1-mm silica cell at 312/385 nm with a detection/quantification limit of 0.06/0.2 ng/ml, a relative standard deviation of 2.3% and recoveries between 95 and 105%. The method is applied to the determination of warfarin residues in water.

Simultaneous determination of benomyl and morestan residues in waters by synchronous solid-phase spectrofluorimetry.

In this paper a new, sensitive, and simple method for simultaneous determination of pesticides morestan and benomyl at trace levels in waters is reported. Both chemicals, showing native fluorescence in solution at neutral medium, were fixed on C-18 silica gel at pH 1, giving a fluorescent system. The benomyl-morestan-silica gel system, after dry, was packed in a 1-mm silica cell and its synchronous fluorescence spectra were recorded at δλ=80 nm for determination of benomyl and δλ=25 nm for determination of morestan. Measurements of fluorescence were performed at λ1=289 nm and λ2=367 nm for benomyl and morestan analysis, respectively. The applicable concentration ranges were from 0.5 to 15.0 ng·ml(-1) for benomyl and from 0.6 to 15.0 ng·ml(-1) for morestan, with relative standard deviations of 1.2 and 1.5% for benomyl and morestan, respectively, being 0.15 and 0.18 ng·ml(-1) its respective detection limits. The method was applied to the simultaneous determination of residues of both pesticides in water of different provenances.

Simultaneous determination of carbaryl and o-phenylphenol residues in waters by first-derivative synchronous solid-phase spectrofluorimetry.

A spectrofluorimetric method for the simultaneous determination of carbaryl (CBL) and o-phenylphenol (OPP) residue mixtures in waters has been developed. Carbaryl was hydrolysed in alkaline medium to give 1-naphthol. This compound and o-phenylphenol were fixed on QAE Sephadex A-25 gel at pH 10.75. The fluorescence of the gel, packed in a 1-mm silica cell, was measured directly with a solid-surface attachment. Overlapping of conventional fluorescence spectra is resolved by using first-derivative synchronous spectrofluorimetry and allows for the complete resolution of the mixture. The range of application is between 0.4 and 25.0 ng/ml for OPP and 0.8 and 25.0 ng/ml for CBL. The detection limits for o-phenylphenol and carbaryl were 0.1 and 0.2 ng/ml, respectively. The accuracy and precision of the method are reported. The method is suitable for determination of carbaryl and o-phenylphenol residues in natural waters. Recoveries from 95 to 105% have been obtained for natural waters spiked with CBL and OPP.