scholarly journals Multiresidue analysis of pesticides in soil by liquid-solid extraction procedure

2012 ◽  
Vol 27 (3) ◽  
pp. 239-244 ◽  
Author(s):  
Rada Djurovic ◽  
Tijana Djordjevic ◽  
Ljiljana Radivojevic ◽  
Ljiljana Santric ◽  
Jelena Gajic-Umiljendic
Keyword(s):  
Extraction Procedure ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Multiresidue Analysis ◽  
Florisil Column ◽  
Solid Extraction ◽  
Relative Standard ◽  
Multiple Analysis ◽  
Detection And Quantification

A multiresidue method for simultaneous determination of four pesticides (diazinon, acetochlor, aldrine and carbofuran) belonging to different pesticide groups, extracted from soil samples, is described. The method presented is based on liquid-solid extraction (LSE) and determination of pesticides, i.e. the pesticides were extracted by methanol- acetone mixture, purified on florisil column and eluted by ethyl acetate-acetone mixture. Optimization of the main parameters affecting the LSE procedure, such as the choice of purification sorbent, as well as the elution solvent and its volume, were investigated in details and optimized. Also, validation of the proposed method was done. Gas chromatography-mass spectrometry (GC-MS) was used for detection and quantification of the pesticides studied. Relative standard deviation (RSD) and recovery values for multiple analysis of soil samples fortified with 30 ?g/kg of each pesticide were below 8% and higher than 89%, respectively. Limits of detection (LOD) for all the compounds studied were less than 4 ?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.

scholarly journals Effects of organic matter and clay content in soil on pesticide adsorption processes

2009 ◽  
Vol 24 (1) ◽  
pp. 51-57 ◽  
Author(s):  
Rada Djurovic ◽  
Jelena Gajic-Umiljendic ◽  
Tijana Djordjevic
Keyword(s):  
Organic Matter ◽  
Extraction Procedure ◽  
Chemical Properties ◽  
Clay Content ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Adsorption Processes ◽  
Pesticide Adsorption

The effect of organic matter and clay content on the adsorption of atrazine, acetochlor, clomazone, pendimethalin and oxyfluorfen in soil samples was studied. In order to determine whether and to what degree different soil properties affect the process of determination of selected pesticides, three soils with different clay and organic matter contents were used. An optimized liquid-solid extraction procedure followed by SPME measurement was applied to analyze the selected pesticides in soil samples. Detection and quantification were done by gas chromatography-mass spectrometry (GC/MS). Relative standard deviation (RSD) values for multiple analyses of soil samples fortified at 30 ?g/kg of each pesticide were below 19%. Limits of detection (LODs) for all compounds studied were less than 2 ?g/kg. The results indicate that soils with different physic-chemical properties have different effects on the adsorption of most pesticides, especially at higher concentration levels.

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.

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.

scholarly journals Rapid Determination of Ethylene Oxide and 75 VOCs in Ambient Air with Canister Sampling and Associated Growth Issues

Separations ◽  
2021 ◽  
Vol 8 (3) ◽  
pp. 35
Author(s):  
Jason Hoisington ◽  
Jason S. Herrington
Keyword(s):  
Ethylene Oxide ◽  
Rapid Determination ◽  
Complex Mixture ◽  
Ambient Air ◽  
Gas Chromatography Mass Spectrometry ◽  
Average Accuracy ◽  
Relative Standard ◽  
Wide Range ◽  
Us Epa

A canister-based sampling method along with preconcentrator-Gas chromatography-Mass Spectrometry (GC-MS) analysis was applied to ethylene oxide (EtO or EO) and 75 other volatile organic compounds (VOCs) in ambient air. Ambient air can contain a large variety of VOCs, and thorough analysis requires non-discriminatory sampling and a chromatographic method capable of resolving a complex mixture. Canister collection of whole air samples allows for the collection of a wide range of volatile compounds, while the simultaneous analysis of ethylene oxide and other VOCs allows for faster throughput than separate methods. The method presented is based on US EPA Method TO-15A and allows for the detection of EtO from 18 to 2500 pptv. The method has an average accuracy of 104% and precision of 13% relative standard deviation (RSD), with an instrument run time of 32 min. In addition, a link between canister cleanliness and ethylene oxide growth is observed, and potential mechanisms and cleaning strategies are addressed.

scholarly journals Optimization of a microwave-assisted extraction procedure for the determination of selected alkyl, aryl, and halogenated phenols in sewage sludge and biosolids

2016 ◽  
Vol 51 (4) ◽  
pp. 344-356 ◽  
Author(s):  
Hing-Biu Lee ◽  
M. Lewina Svoboda ◽  
Thomas E. Peart ◽  
Shirley Anne Smyth
Keyword(s):  
Sewage Sludge ◽  
Extraction Procedure ◽  
Negative Ion ◽  
Gas Chromatography Mass Spectrometry ◽  
Microwave Assisted Extraction ◽  
Alkyl Aryl ◽  
Microwave Assisted ◽  
Assisted Extraction ◽  
Halogenated Phenols

