Solid-phase extraction clean-up of soil and sediment extracts for the determination of various types of pollutants in a single run

Dabrowska, Henryka; Dąbrowski, Ł.; Biziuk, Marek; Gaca, Jerzy; Namieśnik, Jacek

doi:10.1016/s0021-9673(03)00849-5

Cited by 58 publications

(22 citation statements)

References 32 publications

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“…Dentre estas, podem ser citadas a extração com fluido supercrítico (SFE, Supercritical Fluid Extraction), [5][6][7] extração acelerada com solvente (ASE, Accelerated Solvent Extraction), [8][9][10] extração assistida por micro-ondas (MAE, Microwave Assisted Extraction), [11][12][13] ou técnica que utiliza forte agitação como a extração por ultrassom (USE, Ultrasonic Extraction). 4,14,15 Outras técnicas como Soxhlet, [16][17][18] extração em fase sólida (SPE, Solid-Phase Extraction) 19,20 e microextração em fase sólida (SPME, Solid-Phase Micro Extraction) [21][22][23] também são utilizadas para determinação de agrotóxicos em sedimentos. A extração por ultrassom é uma técnica bastante versátil que permite a extração de várias amostras simultaneamente, sem demandar o uso de materiais sofisticados.…”

Section: Introductionunclassified

Aplicação da cromatografia gasosa bidimensional abrangente com microdetector de captura de elétrons para determinação de agrotóxicos em sedimentos

Silva¹,

Zini²,

Caramão³

2011

Quím. Nova

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. Analysis of seven pesticides in sediments was successfully achieved using comprehensive two-dimensional gas chromatography with micro-electron capture detection, as it provided higher sensitivity and less matrix interference. Repeatability and intermediate precision of peak areas and heights were less than 4% and the recovery percentage for the analytes ranged from 52 to 115%. Instrumental LOD and LOQ were in the range of 0.60 to 2.31 mg L -1 and 1.83 to 5.62 mg L -1, respectively. Concentrations of 3.34 mg kg -1 (dry basis) for trifloxystrobin and azoxystrobin (below the LOQ) were found in a sediment sample.Keywords: pesticides; two-dimensional gas chromatography; micro-electron capture detection. INTRODUÇÃOA utilização de agrotóxicos nas produções agrícolas vem obtendo cada vez mais destaque no cenário mundial. O controle de pragas, através do uso de diferentes princípios ativos, reduziu o índice de doenças para os homens e animais e proporcionou aumento na produção agrícola. Contudo, resíduos desses compostos podem permanecer no ambiente por longos períodos e causar impactos nocivos a diferentes ecossistemas. Nesse contexto, o monitoramento desses compostos em diferentes matrizes como ar, água, solo, sedimento e alimentos se torna de extrema importância para que problemas de saúde pública sejam minimizados e/ou evitados. 1O estudo da ocorrência de agrotóxicos em sedimentos fornece informação a respeito da contaminação do corpo hídrico receptor. O sedimento se comporta como fonte de acumulação de poluentes (compostos orgânicos em geral e metais, por exemplo) e este comportamento se relaciona diretamente com sua constituição físico-química. Este fato confere ao sedimento grande importância no que tange à investigação de processos físicos, geoquímicos e biológicos no ambiente.2 As suas propriedades físico-químicas podem influenciar tanto no transporte e destino desses compostos no ambiente quanto no comportamento dos mesmos durante as etapas de extração, limpeza (clean up) e análise instrumental. A interação existente entre os agrotóxicos e o sedimento pode ser bastante forte, resultando em resíduos quimicamente ligados à matriz. Tendo em vista este contexto, esforços significativos vêm sendo realizados para o desenvolvimento de métodos eficientes que possibilitem a análise multirresíduo de agrotóxicos, minimizando etapas de extração e de clean up das amostras. 24 O processo de extração por ultrassom proporciona um contato mais efetivo entre a matriz e o solvente, devido aos processos térmicos, mecânicos e de cavitação acústica. A exposição à irradiação ultrassônica faz com que haja formação de microbolhas, quando a pressão negativa exercida no sistema é alta o suficiente; sendo que, durante períodos de pressão positiva, as bolhas são comprimidas. Quando ocorre um colapso perto da superfície de um sólido, causado pela compressão e expansão das bolhas, as paredes do sólido podem ser danificadas e ter seu conteúdo (analitos) liberado para o meio. 25 Atualmente, a cromatografia gasosa é a técnica mais utilizada p...

