Determination of 49 Organophosphorus Pesticide Residues and Their Metabolites in Fish, Egg, and Milk by Dual Gas Chromatography–Dual Pulse Flame Photometric Detection with Gel Permeation Chromatography Cleanup

2012 ◽  
Vol 60 (8) ◽  
pp. 1906-1913 ◽  
Author(s):  
Lixin Yang ◽  
Heli Li ◽  
Fangang Zeng ◽  
Yinping Liu ◽  
Ruifeng Li ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Pesticide Residues ◽  
Organophosphorus Pesticide ◽  
Gel Permeation Chromatography ◽  
Photometric Detection ◽  
Gel Permeation ◽  
Flame Photometric Detection

scholarly journals Determination of Nitrogen- and Phosphorus-Containing Pesticide Residues in Vegetables by Gas Chromatography with Nitrogen–Phosphorus and Flame Photometric Detection after Gel Permeation Chromatography and a Two-Step Minicolumn Cleanup

2003 ◽  
Vol 86 (6) ◽  
pp. 1241-1251 ◽  
Author(s):  
Eiji Ueno ◽  
Harumi Oshima ◽  
Isao Saito ◽  
Hiroshi Matsumoto
Keyword(s):  
Gas Chromatography ◽  
Pesticide Residues ◽  
Gel Permeation Chromatography ◽  
Good Resolution ◽  
Photometric Detection ◽  
Relative Standard ◽  
Phosphorus Containing ◽  
Gel Permeation ◽  
Flame Photometric Detection ◽  
Nitrogen Phosphorus

Abstract An efficient and reliable multiresidue method for determining pesticide residues in a large number of vegetable samples was studied. First, the important target compounds for monitoring, 52 nitrogen-and/or phosphorus-containing pesticides, were selected. The sample was extracted with acetonitrile, and the separated acetonitrile layer was cleaned up by a salting-out step. The acetonitrile extract was purified by gel permeation chromatography that divided the pesticide eluate into 2 fractions; the pesticide fractions were respectively purified by a 2-step minicolumn cleanup in which the second pesticide fraction was loaded on a silica-gel minicolumn. After a Florisil minicolumn was inserted on the silicagel minicolumn, the first pesticide fraction was loaded on the tandem minicolumn, which was eluted with acetone–petroleum ether (3 + 7). The combined eluate was subjected to dual-column gas chromatography (GC) with nitrogen–phosphorus and flame photometric detection. By application of the optimum cleanup conditions to the 52 pesticides selected, good resolution and low breakdown levels of the pesticides during GC were maintained. Recoveries of the 52 pesticides from fortified cabbage, lettuce, spring onion, and spinach ranged from 72 to 108% with relative standard deviations of 2–17%, except for the recoveries of methamidophos and chlorothalonil. The detection limits of the pesticides were satisfactory (0.001–0.009 mg/kg) for monitoring pesticide residues in vegetables.

scholarly journals Determination of Organotins in Aquatic Food by Gas Chromatography with Pulsed Flame Photometric Detection

2008 ◽  
Vol 91 (3) ◽  
pp. 653-659 ◽  
Author(s):  
Zhao Yun-Feng ◽  
Zhao Kong-Xiang ◽  
Wu Yong-Ning
Keyword(s):  
Gas Chromatography ◽  
Standard Deviation ◽  
Gel Permeation Chromatography ◽  
Photometric Detection ◽  
Relative Standard ◽  
Gel Permeation ◽  
Flame Photometric Detection ◽  
Aquatic Food ◽  
Derivative Products

Abstract A method based on gas chromatography (GC)-pulsed flame photometric detection (PFPD) was developed to determine the levels of organotins in aquatic food. After being purified by gel-permeation chromatography in ethyl actatetetrahydrofuran, the organotin compounds were derivatized by pentylmagnesium bromide. The derivative products were injected into the GC system and detected by PFPD (sulfur mode). The method was validated by analysis of the certified reference material and spiked samples. Recoveries of organotins ranged from 84.1 to 116.6 with relative standard deviation between 1.3 and 16.0 when spiked at levels of 2, 10, and 40 g/kg. The limits of detection varied from 0.1 to 1.2 g/kg for shellfish and 0.1 to 0.5 g/kg for fish. The proposed method was suitable for determining organotins in aquatic foods.

scholarly journals Determination of Organophosphorus Pesticide Residues in Milk

2013 ◽  
Vol 57 (2) ◽  
pp. 185-189 ◽  
Author(s):  
Tomasz Kiljanek ◽  
Alicja Niewiadowska ◽  
Stanisław Semeniuk
Keyword(s):  
Pesticide Residues ◽  
Solid Phase ◽  
Organophosphorus Pesticides ◽  
Organophosphorus Pesticide ◽  
Gel Permeation Chromatography ◽  
Proficiency Tests ◽  
The European Union ◽  
Photometric Detection ◽  
Milk Samples

