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Master's Dissertation
DOI
https://doi.org/10.11606/D.64.2019.tde-08102019-164548
Document
Author
Full name
Jose Maurício Armelim
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
Piracicaba, 2019
Supervisor
Committee
Tornisielo, Valdemar Luiz (President)
Medeiros, Maria Aparecida Carvalho de
Cass, Quezia Bezerra
Title in Portuguese
Ocorrência de antibióticos em fazendas de cultivo de camarão (Litopenaeus vannamei) no estado do Rio Grande do Norte - Brasil
Keywords in Portuguese
Água superficial
Antibióticos
Antimicrobianos
Camarão
Carcinicultura
LC-ESI-MS/MS
Método multiclasses e multiresíduos
Resíduos
Sedimentos
SPE-Off line
SPE-On line
Abstract in Portuguese
Considerando os fatores de uso reconhecido de diferentes antibióticos na carcinicultura mundial, a potencialidade produtiva de camarões da região nordeste brasileira, os escopos de monitoramento de resíduos dos órgãos fiscalizadores e os riscos associados ao uso dos antibióticos à segurança alimentar e saúde pública, quanto a toxicidade e mecanismos de desenvolvimento da resistência microbiana patogênica, principalmente em meio aquático, o estudo teve por objetivo determinar simultaneamente, pela técnica de cromatografia líquida acoplada a espectrometria de massas com fonte de ionização electrospray (LC-ESI-MS/MS), a ocorrência de multiclasses e multiresíduos de 12 antibióticos, pertencentes às tetraciclinas, sulfonamidas, fluoroquinolonas e anfenicóis em amostras de camarão (Litopenaeus vannamei), água e sedimentos, procedentes de 5 fazendas criadoras de camarões com modelos distintos de produção, presentes no estado do Rio Grande do Norte-Brasil. Foram selecionados viveiros em fase de despesca para coleta das 3 matrizes e pontos a montante e jusante dos viveiros, para coleta das matrizes ambientais destinadas ao estudo de distribuição espacial dos resíduos nas fazendas. Parâmetros físico-químicos de qualidade da água foram avaliados durante as coletas. Foram empregadas as técnicas de extração em fase sólida on line a LC-MS/MS para sedimentos, cartuchos Captiva para filtragem dos extratos de músculo de camarões e extração em fase sólida off line a LC-MS/MS em água, com as amostras acondicionadas em cartuchos SPE previamente a realização do transporte ao laboratório. Os métodos cromatográficos foram validados para os parâmetros de seletividade, linearidade, limite de detecção (LD), limite de quantificação (LQ), exatidão, precisão e estabilidade de longa duração dos analitos na matriz. Os LQs encontrados variaram de 0,82 (sulfadimetoxina) a 7,63 (cloranfenicol) ng ml-1 para água, 1,23 (tetraciclina) a 15,99 (cloranfenicol) µg kg-1 para sedimentos e 1,24 (enrofloxacina) a 12,05 (sulfatizol) µg kg-1 para camarão. Resíduos de sulfadimetoxina (23,4 ng L-1) e florfenicol (10,78 a 175,77 ng L-1) foram os únicos antibióticos detectados e quantificados em água de viveiros. Em sedimentos, resíduos de oxitetraciclina, enrofloxacina e norfloxacina foram detectados somente à montante dos viveiros e em níveis -1) e montante (22,63 ng L-1) dos viveiros. A detecção de enrofloxacina e norfloxacina (-1) e oxitetraciclina, enrofloxacina e norfloxacina (< LQ) estiveram sob influência de instabilidade e efeito matriz. Por apresentar particularidades em uso e épocas, estudos para avaliação temporal dos resíduos são também recomendados.
Title in English
Occurrence of antibiotics in shrimp farms (Litopenaeus vannamei) - Rio Grande do Norte state - Brazil
Keywords in English
Antibiotics
Antimicrobials
Carcinicultura
LC-ESI-MS/MS
Multiclass and multiresidue method
Residue
Sediments
Shrimp
SPE-Off line
SPE-On line
Surface water
Abstract in English
Considering the factors of recognized use of different antibiotics in the global shrimp farming, the productive potential of shrimps in the northeastern Brazilian region, the residue monitoring scopes of inspection agencies and the risks associated with the use of antibiotics for food safety and public health, as well as toxicity and mechanisms of development of pathogenic microbial resistance, especially in the aquatic environment, the aim of the study was to determine, by the liquid chromatography coupled to mass spectrometry with source (LC-ESI-MS/MS), the occurrence of multiclasses and multiresidues of 12 antibiotics belonging to tetracyclines, sulfonamides, fluoroquinolones and amphenicols in shrimp (Litopenaeus vannamei), water and sediments from 5 farms shrimp farms with different models of production, present in the state of Rio Grande do Norte-Brazil. Raised nurseries were selected for collection of the 3 matrices and points upstream and downstream of the nurseries, for the collection of environmental matrices destined to the study of spatial distribution of residues in the farms. Physical-chemical parameters of water quality were evaluated during sampling. On line Solid-phase extraction techniques were used to LC-MS/MS for sediment, Captiva cartridges for filtration of shrimp muscle extracts and off-line solid-phase extraction to LC-MS/MS in surface water, with the samples packed in SPE cartridges prior to the transportation to the laboratory.The chromatographic methods validations were done for the parameters of selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision and long-term stability of the analytes in the matrix. LOQs ranged from 0.82 (sulfadimethoxine) to 7.63 (chloramphenicol) ng mL-1 for water, 1.23 (tetracycline) at 15.99 (chloramphenicol) ?g kg-1 for sediment and 1.24 (enrofloxacin) at 12.05 (sulfatiazole) ?g kg-1 for shrimp. Sulfadimethoxine (23.4 ng L-1) and florfenicol (10.78 to 175.77 ng L-1) residues were the only antibiotics detected and quantified in nursery water. In sediments, oxytetracycline, enrofloxacin and norfloxacin residues were detected only upstream of the nurseries and at levels -1) and upstream (22.63 ng L-1) of the nurseries. The detection of enrofloxacin and norfloxacin (< LQ) in sediments, upstream of two farms, suggest the inclusion of the compounds in the National Program for the Control of Residues and Contaminants in Food of Animal Origin (PNCRC/Animal) of the Brazilian Ministry of Agriculture, Livestock, and Food Supply (MAPA), program for monitoring in culture shrimp. The results shown by the real samples for florfenicol (<60 ng L-1) and oxytetracycline, enrofloxacin and norfloxacin (< LQ) were under influence of instability and matrix effect. Due to particularities in use and times, studies for the temporal evaluation of residues are also recommended.
 
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Publishing Date
2019-10-15
 
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