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Sample records for pesticide residue analysis

  1. QA/QC in pesticide residue analysis

    This paper outlines problems related to pesticide residue analysis in a regulatory laboratory that are related to: availability of reference materials, as over 1000 pesticide active ingredients are currently in use and over 400 crops represent a large part of a healthy diet; analysis time; availability of samples in sufficient numbers; uncertainties of the procedures

  2. Analysis of pesticide residues Or a needle in a barn

    This work is about the analysis of pesticide residues as well as the study of soil, air, water and organisms. The solvents used depend on the matrix, types of pesticides, analysis and the equipment. The chromatography engaged with mass spectrometry is one of the most used techniques.

  3. Sampling and sample processing in pesticide residue analysis.

    Lehotay, Steven J; Cook, Jo Marie

    2015-05-13

    Proper sampling and sample processing in pesticide residue analysis of food and soil have always been essential to obtain accurate results, but the subject is becoming a greater concern as approximately 100 mg test portions are being analyzed with automated high-throughput analytical methods by agrochemical industry and contract laboratories. As global food trade and the importance of monitoring increase, the food industry and regulatory laboratories are also considering miniaturized high-throughput methods. In conjunction with a summary of the symposium "Residues in Food and Feed - Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods" held at the 13th IUPAC International Congress of Pesticide Chemistry, this is an opportune time to review sampling theory and sample processing for pesticide residue analysis. If collected samples and test portions do not adequately represent the actual lot from which they came and provide meaningful results, then all costs, time, and efforts involved in implementing programs using sophisticated analytical instruments and techniques are wasted and can actually yield misleading results. This paper is designed to briefly review the often-neglected but crucial topic of sample collection and processing and put the issue into perspective for the future of pesticide residue analysis. It also emphasizes that analysts should demonstrate the validity of their sample processing approaches for the analytes/matrices of interest and encourages further studies on sampling and sample mass reduction to produce a test portion. PMID:25677085

  4. Analysis of pesticide residues and metabolites by radioactive tracers

    A method using radioactive tracers is described for determining residues and metabolites of pesticides. The sensitivity of this technique is very high and it can be better as 10-3?gr per gr. of dry matter. (J.C.)

  5. Pesticide residue quantification analysis by hyperspectral imaging sensors

    Liao, Yuan-Hsun; Lo, Wei-Sheng; Guo, Horng-Yuh; Kao, Ching-Hua; Chou, Tau-Meu; Chen, Junne-Jih; Wen, Chia-Hsien; Lin, Chinsu; Chen, Hsian-Min; Ouyang, Yen-Chieh; Wu, Chao-Cheng; Chen, Shih-Yu; Chang, Chein-I.

    2015-05-01

    Pesticide residue detection in agriculture crops is a challenging issue and is even more difficult to quantify pesticide residue resident in agriculture produces and fruits. This paper conducts a series of base-line experiments which are particularly designed for three specific pesticides commonly used in Taiwan. The materials used for experiments are single leaves of vegetable produces which are being contaminated by various amount of concentration of pesticides. Two sensors are used to collected data. One is Fourier Transform Infrared (FTIR) spectroscopy. The other is a hyperspectral sensor, called Geophysical and Environmental Research (GER) 2600 spectroradiometer which is a batteryoperated field portable spectroradiometer with full real-time data acquisition from 350 nm to 2500 nm. In order to quantify data with different levels of pesticide residue concentration, several measures for spectral discrimination are developed. Mores specifically, new measures for calculating relative power between two sensors are particularly designed to be able to evaluate effectiveness of each of sensors in quantifying the used pesticide residues. The experimental results show that the GER is a better sensor than FTIR in the sense of pesticide residue quantification.

  6. Optimisation of gas chromatography for pesticide residue analysis

    Water and soil contamination due to the variety of pesticides used in agriculture practices is a global environmental pollution problem. Organochlorine pesticides are of special interest in this context as their high chemical stability results in their persistence and bioaccumulation in the environment and animal tissues. Sensitive, rapid and reliable methods for the routine determination of organochlorine residues in environment are thus much needed. In this study for the determination of organochlorine pesticide residue in environmental samples; experimental parameters such as effect of temperature and pressure of GC-ECD were studied and optimized. (Author)

  7. Optimisation of analytical method for pesticide residue analysis in tomato

    In the past, the effect of sample processing on the variability of the results and stability of residues gained very little attention of analyst. The current trend is to analyze 5- 10 g analytical portions to save money and time, and to reduce waste material. The sample processing methods and conditions should be optimized and the analytical method validated or its reproducibility verified. This study is carried out by comparing the efficiency of various equipment and processing procedure and to testing the stability of pesticide residues during sample processing. A stable and easy to analyze organophosphorus compound is applied on the surface of the tomato and processed according to the procedure intended to be used in the laboratory. The extract was analyzed by GCMS. From the thoroughly homogenized material, five replicate analytical portions are withdrawn and extracted. Comparing the expected and measured residues in the analytical portions through the recoveries assesses the stability of residues. (Author)

  8. Pesticide Residues in Food

    This indicator describes the number of pesticide residues detected in fruits, vegetables, grains, meat, and dairy products from across the country and the number of residues exceeding the EPA tolerance for a given pesticide-commodity pair from 1994 to 2009. This information pr...

  9. MULTI-RESIDUE ANALYSIS OF PESTICIDES IN GRAPES IN BIJAPUR DISTRICT

    U.S.Pujeri

    2010-10-01

    Full Text Available Fruit samples of grapes were analyzed for pesticide residues, employing multi-residue analysis by gas- liquid chromatography-mass spectrography (GC-MS/ LCMS/ MS. All the fruit samples showed the presence of pesticide residues with one or other group of pesticides. Some of the grape samples contain more than the minimum residue limit. The increasing interest in the study of pesticides in grapes is justified from an enological point of view, since some pesticides can interfere with fermentative microflora used in wine production, as well as affect consumer safety. There were no significant differences between some pesticide levels found in the whole grape (skin and pulp and in the grape skin. Chlorpyriphos, captan, dichlorovos, oxyfluorfen, fipronoil, 4- bromo-2-chlorophenol and indoxycarb were detected. Nevertheless, consumer intake of pesticides from grapes studied in this work should be decreased as a result of water washing of the grapes. In this paper, multiresidue determination of pesticides using GCMS/ LC-MS/MS are discussed.

  10. Pesticide residue analysis of vegetables by gas chromatography with electron-capture detection.

    Fenoll, Jos; Helln, Pilar; Martnez, Carmen M; Flores, Pilar

    2007-01-01

    A new and original analytical method was developed for the routine analysis of 28 multiclass pesticide residues in vegetables (green pepper, red pepper, and tomato). The extraction was performed with acetone, and the pesticides were partitioned into ethyl acetate-cyclohexane (1 + 1, v/v). Residue levels in vegetables were determined by gas chromatography (GC) with electron-capture detection. Residue identities were confirmed by GC coupled with mass spectrometry in the selected ion monitoring mode. The average recoveries in pepper and tomato obtained for all analytes studied were 67.3 and 123.1%, respectively, with relative standard deviation between 1.8 and 7.0%. The detection limit for the pesticides studied varied from 0.1 to 2.6 microg/kg. The proposed method was applied to the analysis of these compounds in vegetables grown in experimental greenhouses. PMID:17373459

  11. Analysis of Some Pesticide Residues in Cauliflower by High Performance Liquid Chromatography

    Sheheli Islam

    2009-01-01

    Full Text Available Problem statement: Increased use of chemicals on vegetables started gaining momentum and continued its up-trend in Bangladesh. Wide spread use of pesticides in agriculture concern of residue accumulation, which may remain in food and agricultural environment causing concern of human health and risking ecological balance. Attempt made to ensure that their applications were correct and safe and result in no residues in food beyond codex developed maximum residue limits. Approach: This study reported a method based on High Performance Liquid Chromatography (HPLC for determination of pesticide residues used in Cauliflower. Cauliflower sprayed with, 4 different pesticides (diazinon, malathion, chlorpyrifos and cypermethrin at recommended dose and double of recommended dose were analyzed for their residual contents. Samples were collected at same day after application of pesticide. Commercial samples of cauliflowers were collected from different markets of Dhaka city. Reversed-phase HPLC system with UV detection was used for the separation, identification and quantification of all these analytes using acetonitrile-water (70:30, v/v as mobile phase. Results: Limit of detection of 0.02 mg kg-1 was obtained. Calibration curves that constructed for the analytes spiked into samples followed linear relationships with good correlation coefficients (R2>0.990. In the analysis, from vegetables treated with diazinon and chlorpyrifos at recommended and double of recommended doses, residual amounts above respective MRL values were found. Conclusion: Method used permitted the determination of these pesticides in cauliflower at concentration level demanded by current legislation. Attention paid on excess use or abuse of pesticides by judicious application for safety of public health in Bangladesh. Additional data to monitor residues in food and to fill gaps in current knowledge would be helpful in assessing human exposure risks from ingestion of contaminated cauliflower or other vegetables.

  12. Selectivity and sensitivity in coupled chromatographic techniques as applied in pesticide residue analysis

    The advantages and drawbacks of coupled chromatographic techniques are discussed on the basis of selected applications of LC-LC and LC-GC in the analysis of pesticide residues applied to environmental biological samples. (author). 18 refs.; 5 figs.; 2 tabs

  13. Analysis of Vegetables and Fruits Organophosphorus Pesticides Residual Detecting Results in Qingdao Market

    Peilong Xu; Haifeng Zhao

    2015-01-01

    In this study, organophosphorus pesticides residuals of vegetables and fruits in Qingdao market were detected and analyzed and the detecting results provide valuable data for food safety control and agriculture supervisions. Testing method in national standard NY/F761-2008 was applied to detect 16 kind of organophosphorus pesticides residuals in 350 vegetable and fruit samples. Detecting results showed that, in 350 samples, there were 52 positive in pesticide residuals and the qualified rate ...

  14. The use of solid phase extraction method for analysis of residues of pesticides used in banana production in Costa Rica

    Different solid phase extraction devices were tested for the analysis of residues of eleven pesticides used in banana production in Costa Rica. The analysis was performed by using gas chromatograph equipped with NPD and ECD detectors. In general low recoveries and high variation coefficients were found for chlorothalonil, imazalil, terbufos and thiabendazole. For the other pesticides recoveries ranged between 60 and over 100%. (author)

  15. Evaluation of two fast and easy methods for pesticide residue analysis in fatty food matrixes.

    Lehotay, Steven J; Mastovská, Katerina; Yun, Seon Jong

    2005-01-01

    Two rapid methods of sample preparation and analysis of fatty foods (e.g., milk, eggs, and avocado) were evaluated and compared for 32 pesticide residues representing a wide range of physicochemical properties. One method, dubbed the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticide residue analysis, entailed extraction of 15 g sample with 15 mL acetonitrile (MeCN) containing 1% acetic acid followed by addition of 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. After centrifugation, 1 mL of the buffered MeCN extract underwent a cleanup step (in a technique known as dispersive solid-phase extraction) using 50 mg each of C18 and primary secondary amine sorbents plus 150 mg MgSO4. The second method incorporated a form of matrix solid-phase dispersion (MSPD), in which 0.5 g sample plus 2 g C18 and 2 g anhydrous sodium sulfate was mixed in a mortar and pestle and added above a 2 g Florisil column on a vacuum manifold. Then, 5 x 2 mL MeCN was used to elute the pesticide analytes from the sample into a collection tube, and the extract was concentrated to 0.5 mL by evaporation. Extracts in both methods were analyzed concurrently by gas chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry. The recoveries of semi-polar and polar pesticides were typically 100% in both methods (except that basic pesticides, such as thiabendazole and imazalil, were not recovered in the MSPD method), but recovery of nonpolar pesticides decreased as fat content of the sample increased. This trend was more pronounced in the QuEChERS method, in which case the most lipophilic analyte tested, hexachlorobenzene, gave 27 +/- 1% recovery (n=6) in avocado (15% fat) with a<10 ng/g limit of quantitation. PMID:15859091

  16. Evaluation of common organic solvents for gas chromatographic analysis and stability of multiclass pesticide residues.

    Mastovsk, Katerina; Lehotay, Steven J

    2004-06-25

    In this study, we evaluated the suitability of six common organic solvents for gas chromatographic (GC) analysis of pesticides. Three of these, acetone, acetonitrile (MeCN) and ethyl acetate (EtAc), represent extraction solvents commonly used in multiresidue methods for determination of pesticides in produce. The other three, isooctane, hexane and toluene, often serve as exchange solvents before a GC analysis. An ideal solvent for GC analysis of multiclass pesticide residues should be compatible with: the analytes, sample preparation, and GC analysis. This study addresses each aspect with emphasis placed on stability of selected pesticides in the given solvents. In this respect, the exchange solvents proved to be superior to the more polar extraction solvents. Degradation of N-trihalomethylthio fungicides (e.g., captan, folpet, dichlofluanid) in MeCN was observed only in certain lots of the tested MeCN, but even if it occurred, the stability of these analytes as well as that of dicofol and chlorothalonil was dramatically improved by the addition of 0.1% (v/v) acetic acid. Dicofol and chlorothalonil were also unstable in acetone, and pesticides with a thioether group (e.g., fenthion, disulfoton) degraded in the tested EtAc. Formation of isomers of certain pyrethroids (deltamethrin, lambda-cyhalothrin) was recorded in the chromatograms from MeCN and acetone solutions, but this effect more likely occurred during the GC injection than in solution. For several reasons, MeCN was found to be the most suitable solvent for extraction of a wide polarity range of pesticide residues from produce. After acidification, the stability of problematic pesticides in MeCN is acceptable, and MeCN can also serve as a medium for GC injection; therefore solvent exchange is generally not required before GC analysis. If sensitivity is an issue in splitless injection, then toluene was demonstrated to be the best exchange solvent due to its miscibility with MeCN and stronger responses of relatively more polar pesticides (e.g., acephate, methamidophos) as compared to hexane and isooctane. PMID:15230533

  17. Analysis of Vegetables and Fruits Organophosphorus Pesticides Residual Detecting Results in Qingdao Market

    Peilong Xu

    2015-08-01

    Full Text Available In this study, organophosphorus pesticides residuals of vegetables and fruits in Qingdao market were detected and analyzed and the detecting results provide valuable data for food safety control and agriculture supervisions. Testing method in national standard NY/F761-2008 was applied to detect 16 kind of organophosphorus pesticides residuals in 350 vegetable and fruit samples. Detecting results showed that, in 350 samples, there were 52 positive in pesticide residuals and the qualified rate was 85.14% and in these samples, there were 39 samples in which 1 pesticide residual quantity was unqualified, 9 samples in which 2 pesticide residual quantity were unqualified, 3 samples in which 3 pesticide residual quantity were unqualified and 1 samples in which 4 pesticide residual quantity were unqualified. Pesticides residuals were all positive in the vegetables, fruits and grains sold in Qingdao market in 2014 and the situation is especially serious in leaf vegetables. This suggests that the food enterprises should pay more attention to this situation and should control more carefully in food materials safety.

  18. Comparison and evaluation of two methods for the pesticide residue analysis of organophosphates in yerba mate

    Luca, Pareja; Silvina, Niell; Zisis, Vryzas; Joaqun, Gonzlez; Mara Vernica, Cesio; Euphemia P., Mourkidou; Horacio, Heinzen.

    2015-04-01

    Full Text Available Abstract Microwave Assisted Extraction and a modified CEN-QuEChERS methodology were evaluated as extraction and clean up procedures for the simultaneous analysis of 42 organophosphate pesticides in yerba mate (Ilex paraguaiensis). The obtained extracts were analyzed by gas chromatography using a fla [...] me photometric detector. Linearity, recovery percentages, relative standard deviations, detection and quantification limits and matrix effects were determined according to DG-SANCO guidelines for both methods. At 0.2 and 0.5 mg/kg the evaluated methods showed percentages recoveries between 70 and 120% for most of the analytes. Using Microwave Assisted Extraction methodology, 33 pesticide residues could be properly analyzed whereas only 27 could be determined with the proposed modified QuEChERS. All relative standard deviation were below 18% except for omethoate and disulfoton sulfone when evaluated by the modified QuEChERS. The limits of detection in both methodologies were 0.2 mg/kg for most of the analyzed compounds. The average detection limit for QuEChERS was 0.04 mg/kg. For 19 of the analytes determined through Microwave Assisted Extraction the lowest validated level were 0.004 mg/kg. Signal suppression/enhancement was observed for most of the pesticides, thus matrix-matched calibration curves were used for quantification. The Microwave Assisted Extraction and QuEChERS procedures studied could detect the organophosphate pesticides above the MRL fixed for "mate" by the European Union. They have been successfully applied for the determination of organophosphate pesticide residues in commercial samples and the positives were confirmed through GC(ITD)-MS.

  19. Headspace Solid Phase Microextraction in Pesticide Residues Analysis: 2. Apple Samples

    Jelena Milinović

    2007-01-01

    Full Text Available Headspace solid phase microextraction method (HS/SPME, optimised previously for pesticide water solutions, was applied to trace residues of the pesticides chlorpyrifos, fenthion and bifenthrin in apple samples. One-hour extraction procedure was performed at 60oC extraction temperature. Nonpolar polydimethyl siloxane (PDMS fiber was used. Detection and quantification were carried out by gas chromatography/mass spectrometry (GC/MS. A non-pesticide treated apple sample was fortified with the pesticides over a 0.025-1.25 mg/kg concentration range in order to determine analytical parameters of the method applied. Linearity with regression coefficient (R values higher than 0.99 were obtained over the whole concentration range investigated for chlorpyrifos and fenthion, while linear dependence was observed in the 0.1-1.25 mg/kg range for bifenthrin. Relative recovery values for samples fortified at different levels were in the 56.68-82.91% range. Limit of detection (LOD values were determined as follows: 0.014 mg/kg for chlorpyrifos, 0.021 mg/kg for fenthion and 0.053 mg/kg for bifenthrin. Relative standard deviation (RSD values obtained for multiple analysis of the sample fortified at 0.6 mg/kg level were not higher than 20%.

  20. Sample preparation approaches for the analysis of pesticide residues in olives and olive oils

    Agricultural practices generally require the use of pesticides by olive growers for the best olive and olive oil production. Thus, analytical methods are needed to identify and quantify the pesticide residues that may be present, and ensure that the product complies with regulatory requirements. I...

  1. Some applications of solid phase micro extraction (SPME) in the analysis of pesticide residues in food.

    Volante, M; Cattaneo, M; Bianchi, M; Zoccola, G

    1998-05-01

    The Solid Phase Micro-Extraction (SPME) technique was applied to analyze chlorpropham in potatoes and amitraz in honey. The homogenized sample, suspended in water and stirred, was extracted with a 100 microns thick polidimetylsiloxane fiber and desorbed into the injection port of a gas chromatograph/mass-spectrometer (quadrupole) operating in single ion monitoring. Sensitivities down to 0.01 mg/Kg and linear responses in the range of 0.01-0.1 mg/Kg were obtained. The results of SPME pesticide residue analysis in potatoes corresponded to those obtained with a traditional multiresidue method. PMID:9604340

  2. Analysis Method for Pesticides Residues by GC/MS in Lebanese Apple

    The apple's crop can be affected by many pests during the growing season, which requires careful monitoring. Both apple fruit and apple tree need to be treated by pesticides in order to protect them from pests. Such treatment often leads to the accumulation of stable pesticides inside the fruit. The local market provides a large variety of pesticides allowing farmers to use more than one active substance in order to protect their crop, often without proper advice. Monitoring pesticides on apples and other agricultural crops is the best way to protect consumers health from the hazards of pesticides residues. The development of new, rapid and effective method to analyze the multi pesticides residues at trace levels in apple samples is essential. This work describes the extraction procedure and the analytical method developed to detect the pesticide residues using the gas-chromatographic-mass spectrometric approach (GC-MS). The developed method was successfully applied to analyze apple samples collected from different Lebanese markets for a one year period in order to monitor the presence of pesticides and their stability in apple fruits during storage. (author)

  3. Quantitative analysis of pesticide residues in vegetables and fruits by liquid chromatography quadrupole time-of-flight mass spectrometry.

    Saito-Shida, Shizuka; Nemoto, Satoru; Teshima, Reiko; Akiyama, Hiroshi

    2016-01-01

    The applicability of liquid chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) for the quantitative analysis of pesticide residues in vegetables and fruits was demonstrated. The LC-QTOF-MS parameters, such as cone voltage, capillary voltage, collision energy and mass extraction window, were carefully optimised for the analysis of pesticide residues. The LC-QTOF-MS method was validated for 149 pesticides in four vegetables and fruits, i.e. apple, potato, cabbage and spinach, at a spiking level of 0.01mgkg(-1). The samples were prepared according to the Japanese official multi-residue method with a modification to the column clean-up procedure. Of the 149 pesticides, recoveries in the range of 70-120% were achieved for 147 pesticides in apple, 145 in potato, 141 in cabbage and 131 in spinach, with intra-day precisions (RSDs) of <25% and inter-day precisions (RSDs) of <30%, which are within the acceptable range given in the Japanese method validation guideline. Matrix effects were negligible for the majority of the target pesticides. Except for spiroxamine in spinach, no interfering peaks were observed in the blank samples. The target pesticides, except those with low sensitivity, achieved calibration curves with satisfactory linearity, with correlation coefficients (r) greater than 0.995 in the concentration range of 0.002-0.1?gml(-1). Furthermore, the majority of the target pesticides provided more than one fragment ion or isotope ion that could be used for confirmation. The overall results suggest that LC-QTOF-MS is a powerful tool for the quantification of pesticide residues in vegetables and fruits at the level of 0.01mgkg(-1). PMID:26479897

  4. Development of a new cucumber reference material for pesticide residue analysis: feasibility study for material processing, homogeneity and stability assessment

    Grimalt, Susana; Harbeck, Stefan; Shegunova, Penka; Seghers, John; Sejerøe-Olsen, Berit; Emteborg, Håkan; Dabrio, Marta

    2015-01-01

    The feasibility of the production of a reference material for pesticide residue analysis in a cucumber matrix was investigated. Cucumber was spiked at 0.075 mg/kg with each of the 15 selected pesticides (acetamiprid, azoxystrobin, carbendazim, chlorpyrifos, cypermethrin, diazinon, (α + β)-endosulfan, fenitrothion, imazalil, imidacloprid, iprodione, malathion, methomyl, tebuconazole and thiabendazole) respectively. Three different strategies were considered for processing the material, based o...

  5. High-throughput planar solid phase extraction : a new clean-up concept in multi-residue analysis of pesticides

    Oellig, Claudia

    2014-01-01

    Currently, the most serious problems in pesticide residue analysis by liquid chromatography (LC) or gas chromatography (GC) coupled to mass spectrometry (MS) concern the so-called “matrix effects”. The most common way to avoid these effects is the application of matrix-matched calibration standards. Nevertheless, an efficient clean-up undoubtedly is the best way to prevent matrix effects in multi-residue analysis of pesticides in food by LC–MS or GC–MS. For a totally new powerful clean-up ...

  6. Validation of thin-layer chromatographic methods for pesticide residue analysis. Results of the coordinated research projects 1996-2002

    Thin-layer chromatography (TLC) has a long history, but has been used only to a limited extent in pesticide residue analytical laboratories since gas liquid chromatography (GLC) and high performance liquid chromatography (HPLC) became readily available. Recent developments in the quality of plate coating and detection systems, as well as in extraction and cleanup methods have revived interest in TLC. The combination of these procedures with rigid quality control has created a niche for TLC in laboratories working in compliance with ISO 17025 or GLP. The Joint FAO/IAEA Division of Nuclear Techniques in Food and Agriculture recognized the importance of testing pesticide residues, especially in countries with limited resources. A coordinated research programme (CRP) was initiated for investigating the application of TLC detection methods to complement the instrumental techniques in pesticide residue analysis. An initial technical contract provided proof of the concept and elaborated the basic procedures, including a substantial database of retention factors and minimum detectable quantities of pesticides. To satisfy the demands from the eligible laboratories, two similar projects were started in 1997 and 1998. The titles of the projects were as follows: (i) Validation of Thin-layer Chromatographic Screening Methods for Pesticide Residue Analysis; and (ii) Alternative Methods to Gas and High Performance Liquid Chromatography for Pesticide Residue Analysis in Grain. Scientists from 18 countries participated in the above noted two projects. The major tasks of this programme were to adapt the methods, check the repeatability and reproducibility of Rf values, the minimum detectable quantities (MDQ) and apply the methods for determining various pesticide residues in representative matrices. Furthermore, they have extended the methods to other pesticides and commodities of interest in their countries and validated the methods elaborated. This TECDOC includes the most important results of the CRPs. The Rf and MDQ values reported by the participating scientists are compiled in one table for facilitating the assessment of the repeatability and reproducibility of the results. Since the participants were applying the same basic methodology, described in detail in the first article, these methods are only referred to in the other papers. However, the modifications made by the participants are described in their papers. The purpose of this TECDOC is to provide the readers with comprehensive information on the application of TLC detection methods to complement the instrumental techniques in pesticide residue analysis. Further information on any specific topic may be obtained from the authors

  7. Synthesis and surface engineering of magnetic nanoparticles for environmental cleanup and pesticide residue analysis: a review.

    Kaur, Ranjeet; Hasan, Abshar; Iqbal, Nusrat; Alam, Samsul; Saini, Mahesh Kr; Raza, Syed Kalbe

    2014-07-01

    In recent years, water pollution and pesticide accumulation in the food chain have become a serious environmental and health hazard problem. Direct determination of these contaminants is a difficult task due to their low concentration level and the matrix interferences. Therefore, an efficient separation and preconcentration procedure is often required prior to the analysis. With the advancement in nanotechnology, various types of magnetic core-shell nanoparticles have successfully been synthesized and received considerable attention as sorbents for decontamination of diverse matrices. Magnetic core-shell nanoparticles with surface modifications have the advantages of large surface-area-to-volume ratio, high number of surface active sites, no secondary pollutant, and high magnetic properties. Due to their physicochemical properties, surface-modified magnetic core-shell nanoparticles exhibit high adsorption efficiency, high rate of removal of contaminants, and easy as well as rapid separation of adsorbent from solution via external magnetic field. Such facile separation is essential to improve the operation efficiency. In addition, reuse of nanoparticles would substantially reduce the treatment cost. In this review article, we have attempted to summarize recent studies that address the preconcentration methods of pesticide residue analysis and removal of toxic contaminants from aquatic systems using magnetic core-shell nanoparticles as adsorbents. PMID:24777942

  8. Analysis of Pesticide Residues in Fortified Water, Soil and Vegetable Samples

    Seema Tahir

    1999-01-01

    Full Text Available Water, soil and potato samples spiked with insecticides were analyzed for percent recoveries on Gas Chromatograph (GC equipped with Electron Capture Detector (ECD, using capillary column. Percent recoveries of methyl parathion were calculated to be 100, 67 and 94 percent at spiking level of 0.17, 1.7 and 8.7 micro g/liter and 310 and 138 percent for cypermethrin at spiking level of 0.146 and 1.46 g/liter by liquid-liquid extraction. Through solid-phase extraction the percent recovery of deltamethrin was 37 and 78 percent at spiking level of 0.16 and 1.6 micro g/liter. The percent recoveries of deltamethrin through solvent extraction technique were found to be 78 and 86 percent at spiking level of 2.56 and 25.20 micro g/liter, while 81 and 147 percent for deltamethrin and cypermethrin through soxhlet extraction at 8.0 and 8.7 micro g/liter concentration respectively. The percent recoveries at spiking level of 0.1 ppm were calculated to be 0, 5.59, 35.52 and 0 percent, and in 1.00 ppm recovery was calculated to be 91.98, 56.60, 44.56 and 58.93 percent in fortified samples of potato with dimethoate, methyl parathion, endosulfan and cypermethrin, followed by 0, 59.82, 111.20, 11.36 percent in blank spiked at 0.1 ppm respectively. The data presented provides evidence that capillary column GC with ECD detection can be used reliably and advantageously for regulatory determination of pesticide residues in food, water and soil. The different methods described allow quantitative extraction of the pesticides. However, further experiments need to be conducted to ensure consistent results. The reproducibility of analytical methods require that the pesticide residue analysis be performed with the highest possible accuracy and so qualified that, the results obtain reflect the least deviation from the true value.

  9. Residue analysis of organochlorine pesticides in the Mae Klong river of Central Thailand

    The most natural waterways in Thailand are utilized for conventional agricultures, e.g. irrigation and wastewater discharge. Concentrations of 20 organochlorine pesticides (OCPs) were measured in surface sediments collected from the tributaries of the Mae Klong river during 2003-2005. The sampling sites chosen were nearby the rice paddy which organochlorine pesticides were intensively used for crop cultivation. Solid-liquid extraction technique was used for sediment extraction, and gas chromatography with electron capture detector was applied for pesticides determination. Total concentrations of OCPs found were ranged from 4.12 to 214.91 ?g g-1 dw in the first year. In the second year, total residue concentrations in the surface sediments were in the range of 3.26-215.09 ?g g-1 dw. Concentrations of pesticides were greater in dry-season rice cultivation period in both sampling years, and heptachlor epoxide was the contaminant found at highest concentration in this study. In addition, the occurrence of some selected contaminants including DDT, DDD and DDE reflects the recent contamination in the study area. This demonstrates not only that the natural waterway was polluted and contained much pesticide residues, but it also illustrates the necessity of a continuous long-term monitoring of the affected environment

  10. Pesticide residues in locally available cereals and vegetables

    Vegetable samples (pechay, cabbage, lettuce, green beans and tomatoes) bought from public markets in the Metro Manila area were analyzed for pesticide residues using gas chromatography. The samples analyzed in 1968-69 contained high levels of chlorinated pesticides such as DDT, Aldrin, Endrin, and Thiodan, while in the samples analyzed in January 1976, no chlorinated and organophosphate pesticides were detected. Cereal samples (rice, corn and sorghum) were obtained from the National Grains Authority and analyzed for pesticide residues and bromine residues. Total bromine residues was determined by neutron activation analysis. In most of the samples analyzed, the concentrations of pesticide residues were below the tolerance levels set by the FAO/WHO Committee on Pesticide Residues in Foods. An exception was one rice sample from Thailand, the bromine residue content (110ppm) of which exceeds the tolerance level of 50ppm

  11. Social and Economic Dimensions of Pesticide Residues

    Burçak, Aydan Alev

    2015-01-01

    Given their affordable price, ease of use and labour effective nature, pesticides are highly used in agriculture and a variety of sectors and are acknowledged as an effective method for pest control.Pesticide usage resides in several problems such as human health and environmental. The pesticides on or in the agricultural products and in the environment are called pesticide residues. The consumers have an increasing concern about their health because of the pesticide residues on food and wate...

  12. Validation of thin lay chromatographic screening methods for pesticide residue analysis

    Thin layer chromatographic (TLC) separation and detection methods were tested as a cost efficient alternative for identification and quantitative determination of numerous pesticide residues. Over 80% reproducibility was obtained for Rf and MDQ values compared to those previously reported. The applicability of the methods resulted in recovery values between 75 and 100%. The sample load up to 600 mg sample equivalent did not affect the Rf values significantly. (author)

  13. Cost effective screening methods for pesticide residue analysis in fruits, vegetables and cereal grains

    This paper reports the results of studies performed to investigate the potential of applying thin layer chromatography (TLC) detection in combination with selected extraction and cleanup methods, for providing an alternative cost-effective analytical procedure for screening and confirmation of pesticide residues in plant commodities. The extraction was carried out with ethyl acetate and an on-line extraction method applying an acetone-dichloromethane mixture. The extracts were cleaned up with SX-3 gel, an adsorbent mixture of active carbon, magnesia, and diatomaceous earth, and on silica micro cartridges. The Rf values of 118 pesticides were tested in eleven elution systems with UV, and eight biotest methods or and chemical detection reagents. Cabbage, green peas, orange, and tomatoes were selected as representative sample matrices for fruits and vegetables, while maize, rice and wheat represented cereal grains. As an internal quality control measure, marker compounds were applied on each plate to verify the proper elution and detection conditions. The Rf values varied in the different elution systems. The best separation (widest Rf range) was achieved with silica gel (SG)-ethyl acetate (0.05-0.7), SG-benzene, (0.02-0.7) and reverse phase RP-18 F-254S layer with acetone:methanol:water (30:30:30 v/v) (0.1-0.8). The relative standard deviation of Rf values (CVRf) within-laboratory reproducibility was generally less than 20%, except below 0.2 Rf, where the CVRf rapidly increased with decreasing Rf values. The fungi spore inhibition, chloroplast inhibition and enzyme inhibition were found most suitable for detection of pesticides primarily for confirming their identity or screening for known substances. Their use for determination of pesticide residues in samples of unknown origin is not recommended. (author)

  14. Analysis of tomato matrix effect in pesticide residue quantification through QuEChERS and single quadrupole GC/MS

    Ana M, Domnguez; Fabian, Placencia; Francisco, Cereceda; Ximena, Fadic; Waldo, Quiroz.

    2014-04-01

    Full Text Available The detection of pesticide in tomato (Solanum lycopersicum L.) matrix using Gas Chromatography hyphenated to Mass Spectrometry detector (GC/MS) can affect the sensitivity of the analysis by enhancement or suppression of their chromatography response, the percentages of recoveries and leading to erro [...] rs in the quantification of the pesticides. In this study, the matrix effect was investigated using nine pesticides, and "Quick, Easy, Cheap, Effective, Rugged and Safe" (QuEChERS)-GC/MS analytical technique was validated for pesticides multiresidue analysis. The matrix effect was determined using not statistical and statistical procedures including ANOVA, with similar results. Strong negative matrix effect was found for the pesticides trifluralin, 4,4'-DDT, and permethrin, resulting in the increment of the chromatogram background and a decrease in their detection responses. Contrary, an enhancement induced by the matrix presence was obtained for carbaryl and azinphos methyl, showing a positive medium matrix effect. While, dimethoate, simazine, 4,4'-DDE, and iprodione did not exhibit matrix effect. The detection limits (LOD) obtained, varied from 0.003 to 0.1 mg kg-1. Reproducibility was less than 20% for each pesticide. Recoveries were found to be between 71% and 121%, except for dimethoate, carbaryl, and azinphos methyl which reached values lower than 70%. Recoveries relative standard deviations were less than 22%. QuEChERS-GC/MS technique was used for evaluation of fresh commercial tomatoes samples, detecting carbaryl in all of them, but in concentration levels lower than the maximum residue limits according to regulations of Codex.

  15. Analysis of tomato matrix effect in pesticide residue quantification through QuEChERS and single quadrupole GC/MS

    Ana M Domínguez

    2014-04-01

    Full Text Available The detection of pesticide in tomato (Solanum lycopersicum L. matrix using Gas Chromatography hyphenated to Mass Spectrometry detector (GC/MS can affect the sensitivity of the analysis by enhancement or suppression of their chromatography response, the percentages of recoveries and leading to errors in the quantification of the pesticides. In this study, the matrix effect was investigated using nine pesticides, and "Quick, Easy, Cheap, Effective, Rugged and Safe" (QuEChERS-GC/MS analytical technique was validated for pesticides multiresidue analysis. The matrix effect was determined using not statistical and statistical procedures including ANOVA, with similar results. Strong negative matrix effect was found for the pesticides trifluralin, 4,4'-DDT, and permethrin, resulting in the increment of the chromatogram background and a decrease in their detection responses. Contrary, an enhancement induced by the matrix presence was obtained for carbaryl and azinphos methyl, showing a positive medium matrix effect. While, dimethoate, simazine, 4,4'-DDE, and iprodione did not exhibit matrix effect. The detection limits (LOD obtained, varied from 0.003 to 0.1 mg kg-1. Reproducibility was less than 20% for each pesticide. Recoveries were found to be between 71% and 121%, except for dimethoate, carbaryl, and azinphos methyl which reached values lower than 70%. Recoveries relative standard deviations were less than 22%. QuEChERS-GC/MS technique was used for evaluation of fresh commercial tomatoes samples, detecting carbaryl in all of them, but in concentration levels lower than the maximum residue limits according to regulations of Codex.

  16. ESTIMATION OF THE BURDEN OF PESTICIDE RESIDUES IN SLOVAK POPULATION

    Jozef Sokol

    2010-07-01

    Full Text Available Pesticides used in the agriculture have to be applied according to the requirements of good agricultural practice and appropriate law. Pesticides leave detectable residues in agricultural crops, raw materials and ecosystem components. Pesticides reach the human population through the food chain. Information on the type and concentration of pesticide residues in food is in Slovakia collected trough the monitoring programs. Health risks associated with pesticides contaminants in human nutrition are very important and are recently studied by several expert groups. Prerequisite programs are necessary to protect public health. Risk analysis and monitoring of the population burden by pesticide contaminants have to be performed in expert level. The general strategy for assessment of toxicity of pesticides is listed by the World health Organisation. Scientific risk assessment is the basis for taking action and making the legislation at national and European community level.doi:10.5219/69

  17. Analysis of 10 systemic pesticide residues in various baby foods using liquid chromatography-tandem mass spectrometry.

    Yang, Angel; Abd El-Aty, A M; Park, Jong-Hyouk; Goudah, Ayman; Rahman, Md Musfiqur; Do, Jung-Ah; Choi, Ok-Ja; Shim, Jae-Han

    2014-06-01

    Ten systemic pesticides, comprising methomyl, thiamethoxam, acetamiprid, carbofuran, fosthiazate, metalaxyl, azoxystrobin, diethofencarb, propiconazole, and difenoconazole, were detected in 13 baby foods (cereals, boiled potatoes, fruit and milk) using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) for sample preparation and liquid chromatography tandem mass spectrometry for analysis. The matrix-matched calibration curves showed good linearity with determination coefficients (R(2) ) >0.992. The limits of detection and quantitation were 0.0015-0.003 and 0.005-0.01 mg/kg, respectively. The mean recoveries of three different concentrations ranged from 69.2 to 127.1% with relative standard deviations residues. This method is suitable for the identification and quantification of systemic pesticides with matrix-matched standards in various baby foods. PMID:24861738

  18. Multi-residue analysis of traces of pesticides and antibiotics in honey by HPLC-MS-MS.

    Debayle, Delphine; Dessalces, Guy; Grenier-Loustalot, Marie Florence

    2008-06-01

    The aim of this work was to develop an analytical method for simultaneous assay of residues of two families of antibiotics, and three pesticides, in honey. The assays involved a mixture of five tetracyclines, four sulfamides, and the pesticides coumaphos, carbendazim, and amitraz (two metabolites). All the compounds were extracted from honey and pre-concentrated by optimised solid-phase extraction (SPE). Analysis was by high-performance liquid chromatography-mass spectrometry-mass spectrometry (HPLC-MS-MS) using a triple-quadrupole spectrometer in multiple reaction monitoring (MRM) mode in order to identify and quantify the compounds present (Sheth et al J Agric Food Chem 38:1125-1130, 1990). During development of the analytical method a strong matrix effect was found that depended on the floral origin of the honey. This led to the development of a standard additions method to quantify the contaminants sought. PMID:18425645

  19. New tendencies in isotopic analysis of pesticide residues from wines by mass spectrometry in concordance with the European standards

    Multi-isotope analysis, the determination of isotope ratios by mass spectrometry or magnetic resonance spectroscopy, becomes increasingly used in the food industry and by national food control laboratories as a method of authenticating both raw materials and finished products. These highly sophisticated techniques are capable of determining the botanical and geographical origin of a wide variety of foodstuffs, thus providing a means of detecting product adulteration and controlling mislabelling practices which are virtually impossible to circumvent. The European Union has officially adopted the used of isotope analysis as a means of controlling sugar addition in wines. Its successful implementation in the wine-producing Member States has considerably reduced the financial losses which the Community had incurred due to over - capitalisation. Coupling mass spectrometer with gas chromatograph is used for quantitative and qualitative analysis of traces of pesticides from food. The presence of pesticides in foods is harmful for the nervous system, the cardiovascular apparatus and decreases the immunity of human body. In addition, ensuring the foods quality and safety is a requirement, which must be fulfilled for the integration in EU. The subject of this paper is the presentation of the tests results of the isotopic analysis for pesticide residues in wines, in concordance with European Standard. (authors)

  20. Acetonitrile extraction and dual-layer solid phase extraction clean-up for pesticide residue analysis in propolis.

    Oellig, Claudia

    2016-05-01

    Propolis is a very complex mixture of substances that is produced by honey bees and is known to be a rather challenging matrix for residue analysis. Besides resins, flavonoids and phenols, high amount of wax is co-extracted resulting in immense matrix effects. Therefore a suitable clean-up is crucial and indispensable. In this study, a reliable solid phase extraction (SPE) clean-up was developed for pesticide residue analysis in propolis. The clean-up success was quickly and easily monitored by high-performance thin-layer chromatography with different detection possibilities. The final method consists of the extraction of propolis with acetonitrile according to the QuEChERS method followed by an effective extract purification on dual-layer SPE cartridges with spherical hydrophobic polystyrene-divinylbenzene resin/primary secondary amine as sorbent and a mixture of toluene/acetone (95:5, v/v) for elution. Besides fat-soluble components like waxes, flavonoids, and terpenoids, more polar compounds like organic acids, fatty acids, sugars and anthocyanins were also removed to large extent. Method performance was assessed by recovery experiments at spiking levels of 0.5 and 1mg/kg (n=5) for fourteen pesticides that are relevant for propolis. Mean recoveries determined by HPLC-MS against solvent standards were between 40 and 101%, while calculation against matrix-matched standards provided recoveries of 79-104%. Precision of recovery, assessed by relative standard deviations, were below 9%. Thus, the developed dual-layer SPE clean-up enables the reliable pesticide residue analysis in propolis and provides a suitable alternative to time-consuming clean-up procedures proposed in literature. PMID:27059398

  1. Evalualtion of the QuEChERS sample preparation approach for the analysis of pesticide residues in olives

    This paper describes the use of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for extraction and cleanup of 15 pesticide residues of regulatory importance in olives and olive oil. These products contain a high lipid content, which can adversely affect pesticide recoveries an...

  2. [Validation study on a multi-residue analysis of pesticides in agricultural products by using phosphoric acid treatment and GC-MS/MS].

    Makabe, Yuhki; Takahashi, Hiroshi; Enomoto, Tomoko; Aikawa, Takehiko

    2014-01-01

    A rapid method for multi-residue determination of pesticides in agricultural products was validated. The sample was cut into pieces and placed into a mixer cup containing half weight amount of 10% phosphoric acid in order to suppress degradation of easily degraded pesticides, represented by captan, and then homogenized. Pesticides in the phosphoric acid-treated sample were extracted with acetonitrile using a homogenizer, followed by salting out with anhydrous magnesium sulfate and sodium chloride. The extract was cleaned up on a C18 and graphite carbon black/PSA mini-cartridge column. Some pesticides gave tailing peaks, but these peaks became sharp and symmetrical when polyethylene glycol (PEG) 300 was added to the test solution. Recovery tests were performed on nine kinds of agricultural products (brown rice, soybean, spinach, cabbage, potato, orange, apple, strawberry, and Japanese pear) fortified with 170 pesticides at 0.01 and 0.1 ?g/g. Each concentration of pesticide residue was extracted from 2 samples on 5 separate days. The trueness of the method for 147-164 pesticides in each sample was 70-120% with satisfactory repeatability and within-run reproducibility. This method is expected to useful for multi-residue analysis of pesticides in agricultural products. PMID:25212821

  3. Trace analysis of multi-class pesticide residues in Chinese medicinal health wines using gas chromatography with electron capture detection

    Kong, Wei-Jun; Liu, Qiu-Tao; Kong, Dan-Dan; Liu, Qian-Zhen; Ma, Xin-Ping; Yang, Mei-Hua

    2016-01-01

    A method is described for multi-residue, high-throughput determination of trace levels of 22 organochlorine pesticides (OCPs) and 5 pyrethroid pesticides (PYPs) in Chinese medicinal (CM) health wines using a QuEChERS (quick, easy, cheap, effective, rugged, and safe) based extraction method and gas chromatography-electron capture detection (GC-ECD). Several parameters were optimized to improve preparation and separation time while still maintaining high sensitivity. Validation tests of spiked samples showed good linearities for 27 pesticides (R?=?0.99090.9996) over wide concentration ranges. Limits of detection (LODs) and quantification (LOQs) were measured at ng/L levels, 0.062?ng/L and 0.26?ng/L for OCPs and 0.023?ng/L and 0.067?ng/L for PYPs, respectively. Inter- and intra-day precision tests showed variations of 0.659.89% for OCPs and 0.9813.99% for PYPs, respectively. Average recoveries were in the range of 47.74120.31%, with relative standard deviations below 20%. The developed method was then applied to analyze 80 CM wine samples. Beta-BHC (Benzene hexachloride) was the most frequently detected pesticide at concentration levels of 5.6731.55?mg/L, followed by delta-BHC, trans-chlordane, gamma-BHC, and alpha-BHC. The validated method is simple and economical, with adequate sensitivity for trace levels of multi-class pesticides. It could be adopted by laboratories for this and other types of complex matrices analysis. PMID:26883080

  4. Trace analysis of multi-class pesticide residues in Chinese medicinal health wines using gas chromatography with electron capture detection

    Kong, Wei-Jun; Liu, Qiu-Tao; Kong, Dan-Dan; Liu, Qian-Zhen; Ma, Xin-Ping; Yang, Mei-Hua

    2016-02-01

    A method is described for multi-residue, high-throughput determination of trace levels of 22 organochlorine pesticides (OCPs) and 5 pyrethroid pesticides (PYPs) in Chinese medicinal (CM) health wines using a QuEChERS (quick, easy, cheap, effective, rugged, and safe) based extraction method and gas chromatography-electron capture detection (GC-ECD). Several parameters were optimized to improve preparation and separation time while still maintaining high sensitivity. Validation tests of spiked samples showed good linearities for 27 pesticides (R = 0.9909-0.9996) over wide concentration ranges. Limits of detection (LODs) and quantification (LOQs) were measured at ng/L levels, 0.06-2 ng/L and 0.2-6 ng/L for OCPs and 0.02-3 ng/L and 0.06-7 ng/L for PYPs, respectively. Inter- and intra-day precision tests showed variations of 0.65-9.89% for OCPs and 0.98-13.99% for PYPs, respectively. Average recoveries were in the range of 47.74-120.31%, with relative standard deviations below 20%. The developed method was then applied to analyze 80 CM wine samples. Beta-BHC (Benzene hexachloride) was the most frequently detected pesticide at concentration levels of 5.67-31.55 mg/L, followed by delta-BHC, trans-chlordane, gamma-BHC, and alpha-BHC. The validated method is simple and economical, with adequate sensitivity for trace levels of multi-class pesticides. It could be adopted by laboratories for this and other types of complex matrices analysis.

  5. Reduction of pesticide residues on produce by rinsing.

    Krol, W J; Arsenault, T L; Pylypiw, H M; Incorvia Mattina, M J

    2000-10-01

    In 1997 this laboratory initiated a research program with the objective of examining the effect that rinsing of produce with tap water would have on pesticide residues. Samples were obtained from local markets and/or grown at our experimental farm. Because approximately 35% of produce from retail sources contains pesticide residues, growing and treating produce at an experimental farm had the advantage that all such samples contain pesticide residues. Pesticides were applied under normal field conditions to a variety of food crops and the vegetation was allowed to undergo natural weathering prior to harvest. The resulting samples contained field-incurred or "field-fortified" residues. This experimental design was employed to mimic as closely as possible real world samples. Crops were treated, harvested, and divided into equal subsamples. One subsample was processed unwashed, whereas the other was rinsed under tap water. The extraction and analysis method used was a multi-residue method developed in our laboratory. Twelve pesticides were included in this study: the fungicides captan, chlorothalonil, iprodione, and vinclozolin; and the insecticides endosulfan, permethrin, methoxychlor, malathion, diazinon, chlorpyrifos, bifenthrin, and DDE (a soil metabolite of DDT). Statistical analysis of the data using the Wilcoxon signed-rank test showed that rinsing removed residues for nine of the twelve pesticides studied. Residues of vinclozolin, bifenthrin, and chlorpyrifos were not reduced. The rinsability of a pesticide is not correlated with its water solubility. PMID:11052716

  6. [Rapid screening and quantitative analysis of 144 pesticide residues in traditional Chinese medicinal herbs by gas chromatography-tandem mass spectrometry].

    Cheng, Zhi; Zhang, Rong; Liu, Weihua; Wang, Jinhu; Wang, Minglin

    2014-01-01

    An analytical method for the simultaneous determination of 144 pesticide residues in traditional Chinese medicinal herbs was established based on optimized QuEChERS with gas chromatography-tandem mass spectrometry (GC-MS/MS). The influences of different extraction solvents, different buffer systems and different purifying agents on the recoveries of the pesticides were investigated. The pesticide residues in the samples were extracted with acetonitrile, then cleaned-up by mixed sorbents and analyzed by GC-MS/MS in multi-reaction monitoring (MRM) mode. The external standard method was applied to quantify the pesticides. The linear range of the method was from 20 to 2 000 microg/kg with the correlation coefficients (r2) of more than 0. 983. The recoveries of the pesticides at the spiked levels of 20, 50 and 200 microg/kg ranged from 74.3% to 111.8% with the relative standard deviations lower than 15%, except for acephate, amitraz and aldrin. The method was successfully used for the analysis of target pesticides in testing samples, and had a good consistency in results with the existed standard one. This multi-residue analytical method allows for a rapid, efficient, sensitive and reliable screening and quantitative analysis of the target pesticides in traditional Chinese medicinal herbs. PMID:24783870

  7. Radioisotopes in pesticide residues and metabolic studies

    The increasing use of pesticides and their serious role as environmental contaminants necessitate detailed studies of their metabolism,toxicology and environmental fate.The complex problems which are beyond conventional analytical analysis could,and with great precision,be solved by the use of nuclear techniques.Pesticides labelled with radionuclides(H-3,C-14,P-32 and Cl-36) can be used.Compounds labelled with these radionuclides can be easily measured,in very low concentrations, by use of liquid scintillation counters.Metabolism and distribution of the labelled compounds in the plant can be followed by autoradiography.In this study,supported by the IAEA, the following pesticides were investigated, C-14 DDT, C-14 Endosulfan, C-14 Carbaryl, C-14 Carbofuran, C-14 Amitraz, C-14 Aldicarb and C-14 Butocarboxim. The investigations included :a) study of the binding of these compounds in soils. b) study of the : i) fate and dynamics of aldicarb in cotton plant. ii) fate of amitraz in tomatoes. 'this work is part of the programme of studies of pesticide residues in soil, plants and foods, aproject supported by the international Atomic Energy Commission '.(Author)

  8. Headspace Solid Phase Microextraction in Pesticide Residues Analysis:1. Optimisation of Extraction Conditions

    Rada Đurović

    2007-01-01

    Full Text Available The method of headspace solid phase microextraction (HS/SPME was successfully used in a simultaneous multicomponent analysis of hexachlorobenzene (HCB, tefluthrin, heptachlor, aldrin, chlorpyrifos, fenthion and bifenthrin in aqueous medium. Measurementswere performed using a nonpolar polydimethyl siloxane (PDMS fiber. Detection and quantification were done by gas chromatography/mass spectrometry (GC/MS.Optimal conditions for HS/SPME were determined both by performing extraction at different temperatures and examining extraction time profiles at constant temperature. Optimal extraction temperature for each pesticide studied was determined as follows: 60°C for HCB and for heptachlor, 80°C for aldrin and for chlorpyrifos, fenthion and tefluthrin, and temperature exceeding 80°C for bifenthrin. For the pesticide mixture studied, 60°C was identified as the optimum extraction temperature.Based on the time profiles obtained, it was confirmed that satisfactory extraction sensitivity can be obtained even for extraction times shorter than the time required to reach a sorption equilibrium. This conclusion was confirmed by linear concentration profiles obtained for the following ranges: 0.05-10 ng/ml (HCB, 0.05-25 ng/ml (tefluthrin, 0.05-40 ng/ml (heptachlor, 0.05-40 ng/ml (aldrin, 0.05-25 ng/ml (chlorpyrifos, 0.05-25 ng/ml (fenthionand 0.05-25 ng/ml (bifenthrin.Relative standard deviation (RSD values for triplicate measurements did not exceed 15%.

