Solid-phase microextraction of organophosphorus pesticides from water

Sng, Mui Tiang; Lee, F.K.; Lakso, Hans-Åke

doi:10.1016/s0021-9673(96)00727-3

“…[153] Since its development, this innovative technique has found widespread use in environmental analysis. It has, for example, been applied in the determination of volatile organic compounds, [154] biologically active substances, [155] phenols, [156] pesticides, [157] polyaromatic hydrocarbons, and polychlorinated biphenyls [158,159] in water. In a technical note it is presented the application of the SPME hyphenated with a temperature-programmed desorption (TPD) for the analysis of chemicals with wide-ranging volatilities without causing their thermal degradation.…”

Section: Solid-phase Microextraction (Spme)mentioning

confidence: 99%

Sample Preparation for Trace Analysis by Chromatographic Methods

Olariu

¹

,

Vione

²

,

Grinberg

³

et al. 2010

Journal of Liquid Chromatography & Related Technologies

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The determination of trace analytes in complex natural matrices often requires extensive sample extraction and preparation prior to chromatographic analysis. Correct sample preparation can reduce analysis time, sources of error, enhance sensitivity and enable unequivocal identification, confirmation and quantification. This overview considers general aspects on sample preparation techniques for trace analysis in various matrices. The discussed extraction/enrichment techniques cover classical methods, such as Soxhlet and liquid-liquid extractions along with more recently developed techniques like pressurized liquid extraction, liquid phase microextraction (LPME), accelerated microwave extraction, and ultrasoundassisted extraction. This overview also deals with more selective methodologies, such as solid phase extraction (SPE), solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The adopted approach considers the equilibriums involved in each technique. The applicability of each technique in environmental, food, biological and pharmaceutical analyses is discussed, particularly for the determination of trace organic compounds by chromatographic methods.

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“…Since its development, this innovative technique has found widespread use in environmental analysis. It has, for example, been applied in the determination of volatile organic compounds [241], [242], phenols [243], pesticides [244], polyaromatic hydrocarbons, and polychlorinated biphenyls [245] in water. SPME fibers have been used as air sampling devices for volatile organic compounds in ambient and workplace air and give results that are in good agreement with traditional sampling methods [246].…”

Section: Solid-phase Microextraction (Spme)mentioning

confidence: 99%

Sample Preparation for Trace Analysis

Begerow

¹

,

Dunemann

²

2006

Ullmann's Encyclopedia of Industrial Chemistry

2

0

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The article contains sections titled: 1. Introduction 1.1. A Strategy Appropriate to Trace Analysis 1.2. Avoidance of Systematic Errors 1.2.1. Trace Losses and Contamination 1.2.2. Uncertainty 2. Sample Preparation and Digestion in Inorganic Analysis 2.1. Sample Treatment after the Sampling Process 2.1.1. Stabilization, Drying, and Storage 2.1.2. Homogenization and Aliquoting 2.1.3. Requirements with Respect to Materials and Chemicals 2.2. Sample‐Preparation Techniques; General Considerations 2.2.1. Special Factors Associated with Microwave‐Assisted Digestion 2.2.2. Safety Considerations 2.3. Wet Digestion Techniques 2.3.1. Wet Digestion at Atmospheric Pressure 2.3.2. Pressure Digestion 2.3.2.1. Thermally Convective Pressure Digestion 2.3.2.2. Microwave‐Assisted Pressure Digestion 2.4. “Dry” Digestion Techniques 2.4.1. Combustion in Air 2.4.2. Combustion in Oxygen 2.4.3. Cold‐Plasma Ashing 2.4.4. Fusion 2.5. Illustrative Examples 2.5.1. Sample Preparation as a Function of Analytical Method 2.5.2. Combined Use of Multiple Decomposition Techniques 2.5.3. Comparative Merits of the Various Sample‐Preparation Techniques 2.5.4. Decomposition Procedures for Determining Nonmetals 2.6. Evaluation Criteria 2.6.1. Completeness 2.6.2. Uncertainty 2.6.3. Time Factors 2.6.4. The Final Result 2.7. Concentration and Separation of Inorganic Trace Materials 2.8. Automation and Direct Analysis 2.8.1. Automation 2.8.2. Direct Analysis 2.9. Analysis of Element Species 3. Sample Preparation in Organic Analysis 3.1. Sample Treatment after the Sampling Process 3.1.1. Stabilization, Drying, and Storage 3.1.2. Homogenization and Aliquoting 3.1.3. Requirements with Respect to Materials and Chemicals 3.2. Separation of the Analyte 3.2.1. Hydrolysis 3.2.2. Liquid ‐ Liquid Extraction 3.2.3. Soxhlet Extraction 3.2.4. Microwave‐Assisted Solvent Extraction 3.2.5. Supercritical Fluid Extraction (SFE) 3.2.6. Solid‐Phase Extraction (SPE) 3.2.7. Solid‐Phase Microextraction (SPME) 3.2.8. Stir‐Bar Adsorptive Extraction (SBSE) 3.2.9. Miscellaneous Techniques 3.3. Headspace Techniques 3.3.1. Static Headspace Technique 3.3.2. Dynamic Headspace Technique (Purge and Trap) 3.4. Determination of Trace Organic Materials in Air Samples 3.5. Analyte Concentration 3.6. Derivatization 3.7. Coupled Techniques Trace analysis is a very relevant and applications‐oriented branch of analytical chemistry. The sample preparation for trace analysis must be custom‐tailored to the problem at hand. Systematic errors can arise by contact with vessel materials, reagents, or the ambient atmosphere, as well as any change in chemical or physical state. In inorganic analysis, sample preparation has to meet the requirements for a substantially trouble‐free determination of the analyte. Digestion of the matrix (microwave digestion, wet digestion, dry digestion techniques) and subsequent careful comparison of several decomposition techniques is therefore an essentially important step. Some separation and concentration techniques of the analytes are liquid –liquid extraction, solid‐phase extraction, special precipitation reactions, and electrolytic deposition. The introduction of laboratory robots should make it possible to incorporate a significant degree of automation into the time‐consuming, labor‐intensive area of sample preparation as well, leading to more efficient, reliable, and reproducible sample work‐up. The goal of sample preparation in organic trace analysis is to isolate the analyte from the sample matrix (e.g., liquid‐liquid extraction, Soxhlet extraction, microwave‐assisted solvent extraction, steam distillation) and then concentrate it and convert it into a form suitable for analysis by the selected method. Separation and concentration of an analyte must often be followed by some type of derivatization. Various coupled sample preparation and determination processes are increasingly utilized in trace organic analysis.

