Determination of organochlorine pesticides and their metabolites in soil samples using headspace solid-phase microextraction

2001 ◽  
Vol 918 (1) ◽  
pp. 177-188 ◽  
Author(s):  
Ruey-An Doong ◽  
Pei-Lin Liao
Keyword(s):  
Organochlorine Pesticides ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Soil Samples ◽  
Headspace Solid Phase Microextraction

scholarly journals Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

2016 ◽  
Vol 81 (8) ◽  
pp. 923-934 ◽  
Author(s):  
Rada Djurovic-Pejcev ◽  
Tijana Djordjevic ◽  
Vojislava Bursic
Keyword(s):  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Optimum Number ◽  
Polydimethyl Siloxane ◽  
Headspace Solid Phase Microextraction ◽  
Relative Standard ◽  
Detection And Quantification

A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid) belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME) in combination with liquid-solid sample preparation (LS) was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl) content was perfor-med using 100 ?m polydimethyl-siloxane (PDMS) fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS) was used for detection and quantification, obtaining relative standard deviation (RSD) below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 ?g kg-1 of each herbicide. Limits of detection (LOD) were less than 1.2 ?g kg-1 for all the studied herbicides.

Liquid–Solid Sample Preparation Followed by Headspace Solid-Phase Microextraction Determination of Multiclass Pesticides in Soil

2012 ◽  
Vol 95 (5) ◽  
pp. 1331-1337 ◽  
Author(s):  
Rada D Ðurović ◽  
Tijana M Ðorðević ◽  
Ljiljana R Šantrić
Keyword(s):  
Sample Preparation ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Extraction Procedure ◽  
Soil Samples ◽  
Optimum Number ◽  
Headspace Solid Phase Microextraction ◽  
Extraction Solvents ◽  
Development And Validation

Abstract This paper describes development and validation of a multiresidue method for the determination of five pesticides (terbufos, prochloraz, chloridazon, pendimethalin, and fluorochloridone) belonging to different pesticide groups in soil samples by GC/MS, followed by its application in the analysis of some agricultural soil samples. The method is based on a headspace solid-phase microextraction method. Microextraction conditions, namely temperature, extraction time, and NaCl content, were tested and optimized using a 100 μm polydimethylsiloxane fiber. Three extraction solvents [methanol, methanol–acetone (1 + 1, v/v), and methanol–acetone–hexane (2 + 2 + 1, v/v/v)] and the optimum number of extraction steps within the sample preparation stage were optimized for the extraction procedure. LOD values for all the studied compounds were less than 12 μg/kg. Recovery values for multiple analyses of soil samples fortified at 30 μg/kg of each pesticide were higher than 64%. The method was proven to be repeatable, with RSD lower than 15%.

scholarly journals Development and optimization of headspace and headspace-solid phase microextraction for the determination of volatile fuel compounds in environmental sampless

2016 ◽  
Vol 6 ◽  
Author(s):  
María Balseiro-Romero ◽  
Raquel Chaves-Padín ◽  
Carmen Monterroso
Keyword(s):  
Contaminated Soils ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Soil Samples ◽  
Headspace Solid Phase Microextraction ◽  
Fuel Oxygenates ◽  
Volatile Organic ◽  
Benzene Toluene ◽  
Monoaromatic Hydrocarbons

The application of an effective and sensitive analytical method to determine soil contaminants is a crucial step in the monitoring and remediation processes. In the present work, we optimized the analysis of volatile organic compounds (VFOC) commonly present in fuel: oxygenates (FO-MTBE and ETBE-) and monoaromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene (BTEX). Headspace (HS) and headspace-solid phase microextraction (HS-SPME) were optimized in water samples, and validated for contaminated soils, using artificially spiked soils. Contaminants were identified and quantified by gas chromatography coupled to mass spectrometry (GC/MS). Matrix effect correction with surrogate standards resulted essential when analyzing soil samples, especially when the sample exerted a strong sorption on the contaminants.

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