Matrix effects in the determination of acaricides and fungicides in must by gas chromatography with electron-capture and nitrogen-phosphorus detection

1997 ◽  
Vol 778 (1-2) ◽  
pp. 111-117 ◽  
Author(s):  
J.L. Bernal ◽  
M.J. del Nozal ◽  
J.J. Jime´nez ◽  
J.M. Rivera
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Matrix Effects ◽  
Nitrogen Phosphorus

scholarly journals Determination of Malathion, Coumaphos, and Fluvalinate Residues in Honey by Gas Chromatography with Nitrogen–Phosphorus or Electron Capture Detectors

2000 ◽  
Vol 83 (1) ◽  
pp. 178-182 ◽  
Author(s):  
Urania Menkissoglu-Spiroudi ◽  
Grigorios C Diamantidis ◽  
Vassiliki E Georgiou ◽  
Andreas T Thrasyvoulou
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
High Selectivity ◽  
Order Model ◽  
First Order ◽  
Quantitation Limit ◽  
Coefficients Of Variation ◽  
Electron Capture Detectors ◽  
Nitrogen Phosphorus

Abstract A rapid, reliable, and inexpensive extraction method was developed to determine acaricide residues in honey by gas chromatography (GC) with nitrogen–phosphorus (NP) or electron capture (EC) detectors. Because of the high selectivity of the NP detector, no interfering peaks were present and no cleanup was necessary. A simple cleanup step is proposed for the GC–ECD analysis. Recoveries from spiked honey samples ranged from 79 to 94.4%, with coefficients of variation of 0.3–18.5%. The quantitation limit obtained was 0.015 mg/kg for malathion, 0.020 mg/kg for coumaphos, and 0.005 mg/kg for fluvalinate. The method was used to determine the disappearance of malathion and coumaphos residues from honey samples collected from beehives treated with these acaricides. The disappearance of both acaricides was rapid and followed a first-order model for the duration of the experiment.

Capillary Column Gas Chromatography with Nitrogen-Phosphorus Detection for Determination of Nitrogen- and Phosphorus-Containing Pesticides in Finished Drinking Waters: Collaborative Study

1991 ◽  
Vol 74 (2) ◽  
pp. 295-309
Author(s):  
Kenneth W Edgell ◽  
Elizabeth L Jenkins ◽  
Viorica Lopez-Avila ◽  
James E Longbottom
Keyword(s):  
Gas Chromatography ◽  
Drinking Water ◽  
Matrix Effects ◽  
Collaborative Study ◽  
Nitrogen And Phosphorus ◽  
Drinking Waters ◽  
Phosphorus Containing ◽  
Nitrogen Phosphorus Detector ◽  
Nitrogen Phosphorus

Abstract A joint U.S. Environmental Protection Agency/AOAC interlaboratory method validation study was conducted on EPA Method 507, Determination of Nitrogen- and Phosphorus- Containing Pesticides In Finished Drinking Water by Gas Chromatography with a Nitrogen-Phosphorus Detector, to determine the mean recovery and precision for analyses of 45 nitrogen- or phosphorus-containing pesticides in reagent water and finished drinking waters. The study design was based on Youden's nonreplicate plan for collaborative tests of analytical methods. The waters were spiked with 45 nitrogen- or phosphorus-containing pesticides at 6 concentration levels, prepared as 3 Youden pairs. Ten volunteer laboratories extracted the spiked test waters with methylene chloride, performed a solvent exchange with methyl ferf-butyl ether, and analyzed an aliquot of each extract by gas chromatography using a nitrogen-phosphorus detector. Results were analyzed using an EPA computer program, which measured recovery and precision for each of the 45 pesticides and compared the performance of the method between water types. Method 507 was judged acceptable for all analytes tested except merphos, which thermally decomposed in the Injection port of the gas chromatograph. Five compounds (carboxin, disulfoton, metolachlor, pronamlde, and slmazlne) exhibited statistically significant matrix effects for the finished drinking water. The method has been adopted official first action by AOAC.

scholarly journals Determination of Organochlorine, Organophosphorus, and Triazine Pesticide Residues in Wine by Gas Chromatography with Electron Capture and Nitrogen–Phosphorus Detection

