Desenvolvimento de métodos analíticos baseados em imagens digitais e imunossensores para aplicação em amostras farmacêuticas e ambientais
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Data
2022-02-18
Autores
Lamarca, Rafaela Silva
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Editor
Universidade Estadual Paulista (Unesp)
Resumo
O desenvolvimento de dispositivos para análise rápida, e que consuma volumes reduzidos de reagentes e solventes, em consonância com os conceitos de química analítica verde, vêm sendo tema de diversos estudos nas últimas décadas. Neste contexto, esses dispositivos se destacam, por oferecerem resultados equivalentes aos equipamentos de bancada, além de atenderem as demais prerrogativas supracitadas. Nesta tese foram desenvolvidos diferentes dispositivos de análise rápida para determinação de compostos farmacêuticos em amostras ambientais e farmacêuticas. Na primeira parte foram desenvolvidos dispositivos de análises rápidas para determinação de formaldeído, carbamazepina (CBZ), ciprofloxacina (CIP) e norfloxacina (NOR) em formulações farmacêuticas e produtos cosméticos usando imagens digitais captadas por smartphone. Para a determinação de formaldeído foram obtidos limite de detecção (LD) e limite de quantificação (LQ) de 0,200 mg kg-1 e 0,500 mg kg-1, respectivamente. Já para os fármacos, os LD e LQ variaram respectivamente de 3,00 mg L-1 e 5,00 mg L-1 para CBZ; 1,00 mg L-1 e 3,00 mg L-1 para NOR e 1,00 mg L-1 e 3,00 mg L-1 para CIP. As concentrações determinadas nas formulações cosméticas e farmacêuticas foram comparadas por espectrofotometria, e não foram evidenciadas diferenças significativas entre os resultados obtidos. O uso de imagens digitais mostrou-se uma alternativa eficaz, apresentando baixo custo, reduzido volume de amostra e reagentes (8,00 μL requirida para as análises), e com elevado potencial para implementação em laboratórios com limitados recursos para pesquisas. Na segunda parte deste trabalho, desenvolveram-se dois diferentes imunossensores para a determinação de ciprofloxacina em amostras de águas residuárias. Para o imunossensor impedimétrico, na superfície do eletrodo SPCE, foram imobilizados anticorpos anti-CIP para a determinação de CIP nas amostras. Neste imunossensor, foram obtidos respectivamente, LD e LQ de 1,00 x 10-7 μg mL-1 e 1,00 x 10-5 μg mL-1. A concentração determinada na amostra de água residuária foi 2,90 x 10-4 μg mL-1. A recuperação obtida nas amostras utilizando o imunossensor foi de 97 %, utilizando apenas 30,0 μL de amostra. E por fim, foi desenvolvido um imunossensor baseado em fibras ópticas de sílica para a determinação de ciprofloxacina em amostras de águas residuárias. A superfície da fibra óptica foi funcionalizada com um material polimérico condutor e sobre este foi imobilizado anticorpos anti-CIP. O método desenvolvido foi aplicado na determinação de CIP nas águas residuárias, obtendo concentrações de 267 e 549 ng L-1, recuperação de 91 %, limites de detecção e quantificação de 3,30 x 10-3 ng L-1 e 1,00 x 10-2 ng L-1, respectivamente, com uso de apenas 5,00 mL de amostra.