  9. Application of gas chromatography time-of-flight mass spectrometry for target and non-target analysis of pesticide residues in fruits and vegetables

    Hernández Hernández, Félix; Beltrán Arandes, Joaquim; Portolés Nicolau, Tania; Pitarch Arquimbau, María Elena; Cervera Vidal, María Inés

    2012-01-01

    In this work, the capability of gas chromatography coupled to time-of-flight mass spectrometry (GC–TOF MS) for quantitative analysis of pesticide residues has been evaluated. A multiclass method for rapid screening of pesticides (insecticides, acaricides, herbicides and fungicides) in fruit and vegetable matrices has been developed and validated, including detection, identification and quantification of the analytes. To this aim, several food matrices were selected: high water content (apples...

  10. Studies on residue behaviour of certain pesticides used in vegetables

    CÖNGER, Ergün; AKSU, Pelin; YİGİT, Nuran; DOKUMACI, Suna; BALOĞLU, Zehra; BURÇAK, A. Alev

    2012-01-01

    In this study, residue trials for some pesticides on tomatoes, green peppers and cucumbers were established in Ayaş, Nallıhan and Çubuk districts of Ankara province for a period of two years. Plant protection products containing chlorpyriphos, chlorothalonil and lambda-cyhalothrin on tomatoes; chlorpyriphos and metalaxyl-m+mancozeb on cucumbers; cyprodinil+fludioxonil, acetamiprid and chlorpyriphos on green peppers were used. Pesticide residue analysis of samples, that were periodically taken...

  11. Earthworm tolerance to residual agricultural pesticide contamination

    Givaudan, Nicolas; Binet, Françoise; Le Bot, Barbara; Wiegand, Claudia

    This study investigates if acclimatization to residual pesticide contamination in agricultural soils is reflected in detoxification, antioxidant enzyme activities and energy budget of earthworms. Five fields within a joint agricultural area exhibited different chemical and farming histories from...

  12. Liquid chromatography Orbitrap mass spectrometry with simultaneous full scan and tandem MS/MS for highly selective pesticide residue analysis.

    Del Mar Gómez-Ramos, María; Rajski, Łukasz; Heinzen, Horacio; Fernández-Alba, Amadeo R

    2015-08-01

    This paper describes the application of LC/Q-Orbitrap MS for the analysis of pesticide residues in fruit and vegetable commodities. LC/Q-Orbitrap MS working in full scan simultaneously with a single MS/MS scan was used to analyse 139 pesticide residues in QuEChERS extracts of tomato, pepper, orange and green tea. Full scan data were obtained at a resolution of 70,000 whereas MS/MS data were obtained at a resolution of 17,500. Quantitation and detection was carried out using full scan data while MS/MS data were used only for identification. MS/MS scans did not have a negative influence on quantitation under the applied conditions. Some peak area reproducibility problems were the consequence of the low sensitivity for some compounds (aldicarb, chlorpyriphos methyl, fenitrothion and fipronil) under the applied conditions. The relation between the operational parameters (viz. automatic gain control (AGC) target, maximum injection time (IT), underfill ratio, isolation window and apex trigger) and the number of automatically identified compounds was investigated. Mass error and minimal intensity of selected fragment ions were also studied. Various working modes were compared, such as full scan with single MS/MS scan and full scan with multiple MS/MS scans. In both cases, the number of automatically reported pesticides was the same. However full scan with single MS/MS scan ensured more points per peak in full scan mode and better peak area reproducibility. The evaluation of the identification and quantitation capabilities of the instrument was performed through the analysis of 100 real samples. The samples were also analysed by LC-QqQ MS/MS and the results of both analytical systems were compared. The comparison revealed that the two instruments were consistent with each other. They found the same pesticides and neither false positive nor false negatives were reported. Nevertheless the Q-Orbitrap MS allowed one to work in high resolution mass spectrometry, increasing the selectivity and, in full scan mode, permitting the retrospective analysis of the data feature that cannot be achieved with QqQ. PMID:25943259

  13. [Characterizing the toxicity interaction of the binary mixture between DMSO and pesticide by the multi-effect residual analysis (MERA)].

    Huo, Xiang-Chen; Liu, Shu-Shen; Zhang, Jing; Zhang, Jin

    2013-01-01

    Three groups of binary mixtures between dimethylsulfoxide (DMSO) and three widely used pesticides, dimethoate (DIM), dichlorvos (DIC), and metalaxyl (MET), were respectively constructed by using the direct equipartition ray design (EquRay). The luminescent inhibition toxicities of single chemical and binary mixtures to Vibrio qinghaiensis sp. -Q67 were determined by the microplate toxicity analysis (MTA). Selecting the concentration addition (CA) model as an additive reference, we developed a new multi-effect residual analysis (MERA) to quantitatively characterize the deviation of the observed toxicity from that predicted by the CA model, i. e. the degree of toxicity interaction. It was shown that the toxicity interactions between DMSO and pesticide were dominated by antagonism, and the highest antagonism distributed between -23% and -15%. The concentration ranges where antagonism existed and the degree of antagonism were influenced by the components in the mixture, the concentration ratios of the components, and the effect level. A comparison of the MERA with the conventional isobologram and the extended toxic unit summation revealed that the MERA characterizes the degree of toxicity interaction in the view of effect, with less limitation by different concentration ratios or effect levels. Therefore, the MERA can be used to evaluate the complex toxicity interactions taking place in binary mixtures. PMID:23487948

  14. Multi-class, multi-residue analysis of pesticides, polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenyl ethers and novel flame retardants....mass spectrometry

    A multi-class, multi-residue method for the analysis of 13 novel flame retardants, 18 representative pesticides, 14 polychlorinated biphenyl (PCB) congeners, 16 polycyclic aromatic hydrocarbons (PAHs), and 7 polybrominated diphenyl ether (PBDE) congeners in catfish muscle was developed and evaluated...

  15. Pesticide Instrumental Analysis

    This workshop was the evaluation of the pesticides impact on the vegetable matrix with the purpose to determine the analysis by GC / M S. The working material were lettuce matrix, chard and a mix of green leaves and pesticides.

  16. Pesticides residue levels in selected fruits from some Ghanaian markets

    The amount of some pesticide residues in fruits was monitored at five (5) Accra Metropolis markets. Locally produced fruits (pawpaw and tomato) and imported apples were purchased from two supermarkets and three urban markets in Accra metropolis and analyzed by gas chromatography equipped with electron capture detector for pesticide residues. A total of 220 samples of fruits were extracted and analyzed for pesticide residues, mainly organochlorines (γ-HCH, δ-HCH, aldrin, heptachlor, γ-chlordane, heptachlor epoxide, α-endosulfan, p,p'-DDE, endrin, β-endosulfan, o,p'-DDT, endrin aldehyde, p,p'- DDT, endrin ketone and methoxychlor). The data showed that most of the fruit samples analyzed contain residues of the monitored pesticides above the accepted maximum residue limit (MRL) as adopted by the FAO/WHO Codex Alimentarius Commission (CAC). The results obtained showed that 38.6 % fruit samples showed results above the MRL, 48.7 % were below the MRL and 12.7 % contained no detectable level of the monitored pesticides. Data analysis of health risk estimates indicated that, particularly γ-HCH, δ-HCH, o,p'-DDT, p,p'-DDE or p,p'-DDT do not pose a direct hazard to human health, although present in the three fruits (pawpaw, tomato and apple). However, heptachlor, heptachlor epoxide, endrin aldehyde, and endrin ketone levels exceeded the reference dose, indicating a great potential for systemic toxicity, especially in children who are considered to be the most vulnerable population subgroup. Lastly, the public is aware of pesticide residues in fruits and advocates for the curtailing of pesticide use on horticulture produce or strong educational programmes for farmers on control and safer use of pesticides. (au)

  17. Planar solid phase extraction clean-up and microliter-flow injection analysis-time-of-flight mass spectrometry for multi-residue screening of pesticides in food.

    Oellig, Claudia; Schwack, Wolfgang

    2014-07-18

    For multi-residue analysis of pesticides in food, a sufficient clean-up is essential for avoiding matrix effects in liquid and gas chromatography (LC and GC) analysis coupled to mass spectrometry (MS). In the last two years, high-throughput planar solid phase extraction (HTpSPE) was established as a new clean-up concept for pesticide residue analysis in fruits and vegetables (C. Oellig, W. Schwack, 2011) and tea (C. Oellig, W. Schwack, 2012). HTpSPE results in matrix-free extracts almost free of interferences and matrix effects. In this study, a time-of-flight mass spectrometer (TOFMS) was applied to directly analyze HTpSPE extracts for pesticide residues. This HTpSPE-microliter-flow injection analysis (μL-FIA)-TOFMS approach detects all pesticides at once in a single mass spectrum, without a liquid chromatographic separation step. Complete sample information was obtained after the injection of the cleaned extract within a single peak. Recovery studies for seven representative pesticides in four different matrices (apples, red grapes, cucumbers, tomatoes) provided mean recoveries of 86-116% with relative standard deviations of 1.3-10% (n=5) using the mass signal intensities under the entire sample peak. Comparing the mass spectra of sample peaks from spiked extracts and solvent standards indicated the efficiency of HTpSPE clean-up. A pesticide database search detected all spiked pesticides with a low incidence of false-positives. HTpSPE of one sample required a few minutes, and numerous samples could be cleaned in parallel at minimal cost with low sample and solvent consumption. The μL-FIA-TOFMS screening then needed an additional 6min per sample. The novel screening approach was successfully applied to QuEChERS extracts of several real samples, and the pesticides identified by HTpSPE-μL-FIA-TOFMS were identical to the pesticides detected by common target LC-MS/MS analyses. The high degree of concordantly identified pesticides by the new developed HTpSPE-μL-FIA-TOFMS approach and target LC-MS/MS demonstrates the applicability as a routine screening method. PMID:24877980

  18. Assessment of pesticide residues on selected vegetables of Pakistan

    The present study was conducted to determine the pesticide residues on selected summer vegetables. Five vegetables were grown with three replicates in a split plot randomized complete block design. Pesticides were sprayed on vegetables thrice at regular intervals each after 15 days. At maturity the pesticides residues were extracted from edible and leaf portions using anhydrous sodium sulfate and ethyl acetate while adsorption chromatography technique was used for cleanup. The extracts were subjected to high performance liquid chromatography (HPLC) for separation and analysis of the compounds. Significant differences (p<0.05) were found in the pesticides residues on edible portions whereas highly significant differences (p<0.001) were observed for the leafy portions. The residual level of cypermethrin was highest (16.2 mg kg/sup -1/) in edible portion of bitter gourd, while Lambdacyhalothrin and Mancozeb residues were detected high (4.50 mg kg/sup -1/, 6.26 mg kg/sup -1/) in edible portion of bitter gourd and Cucumber respectively. Cypermethrin residues were high (1.86 mg kg/sup -1/) in Okra leaves. Mancozeb and Lambdacyhalothrin residual level was high (1.23 mg kg/sup -1/, and 0.0002 mg kg/sup -1/) in chili and tomato leaves. Cypermethrin residues were readily detected in edible and leaf portion of the selected vegetables. (author)

  19. Analysis of pesticide residues in Brazilian medicinal plants: matrix solid phase dispersion versus conventional (European Pharmacopoeia) methods

    Zuin Vânia G.; Yariwake Janete H.; Lanças Fernando M.

    2003-01-01

    This paper proposes a method based on matrix solid phase dispersion (MSPD) to determine the presence of organochlorine (OC) and organophosphorus (OP) pesticide residues in species of Passiflora L. (passion fruit) leaves by gas chromatography, using an electron capture detector (HRGC-ECD). A comparison with conventional methods, mainly the European Pharmacopoeia method (EP), showed MSPD to be efficient, fast, simple and easy to perform. To date, there are no official methods or limits that tak...

  20. 7 CFR 29.427 - Pesticide residue standards.

    2010-01-01

    ... 7 Agriculture 2 2010-01-01 2010-01-01 false Pesticide residue standards. 29.427 Section 29.427... REGULATIONS TOBACCO INSPECTION Regulations Miscellaneous § 29.427 Pesticide residue standards. The maximum concentration of residues of the following pesticides allowed in flue-cured or burley tobacco, expressed...

  1. Headspace solid phase microextraction in the analysis of pesticide residues – kinetics and quantification prior to the attainment of partition equilibrium

    DRAGAN MARKOVIC

    2007-08-01

    Full Text Available A new theoretical approach to the headspace/solid phase microextraction (HS/SPME process is proposed and tested by the analysis of pesticide residues of water samples. The new approach focuses on mass transfer at the sample/gas phase and gas phase/SPME polymer interfaces. The presented model provides a directly proportional relationship between the amount of analytes sorbed by the SPME fiber and their initial concentrations in the sample. Also, the expression indicates that quantification is possible before partition equilibrium is attained. Experimental data for pesticides belonging to various classes of organic compounds were successfully interpreted by the developed model. Additionally, a linear dependence of the amount of pesticide sorbed on the initial analyte concentration in aqueous solution was obtained for a sampling time shorter than that required to reach sorption equilibrium.

  2. Multi-residue method for the analysis of 85 current-use and legacy pesticides in bed and suspended sediments

    Smalling, K.L.; Kuivila, K.M.

    2008-01-01

    A multi-residue method was developed for the simultaneous determination of 85 current-use and legacy organochlorine pesticides in a single sediment sample. After microwave-assisted extraction, clean-up of samples was optimized using gel permeation chromatography and either stacked carbon and alumina solid-phase extraction cartridges or a deactivated Florisil column. Analytes were determined by gas chromatography with ion-trap mass spectrometry and electron capture detection. Method detection limits ranged from 0.6 to 8.9 ??g/kg dry weight. Bed and suspended sediments from a variety of locations were analyzed to validate the method and 29 pesticides, including at least 1 from every class, were detected.

  3. Clean up of pesticide residues by Gel- Permeation chromatography

    Use of the semi-automatic gel chromatographic system, Type : KL-SX-3 ( GPC) was evaluated for pesticide residue analysis. The clean up procedure was found efficient for large column use (28 mm id. x 20 cm). Recoveries of linuron and pirimiphos-methyl were found 84.3 and 79.8 percent respectively. Fat and pesticide contents are clearly separable. About eighty percent of DDT (88.8%), 91.4% of carbaryl and 98% of carbofuran were recovered in 80-190 ml of cyclohexane-dichloromethane 1 : 1 eluent. In the small column more than 70% of pesticides come out in the initial fractions ( 0-30 ml) of eluent. From this study it is thus concluded that GPC (KL-SX-C) with large column is suitable to separate pesticides from fat and other co-extracts from grain samples, but small column technique is of limited use. (author)

  4. Requiring Pollutant Discharge Permits for Pesticide Applications that Deposit Residues in Surface Waters

    Terence Centner

    2014-05-01

    Full Text Available Agricultural producers and public health authorities apply pesticides to control pests that damage crops and carry diseases. Due to the toxic nature of most pesticides, they are regulated by governments. Regulatory provisions require pesticides to be registered and restrictions operate to safeguard human health and the environment. Yet pesticides used near surface waters pose dangers to non-target species and drinking water supplies leading some governments to regulate discharges of pesticides under pollution discharge permits. The dual registration and discharge permitting provisions are burdensome. In the United States, agricultural interest groups are advancing new legislation that would exempt pesticide residues from water permitting requirements. An analysis of the dangers posed by pesticide residues in drinking water leads to a conclusion that both pesticide registration and pollutant discharge permitting provisions are needed to protect human health and aquatic species.

  5. [Analysis of 112 pesticide residues in vegetables using dispersive-solid phase extraction and gas chromatography-triple quadrupole mass spectrometry].

    Shi, Jiawei; Li, Jige; Wang, Yufei; Fan, Jianzhong

    2012-06-01

    A method was developed and validated for the simultaneous analysis of 112 pesticide residues in vegetables by gas chromatography coupled with triple quadrupole mass spectrometry (GC-QQQ-MS/MS). It is demonstrated that the optimized conditions could provide a more accurate quantitation and lower limit of quantification of the analysis by dispersive-solid phase extraction (D-SPE) cleanup. The samples were extracted with acetonitrile and toluene (8: 1, v/v), and cleaned up by D-SPE. To every 5 mL extraction solution, 0.8 g MgSO4, 0.05 g graphitized carbon black (GCB), 0.1 g ethylenediamine-N-propyl silyl (PSA) and 0.05 g C18 were added. The extracts were analyzed by GC-QQQ-MS/MS using internal standard method. The recoveries of the 112 pesticides at three spiked levels of 20, 50 and 200 microg/kg were ranged from 53.1% to 138.7%, and among which those of 86 pesticides were from 65.0% to 120.0%. The relative standard deviations (RSD) were less than 12%. The limits of quantifications (LOQs) (signal/noise at 10) were between 1.6 and 13.4 microg/kg. The vegetable samples collected from the market such as garlic chives, cucumber and purple cabbage were analyzed, and the residues of triazophos and fenpropathrin were detected in some of these samples. The method can be applied to the routine analysis for the determination of the 112 pesticides in vegetable samples. PMID:23016295

  6. Progress on multi-residue determination of pesticides in food

    ZHU Pan

    2013-02-01

    Full Text Available Food safety is important for the national economy and the people’s livelihood. Development of new analytical techniques and risk assessment for pesticide residues in foods are beneficial for risk management, risk communication and the health of consumer. This paper reviewed the new sample pretreatment techniques, pesticide multi-residue detection technologies and its applications, to provide certain reference for the development and improvement of pesticide residues detection and risk assessment in food.

  7. Determination of pesticide residues in olives by liquid extraction surface analysis followed by liquid chromatography/tandem mass spectrometry

    Gómez-Almenar, M. C.

    2015-06-01

    Full Text Available Nowadays, pesticides are essential in modern agriculture for crop protection, however, this use supposes a potential risk for human health and the environment. Traditional techniques of pesticide determination require the use of laborious and complex extraction methods to separate pesticides from the matrix, above all in fatty matrices like olives. For this reason, a new simple, rapid, cheap and selective method for the extraction and quantification of the most frequently used pesticides in olive growing has been developed. Pesticide determination was carried out by ultra-performance liquid chromatography (UPLC coupled with triple-quadrupole tandem mass spectrometry (MS/MS. Mean recoveries were found in a range between 73 and 114% with relative standard deviations lower than 20% in most pesticides evaluated and the limits of detection (LODs and quantification (LOQs were lower than 4 μg· kg-1 and 8 μg· kg-1, respectively. Finally, this method was applied to the analysis of 25 olive samples where Dimethoate and Terbuthylazine were detected in some cases, but their results were lower than 15 μg· kg-1.Hoy en día los pesticidas son esenciales en la agricultura moderna para la protección de los cultivos pero su uso supone un riesgo para la salud y el medio ambiente. Las técnicas tradicionales de determinación de pesticidas requieren el uso de métodos de extracción complejos a fin de separar los pesticidas de la matriz, sobre todo en matrices grasas como las aceitunas. Por ello, se ha desarrollado un nuevo método simple, rápido, barato y selectivo para la extracción y cuantificación de los pesticidas más frecuentemente utilizados en el cultivo del olivo, empleando cromatografía líquida de ultra-resolución (UPLC acoplada a espectrometría de masas (MS/MS. Las recuperaciones alcanzadas variaron entre el 73 y 114% obteniendo desviaciones estándar relativas inferiores al 20%. Los límites de detección (LD y cuantificación (LQ fueron inferiores a 4 y 8 μg·kg −1, respectivamente. Finalmente, este método fue aplicado en 25 muestras de aceitunas donde se detectaron Dimetoato y Terbutilazina en algunos casos pero con valores inferiores a 15 μg·kg−1.

  8. Determination of organophosphorus pesticide residues in tomatoes by gas chromatography

    Chloropyriphos and malathion are two organophosphorus pesticides from many others pesticides widely used by famers in agriculture .Because of their bad effect on human health, officials standards are set by the international organisations and communities to ensure safer food for consumer .In the same way, scientists over the world are working hard to develop new detection techniques responding to the international requirements. In this study, an ' IAEA-ethylacetate method ', an adaptation of the popular QuEChERS multi residue method, was optimized to analyse chloropyriphos and Malathion residues in tomatoes .Ethyl-Acetate was used as an extraction solvent the PSA was kept for the clean up procedure. GC-NPD is used for samples analysis .The method optimized is specifique, selective with a recovery averaged more than 70 pour cent. A complete validation of the method is necessary to be used for routine analysis.

  9. Review of analytical methods for the determination of pesticide residues in grapes.

    Grimalt, Susana; Dehouck, Pieter

    2016-02-12

    This review presents an overview of analytical methods for the analysis of pesticide residues in grapes and by-products in the last decade. The most widely used detection technique for the determination of pesticides in grapes is mass spectrometry combined with gas and/or liquid chromatography. In general, multi-residue methods with selective sample treatment methodologies have been developed for this purpose. However, this review focuses not only on these common multi-residue methods but also on specific methodologies as single-residue methods for the analysis of pesticides in grapes and by-products. Finally, the limitations of multi-residue methods, the future perspectives and the trends for pesticide residue analysis in grapes are reviewed. PMID:26803907

  10. Distribution of multiple pesticide residues in apple segments after home processing

    Rasmussen, Rie Romme; Poulsen, Mette Erecius; Hansen, H. C. B.

    2003-01-01

    The effects of washing, storing, boiling, peeling, coring and juicing on pesticide residue were investigated for field-sprayed Discovery and Jonagold apples. Residues of chlorpyrifos, cypermethrin, deltamethrin, diazinon, endosulfan, endosulfan sulfate, fenitrothion, fenpropathrin, iprodione......, kresoxim-methyl, lambda-cyhalothrin, quinalphos, tolylfluanid and vinclozolin in the processed apples were analysed by gas chromatography. Statistical analysis showed that reductions of 18-38% were required to obtain significant effects of processing practices, depending on pesticide and apple variety....... Juicing and peeling the apples significantly reduced all pesticide residues. In the case of detectable pesticide residues, 1-24% were distributed in the juice and in the peeled apple. None of the pesticide residues was significantly reduced when the apples were subject to simple washing or coring. Storing...

  11. Determination of pesticide residues in olives by liquid extraction surface analysis followed by liquid chromatography/tandem mass spectrometry

    Gómez-Almenar, M. C.; García-Mesa, J. A.

    2015-01-01

    Nowadays, pesticides are essential in modern agriculture for crop protection, however, this use supposes a potential risk for human health and the environment. Traditional techniques of pesticide determination require the use of laborious and complex extraction methods to separate pesticides from the matrix, above all in fatty matrices like olives. For this reason, a new simple, rapid, cheap and selective method for the extraction and quantification of the most frequently used pesticides in o...

  12. Determination of Pesticide Residues in Fresh and Greenhouse Vegetables

    M.H. Azizi

    2008-04-01

    Full Text Available Regarding the public concerns about serious health risks from pesticide, the occurrences of 105 pesticide residues including Organochlorine, Organophosphorus, Organonitrogen, Dicarboximides, Strobilurin, Triazine, Pyrethroids were assessed using a descriptive method in 25 fresh and greenhouse vegetable samples (fresh carrot, greenhouse tomato and cucumber. Ethyl acetate was used for extraction of pesticides from samples and the extract was cleaned up by Envicarb Solid Phase Extraction column chromatography. Pesticide residues were identified and quantified using gas chromatography ion trap mass spectrometry detector. The mean recoveries and limit of detection of the pesticides in samples were respectively 61.67-117% and the reproducibility of relative standard deviation values for the pesticides was 3.49-14.55%. Our data demonstrated that 80% of the total analyzed samples contained detectable residues including trifluralin, permethrin, chlorpyrifos, fenvalerate, fenpropathrin and iprodione, which were below the accepted maximum residue limits (MRLS adopted by FAO/WHO Codex Commision Alimentarius.

  13. Types of pesticides and determination of their residues

    The pesticide is any material or component used to protect from pests. Its toxic effect is related to the chemical structure, which can be divided into 3 types : 1- Metal pesticides : Sulphur, cupper, zinc, mercury; 2- Vegetal pesticides : advanced and less toxic to the general health; 3- Synthetic organo pesticides : organo chlorine, organophosphorous, carbamate and pyrethroids. Pesticides in the soil undergo biological dissociation according to their concentration and chemical structure. High concentration of the pesticides in the soil may lead to fertility decrease due to destruction of micro-organisms by the pesticides. Many methods are used to analyze the residues of pesticides in plant or soil : 1- Chromatographic methods : Gas chromatography, gas liquid chromatography and high performance liquid chromatography; 2- Spectroscopy methods : spectrophotometer and mass spectrometer; 3- Isotopic methods : based on tracers technique which is the most sensitive and accurate method and can estimate minor amounts of the pesticides. (author)

  14. Multivariate analysis of nutritional information of foodstuff of plant origin for the selection of representative matrices for the analysis of pesticide residues.

    da Silva, Ricardo Jorge Neves Bettencourt; Cames, Maria Filomena Gomes Ferreira Crujo

    2010-07-26

    Testing safety of foodstuffs of plant origin involves the analysis of hundreds of pesticide residues. This control is only cost-effective through the use of methods validated for the analysis of many thousands of analyte/matrix combinations. Several documents propose representative matrices of groups of matrices from which the validity of the analytical method can be extrapolated to the represented matrices after summarised experimental check of within group method performance homogeneity. Those groups are based on an evolved expert consensus based on the empirical knowledge on the current analytical procedures; they are not exhaustive, they are not objectively defined and they propose a large list of representative matrices which makes their application difficult. This work proposes grouping 240 matrices, based on the nutritional composition pattern equivalence of the analytical portion right after hydration and before solvent extraction, aiming at defining groups that observe method performance homogeneity. This grouping was based on the combined outcome of three multivariate tools, namely: Principal Component Analysis, Hierarchical Cluster Analysis and K-Mean Cluster Analysis. These tools allowed the selection of eight groups for which representative matrices with average characteristics and objective criteria to test inclusion of new matrices were established. The proposed matrices groups are homogeneous to nutritional data not considered in their definition but correlated with the studied multivariate nutritional pattern. The developed grouping that must be checked with experimental test before use was tested against small deviations in food composition and for the integration of new matrices. PMID:20638493

  15. Multivariate analysis of nutritional information of foodstuff of plant origin for the selection of representative matrices for the analysis of pesticide residues

    Testing safety of foodstuffs of plant origin involves the analysis of hundreds of pesticide residues. This control is only cost-effective through the use of methods validated for the analysis of many thousands of analyte/matrix combinations. Several documents propose representative matrices of groups of matrices from which the validity of the analytical method can be extrapolated to the represented matrices after summarised experimental check of within group method performance homogeneity. Those groups are based on an evolved expert consensus based on the empirical knowledge on the current analytical procedures; they are not exhaustive, they are not objectively defined and they propose a large list of representative matrices which makes their application difficult. This work proposes grouping 240 matrices, based on the nutritional composition pattern equivalence of the analytical portion right after hydration and before solvent extraction, aiming at defining groups that observe method performance homogeneity. This grouping was based on the combined outcome of three multivariate tools, namely: Principal Component Analysis, Hierarchical Cluster Analysis and K-Mean Cluster Analysis. These tools allowed the selection of eight groups for which representative matrices with average characteristics and objective criteria to test inclusion of new matrices were established. The proposed matrices groups are homogeneous to nutritional data not considered in their definition but correlated with the studied multivariate nutritional pattern. The developed grouping that must be checked with experimental test before use was tested against small deviations in food composition and for the integration of new matrices.

  16. Pesticide residues and bees--a risk assessment.

    Sanchez-Bayo, Francisco; Goka, Koichi

    2014-01-01

    Bees are essential pollinators of many plants in natural ecosystems and agricultural crops alike. In recent years the decline and disappearance of bee species in the wild and the collapse of honey bee colonies have concerned ecologists and apiculturalists, who search for causes and solutions to this problem. Whilst biological factors such as viral diseases, mite and parasite infections are undoubtedly involved, it is also evident that pesticides applied to agricultural crops have a negative impact on bees. Most risk assessments have focused on direct acute exposure of bees to agrochemicals from spray drift. However, the large number of pesticide residues found in pollen and honey demand a thorough evaluation of all residual compounds so as to identify those of highest risk to bees. Using data from recent residue surveys and toxicity of pesticides to honey and bumble bees, a comprehensive evaluation of risks under current exposure conditions is presented here. Standard risk assessments are complemented with new approaches that take into account time-cumulative effects over time, especially with dietary exposures. Whilst overall risks appear to be low, our analysis indicates that residues of pyrethroid and neonicotinoid insecticides pose the highest risk by contact exposure of bees with contaminated pollen. However, the synergism of ergosterol inhibiting fungicides with those two classes of insecticides results in much higher risks in spite of the low prevalence of their combined residues. Risks by ingestion of contaminated pollen and honey are of some concern for systemic insecticides, particularly imidacloprid and thiamethoxam, chlorpyrifos and the mixtures of cyhalothrin and ergosterol inhibiting fungicides. More attention should be paid to specific residue mixtures that may result in synergistic toxicity to bees. PMID:24718419

  17. Organophosphorus pesticides residues in Italian raw milk.

    Pagliuca, Giampiero; Serraino, Andrea; Gazzotti, Teresa; Zironi, Elisa; Borsari, Andrea; Rosmini, Roberto

    2006-08-01

    Organophosphorus pesticides (OPPs), widely used in agriculture, can cause toxic effects to humans and animals. The main purpose of the present work was to determine the contamination in raw milk by the main organophosphorus pesticides used in Italy and to evaluate the opportunity to start specific procedures of risk management along the milk production chain. The samples, collected in 4 Italian dairy plants directly from the tank trucks during the delivering, were representative of 920 tonnes of raw milk. The isolation of the OPPs (acephate, chlorpyriphos, chlorpyriphos-methyl, diazinon, methamidophos, methidathion, phorate, pirimiphos-methyl) was performed by liquid partition followed by clean-up with solid phase extraction. The analyses were carried out by dual column gas chromatography using two nitrogen-phosphorus detectors. Among the 135 samples analysed, 37 were positive in traces and 10 showed an OPP contamination ranging from 5 to 18 microg/kg. The higher results were recorded in the samples collected during the autumn-winter period. The main pollutants detected were acephate and chlorpyriphos. In every positive sample found, the OPP contamination was lower than the maximum residue level (MRL) fixed by the European Commission. PMID:16566853

  18. Determination of pesticide residues in cereal grains

    The applicability of the TLC for determination of pesticide residues in cereal grains was studied using corn, rice and wheat as representative commodities and atrazine, captan, chlorpyrifos, chlortoluron, diazinon, diuron, fenitrothion, metoxuron, prochloraz, triforine as representative compounds. Following the extraction with ethyl acetate the efficiency of extraction was tested with Bio-Rad SX-3 gel, GPC, silica gel, florisil and RP-18 reverse phase silica cartridge. The GPC alone or in combination with silica or florisil cleanup were the most suitable for cleanup of the extracts. The TLC elution characteristics of 131 pesticide active ingredients were tested with eight elution systems. The detectability of the selected compounds was determined with six detection methods including two chemical and four bioassay procedures. In addition to the basic methods, the non-toxic Penicillium cyclopium fungi spore inhibition was introduced and it was found very sensitive for some fungicide compounds. The minimum detectable quantities of the tested compounds ranged from 1 ng to 100 ng. The average recoveries from rice and wheat ranged from 78% to 89%, and the limits of quantitation, LOQ, were between 0.01 and 0.2 mg/kg for the selected ten compounds. (author)

  19. 75 FR 80489 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-12-22

    ... AGENCY Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or... establishment or modification of regulations for residues of pesticide chemicals in or on various commodities... part 174 or part 180 for residues of pesticide chemicals in or on various food commodities. EPA...

  20. 75 FR 54629 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-09-08

    ... AGENCY Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or... establishment or modification of regulations for residues of pesticide chemicals in or on various commodities... part 174 or part 180 for residues of pesticide chemicals in or on various food commodities. EPA...

  1. 75 FR 46924 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-08-04

    ... AGENCY Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or... establishment or modification of regulations for residues of pesticide chemicals in or on various commodities... establishment or modification of regulations in 40 CFR part 174 or part 180 for residues of pesticide...

  2. 75 FR 57942 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-09-23

    ... AGENCY Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or... establishment or modification of regulations for residues of pesticide chemicals in or on various commodities... part 174 or part 180 for residues of pesticide chemicals in or on various food commodities. EPA...

  3. 75 FR 48667 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-08-11

    ... AGENCY Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or... establishment or modification of regulations for residues of pesticide chemicals in or on various commodities... part 174 or part 180 for residues of pesticide chemicals in or on various food commodities. EPA...

  4. 75 FR 65321 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-10-22

    ... AGENCY Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or... establishment or modification of regulations for residues of pesticide chemicals in or on various commodities... part 174 or part 180 for residues of pesticide chemicals in or on various food commodities. EPA...

  5. 76 FR 49396 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    2011-08-10

    ... AGENCY 40 CFR Parts 174 and 180 Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals... residues of pesticide chemicals in or on various commodities. DATES: Comments must be received on or before... part 180 for residues of pesticide chemicals in or on various food commodities. The Agency is...

  6. 76 FR 61647 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2011-10-05

    ... AGENCY 40 CFR Parts 174 and 180 Receipt of Several Pesticide Petitions Filed for Residues of Pesticide... for residues of pesticide chemicals in or on various commodities. DATES: Comments must be received on... part 174 or part 180 for residues of pesticide chemicals in or on various food commodities. The...

  7. 75 FR 60452 - Notice of Filing of Several Pesticide Petitions for Residues of Pesticide Chemicals in or on...

    2010-09-30

    ... AGENCY Notice of Filing of Several Pesticide Petitions for Residues of Pesticide Chemicals in or on... of regulations for residues of pesticide chemicals in or on various commodities. DATES: Comments must... part 180 for residues of pesticide chemicals in or on various food commodities. EPA has determined...

  8. 77 FR 63782 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on a Commodity

    2012-10-17

    ... AGENCY 40 CFR Part 180 Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on... pesticide petition requesting the establishment or modification of regulations for residues of pesticide...), requesting the establishment or modification of regulations in 40 CFR part 180 for residues of...

  9. 78 FR 1798 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    2013-01-09

    ... AGENCY 40 CFR Part 180 Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on... a pesticide petition requesting the establishment or modification of regulations for residues of... establishment or modification of regulations in 40 CFR part 180 for residues of pesticide chemicals in or...

  10. 77 FR 59576 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    2012-09-28

    ... AGENCY 40 CFR Part 180 Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on... a pesticide petition requesting the establishment or modification of regulations for residues of... establishment or modification of regulations in 40 CFR part 180 for residues of pesticide chemicals in or...

  11. 77 FR 26477 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    2012-05-04

    ... AGENCY 40 CFR Part 180 Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on... a pesticide petition requesting the establishment or modification of regulations for residues of... establishment or modification of regulations in 40 CFR part 174 or part 180 for residues of pesticide...

  12. A multi-residue method for pesticides analysis in green coffee beans using gas chromatography-negative chemical ionization mass spectrometry in selective ion monitoring mode.

    Pizzutti, Ionara R; de Kok, Andre; Dickow Cardoso, Carmem; Reichert, Bárbara; de Kroon, Marijke; Wind, Wouter; Weber Righi, Laís; Caiel da Silva, Rosselei

    2012-08-17

    In this study, a new gas chromatography-mass spectrometry (GC-MS) method, using the very selective negative chemical ionization (NCI) mode, was developed and applied in combination with a modified acetonitrile-based extraction method (QuEChERS) for the analysis of a large number of pesticide residues (51 pesticides, including isomers and degradation products) in green coffee beans. A previously developed integrated sample homogenization and extraction method for both pesticides and mycotoxins analysis was used. An homogeneous slurry of green milled coffee beans and water (ratio 1:4, w/w) was prepared and extracted with acetonitrile/acetic acid (1%), followed by magnesium sulfate addition for phase separation. Aliquots from this extract could be used directly for LC-MS/MS analysis of mycotoxins and LC-amenable pesticides. For GC-MS analysis, a further clean-up was necessary. C18- and PSA-bonded silica were tested as dispersive solid-phase extraction (d-SPE) sorbents, separate and as a mixture, and the best results were obtained using C18-bonded silica. For the optimal sensitivity and selectivity, GC-MS detection in the NCI-selected ion monitoring (SIM) mode had to be used to allow the fast analysis of the difficult coffee bean matrix. The validation was performed by analyzing recovery samples at three different spike concentrations, 10, 20 and 50 μg kg(-1), with 6 replicates (n=6) at each concentration. Linearity (r(2)) of calibration curves, estimated instrument and method limits of detection and limits of quantification (LOD(i), LOD(m), LOQ(i) and LOQ(m), respectively), accuracy (as recovery %), precision (as RSD%) and matrix effects (%) were determined for each individual pesticide. From the 51 analytes (42 parent pesticides, 4 isomers and 5 degradation products) determined by GC-MS (NCI-SIM), approximately 76% showed average recoveries between 70-120% and 75% and RSD ≤ 20% at the lowest spike concentration of 10 μg kg(-1), the target method LOQ. For the spike concentrations of 20 and 50 μg kg(-1), the recoveries and RSDs were even better. The validated LOQ(m) was 10, 20 and 50 μg kg(-1) for respectively 33, 3 and 6 of the analytes studied. For five compounds, the European Union method performance requirements for the validation of a quantitative method (average recoveries between 70-120% and repeatability RSD ≤ 20%) were not achieved and 4 problematic pesticides (captan, captafol, folpet and dicofol) could not be detected as their parent compound, but only via their degradation products. Although the matrix effect (matrix-enhanced detector response) was high for all pesticides studied, the matrix interference was minimal, due to the high selectivity obtained with the GC-NCI-MS detection. Matrix-matched calibration for applying the method in routine analysis is recommended for reliable quantitative results. PMID:22771261

  13. [Investigation of pesticide residues in foods distributed in Kitakyushu City].

    Ishikawa, Seiichi; Naetoko, Eri; Kawamura, Seiji; Yamaguchi, Rika; Higuchi, Masayuki; Kojima, Tsutomu; Yamato, Yasuhiro; Takahashi, Masaki

    2004-04-01

    We investigated 160 kinds of pesticide residues in 715 samples of 116 kinds of foods distributed in Kitakyushu city. Sixty kinds of pesticides were detected in 55 kinds of foods (204 samples) in the range of 0.002-22 mg/kg. Five kinds of pesticides in 7 samples violated the residue standards and the indication of "unused". The detection ratios of unregulated pesticide in domestic and imported foods were 27.8 and 33.0%, respectively. Iprodione, dicofol, diethofencarb, procymidone and chlorfenapyr (for domestic food) and total bromine, benomyl, chlorpyrifos, dicofol, fenvalerate, cypermethrin and dimethoate (for imported food) showed relatively high detection ratios. Chinese cabbage, garland chrysanthemum, tomatoes and green teas (domestic) and broccoli, bananas, grapefruit, lemons, oranges, frozen edamame and frozen kidney beans (imported) showed high relative pesticide detection ratios. Residual pesticides were detected with relatively high frequency in imported fruits, imported frozen foods and imported processed foods. PMID:15272606

  14. Fast analysis of multiple pesticide residues in apple juice using dispersive liquid-liquid microextraction and multidimensional gas chromatography-mass spectrometry.

    Cunha, S C; Fernandes, J O; Oliveira, M B P P

    2009-12-18

    A method for the rapid trace analysis of 24 residual pesticides in apple juice by multidimensional gas chromatography-mass spectrometry (MD-GC/MS) using dispersive liquid-liquid microextraction (DLLME) was developed and optimized. Several parameters of the extraction procedure such as type and volume of extraction solvent, type and volume of dispersive solvent and salt addition were evaluated to achieve the highest yield and to attain the lowest detection limits. The DLLME procedure optimized consists in the formation of a cloudy solution promoted by the fast addition to the sample (5 ml) of a mixture of carbon tetrachloride (extraction solvent, 100 microl) and acetone (dispersive solvent, 400 microl). The tiny droplets formed and dispersed among the aqueous sample solution are further joined and sedimented (85 microl) in the bottom of the conical test tube by centrifugation. Once extracted, all the 24 pesticides were directly injected and separated by a dual GC column system, comprising a short wide-bore DB-5 capillary column with low film thickness connected by a Deans switch system to a second chromatographic narrower column, with identical stationary phase. The instrumental setting used, in combination with carefully optimized operational fast GC and MS parameters, markedly decreased the retention times of the targeted analytes. The total chromatographic run was 8 min. Mean recoveries for apple juice spiked at three concentrations ranged from 60% to 105% and the intra-repeatability ranged from 1% to 21%. The limits of detection of the 24 pesticides ranged from 0.06 to 2.20 microg/L. In 2 of a total of 28 analysed samples were found residues of captan, although at levels below the maximum limit legal established. PMID:19896138

  15. Nuclear applications for pesticide residue studies

    Radiotracer techniques offer a powerful tool in understanding the fate of pesticides in soil, plant or food and can be utilised to take suitable corrective procedures to minimise the environmental effects of pesticides. 9 refs

  16. Determination of pesticide residues in fruit-based soft drinks.

    Garca-Reyes, Juan F; Gilbert-Lpez, Bienvenida; Molina-Daz, Antonio; Fernndez-Alba, Amadeo R

    2008-12-01

    Here we report the first worldwide reconnaissance study of the presence and occurrence of pesticides in fruit-based soft drinks. While there are strict regulations and exhaustive controls for pesticides in fruits, vegetables, and drinking water, scarce attention has been paid to highly consumed derivate products, which may contain these commodities as ingredients. In the case of the fruit-based soft drinks industry, there are no clear regulations, relating to pesticides, which address them, even when there is significant consumption in vulnerable groups such as children. In this work, we have developed a screening method to search automatically for up to 100 pesticides in fruit-based soft drinks extracts based on the application of liquid chromatography-electrospray time-of-flight mass spectrometry (LC-TOF MS). The sample extracts injected were obtained by a preliminary sample treatment step based on solid-phase extraction using hydrophilic-lipophilic balanced polymer-based reverse phase cartridges and methanol as eluting solvent. Subsequent identification, confirmation, and quantitation were carried out by LC-TOF MS analysis: the confirmation of the target species was based on retention time matching and accurate mass measurements of protonated molecules ([M + H]+) and fragment ions (obtaining accuracy errors typically lower than 2 ppm). With the proposed method, we measured over 100 fruit-based soft drink samples, purchased from 15 different countries from companies with brands distributed worldwide and found relatively large concentration levels of pesticides in most of the samples analyzed. The concentration levels detected were of the micrograms per liter level, low when considering the European maximum residue levels (MRLs) set for fruits but very high (i.e., 300 times) when considering the MRLs for drinking or bottled water. The detected pesticides (carbendazim, thiabendazole, imazalil and its main degradate, prochloraz and its main degradate, malathion, and iprodione) are mainly those applied to crops in the final stages of production (postharvest treatment), some of them contain chlorine atoms in their structures. Therefore, steps should be taken with the aim of removing any traces of pesticides in these products, in order to avoid this source of pesticide exposure on the consumer, particularly on vulnerable groups with higher exposure, such as children. PMID:19551973

  17. Note on pesticide residues as a function of formulation used

    The total quantities of pesticides needed for adequate pest control may be minimized by the correct choice of methods of formulation and application. This will diminish the total burden of residues in the environment but not necessarily in the crop. Radiolabelled pesticides are useful for small-scale and laboratory tests to elucidate the principles which determine the behaviour of pesticides in the environment and to check analytical methods used for field-scale tests. (author)

  18. Public Health Implications of Pesticide Residues in Meat

    Jadhav V.J. and Waskar V.S.

    2011-08-01

    Full Text Available Use of pesticides in India began in 1948 when DDT was imported for malaria control and BHC for locust control. Since then various synthetic pesticides are used for protection of crops and public health. The persistence nature of some of these pesticides led to their accumulation in animal tissues and subsequently causes human dietary exposure to these pesticides through consumption of animal products viz. meat, milk, eggs and seafoods. Scientific evidence suggest that even such low dose but long term exposure can cause serious health hazards to human health and environment as well. The reports on occurrence of pesticides residues in animal products manufactured in India are fragmentary, but provide confirmation to the fact Indian consumers do get dietary exposure to these pesticides. The role of Insecticide Act and Prevention of Food Adulteration Act enforced in India for judicious pesticide use and safety of consumers of animal products is discussed. [Vet. World 2011; 4(4.000: 178-182

  19. Bound pesticide residues in soils and plants and their determination

    To assess the environmental significance of pesticide residues in soil and plants one must distinguish between two types of residues: those that are extractable with solvents, and those residues that are not extractable with solvent. The extent of bound (non-extractable) residues varies with the plant and pesticide involved and generally increases with time after treatment Bound pesticide residues have been detected in the organic matter fractions of soil, i.e. humic acid, fulvic acid and humin. Several studies have shown that lignin, hemicellulose and pectic polysaccharide are the major bound residues fraction of pesticide in plants. Attempts have been made to extract bound pesticide residues by the milder to harsher methods. Drastic extractive procedures destroy the structure of soil or plants often results in the destruction of the identity of bound residues. The High Temperature Distillation (HTD) and Supercritical Fluid Extraction (SFE) techniques may provide possible means for extraction and identification of bound residues in food products. Regulatory agencies should also consider placing further emphasis on employing more effective extraction techniques and procedures to quantitatively remove bound residues

  20. Pesticide residues in brain tissues of dairy cattle in Lembang

    Indraningsih

    2006-03-01

    Full Text Available The use of pesticides to control plant diseases may cause residual formation in crops, its byproduct and environmental. Furthermore, the use of agriculture byproduct as animal feed may cause poisoning or residual formation in animal products. The purpose of this study is to investigate of pesticide residues in brain tissues of dairy cattle in relation to animal feed as a contamination source. Samples consisted of animal feeds (19 samples of fodder and 6 samples of feed, 31 samples of sera and 25 samples of brain tissues of dairy cattle collected from Lembang, West Java. Feeds and fodders were collected from dairy farms located in Lembang. Sera were directly collected from 31 heads of Frisien Holstein (FH cattle from the same location, while brain tissues of FH cattle were collected from a local animal slaughtering house. Pesticide residues were analysed using gas chromatography (GC. Both residues of organochlorines and organophosphates were detected from brain tissues with average residue concentration OP was 22.7 ppb and OC was 5.1 ppb and a total residue was 27.8 ppb. The pesticide residues in brain tissues are new information that should be taken into consideration since the Indonesian consumed this tissues as an oval. Although pesticides residue concentration was low, pathological changes were noted microscopically from the brain tissues including extracellular vacuolisation, focal necrosis, haemorrhages, dilatation of basement membrane without cellular infiltration. Both pesticide residues were also detected in sera, where OP (9.0 ppb was higher than OC (4.9 ppb. These pesticides were also detected in animal feeds consisting fodders and feeds. Residues of OP (12.0 ppb were higher than OC (1.8 ppb in feeds, but residues of OP (16.8 ppb were lower than OC (18.7 ppb in fodders. Although, pesticide residues in sera and brain tissues were below the maximum residue limits (MRL of fat, the presence of pesticides in brain tissues should be taken into consideration as their effects in brain lesions. There was a correlation between contaminant found in animal feeds and pesticide residues in sera and brain tissues of dairy cattle.

  1. ANALYSIS OF AGED IN-HOME CARPETING TO DETERMINE THE DISTRIBUTION OF PESTICIDE RESIDUES BETWEEN DUST, CARPET, AND PAD COMPARTMENTS

    This report presents results of a study to determine the distribution of pesticides, polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) between dust and carpet components in aged carpeting. Carpeting in eight homes in the Research Triangle Area, which...

  2. Analysis of Trends of the Types of Pesticide Used, Residues and Related Factors among Farmers in the Largest Vegetable Producing Area in the Philippines

    Lu, Jinky Leilanie

    2010-01-01

    The objective of study is to provide an analysis of data trends on the type of pesticide used, exposure factors, and the pesticide-related concerns among the farmers from 2005 to 2010 in one of the largest vegetable producing areas in the Philippines. This is to determine and analyze changes that have occurred for the last five years in order to provide necessary basis in promoting safe usage of pesticides. It is shown in the studies that the most commonly used type of pesticide was Tamaron (...

  3. 76 FR 69692 - Withdrawal of a Pesticide Petition for Residues of Pesticide Chemicals in or on Various Commodities

    2011-11-09

    ... 23, 2010 (75 FR 57942) (FRL-8845-4), which announced the submission of a pesticide petition (PP... AGENCY 40 CFR Part 180 Withdrawal of a Pesticide Petition for Residues of Pesticide Chemicals in or on... establishment or modification of regulations for residues of pesticide chemicals in or on various...

  4. Removal of trace pesticide residues from farm produce

    In view of current food production practices, we must accept the fact that small quantities of pesticide residues will be present in our food supply. The significance of minute quantities of these chemical residues in food over an extended period of time is much debated question and has become a problem for man to face in controlling the total insult to his environment. Tolerance of pesticide residues in food are occasionally revised, some being revised downward. Against this background, it becomes obvious that the effects of processing chemical residues in food is an area where available information should be consolidated and missing information obtained through further research. This is particularly important for developing countries where 'persistent' pesticides are in use and where farmers treat crops with exaggerated quantities of pesticide chemicals to guarantee yields, rmoval of, residues in food processing is affected by type of food, insecticide type; and nature and severity of processing procedure used. Examples of processing methods include peeling; washing, hot water blanching, cooking, canning, chemical and physical treatments for oil refinement, processing of grain into flour and bread, milk into cream and cheese, etc. Removal of pesticide residues is usually incidental to the processing operation. In the present paper the effect of washing and peeling on the decontamination of pesticide residue in mangoes are discussed. (author)

  5. 78 FR 16243 - Codex Alimentarius Commission: Codex Committee on Pesticide Residues (CCPR)

    2013-03-14

    ... on Pesticide Residues (CCPR) AGENCY: Office of the Under Secretary for Food Safety, USDA. ACTION... at the 45th Session of the Codex Committee on Pesticide Residues (CCPR) of the Codex Alimentarius... Committee on Pesticide Residues is responsible for establishing maximum limits for pesticide residues...

  6. Rapid analysis of multiple pesticide residues in fruit-based baby food using programmed temperature vaporiser injectionlow pressure gas chromatographyhigh-resolution time-of-flight mass spectrometry

    A rapid method using programmed temperature vaporizer injectionlow-pressure gas chromatographyhigh-resolution time-of-flight mass spectrometry (PTVLP-GCHRTOFMS) for the analysis of multiple pesticide residues in fruit-based baby food was developed. The fast and inexpensive buffered QuEChERS ext...

  7. SPE Combined with HPLC-APCI-MS Analysis of Pesticides in Water: Method Performance and Application in a Reconnaissance Survey of Residues in Drinking Water in Greater Cairo (Egypt)

    The portability, ease of use, and potential to enhance analyte stability makes solid-phase extraction (SPE) an attractive technique for extracting water samples collected for pesticide residue analysis prior to their shipment to analytical laboratories. The technique is especially valuable when samp...

