Charcoal Column Cleanup Method for Many Organophosphorus Pesticide Residues in Crop Extracts

1969 ◽  
Vol 52 (3) ◽  
pp. 522-526 ◽  
Author(s):  
Randall R Watts ◽  
R W Storherr ◽  
John R Pardue ◽  
Theodore Osgood
Keyword(s):  
Ethyl Acetate ◽  
Potassium Chloride ◽  
Pesticide Residues ◽  
Organophosphorus Pesticides ◽  
Organophosphorus Pesticide ◽  
Analytical Results

Abstract In the charcoal column cleanup method for organophosphorus pesticide residues in crops, the pesticides arc extracted from the crops with ethyl acetate and a 10–20 g aliquot is placed directly on the charcoal adsorbent column for cleanup. The Kuderna-Danish concentrated eluate is analyzed by GLC, using the potassium chloride thermionic detector. Analytical results are presented for pesticide field-treated crops and for crop extracts fortified with a total of 60 parent organophosphorus pesticides and alteration products. Recoveries averaged 90% or better in most cases.

A General Method for Organophosphorus Pesticide Residues in Nonfatty Foods

1971 ◽  
Vol 54 (3) ◽  
pp. 513-516 ◽  
Author(s):  
R W Storherr ◽  
P Ott ◽  
R R Watts
Keyword(s):  
Potassium Chloride ◽  
Pesticide Residues ◽  
Organophosphorus Pesticides ◽  
Extraction Procedure ◽  
Organophosphorus Pesticide ◽  
Flame Photometric Detector ◽  
Chlorinated Hydrocarbon ◽  
Photometric Detector ◽  
General Method

Abstract A method is presented for determining residues of organophosphorus pesticides and alteration products in nonfatty foods. This method employs the acetonitrile extraction procedure as used by FDA for the chlorinated hydrocarbon pesticides. Cleanup is performed with a short charcoal column. GLC, using the potassium chloride thermionic detector or flame photometric detector, is used for determination. Forty-one organophosphorus pesticides and/or alteration products are evaluated.

Collaborative Study of a Method for Organophosphorus Pesticide Residues in Apples and Green Beans

1974 ◽  
Vol 57 (4) ◽  
pp. 930-933
Author(s):  
Ronald R Laski
Keyword(s):  
Potassium Chloride ◽  
Pesticide Residues ◽  
Organophosphorus Pesticides ◽  
Collaborative Study ◽  
Organophosphorus Pesticide ◽  
Oxidation Products ◽  
Green Beans ◽  
Average Recovery ◽  
Oxygen Analog ◽  
Precision And Accuracy

Abstract Ten laboratories took part in a collaborative study of a method for organophosphorus pesticide residues in apples and green beans. Six representative organophosphorus pesticides or oxidation products were determined in duplicate at a different level on each crop. The average recovery of the pesticides, using the gas chromatographic potassium chloride thermionic detection system, had the precision and accuracy expected for parathion, paraoxon, carbophenothion oxygen analog, carbophenothion, and EPN. Interference due to reagents made quantitation of dimethoate inaccurate. The average recovery (%) of the pesticides on apples and beans, respectively, was as follows: dimethoate 125.1 and 112.9; paraoxon 99.3 and 103.7; parathion 86.5 and 92.2; carbophenothion oxygen analog 96.7 and 100.1; carbophenothion 88.8 and 102.6; and EPN 90.8 and 98.3. A separate part of the study involved a comparison between the potassium chloride thermionic gasliquid chromatographic detector and the phosphorus- specific flame photometric detector. A statistical analysis of the results obtained from 5 laboratories indicated that the 2 detection systems were equivalent in both precision and accuracy.

scholarly journals Extraction and Cleanup of Organochlorine and Organophosphorus Pesticide Residues in Fats by Supercritical Fluid Techniques

