scholarly journals Physicochemical Parameters of Real Wastewater Originating from a Plant Protection Products Factory and Modification of the QuEChERS Method for Determination of Captan

Molecules ◽  
2019 ◽  
Vol 24 (12) ◽  
pp. 2203 ◽  
Author(s):  
Ewa Szpyrka ◽  
Maciej Thomas ◽  
Magdalena Podbielska
Keyword(s):  
Matrix Effects ◽  
Solid Phase ◽  
Plant Protection ◽  
Oxygen Demand ◽  
Plant Protection Products ◽  
Electron Capture Detection ◽  
Quechers Method ◽  
Relative Standard ◽  
Real Wastewater

The aim of this study was the modification and application of the QuEChERS method for the preparation and purification of samples in order to determine the level of captan in real wastewater originating from a plant protection products factory which was characterized by a significant content of organic substances [Chemical Oxygen Demand (COD) = 856 ± 128 mg O2/L and Total Organic Carbon (TOC) = 62 ± 9 mg/L]. The optimization of the method consisted of the selection of solvents used for the extraction of captan from wastewater and also sorbents used to purify the extracts by the dispersion of a solid phase extraction technique (dSPE). Two steps were used: extraction and clean-up. In the extraction step, acetonitrile was replaced by anacetonitrile:acetone mixture. In the clean-up step by the dSPE, five sorbents were tested: Florisil®, aluminum oxide (Al2O3), zirconium oxide (ZrO2), silicon oxide (SiO2) and PSA (primary and secondary amine). Concentrations of captan in wastewater extracts were determined by gas chromatography (GC) combined with electron capture detection (μECD). The best recovery parameters and precision of the method were obtained for samples purified using ZrO2 (recovery 98% and precision expressed as relative standard deviation RSD 8%) and Florisil® (recovery 96%, RSD 9%). Limits of detection (LOD) and quantification (LOQ) for determination of captan in diluted extract of wastewater were 0.003 and 0.01 mg/L, respectively. Matrix effects were in the range of −69% to −44% for samples purified by ZrO2 and Florisil®, respectively. The modified and optimized method was applied for fast and simple determination of captan levels in real industrial wastewater samples, in which the concentration of captan in diluted extract was determined to be 4.0 ± 0.3 mg/L.

scholarly journals Determination of Residual Triflumezopyrim Insecticide in Agricultural Products through a Modified QuEChERS Method

Foods ◽  
2021 ◽  
Vol 10 (9) ◽  
pp. 2090
Author(s):  
Sung-Min Cho ◽  
Han-Sol Lee ◽  
Ji-Su Park ◽  
Su-Jung Lee ◽  
Hye-Sun Shin ◽  
...  
Keyword(s):  
Analytical Method ◽  
Matrix Effects ◽  
Solid Phase ◽  
Reference Method ◽  
Quechers Method ◽  
Modified Quechers ◽  
Relative Standard ◽  
The Matrix ◽  
Food Commodities

A rapid and simple analytical method for triflumezopyrim, a new class of mesoionic insecticides and commercialized molecules from DuPont, was developed with a modified QuEChERS method. The pH adjustment was used to improve the extraction efficiency of acetonitrile solvent, and dispersive solid-phase extraction was employed for the clean-up process. The five selected food commodities were used to verify the present optimized method, which displayed good linearity with an excellent correlation coefficient (R2 = 0.9992–0.9998) in the 0.003–0.30 mg/kg calibration range. The method limits of detection (LOD) and quantification (LOQ) were determined to be a value of 0.003 and 0.01 mg/kg, respectively. The mean recovery for the triflumezopyrim was in the 89.7–104.3% range. The relative standard deviations were ≤9.8% for intra- (n = 5) and inter-day (n = 15) precisions at concentrations of 0.01, 0.1, and 0.5 mg/kg in the five representative samples. The matrix effect has been calculated to confirm the effect during ionization of the analyte in the UPLC-MS/MS. The matrix effects of the instrumental analysis showed that triflumezopyrim was less susceptible to matrices. The proposed analytical method in this study has effectively improved the accuracy, selectivity, and sensitivity for the determination of triflumezopyrim in agricultural commodities; therefore, it can serve as a reference method for the establishment of maximum residue limits (MRLs).