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Section: Introductionunclassified

Aplicação da cromatografia gasosa bidimensional abrangente com microdetector de captura de elétrons para determinação de agrotóxicos em sedimentos

Silva¹,

Zini²,

Caramão³

2011

Quím. Nova

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“…Previous studies have focused on classical soil POPs sample preparation methodologies, such as the Soxhlet extraction and cartridge adsorption chromatography method, liquid-liquid extraction, and the concentrated sulfuric acid purification method (Anne et al 1996;Berdie and Grimalt 1998;Chen et al 2002;Concha-Grańa et al 2004;Dabrowska et al 2003;Douglas et al 2000;Lambropoulou et al 2006;Lino and da Silveira 1997;Saito et al 2004;Sporring et al 2005;Tekel and Hatrik 1996;Wiberg et al 2001;Xiong et al 2000). These methods are time-consuming and costly.…”

Section: Introductionmentioning

confidence: 99%

Optimization of extractants, purifying packings, and eluents for analytical extraction of organochlorine pesticides in Hydragric Acrisols

Zhao

Xia

Wang

et al. 2011

Environ Monit Assess

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In this study, we screened for an economic, rapid, and efficient hypotoxic pretreatment method for organochlorine pesticides in soil samples for gas chromatography (GC) analysis. The analytical extraction efficiencies of 11 different extractants, nine types of solid-phase purification (SPP) cartridge packings, and three types of eluents for 13 organochlorine pesticides (OCPs) in spiked and natural Chinese red soil (Hydragric Acrisols) were evaluated using an ultrasonic extraction and solid-phase purification method. High percent recoveries (85-106%) were obtained for the 13 organochlorine pesticides in soil when petroleum ether/acetone/water (10:5:2, v/v) was used an extractant. They were purified using celite SPP cartridge packing and eluted with 9 mL of dichloromethane/petroleum ether (1:9, v/v). The OCPs purification pretreatment of Hydragric Acrisols, using the above method, meets the GC analysis requirements. Compared with other traditional pretreatment methods for OCPs in soil samples, this method has several advantages, such as a short extraction time, reducing the amount of solvent, having no emulsion phenomenon, and hypotoxicity to the laboratory technicians. The concentrations of 1,1,1,-trichloro-2(p-chlorophenyl)-2-(o-chlorophenyl) ethane (DDTs; 3.42-8.08 ng g(-1)) in field soils were higher than the hexachlorocyclohexane concentration (2.94-6.12 ng g(-1)). The 1,1-dichloro-2,2-bis(p-chlorophenyl) ethylene (p,p'-DDE) + 1,1-dichloro-2,2-bis(p-chlorophenyl)-ethane (p,p'-DDD)/p,p'-DDT ratio in this field soil was approximately 2.7, suggesting that no new DDT pollution source was introduced into the sampling site.

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“…[3][4] Before chromatographic analysis, the extracts are usually purified by solid-phase extraction (SPE) with various sorbents, such as C 18 silica and Oasis HLB. [5][6] However, these sorbents are nonselective, usually resulting in low specificity and selectivity. [7][8] Molecular imprinting is a technique for obtaining selective binding sites in highly cross-linked polymers.…”

Section: Introductionmentioning

confidence: 99%

Study on the Binding Characteristic of Methamidophos‐Specific Molecularly Imprinted Polymer and the Interactions between Template and Monomers

Shen

Zhu

Yang

et al. 2008

J Chinese Chemical Soc

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A new molecularly imprinted polymer (MIP) was prepared using methamidophos (MAP) as the template molecule based on non-covalent interaction. The complexes formed between template and monomers before polymerization were characterized by 1 H NMR titration test, FT-IR and UV spectrometry study. These studies indicated that a 1:2 molecular complex formed dominantly between MAP and functional monomers. A model mainly involving cooperative hydrogen interaction was proposed by exact placement of functional groups. Association constant was estimated to be 2.894´10 6 L 2 /mol 2 . When the initial concentration of MAP was 1.0 mmol L -1 , the affinity capacity of MIP was 4.23 times that of NIP. The binding performance of MIP was modeled with the Freundlich isotherm (FI) and the total number of binding sites was calculated to be 33.97 mmol/g. The MIP showed great homogeneity with a heterogeneity index of m = 0.7356. The specificity of MIP was investigated by single-analyte binding and molecularly imprinted solid-phase extraction (MISPE) assays using MAP and other structurally related organophorous pesticides (OPPs). The results indicated that the MIP had a marked preference for MAP.

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Solid-phase extraction clean-up of soil and sediment extracts for the determination of various types of pollutants in a single run

Cited by 58 publications

References 32 publications

Aplicação da cromatografia gasosa bidimensional abrangente com microdetector de captura de elétrons para determinação de agrotóxicos em sedimentos

Aplicação da cromatografia gasosa bidimensional abrangente com microdetector de captura de elétrons para determinação de agrotóxicos em sedimentos

Optimization of extractants, purifying packings, and eluents for analytical extraction of organochlorine pesticides in Hydragric Acrisols

Study on the Binding Characteristic of Methamidophos‐Specific Molecularly Imprinted Polymer and the Interactions between Template and Monomers

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