The development of device which permits fast analysis requiring low consumption of reagents and solvents and in agreement with green analytical chemistry has been researched in recent decades. Moreover, rapid analysis devices highlight, since they offer results equivalent compared to benchtop equipment. In this thesis different rapid analysis devices were developed for determination of pharmaceuticals compounds present in environmental samples and pharmaceutical formulations. In the first part, rapid analysis devices were developed for the determination of formaldehyde, carbamazepine (CBZ), ciprofloxacin (CIP) and norfloxacin (NOR) in pharmaceutical formulations and cosmetic products using digital images captured by smartphone. For the determination of formaldehyde in cosmetic products achieved LD and LQ of 0.200 mg kg-1 and 0.500 mg kg-1, respectively. The method for CBZ, CIP and NOR present in pharmaceuticals products achieved LD and LQ ranged respectively from 3.00 mg L-1 and 5.00 mg L-1 for CBZ; 1.00 mg L-1 and 3.00 mg L-1 for NOR and 1.00 mg L-1 and 3.00 mg L-1 for CIP. The concentrations determined in the cosmetic and pharmaceutical formulations were compared by spectrophotometric, and no significant differences were evidenced between the results obtained. The use of digital images proved to be an effective alternative, environmentally friendly, low cost requiring low sample volume and reagents (8.00 μL) and with high potential for implementation in different laboratories with limited resources for research. In the second part of this thesis, two different immunosensors were developed for the determination of ciprofloxacin in wastewater samples. For the impedimetric immunosensor, on the SPCE electrode surface an anti-CIP antibodies were immobilized for the determination of CIP in the samples. In this immunosensor, LD and LQ of 1.00 x 10-7 μg mL-1 and 1.00 x 10-5 μg mL-1 were obtained, respectively. The concentration determined in the wastewater sample was 2.90 x 10-4 μg mL-1. The recovery obtained in the samples using the immunosensor was 97% recovery using only 30.0 μL of sample. Finally, an immunosensor based on silica fiber optics was developed for the determination of ciprofloxacin in wastewater samples. A conductive polymeric material was functionalized over the optical fiber and anti-CIP antibodies were immobilized on the optical fiber surface. The method developed was applied in the determination of CIP in wastewater obtaining concentrations of 267 and 549 ng L-1, recovery of 91%, LD and LQ limits of 3.30 x 10-3 ng L-1 and 1.00 x 10-2 ng L-1, respectively, using only 5.00 mL of sample.
The development of device which permits fast analysis requiring low consumption of reagents and solvents and in agreement with green analytical chemistry has been researched in recent decades. Moreover, rapid analysis devices highlight, since they offer results equivalent compared to benchtop equipment. In this thesis different rapid analysis devices were developed for determination of pharmaceuticals compounds present in environmental samples and pharmaceutical formulations. In the first part, rapid analysis devices were developed for the determination of formaldehyde, carbamazepine (CBZ), ciprofloxacin (CIP) and norfloxacin (NOR) in pharmaceutical formulations and cosmetic products using digital images captured by smartphone. For the determination of formaldehyde in cosmetic products achieved LD and LQ of 0.200 mg kg-1 and 0.500 mg kg-1, respectively. The method for CBZ, CIP and NOR present in pharmaceuticals products achieved LD and LQ ranged respectively from 3.00 mg L-1 and 5.00 mg L-1 for CBZ; 1.00 mg L-1 and 3.00 mg L-1 for NOR and 1.00 mg L-1 and 3.00 mg L-1 for CIP. The concentrations determined in the cosmetic and pharmaceutical formulations were compared by spectrophotometric, and no significant differences were evidenced between the results obtained. The use of digital images proved to be an effective alternative, environmentally friendly, low cost requiring low sample volume and reagents (8.00 μL) and with high potential for implementation in different laboratories with limited resources for research. In the second part of this thesis, two different immunosensors were developed for the determination of ciprofloxacin in wastewater samples. For the impedimetric immunosensor, on the SPCE electrode surface an anti-CIP antibodies were immobilized for the determination of CIP in the samples. In this immunosensor, LD and LQ of 1.00 x 10-7 μg mL-1 and 1.00 x 10-5 μg mL-1 were obtained, respectively. The concentration determined in the wastewater sample was 2.90 x 10-4 μg mL-1. The recovery obtained in the samples using the immunosensor was 97% recovery using only 30.0 μL of sample. Finally, an immunosensor based on silica fiber optics was developed for the determination of ciprofloxacin in wastewater samples. A conductive polymeric material was functionalized over the optical fiber and anti-CIP antibodies were immobilized on the optical fiber surface. The method developed was applied in the determination of CIP in wastewater obtaining concentrations of 267 and 549 ng L-1, recovery of 91%, LD and LQ limits of 3.30 x 10-3 ng L-1 and 1.00 x 10-2 ng L-1, respectively, using only 5.00 mL of sample.
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Palavras-chave
Águas residuais - Análise, Imagens digitais, Biossensores, Medicamentos, Formaldeído