scholarly journals Multiresidue Determination of Pesticides in Honey by Matrix Solid-Phase Dispersion and Gas Chromatography with Electron-Capture Detection

2001 ◽  
Vol 84 (4) ◽  
pp. 1165-1171 ◽  
Author(s):  
Beatriz Albero ◽  
Consuelo Sánchez-Brunete ◽  
José L Tadeo
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Solid Phase ◽  
Organophosphorus Compounds ◽  
Organophosphorus Pesticides ◽  
Electron Capture Detection ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard

Abstract A multiresidue method was developed for the determination of 15 pesticides (organochlorines, organophosphorus compounds, pyrethroids, and other acaricides) in various commercial honeys (eucalyptus, lavender, orange, rosemary, and multifloral). The analytical procedure is based on the matrix solid-phase dispersion of honey in a mixture of Florisil and anhydrous sodium sulfate; the mixture is placed in small plastic columns and extracted with hexane–ethyl acetate (90 + 10, v/v). The pesticide residues are determined by capillary gas chromatography with electron-capture detection. Recoveries with the method at concentrations between 0.15 and 1.5 μg/g ranged from 80 to 113%, and relative standard deviations were <10% for all the pesticides studied. The pesticide detection limits were within the range 0.5–5 mg/kg for organochlorines, around 3 μg/kg for the chlorinated organophosphorus pesticides studied, near 15 μg/kg for fluvalinate, and about 3 μg/kg for the other pyrethroids.

scholarly journals Evaluation of QuEChERS Method for GC Analysis of Pesticides in Tropical Fruits from Yucatan, Mexico

2018 ◽  
Vol 61 (4) ◽  
Author(s):  
Jocelyn María Coello-Villanueva ◽  
Pablo Oscar Martín Acereto-Escoffié ◽  
Jesús Alberto Barrón-Zambrano ◽  
David Muñoz-Rodríguez
Keyword(s):  
Standard Deviation ◽  
Solid Phase ◽  
Phase Extraction ◽  
Dispersive Solid Phase Extraction ◽  
Tropical Fruits ◽  
Quechers Method ◽  
Dragon Fruit ◽  
Relative Standard ◽  
External Standard

The pesticides intake causes health problems; therefore, food must not exceed the maximum allowable limits. The aim of this work was the evaluation of a multi-residue method for the determination of eleven pesticides in tropical fruits of Yucatan, Mexico. Pesticide extraction was carried out with acetonitrile and clean-up by dispersive solid phase extraction (QuEChERS method). The extracts were analyzed by GC/MS. The quantification was performed by the external standard matrix match calibration. Most of the quantification limits were below 10 ng×g<sup>-1</sup>. In 70% of the cases, the relative standard deviation was lower than 15%. The pesticide recoveries ranged from 67.74% to 138.57%. The method allowed the quantification of pesticides in papaya, melon, dragon fruit and sugar apple.

scholarly journals QuEChERS Method Followed by Solid Phase Extraction Method for Gas Chromatographic-Mass Spectrometric Determination of Polycyclic Aromatic Hydrocarbons in Fish

2015 ◽  
Vol 2015 ◽  
pp. 1-7 ◽  
Author(s):  
Mona Khorshid ◽  
Eglal R. Souaya ◽  
Ahmed H. Hamzawy ◽  
Moustapha N. Mohammed
Keyword(s):  
Polycyclic Aromatic Hydrocarbons ◽  
Solid Phase Extraction ◽  
Aromatic Hydrocarbons ◽  
Solid Phase ◽  
Phase Extraction ◽  
Quechers Method ◽  
Relative Standard ◽  
Fish Samples ◽  
Polycyclic Aromatic