1997 ◽  
Vol 80 (3) ◽  
pp. 639-646 ◽  
Author(s):  
Marvin L Hopper
Keyword(s):  
Supercritical Fluid ◽  
Pesticide Residues ◽  
Corn Oil ◽  
Organophosphorus Pesticides ◽  
Organophosphorus Pesticide ◽  
Cleanup Procedure ◽  
Diet Study ◽  
Study Methodology ◽  
Integrated Extraction ◽  
Organochlorine And Organophosphorus Pesticides

Abstract A supercritical fluid extraction and cleanup procedure was developed for separating organochlorine and organophosphorus pesticides from fats. Supercritical carbon dioxide modified with 3% (v/v) acetonitrile was used to extract the pesticides at 6O°C and separate the pesticides from the fats at 4000 psi and 95°C on an in-line C? silica-based column. The extraction and cleanup procedure gave good recoveries for 43 of 62 nonpolar to moderately polar organochlorine and organophosphorus pesticides from fats, whereas 49 were recovered through conventional Florisil column cleanup before quantitation. This procedure can extract and clean up pesticide residues from 0.65 g animalbased fat and 1.0 g oils. Coeluted residues in the pesticide fraction ranged from 2.5 mg for butterfat to 0.8 mg for corn oil. Results for samples analyzed with this integrated extraction cleanup procedure were reproducible and comparable with results obtained with the current Total Diet Study methodology.

Optimization of Sweep Codistillation Apparatus for Determination of Coumaphos and Other Organophosphorus Pesticide Residues in Animal Fat

1987 ◽  
Vol 70 (3) ◽  
pp. 442-445
Author(s):  
Robert L Brown ◽  
Clinton N Farmer ◽  
Roderick G Millar
Keyword(s):  
Coefficient Of Variation ◽  
Pesticide Residues ◽  
Organophosphorus Pesticides ◽  
Organophosphorus Pesticide ◽  
Optimum Conditions ◽  
Animal Fat ◽  
Sweep Time ◽  
Coefficients Of Variation ◽  
The Mean

Abstract Optimum conditions have been developed for the quantitative recovery of coumaphos from animal fat by using a commercial sweep codistillation unit. Under the conditions specified (255°C distillation temperature, 250 mL/min of nitrogen, 60 min sweep time) and using Florisil trapping, the mean recovery of coumaphos was 91% with a coefficient of variation of 6%. Other organophosphorus pesticides recovered include diazinon, chlorpyrifos, ethion, and bromophos-ethyl with recoveries ranging from 90 to 96% and coefficients of variation ranging between 4 and 6%.

scholarly journals Organochlorine and Organophosphonis Pesticide Residues in Food from Egyptian Local Markets

1996 ◽  
Vol 79 (4) ◽  
pp. 949-952 ◽  
Author(s):  
Salwa M Dogheim ◽  
Sohair A Gad Alla ◽  
Sami M A El-Syes ◽  
Monir M Almaz ◽  
Emel Y Salama
Keyword(s):  
Pesticide Residues ◽  
Organophosphorus Pesticides ◽  
Organophosphorus Pesticide ◽  
Storage Period ◽  
Citrus Fruits ◽  
Fish Samples ◽  
Maximum Residue Limits ◽  
Before And After ◽  
Repeated Use ◽  
Agricultural Use

Abstract A market basket survey was conducted to monitor organochlorine and organophosphorus pesticide residues in potatoes, citrus fruits, and fish collected from local Egyptian markets. Maximum Residue Limits (MRLs) of the Codex Committee on Pesticide Residues for γ-hexachlorocyclohexane (HCH) in potatoes were exceeded in 8 samples and for DDT in 2 samples. The aging of HCH and DDT indicated a recent use of both pesticides during the potato storage period between cultivation seasons. However, such use is illegal because HCH mixture isomers (gammaxane) and DDT have been officially prohibited from agricultural use in Egypt since 1980. The highest residue levels of fenitrothion (3.8 ppm) in potatoes may be due to its repeated use before and after harvest. No organochlorine pesticide residues were found in citrus fruits. None of the detected organophosphorus pesticides exceeded their MRLs. HCH and DDT residue limits were exceeded in 5 and 7 fish samples, respectively, collected from 12 markets throughout the country. The heptachlor MRL was violated in only one fish sample (3.9 ppm).