  8. Variability of matrix effects in liquid and gas chromatography - mass spectrometry analysis of pesticide residues after QuEChERS sample preparation of different food crops

    Gas and liquid chromatography (GC and LC) coupled to sophisticated mass spectrometry (MS) instruments are among the most powerful analytical tools currently available to monitor pesticide residues in food, among other applications. However, both GC-MS and LC-MS are susceptible to matrix effects whi...

  9. 78 FR 70906 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    2013-11-27

    ... AGENCY 40 CFR Part 180 Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on... residues of pesticide chemicals in or on various commodities. DATES: Comments must be received on or before...), requesting the establishment or modification of regulations in 40 CFR part 180 for residues of...

  10. Application of gas chromatography time-of-flight mass spectrometry for target and non-target analysis of pesticide residues in fruits and vegetables.

    Cervera, M I; Portols, T; Pitarch, E; Beltrn, J; Hernndez, F

    2012-06-29

    In this work, the capability of gas chromatography coupled to time-of-flight mass spectrometry (GC-TOF MS) for quantitative analysis of pesticide residues has been evaluated. A multiclass method for rapid screening of pesticides (insecticides, acaricides, herbicides and fungicides) in fruit and vegetable matrices has been developed and validated, including detection, identification and quantification of the analytes. To this aim, several food matrices were selected: high water content (apples, tomatoes and carrots), high acid content (oranges) and high oil content (olives) samples. The well known QuEChERS procedure was applied for extraction of pesticides, and matrix-matched calibration using relative responses versus internal standard was used for quantification. The sample extracts were analyzed by GC-TOF MS. Up to five ions using narrow window (0.02 Da)-extracted ion chromatograms at the expected retention time were monitored using a target processing method. The most abundant ion was used for quantification while the remaining ones were used for confirmation of the analyte identity. Method validation was carried out for 55 analytes in the five sample matrices tested at three concentrations (0.01, 0.05 and 0.5 mg/kg). Most recoveries were between 70% and 120% with relative standard deviations (RSDs) lower than 20% at 0.05 and 0.5mg/kg. At 0.01 mg/kg, roughly half of the pesticides could be satisfactorily validated due to sensitivity limitations of GC-TOF MS, which probably affected the ion ratios used for confirmation of identity. In the case of olive samples, results were not satisfactory due to the high complexity of the matrix. An advantage of TOF MS is the possibility to perform a non-target investigation in the samples by application of a deconvolution software, without any additional injection being required. Accurate-mass full-spectrum acquisition in TOF MS provides useful information for analytes identification, and has made feasible in this work the discovery of non-target imazalil, fluoranthene and pyrene in some of the samples analyzed. PMID:22608778

  11. Influence of different disease control pesticide strategies on multiple pesticide residue levels in apple

    Poulsen, Mette Erecius; Naef, A.; Gasser, S.; Christen, D.; Rasmussen, Peter Have

    Seven pesticide application strategies were investigated to control apple scab (Venturia inaequalis) and powdery mildew (Podosphaera leucotricha) and, at the same time.. fulfil the new quality standards implemented by some German retailers. These demand that pesticide residues should be below 80...

  12. Food safety in Thailand 2: Pesticide residues found in Chinese kale (Brassica oleracea), a commonly consumed vegetable in Asian countries.

    Wanwimolruk, Sompon; Kanchanamayoon, Onnicha; Phopin, Kamonrat; Prachayasittikul, Virapong

    2015-11-01

    There is increasing public concern over human health risks associated with extensive use of pesticides in agriculture. Regulation of pesticide maximum residue limits (MRLs) in food commodities is established in many developed countries. For Thailand, this regulation exists in law but is not fully enforced. Therefore, pesticide residues in vegetables and fruits have not been well monitored. This study investigated the pesticide residues in Chinese kale, a commonly eaten vegetable among Asians. The Chinese kale samples (N = 117) were purchased from markets in Nakhon Pathom Province, Thailand, and analyzed for the content of 28 pesticides. Analysis was performed by the multiresidual extraction followed by GC-MS/MS. Of pesticides investigated, 12 pesticides were detected in 85% of the Chinese kale samples. Although carbaryl, deltamethrin, diazinon, fenvalerate and malathion were found in some samples, their levels were lower than their MRLs. However, in 34 samples tested, either carbofuran, chlorpyrifos, chlorothalonil, cypermethrin, dimethoate, metalaxyl or profenofos was detected exceeding their MRLs. This represents a 29% rate of pesticide detection above the MRL; a rate much higher than in developed countries. Washing vegetables under running water significantly reduced (p residues by 55%. The running water method did not significantly decrease cypermethrin residues in the samples but washing with vinegar did. Our research suggests that routine monitoring of pesticide residues is necessary to reduce the public health risks associated with eating contaminated vegetables. Washing vegetables before consumption is advisable as this helps to reduce the level of pesticide residues in our daily intake. PMID:26093223

  13. [Pesticide residual status in litchi orchard soils in Guangdong, China].

    Yao, Li-Xian; Huang, Lian-Xi; Li, Guo-Liang; He, Zhao-Huan; Zhou, Chang-Min; Yang, Bao-Mei; Guo, Bin

    2010-11-01

    Litchi is a famous tropical and subtropical fruit originated in South China. Guangdong is one of the most important litchi production areas in China. Two hundred and eight soil samples were collected in litchi orchards after harvesting the fruit, in which nine often-used pesticides including metalaxyl, mancozeb, carbendazim, deltamethrin, cypermethrin, cyhalothrin, dipterex, dimethoate and dichlorvos were detected. The results showed that the detectable rates of various pesticides were ranked cypermethrin (59.1%) > carbendazim (51.0%) > mancozeb (11.1%) > metalaxyl (6.7%) > cyhalothrin (3.4%). Dimethoate and dichlorvos were detectable in few soil samples, and deltamethrin and dipterex were undetectable in all samples. The percentages of soil samples where different pesticides could be detected in one sample followed the order: one pesticide detectable (40.4%) > two pesticides simultaneously detectable (31.3%) > pesticide undetectable (18.8%) > three pesticides simultaneously detectable (8.2%) > four pesticides simultaneously detectable (1.4%). The concentrations of mancozeb in detectable samples averaged 39.05 microg x kg(-1), and that of cypermethrin was 7.83 microg x kg(-1). The mean concentrations of the other five pesticides ranged from 0.19 microg x kg(-1) to 1.65 microg x kg(-1). Totally, the pesticide residue status in litchi orchards in Guangdong was venial. PMID:21250457

  14. 40 CFR 158.2082 - Experimental use permit biochemical pesticides residue data requirements table.

    2010-07-01

    ... pesticides residue data requirements table. 158.2082 Section 158.2082 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Biochemical Pesticides § 158.2082 Experimental use permit biochemical pesticides residue data requirements table. (a)...

  15. 40 CFR 158.2172 - Experimental use permit microbial pesticides residue data requirements table.

    2010-07-01

    ... pesticides residue data requirements table. 158.2172 Section 158.2172 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Microbial Pesticides § 158.2172 Experimental use permit microbial pesticides residue data requirements table. (a)...

  16. 40 CFR 158.2130 - Microbial pesticides residue data requirements table.

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Microbial pesticides residue data... (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Microbial Pesticides § 158.2130 Microbial pesticides residue data requirements table. (a) General. Sections 158.100 through 158.130 describe how to...

  17. 40 CFR 158.2040 - Biochemical pesticides residue data requirements table.

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Biochemical pesticides residue data... (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Biochemical Pesticides § 158.2040 Biochemical pesticides residue data requirements table. (a) General. Sections 158.100 through 158.130 describe how to...

  18. Evaluation of a recent product to remove lipids and other matrix co-extractives in the analysis of pesticide residues and environmental contaminants in foods.

    Han, Lijun; Matarrita, Jessie; Sapozhnikova, Yelena; Lehotay, Steven J

    2016-06-01

    This study demonstrates the application of a novel lipid removal product to the residue analysis of 65 pesticides and 52 environmental contaminants in kale, pork, salmon, and avocado by fast, low pressure gas chromatography - tandem mass spectrometry (LPGC-MS/MS). Sample preparation involves QuEChERS extraction followed by use of EMR-Lipid ("enhanced matrix removal of lipids") and an additional salting out step for cleanup. The optimal amount of EMR-Lipid was determined to be 500mg for 2.5mL extracts for most of the analytes. The co-extractive removal efficiency by the EMR-Lipid cleanup step was 83-98% for fatty samples and 79% for kale, including 76% removal of chlorophyll. Matrix effects were typically less than ±20%, in part because analyte protectants were used in the LPGC-MS/MS analysis. The recoveries of polycyclic aromatic hydrocarbons and diverse pesticides were mostly 70-120%, whereas recoveries of nonpolar polybrominated diphenyl ethers and polychlorinated biphenyls were mostly lower than 70% through the cleanup procedure. With the use of internal standards, method validation results showed that 76-85 of the 117 analytes achieved satisfactory results (recoveries of 70-120% and RSD≤20%) in pork, avocado, and kale, while 53 analytes had satisfactory results in salmon. Detection limits were 5-10ng/g for all but a few analytes. EMR-Lipid is a new sample preparation tool that serves as another useful option for cleanup in multiresidue analysis, particularly of fatty foods. PMID:27139213

  19. Pesticide residues in cereal crop grains in Poland in 2013.

    Malinowska, Elżbieta; Jankowski, Kazimierz; Sosnowski, Jacek; Wiśniewska-Kadżajan, Beata

    2015-06-01

    This paper presents the results of the audit on pesticide residues in cereal grains throughout Poland in 2013. The number of all samples of cereal grains was 380. Altogether 292 active substances of plant protection products were checked in the audit. Qualitative and quantative analyses were done according to Polish Standard PN-EN 15562:2008, using the LC-MS/MS technique. The methods (QuEChERS) is based on extraction of residues of plant protection products from a sample using acetonitrile. In the samples analyzed, 62 % of them did not contain any pesticide residues, 34 % of samples of cereal grains contained such residues but below the maximum residue limit, 3 % contained residues over the maximum limit, whereas 1 % of the samples contained illegal substances. The lowest amounts of pesticide residues were found in cereal grains coming from fields with cereal mixtures and in Avena grains, while the highest amounts were in Hordeum and Triticum grains. The substances found most often were fungicide residues. In northern and southern regions of Poland (Silesian, Pomeranian, and Kuyavian-Pomeranian voivodeships), cereal grains with pesticide residues were much more common than in other regions of Poland. PMID:25944754

  20. Development of irradiation technique on degradation residue of pesticide veterinary drugs and mycotoxins in food

    Irradiation technology is a new processing technology, It was widely used in food, medicines and medical supplies, chemical and other industries. In this paper, illustrated their applications in the degradation of pesticides, veterinary drugs and mycotoxins aspects residual pollution in food. Analysis of residual contaminants in food irradiation control study limitations and look forward to the prospect of food irradiation technology. (authors)

  1. Effect of Household Coffee Processing on Pesticide Residues as a Means of Ensuring Consumers' Safety.

    Mekonen, Seblework; Ambelu, Argaw; Spanoghe, Pieter

    2015-09-30

    Coffee is a highly consumed and popular beverage all over the world; however, coffee beans used for daily consumption may contain pesticide residues that may cause adverse health effects to consumers. In this monitoring study, the effect of household coffee processing on pesticide residues in coffee beans was investigated. Twelve pesticides, including metabolites and isomers (endosulfan α, endosulfan β, cypermethrin, permethrin, deltamethrin, chlorpyrifos ethyl, heptachlor epoxide, hexachlorobenzene, p'p-DDE, p'p-DDD, o'p-DDT, and p'p-DDT) were spiked in coffee beans collected from a local market in southwestern Ethiopia. The subsequent household coffee processing conditions (washing, roasting, and brewing) were established as closely as possible to the traditional household coffee processing in Ethiopia. Washing of coffee beans showed 14.63-57.69 percent reduction, while the roasting process reduced up to 99.8 percent. Chlorpyrifos ethyl, permethrin, cypermethrin, endosulfan α and β in roasting and all of the 12 pesticides in the coffee brewing processes were not detected. Kruskal-Wallis analysis indicated that the reduction of pesticide residues by washing is significantly different from roasting and brewing (P 0.05). The processing factor (PF) was less than one (PF < 1), which indicates reduction of pesticides under study during processing of the coffee beans. The cumulative effect of the three processing methods has a paramount importance in evaluating the risks associated with ingestion of pesticide residues, particularly in coffee beans. PMID:26344013

  2. Extraction of pesticide residues from biological and environmental samples

    Various procedures that show potential in offering shorter extraction times with higher recoveries and low consumption of organic solvents are discussed. Solid phase extraction is attracting increasing attention for the isolation of pesticide residues from aqueous solutions and constitutes an alternative to liquid-liquid extraction. Microwave assisted extraction of stable pesticide residues from soil samples appears to be a viable alternative to conventional Soxhlet extraction. Thermal desorption involving high temperature distillation is an innovative method for efficiently extracting certain pesticides from soil, sediment and plant samples. Supercritical fluid extraction is emerging as a valuable technique for the isolation of pesticide residues from soil, plant and food samples, using supercritical fluids as the extraction media. It represents an excellent alternative to the potentially hazardous solvents currently used in conventional methods. The feasibility of employing water based systems for the extraction of certain pesticides from fruits and vegetables has also been investigated. A brief survey is given of these extraction procedures and a comparison made with the techniques widely used for the extraction of pesticides residues from biological and environmental samples. (author). 22 refs, 4 figs, 12 tabs

  3. Food safety in Thailand 2: Pesticide residues found in Chinese kale (Brassica oleracea), a commonly consumed vegetable in Asian countries

    There is increasing public concern over human health risks associated with extensive use of pesticides in agriculture. Regulation of pesticide maximum residue limits (MRLs) in food commodities is established in many developed countries. For Thailand, this regulation exists in law but is not fully enforced. Therefore, pesticide residues in vegetables and fruits have not been well monitored. This study investigated the pesticide residues in Chinese kale, a commonly eaten vegetable among Asians. The Chinese kale samples (N = 117) were purchased from markets in Nakhon Pathom Province, Thailand, and analyzed for the content of 28 pesticides. Analysis was performed by the multiresidual extraction followed by GC–MS/MS. Of pesticides investigated, 12 pesticides were detected in 85% of the Chinese kale samples. Although carbaryl, deltamethrin, diazinon, fenvalerate and malathion were found in some samples, their levels were lower than their MRLs. However, in 34 samples tested, either carbofuran, chlorpyrifos, chlorothalonil, cypermethrin, dimethoate, metalaxyl or profenofos was detected exceeding their MRLs. This represents a 29% rate of pesticide detection above the MRL; a rate much higher than in developed countries. Washing vegetables under running water significantly reduced (p < 0.05) profenofos residues by 55%. The running water method did not significantly decrease cypermethrin residues in the samples but washing with vinegar did. Our research suggests that routine monitoring of pesticide residues is necessary to reduce the public health risks associated with eating contaminated vegetables. Washing vegetables before consumption is advisable as this helps to reduce the level of pesticide residues in our daily intake. - Highlights: • Significant pesticide residues were detected in Chinese kale sold in Thailand. • MRL exceedance was found and this was higher than that seen in developed countries. • Washing vegetables under running water can remove pesticide residues significantly. • To be safe, washing vegetables before consumption is advisable

  4. Food safety in Thailand 2: Pesticide residues found in Chinese kale (Brassica oleracea), a commonly consumed vegetable in Asian countries

    Wanwimolruk, Sompon, E-mail: sompon-999@hotmail.com [Center for Innovation Development and Technology Transfer, Faculty of Medical Technology, Mahidol University, Bangkok 10700 (Thailand); Kanchanamayoon, Onnicha [Center for Innovation Development and Technology Transfer, Faculty of Medical Technology, Mahidol University, Bangkok 10700 (Thailand); Phopin, Kamonrat [Center for Innovation Development and Technology Transfer, Faculty of Medical Technology, Mahidol University, Bangkok 10700 (Thailand); Department of Clinical Microbiology and Applied Technology, Faculty of Medical Technology, Mahidol University, Bangkok 10700 (Thailand); Prachayasittikul, Virapong [Department of Clinical Microbiology and Applied Technology, Faculty of Medical Technology, Mahidol University, Bangkok 10700 (Thailand)

    2015-11-01

    There is increasing public concern over human health risks associated with extensive use of pesticides in agriculture. Regulation of pesticide maximum residue limits (MRLs) in food commodities is established in many developed countries. For Thailand, this regulation exists in law but is not fully enforced. Therefore, pesticide residues in vegetables and fruits have not been well monitored. This study investigated the pesticide residues in Chinese kale, a commonly eaten vegetable among Asians. The Chinese kale samples (N = 117) were purchased from markets in Nakhon Pathom Province, Thailand, and analyzed for the content of 28 pesticides. Analysis was performed by the multiresidual extraction followed by GC–MS/MS. Of pesticides investigated, 12 pesticides were detected in 85% of the Chinese kale samples. Although carbaryl, deltamethrin, diazinon, fenvalerate and malathion were found in some samples, their levels were lower than their MRLs. However, in 34 samples tested, either carbofuran, chlorpyrifos, chlorothalonil, cypermethrin, dimethoate, metalaxyl or profenofos was detected exceeding their MRLs. This represents a 29% rate of pesticide detection above the MRL; a rate much higher than in developed countries. Washing vegetables under running water significantly reduced (p < 0.05) profenofos residues by 55%. The running water method did not significantly decrease cypermethrin residues in the samples but washing with vinegar did. Our research suggests that routine monitoring of pesticide residues is necessary to reduce the public health risks associated with eating contaminated vegetables. Washing vegetables before consumption is advisable as this helps to reduce the level of pesticide residues in our daily intake. - Highlights: • Significant pesticide residues were detected in Chinese kale sold in Thailand. • MRL exceedance was found and this was higher than that seen in developed countries. • Washing vegetables under running water can remove pesticide residues significantly. • To be safe, washing vegetables before consumption is advisable.

  5. Pesticide residue monitoring in Korean agricultural products, 2003-05.

    Cho, T H; Kim, B S; Jo, S J; Kang, H G; Choi, B Y; Kim, M Y

    2009-01-01

    Between 2003 and 2005, a total of 11,716 samples were collected and analysed to determine the level of pesticides residues. Multi-residue methods (MRMs) capable of simultaneously determining 250 pesticides were used. Of the 11,716 samples, 89.1% had no detectable residues and 1.7% had violative residues. The detection rates by commodity group were 11.4, 8.6, 0.3, and 0.02% for vegetables, fruit, grain, mushrooms, and the others, respectively. Agricultural products with pesticide residues were pepper, Perilla frutescens, leafy lettuce and spinach in decreasing order. Of the 250 pesticides that were monitored, 70 pesticides were actually found. Procymidone, endosulfan, chlorfenapyr, metalaxyl, and diethofencarb were frequently detected. Of the samples, parsley, Petasites hybridus, Aster scaber and leek had high violative rates of 23.1, 12.6, 8.2, and 7.9%, respectively. From violative samples, procymidone, endosulfan, metalaxyl, diazinon and chlorpyrifos were frequently detected. The violation rates were 1.71, 1.68, and 1.76% in 2003, 2004 and 2005, respectively, and the detection rates were 8.5, 12.0, and 13.3% in 2003, 2004, and 2005, respectively. PMID:24784964

  6. Comparison of different types of coatings in headspace solid phase micro extraction for the analysis of pesticide residues in vegetables and fruits

    Despite the continuing development of solid-phase micro extraction (SPME) fiber coatings, their selection presents some difficulties for analytes in choosing the appropriate fiber for a particular application. There are many types of SPME coatings available commercially. The most widely used for determination of pesticide residues in vegetable and fruits are polydimethylsiloxane (PDMS) and polyacrylate (PA). A headspace solid phase micro extraction (HS-SPME) procedure using these two commercialized fibers (PDMS and PA) is presented for the determination of selected groups of organo chlorine and organophosphorus pesticides. The extraction performances of these compounds were compared using these two fibers. The optimal experimental procedures for the adsorption and desorption of pesticides were determined. An explanation for the extraction differences is suggested based on the different thickness, polarity of the polymeric film of fibers and the different extracting matrices. In addition, the higher detector response of the pesticides after addition of aliquots of water and an organic solvent to the vegetable and fruit samples are also discussed. The SPME fibers were reusable until a maximum of 120 extractions. Finally, the optimized procedures were applied successfully for the determination of these compounds in vegetable and fruits samples. Mean recoveries for all pesticides were between 75.0-97 % with RSD below 7 %. (author)

  7. A comparative study of allowable pesticide residue levels on produce in the United States

    Neff Roni A

    2012-01-01

    Full Text Available Abstract Background The U.S. imports a substantial and increasing portion of its fruits and vegetables. The U.S. Food and Drug Administration currently inspects less than one percent of import shipments. While countries exporting to the U.S. are expected to comply with U.S. tolerances, including allowable pesticide residue levels, there is a low rate of import inspections and few other incentives for compliance. Methods This analysis estimates the quantity of excess pesticide residue that could enter the U.S. if exporters followed originating country requirements but not U.S. pesticide tolerances, for the top 20 imported produce items based on quantities imported and U.S. consumption levels. Pesticide health effects data are also shown. Results The model estimates that for the identified items, 120 439 kg of pesticides in excess of U.S. tolerances could potentially be imported to the U.S., in cases where U.S. regulations are more protective than those of originating countries. This figure is in addition to residues allowed on domestic produce. In the modeling, the top produce item, market, and pesticide of concern were oranges, Chile, and Zeta-Cypermethrin. Pesticides in this review are associated with health effects on 13 body systems, and some are associated with carcinogenic effects. Conclusions There is a critical information gap regarding pesticide residues on produce imported to the U.S. Without a more thorough sampling program, it is not possible accurately to characterize risks introduced by produce importation. The scenario presented herein relies on assumptions, and should be considered illustrative. The analysis highlights the need for additional investigation and resources for monitoring, enforcement, and other interventions, to improve import food safety and reduce pesticide exposures in originating countries.

  8. Residues of Organochlorine Pesticides in Lake Mariut

    Lake Mariut, a brackish water lake adjoining the Mediterranean Coast of Egypt, has suffered much from intensive pollution in recent years due to the successive increase of human population and industry around it (Saad, 1980). The occurrence and distribution of organochlorine pesticides in the water of Lake Mariut during a period of one year were studied. This study represents an essential part of a pilot project on pollution of Lake Mariut supported by IAEA. The major organochlorine pesticides detected in the water of Lake Mariut were Lindane, p, p'-DDE, o,p'-DDT and p, p'-DDT. The mean concentrations of these pesticides were 2.091, 4.493, 0.009 and 0.134 ppb, respectively. The mean concentration of the calculated total DDT (Σ DDT) was 5.1 PPb

  9. 77 FR 75082 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2012-12-19

    ... expression in the Federal Register of June 29, 2011 (76 FR 38035) (FRL- 8877-2). There are two enforcement... AGENCY 40 CFR Part 180 Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide... for residues of pesticide chemicals in or on various commodities. DATES: Comments must be received...

  10. 76 FR 36479 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    2011-06-22

    ... petition was previously announced in the Federal Register of August 11, 2010 (75 FR 48667) (FRL-8840-6... AGENCY 40 CFR Parts 174 and 180 Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals... residues of pesticide chemicals in or on various commodities. DATES: Comments must be received on or...

  11. 76 FR 33183 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    2011-06-08

    ... CFR 174.532; March 16, 2011; 76 FR 14289 (FRL-8866- 5) when Bacillus thuringiensis eCry3.1Ab protein... AGENCY 40 CFR Part 174 Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on... a pesticide petition requesting the establishment or modification of regulations for residues...

  12. The 2010 European Union Report on Pesticide Residues in Food

    European Food Safety Authority

    2013-03-01

    Full Text Available This report presents the results of the control of pesticide residues in food commodities sampled during the calendar year 2010 in the 27 EU Member States and two EFTA countries (Iceland and Norway. The report also comprises the outcome of the consumer risk assessment of pesticide residues. EFSA presents for the first time the results of a pilot cumulative risk assessment (CRA to multiple chemical residues. Finally, the report provides some recommendations aimed at the improvement of the future monitoring programmes and the enforcement of the European pesticide residue legislation. In total, more than 77,000 samples of approximately 500 different types of food (raw or processed were analysed for pesticide residues by national competent authorities. Considering the results concerning both the national and the EU-coordinated programmes, the total number of analytical determinations reported among all the countries amounted to more than 14 million. The results of the EU-coordinated programme for 2010 showed that 1.6% of total samples analysed exceeded the European legal limits (MRLs. EFSA concluded that the long-term exposure of consumers did not raise health concerns. In assessing the short-term exposure, the pesticide monitoring results revealed that a risk could not be excluded for 79 samples concerning 30 different pesticides if the pertinent food was consumed in high amounts. The results of the CRA are considered indicative as the work on establishing which groups of pesticides are expected to share the same toxicological effects is not yet complete and the final methodological approach needs to be further elaborated. The outcome of the pilot CRA demonstrated that the exposure calculations are affected by significant uncertainties, mainly related to the analytical results reported as “non-detected”. The methodology used in this pilot exercise will be further revised to reduce the uncertainties of the exposure assessment.

  13. Graphene as dispersive solidphase extraction materials for pesticides LC-MS/MS multi-residue analysis in leek, onion and garlic.

    Guan, Wenbi; Li, Changsheng; Liu, Xue; Zhou, Shujing; Ma, Yongqiang

    2014-01-01

    A multi-residue analytical method was validated for 24 representative pesticides residues in onion, garlic and leek. The method is based on modified QuEChERS sample preparation with a mixture of graphene, primary secondary amine (PSA), and graphitised carbon black (GCB) as reversed-dispersive solid-phase extraction (r-DSPE) material and LC-MS/MS. Graphene was first used as an r-DSPE clean-up sorbent in onion, garlic and leek. The results first show that the mixed sorbent of graphene, PSA and GCB has a remarkable ability to clean-up interfering substances in the r-DSPE procedure when compared with the mixture of PSA and GCB. Use of matrix-matched standards provided acceptable results for tested pesticides with overall average recoveries between 70.1% and 109.7% and consistent RSDs 70% recovery. PMID:24224921

  14. Thin layer chromatography as an alternative method for pesticide analysis in rice grains

    The applicability of thin layer chromatography for the analysis of pesticide residues in grains as an alternative method to gas and high performance liquid chromatography was evaluated. Recoveries of six selected pesticides representing different pesticide classes as well as marker compounds for the four TLC detection methods employed ranged from 60 to 102%. The CVs of most of the pesticides analysed were within the range of CV indicated excepted for pesticide residue analysis. Thin layer chromatography can be a useful tool to analyze pesticide residues in rice grains. (author)

  15. Inspection of pesticide residues on food by surface-enhanced Raman spectroscopy

    Shende, Chetan; Gift, Alan; Inscore, Frank; Maksymiuk, Paul; Farquharson, Stuart

    2004-03-01

    Modern agriculture depends on pesticides to curb infestations, increase crop yield and to produce the quantity and quality of food demanded by today's society. However, potential pesticide residue contamination of food is of critical concern to the food industry and the regulators responsible for health and safety. For example, many pesticides kill insects by attacking the central nervous system, and the use of these pesticides above the EPA set tolerance levels (from 0.1 to 50 ppm) could pose a threat to humans, in particular infants. Unfortunately, rapid, chemical analysis of pesticide residues is unavailable, and only a very small fraction of foods are inspected. The greatest concern is food imported from nations that simply ignore US regulations. In an effort to address this need, we have been developing a simple device to collect residues from food surfaces, perform a rapid chemical separation, and detect and identify pesticides by surface-enhanced Raman spectroscopy (SERS). Capillaries are coated with a metal-doped sol-gel that both separates chemicals and generates SER spectra when irradiated. SERS of pesticides at ppm concentrations, and a preliminary product to aid inspectors is presented.

  16. Pesticide persistence and bound residues in soil - regulatory significance

    The paper discusses key aspects of the European Union (EU) regulatory policy related to the persistence and bound residues of agricultural pesticide active substances in soil. This is examined in the context of the EU Authorisations Directive (91/414/EEC) which will gradually replace existing national systems of agricultural pesticide regulation within EU Member States. Discussion is concentrated on this directive, looking in particular at the Uniform Principles therein and the possible ways that these decision-making guidelines could be developed into a regulatory framework. The aim in this process of negotiated development is to identify any questions or data requirements that will be needed for persistent pesticides or soil bound residues, over and above those generally required for all compounds. The present EU regulatory position on soil non-extractable or bound residues is examined and possible future improvements to the system are described and discussed

  17. The determination of pesticide residues and contaminants in vegetables by means of neutron activation analysis. Part of a coordinated programme on nuclear detection and analysis

    Neutron activation techniques have been applied to study the existence of pesticide residues (As, Br, Hg) and pollutants (Cd, Co, Zn) in local vegetable and fruit samples, polished and unpolished glutinous and non-glutinous milled rice, and fish caught in polluted and unpolluted areas of the Gulf of Thailand. Since the baseline levels of these toxic elements in vegetables, fruits, rice and fish are not known as yet, the results cannot be regarded as conclusive. Furthermore, no significant difference was observed in the concentration of these elements in fish caught in polluted and unpolluted areas. The Gulf of Thailand does not therefore appear to be polluted at present. The substoichiometric isotope dilution technique was successfully applied to mercury determinations, and only to a limited extent to Cd due to shutdown of the TRR-1 reactor

  18. Solid Phase Microextraction (SPME) in Determination of Pesticide Residues in Soil Samples

    Rada Đurović

    2011-01-01

    The basic principles and application possibilities of the methods based on solid phase microextraction (SPME) in the analysis of pesticide residues in soil samples are presented in the paper. The most important experimental parameters which affect SPME efficacy in pesticide determination (type and thickness of microextraction fiber, duration of microextraction, temperature at which it is conducted, effect of addition of salts (the effect of efflorescence), ...

  19. Evaluation of pesticide residues in human blood samples from Punjab (India)

    Jasbir Singh Bedi; Gill, J.P.S.; Kaur, P.; Sharma, A.; R. S. Aulakh

    2015-01-01

    Aim: The present study was undertaken to estimate the current status of residues of organochlorine pesticides (OCPs), organophosphates (OPs) and synthetic pyrethroids (SPs) pesticides in human blood. Materials and Methods: Human blood samples were analyzed by gas chromatography and confirmed by gas chromatographymass spectrometry in selective ion monitoring mode. Results: The gas chromatographic analysis of human blood samples collected from Punjab revealed the presence of p,p’-dichloro...

  20. Automated QuEChERS tips for analysis of pesticide residues in fruits and vegetables by GC-MS.

    Kaewsuya, Pakritsadang; Brewer, William E; Wong, Jon; Morgan, Stephen L

    2013-03-13

    This paper reports the development of an automated method of QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) using pipet tips fitted with filtration screens and containing primary-secondary amine, magnesium sulfate, and graphitized carbon black. These tips are referred to as "QuEChERS Tips". Using loosely contained sorbent, dispersive solid phase extraction (dSPE) cleanup was performed with the QuEChERS Tips and automation. The main advantage of the QuEChERS Tips is that they are readily automated because this dSPE method does not require centrifugation. High recoveries (70-117%) and good reproducibilities (<12%) are shown for over 200 pesticides using automated QuEChERS Tips and GC-MS in various sample matrices. PMID:23331058

  1. Fast gas chromatography with solid phase extraction clean-up for ultratrace analysis of pesticide residues in baby food.

    Hercegov, A; Dmtrov, M; Matisov, E; Kirchner, M; Otrekala, R; Stefuca, V

    2005-08-19

    A sample preparation method based on single solvent phase extraction and solid-phase extraction (SPE-NH2) clean-up is studied in combination with fast capillary gas chromatography (GC) to determine 18 selected pesticides belonging to various chemical classes in apples, the common raw material for baby food production and baby food, at the concentration level extraction as well as the simplifying of the whole process of sample preparation was carried out. Recoveries obtained at concentration level of 5 microg/kg (the required value for limit of quantification (LOQ) in baby food) were >90%, except of dimethoate (77.7%) and captan (46.4%) with MS detection. The obtained LOQs were at least 1 order lower than 5 microg/kg for the majority of compounds. The repeatability of gas chromatography-mass spectrometry (GC-MS) measurements of the matrix matched standards expressed as relative standard deviation was captan and cypermethrin. PMID:16114235

  2. Glove accumulation of pesticide residues for strawberry harvester exposure assessment.

    Li, Yanhong; Chen, Li; Chen, Zhenshan; Coehlo, Joe; Cui, Li; Liu, Yu; Lopez, Terry; Sankaran, Gayatri; Vega, Helen; Krieger, Robert

    2011-06-01

    We investigated the accumulation of pesticide residues on rubber latex gloves that are used by strawberry harvesters to protect their skin, reduce pesticide exposure and promote food safety. Gloves accumulated residues of 16 active ingredients including azoxystrobin, bifenthrin, boscalid, captan, cyprodinil, fenhexamid, fenpropathrin, fludioxonil, hexythiazox, malathion, methomyl, naled, propiconazole, pyraclostrobin, quinoline, and quinoxyfen at different times. Glove residue accumulation (t(½) 2.8-3.7 d) was very similar to the dissipation of DFRs (t(½) 2.1-3.0 d) during the first 3 weeks after malathion applications. Dermal malathion dose was 0.2 mg/kg at the preharvest interval and declined to trace levels during the following 3 months. Glove accumulation of malathion indicated trace surface residue availability and was used to assess the relationship between dislodgable foliar residues and potential hand exposure. PMID:21503692

  3. Ecological risk of pesticide residues in the British Columbia environment: 1973-2012.

    Wan, Michael T

    2013-01-01

    An updated ecological risk assessment was conducted to re-evaluate and review the overall risk of pesticide residues to certain aquatic life. The focus was the impact on offsite non-target, freshwater organisms of pesticide operational sprays in British Columbia from 1973 until 2012. The values of risk quotients for pesticides of selected indicator organisms were determined to measure the effect. When compared with organophosphorus, carbamate, and other miscellaneous pesticides, this risk assessment analysis suggests that the historical use of persistent and highly toxic organochlorine pesticides posed, and continue to pose, a deleterious ecological risk. The risk is both short-term acute and long-term sub-acute, chronic toxicity to offsite, non-target aquatic invertebrates and juvenile salmonid fish. Data indicated that these organisms were, and remain, subjected to harmful effects of pesticide residues to varying degrees. Most vulnerable were, and also are, benthic organisms inhabiting bottom sediments. This substrate is the natural sink for persistent pesticide residues, predominantly organochlorine pesticides from historical use, as well as dioxins, furans, and polycyclic aromatic hydrocarbons from wood preservatives, and other sources. Environment Canada's main aquatic protection strategy was a 10 metre no-treatment buffer zone, augmented with an additional appropriate setback along shorelines of fishery and wildlife resource-sensitive water bodies. This study discusses why this guideline was necessary, useful and effective, but was only partially successful. The physical-chemical properties of pesticide residues, from either an individual compound or different compounds in combination, also influence the nature of biological impacts on non-target, aquatic organisms. Few studies have been conducted in British Columbia aquatic environments to investigate the significance of this aspect. PMID:23431973

  4. Global Harmonization of Maximum Residue Limits for Pesticides.

    Ambrus, Árpád; Yang, Yong Zhen

    2016-01-13

    International trade plays an important role in national economics. The Codex Alimentarius Commission develops harmonized international food standards, guidelines, and codes of practice to protect the health of consumers and to ensure fair practices in the food trade. The Codex maximum residue limits (MRLs) elaborated by the Codex Committee on Pesticide Residues are based on the recommendations of the FAO/WHO Joint Meeting on Pesticides (JMPR). The basic principles applied currently by the JMPR for the evaluation of experimental data and related information are described together with some of the areas in which further developments are needed. PMID:25603277

  5. Monitoring pesticides residues and contaminants for some leafy vegetables at the market level

    Pesticide residues and contaminants in selected leafy vegetables, namely (lettuce, garden rocket and salad onion) were monitored at market level in Riyadh City in Saudi Arabia, during the period june to july 2001. Fifteen samples of vegetables from the City vegetable market of Riyadh were collected and subjected to multi-pesticide residue detection and analysis by gas chromatography with mass spectrometer and electron capture detectors (GC/MS,ECD). Results of sample extracts analysis showed that the two vegetables of: garden rocket and salad onion contain pesticide residues and contaminants which have no Maximum Residue Limits (MRL) prescribed by Codex Alimentarius Commission (CAC) collaborate with World Health and Food and Agriculture Organizations (WHO/FAO). Whereas lettuce vegetable was found free of any identified pesticide residues or contaminants. Garden rocket was shown to contain dibutyl phthalate (0.04 ppm)-steryl chloride (0.02 ppm) tridecane (0.06 ppm)-hexadecane (0.07 ppm)-BIS (ethylhexyl) phthalate (0.006 ppm) and pyridinium, 1-hexyl chloride (0.01 ppm). The salad onion was found to contain 9-octadecanamide (0.13 ppm)-tridecane (0.15 ppm) and tetradecane (0.16 ppm). There are no established MRL s for these pesticides and contaminants detected in garden rocket and salad onion, although when impacts on human health were reviewed some of them were found probably hazardous. (Author)

  6. 77 FR 25954 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2012-05-02

    ... disproportionately high and adverse human health impacts or environmental effects from exposure to the pesticides... residues of the biochemical pesticide, Organic Acids Derived from Leonardite, when used as a plant...

  7. Organophosphorus pesticide residues in the total diet of Kuwait

    Levels of phosphorylated pesticide residues in the total diet of Kuwait were determined. A total of 136 core samples (and 90 related items) were analyzed by following the multi-residue methods listed in PAM1. The results indicated that 25 of the items (about 18%) in the Kuwaiti diet contained detectable residues. In total 6 pesticides were detected. Monocrotophos (0.2 mg/kg), diazinon (0.05 mg/kg), and quinalphos (0.022 mg/kg) were present only in one sample. Chloropyriphos-methyl and fenitrothion were the most commonly detected pesticides. Chloropyriphos-methyl was present in 19 items and ranged from (0.01 to 0.33 mg/kg) while fenitrothion was detected in 8 samples, ranging from 0.016 to 0.84 mg/kg. The levels of Chloropyriphos ranged from 0.054 to 0.073 mg/kg, and it was present in 3 samples. The levels of residues were generally low in most of the positive samples. MRL was exceeded in only one of the core samples. Fenitrothion levels in the brown bread were higher than MRL. Pesticides present in wheat flour were responsible for the residues in most of the positive samples. (author)

  8. Multiresidue method for pesticide residue analysis in food of animal and plant origin based on GC or LC and MS or MS/MS.

    Muñoz, Eva; Muñoz, Gloria; Pineda, Laura; Serrahima, Eulalia; Centrich, Francesc

    2012-01-01

    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. PMID:23451398

  9. Pesticide residues in the soil of the Central Jordan Valley

    Soil samples were taken from three zones in the Central Jordan Valley to evaluate the range of contamination with pesticides. Several pesticides belonging to different groups, particularly chlorinated hydrocarbon insecticides such as the DDT family and cyclodienes, were detected. In zone I, most of the chlorinated hydrocarbon insecticides occurred in open fields cultivated with tomatoes at a depth of 30-60 cm, at 0-15 and 15-30 cm in zone II, and at 0-15 and 30-60 cm in zone III. When considering pesticide residues under plastic house conditions cultivated with tomatoes, most of the chlorinated hydrocarbon insecticide residues were detected at a depth of 0-15 and 15-30 cm in zone I, at 0-15, 15-30 and 30-60 cm in zone II, and at 0-15 and 15-30 cm in zone III of the Central Jordan Valley. (author). 13 refs, 3 tabs

  10. Organochlorine Pesticide Residues in Fish Samples from Lagos Lagoon, Nigeria

    David Adeyemi

    2008-01-01

    Full Text Available The organochlorine pesticide (OCPs residues were measured in three species of fish Tilapia zilli (Red belly Tilapia, Ethmalosa fimbriata (Bonga Shad and Chrysichthys nigrodigitatus (Catfish. These fish species are a significant part of the diet of residents of Lagos Nigeria. The organochlorine pesticides analyzed include DDT(pp'1,1,1-trichloro-2,2-bis-(4-chlorophenyl ethane, DDD, DDE (pp 1,1-dichloro-2, 2-bis-(4-chlorophenyl ethylene, HCH (gamma 1,2,3,4,5,6-hexachlorocylohexane, HCB (hexachlorobenzene,Dieldrin (1,2,3,4,10,10-hexachloro-6,7-epoxy-1,4,4a,5,6,7,8,8a octahydro-1,4,5,8 dimethanonaphthalene and transnonachlor. The analysis was done using Gas Chromatograph with Electron Capture Detector. The mean concentration of OCPs ranged from 0.01-8.92 ppm. The concentration of the OCPs (except for HCHs in fish samples in this study were below the extraneous residue limit of 5 ppm, set by the codex alimentarious commission of FAO-WHO-1997. However, the concentrations were higher than those detected during previous studies of fish samples from Lake Victoria, Uganda in Africa. Also the levels were quite high when compared with the allowable Federal Environmental Protection Agency (FEPA, now Federal Ministry of Environment limit and can be harmful if the trend is not checked. The study also showed that concentration of OCPs were higher in adult, than in Juvenile of most of the fish and there was no correlation observed between fat content and total concentration of OCPs.

  11. Radiotracer studies of pesticide residues in stored products

    The current programme was initiated in 1983 and was designed to assist scientists of developing Member States to make safe and effective use of radiotracer techniques for studying pesticide residue problems in stored products. This report represents an appraisal of a group of studies with particular emphasis given to terminal residues at the time of human consumption. A separate abstract was prepared for each of the 12 papers

  12. International Harmonization of Food Safety Assessment of Pesticide Residues.

    Ambrus, Árpád

    2016-01-13

    This paper summarizes the development of principles and methods applied within the program of the FAO/WHO Codex Alimentarius during the past 50 years for the safety assessment of pesticide residues in food and feed and establishing maximum residue limits (MRLs) to promote free international trade and assure the safety of consumers. The role of major international organizations in this process, the FAO capacity building activities, and some problematic areas that require special attention are briefly described. PMID:25660755

  13. Development, validation, and uncertainty measurement of multi-residue analysis of organochlorine and organophosphorus pesticides using pressurized liquid extraction and dispersive-SPE techniques.

    Sanyal, Doyeli; Rani, Anita; Alam, Samsul; Gujral, Seema; Gupta, Ruchi

    2011-11-01

    Simple and efficient multi-residue analytical methods were developed and validated for the determination of 13 organochlorine and 17 organophosphorous pesticides from soil, spinach and eggplant. Techniques namely accelerated solvent extraction and dispersive SPE were used for sample preparations. The recovery studies were carried out by spiking the samples at three concentration levels (1 limit of quantification (LOQ), 5 LOQ, and 10 LOQ). The methods were subjected to a thorough validation procedure. The mean recovery for soil, spinach and eggplant were in the range of 70-120% with median CV (%) below 10%. The total uncertainty was evaluated taking four main independent sources viz., weighing, purity of the standard, GC calibration curve and repeatability under consideration. The expanded uncertainty was well below 10% for most of the pesticides and the rest fell in the range of 10-20%. PMID:21210211

  14. Effects of different washing methods on pesticide organophosphorus residues

    WANG Xiao-Wei

    2013-02-01

    Full Text Available Objective To compare the effects of different washing methods for removing of organophosphorus pesticides residual from the vegetable samples. Methods Four non-toxic substances (rice washing water, flour water, baking soda and dietary alkali were used for the removing of organophosphorus pesticides residual (omethoate was taken for instance from the vegetable samples (cabbage, then detected through phosphor molydate blue after extraction and concentration. Results It was showed the least residual quantity was using flour water. Using single factor experiment and orthogonal experiment, the conditions of best cleaning effect were flour water concentration for 3.5 g per 500 mL water, soaking time for 17 min, soaking temperature for 32 ℃, and the pesticide removal rate reached to 83%. A good linear range was obtained between 0.8~32.0 μg/mL, and the linear equation was Y =0.011X-0.005 with correlation coefficient of 0.9955, the limit of detection was 0.8 μg/mL. Conclusion It is effective to reduce pesticide residues on the fruits and vegetables by using flour water, and the method is simple, convenient and cheap, and suitable for use in daily life.

  15. 9 CFR 318.16 - Pesticide chemicals and other residues in products.

    2010-01-01

    ... 9 Animals and Animal Products 2 2010-01-01 2010-01-01 false Pesticide chemicals and other residues... PREPARATION OF PRODUCTS General § 318.16 Pesticide chemicals and other residues in products. (a) Nonmeat ingredients. Residues of pesticide chemicals, food additives and color additives or other substances in or...

  16. 76 FR 3601 - Codex Alimentarius Commission: Meeting of the Codex Committee on Pesticide Residues

    2011-01-20

    ... Pesticide Residues AGENCY: Office of the Under Secretary for Food Safety, USDA. ACTION: Notice of public... that will be discussed at the 43rd Session of the Codex Committee on Pesticide Residues (CCPR) of the... limits for pesticide residues in specific food items or in groups of food; establishing maximum...

  17. 77 FR 3229 - Codex Alimentarius Commission: Codex Committee on Pesticide Residues (CCPR)

    2012-01-23

    ... Food Safety and Inspection Service Codex Alimentarius Commission: Codex Committee on Pesticide Residues....) positions that will be discussed at the 44th Session of the Codex Committee on Pesticide Residues (CCPR) of... for establishing maximum limits for pesticide residues in specific food items or in groups of...

  18. Fast,low-pressure gas chromatography triple quadrupole tandem mass spectrometry for analysis of 150 pesticide residues in fruits and vegetables

    We developed and evaluated a new method of low-pressure gas chromatography-tandem mass spectrometry (LP-GC/MS-MS) for fast analysis of 150 pesticides in four representative fruits and vegetables. This LP-GC (vacuum outlet) approach entails coupling a 10 m, 0.53 mm i.d., 1 micron film analytical col...

  19. Removal of 16 pesticide residues from strawberries by washing with tap and ozone water, ultrasonic cleaning and boiling

    Lozowicka, Bozena; Jankowska, Magdalena; Hrynko, Izabela; Kaczynski, Piotr

    2015-01-01

    The effects of washing with tap and ozone water, ultrasonic cleaning and boiling on 16 pesticide (ten fungicides and six insecticides) residue levels in raw strawberries were investigated at different processing times (1, 2 and 5 min). An analysis of these pesticides was conducted using gas chromatography with nitrogen-phosphorous and electron capture detection (GC-NPD/ECD). The processing factor (PF) for each pesticide in each processing technique was determined. Washing with ozonated water ...

  20. Evaluation of pesticide residues in human blood samples from Punjab (India

    Jasbir Singh Bedi

    2015-01-01

    Full Text Available Aim: The present study was undertaken to estimate the current status of residues of organochlorine pesticides (OCPs, organophosphates (OPs and synthetic pyrethroids (SPs pesticides in human blood. Materials and Methods: Human blood samples were analyzed by gas chromatography and confirmed by gas chromatographymass spectrometry in selective ion monitoring mode. Results: The gas chromatographic analysis of human blood samples collected from Punjab revealed the presence of p,p-dichlorodiphenyl dichloroethylene (DDE, p,p dichlorodiphenyl dichloroethane (DDD, o,p DDE and ?-endosulfan at mean levels of 15.26, 2.71, 5.62 and 4.02 ng/ml respectively. p,p DDE residue was observed in 18.0% blood samples, and it contributes 55% of the total pesticide burden in human blood. The difference of total dichlorordiphenyl trichloroethane (DDT between different age groups of humans was found to be statistically significant (p<0.05. The difference of DDT and endosulfan between dietary habits, gender and spraying of pesticides was found statistically non-significant, however endosulfan residues were observed only in pesticide sprayers population. Conclusion: Occurrence of p,p DDE, p,p DDD, o,p DDE in human blood indicated restricted use of DDT. However, presence of endosulfan residues in occupationally exposed population is a matter of public health concern.

  1. Effect of handling and processing on pesticide residues in food- a review

    Bajwa, Usha; Sandhu, Kulwant Singh

    2011-01-01

    Pesticides are one of the major inputs used for increasing agricultural productivity of crops. The pesticide residues, left to variable extent in the food materials after harvesting, are beyond the control of consumer and have deleterious effect on human health. The presence of pesticide residues is a major bottleneck in the international trade of food commodities. The localization of pesticides in foods varies with the nature of pesticide molecule, type and portion of food material and envir...

  2. Determination of Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate: Collaborative Study

    A collaborative study was conducted to determine multiple pesticide residues in fruits and vegetables using a quick, simple, inexpensive, and effective sample preparation method followed by concurrent analysis with gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass sp...

  3. Development and comparison of two multi-residue methods for the analysis of select pesticides in honey bees, pollen, and wax by gas chromatography-quadrupole mass spectrometry.

    Li, Yuanbo; Kelley, Rebecca A; Anderson, Troy D; Lydy, Michael J

    2015-08-01

    One of the hypotheses that may help explain the loss of honey bee colonies worldwide is the increasing potential for exposure of honey bees to complex mixtures of pesticides. To better understand this phenomenon, two multi-residue methods based on different extraction and cleanup procedures have been developed, and compared for the determination of 11 relevant pesticides in honey bees, pollen, and wax by gas chromatography-quadrupole mass spectrometry. Sample preparatory methods included solvent extraction followed by gel permeation chromatography (GPC) cleanup and cleanup using a dispersive solid-phase extraction with zirconium-based sorbents (Z-Sep). Matrix effects, method detection limits, recoveries, and reproducibility were evaluated and compared. Method detection limits (MDL) of the pesticides for the GPC method in honey bees, pollen, and wax ranged from 0.65 to 5.92 ng/g dw, 0.56 to 6.61 ng/g dw, and 0.40 to 8.30 ng/g dw, respectively, while MDLs for the Z-Sep method were from 0.33 to 4.47 ng/g dw, 0.42 to 5.37 ng/g dw, and 0.51 to 5.34 ng/g dw, respectively. The mean recoveries in all matrices and at three spiking concentrations ranged from 64.4% to 149.5% and 71.9% to 126.2% for the GPC and Z-Sep methods, with relative standard deviation between 1.5-25.3% and 1.3-15.9%, respectively. The results showed that the Z-Sep method was more suitable for the determination of the target pesticides, especially chlorothalonil, in bee hive samples. The Z-Sep method was then validated using a series of field-collected bee hive samples taken from honey bee colonies in Virginia. PMID:26048827

  4. The Determination of Organochlorine Pesticides Residues in Freshwater of Chalus River (Southern part of Caspian Sea) by Multivariate analysis

    Sh. Najafpour; S.M.V. Farabi; M. Yousefian; F.M. Abbas Alkarkhi; Ganjian Khenary

    2010-01-01

    The multivariate analysis of variance MANOVA was used to analyze the data obtained from this study. No significant difference was shown between the concentrations of all parameters during four seasons and all stations based on MANOVA test. The total percentage of DDE, Kelthane, -BHC, and DDT detected in stations were 63, 56, 50 and 69% over the year, respectively. The maximum concentrations of -BHC (fall), kelthane (fall), DDE (spring) and DDT (summer) were 21.6, 15.4, 9.8 and 9.2µg/l, resp...