A gas chromatography equipped with mass spectrometer (GCMS) method was developed and validated for determination of 16 polycyclic aromatic hydrocarbons (PAHs) in fish using modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for extraction and solid phase extraction for sample cleanup to remove most of the coextract combined with GCMS for determination of low concentration of selected group of PAHs in homogenized fish samples. PAHs were separated on a GCMS with HP-5ms Ultra Inert GC Column (30 m, 0.25 mm, and 0.25 µm). Mean recovery ranged from 56 to 115%. The extraction efficiency was consistent over the entire range where indeno(1,2,3-cd)pyrene and benzo(g,h,i)perylene showed recovery (65, 69%), respectively, at 2 µg/kg. No significant dispersion of results was observed for the other remaining PAHs and recovery did not differ substantially, and at the lowest and the highest concentrations mean recovery and RSD% showed that most of PAHs were between 70% and 120% with RSD less than 10%. The measurement uncertainty is expressed as expanded uncertainty and in terms of relative standard deviation (at 95% confidence level) is±12%. This method is suitable for laboratories engaged daily in routine analysis of a large number of samples.

scholarly journals Interlaboratory Study of a Multiresidue Gas Chromatographic Method for Determination of Organochlorine and Pyrethroid Pesticides and Polychlorobiphenyls in Milk, Fish, Eggs, and Beef Fat

2002 ◽  
Vol 85 (6) ◽  
pp. 1398-1409 ◽  
Author(s):  
François Bordet ◽  
Dary Inthavong ◽  
Jean-Marc Fremy ◽  
D Aspe ◽  
T Durand ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Solid Phase ◽  
Food Samples ◽  
Interlaboratory Study ◽  
Electron Capture Detection ◽  
Precision Data ◽  
Relative Standard ◽  
Pyrethroid Pesticides

Abstract An interlaboratory study was conducted to validate a gas chromatographic (GC) method for determination of 21 organochlorine pesticides, 6 pyrethroid pesticides, and 7 polychlorobiphenyl (PCB) congeners in milk, beef fat, fish, and eggs. The method was performed at low contamination levels, which represent relevant contents in food, and is an extension of the European standard (method NF-EN-1528, Parts 1–4). It enlarges the applicable scope of the reference EN method to pyrethroid pesticides and proposes the use of solid-phase extraction (SPE) as a cleanup procedure. Cryogenic extraction was made, and SPE cleanup was performed with 2 successive SPE cartridges: C18 and Florisil®. After injection of the purified extract onto a GC column, residues were measured by electron capture detection. Food samples (liquid milk, beef fat, mixed fish, and mixed eggs) were prepared, tested for homogeneity, and sent to 17 laboratories in France. Test portions were spiked with 27 pesticides and 7 PCBs at levels from 26 to 45, 4 to 27, 31 to 67, and 19 to 127 ng/g into milk, eggs, fish, and fat, respectively. Based on results for spiked samples, the relative standard deviation for repeatability ranged from 1.5 to 6.8% in milk, 3 to 39% in eggs, 4.5 to 12.2% in fish, and 7 to 13% in fat. The relative standard deviation for reproducibility ranged from 33 to 50% in milk, 29 to 59% in eggs, 31 to 57% in fish, and 30 to 62% in fat. This method showed acceptable intra- and interlaboratory precision data, as corroborated by HORRAT values at low levels of pesticide and PCB contamination. The statistical evaluation of the results was performed according to the International Organization for Standardization (ISO; ISO 3534 standard) and 5725-2 Guideline.

scholarly journals Determination of Eight Synthetic Pyrethroids in Bovine Fat by Gas Chromatography with Electron Capture Detection

2006 ◽  
Vol 89 (5) ◽  
pp. 1425-1431 ◽  
Author(s):  
Christine J Akre ◽  
James D MacNeil
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Solid Phase ◽  
Plant Protection ◽  
Electron Capture Detection ◽  
Synthetic Pyrethroids ◽  
Routine Monitoring ◽  
Chromatographic Peaks ◽  
Time Required