1996 ◽  
Vol 79 (6) ◽  
pp. 1423-1427 ◽  
Author(s):  
Rosario Garcia-Repetto ◽  
Isabel Garrtoo ◽  
Manuel Repetto
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Pesticide Residues ◽  
Solid Phase ◽  
Electron Capture Detection ◽  
Gel Chromatography ◽  
Phase Extraction ◽  
Silica Gel Chromatography ◽  
Nitrogen Phosphorus

Abstract A multiresidue analytical method is described for determining 6 pesticides in wine: chlorpyrifos, dimethoate, quinalphos, simazine, tetradifon, and endosulfan. Wine (200 mL) is extracted with dichloromethane (50 mL, 3 times), and the evaporated extracts are purified by silica gel chromatography. Pesticide residues are eluted with n-hexane, n-hexane-benzene (1 + 1), benzene, benzene–acetone (1 + 1), and acetone. Residues are determined by gas chromatography with nitrogen–phosphorus and electron capture detection, using CPSH-5CB, Carbo wax-20M, and CPSH-19CB columns. Recoveries of pesticides added at 0.025 μg/L were 83–97%, with standard deviations of 0.01–0.05%. Detection limits were 0.13–8.9 ng/L, except for simazine (36.7 μg/L). Results are compared with those obtained with a solid-phase extraction (C18) purification and with different eluant series.

scholarly journals Broad-Spectrum Determination of Pesticides in Groundwater by Gas Chromatography with Electron Capture Detection, Nitrogen–Phosphorus Detection, and Tandem Mass Spectrometry

2001 ◽  
Vol 84 (6) ◽  
pp. 1751-1762 ◽  
Author(s):  
Antonia Garrido Frenich ◽  
Maria Del Carmen Pablos Espada ◽  
Jose Luis Martínez Vidal ◽  
Luis Molina
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Tandem Mass Spectrometry ◽  
Electron Capture ◽  
Electron Capture Detection ◽  
Tandem Mass ◽  
Relative Standard ◽  
Nitrogen Phosphorus ◽  
Pesticides In Groundwater

Abstract Gas chromatography with electron capture detector (ECD), nitrogen–phosphorus detector (NPD), and tandem mass spectrometry (MS/MS) was used to identify 36 pesticides, widely used to control various pest and diseases in vegetables, in water after a preconcentration step on C18 cartridges. The recoveries obtained ranged from 70 to 135% at a fortification level of 100 ng/L with relative standard deviations of <36.2%. The limits of detection and quantitation were ≤48 and ≤160 ng/L, respectively. Important advantages of MS/MS over ECD and NPD in the determination of pesticides are also presented. The proposed analytical methodology was applied to the determination of pesticides in groundwater samples from an agricultural area, the Campo de Dalías (Almería, Spain). The most frequently encountered pesticides were endosulfan sulfate and metalaxyl, whereas the pesticide found at the highest concentration was fenamiphos.

Gas Chromatographic-Electron Capture Detection Method for Determination of 29 Organochlorine Pesticides in Finished Drinking Water: Collaborative Study

1990 ◽  
Vol 73 (2) ◽  
pp. 276-286
Author(s):  
Viorica Lopez-Avila ◽  
Raymond Wesselman ◽  
Kenneth Edgell
Keyword(s):  
Gas Chromatography ◽  
Drinking Water ◽  
Method Validation ◽  
Electron Capture ◽  
Validation Study ◽  
Matrix Effects ◽  
Collaborative Study ◽  
Electron Capture Detection ◽  
Chlorinated Pesticides

Abstract A joint U.S. Environmental Protection Agency/AOAC interlaboratory method validation study was conducted on EPA Method 508, Determination of Chlorinated Pesticides in Water by Gas Chromatography with an Electron Capture Detector, to determine the mean recovery and precision for analyses of 29 pesticides in reagent water and finished drinking water. The study design was based on Youden's nonreplicate plan for collaborative tests of analytical methods. The waters were spiked with 29 pesticides at 6 concentration levels, as 3 Youden pairs. Eleven volunteer laboratories extracted the spiked test waters with methylene chloride, performed a solvent exchange with methyl ferf-butyl ether, and analyzed an aliquot of each extract by gas chromatography with electron capture detection. Results were analyzed using an EPA computer program, Interlaboratory Method Validation Study (IMVS), which measured recovery and precision for each of the 29 pesticides and compared the performance of the method between water types. Method 508 was judged acceptable for all analytes tested. Only 3 analytes (α-chlordane, 4,4′-DDE, and methoxychlor) exhibited practical significant matrix effects. The method has been adopted official first action.

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