Extracción y Clean-up para Análisis de Residuos de Pesticidas en Muestras de Agua y Material en Suspensión del Río de la Plata (original) (raw)
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EVALUACIÓN DE CONTAMINANTES EN AGUA Y SEDIMENTOS DEL RÍO SAN PEDRO EN EL ESTADO DE AGUASCALIENTES
The San Pedro river is the main surface water body in the state of Aguascalientes. It crosses the state from north to south, covering a distance along a straight line of approximately 90 km until it meets the Santiago river in the state of Jalisco. In order to determine the level of pollution in the river and the probable infiltration of pollutants to the aquifer of the valley of Aguascalientes, water and sediment samples were collected from 50 sites along the river. Samples were also taken from 17 wells located near the river (less than 300 m). Two sampling campaigns were carried out, one during the dry season and the other after the rainy season. The pH, dissolved oxygen, BOD5, COD, total-P, total-N, phenols, anilines, detergents (MBAS), fecal coliforms and heavy metals (Al, As, Cd, Cr, Cu, Fe, Hg, Mn, Pb and Zn) were determined. The water of the San Pedro river presented high concentrations of organic matter, total-P, total-N, detergents and fecal coliforms. Some sites showed a moderate Al and Fe pollution. According to the United States Environmental Protection Agency criteria, all the sediment samples were polluted by As, 50% by Pb and Zn, 25% by Cu, and approximately 13% by Mn and Cr. Three sediment samples presented a moderate pollution by Fe, and another three by Hg. The results obtained for the wells did not show conclusive evidence of pollution of the aquifer by the surface water
2020
The analysis of contaminants in foods are a fundamental requirement to ensure its safety and the safety of the consumers. As well as the relevant pollutants, pesticides are also a cause for concern due to their continuous and permanent use at each stage of the production process of crops. Due to the lack of competent laboratories accredited under NTC/ISO 17025:2017 in the country for analysis of pesticides in fruits, it is important to promote laboratory accreditation processes to ensure reliable results and the safety of food that is consumed nationally and exported internationally. One way to track the validity of laboratory tests is to participate in proficiency tests in which the results produced are evaluated. To achieve this objective, it is necessary to have well-characterized reference materials with known amounts of analyte and well-defined properties that allow the comparison in the measurements made. Therefore, in this work, a pilot production of a reference material for pesticide residue analysis in fruits with high water content was developed, as a tool for the evaluation of laboratories that perform this type of analysis. The material was prepared using gulupa as matrix and 10 pesticides with different physicochemical properties (atrazine, boscalid, carbendazim, carbofuran, chlorpyrifos, cymoxanil, heptenophos, malathion, metalaxyl-M and metazachlor). For the characterization of the material, an accurate and reliable measurement method based on the QuEChERS extraction procedure and analysis by liquid chromatography coupled to tandem mass spectrometry CL-MS/MS was developed and validated. The mass fractions together with the combined uncertainties in the material for each pesticide were: atrazine 39.56 µg/kg ± 4.74 µg/kg, boscalid 30.12 µg/kg ± 2.75 µg/kg, carbendazim 88.76 µg/kg ± 9.83 µg/kg, carbofuran 28.78 µg/kg ± 3.55 µg/kg, chlorpyrifos 34.70 µg/kg ± 3.21 µg/kg, cymoxanil 88.17 µg/kg ± 5.98 µg/kg, heptenophos 76.15 µg/kg ± 9.04 µg/kg, malathion 31.11 µg/kg ± 3.42 µg/kg, metalaxyl-M 153.10 µg/kg ± 16.91 µg/kg; metazachlor 19.72 µg/kg ± 2.43 µg/kg. VIII To evaluate the suitability of the reference material, studies were carried out on the homogeneity and stability of the pesticides in matrix. The results indicate that the contribution of the heterogeneity of the pesticides in the samples on uncertainty is between 3.10 % and 6.73 %. For the stability study, an isochronous design was used, three temperature values were evaluated for seventy-nine days (18 °C, 4 °C,-20 °C and-80 °C as the reference temperature value). The results indicate that there was no degradation of any analyte at-20 °C during the period of evaluation, which suggests that at this temperature value the MR should be transported and stored, before and during its participation in intercomparison tests. The contribution to the uncertainty due to the stability of pesticides in matrix is between 2.33 % and 6.63 %. Therefore, as a final result of the pilot production, a protocol for the preparation of the reference material was obtained, which includes the details that should be considered to ensure its homogeneity and stability. These results constitute a good basis for the development of a certified reference material for analysis of pesticide residues in matrix.
AVANCES
Investigación en Ingeniería, 2017
El objetivo del presente estudio piloto fue analizar la toxicidad de los sedimentos del río Pasto en el tramo La Playita-Puente La Carolina en la cuenca alta, una zona con importante actividad agropecuaria donde el agua tiene múltiples usos, utilizando bacterias bioluminiscentes Vibrio fischeri como bioindicadores de toxicidad. El estudio se basó en la hipótesis de que ciertos microcontaminantes derivados del uso pesticidas en la zona, son transportados entre las matrices aguas/sedimentos y son los responsables de los niveles de toxicidad hallados. Los resultados señalan niveles variables de toxicidad y posiblemente el fenómeno predominante sea el transporte de pesticidas o sus metabolitos en la masa de agua. Además, se infiere que posiblemente la concentración de plaguicidas no sea la principal causa de los niveles de toxicidad hallados y probablemente podrían asociarse a otras sustancias derivadas del vertimiento de aguas residuales y lixiviados.
Validación de la metodología para análisis de residuos de plaguicidas en agua para consumo humano
2011
Since pesticides are one of the main chemical substances human beings are exposed to and due to the need to obtain reliable results, the objective of this work is to validate the analytic methodology. It is based on the Environmental Protection Agency (EPA) 505 revision 2.1 (1995): Analysis of organohalide Pesticide and commercial polychlorinated biphenyl (PCB) products in water by microextraction and gas chromatography, using as reference the Maximum Residues Level (MRL) established by the Argentine Food Code, according to ISO17025: 1999. For the extraction of pesticides, liquid-liquid extraction with hexane was used and later identification and classification was done by gas chromatography. The method presents good sensitivity with detection limits ranging from 0.003 to 0.3 ?g/L and quantification limits from 0.01 to 0.9 ?g/L. As regards accuracy, relative standard deviation was below 20% for all the substances analyzed. The method shows excellent linearity in the work range estab...