  5. The Organochlorine Pesticides Residue Levels in Karun River Water

    Behrooz Jannat

    2013-01-01

    Full Text Available Background: The organochlorine pesticides (OCPs are among the most commonly used in water streams around the world. Most of these contaminants are highly hydrophobic and persist in sediments of rivers and lakes. Studies have suggested that OCPs may affect the normal function of the human and wildlife endocrine systems.Objectives: The aim of this study is to determine the concentrations of selected organochlorine pesticides residues [OP'DDT, PP'DDT, alderin, dieldrin, heptachlor, (?,,?,? HCH, (?, endosulfan and metoxychlor] in samples from Karun River water at Khuzestan province in Iran , by GC--ECD.Materials and Methods: Water was extracted with n-hexane and then purified by passing through a glass column packed with Florisil and Na2SO4, which was then eluted with ether: hexane solution v/v.Results: In general, all of 12 investigated organochlorine pesticides (OCPs were detected. Regardless of the kind of OCPs, the highest OCP pollution level in Karun River were seen from August to November 2009 ranging 71.43 89.34 g/L, and the lowest were seen from Dec 2010 to March 2011 at levels of 22.25 - 22.64 g/L. The highest and lowest mean concentrations of 12 investigated pesticides were -Endosulfan and pp' DDT with 28.51and 0.01 g/L respectively.Conclusions: Comparison of total organochlorine pesticides residues concentration with WHO guidelines revealed that the Karun River had total OCPs residues above the probable effect level (0.2-20 g/L, P < 0.05, which could pose a risk to aquatic life.

  6. 75 FR 11173 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-03-10

    ... preamble for FR Doc. 2010-2382 published in the Federal Register of Thursday, February 4, 2010 (75 FR 5790... AGENCY Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or... tolerances in 40 CFR part 180 for residues of the ``insecticide'' fluazifop-p-butyl in various...

  7. 77 FR 59577 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2012-09-28

    ... preamble for FR Doc. 2012-17899, published in the Federal Register of Wednesday, July 25, 2012 (77 FR 43562... AGENCY 40 CFR Part 180 Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals... tolerances for residues of the herbicide pyroxasulfone and its metabolites in or on wheat (grain,...

  8. Towards accreditation of MINT pesticide residue laboratory - a journey

    The laboratory accreditation process under ISO/IEC 17025 is a complex journey, due to several compulsory inputs necessary for obtaining the accreditation. This paper dwells on most of those inputs in the context of MINT Pesticide Residue Laboratory (MPRL), including: 1) Quality work culture; 2) Management commitment; 3) Sustainability of laboratory service appointment; 4) Laboratory personnel; 5) Laboratory equipment; 6) Continual training of personnel; 7) Technical co-operation; 8) Laboratory safety; 9) Special and general budget; 10) Consultancy service; 11) Quality Manual, Procedure, Work Instruction and related documents; 12) Internal Quality Audit (IQA) by MINT Quality Unit, and 13) Teamwork spirit. Based on experience faced and knowledge gained, multiple problems arising during this journey towards MINT Pesticide Residue Laboratory accreditation are also discussed in general, including their solutions. (Author)

  9. Pesticide Residues, Results from the period 2004-2011

    Petersen, Annette; Jensen, Bodil Hamborg; Andersen, Jens Hinge; Poulsen, Mette Erecius; Christensen, Tue; Nielsen, Elsa

    2013-01-01

    The present report presents the results from the 2004-2011 period of the monitoring programmes conducted by The Danish Veterinary and Food Administration. The programmes included commodities of fruit, vegetable, cereals and animal origin using random sampling from food on the Danish market. Since the beginning of the 1960, Denmark has monitored fruit and vegetables for pesticides residues. For the periods 1993-1997 and 1998-2003, results were collated and the dietary exposure was calculated. ...

  10. Levels of Organochlorine Pesticide Residues in Grasscutter (Thryonomys swinderianus Tissues

    Sarah Blankson-Arthur

    2011-06-01

    Full Text Available The study investigated the extent of contamination of with p,p- DDT, p,p-DDE, hexachlorocyclohexane isomers, lindane ((γ-HCH and δ-HCH, dieldrin, aldrin, endrin, endrin aldehyde, endrin ketone, alpha-endosulfan, endosulfan sulfate, chlordane, heptachlor and methoxychlor in tissues of grasscutter (Thryonomys swinderianus, obtained from the Gomoa East district of Ghana. The organochlorine pesticide residues in the samples were soxhlet extracted using a mixture of hexane and acetone. The extracts were cleaned up using florisil and analysed using a gas chromatograph equipped with an electron detector (GCECD. The results indicated that all the analyzed samples were contaminated with the studied organochlorine pesticides. Aldrin and heptachlor were the principal contaminants in all the samples. The muscle had the highest pollutant load followed by the liver and then the kidney. The levels of organochlorine pesticide residues detected in all the tissues were below the accepted Maximum Residue Limits (MRL, as adopted by the WHO/FAO Codex Alimentarius Commission (2005.

  11. Physicochemical composition, minerals, and pesticide residues in organic grape juices

    Alberto, Miele; Luiz Antenor, Rizzon; Sonia Claudia do Nascimento de, Queiroz; Clsio, Gianello.

    2015-03-01

    Full Text Available Demand for organic products is intensified in many countries each year. Following this trend, Brazil produces increasing volumes of organic grape juice. In this way, a survey of organic grape juices made from grapes produced according to this system was carried out where physicochemical composition, [...] minerals, trace elements, and pesticide residues were determined. Variables related to grape juice composition were performed by physicochemical procedures; minerals and trace elements, by inductively plasma optical emission spectrometry; pesticide residues, by liquid chromatography-mass spectrometry. Main results show that the physicochemical composition of organic grape juices was in general in accordance to the Brazilian legislation. The mean concentrations of trace elements were very low, varying from 0.002 (Cd) to 0.970 (Ba) mg L1. Pesticide residues were not detected in any sample analyzed (MRL= 10 g L1). These results show that the Serra Gacha viticultural region present conditions to produce organic grape juices, despite the adverse climate factors that occurs in some years. Nevertheless, these products should be made with grape varieties, such as the labrusca ones, less susceptibles to the main grapevine pathogens.

  12. Clean-up of cereal extracts for gas chromatography-tandem quadrupole mass spectrometry pesticide residues analysis using primary secondary amine and C18

    Herrmann, Susan Strange; Poulsen, Mette Erecius

    2015-01-01

    dispersive solid phase extraction (dSPE) procedure. dSPE clean-up using 25mg/ml extract significantly reduced the major matrix peak observed for wheat extracts. Higher amounts of PSA reduced the analytical response for iprodione and malathion. For oat extract 50-150mg PSA/ml extract was needed to obtain...... pesticides. Based on the present study it is concluded that the optimal dSPE clean-up procedure employs 25mg PSA/ml extract for wheat and 150mg PSA/ml extract for oat.......The level of co-extracted matrix in wheat and oat extracts obtained by the QuEChERS method (EN 15662) is high and the occurrence of free fatty acids generates a major matrix peak in TIC chromatograms (rt. 13-22min). Matrix can compromise the analytical performance in pesticide analysis using GC...

  13. A multi-residue method for the analysis of pesticides and pesticide degradates in water using HLB solid-phase extraction and gas chromatography-ion trap mass spectrometry

    Hladik, M.L.; Smalling, K.L.; Kuivila, K.M.

    2008-01-01

    A method was developed for the analysis of over 60 pesticides and degradates in water by HLB solid-phase extraction and gas-chromatography/mass spectrometry. Method recoveries and detection limits were determined using two surface waters with different dissolved organic carbon (DOC) concentrations. In the lower DOC water, recoveries and detection limits were 80%-108% and 1-12 ng/L, respectively. In the higher DOC water, the detection limits were slightly higher (1-15 ng/L). Additionally, surface water samples from four sites were analyzed and 14 pesticides were detected with concentrations ranging from 4 to 1,200 ng/L. ?? 2008 Springer Science+Business Media, LLC.

  14. Distribution and migration of pesticide residues in mosquito control impoundments St. Lucie County, Florida, USA

    Parkinson, R. W.; Wang, T. C.; White, J. R.; David, J. R.; Hoffman, M. E.

    1993-09-01

    This project was designed to: (1) document the distribution and migration of organochlorine pesticide residues within marsh substrates of 18 St. Lucie County mosquito control impoundments located along the Indian River Lagoon estuary, and (2) evaluate the impact of water management techniques on residue mobility. Our results indicate that detectible concentrations of organochlorine compounds, applied between the late 1940s and early 1950s, are present in 16 of the 18 St. Lucie County mosquito control impoundments. These compounds are primarily restricted to the surficial, organic-rich wetland sediment, which, based upon geotechnical analysis, was exposed to the atmosphere at a time when the impoundments were subjected to pesticide treatment. Contaminated sediments are present below the surficial, organic-rich layer, suggesting that some vertical migration of pesticides has occurred. It is unlikely that leaching associated with the downward percolation of impounded water was responsible for this migration as pesticide residues were never detected within the in situ pore waters. An alternative explanation is that biological processes (e.g., rooting, burrowing) facilitated the downward flux of organochlorine compounds into sediment horizons not subjected to direct treatment. Eighty-eight surface water samples obtained from two impoundments subjected to contrasting water management techniques were analyzed for pesticide content. None of the surficial water samples collected in association with these impoundments contained detectible concentrations of organochlorine compounds. These samples were unfiltered and contained as much as 25 mg/1 of particulate organic matter. This suggests that the currently preferred management technique (RIM), which is designed to maintain water quality, limit mosquito production, and provide for ecological continuity, does not hydraulically mobilize pesticide residues into the Indian River Lagoon estuary.

  15. Miniaturisation and optimisation of the Dutch mini-Luke extraction method for implementation in the routine multi-residue analysis of pesticides in fruits and vegetables.

    Lozano, Ana; Kiedrowska, Barbara; Scholten, Jos; de Kroon, Marijke; de Kok, Andr; Fernndez-Alba, Amadeo R

    2016-02-01

    This paper presents the validation and further miniaturisation of the well-known Dutch mini-Luke method for high water and acid content matrices for 175 pesticides amenable to liquid- and gas chromatography-mass spectrometry. For optimisation of the method, recovery tests with different sample/extraction solvent ratios, varying amounts of dichloromethane and salts were performed with fifty representative pesticides. Solvent consumption could be reduced considerably, especially for the dichloromethane (by a factor of 3). Recovery studies performed with lettuce and orange matrix spiked at 0.005, 0.01 and 0.02 mg/kg yielded average recoveries in the range 70-120% with relative standard deviation values below 20% for almost all the pesticides tested. The linearity over three orders of magnitude was demonstrated (r(2) > 0.99). The matrix effect could be considered as not significant. The limit of quantification was 0.005 mg/kg for 96% of the compounds. The optimised New Dutch mini-Luke ("NL"-) method was applied successfully in routine analysis and the EUPT FV-16 sample. PMID:26304397

  16. Pesticide residues in grapes, wine, and their processing products.

    Cabras, P; Angioni, A

    2000-04-01

    In this review the results obtained in the 1990s from research on the behavior of pesticide residues on grapes, from treatment to harvest, and their fate in drying, wine-making, and alcoholic beverage processing are reported. The fungicide residues on grapes (cyproconazole, hexaconazole, kresoxim-methyl, myclobutanil, penconazole, tetraconazole, and triadimenol), the application rates of which were of a few tens of grams per hectare, were very low after treatment and were not detectable at harvest. Pyrimethanil residues were constant up to harvest, whereas fluazinam, cyprodinil, mepanipyrim, azoxystrobin, and fludioxonil showed different disappearance rates (t(1/2) = 4.3, 12, 12.8, 15.2, and 24 days, respectively). The decay rate of the organophosphorus insecticides was very fast with t(1/2) ranging between 0.97 and 3.84 days. The drying process determined a fruit concentration of 4 times. Despite this, the residue levels of benalaxyl, phosalone, metalaxyl, and procymidone on sun-dried grapes equalled those on the fresh grape, whereas they were higher for iprodione (1.6 times) and lower for vinclozolin and dimethoate (one-third and one-fifth, respectively). In the oven-drying process, benalaxyl, metalaxyl, and vinclozolin showed the same residue value in the fresh and dried fruit, whereas iprodione and procymidone resides were lower in raisins than in the fresh fruit. The wine-making process begins with the pressing of grapes. From this moment onward, because the pesticide on the grape surface comes into contact with the must, it is in a biphasic system, made up of a liquid phase (the must) and a solid phase (cake and lees), and will be apportioned between the two phases. The new fungicides have shown no effect on alcoholic or malolactic fermentation. In some cases the presence of pesticides has also stimulated the yeasts, especially Kloeckera apiculata, to produce more alcohol. After fermentation, pesticide residues in wine were always smaller than those on the grapes and in the must, except for those pesticides that did not have a preferential partition between liquid and solid phase (azoxystrobin, dimethoate, and pyrimethanil) and were present in wine at the same concentration as on the grapes. In some cases (mepanipyrim, fluazinam, and chlorpyrifos) no detectable residues were found in the wines at the end of fermentation. From a comparison of residues in wine obtained by vinification with and without skins, it can be seen that their values were generally not different. Among the clarifying substances commonly used in wine (bentonite, charcoal, gelatin, polyvinylpolypyrrolidone, potassium caseinate, and colloidal silicon dioxide), charcoal allowed the complete elimination of most pesticides, especially at low levels, whereas the other clarifying substances were ineffective. Wine and its byproducts (cake and lees) are used in the industry to produce alcohol and alcoholic beverages. Fenthion, quinalphos, and vinclozolin pass into the distillate from the lees only if present at very high concentrations, but with a very low transfer percantage (2, 1, and 0.1%, respectively). No residue passed from the cake into the distillate, whereas fenthion and vinclozolin pass from the wine, but only at low transfer percentages (13 and 5%, respectively). PMID:10775335

  17. Pesticide residue profile and nutrient characteristics of the Densu River Basin in Ghana

    The Densu River Basin is one of the largest agricultural areas in Ghana. About 80% of people living in this area rely on agricultural activities for subsistence. The practice of using pesticides such as organochlorines, organophosphates, carbamates, pyrethroids and several others in agriculture and public health programs have raised concerns about potentially adverse effects on human health and the environment. Assessment of human health implications of non-point sources within a river basin include pesticide residues analysis of water, sediment and fish and monitoring of physico-chemical parameters in waters that serve as source of drinking water for the entire community within the basin. In this study, a field survey was conducted to assess farmers' knowledge of safe handling and use of pesticides. Nutrient chemistry and surface water characteristics of the Densu River and its tributaries, type and levels of pesticide residues and their trends in water, sediment and fish in the basin were also evaluated. The study also assessed the health risk associated with pesticide contamination of fish from the Basin as well as the relationship between land use and groundwater contamination. Generally surface and ground water bodies in the Densu River basin were found to be polluted with respect to nutrients and pesticides. Waters from the basin were found to be fresh, slightly acidic, and weakly mineralized with low chemical constituents. Nitrate (NO3-N) levels in surface water ranged between 0.12 - 31.07 mgL-1 while ammonia was between 0.01 - 2.10 mgL-1 and that of phosphate was 0.012 - 2.45 mgL-1. Pesticide residues and metabolites detected in water, sediment and fish samples from the Densu River Basin were organochlorines. In an average 96% of fish samples, 13.69% of sediment and 3.30% of water samples, at least one pesticide residue was detected per sample. Of the numerous pesticides evaluated, γ -HCH, DDT, aldrin, dieldrin, DDE, endosulfan sulphate, γ-chlordane, endrin and δ-HCH were detected in fish, water and sediment samples. Aldrin and dieldrin levels detected were above the recommended limit of 0.03 μL-1 with endosulfan, endrin and chlordane registering levels above their recommended limits of 20.0μL-1 and 0.2 μL-1 respectively for drinking water. Pesticide residues in fish samples varied between 0.10 μgKg-1 to 30.90 μgKg-1. The highest level was detected in Hepsetus odoe (HO-N). Contamination pattern of pesticide residues in fish samples was generally in the order of p'p'-DDE > heptachlor > γ- HCH > p'p'-DDT > endosulfan Sulphate > α-endosulfan > δ- HCH > γ-chlordane > dieldrin > endrin ketone > methoxychlor > endrin > aldrin > endrin aldehyde. Data obtained from the field survey regarding safe use of pesticides, toxicity awareness and symptoms among farmers indicated that a very high proportion of farmers were at high risk of pesticide poisoning from occupational exposure. More than 90% of farm workers did not practice safety precaution during pesticide formulation and application leading to considerable prevalence of pesticide related illness in this agricultural community. The presence of pesticide residues in fish was of further concern because fish is the main protein diet for humans in the basin. The estimated dose for aldrin, methoxychlor, γ-chlordane, endrin aldehyde, endrin ketone, endrin, p'p'-DDT and δ-HCH do not pose a direct hazard to human health, although present in fish samples since the values registered were lower than the reference doses. However, γ- HCH, heptachlor, α-endosulfan, endosulfan sulphate, p'p'-DDE and dieldrin levels exceeded the reference dose, indicating a great potential for systemic toxicity in children who are considered to be the most vulnerable population subgroup. In children, between the ages of 0 - 1year, the hazard indices of 2.64, 1.720, 1.736 and 0.792 were computed for α-endosulfan, heptachlor, endosulfan sulphate and dieldrin respectively while for children between the ages 1 -11years, hazard indices for heptachlor, α-endosulfan and endosulfan were 0.573, 0.880 and 0.576 respectively. Although residue levels of pesticide residues were below the maximum permissible intake of Codex Alimentarius Committee of Food and Agricultural Organization on pesticides residues, there was no zero risk because there were pesticide residues present in fish. The results implicitly revealed that improper land use in the basin has led to poor groundwater and surface water quality. (au)

  18. Pesticide Residues in Bovine Milk in Punjab, India: Spatial Variation and Risk Assessment to Human Health.

    Bedi, J S; Gill, J P S; Aulakh, R S; Kaur, Prabhjit

    2015-08-01

    In the present study, gas chromatographic analysis of pesticide residues in bovine milk (n = 312) from Punjab, India, showed chlorpyrifos, DDT, and γ-HCH as the predominant contaminants. In addition, the presence of β-endosulfan, endosulfan suphate, cypermethrin, cyhalothrin, fenvalerate, deltamethrin, malathion, profenofos, and ethion was reported in milk samples. In this study, it was observed that 12 milk samples exceeded the maximum residue limits (MRLs) for γ-HCH (lindane), 18 for DDT and chlorpyrifos, and 1 sample each for endosulfan, cypermethrin, and profenophos. In India, DDT is still permitted for a malaria control program, which may be the plausible reason for its occurrence in milk samples. The spatial variation for presence of pesticide residues in milk indicated greater levels in cotton-growing areas of Punjab. At current levels of pesticide residues in bovine milk, the human health risk assessment in terms of noncancer and cancer hazard was calculated based on both lower-bound [LB (mean residue levels)] and upper-bound [UP (95th percentile level)] limits. It was noticed that cancer and noncancer risk were within United States Environmental Protection Agency prescribed limits for both adults and children at the LB, but children were being exposed to greater risk for DDT and HCH at the 95th-percentile UB level. PMID:26008642

  19. 77 FR 8755 - Receipt of a Pesticide Petition Filed for Temporary Tolerance Exemption for Residues of...

    2012-02-15

    ... Residues of Prohydrojasmon in or on Various Commodities AGENCY: Environmental Protection Agency (EPA... residues of pesticide chemicals in or on various commodities. DATES: Comments must be received on or before... modification of a regulation in 40 CFR part 180 for residues of pesticide chemicals in or on various...

  20. Pesticide residues in fruits and vegetables from South America – A Nordic project

    Hjorth, Karen; Johansen, K.; Holen, B.; Andersson, A.; Christensen, Hanne Bjerre; Siivinen, K.; Toome, M.

    2011-01-01

    The aim of this study was to investigate the amount of pesticide residues in fruits and vegetables from South America. A total of 724 samples of 46 different fruits and vegetables from eight South American countries were collected in 2007. In 19% of the samples no residues were found, 72% of...... need for continuous monitoring of pesticide residues, especially in imported fruits and vegetables....

  1. Exposure assessment of the Belgian population to pesticide residues through fruit and vegetable consumption

    Claeys, Wendie Liliane; De Voghel, Simon; Schmit, Jean-François; Vromman, Valérie; Pussemier, Luc

    2008-01-01

    Abstract The exposure of the Belgian consumer to pesticide residues via the consumption of fruit and vegetables was determined based on data collected in the Belgian food consumption survey performed by the Scientific Institute for Public Health and data of the monitoring programme 2005 of the Belgian Federal Agency for the Safety of the Food Chain. A first screening of pesticide residue exposure was performed by a deterministic approach. For most pesticide residues studied, the ex...

  2. Perspective on Dietary Risk Assessment of Pesticide Residues in Organic Food

    Benbrook, Charles M.; Baker, Brian P.

    2014-01-01

    Previous studies have shown that organically produced food has lower risks of pesticide contamination than food that is not organically produced. However, organically produced food is not entirely free of pesticide residues. A large, high-quality U.S. Department of Agriculture database reports pesticide residues in several dozen organic and conventionally grown foods on an annual basis, and supports detailed analyses of the frequency of residues in conventional and organic food, the number of...

  3. Validation of a methodology multi-residue for the determination of pesticides residuals in strawberry (fragraria spp.) by gas chromatography

    This study describes the validation of multi-residue analytical methodology for the simultaneous determination of 19 organ chlorine, organophosphorus and organ nitrogen pesticides in strawberry. Pesticides residues were extracted from strawberry samples with ethyl acetate, the extracts were cleaned-up by GPC, the quantitative analysis was carried out by high resolution gas chromatography (GC) with a pulsed splitless injection mode and simultaneous detection by m-ECD and NPD coupled in parallel. The methodology is specific, selective, and accurate and robust the calibration curves in matrix matched analytical standards show linearity over the concentration range of 0.04-5.00 mg/kg with limits of detection and quantitation between 0.007-0.5 mg/kg and 0.01-1.00 mg/kg respectively. The recovery experiments yielding averages between 80-110% for most of the pesticides. The distribution of analyze in the laboratory sample was evaluated and it was found its homogeneity. The methodology was applied in field samples and was mainly found Captan residues below MRL

  4. Clean-up of cereal extracts for gas chromatography-tandem quadrupole mass spectrometry pesticide residues analysis using primary secondary amine and C18.

    Herrmann, Susan S; Poulsen, Mette E

    2015-12-01

    The level of co-extracted matrix in wheat and oat extracts obtained by the QuEChERS method (EN 15662) is high and the occurrence of free fatty acids generates a major matrix peak in TIC chromatograms (rt. 13-22min). Matrix can compromise the analytical performance in pesticide analysis using GC-MS/MS. In order to reduce the amount and the effects of matrix we tested the effect of using six different amounts of primary secondary amine (PSA) (0, 25, 50, 100, 150 and 200mg/ml extract) with and without the addition of six different amounts of C18 (0, 25, 50, 100, 150 and 200mg/ml extract) in the dispersive solid phase extraction (dSPE) procedure. dSPE clean-up using 25mg/ml extract significantly reduced the major matrix peak observed for wheat extracts. Higher amounts of PSA reduced the analytical response for iprodione and malathion. For oat extract 50-150mg PSA/ml extract was needed to obtain equally low intensity of the matrix peak. For oat the analytical responses of the target pesticides generally increased with increasing amount of PSA. C18 had no significant effect on the intensity of the major matrix peaks and even resulted in lower analytical responses for several of the target pesticides. Based on the present study it is concluded that the optimal dSPE clean-up procedure employs 25mg PSA/ml extract for wheat and 150mg PSA/ml extract for oat. PMID:26572049

  5. Pesticide Residues, Results from the period 2004-2011

    Petersen, Annette; Jensen, Bodil Hamborg; Andersen, Jens Hinge; Poulsen, Mette Erecius; Christensen, Tue; Nielsen, Elsa

    The present report presents the results from the 2004-2011 period of the monitoring programmes conducted by The Danish Veterinary and Food Administration. The programmes included commodities of fruit, vegetable, cereals and animal origin using random sampling from food on the Danish market. Since...... the beginning of the 1960, Denmark has monitored fruit and vegetables for pesticides residues. For the periods 1993-1997 and 1998-2003, results were collated and the dietary exposure was calculated. In this report data for the analyses carried out in the period 2004-2011 are reported as well as the...

  6. Multi-Residue studies of pesticides in fermented dried cocoa beans and selected cocoa products produced in Ghana

    Cocoa is a major cash crop and contributes significantly to Ghana's economy. Majority of this contribution is as a result of foreign earnings in foreign trade partnership. Cocoa products are consumed locally aside it generating foreign income for the country. Pesticide residues above allowable limits in cocoa beans have potential detrimental effects on human health, depending on the frequency of exposure and/or the potency or toxicity of the pesticide. Pesticide residues on cocoa also attract trade sanctions from international trading partners. The approved pesticides, which are used to control pests in the growing cocoa in Ghana, are: Diazinon, Cypermethrin, Deltamethrin, Acetamiprid, Imidicloprid and Pyrethrums; nevertheless some unapproved pesticides on cocoa such as Pirimiphos-methyl, Chlorpyrifos, Endosulfan, Fenitrotion, Fenvalerate, Permethrin and others find their way for use on cocoa in Ghana. The main objective of this study was to determine the levels of pesticide residues in fermented dried cocoa beans produced and ready for export in Ghana, using gas chromatography mass spectrometry. It also seeks to provide the baseline information on contamination levels of pesticide residues in semi-finished and selected finished fermented dried cocoa beans products. Fermented dried cocoa beans were sampled at random in the two main COCOBOD warehouses located in Tema and Takoradi. Semi-finished and finished cocoa products were obtained from processing industries in Tema. Two extraction methods were used. The second extraction method was as by the QuEChERS method for vegetable oils which was used for the cocoa butter samples only, after being liquefied in water bath at 40 degrees celsius. The investigated pesticides consisted of fifteen organochlorine pesticides, thirteen organophosphorous pesticides and nine synthetic pyrethroids pesticides. Percentage recoveries ranged from 70-110 percent, with instrumental detection limits of 0.3ug/kg, 0.15ug/g and 0.15ug/g for the organochlorine, organophosphorous and synthetic pyrethroids pesticides respectively. Multivariate analysis on the residue data obtained from fermented dried cocoa beans in R-mode and Q-mode grouped the detected pesticides into currently used, previously used and drift from neighbouring crops pesticides applications. It also grouped sampled cocoa beans into four major clusters based on similarities in crop storage and farm practices. Beta-HCH (18.7 μg/kg), Gamma-chlordane (152.0 μg/kg), Methamidophos (18.5 μg/kg), Profenofos (31.8 μg/kg), Allethrin (10.5 μg/kg), Cypermethrin (32.0 μg/kg) and Fenvalerate (14.6 μg/kg) were the average residues concentrations of pesticides that exceeded the Japanese maximum residue levels (MRLs). However, all the detected pesticides with exception of Allethrin were below the MRLs for European Union. From results recorded in semi-finished and finished cocoa beans products produced in Ghana, de-shelling and roasting temperatures drastically reduced the residue levels in the cocoa products, but these were not enough solution for pesticide residues in cocoa beans. And thus raises concern about the health implication of these chemicals for domestic consumption of these products. It is highly recommended that a national quality control laboratory be established to continually monitor pesticides efficacy in order to avoid overdose of pesticides application.[au

  7. Multi-analyst, multi-matrix performance of the QuEChERS approach for pesticide residues in foods and feeds using HPLC/MS/MS analysis with different calibration techniques.

    Lehotay, Steven J; Mastovska, Katerina; Lightfield, Alan R; Gates, Robert A

    2010-01-01

    Three different calibration approaches were applied in HPLC/MS/MS using electrospray ionization for the determination of 14 diverse pesticide residues at different levels in a variety of food matrixes. This study was conducted as part of a 4 day training course for 17 chemists to learn the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) approach to pesticide residue analysis in foods. The analysts were divided into four different teams for the analysis of 12 different matrixes (strawberries, plums, carrots, green peppers, milk, molasses, alfalfa oats, corn silage, dry pet food, soybean, almonds, and foliage). The acetate-buffered QuEChERS protocol gave excellent results in the spiked samples for all matrixes tested. The HPLC/MS/MS calibration techniques consisted of external standardization in solvent solutions, matrix-matching, and the echo-peak technique. Peak areas were normalized to an internal standard in all three approaches. Matrix effects were observed with the corn silage, carrot, and foliage extracts, but they were minimal or nonexistent in the other matrixes. Matrix-matching best compensated for matrix effects, but has logistical difficulties in real-world application and required extra sample preparation compared to the other approaches. The echo-peak technique reduced matrix effects but did not eliminate them. PMID:20480880

  8. 75 FR 35801 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-06-23

    ... published in the Federal Register of January 27, 2010 (75 FR 4274) (FRL-8807-2). A method validation was..., as published in the Federal Register of January 27, 2010 (75 FR 4274) (FRL-8807-2). A method... AGENCY Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in...

  9. Practical tracer investigations of pesticide residues in agricultural ecosystem

    According to the FAO's latest estimates, the world food supply can only be guaranteed if the 1982 agricultural production is increased by approx. 50% by the year 2000. 2/3 of this production increase must be achieved on areas already under cultivation. This means that in addition to balanced mineral fertilization the use of pesticides will have to be intensively continued in order to fully exploit the improved yield potential of the cultivated plants achieved by breeding. The primary research objective is therefore to extend our knowledge of the uptake and effects of pesticides in the plant as well as their persistence in agricultural ecosystems in order to be able to apply them both more efficiently and more safely. The Institute of Radioagronomy at the Kernforschungsanlage Juelich GmbH (Juelich Nuclear Research Centre) is carrying out practical experiments into these problems using 14C-labelled pesticides under field conditions. In this way statements will become possible on the uptake and residue situation in plants, translocation and metabolism in the soil, the balance in the year of application as well as on the uptake of untreated cultures in the crop rotation. Parallel to this, uptake after leaf spraying or after seed grain treatment is being studied under standardized conditions, as well as for example the mineralization, sorption and fixation of active substances and metabolites in the soil. Results from the past 12 years are being utilized as a basis for an evaluation of the state of knowledge. (orig.)

  10. Monitoring of organochlorine pesticides residues in green mussels (Perna viridis) from the coastal area of Thailand.

    Boonyatumanond, Ruchaya; Jaksakul, Areerat; Puncharoen, Pornthip; Tabucanon, Monthip Sriratana

    2002-01-01

    The utilization of organochlorine pesticides for pest control chemical has been of great interest on residue contamination from biological organisms in the environment. Green mussel (Perna viridis) samples were monitored as bioindicators for assessment of the water quality in coastal waters along the Gulf of Thailand. Thirty-six samples were collected from 12 stations during 1997-1999 and analysed for 26 organochlorine pesticide compounds. This paper focuses on the contamination of organochlorine pesticide residues in green mussel (P. viridis) during 1997-1999. The limit of detection of all organochlorine pesticides compounds was at the range of 0.1-8.3 ng g(-1) wet weight and recovery 75-95%. The concentration of organochlorine pesticides residues in green mussel was lower than the maximum residue limit for aquatic animals as recommended by the Ministry of Public Health of Thailand. The trend of organochlorine pesticide residue contamination in this area decreased from 1989 to 1999. PMID:12152831

  11. Monitoring of Pesticide Residues in Fruits and Vegetables and Related Health Risk Assessment in Kumasi Metropolis, Ghana

    Crentsil Kofi Bempah

    2011-11-01

    Full Text Available The objective of present research study was to assess the concentration of pesticide residues in fruits and vegetables from markets in Kumasi and to generate awareness about the lethal effects of these pesticides on human beings as well as to estimate the potential health risks associated with the pesticide residue with regard to consumers. A total of 350 locally produced fruits and vegetables were purchased from six main markets in Kumasi and analyzed by gas chromatography equipped with electron capture detector for organochlorine (gamma-HCH, methoxychlor, aldrin, dieldrin, endrin, p,p’-DDE, p,p’-DDT and pyrethroid (permethrin, cyfluthrin, cypermethrin, fenvalerate, deltamethrin residues. The residual concentrations of selected pesticides in the various fruit and vegetable samples and the potential health risks associated with the exposure to these pesticides were also assessed. The results obtained showed that 37.5% of the fruit and vegetable samples analyzed contained no detectable level of the monitored pesticides, 19.0% of the samples gave results with levels of insecticides residues above the MRL, while 43.5% of the samples showed results below the MRL. The analysis of health risk estimates revealed that none of the pesticides exceeded the reference dose in both fruit and vegetables except endrin which exceeded reference dose in vegetables, suggesting a great potential for systemic toxicity in children considered the most vulnerable population subgroup. Based on observations made in these studies, it is proposed that more extensive monitoring investigation covering all fruits and vegetables in all the ten regions of Ghana be carried out to find the exact position of pesticide residues.

  12. Removal of 16 pesticide residues from strawberries by washing with tap and ozone water, ultrasonic cleaning and boiling.

    Lozowicka, Bozena; Jankowska, Magdalena; Hrynko, Izabela; Kaczynski, Piotr

    2016-01-01

    The effects of washing with tap and ozone water, ultrasonic cleaning and boiling on 16 pesticide (ten fungicides and six insecticides) residue levels in raw strawberries were investigated at different processing times (1, 2 and 5 min). An analysis of these pesticides was conducted using gas chromatography with nitrogen-phosphorous and electron capture detection (GC-NPD/ECD). The processing factor (PF) for each pesticide in each processing technique was determined. Washing with ozonated water was demonstrated to be more effective (reduction from 36.1 to 75.1 %) than washing with tap water (reduction from 19.8 to 68.1 %). Boiling decreased the residues of the most compounds, with reductions ranging from 42.8 to 92.9 %. Ultrasonic cleaning lowered residues for all analysed pesticides with removal of up to 91.2 %. The data indicated that ultrasonic cleaning and boiling were the most effective treatments for the reduction of 16 pesticide residues in raw strawberries, resulting in a lower health risk exposure. Calculated PFs for alpha-cypermethrin were used to perform an acute risk assessment of dietary exposure. To investigate the relationship between the levels of 16 pesticides in strawberry samples and their physicochemical properties, a principal component analysis (PCA) was performed. Graphical abstract ᅟ. PMID:26694708

  13. Development, validation and determination of multiclass pesticide residues in cocoa beans using gas chromatography and liquid chromatography tandem mass spectrometry.

    Zainudin, Badrul Hisyam; Salleh, Salsazali; Mohamed, Rahmat; Yap, Ken Choy; Muhamad, Halimah

    2015-04-01

    An efficient and rapid method for the analysis of pesticide residues in cocoa beans using gas and liquid chromatography-tandem mass spectrometry was developed, validated and applied to imported and domestic cocoa beans samples collected over 2 years from smallholders and Malaysian ports. The method was based on solvent extraction method and covers 26 pesticides (insecticides, fungicides, and herbicides) of different chemical classes. The recoveries for all pesticides at 10 and 50 μg/kg were in the range of 70-120% with relative standard deviations of less than 20%. Good selectivity and sensitivity were obtained with method limit of quantification of 10 μg/kg. The expanded uncertainty measurements were in the range of 4-25%. Finally, the proposed method was successfully applied for the routine analysis of pesticide residues in cocoa beans via a monitoring study where 10% of them was found positive for chlorpyrifos, ametryn and metalaxyl. PMID:25442595

  14. Effect of handling and processing on pesticide residues in food- a review.

    Bajwa, Usha; Sandhu, Kulwant Singh

    2014-02-01

    Pesticides are one of the major inputs used for increasing agricultural productivity of crops. The pesticide residues, left to variable extent in the food materials after harvesting, are beyond the control of consumer and have deleterious effect on human health. The presence of pesticide residues is a major bottleneck in the international trade of food commodities. The localization of pesticides in foods varies with the nature of pesticide molecule, type and portion of food material and environmental factors. The food crops treated with pesticides invariably contain unpredictable amount of these chemicals, therefore, it becomes imperative to find out some alternatives for decontamination of foods. The washing with water or soaking in solutions of salt and some chemicals e.g. chlorine, chlorine dioxide, hydrogen peroxide, ozone, acetic acid, hydroxy peracetic acid, iprodione and detergents are reported to be highly effective in reducing the level of pesticides. Preparatory steps like peeling, trimming etc. remove the residues from outer portions. Various thermal processing treatments like pasteurization, blanching, boiling, cooking, steaming, canning, scrambling etc. have been found valuable in degradation of various pesticides depending upon the type of pesticide and length of treatment. Preservation techniques like drying or dehydration and concentration increase the pesticide content many folds due to concentration effect. Many other techniques like refining, fermentation and curing have been reported to affect the pesticide level in foods to varied extent. Milling, baking, wine making, malting and brewing resulted in lowering of pesticide residue level in the end products. Post harvest treatments and cold storage have also been found effective. Many of the decontamination techniques bring down the concentration of pesticides below MRL. However, the diminution effect depends upon the initial concentration at the time of harvest, substrate/food and type of pesticide. There is diversified information available in literature on the effect of preparation, processing and subsequent handling and storage of foods on pesticide residues which has been compiled in this article. PMID:24493878

  15. A Survey of Determination for Organophosphorus Pesticide Residue in Agricultural Products

    Wen Li

    2013-04-01

    Full Text Available In order to find a fast, high efficient determination method of Organophosphorus Pesticides (OPPs residue because OPPs widely used in crops pest control fields in China are causing fearful risks for environment as well as animals and human health, traditional and advanced determination methods were discussed in the study. Based on the spectrum analysis technology combined colorimetric OPPs residue detection experiments in leafy vegetables showed that the absorbance of color reaction between OPPs residues and suitable colorimetric reagents can be distinguished in ppm level of OPPs residues. The detection limit of chlorpyrifos after color reaction with 0.5% Pbcl2 in acetic acid solution is 0.5 ppm. The conclusion was drawn that the detection technologies were diversified, however, a simple, efficient, rapid and nondestructive detection method is lacking and the spectrum analysis technology combined colorimetric can be a new fast and efficient determination method in the future.

  16. Ecological Risk Assessment of Pesticide Residues in Water from Desert Locust Area in Burkina Faso

    Sylvain Ilboudo; Adama Makoum Toé; Richard Ouédraogo; Moustapha Ouédraogo; Innocent Pierre Guissou

    2014-01-01

    Locust control requires sometimes an important use of pesticides in infested area with concomitant environment contaminations. Using the Gas Chromatography (GC) technical, pesticide residues were determined in water samples collected from locust outbreak areas of Burkina Faso, West Africa. The risk quotient method coupled with probabilistic risk assessment model was used for ecological risk assessment of pesticide detected in water. For ten pesticides belonging to Organophosphates, Pyrethroid...

  17. Investigation into the validity of extrapolation in setting maximum residue levels for pesticides in crops of similar morphology.

    Reynolds, S L; Fussell, R J; MacArthur, R

    2005-01-01

    Field trials were initiated to investigate if extrapolation procedures, which were adopted to limit costs of pesticide registration for minor crops, are valid. Three pairs of crops of similar morphology; carrots/swedes, cauliflower/calabrese (broccoli) and French beans/edible-podded peas; were grown in parallel at four different geographical locations within the UK. The crops were treated with both systemic and non-systemic pesticides under maximum registered use conditions, i.e. the maximum permitted application rates and the minimum harvest intervals. Once mature, the crops were harvested and analysed for residues of the applied pesticides. The limits of quantification were in the range 0.005-0.02 mg kg(-1). Analysis of variance and bootstrap estimates showed that in general, the mean residue concentrations for the individual pesticides were significantly different between crop pairs grown on each site. Similarly, the mean residue concentrations of most of the pesticides in each crop across sites were significantly different. These findings demonstrate that the extrapolations of residue levels for most of the selected pesticide/crop combinations investigated; chlorfenvinphos and iprodione from carrots to swedes; carbendazim, chlorpyrifos, diflubenzuron and dimethoate from cauliflower to calabrese; and malathion, metalaxyl and pirimicarb from French beans to edible-podded peas; appear invalid. PMID:15895609

  18. Investigation of pesticide residues in vegetables and fruits grown in various regions of Hatay, Turkey.

    Sungur, Sana; Tunur, Cetin

    2012-01-01

    In this study, 175 pesticide residues in various vegetable and fruit samples grown in different regions of Hatay, Turkey, were investigated. Residue analyses were performed using liquid chromatography-tandem mass spectrometry with the QuEChERS method. In tomato, plum and apricot samples, pesticide residues were below the limits of detection. In other samples, at least one pesticide residue was detected. Twelve pesticides (acetamiprid, carbendazim, chlorpyrifos, fenarimol, fludioxonil, hexythiazox, imidacloprid, metalaxyl, pyridaben, pyriproxyfen, thiabendozole, triadimenol) were found at levels between 0.003 and 0.759 mg kg(-1). Only in cucumber samples, acetamiprid residues were found at levels greater than the maximum acceptable limit in Turkish Food Codex and European Union maximum residue limits (EU MRLs). In other samples, the detected residue amounts are less than the MRLs declared in the Turkish Food Codex and EU MRLs. PMID:24786407

  19. Overview of pesticide residues in stored pollen and their potential effect on bee colony (Apis mellifera) losses in Spain.

    Bernal, J; Garrido-Bailón, E; Del Nozal, M J; González-Porto, A V; Martín-Hernández, R; Diego, J C; Jiménez, J J; Bernal, J L; Higes, M

    2010-12-01

    In the last decade, an increase in honey bee (Apis mellifera L.) colony losses has been reported in several countries. The causes of this decline are still not clear. This study was set out to evaluate the pesticide residues in stored pollen from honey bee colonies and their possible impact on honey bee losses in Spain. In total, 1,021 professional apiaries were randomly selected. All pollen samples were subjected to multiresidue analysis by gas chromatography-mass spectrometry (MS) and liquid chromatography-MS; moreover, specific methods were applied for neonicotinoids and fipronil. A palynological analysis also was carried out to confirm the type of foraging crop. Pesticide residues were detected in 42% of samples collected in spring, and only in 31% of samples collected in autumn. Fluvalinate and chlorfenvinphos were the most frequently detected pesticides in the analyzed samples. Fipronil was detected in 3.7% of all the spring samples but never in autumn samples, and neonicotinoid residues were not detected. More than 47.8% of stored pollen samples belonged to wild vegetation, and sunflower (Heliantus spp.) pollen was only detected in 10.4% of the samples. A direct relation between pesticide residues found in stored pollen samples and colony losses was not evident accordingly to the obtained results. Further studies are necessary to determine the possible role of the most frequent and abundant pesticides (such as acaricides) and the synergism among them and with other pathogens more prevalent in Spain. PMID:21309214

  20. A survey of organochlorine pesticide residues in cheese samples from three Mexican regions.

    Albert, L A; Alpuche, L; Bárcenas, C; Rendón, J

    1990-01-01

    Organochlorine pesticide residues were determined in cheese samples from three Mexican regions. All samples were found to be contaminated by these residues: p,p'-DDE was present in 100% of the samples. Other pesticides found with high frequencies were HCB, three of the BHC isomers, as well as heptachlor and its epoxide. Also found, although less frequently, were residues of p,p'-DDD, p,p'-DDT, aldrin, dieldrin and endrin. Samples from the region known as Comarca Lagunera had the highest number of pesticides per sample. The highest concentrations of residues were found in cheese samples from the Soconusco and the Comarca Lagunera regions. PMID:15092270

  1. Assessment of pesticide residues in commonly used vegetables in Hyderabad, Pakistan.

    Latif, Yawar; Sherazi, S T H; Bhanger, M I

    2011-11-01

    The aim of present study was to assess pesticide residues in vegetables in the Hyderabad region of Pakistan. The concentrations of six pesticides were determined by gas chromatography coupled with mass selective detector (GC-MSD) in locally produced vegetables purchased from wholesale markets. A total of 200 samples of eight vegetables viz. cauliflower, green chilli, eggplant, tomato, peas, bitter gourd, spinach and apple gourd were analyzed for pesticide residues. The results indicated that almost all samples were contained pesticides, only 39% contained pesticide residues at or below maximum residue limits (MRLs), and 61% contained pesticide residues above MRLs. From the six analyzed pesticides, carbofuran and chlorpyrifos were found above to MRLs with concentrations ranging from 0.01-0.39 and 0.05-0.96 mg/kg, respectively. The results provided important information on the current pesticide contamination status of some commonly used vegetables and pointed an urgent need to control the use of some excessively applied and potentially persistent pesticides, such as carbofuran and chlorpyrifos. PMID:21831431

  2. 75 FR 17715 - Notice of Receipt of a Pesticide Petition Filed for Temporary Tolerance Exemption for Residues of...

    2010-04-07

    ... AGENCY Notice of Receipt of a Pesticide Petition Filed for Temporary Tolerance Exemption for Residues of... exemption from the requirement of a tolerance for residues of pesticide chemicals in or on various... 174 or part 180 for residues of the pesticide chemical prohydrojasmon (PDJ) in or on various...

  3. Validation of a residue method to determine pesticide residues in cucumber by using nuclear techniques

    In this study, a multi-residue method using ethyl acetate for extraction and gel permeation chromatography for clean-up was validated to determine chlorpyrifos, malathion and dichlorvos in cucumber by gas chromatography. For this purpose, homogenized cucumber samples were fortified with pesticides at 0.02 0.2, 0.8 and 1 mg/kg levels. The efficiency and repeatability of the method in extraction and cleanup steps were performed using 14C-carbaryl by radioisotope tracer technique. 14C-carbaryl recoveries after the extraction and cleanup steps were between 92.63-111.73 % with a repeatability of 4.85% (CV) and 74.83-102.22 % with a repeatability of 7.19% (CV), respectively. The homogeneity of analytical samples and the stability of pesticides during homogenization were determined using radio tracer technique and chromatographic methods, respectively.

  4. Assessmet of temporal distribution of pesticide residues in vineyard soils of La Rioja (Spain)

    Pose Juan, Eva; Herrero Hernandez, Eliseo; Soledad Andrades, Maria; Rodriguez Cruz, Maria Sonia; Sanchez Martin, Maria Jesus

    2013-04-01

    The use and application of pesticides in vineyard is a common practice, which is important to prevent pest and diseases and improve the crop health and production, but on the other hand it could involve a potential risk for humans and the environment. For this reason, it is important to develop and validate a simple and fast multiresidue method to determine the presence of these compounds in soils. La Rioja region (Spain) is one of the most important wine-growing regions in Spain, which also entails that could be an important area of pesticide pollution. The objective of this work is to assess the temporal distribution of the possible pesticide pollution in soils from different areas of La Rioja (Spain). The pesticides selected in this study included fungicides (metalaxyl, and its metabolite CGA62826, pyrimethanil, tebuconazole, myclobutanil, kresoxim-methyl, triadimenol and flutriafol); herbicides (fluometuron, terbuthylazine and its metabolites desethylterbuthylazine and hydroxyterbuthylazine, lenacil, ethofumesate and acetochlor) and insecticides (methoxyfenozide and pirimicarb). The pesticide residues were evaluated by two analytical techniques, gas chromatography and liquid chromatography (GC-MS and LC-MS). The extraction procedure of pesticides from soils was optimized using two soil samples (blank soils) with different texture and characteristics collected from areas without pesticide application. Recoveries were studied in soil samples fortified with all pesticides at two levels of concentrations (the agronomic dose, 0.1 mg kg-1, and ten times this dose, 1 mg kg-1). Different extraction solvents were tested. The best results were obtained with methanol:acetone (50:50) mixture or methanol:CaCl2 0.01 M (50:50) mixture for hydroxyterbuthylazine and CGA62826. The accuracy (average recovery) and precision (reproducibility and repeatability) of the method were assessed using six replicates and the limits of detection (LODs) and quantification (LOQs) were estimated. Recoveries were above 70% for all pesticides. Good linear relationships of the calibration curves (0.01-1 μg mL-1) were obtained for all the compounds by the two analytical methods with regression coefficients (r2) higher than 0.99 in the range of concentrations studied. Detection limits were residues were found in most of the soils and an increment in concentrations of these compounds and in the number of positive samples were detected in samples collected in March 2012 in relation to those collected in September 2011. This increase in the number of positive samples was of 30 % for terbuthylazine. Fungicide residues were detected in greater concentrations in samples collected in September. Both behaviours may be related with the time of application of both types of compounds. Herbicides are commonly applied in March-April and fungicides are usually applied in summer, when different grapevine diseases like botrytis or mildiu commonly appear. Moreover, new pesticide residues were detected in March 2012, which were not detected in September 2011 in any soil sample. Further analysis of results is in course.

  5. Pesticide residue assessment in three selected agricultural production systems in the Choluteca River Basin of Honduras

    There is a basic lack of information about the presence of pesticide residues in the environment in Central America. Over the period of February 1995 to June 1997, river, well, lagoon and spring water samples, as well as soil, fish tissue, lagoon bed sediments and some foodstuffs were taken from the greater Cholutecan River Basin of Honduras and analyzed for pesticide residues. These were collected at three separate sites (La Lima, Zamorano and Choluteca), each characterized by differing agricultural production systems. The main pesticide residues found in soil samples were dieldrin and p,p'-DDT, while river water samples were found to have detectable levels of heptachlor, endosulfan and chlorpyrifos, with lagoon and well water also being shown to contain heptachlor. These pesticides detected were in more than 20% of the samples assessed. In river water samples more pesticide residues at higher concentrations were found to be associated with areas of more intensive agricultural production. The fewest pesticides with lowest concentrations were found in the small subwatershed associated with traditional agricultural production. Although the pesticides found in the soils at the three sites were generally similar they tended to be higher in the southern part of the Cholutecan watershed, followed by the central zone, with the lowest concentrations being found in the more traditional production zone. In lagoon and well water samples more pesticides, but mostly in lower concentrations were detected at the traditional production site than at the others. Ten pesticide compounds were detected in fish tissue, mainly organochlorines, some of which were also found in lagoon sediments. In terms of food products, almost no pesticides were detected in vegetables, but the kidney adipose tissue taken from slaughtered cows was shown to have a tendency to contain some organochlorines. Spring water in the traditional agricultural production zone contained three organochlorine compounds as well as chlorpyrifos, but these were detected only in the rainy season. This study indicates that pesticide residues are present and strongly associated with areas of intensive agriculture, although even in the areas practicing more traditional agriculture, pesticide residues were not absent. Further pesticide monitoring is necessary to obtain a more complete picture of the situation and based on this data an effective policy framework to assist in minimizing pesticide residue accumulation may be developed to reduce the adverse impact these compounds are known to have on the environment and human health. This snapshot of the pesticide distribution in three agriculturally distinct regions within the Choluteca watershed indicates that the situation is stable, but should be monitored to determine if pesticides residues will pose a health hazard in the future. (author)

  6. FINGER PRINTING TECHNIQUE FOR DETECTION OF PESTICIDE RESIDUES IN VEGETABLE CROPS

    Syeda Azeem Unnisa

    2014-06-01

    Full Text Available Finger printing technique enables the detection of DDT and HCH residues in vegetables through the development of light green and prussian violet colors respectively. Cut vegetables are pressed against o-tolidine impregnated paper (chromogenic paper and exposed to sunlight where colored spots appear instantly. The pesticides residues of DDT and HCH were determined in 16 samples of 4 varieties of vegetable crops, taken from 4 provinces. The results showed presence results for pesticide residues in vegetable crops.

  7. Effect of household and industrial processing on levels of pesticide residues and degradation products in melons

    Bonnechère, Aurore; Hanot, Vincent; Bragard, Claude; Bedoret, Thomas; Van Loco, Joris

    2012-01-01

    Abstract Two varieties of melons (Cucumis melo) were treated by two fungicides (carbendazim and maneb) and four insecticides (acetamiprid, cyromazin, imazalil and thiamethoxam) to quantify the effect of household processing on the pesticide residues. To ensure sufficiently high levels of residues in flesh and peels, the most concentrated formulations were applied pursuant to Good Agricultural Practices (GAPs). The peeling step decreased the concentration of pesticide residues for ...

