Multiresidue Method for Pesticide Residue Analysis in Food of Animal and Plant Origin Based on GC or LC and MS or MS/MS

2012 ◽  
Vol 95 (6) ◽  
pp. 1777-1796 ◽  
Author(s):  
Eva Muñoz ◽  
Gloria Muñoz ◽  
Laura Pineda ◽  
Eulalia Serrahima ◽  
Francesc Centrich
Keyword(s):  
Residue Analysis ◽  
Gel Permeation Chromatography ◽  
Accreditation Body ◽  
Technical Note ◽  
Plant Origin ◽  
European Regulation ◽  
Multiresidue Method ◽  
Maximum Residue Levels ◽  
Residue Levels

Abstract A multiresidue method based on GC or LC and MS or MS/MS for the determination of 204 pesticides in diverse food matrixes of animal and plant origin is described. The method can include different stages of cleanup according to the chemical characteristics of each sample. Samples were extracted using accelerated solvent extraction. Those with a high fat content or that contained chlorophyll required further purification by gel permeation chromatography and/or SPE (ENVI-Carb). The methodology developed here was fully validated; the LOQs for the 204 pesticides are presented. The LOQ values lie between 0.01 to 0.02 mg/kg. However, in some cases, mainly in baby food, they were as low as 0.003 mg/kg, thereby meeting European Union requirements on maximum residue levels for pesticides, as outlined in European regulation 396/2005 and the Commission Directive 2003/13/EC. The procedure has been accredited for a wide scope of pesticides and matrixes by the Spanish Accreditation Body (ENAC) following ISO/IEC 17025:2005, as outlined in ENAC technical note NT-19.

Gas Chromatographic Determination of Ametryn and Its Metabolites in Tropical Root Crops

1984 ◽  
Vol 67 (2) ◽  
pp. 280-284
Author(s):  
Promode C Bardalaye ◽  
Willis B Wheeler
Keyword(s):  
Anhydrous Sodium Sulfate ◽  
Residue Analysis ◽  
Gel Permeation Chromatography ◽  
Chromatographic Determination ◽  
Solvent System ◽  
Complete Separation ◽  
Flame Photometric Detector ◽  
Root Crops ◽  
Photometric Detector

Abstract Residue analysis of the herbicide ametryn (2-methyIthio-4-ethylamino-s-isopropylamino-s-triazine) is widely known but an analytical method for determining its metabolites has not yet been reported in the literature. A method has been developed for the extraction and determination of ametryn and 3 metabolites, 2-methylthio-4-amino-6-isopropylammo- s-triazine (GS-11354), 2-methylthio-4,6-diamino-.s-triazine(GS- 26831), and 2-methylthio-4-amino-6-ethylamino-s-triazine (GS-11355) in taniers, yams, cassava. Residues were extracted from crops with ethyl acetate-toluene (3 + 1 v/v), using a Polytron homogenizer and anhydrous sodium sulfate added for drying. The extracts were cleaned up by automated gel permeation chromatography on Bio-Beads SX-3 gel in the same solvent system. Quantitative determination was performed by gas chromatographic (GC) analysis on a column packed with 5% DEGS-PS on 100-120 mesh Supelcoport using either an N-P detector or a flame photometric detector (FPD) in the sulfur mode. Minimum detection by the flame photometric detector is 10 ng each for ametryn, GS-11354, and GS-11355 and 21 ng for GS-26831; by the N-P detector, 0.3 ng of each component gives easily quantitatable peaks. On a parts per million basis, starting with 25 g sample, the FPD detected a minimum level of 0.04 p.g/g each for ametryn, GS-11354, and GS-11355, and 0.08 p.g/g for GS-26831. The N-P detector could detect 0.0024 p.g/g for all 4 compounds. In addition to superior sensitivity, instrumental conditions allowed the complete separation of components in 10 min, for the N-P detector; more than 30 min was required for the FPD. Recoveries from fortified crops ranged from 67 to 111% at levels of 0.1-1.0 μg/g.