Abstract A method for simultaneous determination of 13 organophosphorus pesticide residues in milk samples has been developed and validated. The method is based on the extraction of the sample with acetone and petroleum ether, cleanup by gel permeation chromatography, and solid phase extraction, and determination by gas chromatography with flame photometric detection. The recovery, investigated by analysing blank milk samples spiked with azinphos, chlorfenvinphos, chlorpyrifos, chlorpyrifos-methyl, diazinon, fenitrothion, methacrifos, methidathion, parathion-methyl, pyrazophos, and triazophos at concentrations of 10, 20, and 30 μg/kg, and with parathion and pirimiphos-methyl at concentrations of 25, 50, and 75 μg/kg, ranged from 73.1% to 106.2%. Performance characteristics, such as repeatability and within-laboratory reproducibility expressed as coefficient of variation were less than 20%. Measurement uncertainty was lower than 22% for all validated organophosphorus pesticides. The limits of quantification were 10 μg/kg for all compounds and allowed determination of residues at, or even below, the maximum residue limits set by the European Union. The satisfactory z-score results of international proficiency tests confirm good accuracy, reproducibility, and reliability of the developed method.

Determination of Tri-w-Butyltin and Di-/i-Butyltin Compounds in Fish by Gas Chromatography with Flame Photometric Detection

1988 ◽  
Vol 71 (2) ◽  
pp. 360-363 ◽  
Author(s):  
Kumiko Sasaki ◽  
Takashi Ishizaka ◽  
Takashi Suzuki ◽  
Yukio Saito
Keyword(s):  
Gas Chromatography ◽  
Gel Permeation Chromatography ◽  
Mass Spectrometry Analysis ◽  
Spectrometry Analysis ◽  
Photometric Detection ◽  
Flame Photometric Detection ◽  
Methyl Derivatives ◽  
Butyltin Compounds ◽  
Good Agreement

Abstract An analytical method is described for the simultaneous quantitative determination of tri-n-butyltin and di-n-butyltin compounds in fish. The sample was extracted with 0.5N HCl-methanol, and the methanol solution was extracted with hexane. The extract was purified by gel permeation chromatography and treated with Grignard reagent to yield the methyl derivatives, which were determined by gas chromatography with flame photometric detection operated in the tin mode (610 nm). Recoveries of tri-n-butyltin chloride (Bu3SnCl) and di-n-butyltin dichloride (Bu2SnCl2) spiked to fish at the levels of 0.2 and 1.0 ppm ranged from 80 to 105%. Detection limits were 0.02 μg/g for both compounds. Tri-n-butyltin compounds equivalent to Bu3SnCl levels of 0.07-2.0 ppm and di-n-butyltin compounds equivalent to Bu2SnCl2 levels of 0.02-0.11 ppm were found in reared yellowtails, and these values showed good agreement with the results from gas chromatographic-mass spectrometry analysis.

scholarly journals Development of Methods for Determination of the Residues of 15 Pesticides in Medicinal Herbs Isatis indigotica Fort. by Capillary Gas Chromatography with Electron Capture or Flame Photometric Detection

2005 ◽  
Vol 88 (3) ◽  
pp. 720-728 ◽  
Author(s):  
Feng Tang ◽  
Yongde Yue ◽  
Rimao Hua ◽  
Shimei Ge ◽  
Jie Tang
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Pesticide Residues ◽  
Capillary Gas Chromatography ◽  
Medicinal Herbs ◽  
Raw Material ◽  
Isatis Indigotica ◽  
Photometric Detection ◽  
Flame Photometric Detection

Abstract Two multiresidue methods were developed for the determination of 15 pesticides (organochlorines, organphosphorus compounds, pyrethroids, and fungicides) in medicinal herbs Isatis indigotica Fort. and its formulations. The analytical procedure is based on ultrasonic assisted extraction and liquid-liquid extraction (LLE). After solvents were added, the raw material or granule sample was sonicated in an ultrasonic water bath and then centrifuged, filtered, and cleaned up by LLE. The infusion sample was extracted with petroleum ether by LLE. The pesticide residues were determined by capillary gas chromatography with electron-capture or flame photometric detection. Recoveries with the method at concentrations between 0.4 μg/kg and 10 μg/kg ranged from 70.2 to 119.5% for raw material, 73.2 to 105.1% for granule formulation, and 72.8 to 113.3% for infusion formulation. The relative standard deviation values were <20% for all of the pesticides studied. The pesticide detection limits were within the ranges 0.3–0.5 μg/L for endosulfan, 3–7.5 μg/L for pyrethroids, 0.7–32.5 μg/L for organophosphorus pesticides, and 0.1–0.6 μg/L for the other pesticides. The proposed methods are simple and rapid and provide simultaneous determination of pesticide residues in Isatis indigotica Fort. with acceptable recoveries and repeatability and an adequate limit of determination.

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