scholarly journals Detecção de Resíduos de Agrotóxicos no Mel de Abelha

2014 ◽  
Vol 2 (2) ◽  
pp. 17
Author(s):  
F. M. Silva ◽  
D. C. Coelho ◽  
A. V. Machado ◽  
R. O. Costa

<p>As abelhas A. melífera são uns dos mais importantes polinizadores de culturas, além disso, elas produzem mel, própolis, geleia real e cera. O mel, principal produto da atividade apícola, utilizado como alimento, adoçante e para fins terapêuticos (apiterapia), tem a imagem de ser natural, saudável e limpo sendo esse um produto muito valorizado no mercado externo por isso, a busca por rigorosos padrões de qualidade se torna necessária para atender a um mercado consumidor cada vez mais exigente. Dessa forma a identificação da origem floral e geográfica, a ocorrência de adulterações e as contaminações, principalmente com antibióticos e agrotóxicos no mel tem se tornado uma rota importante devido os quais podem acarretar problemas de saúde ao consumidor. A dispersão da matriz em fase sólida (MSPD) combinada às técnicas cromatográficas modernas como cromatografia a gás (GC) e cromatografia a líquido (HPLC) é uma alternativa para evitar os diversos inconvenientes encontrados nos métodos clássicos de extração. A proposta desse trabalho foi pesquisar os diferentes tipos de Análises e metodologias de detecção de resíduos de agrotóxicos no mel de abelha Apresentando diferentes metodologias para a execução de estudos para validação de metodologia em métodos analítico, utilizando as técnicas de dispersão da matriz em fase sólida, cromatografia a gás acoplada à espectrometria de massas e cromatografia líquida de alta eficiência com detector espectrofotométrico com arranjo de diodos.</p><p><strong>Pesticide Residues in Honey Pesticide Residues detection in Bee honey</strong></p><pre> </pre><p><strong> </strong>A. mellifera bees are one of the most important pollinators of crops in addition they produce honey, propolis, royal jelly and wax. Honey, the main product of beekeeping, used as food, sweetener and in therapy (apitherapy), has the image of being natural, healthy and clean making a highly valued product in the foreign market so the search for rigorous standards of quality is needed to meet a consumer market increasingly demanding. Thus the identification of floral and geographical origin, the occurrence of tampering and contamination, especially with antibiotics and pesticides in honey has become an important route because which can cause health problems to consumers. The dispersion of the solid phase matrix (PDDM) combined with modern chromatographic techniques as gas chromatography (GC) and liquid chromatography (HPLC) is an alternative to avoid the various drawbacks found in classical extraction methods. The purpose of this study was to investigate the different types of analyzes and pesticide residue detection methodologies in honey Introducing different methodologies for carrying out studies for validation of a method in analytical methods, using the matrix dispersion techniques in solid phase, gas chromatography coupled to mass spectrometry and high-performance liquid chromatography with UV detector with diode array.</p>

2015 ◽  
Vol 78 (1) ◽  
pp. 151-156 ◽  
Author(s):  
L. S. YU ◽  
F. LIU ◽  
H. WU ◽  
H. R. TAN ◽  
X. C. RUAN ◽  
...  

A method for detection of flumethrin residue in honey by high-performance liquid chromatography was established. After n-hexane–dichloromethane (4:6, vol/vol) extraction, the honey samples were concentrated by rotary evaporation, purified by an Oasis HLB solid-phase extraction column, and detected using a UV detector at 267 nm. The interference of the matrix was greatly reduced by optimizing pretreatment conditions; thus, the minimal detection limit of cyhalothrin was 0.005 mg/kg, the average recovery was 80.8 to 96.8%, and the coefficient of variation was 0.6 to 1.5%. The precision and reproducibility of this method was suitable and applicable for detecting flumethrin residue in honey. With this method, 135 honey samples from seven locations in the People's Republic of China were tested; 77 samples tested positive for flumethrin residue, resulting in a detection rate of 75.3%. Samples from the Guangdong province had the highest flumethrin residue level (0.122 mg/kg) of the locations tested. On the basis of analytical validation, the high-performance liquid chromatography has been shown to be a promising alternative for the analysis of flumethrin residue in honey samples.


2018 ◽  
Vol 10 (1) ◽  
pp. 94
Author(s):  
Iyan Sopyan ◽  
Widiastuty Irawati ◽  
Wiwiek Indriyati

Objective: Bezafibrate is the second generation of fibrate groups used as the drug of choice in the treatment of hyperlipidemia. The purpose of this study is to obtained a validated method for analyzing bezafibrate in urine using solid phase extraction (SPE)-High performance liquid chromatography (HPLC).Methods: Solid phase extraction (SPE) using hydrophilic-lipophilic balance (HLB) cartridge was performed for bezafibrate extraction from urine, afterward, a validation of analysis method using high-performance liquid chromatography (HPLC)-(UV) detection was conducted to parameters, including: selectivity (Rs), linearity (r), accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ). Results: Recovery extraction using SPE resulted %recovery 85-110%. The analysis was performed by high-performance liquid chromatography using reversed phase, C18 octadecylsilane (ODS) columns 250 x 26 mm, particle size 10 μl, with the composition of 0.01 M acetate buffer with pH 3.55: with percent composition (45:55) and 0.8 ml/minute on 230 nm UV detection. Validation includes selectivity, linearity, accuracy, precision LOD, and LOQ have fulfilled requirement value. Conclusion: The result of recovery extraction using SPE and validation of method exhibited the values that fulfilled the requirements and can be used for analysis bezafibrate in the urine.


2018 ◽  
Vol 67 (1) ◽  
pp. 93-102 ◽  
Author(s):  
Lenche Velkoska-Markovska ◽  
Biljana Petanovska-Ilievska ◽  
Aleksandar Markovski

Summary The modern apple production involves the use of large amounts of pesticides that can be found in processed products such as apple juice. Harmful effects of pesticide residues on humans, especially children, are well known, hence the content of pesticide residues in fruit, vegetables and their juices should be controlled. This study presents an application of a new, relatively simple and reliable analytical method for qualitative and quantitative determination of three organophosphorus and one organonitrogen pesticide residues in apple juices. The analysis utilizes reversed-phase high-performance liquid chromatography (RP-HPLC) followed by UV diode array detection. Prior to HPLC analysis, a solid-phase extraction (SPE) was used for analytes concentration and sample clean-up. Specificity, selectivity, linearity, precision, accuracy and limit of quantification (LOQ) were examined to assess the validity of the developed method. The method had satisfactory values of multiple correlation coefficients for calibration curves (R2 ≥ 0.95 ). The precision was evaluated for the retention times and peak areas, and the estimated values for relative standard deviations (RSD) were 0.05 % - 0.18 % and 0.09 % - 0.62 %, respectively, which indicated an excellent precision of the proposed method. Under the established conditions, the recovery of analytes was 93.80 % - 119.41 %, with relative standard deviations below 0.56 %. This method was successfully applied for determination of some organophosphorus and organonitrogen pesticide residues in apple juices which were taken from Macedonian markets. The achieved values for LOQs were low enough compared to the MRLs of the investigated pesticides in apple according to the Regulation (EC) No 396/2005. Detectable residues of the examined pesticides were not found in the analyzed samples.


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