Determination of Polybrominated Biphenyl Residues in Dairy Products

1975 ◽  
Vol 58 (5) ◽  
pp. 978-982
Author(s):  
Norbert V Fehringer
Keyword(s):  
Dairy Products ◽  
Gel Permeation Chromatography ◽  
Fatty Material ◽  
Polybrominated Biphenyls ◽  
Gel Permeation ◽  
Aoac Method ◽  
Residue Levels ◽  
Polybrominated Biphenyl ◽  
Liquid Chromatographic

Abstract A method for the determination of polybrominated biphenyls (PBBs) in dairy products is described. Fat is extracted from the products by the official AOAC method. The PBB residues are separated from the fatty material by gel permeation chromatography prior to gas-liquid chromatographic (GLC) quantitation. An additional cleanup using petroleum ether elution through a miniature Florisil column is necessary for thin layer chromatographic (TLC) confirmation. Recoveries of PBBs from samples fortified at levels from 0.1 to 0.5 ppm ranged from 94 to 104% with an average of 99%. GLC sensitivity permits the estimation of PBB residue levels as low as 0.007 ppm. Routine TLC confirmation is limited by sensitivity to ≥0.2 ppm.

Multiresidue Method for Determination of Organophosphorus Insecticide Residues in Fatty Processed Foods by Gel Permeation Chromatography

1995 ◽  
Vol 78 (6) ◽  
pp. 1502-1512 ◽  
Author(s):  
Anna Sannino ◽  
Paola Mambriani ◽  
Mirella Bandini ◽  
Luciana Bolzoni
Keyword(s):  
Methylene Chloride ◽  
Organophosphorus Compounds ◽  
Gel Permeation Chromatography ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Processed Foods ◽  
Multiresidue Method ◽  
Photometric Detection ◽  
Gel Permeation

Abstract A multiresidue method for quantitative determination of 39 organophosphorus compounds (parent pesticides and their major metabolites) in 7 fatty processed foods is described. Samples are extracted with methylene chloride and cleaned up by automated gel permeation chromatography with a Biobeads SX3 column and a methylene–chloridecyclohexane (15 + 85) eluant. Organophosphorus compounds are quantitated by capillary gas-liquid chromatography with flame photometric detection using OV-1701 and DB-5 columns. Average recoveries from samples fortified at 0.025–1 mg/kg ranged from 50.6% for dichlorvos to 185% for malaoxon. Determination limits were between 0.005 and 0.040 μg/mL. Results were confirmed by gas chromatography/mass spectrometry with selected-ion monitoring.

scholarly journals Assessment of the Pesticide Residue Occurrence in Fruit from the South-Eastern Region of Poland During 2010-2011 Seasons

2012 ◽  
Vol 20 (2) ◽  
pp. 119-126 ◽  
Author(s):  
Magdalena Słowik-Borowiec ◽  
Ewa Szpyrka ◽  
Anna Kurdziel ◽  
Magdalena Grzegorzak ◽  
Aneta Matyaszek
Keyword(s):  
Plant Protection ◽  
Eastern Region ◽  
The South ◽  
Black Currant ◽  
Decomposition Products ◽  
South Eastern ◽  
Maximum Residue Levels ◽  
Residue Levels ◽  
Active Substances

Abstract During the 2010-2011 seasons, analyses of 171 samples of fresh fruit from the south-eastern region of Poland were performed. The research program included the determination of 137 (in 2010) to 152 (in 2011) active substances, together with their metabolites and decomposition products. The analytical methods used in the research were gas chromatography (GC/ECD/NPD) and spectrophotometry (to determine residues of dithiocarbamates). The results were compared with Poland’s allowed maximum residue levels (MRLs).Residues of active plant protection product substances were detected in 85 samples (50%), while 7 (4%) samples had exceeded the MRLs.Violations of MRLs were mainly concerned with the following group of insecticides: cypermethrin (in black currant), esfenwalerate (in raspberry), and the fungicides: propiconazole, and difenoconazole (in gooseberries).

scholarly journals Determination of Florfenicol, Thiamfenicol and Chloramfenicol at Trace Levels in Animal Feed by HPLC–MS/MS

Antibiotics ◽  
2019 ◽  
Vol 8 (2) ◽  
pp. 59 ◽  
Author(s):  
Rosa Elvira Gavilán ◽  
Carolina Nebot ◽  
Ewelina Patyra ◽  
Beatriz Vazquez ◽  
Jose Manuel Miranda ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
Animal Feed ◽  
Simultaneous Detection ◽  
The European Union ◽  
European Regulation ◽  
Official Control ◽  
Liquid Chromatography Tandem Mass ◽  
Residue Levels ◽  
Low Levels