scholarly journals Vinyl Phosphate-Functionalized, Magnetic, Molecularly-Imprinted Polymeric Microspheres’ Enrichment and Carbon Dots’ Fluorescence-Detection of Organophosphorus Pesticide Residues

Polymers ◽  
2019 ◽  
Vol 11 (11) ◽  
pp. 1770 ◽  
Author(s):  
Mao Wu ◽  
Yajun Fan ◽  
Jiawei Li ◽  
Danqing Lu ◽  
Yaping Guo ◽  
...  
Keyword(s):  
Fluorescence Detection ◽  
Pesticide Residues ◽  
Carbon Dots ◽  
Organic Phosphorus ◽  
Organophosphorus Pesticides ◽  
Organophosphorus Pesticide ◽  
Particle Size Analysis ◽  
Size Analysis ◽  
Molecularly Imprinted ◽  
Dual Functional

The rapid detection of organophosphorus pesticide residues in food is crucial to food safety. One type of novel, magnetic, molecularly-imprinted polymeric microsphere (MMIP) was prepared with vinyl phosphate and 1-octadecene as a collection of dual functional monomers, which were screened by Gaussian09W molecular simulation. MMIPs were used to enrich organic phosphorus, which then detected by fluorescence quenching in vinyl phosphate-modified carbon dots (CDs@VPA) originated from anhydrous citric acid. MMIPs and CDs@VPA were characterized by TEM, particle size analysis, FT-IR, VSM, XPS, adsorption experiments, and fluorescence spectrophotometry in turn. Through the fitting data from experiment and Gaussian quantum chemical calculations, the molecular recognition properties and the mechanism of fluorescence detection between organophosphorus pesticides and CDs@VPA were also investigated. The results indicated that the MMIPs could specifically recognize and enrich triazophos with the saturated adsorption capacity 0.226 mmol g−1, the imprinting factor 4.59, and the limit of recognition as low as 0.0006 mmol L−1. Under optimal conditions, the CDs@VPA sensor has shown an extensive fluorescence property with a LOD of 0.0015 mmol L−1 and the linear range from 0.0035 mmol L−1 to 0.20 mmol L−1 (R2 = 0.9988) at 390 nm. The mechanism of fluorescence detection of organic phosphorus with CDs@VPA sensor might be attributable to hydrogen bonds formed between heteroatom O, N, S, or P, and the O−H group, which led to fluorescent quenching. Meanwhile, HN−C=O and Si−O groups in CDs@VPA system might contribute to cause excellent blue photoluminescence. The fluorescence sensor was thorough successfully employed to the detection of triazophos in cucumber samples, illustrating its tremendous value towards food sample analysis in complex matrix.

Determination Method of Organophosphorus Pesticide Residues in Fishs by GPC-GC-PFPD

2011 ◽  
Vol 138-139 ◽  
pp. 1002-1006
Author(s):  
Bin Li ◽  
Fan Gang Zeng ◽  
Wei Fang Ma ◽  
Qi Chun Dong ◽  
Hai Tao Fan ◽  
...  
Keyword(s):  
Pesticide Residues ◽  
Limit Of Detection ◽  
Organophosphorus Pesticides ◽  
Organophosphorus Pesticide ◽  
Gel Permeation Chromatography ◽  
Determination Method ◽  
Average Recovery ◽  
Relative Standard ◽  
Gel Permeation ◽  
Good Repeatability

The 10 organophosphorus pesticides in fish can be rapidly extracted and separated by gel permeation chromatography, and the lipin and organophosphorus pesticides of fish can be seperated. The interfering matters can be well eliminated in this condition, and analysis is more rapid than other methods. The residues of 10 organophosphorus pesticides at same time can be identified and quantified simultaneously by GC-PFPD. This method is simple, rapid, and the average recovery ratios were 71.7%-80.9%.Good repeatability was obtained in all the cases with relative standard deviations (RSDs) lower 11%, and limit of detection was0.0003-0.004 mg·kg-1.