  8. Levels of pesticides residues in the White Nile water in the Sudan.

    Nesser, Gibreel A A; Abdelbagi, Azhari O; Hammad, Ahmed Mohammed Ali; Tagelseed, Mirghani; Laing, Mark D

    2016-06-01

    Twenty-two commonly used pesticides were monitored during autumn, winter, and summer of 2004-2005 in 27 water samples from three sites along the White Nile in Sudan (former Sudan). Sites were selected to reflect pesticides gathered from drainage canals in central Sudan and from upstream sources. Collected samples were extracted and subjected to gas chromatographic analysis. Pesticides levels were measured in nanograms per liter. Pesticides residues were detected in 96 % of the samples with a total residue burden of 4132.6 ng L(-1), and an overall mean concentration and range of 50.99 and not detected-1570 ng L(-1), respectively. Ororganochlorines were the most frequently detected contaminants, which were found in 70 % of the samples, causing a total burden of 2852.8 ng L(-1), followed by pyrethroids 15 % of the samples, with a total burden of 926.5 ng L(-1). The tested herbicides were detected in ˂4 % of the samples with a total burden of 353.3 ng L(-1), while organophosphorus levels were below the detection limit. The most frequent contaminants were the following: heptachlor and its epoxide (52 % of samples), followed by DDTs (dichlorodiphenyltrichloroethanes) (DDT and DDE, in 19 % of the samples), cypermethrin and fenvalerate (in 11 % of the samples), and pendimethalin (in <4 % of the samples). Residues of hexachlorocyclohexane (HCH) isomers (α, β, γ and δ), endosulfan (α and β), p, p-DDD, λ cyhalothrin, deltamethrin, and oxyfluorfen were not detected in the analyzed samples. Generally, levels were least in autumn, and followed by summer and winter. Sources of contamination might include agricultural lands in central Sudan and upstream sources. Both recent and old contaminations were indicated. PMID:27230426

  9. Decontamination of spills and residues of some pesticides and of protective clothing worn during the handling of the pesticides

    Armour, M.A.; Nelson, C.; Sather, P. Briker, Y. [Univ. of Alberta, Edmonton (Canada)] [and others

    1996-12-31

    Users of pesticides may have waste or surplus quantities or spills for disposal. One alternative is to deactivate the pesticide at the handling site by using a straightforward chemical reaction. This option can be practical for those who use relatively small quantities of a large variety of pesticides, for example, greenhouse workers, small farmers, and agricultural researchers. This paper describes practical on-site methods for the disposal of spills or small waste quantities of five commonly used pesticides, Diazinon, Chlorpyrifos, Iprodione, 2,4-D, and Captan. These have been tested in the laboratory for the rate of disappearance of the pesticide, the degree of conversion to nontoxic products, the nature and identity of the products, the practicality of the method, and the ease of reproducibility. Methods selected were shown to be safe for the operator, reliable, and reproducible. Greater than 99% of the starting material had to be reacted under reasonable conditions and length of time. Detailed descriptions of the reactions are presented, so that they can be performed with reproducible results. Protective clothing worn during the handling and application of pesticides may become contaminated. Simple laundering does not always remove all of the pesticide residues. Thus, chronic dermal exposure may result from the pesticide-contaminated clothing. Appropriate methods of laundering using specific pretreatments have been determined. 7 refs.

  10. Public Health Implications of Pesticide Residues in Meat

    Jadhav V.J. and Waskar V.S.

    2011-01-01

    Use of pesticides in India began in 1948 when DDT was imported for malaria control and BHC for locust control. Since then various synthetic pesticides are used for protection of crops and public health. The persistence nature of some of these pesticides led to their accumulation in animal tissues and subsequently causes human dietary exposure to these pesticides through consumption of animal products viz. meat, milk, eggs and seafoods. Scientific evidence suggest that even such low dose but l...

  11. Extension of the QuEChERS Method for Pesticide Residues in Cereals to Flaxseeds, Peanuts, and Doughs

    A simple method was evaluated for the determination of pesticide residues in flaxseeds, doughs, and peanuts using gas chromatography-time-of-flight mass spectrometry (GC-TOF) for analysis. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, which was previously optimized f...

  12. [Rapid Detection of Trace Dimethoate Pesticide Residues Based on Colorimetric Spectroscopy].

    Li, Wen; Sun, Ming; Li, Min-zan; Sun, Hong

    2015-07-01

    In order to detect dimethoate pesticide residues rapidly and safely, a feasible method based on colorimetric spectroscopy was developed. Because dimethoate is one of organophosphorus pesticides containing sulfur, its sulfenyl can react with Pd2+ to produce a yellow complex named palladium sulfide. PdCl2 was used as the color agent, which was dissolved in acetic acid instead of the common concentrated hydrochloric acid. The dimethoate solution was prepared by dissolving the commercial pesticides into distilled water at different concentrations. The pesticide samples were reacted with the same amount of PdC2 solution respectively. The absorbance spectra of the samples after coloring reaction were measured in the region of 300-900 nm by a spectrophotometer. The result showed that the effect of using acetic acid instead of concentrated hydrochloric acid was not only safe but also preferable, and 0.5 mg x kg(-1) was the minimum concentration of the pesticide that could be distinguished in the spectra. The result met the pesticide residue detecting requirements of part fruits and vegetables in the national standard GB2763-2012 regulations. Further studies on random 40 dimethoate samples from 0.5 to 88 mg x kg(-1) were carried out. Thirty samples were randomly selected to establish the training model and remaining 10 samples were used to test the model. The preprocessing methods were carried on the spectrum data such as normalization and smoothing to get a better effect through comparison their prediction results with the correlation coefficient (r) and the root mean square error of cross-validation (RMSEP). The principal component analysis (PCA) method and partial least squares (PLS) method were used to establish prediction models respectively in the different wave ranges. By calculating the correlation coefficient of dimethoate samples in 350-900 nm the maximum of 0.9572 was obtained at wavelength 458 nm, so 453-463 and 400-600 nm were selected as feather regions. Experiments showed that the effect of SG preprocessing on the absorbance spectra in the region of 350-900 and 400-600 nm was obvious, and PLS method were better than PCA method. The optimum model was obtained in the region of 400-600 nm, when principal component number was 4, the training set r=0.9941, RMSEP=2.7703 and the validation set r=0.9933, RMSEP = 2.2148. This method was safe in operation and the colorimetric reaction time was 2 min, which provided theoretical and technical support for further studying on development of rapid, safe organophosphorus pesticide detection instrument. PMID:26717773

  13. Analysis of organo-chlorine pesticides residue in raw coffee with a modified "quick easy cheap effective rugged and safe" extraction/clean up procedure for reducing the impact of caffeine on the gas chromatography-mass spectrometry measurement.

    Bresin, Bruno; Piol, Maria; Fabbro, Denis; Mancini, Maria Antonietta; Casetta, Bruno; Del Bianco, Clorinda

    2015-01-01

    The control of pesticide residues on raw coffee is a task of great importance due to high consumption of this beverage in Italy and in many other countries. High caffeine content can hamper extraction and measurement of any pesticide residue. A tandem extraction protocol has been devised by exploiting the quick easy cheap effective rugged and safe (QuEChERS) scheme for extraction, coupled to a dispersive liquid-liquid micro-extraction (DLLME) in order to drastically reduce caffeine content in the final extract. Gas chromatography-mass spectrometry (GC-MS) has been used for quantification of organo-chlorine pesticides in single ion monitoring (SIM) mode. Method has been validated and performances meet the criteria prescribed by European Union regulations. PMID:25537171

  14. Multi pesticide and PCB residues in Nile tilapia and catfish in Assiut city, Egypt.

    Yahia, Doha; Elsharkawy, Eman E

    2014-01-01

    The current study investigated the levels of multi pesticide residues in the highly consumed types of Nile fish in Egypt: tilapia and cat fish. A total of 50 Nile tilapia (Oreochromis niloticus) and 50 African catfish (Clarias gariepinus) were collected from two areas in Assiut city, where most industries are situated and where agricultural activities and raising of farm animals are the main activities. In the first area, Elwasta, there is an electrical power station, and the second area, Mankbad, there is a cement factory. Fish samples were analyzed by High Resolution Gas Chromatography/Mass Spectrometry. Average pesticide residue concentrationsSE in muscle of tilapia and catfish (n = 10 pooled samples with five fish each) were determined. The results indicated the presence of different types of organophosphorous (OPs), organochlorine (OC), polychlorinated biphenyles (PCBs), hexachlorobenzene (HCB) and trifluralin pesticides in Elwasta and Mankbad in varying degrees. Diazenon was the only OP pesticide which exceeded the permissible limit in both investigated areas with the two types of fish. On the other hand, OCs, PCBs, HCB and trifluralin pesticide residue levels have not exceeded the maximum allowable concentration limit. In general, a higher pesticide residue level was obtained in Mankbad than Elwasta. In addition, higher values are realized for the detected pesticide residues in cat fish than tilapia. The results of the study have shown the extensive and recent use of these types of pesticides in the present time in Egypt. PMID:23911921

  15. Assessment of pesticide residues in some fruits using gas chromatography coupled with micro electron capture detector

    A very sensitive analytical method for the determination of 26 pesticides in some fruits based on solid phase extraction (SPE) cleanup was developed using gas chromatography (GC) coupled with micro electron capture detector (mu ECD). The identity of the pesticides was confirmed by gas chromatography mass spectroscopy (GC-MS) using selected ion monitoring (SIM) mode. Ethyl acetate was used as a solvent for the extraction of pesticide residues with assistance of sonication. For cleanup an octadecyl, C18 SPE column was used. A linear response of mu ECD was observed for all pesticides with good correlation coefficients (>0.9992). Proposed method was successfully applied for the determination of pesticide residues in the orange, apple, and grape fruits. Average recoveries achieved for all of the pesticides at fortification levels of 0.05, 1.0 and 2.0 mu g g/sup -1/ in analyzed fruits were above 90% with relative standard deviations (RSD) less than 6%. (author)

  16. Monitoring of some pesticides residue in consumed tea in Tehran market

    Maryam Amirahmadi; Shahram Shoeibi; Mehdi Abdollahi; Hossein Rastegar; Roya Khosrokhavar; Morteza Pirali Hamedani

    2013-01-01

    Abstract Tea is an agricultural product of the leaves, leaf buds, and internodes of various cultivars and sub-varieties of the Camellia sinensis plant, processed and vulcanized using various methods. Tea is a main beverage in Iranian food basket so should be free from toxic elements such as pesticides residue. There is no data bank on the residue of pesticides in the consumed black tea in Iran. The present study is the first attempt for monitoring of 25 pesticide residues from different chemi...

  17. Perspective on Dietary Risk Assessment of Pesticide Residues in Organic Food

    Charles M. Benbrook

    2014-05-01

    Full Text Available Previous studies have shown that organically produced food has lower risks of pesticide contamination than food that is not organically produced. However, organically produced food is not entirely free of pesticide residues. A large, high-quality U.S. Department of Agriculture database reports pesticide residues in several dozen organic and conventionally grown foods on an annual basis, and supports detailed analyses of the frequency of residues in conventional and organic food, the number of residues found in an average sample of food, residue levels, and potential dietary risk. These data are used to estimate pesticide dietary exposures and relative risk levels, and to assess the impacts of the current pesticide-related provisions of the National Organic Program (NOP rule. Fraud appears to be rare based on the available data. Most prohibited residues found in organic produce are detected at levels far below the residues typically found in food grown with pesticides. Relatively high-risk residues are more common in imported foods—both organic and conventional—compared to domestically grown food. The authors conclude that incorporating relative dietary risk into the organic standard would be a more precautionary, risk-based approach than targeting enforcement to organic foods found to contain 5% or more of the applicable Environmental Protection Agency (EPA tolerance.

  18. The Assessment of Pesticides Residues in Some Organic Cultivated and Wild-Collected Medicinal Plants in Albania

    FERDI BRAHUSHI; ENDRIT KULLAJ

    2014-01-01

    Pesticide residues in environment are found in soil, water and plants due to the extensive use of pesticides for agricultural purposes. The residues of pesticides in medicinal plants are of high concern as they are toxic for human life since these plants are used for medicinal purposes. The objective of current study was to estimate the presence of pesticide residues in some organic cultivated and wild-collected medicinal plants in Albania during the years 2010–2013. The determination of pest...

  19. Pesticide management and their residues in sediments and surface and drinking water in the Mekong Delta, Vietnam.

    Toan, Pham Van; Sebesvari, Zita; Bläsing, Melanie; Rosendahl, Ingrid; Renaud, Fabrice G

    2013-05-01

    Public concern in Vietnam is increasing with respect to pesticide pollution of the environment and of drinking water resources. While established monitoring programs in the Mekong Delta (MD) focus on the analysis of organochlorines and some organophosphates, the environmental concentrations of more recently used pesticides such as carbamates, pyrethroides, and triazoles are not monitored. In the present study, household level pesticide use and management was therefore surveyed and combined with a one year environmental monitoring program of thirteen relevant pesticides (buprofezin, butachlor, cypermethrin, α-endosulfan, β-endosulfan, endosulfan-sulfate, fenobucarb, fipronil, isoprothiolane, pretilachlor, profenofos, propanil, and propiconazole) in surface water, soil, and sediment samples. The surveys showed that household level pesticide management remains suboptimal in the Mekong Delta. As a consequence, a wide range of pesticide residues were present in water, soil, and sediments throughout the monitoring period. Maximum concentrations recorded were up to 11.24 μg l(-1) in water for isoprothiolane and up to 521 μg kg(-1) dm in sediment for buprofezin. Annual average concentrations ranged up to 3.34 μg l(-1) in water and up to 135 μg kg(-1) dm in sediment, both for isoprothiolane. Occurrence of pesticides in the environment throughout the year and co-occurrence of several pesticides in the samples indicate a considerable chronic exposure of biota and humans to pesticides. This has a high relevance in the delta as water for drinking is often extracted from canals and rivers by rural households (GSO, 2005, and own surveys). The treatment used by the households for preparing surface water prior to consumption (flocculation followed by boiling) is insufficient for the removal of the studied pesticides and boiling can actually increase the concentration of non-volatile pollutants. PMID:23500396

  20. Comparison of Target and Non-target Mortality Rates from Residual Pesticide on HESCO Material

    We conducted a series of tests to determine if pesticides applied as persistent treatments (residual pesticides) to militarily relevant textile materials to kill mosquitoes, flies, and other disease and nuisance pests might also impact populations of beneficial insects. We exposed samples of pestic...

  1. Pesticide residues in individual versus composite samples of apples after fine or coarse spray quality application

    Poulsen, Mette E.; Wenneker, Marcel; Withagen, Jacques; Christensen, Hanne B.

    2012-01-01

    In this study, field trials on fine and coarse spray quality application of pesticides on apples were performed. The main objectives were to study the variation of pesticide residue levels in individual fruits versus composite samples, and the effect of standard fine spray quality application...

  2. Environmental impact and remediation of residual lead and arsenic pesticides in soil

    Lead arsenate (PbHAsO4) was used as a pesticide for over 50 years in orchards throughout the world, and residual lead and arsenic have been found in high concentrations in these orchard soils long after the pesticide use ended. These high concentrations of lead and arsenic may create a potential ri...

  3. [Rapid screening of 176 pesticide residues in vegetables by ultra fast liquid chromatography-tandem mass spectrometry].

    Zheng, Shuning; Li, Lingyun; Lin, Huan; Zhao, Wen; Zhang, Yanguo; Yao, Zhoulin; Liu, Su

    2013-01-01

    A multiresidue analytical method for rapid screening of 176 pesticide residues in vegetables was developed by using ultra fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS). The vegetable samples were extracted by acetonitrile. It is not necessary for the extract to make a further purification after salting out. Multiple reaction monitoring with information-dependent acquisition of enhanced product ion (MRM-IDA-EPI) was used for the analysis. Based on EPI spectra and chromatographic peak area, identification and quantification of the 176 pesticide residues in vegetables were carried out by using library search technique. All the pesticides had the good linearity within their respective linear ranges (r > 0.99). The average recoveries of the 174 pesticides except for carbosulfan and cyromazine were in the range of 72.4% to 126.4% with the relative standard deviations (RSDs) from 1.0% to 18.7%. The limits of detection and quantification of the method were 0.005 - 2.0 microg/kg and 0.1 - 10 microg/kg, respectively. The results demonstrated that the method has distinct advantages of rapid speed, high sensitivity and good accuracy. Therefore, this method is suitable for the rapid screening of pesticide residues in vegetables. PMID:23667993

  4. Health Risk Assessment of Pesticide Residues via Dietary Intake of Market Vegetables from Dhaka, Bangladesh

    Md. Shakhaoat Hossain

    2013-02-01

    Full Text Available The present study was designed to assess the health risk of pesticide residues via dietary intake of vegetables collected from four top agro-based markets of Dhaka, Bangladesh. High performance liquid chromatography with a photo diode array detector (HPLC-PDA was used to determine six organophosphorus (chlorpyrifos, fenitrothion, parathion, ethion, acephate, fenthion, two carbamate (carbaryl and carbofuran and one pyrethroid (cypermethrin pesticide residues in twelve samples of three common vegetables (tomato, ladys finger and brinjal. Pesticide residues ranged from below detectable limit (<0.01 to 0.36 mg/kg. Acephate, chlorpyrifos, ethion, carbaryl and cypermethrin were detected in only one sample, while co-occurrence occurred twice for fenitrothion and parathion. Apart from chlorpyrifos in tomato and cypermethrin in brinjal, all pesticide residues exceeded the maximum residue limit (MRL. Hazard risk index (HRI for ethion (10.12 and carbaryl (1.09 was found in ladys finger and tomato, respectively. Rest of the pesticide residues were classified as not a health risk. A continuous monitoring and strict regulation should be enforced regarding control of pesticide residues in vegetables and other food commodities.

  5. Review on Sources and Handling Method of Pesticide Residues in Animal Products

    Indraningsih

    2006-06-01

    Full Text Available Field studies and literature search showed that some pesticide residues either organochlorines (OC or organophosphates (OP were detected in animal products (meat and milk . Pesticide residues in meat collected from West Java were detected at the level of 0 .8 ppb lindane and 62 ppb diazinon . While in meat from Lampung was detected at the level of 7 ppb lindane . 2 .7 heptachlor, 0 .8 endosulfan and 0 .5 ppb aldrin . Furthermore, pesticide residues were also detected in the milk collected from West, Central and East Java . The levels of lindane were 2,3 ; 15,9 ; 0,2 ppb ; heptachlor 8 ; 0 .4 and 0,05 ppb; diazinon 8 ; 0 and 1,8 ppb; CPM 0,4 ; 0,8 and 0 ppb ; endosulfan 0,1 ; 0,04 and 0,05 ppb for West, Central and East Java, respectively . The source of pesticide contamination in animal products is generally originated from feed materials, fodders . contaminated soils and water around the farm areas . Minimalization approach of pesticide residues in animal products could be conducted integratedly, such as through chemical process, biodegradation using microorganisms . Organic farming system is recognised as an alternative that may be applied to minimise contamination on agricultural land, eventually reducing pesticide residues in the agricultural products . Feeding with organic agricultural by-products with low pesticide residues appears to reduce pesticide residues in animal products . In order to eliminate pesticide contamination in soil, it has to be conducted progressively by implementing sustainable organic farming .

  6. Effects of processing treatment on pesticide residues in fruits and their products

    The influence of processing treatments on pesticide residues in fruits and their products was reviewed. The effects on pesticide residues and relative control treatments for each processing step, including peeling, washing, sterilization, juicing, clarification, filtration, drying and fermentation, were discussed, respectively. Meanwhile we analyzed the future development prospectin of this field, in order to provide some suggestions for commercial fruit industry and consumers' health. (authors)

  7. Monitoring of some pesticides residue in consumed tea in Tehran market

    Hamedani Morteza Pirali

    2013-01-01

    Full Text Available Abstract Tea is an agricultural product of the leaves, leaf buds, and internodes of various cultivars and sub-varieties of the Camellia sinensis plant, processed and vulcanized using various methods. Tea is a main beverage in Iranian food basket so should be free from toxic elements such as pesticides residue. There is no data bank on the residue of pesticides in the consumed black tea in Iran. The present study is the first attempt for monitoring of 25 pesticide residues from different chemical groups in tea samples obtained from local markets in Tehran, I.R. Iran during the period 2011. A reliable and accurate method based on spiked calibration curve and QuEChERS sample preparation was developed for determination of pesticide residues in tea by gas chromatography–mass spectrometry (GC/MS. The using of spiked calibration standards for constructing the calibration curve substantially reduced adverse matrix-related effects and negative recovery affected by GCB on pesticides. The recovery of pesticides at 3 concentration levels (n = 3 was in range of 81.4 - 99.4%. The method was proved to be repeatable with RSDr lower than 20%. The limits of quantification for all pesticides were ≤20 ng/g. 53 samples from 17 imported and manufactured brand were analyzed. Detectable pesticides residues were found in 28.3% (15 samples of the samples. All of the positive samples were contaminated with unregulated pesticides (Endosulfan Sulfate or Bifenthrin which are established by ISIRI. None of the samples had contamination higher than maximum residue limit set by EU and India.

  8. Monitoring of Some Pesticides Residue in Consumed tea in Tehran Market

    Maryam Amirahmadi

    2013-01-01

    Full Text Available Tea is an agricultural product of the leaves, leaf buds, and internodes of various cultivars and sub-varieties of the Camellia sinensis plant, processed and vulcanized using various methods. Tea is a main beverage in Iranian food basket so should be free from toxic elements such as pesticides residue. There is no data bank on the residue of pesticides in the consumed black tea in Iran. The present study is the first attempt for monitoring of 25 pesticide residues from different chemical groups in tea samples obtained from local markets in Tehran, I.R. Iran during the period 2011. A reliable and accurate method based on spiked calibration curve and QuEChERS sample preparation was developed for determination of pesticide residues in tea by gas chromatography--mass spectrometry (GC/MS. The using of spiked calibration standards for constructing the calibration curve substantially reduced adverse matrix-related effects and negative recovery affected by GCB on pesticides. The recovery of pesticides at 3 concentration levels (n = 3 was in range of 81.4 - 99.4%. The method was proved to be repeatable with RSDr lower than 20%. The limits of quantification for all pesticides were <=20 ng/g. 53 samples from 17 imported and manufactured brand were analyzed. Detectable pesticides residues were found in 28.3% (15 samples of the samples. All of the positive samples were contaminated with unregulated pesticides (Endosulfan Sulfate or Bifenthrin which are established by ISIRI. None of the samples had contamination higher than maximum residue limit set by EU and India.

  9. Biosensors for detection of pesticide residues: current status, challenges and future perspectives

    YAO Xue-Peng

    2013-02-01

    Full Text Available Public concerns over pesticide residues in food had been increasing because of their bioaccumulation effects and their great danger to the environments and human’s heath. It was therefore imperative to detect the pesticide residue using all available analytical methods, especially highly sensitive, simple, rapid and low cost. The biosensor detection strategies held a great promise for the detection of agricultural pesticides, attributing to their key features such as high sensitivity, fast response, robustness, low cost, and miniaturization. This paper reviewed the advances in the design and fabrication of biosensor for pesticide detection and their applications in the food and environment safety. Both advantages and drawbacks of these techniques were summarized. Finally, challenges and perspectives in further developing pesticide biosensors were also discussed.

  10. Occurrence of pesticide non extractable residues in physical and chemical fractions from two natural soils.

    Andreou, K.; Jones, K.; Semple, K.

    2009-04-01

    Distribution of pesticide non extractable residues resulted from the incubation of two natural soils with each of the isoproturon, diazinon and cypermethrin pesticide was assessed in this study. Pesticide non extractable residues distribution in soil physical and chemical fractions is known to ultimately affect their fate. This study aimed to address the fate and behaviour of the non extractable residues in the context of their association with soil physical and chemical fractions with varying properties and characteristics. Non extractable residues were formed from incubation of each pesticide in the two natural soils over a period of 24 months. Soils containing the non extractable residues were fractionated into three solid phase fractions using a physical fractionation procedure as follows: Sediment (SED, >20 ?m), (II) Microaggregate (MA, 20-2 ?m) and (III) Colloid phase (COL, 2-0.05 ?m). Each soil fraction was then fractionated into organic carbon chemical fractionations as follows: Fulvic acid (FA), Humic acid (HA) and Humin (HM). Significant amount of the pesticides was lost during the incubation period. Enrichment factors for the organic carbon and the 14C-pesticide residues were higher in the MA and COL fraction rather than the SED fraction. Greater association and enrichment of the fulvic acid fraction of the organic carbon in the soil was observed. Non extractable residues at the FA fraction showed to diminish while in the HA fraction were increased with decreasing the fraction size. An appreciable amount of non extractable residues were located in the HM fraction but this was less than the amount recovered in the humic substances. Long term fate of pesticide non extractable residues in the soil structural components is important in order to assess any risk associated with them.

  11. Pesticides residues in the Prochilodus costatus (Valenciennes, 1850) fish caught in the São Francisco River, Brazil.

    Oliveira, Fabiano A; Reis, Lilian P G; Soto-Blanco, Benito; Melo, Marília M

    2015-01-01

    The objective of this study was to determine the levels of pesticides in the fish Prochilodus costatus caught in São Francisco River, one of most important rivers in Brazil. Thirty-six fish were captured in three different areas, and samples of the dorsal muscle and pooled viscera were collected for toxicological analysis. We evaluated the presence of 150 different classes of insecticides, fungicides, herbicides and acaricides by multiresidue analysis technique using liquid chromatography-tandem mass spectrometry (LC-MS/MS), with the limit of detection of 5 ppb. In this study, organophosphorus and carbamate pesticides were detected at the highest levels in the caught fish. Among the 41 organophosphorus pesticides surveyed, nine types were detected (chlorpyrifos, diazinon, dichlorvos, disulfoton, ethion, etrimfos, phosalone, phosmet and pyrazophos) in the muscle, viscera pool, or both in 22 (61.1%) fish. Sampled tissues of 20 (55.6%) fish exhibited at least one of the eight evaluated carbamate pesticides and their metabolites: aldicarb, aldicarb sulfoxide, carbaryl, carbofuran, carbosulfan, furathiocarb, methomyl and propoxur. Fungicides (carbendazim, benalaxyl, kresoxim-methyl, trifloxystrobin, pyraclostrobin and its metabolite BF 500 pyraclostrobin), herbicides (pyridate and fluasifop p-butyl), acaricide (propargite) and pyrethroid (flumethrin) were also detected. In conclusion, P. costatus fish caught in the São Francisco River contained residues of 17 different pesticides, in both muscles and the viscera pool, indicating heavy environmental contamination by pesticides in the study area. PMID:25844860

  12. Radiotracer studies of pesticide residues in food plants

    Researches using radiotracers as means for the rapid generation of background data critical for the efficient and safe use of pesticides at the Pesticide Toxicology and Chemistry Laboratory of the National Crop Protection Center, University of the Philippines, Los Banos, Laguna are described. Methodologies as well as results and discussions of the researches done are given. (ELC) 4 tabs.; 11 figs.; 16 refs

  13. Determination of pesticide residue in selected fruits and vegetable

    Food contamination due to indiscriminate use of pesticides has become a serious problem. Fruits samples of tomato, grapes, musk melon, parsimen and vegetable samples of potato, pea, spinach, cabbage and pumpkin ere collected from local market of Peshawar, coming from different regions. All samples were extracted, purified and analyzed for the commonly used pesticides. Dichlorovas, BHC, Atrazine, Daizinon, Methadiathion and Cypermethrin were detected by Gas Chromatography. These pesticides were detected in vegetable samples Id Atrazine were found in potato sample and not detected in other samples. Large concentration of Cypermethrin (44.6) was detected in the pea sample. All the vegetables samples have maximum concentration of pesticides, which is higher than their MRLs, but in pumpkin no one of the above pesticides were detected. In fruits samples, dichlorovas, atrazine, diazinon, methadiathion. Cypermethrin were detected. BHC was not present in fruits samples. All these pesticides were above the MRLs. The study concluded that agriculture crops are highly contaminated due to the uncontrolled use of pesticides in project area and suggested that pesticides should be applied in calculated dose to avoid resistance and persistence due to over and under dose application. (author)

  14. Multi-class, multi-residue analysis of pesticides, polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenyl ethers and novel flame retardants in fish using fast, low-pressure gas chromatography–tandem mass spectrometry

    Highlights: ► A method for analysis of POPs and novel flame retardants in catfish was developed. ► The method is based on a QuEChERS extraction, d-SPE clean-up and low pressure GC/MS–MS. ► The method validation demonstrated good recoveries and low detection limits. ► The method was successfully applied for analysis of catfish samples from the market. - Abstract: A multi-class, multi-residue method for the analysis of 13 novel flame retardants, 18 representative pesticides, 14 polychlorinated biphenyl (PCB) congeners, 16 polycyclic aromatic hydrocarbons (PAHs), and 7 polybrominated diphenyl ether (PBDE) congeners in catfish muscle was developed and evaluated using fast low pressure gas chromatography triple quadrupole tandem mass spectrometry (LP-GC/MS–MS). The method was based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction with acetonitrile and dispersive solid-phase extraction (d-SPE) clean-up with zirconium-based sorbent prior to LP-GC/MS–MS analysis. The developed method was evaluated at 4 spiking levels and further validated by analysis of NIST Standard Reference Materials (SRMs) 1974B and 1947. Sample preparation for a batch of 10 homogenized samples took about 1 h/analyst, and LP-GC/MS–MS analysis provided fast separation of multiple analytes within 9 min achieving high throughput. With the use of isotopically labeled internal standards, recoveries of all but one analyte were between 70 and 120% with relative standard deviations less than 20% (n = 5). The measured values for both SRMs agreed with certified/reference values (72–119% accuracy) for the majority of analytes. The detection limits were 0.1–0.5 ng g−1 for PCBs, 0.5–10 ng g−1 for PBDEs, 0.5–5 ng g−1 for select pesticides and PAHs and 1–10 ng g−1 for flame retardants. The developed method was successfully applied for analysis of catfish samples from the market.

  15. Pesticide residues in raspberries (Rubus idaeus L.) and dietary risk assessment.

    ?ozowicka, B; Kaczy?ski, P; Jankowska, M; Rutkowska, E; Hrynko, I

    2012-01-01

    The aim of this study was to evaluate the residues of 140 pesticides in raspberries from north-eastern Poland (2005-2010). Gas chromatography with electron capture detector (GC-ECD) and nitrogen phosphorous detector (GC-NPD) was used. Among the 128 samples, 66 (51.6%) were found to detect residues: 14.1% contained one pesticide and around 38% multiple pesticide residues. The most frequently detected were pyrimethanil residues (36.0%). Twenty-seven (21.1%) raspberry samples exceeded the maximum residue limits. The estimated daily intakes ranged from 0.003% to 3.183% of the acceptable daily intake (ADI) for adults 0.008% and 9.7% for toddlers, respectively. The most critical case is procymidone, the acute risk was 180.9% of acute reference dose (ARfD) for toddlers and for adults (83% of ARfD) which is high. PMID:24779781

  16. Detection of Organochlorine and Organophosphorus Pesticides Residues in Water Samples of Taragong Thana in Rangpur District in Bangladesh

    Arafin Gulsan Ara

    2014-02-01

    Full Text Available This study was undertaken to identify Organochlorine and Organophosphorous pesticides residues in water samples of some paddy fields, ponds and tubewells in Rangpur district (Taragong Thana of Bangladesh by using High Performance Liquid Chromatography (HPLC. Among thirty samples, Organophosphorus (Malathion pesticide was found in twelve samples while Organocholorine was absent. The level of the pesticide residues (Malathion were found in the range of 2 to 221 ppm, which were above the maximum acceptable levels of total and individual pesticide contamination.

  17. Influence of the processing factors on pesticide residues in fruits and vegetables and its application in consumer risk assessment

    Keikotlhaile, Boitshepo Miriam

    2011-01-01

    Pesticides are widely used in food production to increase food security despite the fact that they can have negative health effects on consumers. Pesticide residues have been found in various fruits and vegetables; both raw and processed. One of the most common routes of pesticide exposure in consumers is via food consumption. Most foods are consumed after passing through various culinary and processing treatments. In this thesis the influence of the processing factors on pesticide residues i...

  18. Organochlorine Pesticide Residues in the Major Rivers of Southern Thailand

    Abd Naser Haji Samoh

    2009-01-01

    Full Text Available Environmental contaminations by organochlorine pesticides (OCPs of inland water have been a global issue, since most of these compounds are very persistent, bioaccumulative and toxic compounds. Due to the widespread use of DDT for malaria vector eradication programs in the past and no comprehensive works have been conducted to assess trace organic pollutants in river waters, this work is the first effort to assess the contamination levels of OCPs in the major rivers of Southern Thailand. The objectives of this study were to determine the concentration levels of OCPs and oil and grease in the 3 major rivers and to compare the present results with surrounding regions for further assessment of OCPs contamination status in inland waters of Southern Thailand. The water samples were collected along the 3 major rivers (Saiburi, Patani and Tiba River during June 2007-February 2008. Water samples were solid phase extracted with Supelco C-18 cartridge (1g/6 mL and quantified by gas chromatograph (GC-ECD. The concentration of oil and grease was determined by gravimetric method and reported as hexane extractable material (HEM and silica gel treated hexane extractable material (SGT-HEM. Several parameters of waters such as total suspended solid, pH, turbidity, and conductivity were measured. The commonly found OCP residues in these rivers were β-HCH, γ-HCH, heptachlor epoxide, endosulfan 1, p,p’- DDE and endrin aldehyde. The overall results showed that Saiburi River was more polluted with OCPs than Patani and Tiba River, especially p, p’-DDE which was detected in the wide range concentration of 9.6 to 203.1 ng/mL. For oil and grease contamination, Tiba River waters were found to be more polluted than either Patani or Saiburi River. The experimental procedures and analytical results together with the possible sources of OCPs and its environmental impacts are presented.

  19. Production of apple-based baby food: changes in pesticide residues.

    Kovacova, Jana; Kocourek, Vladimir; Kohoutkova, Jana; Lansky, Miroslav; Hajslova, Jana

    2014-01-01

    Apples represent the main component of most fruit-based baby food products. Since not only fruit from organic farming, but also conventionally grown fruit is used for baby food production, the occurrence of pesticide residues in the final product is of high concern. To learn more about the fate of these hazardous compounds during processing of contaminated raw material, apples containing altogether 21 pesticide residues were used for preparation of a baby food pure both in the household and at industrial scale (in the baby food production facility). Within both studies, pesticide residues were determined in raw apples as well as in final products. Intermediate product and by-product were also analysed during the industrial process. Determination of residues was performed by a sensitive multi-detection analytical method based on liquid or gas chromatography coupled with mass spectrometry. The household procedure involved mainly the cooking of unpeeled apples, and the decrease of residues was not extensive enough for most of the studied pesticides; only residues of captan, dithianon and thiram dropped significantly (processing factors less than 0.04). On the other hand, changes in pesticide levels were substantial for all tested pesticides during apple processing in the industrial baby food production facility. The most important operation affecting the reduction of residues was removal of the by-products after pulping (rest of the peel, stem, pips etc.), while subsequent sterilisation has an insignificant effect. Also in this case, captan, dithianon and thiram were identified as pesticides with the most evident decrease of residues. PMID:24720736

  20. Occurrence of non extractable pesticide residues in physical and chemical fractions of two soils

    Andreou, Kostas; Semple, Kirk; Jones, Kevin

    2010-05-01

    Soils are considered to be a significant sink for organic contaminants, including pesticides, in the environment. Understanding the distribution and localisation of aged pesticide residues in soil is of great importance for assessing the mobility and availability of these chemicals in the environment. This study aimed to characterise the distribution of radiolabeled herbicide isoproturon and the radiolabeled insecticides diazinon and cypermethrin in two organically managed soils. The soils were spiked and aged under laboratory conditions for 17 months. The labile fraction of the pesticides residues was recovered in CaCl2 (0.01M) and then subjected to physical size fractionation using sedimentation and centrifugation steps, with >20μm, 20-2μm and 2-0.1μm soil factions collected. Further, the distribution of the pesticide residues in the organic matter of the fractionated soil was investigated using a sequential alkaline extraction (0.1N NaOH) into humic and fulvic acid and humin. Soil fractions of 20-2μm and 2-0.1μm had the largest burden of the 14C-residues. Different soil constituents have different capacities to form non-extractable residues. Soil solid fractions of 20-2 µm and 20 µm). Fulvic acid showed to play a vital role in the formation and stabilisation of non-extractable 14C-pesticide residues in most cases.Assessment of the likelihood of the pesticide residues to become available to soil biota requires an understanding of the structure of the SOM matrix and the definition of the kinetics of the pesticide residues in different SOM pools as a function of the time.

  1. Pesticide residues in the marine environment and analytical quality assurance of the results

    A brief review is given of the information that is available on the distribution and levels of pesticide residues in marine systems. Residues detected in coastal waters largely reflect the regional use of pesticides (e.g. DDTs, atrazine), although for more volatile and environmentally persistent compounds (e.g. hexachlorocyclohexane, lindane) long range atmospheric transport also contributes to their far field dispersal in the oceans. Despite the increasing number of pesticide reports in the scientific literature, data on residues are still very scarce for extensive coastal areas in regions of intensive pesticide usage such as the tropics. Therefore, the aim of IAEA Co-ordinated Research Programmes is to assist with the implementation of pesticide monitoring in tropical coastal ecosystems and with experimental research on pesticide cycling and its effects on the marine environment. The results of worldwide laboratory intercomparison exercises organized by the IAEA for analyses of the organochlorine pesticides in marine samples highlight the need to further improve quality control of the analytical results. Although research on marine contamination by pesticide residues is progressing, in view of the high number of compounds and formulations in use it is unlikely that all the data required for environmental risk assessment of agrochemical residues in marine ecosystems will be generated with sufficient rapidity. Therefore, enhanced development through experimental research with model compounds and subsequent modelling is required. Nevertheless, from current knowledge it is clear that environmental management programmes for coastal ecosystems should urgently adopt measures to prevent or reduce the impact of agrochemical residues on biological resources such as fisheries and aquaculture. (author). 71 refs, 7 figs, 2 tabs

  2. Monitoring pesticide residues in greenhouse tomato by combining acetonitrile-based extraction with dispersive liquid-liquid microextraction followed by gas-chromatography-mass spectrometry.

    Melo, Armindo; Cunha, Sara C; Mansilha, Catarina; Aguiar, Ana; Pinho, Olvia; Ferreira, Isabel M P L V O

    2012-12-01

    A multiclass and multiresidue method for pesticide analysis in tomato was validated. Extraction and pre-concentration of the pesticide residues from acetonitrile extracts was performed by using dispersive liquid-liquid microextraction (DLLME) technique, followed by gas chromatography-mass detection. DLLME was performed using carbon tetrachloride as extractive solvent and acetonitrile extract as dispersive solvent, in order to increase enrichment factor of the extraction procedure. Validation parameters indicated the suitability of the method for routine analyses of thirty pesticides in a large number of samples. In general, pesticide recoveries ranged between 70% and 110% and repeatability ranged between 1% and 20%. The proposed method was applied to the monitoring of pesticides in tomatoes grown during winter in greenhouses. Among the compounds considered in this work, cyprodinil was found in tomato at concentrations of 0.33mg/kg, other pesticides like azoxystrobin, fenhexanid, tolyfluanid, ?-cyhalothrin and trifloxystrobin were also detected, but, not quantified. PMID:22953826

  3. Multiresidue pesticide analysis by capillary gas chromatography-mass spectrometry.

    Wong, Jon W; Zhang, Kai; Hayward, Douglas G; Kai-Meng, Chin

    2011-01-01

    A multiresidue pesticide method using a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) procedure and capillary gas chromatography-mass spectrometry (GC-MS) is described for the determination of 166 organochlorine, organophosphorus, and pyrethroid pesticides, metabolites, and isomers in spinach. The pesticides from spinach were extracted using acetonitrile saturated with magnesium sulfate and sodium chloride, followed by solid-phase dispersive cleanup using primary-secondary amine and graphitized carbon black sorbents and toluene. Analysis is performed using different GC-MS techniques emphasizing the benefits of non-targeted acquisition and targeted screening procedures. Non-targeted data acquisition of pesticides in the spinach was demonstrated using GC coupled to a single quadrupole mass spectrometery (GC-MS) in full scan mode or multidimensional GC-time-of-flight mass spectrometery (GC ? ?GC-TOF/MS), along with deconvolution software and libraries. Targeted screening was achieved using GC-single quadrupole mass spectrometry in selective ion monitoring (GC-MS/SIM) mode or -tandem mass spectrometry (GC-MS/MS) in multiple reaction monitoring mode. The development of these techniques demonstrates the powerful use of GC-MS for the screening, identification, and quantitation of pesticide residues in foods. PMID:21643907

  4. Pesticide residues in the water and fish (lagoon tilapia samples from lagoons in Ghana

    D.K. Essumang

    2009-04-01

    Full Text Available This study was to ascertain the presence and subsequent amount of four organochlorine pesticides: dichlorodiphenyl dichloroethylene (2,4’-DDE, 4,4’-dichlorodiphenyldichloroethane (4,4’-DDD, p,p’-dichloro- diphenyltrichloroethane [p,p’-DDT (r (i (f] and Propiconazol (f; and four organophosphorous pesticides: Fenitrothion (i, Chlorpyrifos (i, Dichlorvos (a (i and Diazinon (a (i in Chemu lagoon (Tema, Korle lagoon (Accra, Fosu lagoon (Cape Coast and the Etsii lagoon (Abandzi. Liquid-liquid and liquid-solid extraction technique was employed to extract pesticide residues in water and fish samples, respectively, using 1:1 (v/v ethyl acetate/dichloromethane mixture before being analyzed by gas chromatography. The highest level of pesticide contaminations was recorded in the Chemu lagoon as compared to the Korle lagoon and Fosu lagoon, with the Etsii lagoon showing the least contamination. The total average pesticide residues in water samples from the four lagoons: Chemu, Korle, Fosu and Etsii are 2.6384 mg/L, 0.4992 mg/L, 0.3045 mg/L and 1.3629 mg/L, respectively. The total average pesticide residues obtained in fish samples (Sarotherodon melaanothern from the Fosu and Etsii lagoons are 0.0155 mg/kg and 0.0088 mg/kg, respectively. This shows some level of exposure of pesticide which would be harmful to human.

  5. 75 FR 53690 - Notice of Receipt of Pesticide Petition Filed for Residues of Potassium Peroxymonosulfate in or...

    2010-09-01

    ... AGENCY Notice of Receipt of Pesticide Petition Filed for Residues of Potassium Peroxymonosulfate in or on... regulations for residues of potassium peroxymonosulfate in or on various commodities. DATES: Comments must be... for residues of pesticide chemicals in or on various food commodities. EPA has determined that...

  6. Method for Reduction of Pesticide Residue Levels in Raspberry and Blackcurrant Based on Utilization of Ozone

    Balawejder Maciej

    2014-12-01

    Full Text Available The method for the reduction of pesticide residues in soft fruits based on utilization of ozone was proposed. The procedure allows for effective reduction of boscalid residues by 38% in raspberries, and about 58% thiram in blackcurrants. Furthermore, it can be used on an industrial scale.

  7. Monitoring of multiple pesticide residues in some fruits in Karachi, Pakistan

    One hundred and twenty samples of different fruits including apple, apricot, persimmon, chiku, citrus, grapes, guava, mango, papaya, peach, plum and pomegranate procured from different selling points of Karachi, Pakistan during 2008-2009, were analyzed for monitoring of multiple pesticide residues using GC/FID and HPLC/UV. The results showed exceeding level of contamination. On an average 62.5% samples contained residues of pesticides while 22% samples exceeded the maximum residue limits (MRLs) as given by FAO/WHO (Anon., 2000). (author)

  8. Survey of pesticide residues in table grapes: Determination of processing factors, intake and risk assessment

    Poulsen, Mette Erecius; Hansen, H.K.; Sloth, Jens Jørgen; Christensen, Hanne Bjerre; Andersen, Jens Hinge

    2007-01-01

    The differences in residue pattern between Italy and South Africa, the main exporters of table grapes to the Danish market, were investigated. The results showed no major differences with respect to the number of samples with residues, with residues being found in 54-78% of the samples. Exceedances......). However, no significant effect was found for organophosphorus pesticides and pyrethroids, whereas the number of samples with residues of benzilates, phenylamids and triazoles was insufficient to demonstrate any significant effects. An intake calculation showed that the average intake from Italian grapes...... was 3.9 mu g day(-1) for pesticides and 21 mu g day(-1) for copper. Correspondingly, the intakes from South African grapes were 2.6 and 5.7 mu g day(-1) respectively. When the total exposure of pesticides from grapes were related to acceptable daily intake, expressed as the sum of Hazard Quotients...

  9. The Assessment of Pesticides Residues in Some Organic Cultivated and Wild-Collected Medicinal Plants in Albania

    FERDI BRAHUSHI

    2014-06-01

    Full Text Available Pesticide residues in environment are found in soil, water and plants due to the extensive use of pesticides for agricultural purposes. The residues of pesticides in medicinal plants are of high concern as they are toxic for human life since these plants are used for medicinal purposes. The objective of current study was to estimate the presence of pesticide residues in some organic cultivated and wild-collected medicinal plants in Albania during the years 2010–2013. The determination of pesticides residues in medicinal plants was achieved by using extraction of plant material with organic solvent, clean up procedure and followed by detection with chromatography techniques. Among the detected pesticide residuesin the wild–collected plants as Malva sylvestris, Fragaria vesca, Bellis perennis were DDT, Dimethoat, Pirimiphos-methyl, Chlorpyriphos-ethyl, Carbendazim/Benomyl, Acetamiprid and Diphenylamine. Whereas in the cultivated medicinal plants as Calendula officinalis, Centaurea cyani, Salvia officinalis, Sideritis raeseri, the most common detected pesticide residues were Dimethoat, Chlorpyriphos, Pirimiphos-methyl, DDT and Carbendazim. The presence of pesticides in medicinal plant is related to the past use of pesticides as DDT and actual use of pesticides like Dimethoat, Pirimiphos-methyl, Chlorpyriphos, Acetamiprid, etc. Therefore, the quality of medicinal plants can be evaluated through estimation of pesticides residues in medicinal plants and comparison of the obtained values with acceptable limit values.

  10. Exposure of several Belgian consumer groups to pesticide residues through fresh fruit and vegetable consumption

    Claeys, Wendie L.; Schmit, Jean-François; Bragard, Claude; Maghuin-Rogister, Guy; Pussemier, Luc; Schiffers, Bruno

    2011-01-01

    The output of a pesticide surveillance program (detection frequency and number of exceeding measures) can lead to unnecessary concern among consumers since they lack information concerning the actual exposure. In this study, the exposure to pesticide residues through fruit and vegetable consumption is evaluated based on the 2008 surveillance data of the Belgian Federal Agency for the Safety of the Food Chain (FASFC). Results (deterministic and probabilistic approach) demonstrate that the c...

  11. Classification and modelling of non-extractable residue (NER) formation from pesticides in soil

    Kästner, M.; Nowak, K. M.; Miltner, A.; Trapp, Stefan; Schaeffer, A.

    2015-01-01

    This presentation provides a comprehensive overview about the formation of nonextractable residues (NER) from organic pesticides and contaminants in soil and tries classifying the different types. Anthropogenic organic chemicals are deliberately (e.g. pesticides) or unintentionally (e.g. polyaromatic hydrocarbons [PAH], chlorinated solvents,pharmaceuticals) released in major amounts to nearly all compartments of the environment. Soils and sediments as complex matrices provide a wide variety o...

  12. SETTING MRLS FOR PESTICIDE RESIDUES IN FOOD BASED ON EU UNIFORM CRITERIA

    Valentina L. Christova-Bagdassarian; JULIETA A. TISHKOVA; JULIANA RUMENOVA TASHEVA-PETKOVA; Atanassova, M.

    2014-01-01

    Objective: Pesticides are used worldwide. They are applied during the growing season and part of the amount may remain in or on treated crop. Pesticides can drift to nearby areas and contaminate crops that were not treated. The MRLs are the maximum amount of a pesticide permitted in or on food (& feed), expressed in mg/kg or ppm and always defined for the active substance – crop combination. MRL should be set according to residue trials under Good Agricultural Practice (GAP) and under the con...

  13. Solid phase extraction and chromatographic determination of pesticide residues in water samples: DDT and its metabolites

    Solid phase extraction cartridge embedded with octadecyl C/sub 18/ chain bounded to silica particles were used for the isolation and trace enrichment of pesticides from water samples collected from cotton, rice growing and municipal areas. The eluents were analyzed with HPLC using methanol (100%) as mobiles phase at different UV-Visible wavelengths. DDT and its metabolites were found in all areas but were not present in all samples. Concentration of pesticide residues varies from sample to sample and was in the range of 0.017 ng ml/sup -1/. Overall, recoveries ranged from 84%-91% for all target pesticides. (author)

  14. Survey of pesticide residues in table grapes: Determination of processing factors, intake and risk assessment

    Poulsen, Mette Erecius; Hansen, H.K.; Sloth, Jens Jørgen; Christensen, Hanne Bjerre; Andersen, Jens Hinge

    2007-01-01

    ). However, no significant effect was found for organophosphorus pesticides and pyrethroids, whereas the number of samples with residues of benzilates, phenylamids and triazoles was insufficient to demonstrate any significant effects. An intake calculation showed that the average intake from Italian grapes...... was 3.9 mu g day(-1) for pesticides and 21 mu g day(-1) for copper. Correspondingly, the intakes from South African grapes were 2.6 and 5.7 mu g day(-1) respectively. When the total exposure of pesticides from grapes were related to acceptable daily intake, expressed as the sum of Hazard Quotients...

  15. Assessment of pesticide residues in strawberries grown under various treatment regimes.

    Kovacova, Jana; Hrbek, Vojtech; Kloutvorova, Jana; Kocourek, Vladimir; Drabova, Lucie; Hajslova, Jana

    2013-01-01

    The dynamics of pesticide residues in strawberries that involved quantification of pesticide residues in ripe fruits after model treatment was evaluated in repeated field trials conducted over 3 years. Sixteen commercial pesticide formulations in various combinations were employed in applications from 7 to 44 days before harvest. Altogether 21 active ingredients and some of their metabolites were determined in treated strawberries using LC-MS and GC-MS methods. Except for propargite, the concentrations of all active ingredients declined below the respective MRLs (Regulation (EC) No. 396/2005); nevertheless, most of the tested fungicides often persisted above the 0.01 mg kg? limit required by baby food producers to avoid the risk of exceeding the 'baby food limit' established in Commission Directive 2006/141/EC. On the other hand, residues of the majority of tested insecticides, namely spinosad, pymetrozine, deltamethrin, lambda-cyhalothrin and azadirachtin, declined below this limit. PMID:24303788

  16. Pesticides Residues in Smoked Fish Samples from North-Eastern Nigeria

    A. Mustapha

    2010-01-01

    Full Text Available Smoked fish species, Clarias sp., Gymnarchus niloticus and Tilapia sp., sampled from the open markets in North-Eastern Nigeria were investigated for the presence and concentration levels of pesticide residues of DDT, dichlorvos and lindane. The GC-MS and GC-FID techniques were employed in the determination of the pesticide residue. The obtained results showed positive identification of op-DDT (2.844-4.220 μg g-1, pp-DDT (3.821-4.479 μg g-1, dichlorvos (2.844-4.220 μg g-1 and lindane (3.479-9.878 μg g-1. Gymnarchus niloticus showed consistently higher pesticide residue levels in the studied smoked fish samples followed by Clarias sp. and then Tilapia sp.

