Samples of whole fluid pasteurized, UHT and powdered milk were analyzed for the presence of organophosphorus pesticide residues (OPR) using the QuEChERS method with detection by GC-FPD and confirmation by UPLC-MS/MS. A total of 23% of fluid milk samples and 27% of powdered milk samples contained at least one organophosphorus residue. The OPR found in the samples showed these can reach the milk and remain even after pasteurization, sterilization and drying processes. Some domestic sanitary residues were also present in the powdered milk samples. These residues have no LMR in Brazilian food legislation and are therefore not taken into account in food intake evaluations. There was an unidentified chromatographic peak in 30% of all the liquid and powdered milk samples, indicating the presence of some other contaminant.

Atualmente, a substância utilizada para o combate do vetor da dengue é o diflubenzuron, um larvicida que possui como principal efeito no ser humano a formação demetemoglobina. A determinação do percentual de metemoglobina (MHb) no sangue permite estabelecer a relação com a exposição ao diflubenzuron, sendo utilizada como indicador de efeito. O objetivo do presente trabalho foi avaliar a efetividade do uso da MHb como indicador da exposição ao diflubenzuron por meio da determinação de sua concentração no sangue de guardas de endemias atuantes em dois municípios do Estado do Rio de Janeiro. Para a avaliação da MHb, foi utilizado o método de análise preconizado por Evelyn-Malloy, a espectrofotometria no visível λmáx=630 nm, e as informações complementares foram obtidas por intermédio da aplicação de questionários semiestruturados. Foi observado que a maioria dos trabalhadores não fazia uso de Equipamento de Proteção Individual (EPI) e atuava em condições de trabalho insalubres e sem treinamento adequado. Houve redução de cerca de 0,05% da concentração da MHb após a exposição ao diflubenzuron, com correlação inversa deste indicador de efeito com a variável fumo (R= -0,742; p=0,035). Dado que a MHb pode ser formada após exposição a diversas substâncias químicas e considerando as dificuldades na logística de execução desta análise, estudos sobre novos biomarcadores mais sensíveis e seletivos são necessários.

Currently, the substance used to combat the dengue vector is diflubenzuron, a larvicide which produces methemoglobin (MHb) in humans. During his working process, applicators may be exposed to this substance at different levels, which depend on the care they adopt in handling and application. Knowing the profile of workers is important to characterize the population and assess the risks they face. The determination of the percentage of MHb in the blood allows to establish a relationship with exposure to diflubenzuron, being used as an indicator of effect. The objective of this study was to evaluate the extent to which these factors can affect the exposure of active endemic guards in two municipalities of the State of Rio de Janeiro contributed to a better understanding of the issues arising from this work process. It was observed that most workers did not use Personal Protective Equipment (PPE) and worked in unsafe working conditions and without proper training. Was observed a large difference in knowledge of the risks arising from the work they perform in the two counties, showing weaknesses in the basic training of these professionals. There was a reduction of about 0.05% of the MHb concentration after exposure to diflubenzuron, with an inverse correlation between this indicator variable effect with smoking (R= -0.742; p=0.035). Since MHb can be formed after exposure to various chemicals and considering the logistical difficulties in implementing this analysis, studies on new more sensitive and selective biomarkers are needed.

This paper regards the implementation of the QuEChERS method for the analysis by GC-FPD of 53 different pesticides from the organophosphate class, in whole UHT and pasteurized milk. Selectivity, linearity, repeatability, recovery and limits of detection and quantification were evaluated. Of all pesticide recoveries, 51 were considered satisfactory since the values ranged from 70 to 120% with RSD < 20%. The quantification limits ranged from 0.005 to 0.4 mg kg-1. The QuEChERS method was suitable for determination of 52 pesticides, presenting several advantages - quick, cheap, easy, effective, rugged and safe - with regard to other traditional methodologies.

Um modelo de procedimento para validação de método de ensaio para determinação de cinco agrotóxicos (γ - HCH, clorotalonil, fenitrotiona, clorpirifós e procimidona em matriz tomate) é demonstrado através da análise cromatográfica. A amostra processada é extraída com 30 mL de acetona e em seguida com 60 mL de uma mistura diclometano: éter de petróleo (1:1). O volume total é centrifugado e a alíquota orgânica é filtrada sob Na2SO4. Um mililitro de extrato orgânico é concentrado e dissolvido em um mililitro de iso-octano. Um microlitro do extrato é analisado no cromatógrafo a gás com detector por captura de elétrons - CG/DCE. Foram avaliados seletividade, linearidade, repetitividade, recuperação e limites de detecção e de quantificação. As recuperações obtidas variaram de 70 a 110%, considerando-se os níveis de adição de agrotóxicos/amostra de 0,02 a 2,50 mg.kg-1. Os limites de detecção do método variaram de 0,004 a 0,006 mg.kg-1 e os de quantificação entre 0,014 e 0,020 mg.kg-1.

A validation procedure model of a multiresidue method is presented for chromatographic analyses of five pesticides residues γ-HCH, chlorothalonil, fenitrothion, chlorpyrifos and procymidone applied on tomatoes. The tomatoes were processed and extracted by acetone plus a mixture of dichloromethane:petroleum benzine (1:1). The volume was centrifuged and was then filtered under Na2SO4. One milliliter of organic extract was concentrated then diluted in isooctane and one microliter was analyzed in the gas chromatograph with electron capture detector - GC/ECD. The parameters evaluated were selectivity, linearity, repeatability, recovery, and limits of detection and quantification. The recovery ranged from 70 to 110% in the concentration range of 0.02 to 2.50 mg.kg-1. The limits of detection ranged from 0.004 to 0.006 mg.kg-1 and the limits of quantification were between 0.014 to 0.02 mg.kg-1.

A proficiency assay of the determination of dithiocarbamate pesticide residues in banana was carried out. Fourteen laboratories participated in this study. Homogeneity and stability testing were performed by INCQS on the samples sent to the laboratories. Analytical results supplied by the pesticide residues laboratory of the VWA/KvW, Amsterdam, Holland, were used to define the designated value for the thiram concentration in the study samples. RESULTS: Fifty percent of the participating laboratories had satisfactory results. Efforts are needed to improve the precision of the analytical results and to decrease the number of false negative results observed.