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.

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 Determination of Se4+ in Drinkable Water by Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry

2000 ◽  
Vol 83 (5) ◽  
pp. 1082-1086 ◽  
Author(s):  
Maurizio Guidotti
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Tap Water ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Drinkable Water

Abstract A method was developed for the selective determination of Se4+ in drinkable water by solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS). Se4+ was selectively derivatized to ethane, 1,1′-selenobis by reaction with sodium tetraethylborate, extracted by the SPME fiber, and determined by GC/MS. Both headspace (HS)–SPME and direct SPME were studied. The method requires only a few milliliters of sample and 20 min for completion. At 2.0 μg/L concentration, the relative standard deviation was 10.1% for HS–SPME and 9.1% for direct SPME. For HS–SPME, the theoretical detection limit was 81 ng/L and 166 ng/L for direct SPME. The recovery rate was 95%. The method was used to determine Se4+ in 10 tap water samples.

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.

Optimization of HS-SPME for GC-MS Analysis of Volatiles Compounds in Roasted Sesame Oil

2014 ◽  
Vol 881-883 ◽  
pp. 61-64
Author(s):  
Zhao Xi Fang ◽  
Guo Qin Liu ◽  
Xue De Wang ◽  
Li Juan Han ◽  
Bing Ge Liu
Keyword(s):  
Solid Phase Microextraction ◽  
Capillary Column ◽  
Solid Phase ◽  
Sesame Oil ◽  
Operating Conditions ◽  
Extraction Time ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Volatiles Compounds

This paper was to develop a simple and rapid headspace solid-phase microextraction (HS-SPME) method coupled with gas chromatography–mass spectrometry (GC-MS) for the determination of volatiles compounds from the roasted sesame oil (RSO). A HP-5MS capillary column (30 m × 0.25 mm I.D. × 0.25 mm film thick) was used for GC-MS, and a 50/30 μm divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was used to extract volatiles compounds. The condition was optimized by varying the sample-to-headspace ratio (0.5-2.5 g/15 ml), extraction time (10-50 min) and Splitless time (0.5-4 min). The results showed that the optimal operating conditions occurred at (extraction temperature:40°C, sample-to-headspace ratio: 1.5 g/15 ml, extraction time: 40 min, Splitless time: 1 min) for the analyze method.

scholarly journals Determination of Bisphenol Ain Water by Isotope Dilution Headspace Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry Without Derivatization

2008 ◽  
Vol 91 (3) ◽  
pp. 622-629 ◽  
Author(s):  
Xu-Liang Cao ◽  
Jeannette Corriveau
Keyword(s):  
Detection Limit ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Method Detection Limit ◽  
Spme Fiber ◽  
Relative Standard ◽  
Headspace Spme ◽  
Epoxy Resin Adhesive

Abstract The original solid-phase microextraction (SPME) fibers use an epoxy resin adhesive that releases bisphenol A (BPA) during thermal desorption of the fiber. This adversely affects the method detection limit and accuracy when these products are used for the determination of BPA. In this work, 5 new metal alloy SPME fibers that do not use epoxy resins were compared for the extraction of BPA in water. The performance of the optimum SPME fiber with 60 m carbowax-polyethylene glycol coating for the headspace SPME of BPA in water was investigated systematically under different extraction conditions. Salt was found to increase the partitioning of BPA from water into the headspace until saturation was reached. Partitioning of BPA from water into the headspace also increased at higher extraction temperatures, as did longer extraction times. However, extraction of BPA from water onto the SPME fiber was not improved for solutions adjusted to pH 2 compared to the unadjusted neutral solutions. The new BPA method showed good linearity over the concentration range of 2.5 to 40 g/L [correlation coefficient (r2) = 0.995] .The method detection limit for BPA was 0.5 g/L, while the instrument detection limit was as low as 0.05 g/L. Good repeatability was observed for BPA at levels of 5 and 20 g/L with relative standard deviation values <10. The automated headspace SPME method developed in this work was used to investigate migration of BPA from polycarbonate bottles into water, and levels of BPA in water ranged from 1.7 to 4.1 g/L.

Analysis of Organochlorine Pesticides in Soil Using Optimized FMAE-GC/MS

2012 ◽  
Vol 518-523 ◽  
pp. 2348-2351
Author(s):  
Shan Shan He ◽  
Yu Jun Wang ◽  
Ling Cao ◽  
Yan Xin Wang ◽  
Chuang Ju Dong
Keyword(s):  
Organochlorine Pesticides ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Microwave Assisted Extraction ◽  
Good Recovery ◽  
Extraction Solvent ◽  
Microwave Assisted ◽  
Assisted Extraction ◽  
Relative Standard

A focused microwave-assisted extraction (FMAE) was optimized and coupled to gas chromatography–mass spectrometry for the determination of organochlorine pesticides in soil samples. According to the result, the combination of 20 min extraction time at 48 °C and a mixture of 1+1 of n-hexane-acetone as extraction solvent is the best conditions. The recovery values is 72.8%～96.4% in the above conditions. The relative standard deviation was 4.39%~13.18%. We have good recovery values when spiked 20ng, 40ng and 60ng standard into 5.00g soil sample.

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