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“…11,12 The application of SPME for retention of pesticides has been reported in various matrices including soil, 8 food, 13,14 river water, 15 rain water, 16 raw and treated water, 17 groundwater 18,19 and aqueous matrizes. [20][21][22][23][24][25][26] The technique consists in the extraction of analytes using a silica fiber coated with a layer of sorbent, which is exposed directly in the sample or in the headspace. After the equilibrium time has been reached, the fiber is introduced into the chromatographic system for desorption of the analytes.…”

Section: Introductionmentioning

confidence: 99%

Multiresidue methods for determination of pesticides using SPME and SPE followed by GC-NPD system: a comparative study

Milhome

¹

,

Sousa

²

,

Keukeleire

³

et al. 2011

J. Braz. Chem. Soc.

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Neste estudo, métodos multirresíduos usando extração em fase sólida (SPE) e microextração em fase sólida (SPME) são comparados na determinação de pesticidas em amostras aquosas. Parâmetros como tipo de fibras e espessura, solvente de eluição, volume da amostra, tempo de equilíbrio, coeficiente de partição e solubilidade foram investigados. Resultados satisfatórios foram obtidos para a análise de pesticidas usando cartuchos C18 e acetato de etila como eluente, com taxas de recuperação entre 75-107%. As melhores condições para SPME foram com uma fibra PDMS 100 µm de espessura, volume de amostra de 40 mL, e tempo de equilíbrio de 45 min. O método SPME é o mais adequado para a análise de pesticidas em água, devido à sua rapidez e simplicidade e ao não uso de solventes. Os limites de detecção e quantificação são inferiores aos limites de concentração máximos estabelecidos pelas autoridades brasileiras, sendo portanto aceitável.In this study, multiresidue method using solid phase extraction (SPE) and solid phase microextraction (SPME) are compared in the determination of pesticides in aqueous samples. Parameters such as fiber type and thickness, elution solvent, sample volume, equilibration time, partition coefficient and solubility were investigated. Satisfactory results were obtained for the analysis of pesticides using C18 cartridges and ethyl acetate as eluent, whith recovery rates between 75-107%. The best conditions for SPME fiber were PDMS with a 100 mm thick, sample volume of 40 mL, and reaction time was 45 min. SPME method is most suitable for the analysis of pesticides in water, due to its speed and simplicity and solvent-free. The limits of detection and quantification are below the maximum concentration limits established by Brazilian authorities and therefore acceptable.Keywords: pesticides, SPME, water analysis, microextraction, partition coefficient IntroductionThe protection of water quality is a real concern of government agencies that control public health. The worldwide intensive use of pesticides plays a key role in environmental contamination, especially in water resources. In the last years, Brazil has been considered the largest consumer of pesticides in the world. 1 Only in 2009, around 1 million ton of pesticides were sold in the country,mainly applied in soybean, corn, sugarcane and cotton cultures. 1 According to ANDEF, there were about 475 active ingredients and 1278 products registered. 2 Pesticides that remain in the environment or reach the aquatic systems pose risks to animal species by their toxicity and ability to bio-accumulate along the food chain. 3 The European Community has set the value of 0.1 mg L -1 for any individual pesticide and 0.5 mg L -1 for the total pesticide residues of pesticides. In Brazil, the maximum concentrations of pesticides in water are regulated by the Administrative Rule No. 518/2004 (drinking water) of the Milhome et al. 2049 Vol. 22, No. 11, 2011 Ministry of Health, by The National Environment Council (CONAMA) Resolution No. 357/2005(classification o...

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Solid-phase microextraction of organophosphorus pesticides from water

Cited by 75 publications

References 5 publications

Sample Preparation for Trace Analysis by Chromatographic Methods

Sample Preparation for Trace Analysis by Chromatographic Methods

Sample Preparation for Trace Analysis

Multiresidue methods for determination of pesticides using SPME and SPE followed by GC-NPD system: a comparative study

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