Development and validation of a GC-MS method for determination of 39 common pesticides in estuarine water – targeting hazardous amounts in the Douro River estuary

Rocha, Maria João; Ribeiro, Marta F. T.; Cruzeiro, Catarina; Figueiredo, Francisco; Rocha, Eduardo

doi:10.1080/03067319.2011.581366

Cited by 30 publications

(14 citation statements)

References 28 publications

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“…From previous studies, it was concluded that the current SPE technique followed by GC-MS analysis was considered suitable for environmental analysis of pesticides in the DAP fraction (Rocha et al 2011). Also, the presently validated USE method, followed by GC-MS/ MS, proved to be an ideal protocol to analyze pesticides from the SPM fraction, following all the validation parameters of the European guidelines (EU 2010).…”

Section: Discussionmentioning

confidence: 97%

“…The protocol used for the extraction of pesticides from DAP fraction, followed a previous solid-phase extraction (SPE; Rocha et al 2011) and a GC-MS/ MS analytical protocol recently amplified, for the analysis of 56 pesticides (Cruzeiro et al 2015). The recovery rates were always above 71 %, and limits ranged from 0.4 to 1.3 ng/L.…”

Section: Sample Preparationmentioning

confidence: 99%

“…The target and qualifier ions (MS) were determined by injection of individual pesticide standards, using full-scan mode (40-650 m/z). The product ions were compared with other methods (Lian et al 2010;Rocha et al 2011;Wong et al 2010;X. Yang et al 2011) and supported by NIST Mass Spectral Search Program (version 2.0, 2005) library to create a selected ion monitoring (SIM; Table 1).…”

Section: Sample Preparationmentioning

confidence: 99%

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Occurrence and seasonal loads of pesticides in surface water and suspended particulate matter from a wetland of worldwide interest—the Ria Formosa Lagoon, Portugal

Cruzeiro

Pardal²,

Rocha

et al. 2015

Environ Monit Assess

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Two novel methods were developed to extract and quantify 56 pesticides in surface waters, considering their content in both dissolved aqueous phase (DAP) and suspended particulate matter (SPM) fractions. These procedures were applied to coastal samples taken seasonally during 2012-2013, from three strategic sampling sites along the Ria Formosa Lagoon (south of Portugal). Briefly, 500 mL of water samples were filtrated, separating both fractions. The DAP fraction was extracted and pre-concentrated by solid-phase extraction (SPE), while the SPM was extracted using ultrasonic extraction technique (USE). Both fractions were then analyzed, and the pesticides were quantified and identified, within 35 min, by gas chromatography (GC) coupled to mass spectrometry (GC-MS and GC-MS/MS), respectively. The extraction of pesticides from the SPM fraction showed average recoveries of 102%, detection limits below 2.2 ng/L, and quantification limits ranging from 0.3 to 6.6 ng/L. Considering the real water samples, 73% of the selected pesticides were quantified in both DAP and SPM fractions (ΣDAP+SPM 2.3 μg/L) and their maximum levels were measured in autumn and winter. By category, the global loads of fungicides, herbicides, and insecticides were ≈407, ≈323, and ≈1.6 μg/L, respectively. Thirty-one percent of the quantified pesticides exceeded the European directives levels (2008/105/EC and 98/83/EC). From the total loads, the SPM fraction contribution was 32%, showing the importance of measuring pesticides in that fraction. The water physicochemical parameters revealed that the total nitrogen amounts were very high relatively to the legal required values, mainly close to the city of Faro (2.6 mg/L). In light of the above, measures are in need to meet European directives and protect both fauna and humans that use this area for leisure.

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Section: Discussionmentioning

confidence: 97%

Section: Sample Preparationmentioning

confidence: 99%

Section: Sample Preparationmentioning

confidence: 99%

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Occurrence and seasonal loads of pesticides in surface water and suspended particulate matter from a wetland of worldwide interest—the Ria Formosa Lagoon, Portugal

Cruzeiro

Pardal²,

Rocha

et al. 2015

Environ Monit Assess

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“…Besides, the area is one of the most industrialized of the country, supporting many industries, namely textiles, metal plating, leather tanning, rubber and plastic, cutlery and metalworking; high levels of pollution was registered in the last decades. As summarized by Rocha et al (2012a;2013b), the Douro river is an international watercourse that originates in north-central Spain, runs along the Spanish-Portuguese border, and enters the Atlantic Ocean at the city of Porto. The latter area is densely inhabited, with more than 700,000 residents in the last 8 km of the estuary.…”

Section: Sampling Areamentioning

confidence: 99%

“…However, the presence and effects of genotoxic pollutants cannot be discarded, and it is likely to occur, namely facing reports of pollution by different classes of chemicals. This is the case of the estuaries Mondego, Douro and Ave rivers, in Portugal, where chemical surveys have been systematically disclosing significant amounts of pollutants of various classes, often within biologically hazardous ranges (Carvalho et al 2009;Díez et al 2005;Madureira et al 2009Madureira et al , 2010Ramalhosa et al 2005;Ribeiro et al 2009a, b;Rocha et al 2011Rocha et al , 2012aRocha et al , b, 2013a. Taking all into consideration, we suspected that fish living in those estuaries faced different levels of stress, and could be differently impacted by genotoxicity.…”

