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Master's Dissertation
DOI
https://doi.org/10.11606/D.11.2021.tde-05082021-161735
Document
Author
Full name
Karoline Rayzel Rodrigues de Campos
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
Piracicaba, 2021
Supervisor
Committee
Mattos, Wanessa Melchert (President)
Sasaki, Milton Katsumi
Virgilio, Alex
Title in Portuguese
Emprego da extração sólido-líquido por partição à baixa temperatura para extração de propoxur de amostras de carne bovina
Keywords in Portuguese
Carne bovina
Extração sólido líquido
Imagens digitais
Propoxur
Química verde
Abstract in Portuguese
Propoxur é um pesticida empregado no controle de pragas como carrapatos, pulgas, baratas e vários outros insetos, sendo permitido, de acordo com órgãos regulamentadores, a concentração de até 50 μg kg-1 em amostras de carne bovina. Dentre os procedimentos relatados na literatura utilizando preparo de amostras para determinação de propoxur, estão a extração líquido-líquido convencional, extração por fluido supercrítico, extração em fase sólida e QuEChERS, extrações estas que apresentam como característica comum o emprego de elevados volumes de solventes orgânicos. Neste contexto, foi desenvolvido um procedimento de extração limpo para determinação de propoxur em carne bovina. O procedimento experimental otimizado consistiu da pesagem de 0,25 g de amostra, previamente moída, de carne fortificada, adição de 1 mL de metanol em tubo tipo Eppendorf®, agitação por 10 min a 200 rpm, centrifugação por 20 min a 2000 rpm e refrigeração a -80°C por 60 min. Em seguida, a fase orgânica foi vertida para outro tubo tipo Eppendorf®, ao qual reagentes apropriados foram adicionados para formação do azul de indofenol, e a determinação por imagens digitais foi realizada in situ. A resposta linear foi obtida para o intervalo de 3,0x10-5 a 8,0x10-4 mol L-1 de propoxur, descrita pela equação Sinal Analítico = 73 + 103x103 C (mol L-1), R = 0,999. Os limites de detecção e quantificação foram estimados em 3,0x10-5 mol L-1, coeficiente de variação (n = 11) foi estimado em 0,66%. Estudos de adição e recuperação de propoxur em amostras de carne bovina foram realizados obtendo porcentagem de recuperação entre 100 e 128%. O procedimento analítico desenvolvido é uma alternativa de preparo de amostra limpo, empregando baixos volumes de solvente orgânico e atendendo aos preceitos da química verde.
Title in English
Use of solid-liquid extraction with low temperature partitioning for extraction of propoxur in meat samples
Keywords in English
Digital images
Green chemistry
Meat
Propoxur
Solid liquid extraction
Abstract in English
Propoxur is a pesticide used to control pests such as ticks, fleas, cockroaches and various other insects, being allowed, according to regulatory agencies, the concentration of up to 50 μg kg-1 in meat samples. Among the reported procedures in literature for sample preparation aiming propoxur determination, the conventional liquid-liquid extractions, supercritical fluid extraction, solid-phase extraction and QuEChERS, extractions which have as a common feature the use of high volumes of organic solvents. In this context, a clean extraction procedure was developed to determine propoxur in meat. The optimized experimental procedure consisted of weighing 0.25 g of sample, previously minced, of fortified meat, 1 mL of methanol, were added in an Eppendorf ® type tube, stirred for 10 min at 200 rpm, centrifuged for 20 min at 2000 rpm and refrigerated at -80°C for 60 min. Then, the organic phase was poured into another Eppendorf ® tube, where appropriate reagents were added for indophenol blue formation, and the determination by digital image was performed in situ. Linear response was obtained between 3.0x10-5 to 8.0x10-4 mol L-1 of propoxur, described by the equation Analytical Signal = 73 + 103x103 C (mol L-1), R = 0.999. Limits of detection and quantification were estimated as 3.0x10-5 mol L-1, coefficient of variation (n = 11) was estimated as 0.66%. Studies of addition and recovery of propoxur in beef samples were performed obtaining a recovery percentage between 100 and 128%. The analytical procedure developed is an alternative for clean sample preparation, using low volumes of organic solvent and complying with the precepts of green chemistry.
 
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Publishing Date
2021-08-09
 
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