RESUMO
A novel method for determination of carbaryl in effluent was proposed in this study. The kinetic evolution of excitation-emission matrix fluorescence (EEM) for the pesticide were recorded and come into being a four-way data array. The four-way fluorescence data were analyzed using the parallel factor analysis (PARAFAC). The methodology exploits the second-order advantage of three-order calibration based on quadrilinear parallel factor analysis, allowing analyte concentrations to be estimated even in the presence of an uncalibrated fluorescent background. It gave the satisfactory results for determination of the carbaryl in effluent samples. In addition, the kinetic study of degradation of carbaryl was performed according to the kinetic profile provided by the calibration.
Assuntos
Carbaril/análise , Praguicidas/análise , Espectrometria de Fluorescência/métodos , Calibragem , Hidrólise , Cinética , ÁguaRESUMO
The present paper presents a novel method for simultaneous determination of the three pesticides, carbaryl, carbendazim and 1-naphthol in honey. The excitation-emission matrix fluorescence data from calibration and prediction samples composed a three-way data array and then were analyzed using the second-order calibration method based on the self-weighted alternating trilinear decomposition (SWATLD). The second-order advantage of the SWATLD-based second-order calibration method was exploited, which makes it possible that calibration can be performed even in the presence of unknown interferences. The method was applied to determine the pesticides in the complex matrix of the honey sample. After the calibration step the recoveries of carbendazim and 1-naphthol were satisfactory. The quantification of carbaryl using the second-order standard addition method (SOSAM) based on SWATLD and the high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS) were performed to validate the concentration of carbaryl in honey samples.
Assuntos
Mel/análise , Praguicidas/análise , Calibragem , Cromatografia Líquida de Alta Pressão , Fluorescência , Espectrometria de Massas , Estrutura Molecular , Praguicidas/química , Software , Fatores de TempoRESUMO
This paper proposes a new and effective approach for the quantitative analysis of sulpiride, a significant antipsychotic drug, in human urine samples by the incorporation of excitation-emission matrix (EEM) fluorescence and second-order calibration methodologies based on the alternating fitting residue (AFR) and self-weighted alternating trilinear decomposition (SWATLD) algorithms. With the application of a second-order advantage, the proposed strategy could be utilized for a direct concentration determination of sulpiride with a simple pretreatment step, even in the presence of serious natural fluorescent interferences. The average recoveries of sulpiride in complex urine samples by using AFR and SWATLD with an estimated component number of three were 101.2 +/- 2.1 and 94.4 +/- 0.7%, respectively. Moreover, the accuracy of the two algorithms was also evaluated through elliptical joint confidence region (EJCR) tests as well as the figures of merit, such as sensitivity (SEN), selectivity (SEL) and limit of detection (LOD). The experimental results demonstrated that both algorithms, as promising quantitative alternatives, have been satisfactorily applied to the determination of sulpiride in human urine, but the performance of AFR was slightly better than that of SWATLD.