Section: Introductionmentioning

confidence: 99%

Frequency of micronuclei and of other nuclear abnormalities in erythrocytes of the grey mullet from the Mondego, Douro and Ave estuaries—Portugal

Carrola

Santos

Rocha

et al. 2014

Environ Sci Pollut Res

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Fish are bioindicators of water pollution, and an increased rate of their erythrocyte nuclear morphological abnormalities (ENMAs)-and particularly of erythrocyte micronuclei (EMN)-is used as a genotoxicity biomarker. Despite the potential value of ENMAs and MN, there is scarce information about fish captured in Iberian estuaries. This is the case of the Portuguese estuaries of the Mondego, Douro and Ave, suffering from different levels of environmental stress and where chemical surveys have been disclosing significant amounts of certain pollutants. So, the aim of this study was to evaluate genotoxicants impacts and infer about the exposure at those ecosystems, using the grey mullet (Mugil cephalus) as bioindicator and considering the type and frequency of nuclear abnormalities of erythrocytes as proxies of genotoxicity. Sampling of mullets was done throughout the year in the important Mondego, Douro and Ave River estuaries (centre and north-western Portugal). The fish (total n=242) were caught in campaigns made in spring-summer and autumnwinter, using nets or fishing rods. The sampled mullets were comparable between locations in terms of the basic biometric parameters. Blood smears were stained with Diff-Quik to assess the frequencies of six types of ENMAs and MN (given per 1,000 erythrocytes). Some basic water physicochemical parameters were recorded to search for fluctuations matching the ENMAs. Overall, the most frequent nucleus abnormality was the polymorphic type, sequentially followed by the blebbed/ lobed/notched, segmented, kidney shaped, vacuolated, MN and binucleated. The total average frequency of the ENMAs ranged from 73‰ in the Mondego to 108‰ in the Ave. The polymorphic type was typically ≥50 % of the total ENMAs, averaging about 51‰, when considering all three estuaries. The most serious lesion-the MN-in fish from Mondego and Douro had a similar frequency (≈0.38‰), which was significantly lower than that in the Ave (0.75‰). No significant seasonal differences existed as to the MN rates and seasonal differences existed almost only in the Douro, with the higher values in AW. In general, the pattern of ENMAs frequencies was unrelated with the water physicochemical parameters. Considering the data for both the total ENMAs and for each specific abnormality, and bearing in mind that values of MN in fish erythrocytes >0.3‰ usually reflect pollution by genotoxicants, it is suggested that mullets were likely being chronically exposed to such compounds, even in the allegedly less polluted ecosystem (Mondego). Moreover, data supported the following pollution

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Priority Substances and Emerging Organic Pollutants in Portuguese Aquatic Environment: A Review

Ribeiro

Tiritan

2015

Reviews of Environmental Contamination and Toxicology Volume 238

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Aquatic environments are among the most noteworthy ecosystems regarding chemical pollution due to the anthropogenic pressure. In 2000, the European Commission implemented the Water Framework Directive, with the aim of progressively reducing aquatic chemical pollution of the European Union countries. Therefore, the knowledge about the chemical and ecological status is imperative to determine the overall quality of water bodies. Concerning Portugal, some studies have demonstrated the presence of pollutants in the aquatic environment but an overall report is not available yet. The aim of this paper is to provide a comprehensive review about the occurrence of priority substances included in the Water Framework Directive and some classes of emerging organic pollutants that have been found in Portuguese aquatic environment. The most frequently studied compounds comprise industrial compounds, natural and synthetic estrogens, phytoestrogens, phytosterols, pesticides, pharmaceuticals and personal care products. Concentration of these pollutants ranged from few ng L(-1) to higher values such as 30 μg L(-1) for industrial compounds in surface waters and up to 106 μg L(-1) for the pharmaceutical ibuprofen in wastewaters. Compounds already banned in Europe such as atrazine, alkylphenols and alkylphenol polyethoxylates are still found in surface waters, nevertheless their origin is still poorly understood. Beyond the contamination of the Portuguese aquatic environment by priority substances and emerging organic pollutants, this review also highlights the need of more research on other classes of pollutants and emphasizes the importance of extending this research to other locations in Portugal, which have not been investigated yet.

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Development and validation of a GC-MS method for determination of 39 common pesticides in estuarine water – targeting hazardous amounts in the Douro River estuary

Cited by 30 publications

References 28 publications

Occurrence and seasonal loads of pesticides in surface water and suspended particulate matter from a wetland of worldwide interest—the Ria Formosa Lagoon, Portugal

Occurrence and seasonal loads of pesticides in surface water and suspended particulate matter from a wetland of worldwide interest—the Ria Formosa Lagoon, Portugal

Frequency of micronuclei and of other nuclear abnormalities in erythrocytes of the grey mullet from the Mondego, Douro and Ave estuaries—Portugal

Priority Substances and Emerging Organic Pollutants in Portuguese Aquatic Environment: A Review

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