A microwave-assisted extraction method for the determination of 15 alkyl, aryl, and halogenated phenols in sewage sludge and biosolids samples was developed and optimized. The effects of solvent, temperature, time, moisture content, acid, and number of extractions on the recovery of phenols were evaluated. Results indicated that extraction solvent had the greatest impact on the recovery of all phenols while pH had the largest effect on recovery of hexachlorophene and pentachlorophenol. Wet sludge samples were extracted with acetone-hexane mixture in the presence of glacial acetic acid. The extract was evaporated, acetylated by acetic anhydride and cleaned up by silica gel. For dry sludge samples, an optional procedure for the simultaneous extraction and acetylation of phenols was also proposed. Triclosan (TCS) and the alkyl and aryl phenols in sludge extracts were analyzed by gas chromatography-mass spectrometry (GC-MS) in electron-impact mode while polyhalogenated phenols were analyzed by GC-MS in negative ion chemical ionization mode. Method detection limits were ca. 200 ng/g for nonylphenol, <25 ng/g for TCS and other alkyl and aryl phenols, and <5 ng/g for other halogenated phenols. This method has been applied to the determination of phenolic compounds in over 150 sludge and biosolids samples since 2009.

scholarly journals Determination of Chlorinated Phenols in Water and Soil by Capillary Zone Electrophoresis

1997 ◽  
Vol 80 (6) ◽  
pp. 1308-1314 ◽  
Author(s):  
Wayne E Rae ◽  
Charles A Lucy
Keyword(s):  
Capillary Zone Electrophoresis ◽  
Fused Silica ◽  
Soil Samples ◽  
Chlorinated Phenols ◽  
Relative Standard ◽  
Zone Electrophoresis ◽  
Water And Soil Samples ◽  
Fused Silica Capillary ◽  
Capillary Zone

Abstract A capillary zone electrophoresis (CZE) method was developed to separate and determine chlorinated phenols in water and soil samples. A mixture of 16 chlorinated phenols was resolved in 25 min by using a 77 cm (70 cm to detector) × 75 μm fused silica capillary with 0.015M tetraborate/0.045M phosphate (pH 7.3) buffer at 22 kV. Calibration linearities for water samples in the low parts-permillion range were good (correlation coefficient > 0.99) for all solutes except p-chlorophenol. Average precision was 17% relative standard deviation. Typical detection limits were in the 200 μg/L range. Recoveries of chlorinated phenols from synthetic soil samples with methanol were quantitative.

scholarly journals Gas Chromatographic Determination of Chlorothalonil in Leaves and Roots of Scrophularia and in Soil

1996 ◽  
Vol 79 (2) ◽  
pp. 587-588 ◽  
Author(s):  
Lan Zhao ◽  
De-Fang Fan
Keyword(s):  
Electron Capture ◽  
Chromatographic Method ◽  
Detection Limits ◽  
Chromatographic Determination ◽  
Soil Samples ◽  
Florisil Column ◽  
Glass Column ◽  
Leaves And Roots ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method is described for determination of chlorothalonil residues in leaves and roots of Scrophularia and in soil. Samples were extracted with acetone and cleaned up on a Florisil column. Chlorothalonil residues are chromatographed directly on a glass column of 1.5% OV-17 and 2% QF-1 coated on 80-100 mesh Chromosorb W (HP) support and measured with a 63Ni electron capture detector. Detection limits are 0.001 ppm for leaf, 0.005 ppm for root, and 0.001 ppm for soil.

scholarly journals Monitoring the Levels of Biogenic Amines in Canned Fish Products Marketed in Ghana

2020 ◽  
Vol 2020 ◽  
pp. 1-6 ◽  
Author(s):  
Alexander Weremfo ◽  
Meinster Kodjo Eduafo ◽  
Hakim Agyei Gyimah ◽  
Samuel Abassah-Oppong
Keyword(s):  
Biogenic Amines ◽  
Hplc Method ◽  
Ion Pair ◽  
Human Consumption ◽  
Fish Products ◽  
Canned Fish ◽  
Relative Standard ◽  
Excellent Selectivity ◽  
Detection And Quantification

An ion-pair HPLC method with postcolumn o-phthalaldehyde (OPA) derivatization and fluorescence detection was validated for quantitative determination of five biogenic amines (histamine, tyramine, cadaverine, putrescine, and agmatine) in canned fish products (mackerel, sardine, and tuna) marketed in Ghana. The validated method exhibited excellent selectivity and good linearity (R2 > 0.9990) for all the amines. The limits of detection and quantification for studied biogenic amines were in the range of 0.32–0.78 mg·kg−1 and 1.10–2.57 mg·kg−1, respectively. Also, a satisfactory recovery was obtained for all the amines (82.1–101.4%), and the relative standard deviations were lower than 9.3% under repeatability conditions for the studied amines. Subsequently, the method was applied to the analysis of biogenic amines in canned fish products to estimate the safety of Ghanaian consumers. The maximum levels of histamine, tyramine, cadaverine, putrescine, and agmatine detected in the analysed canned fish products were 64.05 mg·kg−1, 27.44 mg·kg−1, 27.23 mg·kg−1, 18.74 mg·kg−1, and 52.72 mg·kg−1, respectively. Thus, the levels of biogenic amines detected in the canned fish products were lower than the acceptable levels and, therefore, can be considered relatively safe for human consumption.

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