Determinação de fenitrotion em alvos artificiais de algodão por HPLC-UV e de pesticidas em resíduos sólidos por GC/MS

Content Provider	Semantic Scholar
Author	Barcellos, Michelle
Copyright Year	2017
Abstract	This work has as main focus the development of methodologies for the determination of agrochemicals in different matrices. The first chapter deals with the evaluation of the level of exposure of farmers in agricultural tractors with sealed cabins, during the actual application of fenitrotion in apple orchards. The exposure was evaluated through the use of artificial cotton targets with subsequent ultrasonic extraction and determination by liquid chromatography with ultraviolet detection (HPLC-UV). For the latter, a maximum response experimental design using the mobile phase composition of 35:65 (water: acetonitrile), column temperature at 40 ° C and mobile phase flow rate of 1.0 mL min was applied. The method was evaluated by criteria stipulated by ANVISA, showing good selectivity and calibration by addition of standard on the linear matrix in the range of 0.50 to 2.01 mL min. The methodology was shown to be accurate and accurate, with coefficients of variation between 0.17 and 3.41% and recovery levels between 94 and 104%. The method was able to detect fenitrothion on the matrix from 0.18 mg kg and quantify it from 0.50 mg kg. All actual samples of artificial cotton targets showed fenitrothion values below the detection limit of the method. The second chapter deals with the application of methodologies proposed by the Brazilian Standard, NBR 10004/2004, in the preparation of samples and determination of eighteen pesticides in diatomaceous and wastewater matrices from the petroleum industry. The liquid samples were submitted to liquid microextraction and the solid samples were subjected to ultrasonic extraction, determined by gas chromatography and mass spectrometry (GC/MS). The evaluation of the method showed ideal linearity (r> 0.99) in the external calibration for all analytes in two linear ranges studied, curve 1 of 0.5 to 10 μg L and curve 2 of 10 to 200 μg L . The daily precision of the method presented a slight imprecision, with variations between 7.80 and 13.50% for curve 1 and between 6.15 and 8.78% for curve 2. The intermediate precision presented values with greater variation, with Between 23.6 and 33.0% for curve 1 and 19.0 to 30.5% for curve 2. The accuracy of the method presented adequate values, with recovery levels between 94.4 and 103.7% for Curve 1, 103 to 109.8% and curve 2. Finally, the limits of detection and quantification demonstrated the ability of the method to determine the analytes within the limits stipulated by NBR 10004.
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Language	English
Access Restriction	Open
Content Type	Text
Resource Type	Article