  17. Photoacoustic Spectroscopy as a Non-destructive Tool for Quantification of Pesticide Residue in Apple Cuticle

    Liu, Lixian; Wang, Yafei; Gao, Chunming; Huan, Huiting; Zhao, Binxing; Yan, Laijun

    2015-06-01

    Photoacoustic spectroscopy (PAS), the non-destructive method to detect residue of dimethyl-dichloro-vinyl-phosphate (DDVP) pesticide in a cuticle of apple, is described. After constructing the PA experimental setup and identifying three characteristic peaks of DDVP in the near ultraviolet region, the PA spectra of an apple cuticle contaminated with DDVP were collected. The artificial neural network method was then applied to analyze data quantitatively. The results show a correlation coefficient exceeding 0.99 and a detection limit of 0.2 ppm, which is within the national food safety standard for maximum residue limits for pesticides in food (GB 2763-2012). This fact and the non-destructive character of PAS make the approach promising for detection of pesticide residue in fruits.

  18. Monitoring and risk assessment of 74 pesticide residues in Pu-erh tea produced in Yunnan, China.

    Chen, Hongping; Wang, Qinghua; Jiang, Ying; Wang, Chuanpi; Yin, Peng; Liu, Xin; Lu, Chengyin

    2015-01-01

    A number of 100 Pu-erh tea samples from the 2013 harvest in Yunnan Province (China) were analysed for 74 pesticides. A total of 11 pesticides were detected. At least one pesticide was detected in 56% of the samples. None of these samples contained the 74 monitored pesticides at concentrations above the Chinese maximum residual levels. Imidacloprid, bifenthrin and acetamiprid were most frequently found, with percentages of 53%, 46% and 31%, respectively. These were also the top three pesticides with maximum concentrations of 140, 246 and 672 μg kg⁻¹, respectively. Residual levels of the monitored pesticides showed no significant correlation with the production time or area of Pu-erh tea. Whereas a high incidence of pesticide residues was detected in Pu-erh tea, the contamination levels observed do not pose any serious health risks. PMID:25308103

  19. Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification

    Book Chapter 18, titled Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification, will be published in the book titled High Performance Liquid Chromatography in Pesticide Residue Analysis (Part of the C...

  20. Residual Effects of Some Conventional and Biorational Pesticides on Ladybird Beetle, Adonia variegata Goeze

    Mohammed A. Al-Doghairi; Suloiman AL-Rehiayani; Osman, Khaled A.; Eltayeb A. Elhag

    2004-01-01

    A variety of pesticides is used in alfalfa field to control pests. Biological control agents are also used to control these pests, therefore it is important to understand the effects of such pesticides on these beneficial insects. The present study was carried out to examine the residual effects of Dursban and Fenvalerate as conventional pesticides as well as Bio-Fly and Bio-Neem as biorational pesticides on ladybird beetle, Adonia variegata Goeze using panel exposure technique. Dursban was h...

  1. Pesticides Residues in Smoked Fish Samples from North-Eastern Nigeria

    A. Mustapha; Y.I. Adamu; S.S. Hati; U. Musa

    2010-01-01

    Smoked fish species, Clarias sp., Gymnarchus niloticus and Tilapia sp., sampled from the open markets in North-Eastern Nigeria were investigated for the presence and concentration levels of pesticide residues of DDT, dichlorvos and lindane. The GC-MS and GC-FID techniques were employed in the determination of the pesticide residue. The obtained results showed positive identification of op-DDT (2.844-4.220 μg g-1), pp-DDT (3.821-4.479 μg g-1), dichlorvos (2.844-4.220 μg g-1) and lindane (3.479...

  2. A multi-residue method for the determination of pesticides in tea using multi-walled carbon nanotubes as a dispersive solid phase extraction absorbent.

    Hou, Xue; Lei, Shaorong; Qiu, Shiting; Guo, Lingan; Yi, Shengguo; Liu, Wei

    2014-06-15

    A modified QuEChERS (quick, easy, cheap, effective, rugged and safe) method using multi-walled carbon nanotubes (MWCNTs) as a dispersive solid phase extraction (d-SPE) absorbent was established for analysis of 78 pesticide residues in tea. A 6 mg MWCNT sample was selected as the optimised amount based on the distribution of pesticide recoveries and clean-up efficiency from 6 mL acetonitrile extracts. The matrix effects of the method were evaluated and matrix-matched calibration was recommended. The method was validated employing gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) at the spiked concentration levels of 0.05, 0.1 and 0.15 mg kg(-1). For most of the targeted pesticides, the percent recoveries range from 70% to 120%, with relative standard deviations (RSDs) pesticide residues. PMID:24491709

  3. Isotopic control of methods for the determination of residues of chlorinated hydrocarbon pesticides Pt. 1

    The determination of residues of chlorinated hydrocarbon pesticides is of importance mainly in case of foods of animal origin. However, this determination is made slower or even inhibited by a number of difficulties. Extraction and clean-up procedures are of primary importance even in case of the most polished methods of pesticide analysis problems. The isotopic method was used for testing the mentioned steps. Experiments were carried out with radioactive C-14 isotope. According to the results of control tests, data varying within relatively wide limits have been obtained, depending on the applied method. In each case where the boiling point of the solvent permits, the use of the Kuderna--Danish instrument is advisable. In case of a solvent of higher boiling point a combined method is more expedient. For this purpose a method has been suggested which enables the evaporation of the sample to be carried out without any practical loss of agent, thus the obtained analytical results can be considered as perfectly reliable ones. (P.J.)

  4. Assessment of Pesticide Residues in Some Fruits Using Gas Chromatography Coupled with Micro Electron Capture Detector

    M. I. Bhanger

    2011-12-01

    Full Text Available A very sensitive analytical method for the determination of 26 pesticides in some fruits based on solid phase extraction (SPE cleanup was developed using gas chromatography (GC coupled with micro electron capture detector (μECD. The identity of the pesticides was confirmed by gas chromatography mass spectroscopy (GC-MS using selected ion monitoring (SIM mode. Ethyl acetate was used as a solvent for the extraction of pesticide residues with assistance of sonication. For cleanup an octadecyl, C18 SPE column was used. A linear response of μECD was observed for all pesticides with good correlation coefficients (>0.9992. Proposed method was successfully applied for the determination of pesticide residues in the orange, apple, and grape fruits. Average recoveries achieved for all of the pesticides at fortification levels of 0.05, 1.0 and 2.0 μg g-1 in analyzed fruits were above 90% with relative standard deviations (RSD less than 6

  5. Monitoring survey of the use patterns and pesticide residues on vegetables in the Niayes zone, Senegal.

    Diop, Amadou; Diop, Yrim M; Thiar, Dine D; Cazier, Fabrice; Sarr, Serigne O; Kasprowiak, Amaury; Landy, David; Delattre, Franois

    2016-02-01

    The main objective of this work was to determine the impact of pesticide use practices on vegetables contamination in the Niayes zone of Dakar. A preliminary survey involving 200 farmers, showed the application of pesticides belonging to different groups on vegetable crops. Use practices in terms of application intervals and methods, measuring tools and dosage were not in compliance with good agricultural practices. In view of survey results, investigations on vegetable contamination were conducted. Therefore, 175 vegetable samples including cabbage (31 samples), lettuce (88 samples), tomato (57 samples) collected from four sites of the Niayes zone during four campaigns, were analyzed for residues of 21 pesticides, eighteen of which (18) were cited to be used by farmers. The results indicated that 65% of tomato samples, 71% of lettuce and 93% of cabbage contained one or more detectable residues. Among the monitored pesticides dicofol, chlorpyrifos, DDTs, dimethoate, and ?-cyhalothrin were the most predominant, found in at least 35% of samples for each vegetable. The frequencies of pesticide detection were, generally in agreement with the citation frequencies. The results provided important information on vegetable contamination status and pointed an urgent need to control pesticide use. PMID:26519803

  6. 40 CFR 180.7 - Petitions proposing tolerances or exemptions for pesticide residues in or on raw agricultural...

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Petitions proposing tolerances or exemptions for pesticide residues in or on raw agricultural commodities or processed foods. 180.7 Section 180... proposing tolerances or exemptions for pesticide residues in or on raw agricultural commodities or...

  7. Residue levels and risk assessment of pesticides in nuts of China.

    Liu, Yihua; Shen, Danyu; Li, Shiliang; Ni, Zhanglin; Ding, Ming; Ye, Caifen; Tang, Fubin

    2016-02-01

    The pesticide residue levels of three nuts (chestnut, walnut, pinenut) collected from seven main producing areas of China were investigated. Twenty-nine pesticides, including organophosphates (OPs), organochlorines (OCs), pyrethroids (PYs) and two fungicides (triadimefon and buprofezin) were analyzed by gas chromatography (GC). Four OPs (acephate, dimethoate, chlorpyrifos and parathion-methyl) were found in 11.4% samples, with the concentrations of 19.0 µg kg(-1) to 74.0 µg kg(-1). Six OCs (DDT, HCH, endosulfan, quintozene, aldrin and dieldrin) were found in 18.2% samples, with the concentrations of 2.0 µg kg(-1) to 65.7 µg kg(-1). Among OCs, p,p-DDE and α-HCH were the dominant isomer for DDT and HCH. Five PYs (fenpropathrin, fenvalerate, cypermethrin, bifenthrin and cyhalothrin) were found in 15.9% samples, with the concentrations of 2.5 µg kg(-1) to 433.0 µg kg(-1). Fenpropathrin was the most frequently detected pesticide. In addition, triadimefon and buprofezin were detected only in two samples. For the tested nuts, 25.0% samples with multiple residues (containing more than two pesticides) were noted, even up to 9.1% samples with five pesticide residues. The residue of 15.9% samples was higher than the maximum residue limits (MRLs) of China. The short-term risks for the tested nuts were below 1.2%, and the highest long-term risk was 12.58%. The cumulative risk (cHI) for the tested pesticides were 8.43% (OPs), 0.42% (OCs), 12.82% (PYs) and 0.15% (fungicides), respectively. The total cHI was 21.82%. There was no significant health risk for consumers via nuts consumption. PMID:26408971

  8. Organochlorine pesticide residues in the northern Indian Ocean

    Shailaja, M.S.; Sarkar, A.

    are: 4.0 to 5.9 ppb in zooplankton; 0.3 to 8.6 ppb in fish and 0.02 to 720.0 ppb in sediments. Some of the other organochlorine pesticides detected in sediments from the Bay of Bengal are: lambda -HCH (lindance) 0.01 to 0.21 ppb; aldrin 0.01 to 0.5 ppb...

  9. Pesticide Residues and Bees – A Risk Assessment

    Sanchez-Bayo, Francisco; Goka, Koichi

    2014-01-01

    Bees are essential pollinators of many plants in natural ecosystems and agricultural crops alike. In recent years the decline and disappearance of bee species in the wild and the collapse of honey bee colonies have concerned ecologists and apiculturalists, who search for causes and solutions to this problem. Whilst biological factors such as viral diseases, mite and parasite infections are undoubtedly involved, it is also evident that pesticides applied to agricultural crops have a negative i...

  10. MARKET BASKET SURVEY FOR SOME PESTICIDES RESIDUES IN FRUITS AND VEGETABLES FROM GHANA

    Crentsil Kofi Bempah

    2012-12-01

    Full Text Available A study was conducted to investigate the organochlorine, organophosphorus and synthetic pyrethroid pesticide residues in fruits and vegetables from markets in Ghana. For this purpose, a total of 309 fruits and vegetable samples, were collected and analyzed by gas chromatography with electron capture detector. The obtained results showed that the predominance of organochlorine followed by organophosphorus and synthetic pyrethroid pesticides in most of the analyzed samples. The detected concentrations of them were most significant in vegetable samples. The results obtained showed that 39.2 % of the fruits and vegetable samples analyzed contained no detectable level of the monitored pesticides, 51.0 % of the samples gave results with trace levels of pesticide residues below the maximum residue limit (MRL, while 9.8 % of the samples were above the MRL. The findings point to the urgent need to establish reliable monitoring programs for pesticides, so that any exceedance in concentration over environmental quality standards can be detected and appropriate actions taken.

  11. Pesticide residues in fish with emphasis on the application of nuclear techniques

    Fish play an important role in the assessment of the fate and effect of pesticides in the aquatic environment, both on intentional and unintentional release. The roles of fish toxicity and human consumption are discussed with respect to uptake, metabolism and excretion, and including residues. In this context a great deal of work has been done with labelled pesticides which has had to be evaluated comparatively with other organisms. Accumulation, as a factor of pesticide mobility and an indicator of toxicity, has been very intensively studied in fish. As the latter are model ecological organisms for accumulation, many parallel investigations have been carried out with labelled and non-labelled material. Owing to the generally low metabolic rate detected, accumulation in fish is largely due to the parent compound in the case of persistent pesticides. The methods used ranged from simple laboratory tests to experiments in the open environment. (author)

  12. Organochlorinated pesticide residues in coastal sediment from the Muda rice granary area, Peninsular Malaysia

    A study was done on the speciation and analysis of organochlorine pesticides in sediment collected from coastal water of Peninsular Malaysia along the Straits of Malacca, namely the coastal water areas of Kedah, Perlis and Perak. Sediment samples were collected using a box coring device at four stations in coastal waters along the Muda rice granary area and four other stations outside the area. The main objective of the study was to monitor the level of contamination by compounds that have been used to control pests particularly in rice granary areas. The detection and quantification of the compounds were done with the GC-ECD. The capability of the method used was examined by analysis of Standard Reference Material obtained from NIST, USA. The mean concentrations of organochlorine pesticide compounds in the coastal water area along the Muda area was 11.17 ± 3.76 ng/g, dry weight (range 7.64-19.86 ng/g, dry weight) whilst those in other areas was 4.14 ± 1.36 ng/g, dry weight (range 2.29-5.10 ng/g, dry weight). The average concentration of the DDT group in the Muda area was 4.22 ± 2.39 ng/g, dry weight, whilst the non-DDT group was 6.94 ± 2.01 ng/g, dry weight. Outside the Muda area, the average concentration of the DDT group was 1.26 ± 0.58 ng/g, dry weight. The non-DDTgroup had a mean concentration of 2.88 ± 0.80 ng/g, dry weight. Even though the concentration of the organochlorinated pesticides in the Muda area was higher, it was still lower than levels reported worldwide. For example, at the Gulf of Mexico (range DDT<0.02-454.00 ng/g, dry weight), Arabian Sea (range DDT 7.4-179.1 ng/g), Gulf of Bengal (range DDT<0.22-720.0 ng/g, dry weight) and Colombian Caribbean (range DDT 38.0-266.0 ng/g, dry weight). Being aware of the sensitivity of marine life, especially crustacean to organochlorines and ensuring the sustainability of rice production in the Muda area, continued monitoring of the level of pesticides residues of the coastal water of the Muda granary area should be undertaken, lack of which could be damaging to the marine ecosystem as the compounds are persistent in the environment. (Author)

  13. Pesticide residues and microbial contamination of water resources in the MUDA rice agroecosystem

    Studies on the water resources of the Muda rice growing areas revealed evidence of pesticide residues in the agroecosystem. While the cyclodiene endosulfan was found as a ubiquitous contaminant, the occurrence of other organochlorine insecticides was sporadic. The presence of 2,4-D, paraquat and molinate residues was also evident but the occurrence of these herbicides was seasonal. Residue levels of molinate were generally higher than those from the other herbicides. The problem of thiobencarb and carbofuran residues was not encountered. Analyses for microbial contamination revealed that the water resources were unfit for drinking; coliform counts were higher during certain periods of the year than others. (Author)

  14. Optical instrument development for detection of pesticide residue in apple surface

    Dhakal, Sagar; Li, Yongyu; Peng, Yankun; Chao, Kuanglin; Qin, Jianwei

    2013-05-01

    Apple is the world largest produced and consumed fruit item. At the same time, apple ranks number one among the fruit item contaminated with pesticide. This research focuses on development of laboratory based self-developed software and hardware for detection of commercially available organophosphorous pesticide (chlorpyrifos) in apple surface. A laser light source of 785nm was used to excite the sample, and Raman spectroscopy assembled with CCD camera was used for optical data acquisition. A hardware system was designed and fabricated to clamp and rotate apple sample of varying size maintaining constant working distance between optical probe and sample surface. Graphical Users Interface (GUI) based on LabView platform was developed to control the hardware system. The GUI was used to control the Raman system including CCD temperature, exposure time, track height and track centre, data acquisition, data processing and result prediction. Different concentrations of commercially available 48% chlorpyrifos pesticide solutions were prepared and gently placed in apple surface and dried. Raman spectral data at different points from same apple along the equatorial region were then acquired. The results show that prominent peaks at 341cm-1, 632cm-1 and 680 cm-1 represent the pesticide residue. The laboratory based experiment was able to detect pesticide solution of 20ppm within 3 seconds. A linear relation between Raman intensity and pesticide residue was developed with accuracy of 97.8%. The result of the research is promising and thus is a milestone for developing industrially desired real time, non-invasive pesticide residue detection technology in future.

  15. Multiresidue analysis of pesticides in traditional Chinese medicines using gas chromatography - negative chemical ionization tandem mass spectrometry

    In this study, a residue analysis method for the simultaneous determination of 107 pesticides in the traditional Chinese medicines (TCMs), Angelica sinensis, Angelica dahurica, Leonurus heterophyllus Sweet, Pogostemon cablin, and Lonicera japonica Thunb, was developed using gas chromatography couple...

  16. Studies on the residual levels of pesticide pollution in the sathiar reservoir

    The monitoring of pesticide residual levels was done is reservoir water, mud, zooplankton, live and dead fish muscle and gill tissue for a period from November 1976 to January 1978. Using electron capture detector, both organochlorine and organophosphorus pesticide residues have been detected in the Sathiar Ecosystem. In nanogram levels they have shown a general increase in the course of one year. Of the former group, BHC appeared to persist undergraded in the fish muscle. With reference to DDT and DDE it is the latter which has registered increased levels in soil, water and fish. Endrin was detected only in water. The organophosphorus pesticides represented by parathion appears only in traces in the water as flood water fills Sathiar resorvoir and is degraded completely (possibly as phenolic compounds) and utilised. (author)

  17. FINGER PRINTING TECHNIQUE FOR DETECTION OF PESTICIDE RESIDUES IN VEGETABLE CROPS

    Syeda Azeem Unnisa

    2014-01-01

    Finger printing technique enables the detection of DDT and HCH residues in vegetables through the development of light green and prussian violet colors respectively. Cut vegetables are pressed against o-tolidine impregnated paper (chromogenic paper) and exposed to sunlight where colored spots appear instantly. The pesticides residues of DDT and HCH were determined in 16 samples of 4 varieties of vegetable crops, taken from 4 provinces. The results showed presence results for ...

  18. Investigations on antibody binding to a micro-cantilever coated with a BAM pesticide residue

    Bache, Michael; Taboryski, Rafael Jozef; Schmid, Silvan; Aamand, Jens; Jakobsen, Mogens Havsteen

    2011-01-01

    The attachment of an antibody to an antigen-coated cantilever has been investigated by repeated experiments, using a cantilever-based detection system by Cantion A/S. The stress induced by the binding of a pesticide residue BAM (2,6 dichlorobenzamide) immobilized on a cantilever surface to anti-B...

  19. [Determination of endosulfan pesticide residues in Litopenaeus vannamai by capillary gas chromatography].

    Liu, Xiaosong; Huang, Daxin; Lu, Shengyu

    2007-05-01

    A method is described for the determination of endosulfan pesticide residues in Litopenaeus vannamai by capillary gas chromatography. The residues of alpha-endosulfan and beta-endosulfan were extracted from the sample with ethyl acetate, and the extract was cleaned up using a neutral alumina column and an active carbon column after concentrated and then eluted with a mixture of n-hexane-ethyl acetate (1 : 1, v/v). During the process of purification, the flow rate of eluent was controlled within 3 mL/min. The eluate was collected and evaporated to 1 mL for analysis. The determination was performed on a gas chromatograph equipped with an electron capture detector. The retention time was used for qualification and the external calibration standard was used for quantitation. The results obtained showed that the recoveries were 80.5% - 97.3% for alpha-endosulfan and 81.1% - 109.5% for beta-endosulfan. The limit of detection (LOD) was 0. 002 mg/kg, and the limit of quantitation (LOQ) was 0. 007 mg/kg for both. The precision of the method, expressed as the relative standard deviation for the within-laboratory repeatability, was generally below 8.5%. The method was used for the analysis of Litopenaeus vannamai samples from Guangxi Province, a Litopenaeus vannamai aquiculture area in south China. PMID:17679437

  20. Pesticide residues in Italian Ready-Meals and dietary intake estimation.

    Lorenzin, Michele

    2007-01-01

    The investigations carried out during 2005 by state-run Italian laboratories within the framework of controls seeking pesticide residues monitoring in foodstuffs involve quantifying the levels of such residues in fruit and vegetable produce and their processed products: oil, wine and fruit juices. The Italian Ready-Meal Residue Project, promoted by the pesticides working group of Italian Environmental Agencies, seeks to asses the quantity of pesticides in pre-prepared (ready-to-eat) lunches (comprising a first course, side dish, fruit, bread and wine), and to quantify the amounts consumed and compare with the acceptable daily intake ADIs. The data provided by 16 laboratories which analyzed 50 complete meals in 2005 (samples taken on 8 February, 26 May, 24 October, 21 December 2005) showed residues in 39 lunches, with an average number of 2.4 pesticides in each meal and a maximum of 10 pesticides. The most frequently found substances were: pirimiphos-methyl (20 times), procymidone (17), pyrimethanil (7), iprodione (7), cyprodinil (7), fenitrothion (6), diphenylamine (6), chlorpyrifos (6), metalaxyl (5) and chlorpyrifos-methyl (5). The distribution of residues among each dish of the meal was also examined, and the results showed that: 77.3% of the residues were present in the fruit, 14.9% in the wine, 3.0% in the main course, 2.8% in the bread and 2.1% in the side dish. Assuming that two meals are consumed per day, the daily intake of pesticide residues was calculated on a daily basis, in relation to normal body weight (60 kg for an adult, 40 kg for a teenager, 20 kg for a child) and compared with the ADI values established by the European Union. In the case of adults, the average daily intake of pesticides in relation to ADI was 2.6% with a maximum of 73.3%; for teenagers it was 4.9% with a maximum of 109% and for children it was 9.8% with a peak of 219%. PMID:17763040

  1. Quantitative Structure Activity Relationship and Risk Analysis of Some Pesticides in the Goat milk

    Faqir Muhammad

    2013-01-01

    Full Text Available The detection and quantification of different pesticides in the goat milk samples collected from different localities of Faisalabad, Pakistan was performed by HPLC using solid phase microextraction. The analysis showed that about 50% milk samples were contaminated with pesticides. The mean+/-SEM levels (ppm of cyhalothrin, endosulfan, chlorpyrifos and cypermethrin were 0.34+/-0.007, 0.063+/-0.002, 0.034+/-0.002 and 0.092+/-0.002, respectively; whereas, methyl parathion was not detected in any of the analyzed samples. Quantitative structure activity relationship (QSAR models were suggested to predict the residues of unknown pesticides in the goat milk using their known physicochemical characteristics including molecular weight (MW, melting point (MP, and log octanol to water partition coefficient (Ko/w in relation to the characteristics such as pH, % fat, specific gravity and refractive index of goat milk. The analysis revealed good correlation coefficient (R2 = 0.985 for goat QSAR model. The coefficients for Ko/w and refractive index for the studied pesticides were higher in goat milk. This suggests that these are better determinants for pesticide residue prediction in the milk of these animals. Based upon the determined pesticide residues and their provisional tolerable daily intakes, risk analysis was also conducted which showed that daily intake levels of pesticide residues including cyhalothrin, chlorpyrifos and cypermethrin in present study are 2.68, 5.19 and 2.71 times higher, respectively in the goat milk. This intake of pesticide contaminated milk might pose health hazards to humans in this locality.

  2. De-contamination of pesticide residues in food by ionizing radiation

    The role of gamma irradiation on removal of pesticides in aqueous solutions or in vegetables and fruits was investigated. Radiation - induced decontamination of pesticides is generally greater in aqueous solutions than in selected vegetables and fruits. Residues of malathion (0.5 ppm in potatoes, 8 ppm in onions and dates), pirimiphos-methyl (1 ppm in onions and grapes) and cypermethrin (0.05 ppm in potatoes and 0.1 ppm in onions) were not reduced to below maximum residue limits (MRLs) for irradiation doses up to 1 kGy. The same trend was observed when irradiation was performed for grapes fortified with malathion (8 ppm) and cypermethrin (2 ppm) for absorbed doses up to 2 kGy. Ionizing radiation reduced the residues of pirimiphos-methyl (0.05 ppm in potatoes at1 kGy, 1 ppm in grapes at 2 kGy and 0.1 ppm in dates at1 kGy), malathion (8 ppm in grapes at 7 kGy) and cypermethrin (2 ppm in grapes at 7 kGy) to below maximum residue limits (MRLs). - Highlights: ► The role of irradiation on removal of pesticides in aqueous solutions or in food products was investigated. ► Radiation-induced removal of pesticides is generally greater in aqueous solutions than in food products. ► Radiation can reduce the pirimiphos-methyl in potatoes, grapes and dates to below MRLs. ► Radiation can reduce the malathion and cypermethrin in grapes to below MRLs. ► Radiation is used for dual objectives of reducing pesticide residues and improving food safety.

  3. Analysis of pesticides on or in fruit by surface-enhanced Raman spectroscopy

    Shende, Chetan S.; Inscore, Frank; Gift, Alan; Maksymiuk, Paul; Farquharson, Stuart

    2004-11-01

    Pesticides are a key component in protecting crops and producing the quantity of food required by today's world population. However, since excessive concentrations pose a threat to human health, the USA sets strict tolerance levels to ensure public safety. Unfortunately, many other countries ignore these regulations and imported food exceeding these levels or contaminated with banned pesticides is a common occurrence. Furthermore, rapid chemical analysis of pesticide residues is unavailable, and only a very small fraction of foods are inspected. The greatest concern is fruit, for which an estimated 12 million tons were imported in 2003. In an effort to address this need, we have been developing a simple and rapid procedure to analyze for pesticides on fruit surfaces or in the juice of fruits. The procedure employs metal-doped sol-gel filled capillaries that both chemically extracts the pesticide and generates surface-enhanced Raman spectra when irradiated. The SERS-active capillaries, sensitivity, and preliminary fruit analyses are presented.

  4. Influence of the nature and age of cover crop residues on the sorption of three pesticides

    Cassigneul, Ana; Alletto, Lionel; Chuette, Delphine; Le Gac, Anne-Laure; Hatier, Jules; Etievant, Veronique; Bergheaud, Valrie; Baumberger, Stphanie; Mchin, Valrie; Justes, Eric; Benoit, Pierre

    2013-04-01

    In agricultural fields, soil and water quality preservation is strongly influenced by pesticides use and behavior. To limit the environmental impacts of agricultural activities, best management practices such as the use of cover crops are encouraged. Cover crops during the fallow period were found to be efficient in reducing nitrate leaching, controlling soil erosion, improving soil organic content and enhancing soil biological activity. This technique was also found to modify soil water dynamics in the following crop. According to these effects, modifications on pesticide behavior in soil, such as sorption, degradation and transport, are expected (Alletto et al., 2012 ; 2013). In this study, the impact of the nature and level of decomposition of cover crop was studied on the sorption characteristics of three pesticides. These pesticides differed in their physicochemical characteristics (hydrophobicity, solubility, persistence) and were two herbicides, S-metolachlor and glyphosate, which are largely used in maize production and predominantly found as pollutants in water; and one fungicide, epoxiconazole. Correlations between pesticide sorption and physicochemical characteristics of the cover crop residues were studied. Residues of oat, turnip rape, red clover and phacelia were collected in March 2011 and incubated at 28C and at the water holding capacity during 0, 6, 28 or 56 days. For each date, adsorption of the three radiolabeled pesticides was measured in batch on the different cover crop residues, and their biochemical composition (Van Soest fractionation), hydrophobicity (contact angle measurement) and C/N ratio were determined. Results showed that the adsorption of the pesticides differed significantly according to (i) the pesticide, (ii) the nature of cover crop, (iii) the decomposition level of the cover crop and the interaction cover crop x decomposition time. Epoxiconazole was the most adsorbed molecule, with Kd values ranging from 161 30 L/Kg (oat, turnip rape, phacelia) to 206 45 L/Kg (red clover); and glyphosate was the less adsorbed, with Kd values ranging from 1 1 L/Kg (oat, red clover) to 9 1 L/Kg (phacelia) at day 0. Differences between pesticides were expected considering the hydrophobicity of these molecules. Adsorption of the three pesticides increased with decomposition time (up to sevenfold for glyphosate on oat), and was negatively correlated with C/N ratio (-0.73nature and level of decomposition of cover crop at the soil surface influenced the mobility of pesticides as it was observed in decomposing mulch of crop residues (Aslam et al., 2013). As a result, the type of cover crop and the changes of cover crop residues composition during decomposition in field may control differently the movement of non-ionic pesticides compared to ionic compounds such as glyphosate, largely used in conservation agriculture practices. Keywords : Cover crops ; Glyphosate ; S-metolachlor ; Epoxiconazole ; Mulch; Sorption ; Biochemical composition References Alletto L., Benoit P., Justes E., Coquet Y. 2012. Effects of tillage and fallow period management on the fate of the herbicide isoxaflutole in an irrigated continuous-maize field. Agriculture, Ecosystems Environment, 153, 40- 49. http://dx.doi:10.1016/j.agee.2012.03.002 Alletto L., Benoit P., Coufignal M., Bergheaud V., Dumny V., Longueval D., Barriuso E. 2013. Sorption and mineralization of S-metolachlor in 51 fields cultivated with conservation tillage. Soil Tillage Research 128, 97-103. http://dx.doi.org/10.1016/j.still.2012.11.005 Aslam S., Garnier P., Rumpel C., Parent S., Benoit P. 2013. Adsorption and desorption behavior of selected pesticides as influenced by decomposition of maize mulch. Chemosphere, in press. http://dx.doi.org/10.1016/j.chemosphere.2012.12.005

  5. Determination of pesticide residue transfer rates (percent) from dried tea leaves to brewed tea.

    Wang, Jian; Cheung, Wendy; Leung, Daniel

    2014-01-29

    This paper presents a study on pesticide residue transfer rates (%) from dried tea leaves to brewed tea. In the study, a brewing procedure simulated the preparation of a hot tea drink as in routine. After brewing, pesticide residues were extracted from brewed tea using a method known as QuEChERS (quick, easy, cheap, effective, rugged, and safe). An UHPLC/ESI-MS/MS method was developed and validated to identify and quantify up to 172 pesticides in both tea leaves and brewed tea samples. Quantification was achieved using matrix-matched standard calibration curves with isotopically labeled standards or a chemical analogue as internal standards, and the calibration curves consisted of six points (0.4, 2.0, 8.0, 16.0, 24.0, and 40.0 μg/L equivalent in sample). The method was validated at four concentration levels (4.0, 12, 20.0, and 32.0 μg/L equivalent in sample) using five different brewed tea matrices on two separate days per matrix. Method performance parameters included overall recovery, intermediate precision, and measurement uncertainty, which were evaluated according to a nested experimental design. Approximately, 95% of the pesticides studied had recoveries between 81 and 110%, intermediate precision ≤20%, and measurement uncertainty ≤40%. From a pilot study of 44 incurred tea samples, pesticide residues were examined for their ability to transfer from dried tea leaves to brewed tea. Each sample, both tea leaves and brewed tea, was analyzed in duplicate. Pesticides were found to have different transfer rates (%). For example, imidacloprid, methomyl, and carbendazim had transfer rates of 84.9, 83.4, and 92.4%, respectively. PMID:24377499

  6. Influence of pH on pesticide sorption by soil containing wheat residue-derived char

    Field burning of crop residues incorporates resulting chars into soil and may thus influence the environmental fate of pesticides in the soil. This study evaluated the influence of pH on the sorption of diuron, bromoxynil, and ametryne by a soil in the presence and absence of a wheat residue-derived char. The sorption was measured at pHs ?3.0 and ?7.0. Wheat char was found to be a highly effective sorbent for the pesticides, and its presence (1% by weight) in soil contributed >70% to the pesticide sorption (with one exception). The sorption of diuron was not influenced by pH, due to its electroneutrality. Bromoxynil becomes dissociated at high pHs to form anionic species. Its sorption by soil and wheat char was lower at pH ?7.0 than at pH ?3.0, probably due to reduced partition of the anionic species of bromoxynil into soil organic matter and its weak interaction with the carbon surface of the char. Ametryne in its molecular form at pH ?7.0 was sorbed by char-amended soil via partitioning into soil organic matter and interaction with the carbon surface of the char. Protonated ametryne at pH ?3.0 was substantially sorbed by soil primarily via electrostatic forces. Sorption of protonated ametryne by wheat char was also significant, likely due not only to the interaction with the carbon surface but also to interactions with hydrated silica and surface functional groups of the char. Sorption of ametryne by char-amended soil at pH ?3.0 was thus influenced by both the soil and the char. Environmental conditions may thus significantly influence the sorption and behavior of pesticides in agricultural soils containing crop residue-derived chars. - Wheat char was effective for adsorption of pesticides in soil, with efficacy varying with pH and particular pesticides

  7. A residue-free green synergistic antifungal nanotechnology for pesticide thiram by ZnO nanoparticles

    Xue, Jingzhe; Luo, Zhihui; Li, Ping; Ding, Yaping; Cui, Yi; Wu, Qingsheng

    2014-07-01

    Here we reported a residue-free green nanotechnology which synergistically enhance the pesticides efficiency and successively eliminate its residue. We built up a composite antifungal system by a simple pre-treating and assembling procedure for investigating synergy. Investigations showed 0.25 g/L ZnO nanoparticles (NPs) with 0.01 g/L thiram could inhibit the fungal growth in a synergistic mode. More importantly, the 0.25 g/L ZnO NPs completely degraded 0.01 g/L thiram under simulated sunlight irradiation within 6 hours. It was demonstrated that the formation of ZnO-thiram antifungal system, electrostatic adsorption of ZnO NPs to fungi cells and the cellular internalization of ZnO-thiram composites played important roles in synergy. Oxidative stress test indicated ZnO-induced oxidative damage was enhanced by thiram that finally result in synergistic antifungal effect. By reducing the pesticides usage, this nanotechnology could control the plant disease economically, more significantly, the following photocatalytic degradation of pesticide greatly benefit the human social by avoiding negative influence of pesticide residue on public health and environment.

  8. A residue-free green synergistic antifungal nanotechnology for pesticide thiram by ZnO nanoparticles

    Xue, Jingzhe; Luo, Zhihui; Li, Ping; Ding, Yaping; Cui, Yi; Wu, Qingsheng

    2014-01-01

    Here we reported a residue-free green nanotechnology which synergistically enhance the pesticides efficiency and successively eliminate its residue. We built up a composite antifungal system by a simple pre-treating and assembling procedure for investigating synergy. Investigations showed 0.25?g/L ZnO nanoparticles (NPs) with 0.01?g/L thiram could inhibit the fungal growth in a synergistic mode. More importantly, the 0.25?g/L ZnO NPs completely degraded 0.01?g/L thiram under simulated sunlight irradiation within 6?hours. It was demonstrated that the formation of ZnO-thiram antifungal system, electrostatic adsorption of ZnO NPs to fungi cells and the cellular internalization of ZnO-thiram composites played important roles in synergy. Oxidative stress test indicated ZnO-induced oxidative damage was enhanced by thiram that finally result in synergistic antifungal effect. By reducing the pesticides usage, this nanotechnology could control the plant disease economically, more significantly, the following photocatalytic degradation of pesticide greatly benefit the human social by avoiding negative influence of pesticide residue on public health and environment. PMID:25023938

  9. Investigation and Measurement of Pesticidal Residues; Benomil and Mancazeb in Cucumber Produced in Mazandaran.

    B Shabankhani

    2006-01-01

    Full Text Available Introduction: Considering the importance and usefulness of fruits in peoples daily diet as they play an important role in determining public health and also considering the significance of pesticide residues in foods and fruits , measurement of which has been repeatedly reiterated by WHO and FAO, this research was done. Irregular use of pesticides by farmers knowingly or unknowingly without observing its caress period has led to the contact of these pesticides with humans through foods and fruits and in the long run, they will surely cause chronic complications . Methods: In this study, after collecting cucumbers form 76 sample regions, we rinsed them carefully, sliced them thinly and mashed them up. Then, we extracted them three times with n butyl acetate. Later, we evaporated the solvent. At the end, we measured the residue by chromatographic gas (GC and detector (ECD. Results and Conclusion: The results obtained were analyzed with the help of two-way ANOVA. It indicated that there is a correlation between the investigated regions and the residual amount (P>0.05. Calculation of the mean ratings showed that the levels of these two pesticides are higher than the acceptable level in most of the regions. (0.01

  10. Pesticide Residues Contamination of Vegetables and their Public Health Implications in Ghana

    Botwe, B. O.

    2011-08-01

    Full Text Available This study aimed at determining the residues concentrations of pesticides in vegetables, and assessing the health risk due to the daily consumption of contaminated vegetables for adults in the prominent farming community of Akumadan in Ghana. Fifteen pooled samples, belonging to five vegetable types (tomato, cabbage, pepper, onion and eggplants purchased from local markets across Ghana were analysed for DDTs, endosulfan, HCHs, methoxychlor, dimethoate and lambda-cyhalothrin using GC-MS. The concentrations of the pesticides ranged from 0.01 to 46.95 µg/kg wet weight. Dietary data were collected from 130 residents. By combining the dietary and contaminant data, dietary exposure to the identified pesticides was calculated. Dietary exposure to pesticide residues at Akumadan is low and there is no associated health risk. However, the results of persistent contaminants are of particular health concern because of this persistence. The estimated exposure distributions were shown to be insensitive to valuation of the non-detect residue samples.

  11. Determination of pesticide residue levels in omani and UAE vegetable farm soils

    In the investigation of 40 different vegetable growing farms of Al-Batinah (Oman) and Al - Ain (UAE) regions different pesticide residues were found to be present on all soil samples which varied in their types and levels according to the region. In Omani soil samples, cypermethrin was the most frequent pesticide, followed by chlorpyrifos, malathion, phenthoate, triazophos and deltamethrin. In UAE farm soil samples, chlorpyrifos, cypermethrin and deltamethrin were detected in all the regions, while phenthoate was detected in the Eastern and Northern regions only. (author)

  12. Pesticide residues in food of plant origin from Southeast Asia – A Nordic project

    Skretteberg, L. G.; Lyrån, B.; Holen, B.; Jansson, A.; Fohgelberg, P.; Siivinen, K.; Andersen, Jens Hinge; Jensen, Bodil Hamborg

    2015-01-01

    reason for the increased control for certain food products from Southeast Asia was that the official control had revealed many products with too high levels of pesticide residues. In 60% of the samples we did not find any residues, while 28% had residues below or at the MRLs. Results above the MRLs were...... found in 12% of the samples. In comparison 6% of surveillance samples from third countries and 1.5% of surveillance samples from the EU and EFTA countries exceeded the MRL in the EU monitoring program in 2011. The estimated acute intake was higher than 100% of the ARfD in several samples and some of the...

  13. Organochlorine pesticide residues in human milk samples from Comarca Lagunera, Mexico, 1976.

    Albert, L; Vega, P; Portales, A

    1981-12-01

    Milk samples were obtained from 15 nursing mothers in the agricultural region of Comarca Lagunera, Mexico, and were analyzed for organochlorine pesticide residues. Nine different types of residues were found. Of these, p,p'-DDE, p,p'-DDT, and beta-BHC occurred most frequently. All samples had concentrations of DDT-derived compounds higher than the practical limit recommended by the U.N. Food and Agriculture Organization/World Health Organization for DDT in cows' milk. Residues of other chlorinated hydrocarbons were present at levels similar to those found in human milk in other developing countries. PMID:7348797

  14. Problems of positive list system revealed by survey of pesticide residue in food.

    Iwasaki, Mariko; Sato, Itaru; Jin, Yihe; Saito, Norimitsu; Tsuda, Shuji

    2007-05-01

    The positive list system became effective from May 29, 2006 to improve the regulation of residual agricultural chemicals (pesticides, feed additives and veterinary drugs) in foods. In accordance with the system, we investigated pesticide residues in 50 agricultural products purchased in Morioka city from March to November 2006. Analyses were performed according to the "Multiresidue Method for Agricultural Chemicals by GC/MS", the Notice of the Ministry of Health, Labour and Welfare. Five pesticides and two non-agricultural chemicals were detected from 16 samples. Ortho-phenylphenol (OPP) was detected from 8 samples: immature pea, snap bean, kiwi, plain-boiled bamboo shoot, mango, white asparagus, lemon and domestic shiitake mushroom. Maximum residue limits (MRLs) have not been established for these products, and they exceeded the uniform level of 0.01 ppm. DDT was detected from Philippines banana (0.30 ppm) and Korean paprika (0.45 ppm). The residual level in Philippines banana was lower than the MRL, but Korean paprika exceeded its MRL. Chlorpyrifos, Thiabendazole and Imazaril were detected from citrus imported from the U.S.A., but their residue levels were lower than the respective MRLs. Aniline and 2-pyrrolidone were detected from several imported products. These two may not be regulated by the positive list system because they are not agricultural chemicals, although their derivatives are used as pesticides or veterinary drugs. Three problems have been revealed from this survey: 1) application of the uniform level to minor agricultural products, 2) residues of non-agricultural chemicals whose toxicity is uncertain, 3) metabolites of agricultural chemicals, which are also regulated by the positive list system, have not been clearly defined. PMID:17538241

  15. Studies of the magnitude and nature of pesticide residues in stored products, using radiotracer techniques

    Growing world population and food demand have dictated the introduction of intensive agricultural practices, including the use of an increasing range of agrochemicals. The utilization of these chemicals has a positive and often dramatic impact on agricultural production, but every effort has to be made to ensure safety in use. This is a dynamic challenge for many countries and necessitates the implementation of adequate monitoring programmes. Even when pesticide use conforms to currently adopted standards of good management practice, undesirable side effects may occur and could, at times, endanger public health. Nuclear techniques provide a valuable tool for studying pesticide residues in stored food commodities. Radioisotopes can be used to determine total quantities of residue present, the nature of the residue (i.e. both undecomposed parent material and reaction products), rates of breakdown and loss and distribution in the food material. All of this information is essential for health and regulatory authorities to establish and maintain comprehensive tolerance standards that will protect the health of the consumer. The use of 14C labelled compounds constitutes a superior and unrivalled tool, in particular for the detection and quantification of grain bound residues. All pesticide residues remaining on or in food materials are of potential concern to human health. Surface residues that remain on commodities such as grain may present an occupational risk to workers exposed to dust emanating from the commodity; residues that remain in food may be a hazard to the consumer. The nature of the residue, the quantity present and its toxicological significance should be known so that tolerance levels can be established and complied with. Refs, figs and tabs

  16. Modelling non-systemic pesticide residues in fruits with initial deposit variability and weather effects.

    Huo, R; Salazar, J D; Hyder, K; Xu, X-M

    2007-11-01

    A flexible and generic model was developed to predict the decline of residues of a non-systemic pesticide for both single and multi-spray situations as well as for different tree canopy zones. The model predicts not only the average residue levels, but also the confidence interval of the residues through either a deterministic or a stochastic approach. This generic model includes several key aspects of residue fates in the environment: initial deposit, physical loss and growth dilution. The model considers a tree canopy in three distinct zones for which initial deposition of pesticides may differ. In addition to predicting the average residue within each zone, it also estimates the 95 and 99% confidence intervals of residues on individual fruit within each zone. For the purpose of evaluation, this model was parameterized specifically for captan, one of the most important non-systemic fungicides used to control disease in horticultural crops. The observed average initial deposit for each zone was used in the evaluation. The overall correlation between predicted average residues and those observed on apple fruit in two applications was 0.93. Confidence intervals were also predicted accurately. PMID:17852401

  17. Impact of long term applications of cotton pesticides on soil biological properties, dissipation of [14C]-methyl parathion and persistence of multi-pesticide residues

    Biological parameters were followed in soils from a cotton farm (Tatui) where the recommended pesticides have been used for years, and from an experimental field (Sao Paulo) which was subdivided in two areas: one received the recommended pesticides and the other was maintained untreated. The soil bioactivities monitored from 1995 to 1998, after different pesticide applications, were: basal and glucose-induced respiration; anaerobic activity; nitrification rate; activity of the enzymes: dehydrogenase, aryl sulfatase and arginine deaminase; the soil capacity to mineralize an aromatic pesticide molecule ([14C]-2,4-D), fungal and bacterial contributions for soil respiration until the beginning of 1998, and fungal and bacterial numbers from the beginning of 1998. The dissipation of [14C]-methyl parathion - one of the recommended pesticides - was followed by radiometric techniques only in Sao Paulo, but persistence of multi-residues was determined in both soils by gas-liquid chromatography. All the biological parameters varied each sampling time and values also varied among soil samples, being inhibited or stimulated by the different pesticide applications, but they mostly recovered the initially detected activity. Dissipation of methyl parathion was fast and not affected by the other pesticide applications. Pesticide residues varied between the two soils but were mostly low after all applications, which indicates their dissipation. (author)

  18. Presence of pesticide residues in water, sediment and biological samples taken from aquatic environments in Honduras

    The objective of this study was to detect the presence of persistent pesticides in water, sediment and biological samples taken from aquatic environments in Honduras during the period 1995-98. Additionally, the LC50 for 2 fungicides and 2 insecticides on post-larval Penaeus vannamei was determined in static water bioassays. A total of 80 water samples, 16 sediment samples and 7 biological samples (fish muscle tissue) were analyzed for detection of organochlorine and organophosphate pesticide residues. The results of sample analyses indicate a widespread contamination of Honduran continental and coastal waters with organochlorine pesticides. Most detections were of low (50 values and were therefore found to be much more toxic to the post-larval shrimp than the fungicides tridemorph and propiconazole. (author)

  19. Organochlorine pesticide residues in animals of Tasmania, Australia-1975-77.

    Bloom, H; Taylor, W; Bloom, W R; Ayling, G M

    1979-12-01

    Animals taken in Tasmania including duck (Anas superciliosa), eel (Anguilla australis), English perch (Perca fluviatilis), white-faced heron (Ardea pacifica), brown trout (Salmo trutta), European starling (Strunus vulgaris), cat (Felis cattus), cormorant (Phalacrocorax sp.), mutton bird (Puffinus tenuirostris), Tasmanian devil (Sarcophilus harrisii), rainbow trout (Salmo gairdnerii), Tasmanian raven (Corvus mellori), tench (Tinca tinca), and quail (Coturnix sp.) were sampled for p,p'-DDE, pp,p'-TDE, p,p'-DDT, lindane, dieldrin, and hexachlorobenzene. Pesticide residue levels exceeded 0.1 ppm in at least one animal from each area and in the majority of animals sampled from all areas. Pesticide sources could not be determined, partly because migratory species such as ducks, mutton birds, cormorants, and eels may have ingested pesticides outside of Tasmania. PMID:537866

  20. Valuation of solid phase extraction disks in the determination of pesticide residues in surface and groundwater in Panama

    In Panama large quantities of pesticides are used in agriculture and livestock farming and there is increasing concern about their impact on public health and the environment. Chiriqui is the Province that registers the largest number of producers whose activities have impact on the environment, especially on surface and groundwater. Systematic monitoring programmes are non-existent due, in part, to the high cost of laboratory determination of environmental residues of pesticides. Within the framework of the FAO/IAEA/SIDA Coordinated Research Programme, efforts were focused on evaluating and optimising the use of solid phase extraction C18 membrane disks in the analysis of surface and groundwater samples to determine pesticide residues. Factors studied were the effect of pre-washing and conditioning of the disks, flow rates, concentration level and matrix effects of field samples. Four pesticides, carbofuran, chlorothalonil, ametryn and chlorpyrifos were selected for these tests because preliminary analysis showed their presence in surface and groundwater. The technique significantly reduces the amount of organic solvents used as compared with the liquid-liquid extraction method. Quantifiable detection limits (QL) for the method were found to be 0.003 μg/L carbofuran, 0.016 μg/L chlorothalonil, 0.007 μg/L ametryn and 0.003 μg/L chlorpyrifos, when using standard spiked solutions. Recovery (%) was high when standard mixtures were used for the test runs but low when real surface water samples were tested, especially for chlorothalonil which was not recovered at all. (author)

  1. Organochlorine Pesticides Residues in the Breast Milk of Some Primiparae Mothers in La Community, Accra, Ghana

    Anita Osei Tutu

    2011-03-01

    Full Text Available This study was conducted to determine the types and levels of Organochlorine pesticide residues in the breast milk of 21 primiparae mothers in La, a suburb of Accra an urban community in the Greater Accra region of Ghana. Liquid-liquid extraction procedure was employed and extract clean-up was done using silica gel solid phase extraction. Fourteen (14 different organochlorine pesticides residues namely p,p’-DDT, p,p’-DDE, gamma-HCH, delta-HCH, heptachlor, aldrin, Endrin, endrin-aldehyde, endrin-ketone, alpha-endosulphan, endosulphan-sulphate, gamma-chlordane, dieldrin, and methoxychlor were identified and quantified in the individual breast milk samples using a Gas Chromatograph (GC with an Electron C apture detector. The GC recoveries of spiked samples were between 89 to 97%. P,p’- DDE recorded 100% incidence ratio. Also p,p’-DDT, delta-HCH, gamma-HCH, and endosulfan sulfate recorded incidence ratios of 76.79, 95.25, 80.95 and 85.71%, respectively for the breast milk samples. The concentrations of organochlorine pesticide residues in the human breast milk samples ranged from 1.839 to 99.05 :μg/kg fats. With the exception of Endosulphan Sulphate whose mean concentration (99.052 :μg/kg was above the Australian Maximum Residue Limit (MRL of 20 :μg/kg for milk, the mean concentrations for all the other organochlorines detected were below their respective limits.

  2. Presence of pesticide residues in different types of fruits and vegetables originated from the Republic of Macedonia

    Kostik, Vesna; Bauer, Biljana

    2015-01-01

    The Republic of Macedonia is an agricultural developing country with a large production of different types of vegetables and fruits in open fields as well in greenhouses. Most fruits and vegetables are treated with pesticides on several occasions during the growing season. At the same time, pesticides can pose risks if they are not applied according to Good Agricultural Practice (GAP). The present study investigates pesticide residues in samples of fresh fruits and vegetables produced in ...

  3. Pesticide pressure and fish farming in barrage pond in Northeastern France. Part II: residues of 13 pesticides in water, sediments, edible fish and their relationships.

    Lazartigues, Angélique; Thomas, Marielle; Cren-Olivé, Cécile; Brun-Bellut, Jean; Le Roux, Yves; Banas, Damien; Feidt, Cyril

    2013-01-01

    Residues of pesticides in fish farming productions from barrage ponds are seldom studied in spite of increasing health questionings and environmental concerns. The purpose of this study is to establish the pesticide contamination profiles of sediments and edible fish from five ponds in Northeastern France. Multi-residues method and liquid chromatography-tandem mass spectrometry analysis were used to quantify 13 pesticides (azoxystrobin, carbendazim, clomazone, diflufenican, dimethachlor, fluroxypyr, iprodion, isoproturon, mesosulfuron-methyl, metazachlor, napropamid, quizalofop and thifensulfuron-methyl). Ten sediments and 143 muscles samples were analysed, corresponding to two successive fishing campaigns (first fishing date and second fishing date (P2), about 1 year later) on five sites (noted C-0, C-25, C-45, C-75 and C-85 to express the increasing gradient of crop area). Isoproturon was present in all sediments samples (1.8-56.4 μg/kg dry weight). During P2 period, carbendazim was quantified in the fish of site C-0 (0.09 ± 0.02, 0.2 ± 0.1 and 0.17 ± 0.06 μg/kg wet weight (ww) for roach, carp and perch, respectively). Metazachlor was only quantified in perch of the site C-25 (0.13 ± 0.02 μg/kg ww). Concentrations of isoproturon were similar for the sites C-45 and C-75 with 0.4 ± 0.1 and 0.75 ± 0.06 μg/kg ww for carp and perch, respectively. Contamination of fish reflected generally concentrations in surroundings. Isoproturon was the most concentrated and its main source was water for perch while carp was exposed through both water and sediments, highlighting their life strategies in pond. PMID:22961490

  4. [Pesticide residues in drinking water of an agricultural community in the state of Mrida, Venezuela].