Administration of florfenicol and thiamfenicol through medicated feed is permitted within the European Union, always following veterinary prescription and respecting the withdrawal periods. However, the presence of low levels of florfenicol, thiamfenicol, and chloramfenicol in non-target feed is prohibited. Since cross-contamination can occur during the production of medicated feed and according to Annex II of the European Regulation 2019/4/EC, the control of residue levels of florfenicol and thiamfenicol in non-target feed should be monitored and avoided. Based on all the above, a sensitive and reliable method using liquid chromatography tandem mass spectrometry was developed for the simultaneous detection of chloramfenicol, florfenicol, and thiamfenicol at trace levels in animal feed. Analytes were extracted from minced feed with ethyl acetate. Then, the ethyl acetate was evaporated, the residue was resuspended in Milli-Q water and the extract filtered. The method was in-house validated at carryover levels, with concentration ranging from 100 to 1000 µg/kg. The validation was conducted following the European Commission Decision 2002/657/EC and all performance characteristics were successfully satisfied. The capability of the method to detect amfenicols at lower levels than any prior perspective regulation literature guarantees its applicability in official control activities. The developed method has been applied to non-compliant feed samples with satisfactory results.

scholarly journals Pesticide residues in cow’s milk

Mljekarstvo ◽  
2021 ◽  
Vol 71 (3) ◽  
pp. 165-174
Author(s):  
Milivoje Ćosić ◽  
Keyword(s):  
Pesticide Residues ◽  
Large Series ◽  
The Other ◽  
Milk Samples ◽  
Commission Regulation ◽  
Maximum Residue Levels ◽  
Residue Levels ◽  
Quality Of Milk

Quality of milk plays a key role in its wide consumption but also of its involvement in a large series of derived products, such as yogurt, cheese, butter, and ice cream. An effective LC-MS/MS method has been validated for the determination of 81 different pesticide residues in milk samples. The analyses comprised 44 milk samples collected during 2019. From all inspected pesticides, only metalaxyl (present in 11.36 % samples), bifenthrin and metolachlor (9.09 %), dimethoate (4.55 %), prochloraz and thiacloprid were detected in 2.27 % of analysed samples. The detections of trifloxystrobin and bifenthrin were above the maximum residue levels (MRLs). The Commission Regulation (EU) 2017/1135 standardizes the MRLs for dimethoate and omethoate in certain products, but a MRL for dimethoate residues in milk has not been established jet. All the other pesticide detections were below the MRLs.

scholarly journals Distribution, source apportionment and health risk assessment of organochlorine pesticides in drinking groundwater

2021 ◽  
Author(s):  
John A. O. Oyekunle ◽  
Abiodun O. Adegunwa ◽  
Odunayo T. Ore
Keyword(s):  
Risk Assessment ◽  
Health Risk ◽  
Organochlorine Pesticides ◽  
Health Risk Assessment ◽  
The European Union ◽  
Groundwater Samples ◽  
Maximum Residue Levels ◽  
Residue Levels ◽  
High Concentrations

Abstract Groundwater samples of Ile-Ife, Osun State, Nigeria were investigated for their organochlorine pesticides (OCPs) levels. Probable sources of the OCPs and health risks associated with their consumption along with the water were determined in order to establish the potability of the groundwater samples. Quantitative determination of the OCPs was carried out by Gas Chromatography coupled with Electron Capture Detector (GC-ECD) after liquid-liquid extraction with dichloromethane (DCM). Results indicated that all the analyzed OCPs except p,p'-dichlorodiphenylethane were detected with high concentrations in the groundwater. Heptachlor (14.60±3.60 µg L-1) and methoxychlor (12.60±2.20 µg L-1) showed dominant concentrations that were higher than 0.02 ng L-1 maximum residue levels (MRLs) recommended by the European Union. Levels of the OCPs in the samples followed the decreasing trend: cyclodienes > diclorophehylethanes > chlorinated cyclohexanes, while the predominant source of the analyzed pesticides could be ascribed to aerial transportation from fresh applications in homes within the community. The carcinogenic health risk assessment also revealed consistent higher values of HQ and CR in children as opposed to adults, indicating that children are the more vulnerable population to the analyzed environmental contaminants.

scholarly journals Distribution, source apportionment and health risk assessment of organochlorine pesticides in drinking groundwater

2021 ◽  
Author(s):  
John A. O. Oyekunle ◽  
Abiodun O. Adegunwa ◽  
Odunayo T. Ore
Keyword(s):  
Risk Assessment ◽  
Health Risk ◽  
Organochlorine Pesticides ◽  
Health Risk Assessment ◽  
The European Union ◽  
Groundwater Samples ◽  
Maximum Residue Levels ◽  
Residue Levels ◽  
High Concentrations