Abstract Synthetic pyrethroids are among the most widely used classes of insecticides, and their uses are varied, including plant protection, animal dips, and as a treatment for human clothing and bedding in very hot climates. Veterinary applications include ear tags, pour-on formulations, sprays, and dips. Persistent residues have been reported in livestock, and routine monitoring programs in other countries have found detectable residues of various pyrethroids in fat. A method has been developed using solid-phase extraction that reduces the quantities of solvents used, the time required, and the amount of glassware used compared to an earlier method on which it was based. The scope of analytes tested included the 5 compounds cited in the earlier method (flucythrinate, permethrin, cypermethrin, fenvalerate, and deltamethrin) and, in addition, cyfluthrin, λ-cyhalothrin, and fluvalinate. Sample extracts were analyzed by gas chromatography with electron capture detection using selected chromatographic peaks characteristic of each compound. Limits of quantification for the compounds were from 25-50 μg/kg, with a linear response for all compounds to 200 μg/kg. Recoveries ranged from 80 to 123%.

scholarly journals Determination of Decabromobiphenyl Ether in Water and Sediment Samples by Gas Chromatography with Electron Capture Detection

1997 ◽  
Vol 80 (1) ◽  
pp. 102-108 ◽  
Author(s):  
Hitoshi Yamamoto ◽  
Tameo Okumura ◽  
Yoshinori Nishikawa ◽  
Hiroe Konishi
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Sea Water ◽  
Solid Phase ◽  
Electron Capture Detection ◽  
Sediment Samples ◽  
Water And Sediment ◽  
Relative Standard ◽  
Water And Sediment Samples

Abstract Traces of decabromobiphenyl ether (DBBE) in water and sediment were determined by capillary gas chromatography with electron capture detection. Rapid sample preparation techniques such as disk-type C18 solid-phase extraction and cartridge- type Florisil extraction were used to clean up water and sediment samples, respectively. The detection limits of DBBE were 0.12 ng/mL and 9.7 ng/g in water and sediment, respectively. Average recoveries of DBBE added to river water, sea water, and sediment were 103%, with a relative standard deviation (RSD) of 8.6%; 87%, with an RSD of 10.7%; and 91%, with an RSD of 6.3%, respectively.

scholarly journals Simultaneous Determination of Residues of Chloramphenicol, Florfenicol, Florfenicol Amine, and Thiamphenicol in Shrimp Tissue by Gas Chromatography with Electron Capture Detection

2000 ◽  
Vol 83 (1) ◽  
pp. 26-30 ◽  
Author(s):  
Allen P Pfenning ◽  
José E Roybal ◽  
Heidi S Rupp ◽  
Sherri B Turnipseed ◽  
Steve A Gonzales ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
Electron Capture ◽  
Solid Phase ◽  
Internal Standard ◽  
Electron Capture Detection ◽  
Organic Layer ◽  
Standard Curve ◽  
Quantitation Limit ◽  
Relative Standard

Abstract A gas chromatographic (GC) method is presented for determining residues of chloramphenicol (CAP), florfenicol (FF), florfenicol amine (FFa), and thiamphenicol (TAP) in shrimp tissues, with meta-nitrochloramphenicol (mCAP) as the internal standard. The composited shrimp is extracted with basic ethyl acetate, followed by an acetonitrile–basic ethyl acetate mixture. This extract is centrifuged, filtered, evaporated, and reconstituted in water; the reconstituted extract is acidified, defatted with hexane, and passed through a propylsulfonic acid (PRS) and C18 solid-phase extraction (SPE) system. The C18 SPE column is eluted with methanol, and the PRS SPE column is eluted with basic MeOH plus counter ion. The combined eluates are evaporated, reconstituted in acetonitrile, and derivatized with Sylon BFT. After derivatization, the addition of toluene directly to the sample, followed by the addition of basic water, quenches the derivatization process. After centrifugation, the organic layer is carefully removed, and the analytes are determined by GC with electron capture detection. Shrimp tissues were fortified with fenicols (i.e., CAP, FF, FFa, and TAP) at 5, 10, 20, 40, and 80 ng/mL. Overall recoveries were 88, 101, 91, and 84% with overall interassay (between-day) variabilities (i.e., relative standard deviations) of 5.3, 9.4, 12.8, and 7.4% for CAP, FF, FFa, and TAP, respectively. The method detection limits were calculated as 0.7, 1.4, 2.4, and 1.3 ng/g (ppb) for CAP, FF, FFa, and TAP, respectively, based on a 10 g sample. The quantitation limit as determined empirically by this method is the lower limit of the standard curve, which is about 5 ng/g (ppb) for each analyte.