    Flores-Garca, Mery Elisa; Molina-Morales, Yuri; Balza-Quintero, Alirio; Bentez-Daz, Pedro Rafael; Miranda-Contreras, Leticia

    2011-12-01

    The aim of this study was to determine the presence of pesticides in drinking water from six aqueducts in a region of intense agricultural activity in the state of Merida, Venezuela. The study was conducted for four continuous weeks, between May and June 2008. Pesticide residues were analyzed by solid phase extraction (SPE) and liquid chromatography (HPLC) with diode array detector (DAD). The method SPE-HPLC-DAD met the criteria of analytical validation, with good linearity (R2: 0.9840 to 0.9999), precision (coefficient of inter-day variability from 1.47 to 6.25%), accuracy (relative standard deviation 0.9 to 9.20%) and sensitivity (LOD mancozeb with 0.400 microg/L). Seven of the thirteen selected pesticides have a recovery rate between 100% and 70%, the rest between 61% and 37%. Ten pesticides of the following chemical groups, were detected in 72 samples analyzed: organophosphates, carbamates, triazines and urea derivatives. The pesticides with the highest frequency of detection were: carbofuran and atrazine (39%), malathion (25%), dimethoate and metribuzin (19%). The pesticides found at high levels were diazinon (26.31 microg/L), methamidophos (10.99 microg/L), malathion (2.03 microg/L) and mancozeb (1.27 microg/L). Pesticide levels did not exceed the maximum allowed by Venezuelan law, however, according to international standards (EU and EPA-USA) values were above the maximum permissible levels. This study demonstrates the urgent need for systematic monitoring of the quality of water for human consumption in regions of high agricultural productivity. PMID:22523840

  5. Consumers’ Willingness to Pay for Cabbage with Minimized Pesticide Residues in Southern Benin

    Faustin Vidogbéna

    2015-10-01

    Full Text Available Cabbage (Brassicaceae is one of the most frequently consumed exotic vegetables in Benin and also the most affected by insects. To meet growing food demand, farmers rely heavily on synthetic pesticides that are harmful for themselves, consumers and the environment. Integrated pest management has been proposed as the means to improve vegetable productivity and quality in many developing countries. One approach is to substitute pesticides with physical barriers to insects, like nets. Here, we assess consumers’ perceptions about cabbage and their purchasing behavior towards cabbage that was produced using these nets in two major cities in Benin. Results indicate that consumers are aware of the health risks associated with intensive use of pesticides but were not able to recognize the quality difference between cabbage produced under nets from those using pesticides. All consumers were willing to pay a price premium for cabbage with minimized pesticides residues compared with conventionally produced cabbage, the average premium being 38%. Women, older, highly educated consumers and those able to distinguish cabbage qualities were willing to pay the most. We suggest that farmers will obtain higher prices if their production of cabbage with preferred characteristics is accompanied by an improved marketing strategy.

  6. SETTING MRLS FOR PESTICIDE RESIDUES IN FOOD BASED ON EU UNIFORM CRITERIA

    VALENTINA L. CHRISTOVA-BAGDASSARIAN

    2014-07-01

    Full Text Available Objective: Pesticides are used worldwide. They are applied during the growing season and part of the amount may remain in or on treated crop. Pesticides can drift to nearby areas and contaminate crops that were not treated. The MRLs are the maximum amount of a pesticide permitted in or on food (& feed, expressed in mg/kg or ppm and always defined for the active substance – crop combination. MRL should be set according to residue trials under Good Agricultural Practice (GAP and under the condition that: Daily Consumer Intake < Acceptable Daily Intake. The residue definition of active substance is derived from plant and animal metabolism. Supervised trials are the primary source of information for estimating maximum residue levels and calculating International Estimated Daily Intake. The agricultural practice the worst-case situation should be used to generate data from supervised trials to define the MRL. As the number of controlled field tests, and hence the data for MRL proposal is not large, the usual statistical models are inappropriate. Methods: Two methods for calculating proposed pre-harvest intervals (PHI and maximum residue levels are used. The first one (Rmax has proved its worth in many cases since 1981, and the second (Rber has been developed by the Federal Biological Research Centre for Agriculture and Forestry in Braunschweig/Germany. Both methods are described briefly. The first one is suitable for a larger number of data. It assumes a normal distribution of random variables, which are not always assumed with sufficient certainty. The second one uses a non-parametric distribution- and it is appropriate for more limited number of trials. Several case studies are discussed. The MRL Regulation on pesticide residues in food is a great progress towards better protection of children and consumer in general. Conclusions: Uniform criteria have to be used for evaluation of residue trials and MRLs setting process. Knowledge of the European approach in establishing the pesticide residue levels is useful for all countries in the world that have a policy of restriction of persistent organic pollutants in the environment aiming towards food safety for people of all ages.

  7. 75 FR 1773 - Notice of Receipt of a Pesticide Petition Filed for Residues of Polymeric Polyhydroxy Acid in or...

    2010-01-13

    ... AGENCY Notice of Receipt of a Pesticide Petition Filed for Residues of Polymeric Polyhydroxy Acid in or... establishment of a regulation for residues of the plant growth regulator, polymeric polyhydroxy acid, in or on... (FFDCA), 21 U.S.C. 346a, proposing the establishment of a regulation in 40 CFR part 180 for residues...

  8. Persistent organochlorine pesticide residues in water and sediment samples from Lake Manyas, Turkey.

    Erkmen, Belda; Yerli, Sedat Vahdet; Erk'akan, Füsun; Kolankaya, Dürdane

    2013-03-01

    The extent of organochlorine pesticides (OCPs) contamination in Manyas Lake (Bird Lake) and its tributary rivers and streams which is situated near the South-eastern coasts of the Marmara Sea in Turkey was investigated. Residues of OCPs in surface water and sediment samples were analysed by gas chromatography equipped with electron capture detector. The total OCPs concentration (sigmaOCPs) in water and sediment samples ranged from 1.43 to 8.6 microg l(-1) and from 17.05 to 39.14 ng g(-1), respectively. According to the concentrations and detection frequencies, HCHs, DDTs, heptachlor and heptachlor epoxide were the most dominant compounds among the OCPs. The results showed that Manyas Lake was still contaminated by organochlorine pesticides and their residues despite bans on the production and usage over a long time. PMID:24620575

  9. Optimization of immunochemistry for sensing techniques to detect pesticide residues in water

    Uthuppu, Basil; Kostesha, Natalie; Jakobsen, Mogens Havsteen; Kiersgaard, S M; Aamand, J; Jorgensen, C

    2011-01-01

    We are working on the development of a real-time electrochemical sensor based on an immunoassay detection system to detect and quantify the presence of pesticide residues in ground water. Highly selective and sensitive immuno-reactions are being investigated to be optimized in order to bring them...... into the level of real-time in-line sensors. In this project a competitive immunoassay between surface immobilized 2,6-dichlorobenzamide (BAM) haptens and BAM present in the water sample using an anti-BAM monoclonal antibody is being described. 2,6-Dichlorobenzamide (BAM) is a degradation product of...... the herbicide, dichlobenil which has been used extensively in the past and it is among the most frequently found pesticide residues in European ground water. BAM is highly resistant to further degradation and is fairly soluble in water. We have synthesized and immobilized a small library of BAM...

  10. Pesticide analysis in rose wines by micellar electrokinetic chromatography.

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Borges-Miquel, Teresa M; Rodríguez-Delgado, Miguel Angel

    2007-12-01

    In this work, the determination of 11 pesticides (pirimicarb, metalaxyl, pyrimethanil, procymidone, nuarimol, azoxystrobin, tebufenozide, fenarimol, benalaxyl, penconazole, and tetradifon) in rose wines by micellar EKC (MEKC) using reversed electrode polarity stacking mode (REPSM) as online preconcentration strategy is described. The MEKC buffer consisted of 100 mM sodium tetraborate and 30 mM SDS at pH 8.5 with 6% v/v 1-propanol. A solid-phase microextraction (SPME) procedure using PDMS/divinylbenzene (PDMS/DVB) fibers was applied to extract the selected pesticides from the rose wine samples. The comparison between the calibration curves obtained from hydroalcoholic solutions (12% v/v ethanol) and from rose wines (matrix matched calibration) showed the existence of a strong matrix effect. Furthermore, a comparison with calibration curves obtained with white wine samples also showed significant differences for most of the analyzed pesticides. As a result, a matrix matched calibration was developed. Quantitative extraction from spiked wine samples was carried out in triplicate at two levels of concentration (range 0.18-6.00 mg/L). LODs between 0.040 and 0.929 mg/L were achieved, which are below the maximum residue limits (MRLs) established for wine grapes (except for pirimicarb) by the EU and Spain legislation as well as by the Codex Alimentarius. The established method - which is solvent free, cost effective, and fast - was also applied to the analysis of several homemade rose wine samples and a commercial one. Two of the selected pesticides were found in some of the analyzed samples. PMID:18027361

  11. Management-oriented sensitivity analysis for pesticide transport in watershed-scale water quality modeling using SWAT

    The Soil and Water Assessment Tool (SWAT) was calibrated for hydrology conditions in an agricultural watershed of Orestimba Creek, California, and applied to simulate fate and transport of two organophosphate pesticides chlorpyrifos and diazinon. The model showed capability in evaluating pesticide fate and transport processes in agricultural fields and instream network. Management-oriented sensitivity analysis was conducted by applied stochastic SWAT simulations for pesticide distribution. Results of sensitivity analysis identified the governing processes in pesticide outputs as surface runoff, soil erosion, and sedimentation in the study area. By incorporating sensitive parameters in pesticide transport simulation, effects of structural best management practices (BMPs) in improving surface water quality were demonstrated by SWAT modeling. This study also recommends conservation practices designed to reduce field yield and in-stream transport capacity of sediment, such as filter strip, grassed waterway, crop residue management, and tailwater pond to be implemented in the Orestimba Creek watershed. - Selected structural BMPs are recommended for reducing loads of OP pesticides.

  12. Organochlorine pesticide residue levels in soil from the Nyando River catchment, Kenya

    Abong'o, Deborah; Wandiga, Shem; Jumba, Isac; Van den Brink, Paul; Nazariwo, Betty; Madadi, Vincent; Wafula, Godfrey; Kylin, Henrik; Nkedi-Kizza, Peter

    2015-01-01

    Soil samples were collected from six locations representative of the Nyando River catchment area of the Lake Victoria over a period of two years. Sampling was done four times in the year in February, May, September and December 2005 and 2006 in farms where maize, tea, sugar cane, coffee, rice and vegetables have been grown over the years. This coincided with the effects of different seasons and farming activities on residue levels of the pesticides in use. The objective was to investigate lev...

  13. Organochlorine pesticide residue levels in soil from the Nyando river catchment, Kenya

    Abong'o, D.A.; S.O. Wandiga; Jumba, I.O.; Brink, van den, W.; Nazariwo, B.B.; Madadi, V.O.; Wafula, H.; Kylin, H.

    2015-01-01

    Soil samples were collected from six locations representative of the Nyando River catchment area of the Lake Victoria over a period of two years. Sampling was done four times in the year in February, May, September and December 2005 and 2006 in farms where maize, tea, sugar cane, coffee, rice and vegetables have been grown over the years. This coincided with the effects of different seasons and farming activities on residue levels of the pesticides in use. The objective was to investigate lev...

  14. Determination of pesticide residues in plant-based foods from the Republic of Macedonia

    Kostik, Vesna; Angelovska, Bistra; Kiroska-Petreska, Evgenija; Bauer, Biljana

    2014-01-01

    The present study investigates pesticide residues in samples of fresh and processed fruits and vegetables produced in Republic of Macedonia. Investigations were carried out as a part of the National Monitoring Programme under the recommendations of the European Food Safety Authority (EFSA). From September 2012 to June 2013, a total of 168 samples of different fresh vegetables: tomato, paprika, cucumber, potato, onion, carrot, cabbage; processed vegetables: pasteurized paprika, ketchup; fresh ...

  15. Guidance on the use of probabilistic methodology for modelling dietary exposure to pesticide residues

    Hart, A; Ossendorp, B.C.; Hamey, P.; Van Klaveren, J.; Kennedy, M.; Miller, D.C.M.; Petersen, A.; Pico, Y.; Stromberg, A.; van der Voet, H.

    2012-01-01

    The European Food Safety Authority (EFSA) asked the Panel on Plant Protection Products and their Residues to provide guidance on methodology for performing probabilistic dietary exposure assessment of single or multiple active substances, as a potential additional tool to supplement or complement the standard deterministic methodologies which are currently used in the EU for conducting dietary exposure assessments for pesticides. Specific guidance is provided for basic assessments but not for...

  16. Organochlorine Pesticide Residues in Sediments and Waters from Cocoa Producing Areas of Ondo State, Southwestern Nigeria

    Aderonke Adetutu Okoya; Aderemi Okunola Ogunfowokan; Olabode Idowu Asubiojo; Nelson Torto

    2013-01-01

    This study investigated levels of organochlorine pesticide (OCP) residues in water and sediment samples from eleven rivers serving as drinking water sources and receiving runoff from nearby cocoa plantations in Ondo State, Nigeria. Twenty-two composite samples of surface water and sediments (0–3 cm) were collected randomly using grab technique and replicated thrice per season. The efficiency of the two techniques [supercritical fluid extraction (SFE) and liquid/liquid extraction (LLE)] was ev...

  17. Assessment of organochlorine pesticides and atrazine residues in Maize Produced in Ghana using GC-ECD/ GC-MS

    Maize is consumed by over 95% of the Ghanaian populace and the practice of using atrazine, lindane and other organochlorine pesticides in its production has raised concerns about potential adverse effects on human health and the environment. A field survey was conducted in this study to assess farmers’ knowledge of safe handling and use of these chemicals as well as toxicity awareness and symptoms among farmers and traders. Residues of the pesticides in maize samples as well as the potential health risk associated with exposure to them were also evaluated. Data obtained from the field survey indicate that a large proportion of farmers are at risk of pesticide poisoning through occupational exposure. Over 80 % of applicators do not apply safety precautions during pesticide mixing and application; resulting in considerable prevalence of pesticide related illnesses in the study area. Residues of lindane and atrazine were below detection limits of 0.005 mg/kg and 0.010 mg/kg respectively of the GC-ECD/MS used for the analysis; except in the Ashanti region where atrazine was 0.05 mg/kg which is within the EU-MRL of 0.1 mg/kg. However, minute concentrations of other organochlorines (endrin- 0.007 mg/kg; heptachlor- 0.023 mg/kg; alpha-endosulfan- 0.013 mg/kg) were found in maize samples from Brong Ahafo, Eastern, Central and Upper west regions. Though endrin and alpha-endosulfan were below the EU-MRL of 0.01 mg/kg and 0.10 mg/kg respectively, heptachlor was slightly above the EU-MRL of 0.01 mg/kg. The estimated doses for all these other organochlorines pesticides do not pose direct hazard to human health because their estimated dose values were lower than toxic thresholds and reference doses. However, due to the unsafe application practices by applicators, there exists a potential risk for systemic and carcinogenic health effects by these chemicals in the study area. (au)

  18. Contribution to the food products' analysis: A research and evaluation on the hemolytic effect of some pesticides used in Lebanon.

    Al-Alam, Josephine; Millet, Maurice; Chbani, Asma; Fajloun, Ziad

    2015-01-01

    Pesticides are a real concern for the society as their use has become critical, leading sometimes to their accumulation as residues in fruits and vegetables. After examining the pesticides sold in Northern Lebanon, this study is focused on the analysis and identification of pesticides residues in fruits and vegetables that are harvested in this region and treated with the locally sold pesticides. Results show: first, (i) a use of Zineb by the name of another pesticide Micronized Sulfur to avoid prosecution; (ii) a significant presence of Metalaxyl in lemons and oranges; (iii) a significant presence of Trifluralin in strawberries; and (iv) a significant presence of Zineb in lemons and tomatoes. Second, with the use of hemolytic tests on human blood results show: (i) a critical concentration and a significant hemolytic effect of some pesticides used in Lebanon; and (ii) an absence of hemolytic effect in the collected fractions of the different analyzed fruit extracts containing pesticides. Finally, this work is the first step for pesticides' analysis in vegetables and fruits in Lebanon, initiating a wider analytical study in order to control and examine the use of pesticides which, according to our results, could have an adverse effect on human health over a long term. PMID:26357889

  19. Pesticide residues in some herbs growing in agricultural areas in Poland

    Elżbieta MALINOWSKA; Jankowski, Kazimierz

    2015-01-01

    The aim of this paper was to assess residue content of plant protection products in selected herbs: Achillea millefolium L., Cichorium intybus L., Equisetum arvense L., Polygonum persicaria L., Plantago lanceolata L., and Plantago major L. The study comprises herbs growing in their natural habitat, 1 and 10 m away from crop fields. The herbs, 30 plants of each species, were sampled during the flowering stage between 1 and 20 July 2014. Pesticide residue content was measured with the QuECHERS ...

  20. A residue-free green synergistic antifungal nanotechnology for pesticide thiram by ZnO nanoparticles

    Jingzhe Xue; Zhihui Luo; Ping Li; Yaping Ding; Yi Cui; Qingsheng Wu

    2014-01-01

    Here we reported a residue-free green nanotechnology which synergistically enhance the pesticides efficiency and successively eliminate its residue. We built up a composite antifungal system by a simple pre-treating and assembling procedure for investigating synergy. Investigations showed 0.25 g/L ZnO nanoparticles (NPs) with 0.01 g/L thiram could inhibit the fungal growth in a synergistic mode. More importantly, the 0.25 g/L ZnO NPs completely degraded 0.01 g/L thiram under simulated sunligh...

  1. Determination of pesticide residues in fruits of Nawabshah district, Sindh, Pakistan

    Eight fruit samples of apple, guava, orange, grapes, pear, persimmon, banana and pear purchased from the local markets of Nawabshah district, Sindh and residues of pesticide of organophosphate (OP), pyrethroid and organochlorine (OC) (i.e., dichlorvos, fenvalerate, dimethoate, methyl parathion, fenitrothion, cypermethrin, endosulfan, deltamethrin, mevinphos, chlorpyriphos, profenofos and dicofol) were monitored in fruit samples by Gas Chromatography (GC). All the fruit samples were found contaminated except banana and among these only apple samples were found exceeding the maximum residue limits (MRL) of Codex Alimentarius Commission. (author)

  2. 75 FR 32463 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-06-08

    ... Cosmetic Act (FFDCA), 21 U.S.C. 346a, proposing the establishment or modification of regulations in 40 CFR... method to determine residues in raw agricultural commodities has not been proposed. No residue chemistry... organic solvent extraction, column cleanup and quantitation by LC/MS/MS. The method of analysis in...

  3. Formation of non-extractable pesticide residues: observations on compound differences, measurement and regulatory issues

    Six major use pesticides (Atrazine, Dicamba, Isoproturon, Lindane, Paraquat and Trifluralin) with differing physico-chemical properties were evaluated for the significance of 'bound' or non extractable residue formation. Investigations were carried out in purpose-built microcosms where mineralization, volatilisation, 'soil water' extractable and organic solvent extractable residues could be quantified. Extractable residues were defined as those accessible by sequential extraction where the solvent used became increasingly non-polar. Dichloromethane was the 'harshest' solvent used at the end of the sequential extraction procedure. 14C-labelled volatilised and 14CO2 fractions were trapped on exit from the microcosm. The pesticides were categorised into 3 classes based on their behaviour. (i) Type A (Atrazine, Lindane and Trifluralin) in which ring degradation was limited as was the formation of non-extractable residues; the remainder of the 14C-activity was found in the extractable fraction. (ii) Type B (Dicamba and Isoproturon) in which approximately 25% of the 14C-activity was mineralised and a large portion was found in the non-extractable fraction after 91 days. Finally, Type C (Paraquat) in which almost all of the 14C-activity was quickly incorporated into the non-extractable fraction. The implications of the data are discussed, with respect to the variability and significance of regulatory aspects of non-extractable residues

  4. [Validation study on a rapid multi-residue method for determination of pesticide residues in vegetables and fruits by LC-MS/MS].

    Takatori, Satoshi; Yamamoto, Haruna; Fukui, Naoki; Yamaguchi, Satoko; Kitagawa, Yoko; Kakimoto, You; Osakada, Masakazu; Okihashi, Masahiro; Kajimura, Keiji; Obana, Hirotaka

    2013-01-01

    A validation study was conducted on a rapid multiresidue method for determination of pesticide residues in vegetables and fruits by LC-MS/MS. Pesticide residues in the vegetables or fruits were extracted with acetonitrile in a disposable tube using a homogenizer, followed by salting out with anhydrous magnesium sulfate and sodium chloride in the presence of citrate salts for buffering. The extract was purified with a double-layered cartridge column (graphite carbon black/primary secondary amine silica gel; GCB/PSA). For citrus fruits a purification step with a C18 column was added (this column was connected to the GCB/PSA column). After removal of the solvent, the extract was resolved in methanol/water and analyzed by means of LC-MS/MS. The method was validated according to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan; recovery tests were performed on 8 kinds of vegetables and fruits [cabbage, cucumber, Japanese radish, onion, potato, spinach, Amanatsumikan (a citrus fruit) and apple] by fortification of 161 pesticide residues at the concentrations 0.01 and 0.05 ?g/g (each concentration of pesticide residue was extracted from 2 samples on 5 separate days). The trueness of the method for 127 pesticides in all 8 commodities was 70-120% with satisfactory repeatability and within-run reproducibility. This method is concluded to be applicable for determination of pesticide residues in vegetables and fruits. PMID:23863370

  5. Bound pesticide residues in soil, plants and food with particular emphasis on the application of nuclear techniques

    Although so-called bound residues have been detected for all classes of chemicals investigated so far, their quantitative levels have wide-ranging differences, depending on the chemical structure of the pesticide; phenols and nitrogen-containing pesticides exhibit the highest binding rates. The portion of bound residues in soil and plants increases with time and varies with environmental conditions (soil and plant type, climatic conditions, etc.). So far the chemical identity of bound residues has only been elucidated for a limited number of model substances by using various liberation techniques. Most information is available on anilines; models have been developed demonstrating their copolymerization into natural macromolecules (humic acids, lignin). Misinterpretation of natural products assimilated from totally degraded pesticides, as bound xenobiotic residues can only be excluded by the sophisticated separation and identification procedures of all residues. Studies on the persistence of bound residues showed differing mineralization rates, depending on the chemical structures of the pesticides; research on the bioavailability revealed that for all pesticides low amounts of soil-bound residues are taken up by plants, and that plant-bound residues are eliminated rather quickly by mammals in the faeces. (author)

  6. Effect of Chinese traditional cooking on eight pesticides residue during cowpea processing.

    Huan, Zhibo; Xu, Zhi; Jiang, Wayne; Chen, Zhiqiang; Luo, Jinhui

    2015-03-01

    Thermal processing can concentrate residues or convert residues to more toxic metabolites in food. Chinese traditional cooking pays more attention to thermal processing and more vegetables were eaten after thermal processing. In this study, the effect of Chinese traditional cooking (washing, blanching, stir-frying, frying and combined operations) on eight pesticides residues (pyridaben, procymidone, chlorothalonil, difenoconazole, α-cypermethrin, bifenthrin, S-fenvalerate and λ-cyhalothrin) in cowpea which was one of the most important legume crops in China was examined. Result showed washing and blanching could reduce residues with low Kow while stir-frying and frying were more effective to residues with high Kow; stir-frying and frying could concentrate residues with low Kow; the residue levels in oil increased following increasing frying time and frequency especially the residues with high Kow; one metabolite studied in this paper was not detected. Blanching (5 min) followed by stir-frying (3 min) was the most effective combined operation. PMID:25306325

  7. Toxaphene and other chlorinated pesticide residues in butter (1972 - 1978) and canned beef (1976 - 1977) in Kenya

    This paper reports the analysis of butter sample manufactured 1972-1978 and canned beef samples manufactured 1976-1977 in Kenya for pesticide residues, particularly for toxaphene, the main acaricide in use from 1960-1976. It was found that levels of toxaphene in butter ranged from 6.5-16.2 ppm (fat basis) during extensive use of acricide, which gradually decreased to non-detectable levels by 1978. Toxaphene residues in canned beef ranged from 1.2-18.5 ppm (fat basis) during 1976. Traces were still evident (0.2-0.7 ppm) by 1977. Low levels of BHC and DDE were also indicated in the samples. The levels ranged from 0.1-0.28 ppm total BHC and 0.02-0.27 DDE (fat basis ) in the butter. Canned beef samples indicated levels of 0.02-0.06 ppm total BHC and 0.02-0.57 ppmDDE(fat basis). (author)

  8. Rapid analysis for 567 pesticides and endocrine disrupters by GC/MS using deconvolution reporting software

    Wylie, P.; Szelewski, M.; Meng, Chin-Kai [Agilent Technologies, Wilmington, DE (United States)

    2004-09-15

    More than 700 pesticides are approved for use around the world, many of which are suspected endocrine disrupters. Other pesticides, though no longer used, persist in the environment where they bioaccumulate in the flora and fauna. Analytical methods target only a subset of the possible compounds. The analysis of food and environmental samples for pesticides is usually complicated by the presence of co-extracted natural products. Food or tissue extracts can be exceedingly complex matrices that require several stages of sample cleanup prior to analysis. Even then, it can be difficult to detect trace levels of contaminants in the presence of the remaining matrix. For efficiency, multi-residue methods (MRMs) must be used to analyze for most pesticides. Traditionally, these methods have relied upon gas chromatography (GC) with a constellation of element-selective detectors to locate pesticides in the midst of a variable matrix. GC with mass spectral detection (GC/MS) has been widely used for confirmation of hits. Liquid chromatography (LC) has been used for those compounds that are not amenable to GC. Today, more and more pesticide laboratories are relying upon LC with mass spectral detection (LC/MS) and GC/MS as their primary analytical tools. Still, most MRMs are target compound methods that look for a small subset of the possible pesticides. Any compound not on the target list is likely to be missed by these methods. Using the techniques of retention time locking (RTL) and RTL database searching together with spectral deconvolution, a method has been developed to screen for 567 pesticides and suspected endocrine disrupters in a single GC/MS analysis. Spectral deconvolution helps to identify pesticides even when they co-elute with matrix compounds while RTL helps to eliminate false positives and gives greater confidence in the results.

  9. Pesticide residues in some herbs growing in agricultural areas in Poland.

    Malinowska, Elżbieta; Jankowski, Kazimierz

    2015-12-01

    The aim of this paper was to assess residue content of plant protection products in selected herbs: Achillea millefolium L., Cichorium intybus L., Equisetum arvense L., Polygonum persicaria L., Plantago lanceolata L., and Plantago major L. The study comprises herbs growing in their natural habitat, 1 and 10 m away from crop fields. The herbs, 30 plants of each species, were sampled during the flowering stage between 1 and 20 July 2014. Pesticide residue content was measured with the QuECHERS method in the dry matter of leaves, stalks, and inflorescence, all mixed together. Out of six herb species growing close to wheat and maize fields, pesticide residues were found in three species: A. millefolium L., E. arvense L., and P. lanceolata L. Most plants containing the residues grew 1 m away from the wheat field. Two active substances of fungicides were found: diphenylamine and tebuconazole, and one active substance of insecticides: chlorpyrifos-ethyl. Those substances are illegal to use on herbal plants. Samples of E. arvense L. and P. lanceolata L. contained two active substances each, which constituted 10% of all samples, while A. millefolium L. contained one substance, which is 6.6% of all samples. PMID:26612566

  10. De-contamination of pesticide residues in food by ionizing radiation

    Basfar, Ahmed A.; Mohamed, Khaled A.; Al-Saqer, Omar A.

    2012-04-01

    The role of gamma irradiation on removal of pesticides in aqueous solutions or in vegetables and fruits was investigated. Radiation - induced decontamination of pesticides is generally greater in aqueous solutions than in selected vegetables and fruits. Residues of malathion (0.5 ppm in potatoes, 8 ppm in onions and dates), pirimiphos-methyl (1 ppm in onions and grapes) and cypermethrin (0.05 ppm in potatoes and 0.1 ppm in onions) were not reduced to below maximum residue limits (MRLs) for irradiation doses up to 1 kGy. The same trend was observed when irradiation was performed for grapes fortified with malathion (8 ppm) and cypermethrin (2 ppm) for absorbed doses up to 2 kGy. Ionizing radiation reduced the residues of pirimiphos-methyl (0.05 ppm in potatoes at1 kGy, 1 ppm in grapes at 2 kGy and 0.1 ppm in dates at1 kGy), malathion (8 ppm in grapes at 7 kGy) and cypermethrin (2 ppm in grapes at 7 kGy) to below maximum residue limits (MRLs).

  11. Organochlorine pesticide residues in catfish, Tachysurus thalassinus (Ruppell, 1835), from the South Patches of the Bay of Bengal

    Pesticide concentrations in fish were lower than recommended for human consumption. - Organochlorine pesticides (p,p'-DDT, p,p'-DDD, p,p'-DDE, aldrin, lindane, and heptachlor) were measured in muscle tissue of catfish (Tachysurus thalassinus) during the dry and wet season. Catfish were collected from the South Patches of the Bay of Bengal during October-December 1997 and May-July 1998. Tissue residues were analyzed by using gas-chromatography (GC) in electron capture detector (ECD) mode and were verified by thin layer chromatography (TLC). The pesticide residues levels were found in order of ? DDT>Heptachlor>Lindane>Aldrin. Higher levels of pesticide residues were found in all samples during dry season, as compared with the wet season, primarily due to elevated lipid content in fishes. A positive correlation and linear relationship was observed between the pesticide residues (?DDT and ?OCs) and lipid content of fishes. However, the concentrations of pesticide residues in the muscle were found to be lower than the FAO/WHO [(1993) Food standards programme. Codex Alimentarius Commission, vol. 9 (4) pp. 149-158] recommended permissible limit for human consumption

  12. Enhanced Dissipation of Triazole and Multiclass Pesticide Residues on Grapes after Foliar Application of Grapevine-Associated Bacillus Species.

    Salunkhe, Varsha P; Sawant, Indu S; Banerjee, Kaushik; Wadkar, Pallavi N; Sawant, Sanjay D

    2015-12-23

    Disease management in vineyards with fungicides sometimes results in undesirable residue accumulations in grapes at harvest. Bioaugmentation of the grape fructosphere can be a useful approach for enhancing the degradation rate and reducing the residues to safe levels. This paper reports the in vitro and in vivo biodegradation of three triazole fungicides commonly used in Indian vineyards, by Bacillus strains, namely, DR-39, CS-126, TL-171, and TS-204, which were earlier found to enhance the dissipation rate of profenophos and carbendazim. The strains utilized the triazoles as carbon source and enhanced their in vitro rate of degradation. Myclobutanil, tetraconazole, and flusilazole were applied in separate vineyard plots at field doses of 0.40 g L(-1), 0.75 mL L(-1), and 0.125 mL L(-1), respectively. Residue analysis of field samples from the treated fields reflected 87.38 and >99% degradations of myclobutanil and tetraconazole, respectively, by the strain DR-39, and 90.82% degradation of flusilazole by the strain CS-126 after 15-20 days of treatment. In the respective controls, the corresponding percent degradations were 72.07, 58.88, and 54.28, respectively. These Bacillus strains could also simultaneously degrade the residues of profenofos, carbendazim, and tetraconazole on the grape berries and can be useful in multiclass pesticide residue biodegradation. PMID:26492206

  13. Monitoring of pesticide residues in apples, lettuce and potato of the Slovene origin, 2001-04.

    Cesnik, H Basa; Gregorcic, A; Bolta, S Velikonja; Kmecl, V

    2006-02-01

    Apples, lettuce and potatoes (404 samples) produced in the Republic of Slovenia were analysed for pesticide residues at the Agricultural Institute of Slovenia, Ljubljana, in 2001-04. Sampling from eight agricultural production areas was performed at market producers at the harvesting of products or in storehouses after the pre-harvest interval of plant protection products used. Samples exceeding the maximum residue levels were the following: three apple samples (2.0%) containing 0.33-2.24 mg kg(-1) (phosalone and tolylfluanid), three lettuce samples (3.1%) containing 0.14-6.36 mg kg(-1) (dimethoate, dithiocarbamates and metalaxyl) and 36 potato samples (23.1%) containing 0.06-0.51 mg kg(-1) (dithiocarbamates). Residues of two or more active substances were found in 73 apple samples (48.3%), of which the maximum residue limit (MRL) was exceeded by three samples (2.0%) with the values ranging from 0.33 to 2.24 mg kg(-1), and nine lettuce samples (9.3%), for which the MRL was exceeded by three samples (3.1%) with values from 0.14 to 6.36 mg kg(-1). In potato samples, only residues of dithiocarbamates or no residues at all were found. Residues of the dithiocarbamate group were the most frequently found, i.e. in 66 apple samples (43.7%), 30 lettuce samples (30.9%) and 38 potato samples (24.4%). PMID:16449059

  14. Resduos de agrotxicos em alimentos: uma preocupao ambiental global - Um enfoque s mas Residues of pesticides in food: a global environmental preoccupation - Focussing on apples

    Isabel Cristina Sales Fontes Jardim

    2009-01-01

    Full Text Available This paper describes the use of pesticides in agriculture. Research has shown that significant quantities of pesticide residues have been found in many types of foods. Thus, an overview is given of pesticide residue determinations in fruits and vegetables, with special attention to apples. The toxicity and the adverse effects possibly caused by the exposure of these compounds are alerting the scientific community to develop studies about the validation of analytical methods for multiresidue pesticide determination in these samples. This review shows that pesticide-residue determination in apples is becoming a very important and challenging issue.

  15. Isotope aided studies of pesticide residues during food processing. Report of a final research co-ordination meeting held in Bangkok, Thailand, 31 January - 4 February 1994

    The use of agrochemicals in general and pesticides in particular has greatly aided crop production, protected man from diseases, decreased losses of stored grains and has generally improved man's welfare. One of the steps in ensuring safety of pesticides is adequate monitoring programmes for residue levels in food products and the agricultural environment. Oil-bearing plants often receive heavy pesticide treatment and known to accumulate high concentration of pesticide residues. Technical documents included in this volume report effect of refining or processing of various oil crops like soybean, olive oil, coconut, rapeseed, sunflower cottonseed corn, peanut oil on 14C-compound pesticide residues. Refs, figs and tabs

  16. Investigations on antibody binding to a micro-cantilever coated with a BAM pesticide residue

    Aamand Jens

    2011-01-01

    Full Text Available Abstract The attachment of an antibody to an antigen-coated cantilever has been investigated by repeated experiments, using a cantilever-based detection system by Cantion A/S. The stress induced by the binding of a pesticide residue BAM (2,6 dichlorobenzamide immobilized on a cantilever surface to anti-BAM antibody is measured using the CantiLab4 system from Cantion A/S with four gold-coated cantilevers and piezo resistive readout. The detection mechanism is in principle label-free, but fluorescent-marked antibodies have been used to subsequently verify the binding on the cantilever surface. The bending and increase in mass of each cantilever has also been investigated using a light interferometer and a Doppler Vibrometer. The system has been analyzed during repeated measurements to investigate whether the CantiLab4 system is a suited platform for a pesticide assay system.

  17. Classification and modelling of non-extractable residue (NER) formation from pesticides in soil

    Kästner, M.; Nowak, K. M.; Miltner, A.; Trapp, Stefan; Schaeffer, A.

    2015-01-01

    undergo turnover processes and can be volatilised, leached to the groundwater, degraded by microorganisms or taken up and enriched by living organisms. Xenobiotic NER may be derived from parent compounds and primary metabolites that are sequestered (sorbed or entrapped) within the soil organic matter......This presentation provides a comprehensive overview about the formation of nonextractable residues (NER) from organic pesticides and contaminants in soil and tries classifying the different types. Anthropogenic organic chemicals are deliberately (e.g. pesticides) or unintentionally (e.......g. polyaromatic hydrocarbons [PAH], chlorinated solvents, pharmaceuticals) released in major amounts to nearly all compartments of the environment. Soils and sediments as complex matrices provide a wide variety of binding sites and are the major sinks for these compounds. Many of the xenobiotics entering soil...

  18. 40 CFR 158.2171 - Experimental use permit microbial pesticides product analysis data requirements table.

    2010-07-01

    ... pesticides product analysis data requirements table. 158.2171 Section 158.2171 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Microbial Pesticides § 158.2171 Experimental use permit microbial pesticides product analysis data requirements...

  19. 40 CFR 158.2120 - Microbial pesticides product analysis data requirements table.

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Microbial pesticides product analysis... AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Microbial Pesticides § 158.2120 Microbial pesticides product analysis data requirements table. (a) General. Sections 158.100 through...

  20. A novel chemiluminescence assay of organophosphorous pesticide quinalphos residue in vegetable with luminol detection

    Yao Xin

    2010-06-01

    Full Text Available Abstract Background Organophosphorous pesticides are the most popular pesticides used in agriculture. As acetylcholinesterase inhibitors, organophosphorous pesticides are toxic organic chemicals. The control and detection of organophosphorous pesticide residue in food, water, and environment therefore plays a very important role in maintaining physical health. A sensitive, rapid, simple chemiluminescence(CL method has been developed for the determination of quinalphos based on the reaction of quinalphos with luminol-H2O2 in an alkaline medium. The method has been applied to detection of quinalphos in vegetable samples with satisfactory results. Results The CL method for the determination of organophosphorous pesticide quinalphos is based on the phenomenon that quinalphos can apparently enhance the CL intensity of the luminol-H2O2 system. The optimal conditions were: luminol concentration 5.0 10-4 mol/L, H2O2 concentration 0.05 mol/L.pH value 13. In order to restrain the interference from metal ions, 1.0 10-3 mol/L of EDTA was added to the luminol solution. The possible mechanism was proposed. Conclusion Under the optimum reaction conditions, CL was linear with the concentration of quinalphos in the range of 0.02 ?g/mL -1.0 ?g/mL and the detection limit was 0.0055 ?g/mL (3?. This method has been successfully applied to the detection of quinalphos in vegetable samples. According to the experimental data, the average recoveries for quinalphos in cherry tomato and green pepper 97.20% and 90.13%. Meanwhile, the possible mechanism was proposed.

  1. Determination of pesticide residues in tea by gas chromatography/triple quadrupole mass spectrometry with solid-phase extraction.

    Zhao, Chang-Le; Ding, Rui-Yan; Huo, Lu-Ge; Li, Hui-Dong; Dong, Zhan; Wang, Fen-En; Yang, Guo-Sheng; Lu, Xiao; Aboul-Enein, Hassan Y

    2014-01-01

    An analytical method was developed for determination of multipesticide residues, including organophosphorus, organohalogen, pyrethroid, and organonitrogen, in tea at trace levels by GC coupled with triple quadrupole mass chromatography (QqQ-MS/MS). Scan time was selected in order to optimize QqQ-MS/MS conditions. The key parameters for controlling cleanup performance were optimized, including SPE cartridge type and elution solvent volume. Acetonitrile was the extraction solvent, and a novel multilayer SPE cartridge, Cleanert TPT, was used in the cleanup step. The recoveries of the studied pesticides at 5.0, 10.0, and 25.0 microg/kg were in the range of 77.8 to 103.8% with an RSD of less than 14%. Determination coefficient (R2) values between 0.9951 and 0.9998 were obtained for all target compounds. The LOD was between 0.002 and 1.0 microg/kg, and LOQs were 0.0066-3.3 microg/kg, which satisfied the maximum residue limits for pesticides in tea recommended by the European Union and Japan. The optimized method was applied to the analysis of real tea samples obtained from the local market. PMID:25145129

  2. [Determination of 30 carbamate pesticide residues in vegetative foods by QuEChERS-liquid chromatography-tandem mass spectrometry].

    Da, Jing; Wang, Gangli; Cao, Jin; Zhang, Qingsheng

    2015-08-01

    Via the classification of vegetative foods in British Standard EN 15662, six representative food matrices were chosen in the current study. The QuEChERS method for each matrix was optimized. The 30 carbamate pesticide residues in the samples after pretreatment were determined by liquid chromatography-tandem mass spectrometry in positive ionization mode. According to the experimental results, the linear ranges were 1-100 µg/kg for aldicarb sulfone and 2-100 µg/kg for the others. The recoveries at three spiked levels of 5, 20 and 100 µg/kg in the six representative matrices were between 56.13% and 127.6%, with the RSDs between 0.47% and 16%. The limits of quantification (S/N-10) were in the range of 0.041-1.9 kg/kg. In conclusion, this method provides a sensitive and efficient way suitable for the analysis of the 30 carbamate pesticide residues in vegetative foods. PMID:26749859

  3. Residual gas analysis device

    Thornberg, Steven M. (Peralta, NM)

    2012-07-31

    A system is provided for testing the hermeticity of a package, such as a microelectromechanical systems package containing a sealed gas volume, with a sampling device that has the capability to isolate the package and breach the gas seal connected to a pulse valve that can controllably transmit small volumes down to 2 nanoliters to a gas chamber for analysis using gas chromatography/mass spectroscopy diagnostics.

  4. Rapid and effective sample clean-up based on magnetic multiwalled carbon nanotubes for the determination of pesticide residues in tea by gas chromatography-mass spectrometry.

    Deng, Xiaojuan; Guo, Qianjin; Chen, Xiaoping; Xue, Tao; Wang, Hui; Yao, Pei

    2014-02-15

    In this work, amine-functionalised magnetic nanoparticles and multiwalled carbon nanotubes (MNPs/MWCNTs) composites were synthesised by a simple method and applied as an adsorbent for rapid clean-up of acetonitrile extracts of tea samples prior to analysing eight pesticide residues by gas chromatography-mass spectrometry. Several parameters affecting the sampling and treatment efficiency were investigated, including extraction solvent, sonication time, weight ratio of MWCNTs to MNPs in the composites, amount of adsorbent, clean-up time and washing solution. Under the optimised conditions, the recoveries obtained for each pesticide ranged from 72.5% to 109.1% with relative standard deviations lower than 12.6%. Limit of quantification ranged from 0.02 to 0.08 mg kg⁻¹. The established method was successfully applied to the analysis of pesticide residues in real tea samples. The results indicated that the use of MNPs/MWCNTs composites allowed the simple and expeditious clean-up of complex tea samples for subsequent determination of pesticide residues. PMID:24128556

  5. Chlorinated pesticide residues in surface sediments from the River Kaveri, south India.

    Rajendran, R B; Subramanian, A N

    1999-03-01

    Chlorinated compounds have preferential attraction for organic phases found in sediments. Usage of chlorinated pesticides in agriculture and vector control is more in developing countries. The residue levels of HCH isomers, and DDT, and its metabolites were quantified in surface sediments from the River kaveri and Coleroon in Tamil Nadu state, South India. The concentration of HCH ranged from 4.35 to 158.4 ng g-1 (dry wt.). Among the isomers of HCH, alpha-HCH is predominant followed by beta and gamma-HCH. The levels of DDT varied from 0.69 to 4.85 ng g-1 (dry wt.). Among the DDT compounds, p,p'-DDE quantified more (> 40%) in all the sites. This suggests that p,p'-DDE is a major breakdown (dehydrochlorination) product of DDT in the sediment compartment. Higher concentration of HCH residues reveals its large usage in agriculture. The flux of pesticide residues from land to river including downward flux to sediment is less. PMID:10192957

  6. Adaptation and validation of the TLC detection methods in determination of pesticide residues in grain

    This work was performed to investigate the possibilities of applying prescribed TLC detection methods in combination with GPC cleanup procedure in grains as alternative methods to gas and high performance liquid chromatography for pesticide residue analyses. The MDQ, RF and RRf values of marker and selected compounds were close to those reported in the basic method. The recoveries and reproducibility of the method obtained with wheat and rice samples in our laboratory were within the limits specified by the Codex GLs on method validation. The recoveries determined by GC analyses were practically the same which confirms the accuracy of TLC detection. (author)

  7. Evaluation of pesticide residues in drinking water in different areas of khyber pakhtunkhwa, pakistan

    Flood in 2010 severely effected different areas of Khyber Pakhtunkhwa, Sindh, lower Punjab as well as some parts of Balochistan, Pakistan. After the flood, samples of drinking water were collected from the affected areas i.e. Akora Khattak and Buner, Khyber Pakhtunkhwa and pesticides residues were determined quantitatively in these samples employing GC-MS technique. Among the samples collected from Akora Khattak, chlorpyrifos was found in high amounts i.e. 0.040 ppm, in sample no. 6 while methamidophos and methiocarb were found in appreciable quantities i.e. 0.026 ppm and 0.038 ppm, respectively, in sample no. 4. Methamidophos and methiocarb were found in appreciable amounts i.e. 0.039 ppm and 0.034 ppm, respectively, in sample no. 17 among the samples obtained from Buner. Concentrations were found at the level below 0.01 ppm in most of the pesticides under study. From the results it appears that drinking water sources in the area under study have been contaminated with pesticides which is a health hazard and may be a source of various diseases in these areas. (author)

  8. Evaluation of the performance of a castor-oil based formulation in limiting pesticide residues in strawberry crops

    Mrio Srgio, Galhiane; Sandra Regina, Rissato; Lucdio de Sousa, Santos; Gilberto Orivaldo, Chierice; Marcos Vincius de, Almeida; Terezinha, Fumis; Ins, Chechim; Alosio Costa, Sampaio.

    Full Text Available A study was made to evaluate the effect of a castor oil-based detergent on strawberry crops treated with different classes of pesticides, namely deltamethrin, folpet, tebuconazole, abamectin and mancozeb, in a controlled environment. Experimental crops of greenhouse strawberries were cultivated in f [...] ive different ways with control groups using pesticides and castor oil-based detergent. The results showed that the group 2, which was treated with castor oil-based detergent, presented the lowest amount of pesticide residues and the highest quality of fruit produced.

  9. Evaluation of the performance of a castor-oil based formulation in limiting pesticide residues in strawberry crops

    Mrio Srgio Galhiane

    2012-01-01

    Full Text Available A study was made to evaluate the effect of a castor oil-based detergent on strawberry crops treated with different classes of pesticides, namely deltamethrin, folpet, tebuconazole, abamectin and mancozeb, in a controlled environment. Experimental crops of greenhouse strawberries were cultivated in five different ways with control groups using pesticides and castor oil-based detergent. The results showed that the group 2, which was treated with castor oil-based detergent, presented the lowest amount of pesticide residues and the highest quality of fruit produced.

  10. Monitoring of pesticide residues in market basket samples of vegetable from Lucknow City, India: QuEChERS method.

    Srivastava, Ashutosh K; Trivedi, Purushottam; Srivastava, M K; Lohani, M; Srivastava, Laxman Prasad

    2011-05-01

    The study was conducted on 20 vegetables including leafy, root, modified stem, and fruity vegetables like bitter gourd, jack fruit, french-bean, onion, colocassia, pointed gourd, capsicum, spinach, potato, fenugreek seeds, carrot, radish, cucumber, beetroot, brinjal, cauliflower, cabbage, tomato, okra, and bottle gourd. Forty-eight pesticides including 13 organochlorines (OCs), 17 organophosphates (OPs), 10 synthetic pyrethriods (SPs), and eight herbicides (H) pesticides were analyzed. A total number of 60 samples, each in triplicates, were analyzed using Quick, Easy, Cheap, Effective, Rugged, and Safe method. The quantification was done by GC-ECD/NPD. The recovery varies from 70.22% to 96.32% with relative standard deviation (RSD) of 15%. However the limit of detection ranged from 0.001-0.009 mg kg(-1)for OCs, SPs, OPs, and H, respectively. Twenty-three pesticides were detected from total 48 analyzed pesticides in the samples with the range of 0.005-12.35 mg kg(-1). The detected pesticides were: ?-HCH, Dicofol, ?-Endosulfan, Fenpropathrin, Permethrin-II, ?-cyfluthrin-II, Fenvalerate-I, Dichlorvos, Dimethoate, Diazinon, Malathion, Chlorofenvinfos, Anilophos, and Dimethachlor. In some vegetables like radish, cucumber, cauliflower, cabbage, and okra, the detected pesticides (?-HCH, Permethrin-II, Dichlorvos, and Chlorofenvinfos) were above maximum residues limit (MRL) (PFA 1954). However, in other vegetables the level of pesticide residues was either below detection limit or MRL. PMID:20632088

  11. Exploring matrix effects in liquid chromatography-tandem mass spectrometry determination of pesticide residues in tropical fruits.

    Botero-Coy, Ana María; Marín, José M; Serrano, Roque; Sancho, Juan Vicente; Hernández, Félix

    2015-05-01

    Tropical fruits are being increasingly consumed around the world because of their appreciated characteristics, particularly their high nutritional value and distinctive taste, which are different from those of traditional fruits. Owing to their introduction into international markets it is necessary to have a reliable analytical methodology available for the sensitive determination of pesticide residues in order to monitor the compliance of maximum residue limits (MRLs). From an analytical point of view, tropical fruits have generally been far less studied than other fruits frequently consumed in the European Union or USA, which are among the most important markets. In this work, LC-MS/MS-based methodology using a triple quadrupole analyzer was developed for the multi-residue determination of selected pesticides and metabolites in tropical fruits, which were selected among the most popular in Colombia, one of the most important suppliers of tropical fruits around the world. After selection of a QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe)-based sample treatment, the study focused on the evaluation of matrix effects, in order to find a simple way for their correction. Twelve different food matrices were selected to perform this study: the seven Colombian tropical fruits of highest value for domestic and international markets (uchuva, tamarillo, granadilla, gulupa, maracuya, papaya, and pithaya), and five more matrices highly consumed in Colombia (lulo, carambolo, feijoa, mangostan, and guayaba). Twenty compounds, including pesticides widely applied in tropical fruits pest control and several metabolites considered in residue definition, were used as model compounds in this work. Correction factors were used on the basis of calibration graphs obtained with standards in solvent and in matrix, and their usefulness was supported by validation of the method in all the matrices tested at 0.01 and 0.1 mg/kg. The analysis of real-world samples revealed the presence of several target compounds that were identified by the acquisition of two MS/MS transitions, and by ion intensity ratio and retention time agreement. PMID:25772561

  12. Pesticide residues in vineyard soils from Spain: Spatial and temporal distributions.

    Pose-Juan, Eva; Sánchez-Martín, María J; Andrades, M Soledad; Rodríguez-Cruz, M Sonia; Herrero-Hernández, Eliseo

    2015-05-01

    Spatial and temporal evaluations of seventeen pesticides and some of their degradation products were carried out in seventeen vineyard soils from La Rioja region (Spain). The soils were sampled in March, June and October 2012, and the pesticides were selected among those previously detected in surface and ground waters from the same area. All pesticides were detected in some of the soils in the three different areas of La Rioja at the different sampling times, with only the metalaxyl metabolite, CGA-62826, not being detected in any of the soils sampled in October. The highest concentrations were determined for the fungicides metalaxyl (11.5 μg kg(-1)) and triadimenol (26.1 μg kg(-1)), the herbicides fluometuron (174.6 μg kg(-1)) and terbuthylazine (403.3 μg kg(-1)), and the insecticide methoxyfenozide (4.61 μg kg(-1)). While the highest total concentration of pesticides was detected in March, the highest number of positive detections was recorded in June (46), as opposed to 26 and 19 in March and October, respectively. Significant differences were detected in the concentrations of herbicides in soils from the three areas in La Rioja, but this was not the case for the fungicides and the insecticides. The study revealed a more intensive use of herbicides in March, while the use of insecticides and fungicides probably depended on the specific needs of crops and/or the onset of diseases. The results are consistent with the residues found in waters in the region, and highlight the need to implement strategies for more efficient application of these compounds to avoid risk of water contamination. PMID:25679815

  13. Pesticides

    ... of children. Wear any protective clothing, such as rubber gloves, specified by the manufacturer. When using pesticides ... base of shower, dishes left in sinks). Seal cracks and crevices where cockroaches may enter the house. ...