A Comparative Study of Sensitivity of Acetylcholinesterase in Detection of Organophosphorus Pesticide Residues

2008 ◽  
Vol 4 (3) ◽  
Author(s):  
Sun Xia ◽  
Xiangyou Wang ◽  
Xiao yu Wang ◽  
Zhe Liu
Keyword(s):  
Pesticide Residues ◽  
Ache Activity ◽  
Specific Activity ◽  
Organophosphorus Pesticides ◽  
Low Cost ◽  
Organophosphorus Pesticide ◽  
High Specific Activity ◽  
Good Choice ◽  
Chicken Liver ◽  
Chicken Brain

In this paper, four enzymes from different sources used for pesticide detection were tested and compared: homogenate from chicken liver, chicken brain and cyprinoids brain were made respectively in the laboratory and Acetylcholinesterase (AChE) was purchased from Musca domestica. The inhibition of AChE activity under different concentrations of omethoate, trichlorfon and dichlorvos were compared. The results showed that the AChE activity in chicken liver and cyprinoids brain were very low. The capacities of activity inhibition of other two kinds of AChE were better. Chicken brain-esterase's inhibition rate achieved 24.16%, 50.56%, and 54.1% for 100ug/L of omethoate, trichlorfon and dichlorvos respectively. Chicken brain-esterase has high specific activity, is low cost, and easy to prepare, and the inhibition of the sensitivity to three organophosphorus pesticides is significantly higher than enzymes from chicken liver and cyprinoids brain. So the chicken brain-esterase could be a good choice to use to detect pesticide residues in agricultural products.

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.

Modified Storherr Method for Determination of Organophosphorus Pesticides in Nonfatty Food Total Diet Composites

1981 ◽  
Vol 64 (3) ◽  
pp. 714-719
Author(s):  
Louis J Carson
Keyword(s):  
Liquid Chromatography ◽  
Pesticide Residues ◽  
Organophosphorus Pesticides ◽  
Organophosphorus Pesticide ◽  
Gas Liquid Chromatography ◽  
Flame Photometric Detector ◽  
Limit Of Quantitation ◽  
Total Diet ◽  
Residue Levels

Abstract The method of Storherr et al. for organophosphorus pesticide residues in nonfatty foods has been modified to permit its use in analyzing the composites of nonfatty foods in the Food and Drug Administration Total Diet Program. Modifications were designed to permit the examination by gas-liquid chromatography (GLC) of the larger weight (100 mg) of sample equivalent required by the Total Diet program. To achieve a limit of quantitation of 2 ppb parathion, the organophosphorus pesticides are determined by GLC equipped with flame photometric detector (P-mode) and/or KCl thermionic detector. Recovery data, ranging from 70 to 133%, are presented for fortification (2-10 ppb) of organophosphorus pesticides in 7 nonfatty food Total Diet composites. The modified Storherr method was successfully tested in an intralaboratory method trial of 2 Total Diet composites (potatoes and legumes) fortified at 5-13 ppb with malathion, parathion, paraoxon, and monocrotophos. In addition, the modified Storherr method was compared to existing FDA Total Diet methodology for the determination of incurred organophosphorus residues. Residue levels found by both methods were similar for malathion (30 ppb), parathion (7 ppb), and diazinon (1 ppb), but only the modified Storherr method was capable of determining about 10 ppb dimethoate and phorate in the cereals and grains composite.

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