Fast determination of methyl chloride and methyl bromide emissions from dried plant matter and soil samples using HS-SPME and GC-MS: method and first results

2009 ◽  
Vol 6 (4) ◽  
pp. 311 ◽  
Author(s):  
Noureddine Yassaa ◽  
Asher Wishkerman ◽  
Frank Keppler ◽  
Jonathan Williams
Keyword(s):  
Methyl Bromide ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Methyl Chloride ◽  
Field Studies ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Spme Fibre ◽  
Non Destructive

Environmental context. Headspace solid-phase microextraction (HS-SPME) and analysis by gas chromatography–mass spectrometry (GC/MS) system has been employed for quantifying the emissions of methyl chloride (CH3Cl) and methyl bromide (CH3Br) from plants and soils. Compared with more commonly used techniques, HS-SPME coupled to GC/MS is simple, fast, sensitive, economical and non-destructive, with potential for laboratory-based and field studies. Abstract. Headspace solid-phase microextraction (HS-SPME) and gas chromatography–mass spectrometry (GC/MS) system have been employed for quantifying the emissions of methyl chloride (CH3Cl) and methyl bromide (CH3Br) from plants and soils. Seven SPME fibre coatings including 75 μm Carboxen-polydimethylsiloxane (CAR-PDMS), 85 μm Carboxen-PDMS (CAR-PDMS), 50/30 μm divinylbenzene-CAR-PDMS (DVB-CAR-PDMS), 65 μm DVB-PDMS, 65 μm carbowax-DVB (CW-DVB), 30 μm PDMS (PDMS) and 100 μm PDMS, were tested by comparing their sampling efficiencies towards CH3Cl and CH3Br. Key parameters such as extraction time, desorption temperature and time were all optimised in this work. The optimum conditions were found with CAR-PDMS 75 μm as an SPME fibre coating, a 1-min sampling time, a 50°C incubation temperature and a 2-min desorption time and a 250°C desorption temperature. These conditions were used for the determination of CH3Cl and CH3Br emission rates from different plant species as well as soil samples. Compared with more commonly used techniques, HS-SPME coupled to GC/MS is simple, fast, sensitive, economical and non-destructive, with potential for laboratory-based and field studies.

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.

scholarly journals Determination of atrazine, acetochlor, clomazone, pendimethalin and oxyfluorfen in soil by a solid phase microextraction method

2008 ◽  
Vol 23 (4) ◽  
pp. 265-271 ◽  
Author(s):  
Rada Djurovic ◽  
Jelena Gajic-Umiljendic ◽  
Tijana Djordjevic
Keyword(s):  
Sample Preparation ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Soil Samples ◽  
Extraction Time ◽  
Gas Chromatography Mass Spectrometry ◽  
Optimum Number ◽  
Extraction Solvent ◽  
Relative Standard

A solid phase microextraction (SPME) method for simultaneous determination of atrazine, acetochlor, clomazone, pendimethalin and oxyfluorfen in soil samples was developed. The method is based on a combination of conventional liquid-solid procedure and a following SPME determination of the selected pesticides. Initially, various microextraction conditions, such as the fibre type, desorption temperature and time, extraction time and NaCl content, were investigated and optimized. Then, extraction efficiencies of several solvents (water, hexane, acetonitrile, acetone and methanol) and the optimum number of extraction steps within the sample preparation step were optimized. According to the results obtained in these two sets of experiments, two successive extractions with methanol as the extraction solvent were the optimal sample preparation procedure, while the following conditions were found to be most efficient for SPME measurements: 100 ?m PDMS fibre, desorption for 7 min at 2700C, 30 min extraction time and 5% NaCl content (w/v). Detection and quantification were done by gas chromatography-mass spectrometry (GC/MS). Relative standard deviation (RSD) values for multiple analysis of soil samples fortified at 30 ?g/kg of each pesticide were below 19%. Limits of detection (LOD) for all the compounds studied were less than 2 ?g/kg.

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