Abstract Groundwater samples of Ile-Ife, Osun State, Nigeria were investigated for their organochlorine pesticides (OCPs) levels. Probable sources of the OCPs and health risks associated with their consumption along with the water were determined in order to establish the potability of the groundwater samples. Quantitative determination of the OCPs was carried out by Gas Chromatography coupled with Electron Capture Detector (GC-ECD) after liquid-liquid extraction with dichloromethane (DCM). Results indicated that all the analyzed OCPs except p,p'-dichlorodiphenylethane were detected with high concentrations in the groundwater. Heptachlor (14.60±3.60 µg L-1) and methoxychlor (12.60±2.20 µg L-1) showed dominant concentrations that were higher than 0.02 ng L-1 maximum residue levels (MRLs) recommended by the European Union. Levels of the OCPs in the samples followed the decreasing trend: cyclodienes > diclorophehylethanes > chlorinated cyclohexanes, while the predominant source of the analyzed pesticides could be ascribed to aerial transportation from fresh applications in homes within the community. The carcinogenic health risk assessment also revealed consistent higher values of HQ and CR in children as opposed to adults, indicating that children are the more vulnerable population to the analyzed environmental contaminants.

scholarly journals Evaluation of Immunoassays as an Alternative for the Rapid Determination of Pesticides in Wine and Grape Samples

2010 ◽  
Vol 93 (1) ◽  
pp. 2-11 ◽  
Author(s):  
Nerea Argarate ◽  
María Arestin ◽  
Javier Ramón-Azcón ◽  
Begoña Alfaro ◽  
Alejandro Barranco ◽  
...  
Keyword(s):  
Rapid Determination ◽  
Grape Juice ◽  
White Wine ◽  
Accuracy And Precision ◽  
Final Measurement ◽  
The Matrix ◽  
Maximum Residue Levels ◽  
Simple Extraction ◽  
Residue Levels

Abstract The main objective of this paper is to address the performance of immunochemical assays for the detection of the residues of three pesticides [atrazine, bromopropylate, and 2,4,6-trichlorophenol (TCP)] in real winery samples, such as wine, grapes, and grape juice. Different approaches have been evaluated to minimize interferences from the matrixes, and suitable working protocols have been established in order to achieve the necessary LODs, accuracy, and precision for real samples. A simple dilution of the sample proved to be sufficient for the determination of atrazine and bromopropylate in red and white wine and grape juice at the required levels of concentration. However, for TCP, an SPE procedure has been optimized using amino cartridges. The recoveries were above 85% in all cases, and the LOD values were below the parts per billion level, except for bromopropylate, which ranged between 2 and 50 µg/L, depending on the matrix. The grape matrix effect could be resolved by a simple extraction with methanol. Complete recoveries were obtained, and the final measurement procedures were able to determine selected pesticides below their maximum residue levels. The newly developed methods have been compared with standard chromatographic methods.

General Method for Determination of Pesticide Residues in Samples of Plant Origin, Soil, and Water. III. Gas Chromatographic Analysis and Confirmation

1981 ◽  
Vol 64 (3) ◽  
pp. 749-768
Author(s):  
Árpád Ambrus ◽  
Éva Visi ◽  
Ferenc Zakar ◽  
Éva Hargitai ◽  
László Szabó ◽  
...  
Keyword(s):  
Chromatographic Analysis ◽  
Residue Analysis ◽  
Gas Liquid Chromatography ◽  
Pesticide Residue Analysis ◽  
Temperature Programming ◽  
Plant Origin ◽  
Relative Retention ◽  
Soil And Water ◽  
General Method

Abstract Gas-liquid chromatography is widely used in pesticide residue analysis, and numerous packings of various polarity are recommended. We selected OV-22, OV-101, NPGS, SE-30 (3% on Gas-Chrom Q), and 1.95% SP-2401/1.5% SP-2250 on Supelcoport as basic packings. Relative retention times for aldrin and parathion-methyl were determined at 140,160, 180, or 200°C and during temperature programming. OV-22 and OV-101 were most suitable for general purposes. A study on the performance of thermionic delectors suggested that their performance can be characterized and should be regularly controlled with test substances containing different hetero elements. Columns as short as 45-90 cm were suitable for screening purposes, and their advantages over traditional long columns are demonstrated. The fractionation of pesticides in an extract on silica gel columns was effective and practical for the confirmation of pesticides.

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