scholarly journals Determination of pesticides residues in quinoa (Chenopodium quinoa Willd) using QuEChERS and LC-MS/MS

2018 ◽  
pp. 421
Author(s):  
Franz Zirena Vilca ◽  
Graziela Cristina Rossi Moura Andrade ◽  
Walter Alejandro. Zamalloa Cuba ◽  
Valdemar Luiz. Tornisielo
Keyword(s):  
Acetic Acid ◽  
Mobile Phase ◽  
Matrix Effects ◽  
Solid Phase ◽  
Chenopodium Quinoa ◽  
Phase Extraction ◽  
Dispersive Solid Phase Extraction ◽  
Quechers Method ◽  
Pesticides Residues

The QuEChERS method was optimized and validated for the determination of 40 pesticides in 37 samples of quinoa from the harvest 2010-2011 in Puno - Peru. The method involves extraction with 1% acetic acid acetonitrile with CH3COONa anhydrous and MgSO4 followed by dispersive solid-phase extraction with PSA and C18. Analyses were performed with LC-MS/MS using C18 column 150 mm x 2.1 x 3.5 µm, water and acetonitrile 0.1% formic acid used as mobile phase. Spiked quinoa blank at 0.01 and 0.1 mg kg-1 was employed to evaluate recovery ranging from the 31.6 and 125.1% with RSD ≤ 23. The method showed linearity r2 ≥ 0.99 and limits of quantification ranged from 0.001 and 0.01 mg kg-1, and was not observed a matrix effects.  No pesticides residues were observed in the analyzed samples.

Residue Analysis of Organophosphorus and Organochlorine Pesticides in Fatty Matrices by Gas Chromatography Coupled with Electron-Capture Detection

2006 ◽  
Vol 61 (5-6) ◽  
pp. 341-346 ◽  
Author(s):  
Jae-Woo Park ◽  
A. M. Abd El-Aty ◽  
Myoung-Heon Lee ◽  
Sung-Ok Song ◽  
Jae-Han Shim
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Simple Procedure ◽  
Linear Regression Analysis ◽  
Residue Analysis ◽  
Electron Capture Detection ◽  
Relative Standard ◽  
Wide Range ◽  
Repeatability And Reproducibility

A multiresidue method for the simultaneous determination of 22 organochlorine (OCs) and organophosphorus (Ops) pesticides (including isomers and metabolites), representing a wide range of physicochemical properties, was developed in fatty matrices extracted from meat. Pesticides were extracted from samples with acetonitrile/n-hexane (v :v, 1:1). The analytical screening was performed by gas chromatography coupled with electron-capture detection (ECD). The identification of compounds was based on their retention time and on comparison of the primary and secondary ions. The optimized method was validated by determining accuracy (recovery percentages), precision (repeatability and reproducibility), and sensitivity (detection and quantitation limits) from analyses of samples fortified at 38 to 300 ng/g levels. Correlation coefficients for the 22 extracted pesticide standard curves (linear regression analysis, n = 3) ranged from 0.998 to 1.000. Recovery studies from 2 g samples fortified at 3 levels demonstrated that the GC-ECD method provides 64.4-96.0% recovery for all pesticides except 2,4′-DDE (44.6-50.4%), 4,4′-DDE (51.1-57.5%) and 2,4′-DDT (50.0-51.2%). Both repeatability and reproducibility relative standard deviation values were < 20% for all residues. Detection limits ranged from 0.31 to 1.27 ng/g and quantification limits were between 1.04 and 4.25 ng/g. The proposed analytical method may be used as a simple procedure in routine determinations of OCs and Ops in meat. It can also be applied to the determination of pesticide multi-residues in other animal products such as butter and milk.

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