  14. Distribution, fate and effects of pesticide residues in tropical coastal lagoons of northwestern Mexico.

    Carvalho, F P; Gonzalez-Farias, F; Villeneuve, J P; Cattini, C; Hernandez-Garza, M; Mee, L D; Fowler, S W

    2002-11-01

    Analyses of pesticide residues in sediments, water and biota of the Altata-Ensenada del Pabellon coastal lagoon system in Sinaloa, Mexico, showed the presence of organochlorine and organophosphorus compounds. For all the compounds analysed, concentrations in sediments were higher near the points of water discharge from ponds and drainage from the agricultural area. Among the organochlorines, total DDTs displayed the largest sedimentary reservoir, followed by total endosulfans and chlorpyrifos. In sediments, as well as in biota, pp'-DDT concentrations were lower than those of DDT metabolites, which confirms the reduction in the previous massive use of this compound in agriculture. Endosulfan is currently used in the region and endosulfan residues in lagoon sediments attained levels considered to be toxic to meiofauna, therefore constituting an ecological risk to lagoon ecosystems. There was a large sedimentary reservoir of chlorpyrifos but its ecotoxicological risk is difficult to assess due to lack of adequate comparative data. Nevertheless, concentrations of chlorpyrifos which approach acute toxic levels for shrimp were recorded in lagoon water. This suggests that drainage from agricultural fields during high runoff may, on occasion, cause mass mortality of shrimp and fish Organophosphorus pesticides are widely regarded to degrade very rapidly in aquatic systems. Experimental research performed with 14C-labelled chlorpyrifos and parathion has shown that they may be stabilised for relatively long periods of time through sediment-water partitioning. This extension of their environmental half-lives increases their potential for impacting on coastal ecosystems. Since organophosphorus pesticides are highly toxic for aquatic organisms at concentrations generally lower than organochlorines, their presence in the lagoon water and sediment is a matter for much concern. The increased use of tropical coastal lagoons for shrimp and fish farming requires the implementation of environmental management practices to protect these ecosystems from the impact of agricultural activities. Environmental management aims to preserve the ecosystem integrity of these coastal lagoons and, through improving the water quality, to allow the development of aquaculture and reduce human exposure to pesticide residues in food. PMID:12472156

  15. Effects of organic and conventional rice on protein efficiency ratio and pesticide residue in rats

    Wanpen Mesomya

    2012-11-01

    Full Text Available The comparative effects of organic rice and conventional rice on the protein efficiency ratio (PER in rats were investigated by feeding 40 male Sprague-Dawley rats for four weeks with three experimental diets containing polished conventional rice (PCR, unpolished conventional rice (UCR, unpolished organic rice (UOR and a control protein diet (casein under standardised conditions. All diets were prepared according to AOAC guidelines. The results showed no statistically significant difference (P > 0.05 among the values of PER (2.75 ± 0.14 - 2.80 ± 0.09 in rats fed with diets containing PCR, UCR or UOR. Similar growth was also observed among the three groups fed with different experimental diets. Additionally, residues of pesticides, viz. carbofuran, methyl parathion, p-nitrophenol and -cyfluthrin, in rat blood and rice samples were determined using liquid chromatography–electrospray ionisation tandem mass spectrometry. Pesticide residues were not detected in all serum samples of experimental rats and only p-nitrophenol was found (8.23 ± 0.65 - 12.84 ± 2.58 mg/kg in all samples of the cooked rice diets, indicating that organic rice produced similar effect as conventional rice on PER and growth in rats.

  16. Assessing the distribution and human health risk of organochlorine pesticide residues in sediments from selected rivers.

    Ogbeide, Ozekeke; Tongo, Isioma; Ezemonye, Lawrence

    2016-02-01

    Sediment samples from major agricultural producing areas in Edo state Nigeria were analysed for ?-HCH, ?-HCH, ?-HCH and ?DDT with the aim of elucidating contamination profiles, distribution characteristics, carcinogenic and non-carcinogenic risk of these compounds in these regions. Analysis was done using a gas chromatography (GC) equipped with electron capture detector (ECD), while health risk assessment was carried out using the Incremental Lifetime Cancer Risk (ILCR) and the chronic daily intake (CDI). Results showed varying concentrations of ?-HCH, ?-HCH, ?-HCH and ?DDT pesticides in sediment samples with hexachlorocyclohexane (?HCHs) (4.6g/g/dw) being the dominant contaminants as it was widely detected in all samples and stations. Source identification revealed that the current levels of HCHs and DDT in sediments were attributed to both historical use and fresh usage of these pesticides. Risk estimates using ILCR and CDI showed that the risk of cancer and non-cancer effects was highest when exposure route was through ingestion. Furthermore, model projections highlights children as high risk population groups for non-dietary exposure to OCPs. These findings suggests the need for increased monitoring programmes, with a wider scope for both currently used pesticides and legacy/banned pesticides. PMID:26476770

  17. Shell thickness-dependent Raman enhancement for rapid identification and detection of pesticide residues at fruit peels.

    Liu, Bianhua; Han, Guangmei; Zhang, Zhongping; Liu, Renyong; Jiang, Changlong; Wang, Suhua; Han, Ming-Yong

    2012-01-01

    Here, we report the shell thickness-dependent Raman enhancement of silver-coated gold nanoparticles (Au@Ag NPs) for the identification and detection of pesticide residues at various fruit peels. The Raman enhancement of Au@Ag NPs to a large family of sulfur-containing pesticides is ~2 orders of magnitude stronger than those of bare Au and Ag NPs, and there is a strong dependence of the Raman enhancement on the Ag shell thickness. It has been shown for the first time that the huge Raman enhancement is contributed by individual Au@Ag NPs rather than aggregated Au@Ag NPs with "hot spots" among the neighboring NPs. Therefore, the Au@Ag NPs with excellent individual-particle enhancement can be exploited as stand-alone-particle Raman amplifiers for the surface identification and detection of pesticide residues at various peels of fruits, such as apple, grape, mango, pear, and peach. By casting the particle sensors onto fruit peels, several types of pesticide residues (e.g., thiocarbamate and organophosphorous compounds) have been reliably/rapidly detected, for example, 1.5 nanograms of thiram per square centimeter at apple peel under the current unoptimized condition. The surface-lifting spectroscopic technique offers great practical potentials for the on-site assessment and identification of pesticide residues in agricultural products. PMID:22122589

  18. Pesticides in persimmons, jujubes and soil from China: Residue levels, risk assessment and relationship between fruits and soils.

    Liu, Yihua; Li, Shiliang; Ni, Zhanglin; Qu, Minghua; Zhong, Donglian; Ye, Caifen; Tang, Fubin

    2016-01-15

    Extreme and uncontrolled usage of pesticides produces a number of problems for vegetation and human health. In this study, the existence of organophosphates (OPs), organochlorines (OCs), pyrethroids (PYs) and fungicides (FUs) were investigated in persimmons/jujubes and their planted soils, which were collected from China. One OP (dimethoate), three OCs (DDT, quintozene and aldrin), six PYs (bifenthrin, fenpropathrin, cyhalothrin, cypermethrin, fenvalerate and deltamethrin) and two FUs (triadimefon and buprofezin) were found in 36.4% of persimmons and 70.8% of jujubes, with concentrations from 1.0 μg/kg to 2945.0 μg/kg. The most frequently detected pesticides in the two fruits were fenpropathrin in persimmons and cypermethrin in jujubes, with the detection frequencies of 30.0% and 22.7%, respectively. The residues of 4.5% (persimmon) and 25.0% (jujube) of samples were higher than the maximum residue limits (MRLs) of China. Compared with the fruits, more types of pesticides and higher residues were observed in their planted soils. The most frequently detected pesticides were HCH in persimmon soil and DDT in jujube soil, with the detection frequencies of 10.9% and 12.7%, respectively. For the tested samples, 39.1% of fruit samples and 63.0% of soil samples with multiple residues (containing more than two pesticides) were noted, even up to 8 residues in fruits and 14 residues in soils. Except for cyhalothrin, the other short-term risks for the tested pesticides in the fruits were below 10%, and the highest long-term risk was 14.13% for aldrin and dieldrin. There was no significant health risk for consumers via consumption of the two fruits. PMID:26544891

  19. Simultaneous determination of 200 pesticide residues in honey using gas chromatography-tandem mass spectrometry in conjunction with streamlined quantification approach.

    Shendy, Amr H; Al-Ghobashy, Medhat A; Mohammed, Moustapha N; Gad Alla, Sohair A; Lotfy, Hayam M

    2016-01-01

    A sensitive, accurate and reliable multi-class GC-MS/MS assay protocol for quantification and confirmation of 200 common agricultural pesticides in honey was developed and validated according to EU guidelines. A modified extraction procedure, based on QuEChERS method (quick, easy, cheap, effective, rugged and safe) was employed. Mass spectrophotometric conditions were individually optimized for each analyte to achieve maximum sensitivity and selectivity in MRM mode. The use of at least two reactions for each compound allowed simultaneous identification and quantification in a single run. The pesticides under investigation were separated in less than 31min using the ultra-inert capillary column (DB-35MS). For all analytes, neat standard calibration curves in conjunction with correction for matrix effect were successfully employed. The detection limits of the assay ranged from 1.00 to 3.00ngmL(-1) for the studied pesticides. The developed assay was linear over concentration range of 10.00-500.00ngmL(-1), with correlation coefficient of more than 0.996. At the LOQ, 81% of the studied pesticides were efficiently recovered in the range of 70.00-120.00%, with CV% less than 15.00% while 99.3% compounds had mean percentage recovery of 60.00-140.00%, with CV% less than 21.00% (N=18, over three different days). The proposed assay was successfully applied for the analysis of the studied pesticide residues in one PT sample and 64 commercial honey samples collected over 1year from different districts around Egypt. Results revealed that only one honey sample out of the 64 analyzed samples was contaminated with tau-Fluvalinate (10.00?gkg(-1)). This wide scope assay protocol is applicable for monitoring pesticide residues in honey by national regulatory authorities and accredited labs; that should help ensure safety of such widely used product. PMID:26687165

  20. Results from the monitoring of pesticide residues in fruit and vegetables on the Danish market 1998-99

    Andersen, Jens Hinge; Poulsen, Mette Erecius

    2001-01-01

    The objective of the Danish pesticide monitoring programme for fruit and vegetables was to check for compliance with the maximum residue levels in foods and to monitor the residue levels to assess the pesticide exposure of the Danish population. Sampling plans were designed based on previous...... consumption and no detected residues. Within each commodity, the sampling was random. Samples (n = 4150) of mainly fresh, conventionally grown fruit and vegetables were taken throughout the chain of suppliers including foodprocessing companies. Of the samples, 3% were frozen products and 2% were organically....... Residues were found in 54% of the samples of fruit but only in 13% of the vegetables. Residues above the MRL were found in 4% of all samples of fruit and in 1% of vegetables....

  1. Evaluation of ozonation technique for pesticide residue removal and its effect on ascorbic acid, cyanidin-3-glucoside, and polyphenols in apple (Malus domesticus) fruits.

    Swami, Saurabh; Muzammil, Raunaq; Saha, Supradip; Shabeer, Ahammed; Oulkar, Dasharath; Banerjee, Kaushik; Singh, Shashi Bala

    2016-05-01

    Ozonated water dip technique was evaluated for the detoxification of six pesticides, i.e., chlorpyrifos, cypermethrin, azoxystrobin, hexaconazole, methyl parathion, and chlorothalonil from apple fruits. Results revealed that ozonation was better than washing alone. Ozonation for 15 min decreased residues of the test pesticides in the range of from 26.91 to 73.58%, while ozonation for 30 min could remove the pesticide residues by 39.39-95.14 % compared to 19.05-72.80 % by washing. Cypermethrin was the least removed pesticide by washing as well as by ozonation. Chlorothalonil, chlorpyrifos, and azoxystrobin were removed up to 71.45-95.14 % in a 30-min ozonation period. In case of methyl parathion removal, no extra advantage could be obtained by ozonation. The HPLC analysis indicated that ozonation also affected adversely the ascorbic acid and cyanidin-3-glucoside content of apples. However, 11 polyphenols studied showed a mixed trend. Gallic acid, 3,4-dihydroxybenzoic acid, catechin, epicatechin, p-coumaric acid, quercetin-3-O-glucoside, quercetin, and kaempferol were found to decrease while syringic acid, rutin, and resveratrol were found to increase in 30-min ozonation. PMID:27098519

  2. Results from the monitoring of pesticide residues in fruit and vegetables on the Danish market 1998-99

    Andersen, Jens Hinge; Poulsen, Mette Erecius

    2001-01-01

    The objective of the Danish pesticide monitoring programme for fruit and vegetables was to check for compliance with the maximum residue levels in foods and to monitor the residue levels to assess the pesticide exposure of the Danish population. Sampling plans were designed based on previous...... findings and on food consumption data. Approximately 60% of the samples were selected on the basis of positive findings in samples from the previous 5 years. The remaining samples reflected the pattern of food consumption in Denmark. In addition, a rolling programme is maintained for commodities with a low...

  3. Influence of alternating soil drying and wetting on the desorption and distribution of aged 14C-labeled pesticide residues in soil organic fractions

    Jablonowski, N. D.; Mucha, M.; Thiele, B.; Hofmann, D.; Burauel, P.

    2012-04-01

    A laboratory experiment was conducted to evaluate the effect of alternating soil drying and wetting on the release of aged 14C-labeled pesticide residues and their distribution in soil organic fractions (humic acids, fulvic acids, and humin substances). The used soils (gleyic cambisol; Corg 1.2%, pH 7.2) were obtained from the upper soil layer of two individual outdoor lysimeter studies containing either environmentally long-term aged 14C residues of the herbicide ethidimuron (ETD; 0-10 cm depth; time of aging: 9 years) or methabenzthiazuron (MBT; 0-30 cm depth; time of aging: 17 years). Triplicate soil samples (10 g dry soil equivalents) were (A=dry/wet) previously dried (45° C) or (B=wet/wet) directly mixed with pure water (1+2, w:w), shaken (150 rpm, 1 h), and centrifuged (~2000 g). The resulting supernatant was removed, filtered (0.45 μm) and subjected to 14C activity analysis via liquid scintillation counter (LSC), dissolved organic carbon (DOC) analysis, and LC-MS-MS analysis. This extraction procedure was repeated 15 individual times, for both setups (A) and (B). To determine the distribution of the aged 14C labelled pesticide residues in the soil organic matter fractions, the soil samples were subject to humic and fulvic acids fractionations at cycles 0, 4, 10, and 15. The residual pesticide 14C activity associated with the humic, fulvic, and humin substances (organic fraction remaining in the soil) fractions was determined via LSC. The water-extracted residual 14C activity was significantly higher in the extracts of the dry/wet, compared to the wet/wet soil samples for both pesticides. The total extracted 14C activity in the dry/wet soil extracts accounted for 51.0% (ETD) and 15.4% (MBT) in contrast to 19.0% (ETD) and 4.7% (MBT) in the wet/wet extracts after 15 water extractions. LC-MS-MS analysis revealed the parent compound ETD 27.9 μg kg-1 soil (dry/wet) and 10.7 μg kg-1 soil (wet/wet), accounting for 3.45 and 1.35% of total parent compound initially applied after a total of 10 water extractions, respectively. MBT was detected but not quantified, whereas its metabolite MABT (2-methylamino-benzothiazole) was detected (0.8 vs 0.3 μg kg-1, in dry/wet vs wet/wet soil water extracts, respectively) after 10 water extractions. These results demonstrate the long-term persistence of ETD and MBT and metabolites and their remobilization potential facilitated by soil drying and rewetting. For all samples, the DOC content was significantly higher for the water extracts obtained after dry/wet cycles compared to values obtained from the constantly moistened soil samples. The DOC and water extracted residual 14C activity correlated positively. This result indicates that pesticide residues are associated with DOC which might function as a shuttle for the distribution of pesticide residues. This molecular association can be released into solution where it might be degraded co-metabolically. Overall, the results suggest that intermittent soil drying and rewetting alters the disaggregation of soil aggregates, resulting in a release of entrapped organic carbon and pesticide molecules. Furthermore, analysis of the organic fractions obtained from the 14C pesticide residues containing soil revealed that 14C residues were mainly associated with the humin fraction. The analysis of the organic fractions revealed that extractable residual 14C activity of ETD was more associated with the fulvic acid fraction compared to the residual pesticide 14C activity of MBT, being more associated with the humic acid fraction. For 14C MBT residues, the distribution of the 14C residues in the organic fractions remained rather equal throughout the water extraction cycles. This observation can be supported by the non-mobile character of MBT in soil and its higher KOC value of 247-587 compared to the rather mobile pesticide ETD with a KOC value of 37.1-149. However, for both pesticides a decrease of residual 14C activity in the humic and fulvic acid fractions throughout the water extractions cycles was observed. This observation was more pronounced in the samples of the dry/wet setup.

  4. 77 FR 59578 - Notice of Filing of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2012-09-28

    ...), with a minimum number average molecular weight (in amu) of 500,000, under 40 CFR 180.920 when used as...) number and the pesticide petition number (PP) for the petition of interest as shown in the body of this... contact person, with telephone number and email address, is listed at the end of each pesticide...

  5. Determination of Pesticide Residues in Soil by Modified Matrix Solid-Phase Dispersion and Gas Chromatography

    Modified matrix solid-phase dispersion (MMSPD) and gas chromatography have been developed for quantitative analysis of various classes of pesticides (pirimicarb, metalaxyl, metolachlor, isopropalin and pendimethalin) in soil. MMSPD used Florisil as dispersant and acetone as solvent. Determination was carried out by gas chromatography with nitrogen-phosphorus detection (GC-NPD). The effect of the residence time of pesticides in soil on the recoveries was studied. MMSPD was compared with continuous liquid-solid extraction (LSE). MMSPD had good extraction efficiency and cleanup efficiency and the extract obtained could be directly subjected to GC analysis without further purification. The method gave recoveries ranging from 93% to 100% with relative standard deviations (RSDs) lower than 10%. The limits of detection (LODs) ranged from 0.2 to 2.0 ng g-1

  6. Proposal for field-based definition of soil bound pesticide residues.

    Boesten, J J T I

    2016-02-15

    The environmental significance of soil bound pesticide residues (SBPR) is potentially large because approximately one third of the applied mass of the pesticides in agriculture ends up as SBPR. At EU level, there is little regulatory guidance available on the environmental risk assessment of SBPR in spite of some 50years of SBPR research. This lack of guidance is partially caused by the fact that the current definitions of SBPR are founded on non-extractability in soil in the laboratory whereas for the environmental risk assessment not the soil in the laboratory but the soil in the field is the system of interest. Therefore a definition of SBPR is proposed that is based on the field soil: a molecule (further called 'the mother molecule') is soil bound if a relevant part of this molecule has become part of the solid phase in the soil and if this relevant part will never be released again to the liquid phase in soil under relevant field conditions in the form of this mother molecule or in the form of another molecule that may possibly raise environmental or human toxicological concerns. This mother molecule may be the parent substance that is applied to the soil but it may also be a metabolite of this parent substance. A consequence of the definition is that the SBPR terminology becomes more precise because the mother molecule of the soil bound residue has to be specified. A further consequence is that very strong but reversible sorption of molecules such as paraquat is not considered soil-bound residue anymore (as may be demonstrated by a self-exchange extraction procedure). Furthermore, the definition requires that risk managers have to define what they consider as 'relevant field conditions' (e.g. include also changes of agricultural fields into forests?). PMID:26657254

  7. Occurrence and possible fate of organochlorine pesticide residues at Manzala Lake in Egypt as a model study.

    Kamel, Essam; Moussa, Saad; Abonorag, Mostafa A; Konuk, Muhsin

    2015-01-01

    Persistence of the residue of organochlorine pesticides (OCPs) became a great danger to our environment long ago. In this study, the persistence of OCPs at Manzala Lake in Egypt was determined. Four different sites were investigated: the El-Gamel, El-Kowar, El-Rasoah, and Janb El-Timsah regions. Among these, the El-Kowar region had the highest concentration of total OCPs in the sediment samples when compared to other regions during both 2012 and 2013. In fact, generally, the residues of OCPs in the sediment samples were significantly higher in all tested sites in comparison with other compartments. Conversely, OCP residues were undetectable in water samples at both the El-Gamel region and the El-Rasoah site in the studied seasons. The data proved that the sediment layer plays a sourcing role in OCP persistence in the aquatic ecosystem. Data analysis also indicated that there was an external source for OCP contamination in the Manzala Lake ecosystem that most likely comes from Nile Basin countries and which extends the expected half-life of these compounds. It could be exemplified by DDT, the half-life of which increased from 30 to approximately 47 years. PMID:25424498

  8. Multi-residue analysis of 30 currently used pesticides in fine airborne particulate matter (PM 2.5) by microwave-assisted extraction and liquid chromatography-tandem mass spectrometry.

    Coscollà, Clara; Yusà, Vicent; Beser, Ma Isabel; Pastor, Agustin

    2009-12-18

    A confirmatory and rapid procedure has been developed for the determination of 30 currently used pesticides (CUP) in fine airborne particulate matter (PM 2.5) at trace level. The proposed method includes extraction of PM 2.5-bound pesticides by microwave-assisted extraction (MAE) followed by a direct injection into LC-MS/MS. The main parameters affecting the MAE extraction (time, temperature and volume of solvent) were optimised using statistical design of experiments (DoE). The matrix effect was also evaluated. Recoveries ranged from 72 to 109% and the limit of quantification (LoQ) was 32.5 pg m(-3) for chlorpyrifos, 13.5 pg m(-3) for fenhexamid, imazalil and prochloraz, and 6.5 pg m(-3) for the rest of pesticides, when air volumes of 760 m(3) were collected. The method was applied to 54 samples collected from three stations of the atmospheric monitoring network of the Regional Valencia Government (Spain) during April-July 2009. Nineteen out of 30 pesticides investigated were found in at least one sample: omethoate, carbendazim, acetamiprid, thiabendazole, malathion, flusilazole, metalaxyl, azoxystrobin, iprovalicarb, myclobutanil, tebuconazole, triflumizole, cyprodinil, tebufenpyrad, buprofezin, pyriproxyfen, hexythiazox, flufenoxuron and fenazaquin. The measured concentrations ranged from 6.5 to 1208 pg m(-3). To our knowledge, 11 of the pesticides detected have been reported for the first time in ambient air. PMID:19913234

  9. Screening and quantification of pesticide residues in fruits and vegetables making use of gas chromatography-quadrupole time-of-flight mass spectrometry with atmospheric pressure chemical ionization.

    Cervera, M I; Portolés, T; López, F J; Beltrán, J; Hernández, F

    2014-11-01

    An atmospheric pressure chemical ionization source has been used to enhance the potential of gas chromatography coupled with quadrupole time-of-flight (QTOF) mass spectrometry (MS) for screening and quantification purposes in pesticide residue analysis. A screening method developed in our laboratory for around 130 pesticides has been applied to fruit and vegetable samples, including strawberries, oranges, apples, carrots, lettuces, courgettes, red peppers, and tomatoes. Samples were analyzed together with quality control samples (at 0.05 mg/kg) for each matrix and for matrix-matched calibration standards. The screening strategy consisted in first rapid searching and detection, and then a refined identification step using the QTOF capabilities (MS(E) and accurate mass). Identification was based on the presence of one characteristic m/z ion (Q) obtained with the low collision energy function and at least one fragment ion (q) obtained with the high collision energy function, both with mass errors of less than 5 ppm, and an ion intensity ratio (q/Q) within the tolerances permitted. Following this strategy, 15 of 130 pesticides were identified in the samples. Afterwards, the quantitation capabilities were tested by performing a quantitative validation for those pesticides detected in the samples. To this aim, five matrices were selected (orange, apple, tomato, lettuce, and carrot) and spiked at two concentrations (0.01 and 0.1 mg/kg), and quantification was done using matrix-matched calibration standards (relative responses versus triphenyl phosphate used as an internal standard). Acceptable average recoveries and relative standard deviations were obtained for many but not all pesticide-matrix combinations. These figures allowed us to perform a retrospective quantification of positives found in the screening without the need for additional analysis. Taking advantage of the accurate-mass full-spectrum data provided by QTOF MS, we searched for a higher number of compounds (up to 416 pesticides) in a second stage by performing extra data processing without any new sample injection. Several more pesticides were detected, confirmed, and/or tentatively identified when the reference standard was unavailable, illustrating in this way the potential of gas chromatography-QTOF MS to detect pesticides in addition to the ones targeted in quantitative analysis of pesticides in food matrices. PMID:24828980

  10. Occurrence and spatial distribution of pesticide residues in butter and ghee (clarified butter fat) in Punjab (India).

    Bedi, J S; Gill, J P S; Aulakh, R S; Kaur, Prabhjit

    2016-02-01

    The present study was undertaken to monitor organochlorine, organophosphate, and synthetic pyrethroid pesticide residues in butter (n?=?55) and ghee (n?=?56) samples collected from three different regions of Punjab. The estimation of pesticide residues was done by multiple residue analytical technique using gas chromatography equipped with GC-ECD and GC-FTD. The confirmation of residues was done on gas chromatography mass spectrometry in both selective ion monitoring (SIM) and scan mode. Results indicated the presence of hexacholorocyclohexane (HCH) and p,p' DDE as predominant contaminant in both butter and ghee. Residues of HCH were detected in 25 and 23% samples of butter and ghee, respectively, while residues of p,p' DDE were recorded in 29 and 25% of butter and ghee samples, respectively. None of the butter and ghee sample violated the MRL values of 200ngg(-1) for HCH and 1250ngg(-1) for dichorodiphenyl tricholorethane (DDT). The presence of endosulfan, cypermethrin, fenvalerate, deltamethrin, and chlorpyrifos were observed in a few butter and ghee samples at traces. The spatial variation for comparative occurrence of pesticide residues indicated higher levels in the south-western region of Punjab. Additionally, the temporal variation indicated the significant reduction of HCH and DDT levels in butter and ghee in Punjab. PMID:26781716

  11. Validation of pestice multi residue analysis method on cucumber

    In this study we aimed to validate the method of multi pesticide residue analysis on cucumber. Before real sample injection, system suitability test was performed in gas chromatography (GC). For this purpose, a sensitive pesticide mixture was used for GC-NPD and estimated the performance parameters such as number of effective theoretical plates, resolution factor, asymmetry, tailing and selectivity. It was detected that the system was suitable for calibration and sample injection. Samples were fortified at the level of 0.02, 0.2, 0.8 and 1 mg/kg with mixture of dichlorvos, malathion and chloropyrifos pesticides. In the fortification step 14C-carbaryl was also added on homogenized analytical portions to make use of 14C labelled pesticides for the determining extraction efficiency. Then the basic analytical process, such as ethyl acetate extraction, filtration, evaporation and cleanup, were performed. The GPC calibration using 14C- carbaryl and fortification mixture (dichlorvos, malathion and chloropyrifos) showed that pesticide fraction come through the column between the 8-23 ml fractions. The recovery of 14C-carbaryl after the extraction and cleanup step were 92.63-111.73 % and 74.83-102.22 %, respectively. The stability of pesticides during analysis is an important factor. In this study, stability test was performed including matrix effect. Our calculation and t test results showed that above mentioned pesticides were not stabile during sample processing in our laboratory conditions and it was found that sample comminution with dry ice may improve stability. In the other part of the study, 14C-chloropyrifos was used to determine homogeneity of analytical portions taken from laboratory samples. Use of 14C labelled pesticides allows us for quick quantification analyte, even with out clean-up. The analytical results show that after sample processing with waring blender, analytical portions were homogenous. Sample processing uncertainty depending on quantity of analytical portions was calculated from sampling constant equation (Ks=WxCVsp2). CVsp for 50 g was 4.539% and 8.033% for 5 g analytical portions.

  12. Simultaneous determination of 50 residual pesticides in Flos Chrysanthemi using accelerated solvent extraction and gas chromatography.

    Huang, Xiaohui; Zhao, Xinghui; Lu, Xiaotong; Tian, Huaiping; Xu, Ajing; Liu, Yan; Jian, Zhang

    2014-09-15

    A gas chromatographic method for simultaneous determination of 50 organochlorine (OCP) and pyrethroid (PP) pesticides in Flos Chrysanthemi was established. Accelerated solvent extraction (ASE) technique was used to extract the target compounds, cleaned with alumina neutral-florisil column, and eluted by mixed solvents of ethyl acetate and hexane (15:85, v/v). Selected pesticides were identified using HP-5 and DB1701 capillary dual column and detected by electron-capture detector. Quantitative analysis was performed using an external standard by HP-5 capillary column. Results showed that recoveries were 73.4-120.1%, and the relative standard deviations (RSDs) were 1.6-12.4%. The limits of detection of the method were 0.0021-0.0069 mg/kg, and the limits of quantity were 0.0064-0.0210 mg/kg. PMID:25062509

  13. Predicting pesticide fate in the hive (part 1): experimentally determined ?-fluvalinate residues in bees, honey and wax

    Bonzini, Sara; TREMOLADA Paolo; Bernardinelli, Iris; Colombo, Mario; Vighi, Marco

    2011-01-01

    ?-Fluvalinate residues in bees, honey and wax were measured in two experimental hives treated with Apistan to test a multi-compartmental predictive model. Pesticide residues were monitored for 30days after treatment in bees and for up to 180days in honey and wax. Concentrations ranged between 14 and 160ngg?1 f.w. in bees and between 98 and 1630ngg?1 in wax, while no residues were detected above the analytical limit (2.5ngg?1) in honey. ?-Fluvalinate residues are discussed in the conte...

  14. A rapid, solid phase extraction (SPE technique for the extraction and gas chromatographic determination lindane pesticide residue in tissue and milk

    Yuningsih

    2006-03-01

    Full Text Available Organochlorine pesticide contamination in feed can cause residue in animal product (tissue and milk, so its become a problem in food safety. Solid phase extraction (SPE has been carried out for determination organochlorine pesticide residues in food animal production. The technique was rapid, not costly and produce limited amount of hazardous-waste. Samples were homogenized with acetonitrile trough cartridge C18, eluted in fluorocyl column with 2% ether-petroleum or acetonitrile fortissue and milk samples respectively. The recoveries of tissue sample by addition lindane standard solution: 0.50 and 1.00 μg are 85.10 and 103.10% respectively, while that of milk with the addition of 0.50, 1.00 and 1.50 μg are 83.80, 88.69 and 91.24% respectively. Three replicates were carried out for every sample. According of validation criteria of FAO/IAEA the recovery for analysis of pesticide residues was 70-110%. Therefore, the method is applicable.

  15. A multi-residue method for the determination of 90 pesticides in matrices with a high water content by LC-MS/MS without clean-up.

    Madureira, Fernando Diniz; da Silva Oliveira, Fabiano Aurélio; de Souza, Wesley Robert; Pontelo, Ana Paula; de Oliveira, Mauro Lúcio Gonçalves; Silva, Gilsara

    2012-01-01

    A method using QuEChERS extraction and LC-MS/MS in electrospray positive ionisation mode was developed and validated for the analysis of 90 pesticides in a high water content matrix (tomato) in a single chromatographic run. To assess the intra-laboratory reproducibility of the method, validation was conducted on four different days by two different analysts. The validation data was treated using a spreadsheet developed in-house, which sets the most appropriate model for linear fit by determining whether the residuals of the calibration curves are homocedastic or heterocedastic. A statistical test for the significance of regression was also carried out. Calibration was always matrix-matched and the curves were obtained over the range 0.0075-0.10 or 0.020-0.125 mg kg(-1). Identification of analytes was based on retention times and MRM ratios. Recoveries were assessed at four different levels for each analyte and were between 73 and 106%, with relative standard deviations under reproducibility conditions of pesticide analysed were below 50%. Previous validation of the same method, applied to papaya samples and satisfactory results obtained in various proficiency tests with different high water content matrices, demonstrated the applicability of the method to these classes of commodities, without clean-up. The validated method will be applied routinely in the pesticide residues monitoring programme that constitutes the National Residue and Contaminant Control Plan of Brazil. PMID:22059454

  16. Rapid detection of pesticides not amenable to multi-residue methods by flow injection-tandem mass spectrometry.

    Mol, Hans G J; van Dam, Ruud C J

    2014-11-01

    Flow injection combined with tandem mass spectrometry (MS/MS) was investigated for the rapid detection of highly polar pesticides that are not amenable to multi-residue methods because they do not partition into organic solvents and require dedicated chromatographic conditions. The pesticides included in this study were amitrole, chlormequat, cyromazine, daminozide, diquat, ethephon, fosetyl-Al, glufosinate, glyphosate and its metabolite aminomethylphosphonic acid, maleic hydrazide, mepiquat and paraquat. The composition of the flow-injection solvent was optimized to achieve maximum MS/MS sensitivity. Instrumental limits of detection varied between <0.05 and 1 pg. Fruit, vegetable, cereal, milk and kidney samples were extracted with water (1% formic acid in case of paraquat/diquat) and ten times diluted in either methanol/0.1% formic acid, methanol/0.1% ammonia or acetonitrile/0.1% ammonia, depending on the pesticide. The ion suppression observed depended strongly on both the matrix and the pesticide. This could be largely compensated for by matrix-matched calibration, but more accurate quantification was obtained by using isotopically labelled standards (commercially available for most of the pesticides studied). The method detection limits ranged from 0.02 mg/kg for chlormequat and mepiquat to 2 mg/kg for maleic hydrazide and were 0.05-0.2 mg/kg for most other pesticide/matrix combinations. This was sufficiently low to test compliance with EU maximum residue limits for many relevant pesticide/commodity combinations. The method substantially reduces the liquid chromatography-MS/MS capacity demand which for many laboratories is prohibitive for inclusion of these pesticides in their monitoring and surveillance programmes. PMID:24518902

  17. Comparison pesticide residue levels in the surface of Bertam River in Cameron Highlands, Pahang

    Haron, S. H.; Ismail B., S.

    2015-09-01

    The presence of pesticide residues in the surface water of Bertam River in the agricultural areas of Cameron Highlands in Pahang, Malaysia was monitored from May to October 2014. The sampling sites were located at 10 sampling points along the Bertam River in the vegetable planting areas. The extraction method of the pesticide (organophosphate/pyrethroid) from the river samples used solid phase extraction followed by gas chromatography (with electron capture detector, ECD). Insecticides, cypermethrin and chlorpyrifos were found in the surface water of Bertam River. High level concentrations of those insecticides in the river were observed during the period from May to October 2014, a period which included both seasons (wet and dry seasons). The highest concentration of 2.66 µg/mL and 1.23 µg/mL of cypermethrin was observed during the wet and dry seasons respectively. This could be due to the frequent usage of the above-mentioned insecticides coupled with contamination that could have originated from the application sites. Meanwhile, the lowest concentration detected in the surface water was chlorpyrifos (0.11 µg/mL and 0.17 µg/mL) during the dry and wet seasons, respectively.

  18. Comparison pesticide residue levels in the surface of Bertam River in Cameron Highlands, Pahang

    The presence of pesticide residues in the surface water of Bertam River in the agricultural areas of Cameron Highlands in Pahang, Malaysia was monitored from May to October 2014. The sampling sites were located at 10 sampling points along the Bertam River in the vegetable planting areas. The extraction method of the pesticide (organophosphate/pyrethroid) from the river samples used solid phase extraction followed by gas chromatography (with electron capture detector, ECD). Insecticides, cypermethrin and chlorpyrifos were found in the surface water of Bertam River. High level concentrations of those insecticides in the river were observed during the period from May to October 2014, a period which included both seasons (wet and dry seasons). The highest concentration of 2.66 µg/mL and 1.23 µg/mL of cypermethrin was observed during the wet and dry seasons respectively. This could be due to the frequent usage of the above-mentioned insecticides coupled with contamination that could have originated from the application sites. Meanwhile, the lowest concentration detected in the surface water was chlorpyrifos (0.11 µg/mL and 0.17 µg/mL) during the dry and wet seasons, respectively

  19. Monitoring of pesticide residues in apples, lettuce and potato of the Slovene origin in the years 2001 to 2004

    Helena BAŠA ČESNIK; Ana GREGORČIČ; Velikonja Bolta, Špela; Kmecl, Veronika

    2006-01-01

    Abstract 404 samples of apples, lettuce and potato produced in the Republic of Slovenia were analysed for pesticide residues at the Agricultural Institute of Slovenia in the years 2001 to 2004. Surveillance sampling in eight agricultural production areas was performed at market producers at the harvesting of products or in storehouses, after the pre-harvest interval of plant protection products used. Samples exceeding the maximum residue levels were the following: 3 apple samples (...

  20. Requiring Pollutant Discharge Permits for Pesticide Applications that Deposit Residues in Surface Waters

    Terence Centner; Nicholas Eberhart

    2014-01-01

    Agricultural producers and public health authorities apply pesticides to control pests that damage crops and carry diseases. Due to the toxic nature of most pesticides, they are regulated by governments. Regulatory provisions require pesticides to be registered and restrictions operate to safeguard human health and the environment. Yet pesticides used near surface waters pose dangers to non-target species and drinking water supplies leading some governments to regulate discharges of pesticid...

  1. 78 FR 70007 - Receipt of a Pesticide Petition Filed for Residues of a Pesticide Chemical in or on Various...

    2013-11-22

    ... data may be needed before EPA can make a final determination on this pesticide petition. Pursuant to 40...-incorporated protectant (PIP), Bacillus thuringiensis Cry1F protein, in or on soybean. The petitioner...

  2. Investigation of organochlorine pesticide residues in samples of 40 nursing mothers residing in Tehran

    Afshar M

    1997-09-01

    Full Text Available Organochlorine pesticides are a group of persistant compounds which have been used for a long time. Due to their stability, some of them such as DDT, BHC and their derivatives are still used in the areas with malaria epidemic condition, hence the chance of food contamination always exists. The present survey demonstrated that human milk is one of the best indicator substances in monitoring the environment and human body contamination by organochlorine compounds. We studied the level of residues in the milk of nursing mothers who could be exposed to these compounds through food chain in their contaminated environment. In this investigation, we collected 40 samples from the nursing mothers of two hospitals located in the north and south of Tehran. Detection was carried out by Gas chromatography (GC with 3% OV17 column and Ni63 ECD (Electron Capture Detector. Reference substances were obtained from WHO. Results are discussed in the text.

  3. The determination of pesticide residues in local vegetables by means of neutron activation technique

    Analytical methods based on neutron activation have been developed for studying pesticides residues of bromine, arsenic and mercury in local vegetables and fruits. The concentration of bromine, arsenic and mercury in samples are enriched prior to neutron irradiations by a technique of dry-ashing and freeze-drying for the determination of arsenic, bromine and mercury respectively. The element bromine is determined instrumentally while arsenic and mercury are determined destructively using a distillation technique. The limit of detection under the conditions used for bromine, arsenic and mercury as obtained are 0.01, 0.001 and 0.0001 microgram respectively. A total of 45 varieties of vegetables and 20 varieties of fruits are analyzed. The results of the investigation and the concentration range in part per million of bromine, arsenic and mercury are also presented

  4. Study of the effect of gamma irradiation on phenolic compounds and pesticides residues

    The aim of this study was to show the effects of this process of conservation on the polyphenol rate and the antioxidant capacity of polyphenols of quince, of the cocoa and those of sage, then to study its effects on the pesticides residues in the sage sheets. The irradiation of quince polyphenols, increased the polyphenols rate as well as the antioxidant capacity. In the case of cocoa polyphenols, we don't have ace observed many differences between the irradiated and not irradiated samples, and in the case of sage polyphenols, the polyphenol rate as well as the antioxidant capacity decreased. Finally, irradiation of parathion caused degradation of this molecule, and the polyphenol rate as well as the antioxidant capacity pf polyphenols of the sheets of sage soaked with parathion was a less decreased than polyphenols of the sheets not soaked with parathion. (Author). 37 refs

  5. Determination of 23 pesticide residues in leafy vegetables using gas chromatography-ion trap mass spectrometry and analyte protectants.

    González-Rodríguez, Rosa Ma; Rial-Otero, Raquel; Cancho-Grande, Beatriz; Simal-Gándara, Jesús

    2008-07-01

    A gas chromatographic method was developed for simultaneously determining residues of 12 insecticides (acrinathrin, bifenthrin, carbofuran, cyfluthrin, lambda-cyhalothrin, cypermethrin, chlorfenvinphos, deltamethrin, esfenvalerate, fenamiphos, methiocarb and tau-fluvalinate) and 11 fungicides (cyprodinil, fludioxonil, iprodione, metalaxyl, penconazole, pyrimethanil, procymidone tebuconazole, triadimefon, triadimenol and vinclozolin) in leafy vegetables. Samples were extracted with acetonitrile and cleaned-up with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. The eluate was finally evaporated and redissolved with 0.5 mL of acetone containing the internal standards (pentachlorobenzene and fenpropathrin) and three analyte protectants (3-ethoxy-1,2-propanediol, d-sorbitol and l-gulonic acid gamma-lactone). The addition of analyte protectants allows to avoid the matrix-induced response enhancement effect on quantitation process with absolute recoveries ca. 100%. Precision (expressed as relative standard deviation) was lower than 10% for all pesticides and finally, limits of detection were also 10-20 times lower than maxima residue levels (MRLs) established by European Regulation. The proposed method was applied to determine pesticide residues in commercial leafy vegetables (lettuce, Swiss chard and spinach) purchased from markets in Orense (NW Spain). Pesticide residues were detected in 84% of the total samples (63 from 75 samples) and pesticide concentrations were higher than MRL in 18 samples. PMID:18343389

  6. Residues in food and feed topic area at the 13th IUPAC International Congress of pesticide chemistry

    The organizers of two symposia in the “Residues in Food and Feed” topic area held at the 13th IUPAC International Congress of Pesticide Chemistry introduce the papers that were contributed to this special section in the Journal. The symposia were titled “Taking Advantage of Advanced Analytical Tool...

  7. Multiresidue analysis of pesticides in olive oil by gel permeation chromatography followed by gas chromatography-tandem mass-spectrometric determination

    A method for the multiresidue analysis of olive oil samples for 26 pesticides is proposed. Residual pesticides are extracted from oil using an n-hexane/acetonitrile mixture, extracts being cleaned-up by gel permeation chromatography (GPC) for analysis by gas chromatography-tandem mass spectrometry (GC-MS/MS). Electron ionization and chemical ionization are employed in a single analysis for the determination of pesticides. Pesticide recoveries from virgin and refined olive oil spiked with 10, 100 and 250 μg/kg concentrations of the pesticides ranged from 83.8 to 110.3%. The proposed method features good sensitivity: its limits of quantification are low enough to allow pesticide residues to be determined at concentrations below the maximum residue levels legally accepted. The precision, expressed as relative standard deviation, ranges from 4.93 to 8.11%. Applicability was tested on 40 olive oil samples. Several pesticides were detected in most of the virgin olive oil samples. By contrast, refined olive samples contained few pesticides, and only endosulfan sulphate was detected in all

  8. Development of a fieldable rapid pesticide exposure analysis sensing system

    Spencer, Kevin M.; Clauson, Susan L.; Spencer, Sarah A.; Sylvia, James M.; Vallejos, Quirina M.; Quandt, Sara A.; Arcury, Thomas A.

    2010-04-01

    Despite the recent interest in organically grown foods, most agricultural crops use multiple pesticides to optimize yield. There are many persons whose health may be affected by the spraying; there is the active applicator and the passive neighbors. In between these extremes are the farm workers who pick the crops anywhere from days to weeks after application. How much pesticide residue are these workers exposed to during a workday and how much is transferred back to the residence? Despite the low vapor pressures, what is the true concentration of pesticides surrounding a person when pesticides adsorbed to particulate matter are included? What is the relationship between the concentration around an individual and the amount adsorbed/ingested? To answer these questions on a statistically significant scale in actual field conditions, a portable, fast, inexpensive measurement device is required. We present herein results obtained using Surface-Enhanced Raman Spectroscopy (SERS) that demonstrate the capability to detect < 100 organophosphate, organochlorine and carbamate-based pesticides in the vapor phase as well as the ability of SERS sensors to detect a particular analyte in a synthetic urine matrix. We will also present data collected from CDC quantified urine samples and will present results obtained in a field test wherein SERS sensors wore worn as dosimeters in the field and real-time vapor sampling of the farm workers barracks was performed. The issue of potential interferences will also be discussed.

  9. European Pesticide Tax Schemes in Comparison: An Analysis of Experiences and Developments

    Thomas Böcker

    2016-04-01

    Full Text Available Policy measures are needed to reduce the risks associated with pesticides’ application in agriculture, resulting in more sustainable agricultural systems. Pesticide taxes can be an important tool in the toolkit of policy-makers and are of increasing importance in European agriculture. However, little is known about the effects of such tax solutions and their impacts on the environment, farmers, and human health. We aim to fill this gap and synthesize experiences made in the European countries that have introduced pesticide taxes, i.e., France, Denmark, Norway, and Sweden. The major findings of our analysis are: (1 overall, the effectiveness of pesticide taxes is limited, but if a tax on a specific pesticide is high enough, the application and the associated risks will be reduced significantly; (2 in all countries, hoarding activities have been observed before a tax introduction or increase. Therefore, short-term effects of taxes are substantially smaller than long-term effects; (3 differentiated taxes are superior to undifferentiated taxes because fewer accompanying measures are required to reach policy goals; (4 tax scheme designs are not always in line with the National Action Plan targets. Low tax levels do not necessarily lead to a reduction of pesticide input and differentiated taxes do not necessarily lead to fewer violations of water residue limits.

  10. Detection of residual organochlorine and organophosphorus pesticides in agricultural soil in Rio Verde region of San Luis Potosi, Mexico.

    Velasco, Antonio; Hernández, Sergio; Ramírez, Martha; Ortíz, Irmene

    2014-01-01

    Organochlorine pesticides were intensively used in Mexico from 1950 until their ban and restriction in 1991. However, the presence of these compounds is commonly reported in many regions of the country. The aim of the present study was to identify and quantify residual organochlorine and organophosphorus pesticides in agricultural soil in Rio Verde region, San Luis Potosi state, which has been identified as possibly polluted by pesticides. Composed samples from 24 zones covering an area of approximately 5,440 ha were analyzed. The most frequently found pesticides were p,p'-DDT followed by ,p,p'-DDE, heptachlor, endosulfan and γ-HCH whose frequency rates were 100, 91, 83 and 54%, respectively. The concentration of p,p'-DDT in the crops grown in these soils was in the following order: chili > maize > tomato > alfalfa. The results obtained in this study show that p,p'-DDT values are lower or similar to those found in other agricultural regions of Mexico. Methyl and ethyl parathion were the most frequent organophosphate pesticide detected in 100% and 62.5% of the samples with average concentrations of 25.20 and 47.48 μg kg(-1), respectively. More research is needed to establish the background levels of pesticides in agricultural soils and their potential ecological and human health effects in this region. PMID:24813984

  11. Evaluation of Quechers Sample Preparation and GC Mass Spectrometry Method for the Determination of 15 Pesticide Residues in Tomatoes Used in Salad Production Plants

    JAHANMARD, Elham; ANSARI, Fatemeh; FEIZI, Mansour

    2016-01-01

    Background: The present study was the first attempt for determination and measurement of pesticide residues in tomatoes used in salad production plants in Isfahan, central Iran. Methods: A multiresidue method based on modified QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation, followed by Gas Chromatography Mass Spectrometry (GC–MS) was developed and validated for the determination of 15 pesticides (permethrin, primicarb, dichlorvos, diazinone, fenpropathrin, carbaryl, chlorpyrifos, malathion, chlortalonil, brompropilate, propargit, tetradifone, phosalone, iprodion and endosulfane) from different classes. The recovery yields ranged from 83.84 to 119.73%and the relative standard deviation (RSD) was below 20.54%. The limits of detection (LODs) were between 1.63to 10.5 mg/kg and the limits of quantifications (LOQs) were between 5.43to35 mg/kg. The method has been successfully applied to the analysis of 22 tomato samples obtained from salad production plants in Isfahan in Sep to Dec 2014. Results: An amount of 31.81% of samples showed contamination above maximum residue levels (MRLs) with pesticides. In addition, 13.6% of samples had contamination with diazinone and 18.18% of samples with chlorpyrifos. Conclusion: A full consideration is essential for tomatoes used in salad and food productions. It suggests a need for revision of the current trend of supervision for tomatoes and other vegetables presented in wholesale markets. In all, the study confirms that pesticide residue determination in food products, especially in raw fruits and vegetables, is a very demanding task in public health safety and trade.

  12. Total diet study on pesticide residues in France: levels in food as consumed and chronic dietary risk to consumers.

    Nougadère, Alexandre; Sirot, Véronique; Kadar, Ali; Fastier, Antony; Truchot, Eric; Vergnet, Claude; Hommet, Frédéric; Baylé, Joëlle; Gros, Philippe; Leblanc, Jean-Charles

    2012-09-15

    Chronic dietary exposure to pesticide residues was assessed for the French population using a total diet study (TDS) to take into account realistic levels in foods as consumed at home (table-ready). Three hundred and twenty-five pesticides and their transformation products, grouped into 283 pesticides according to their residue definition, were sought in 1235 composite samples corresponding to 194 individual food items that cover 90% of the adult and child diet. To make up the composite samples, about 19,000 food products were bought during different seasons from 2007 to 2009 in 36 French cities and prepared according to the food preparation practices recorded in the individual and national consumption survey (INCA2). The results showed that 37% of the samples contained one or more residues. Seventy-three pesticides were detected and 55 quantified at levels ranging from 0.003 to 8.7mg/kg. The most frequently detected pesticides, identified as monitoring priorities in 2006, were the post-harvest insecticides pirimiphos-methyl and chlorpyrifos-methyl-particularly in wheat-based products-together with chlorpyrifos, iprodione, carbendazim and imazalil, mainly in fruit and fruit juices. Dietary intakes were estimated for each subject of INCA2 survey, under two contamination scenarios to handle left-censored data: lower-bound scenario (LB) where undetected results were set to zero, and upper-bound (UB) scenario where undetected results were set to the detection limit. For 90% of the pesticides, exposure levels were below the acceptable daily intake (ADI) under the two scenarios. Under the LB scenario, which tends to underestimate exposure levels, only dimethoate intakes exceeded the ADI for high level consumers of cherry (0.6% of children and 0.4% of adults). This pesticide, authorised in Europe, and its metabolite were detected in both cherries and endives. Under the UB scenario, that overestimates exposure, a chronic risk could not be excluded for nine other pesticides (dithiocarbamates, ethoprophos, carbofuran, diazinon, methamidophos, disulfoton, dieldrin, endrin and heptachlor). For these pesticides, more sensitive analyses of the main food contributors are needed in order to refine exposure assessment. PMID:22595191

  13. Analytical method for simultaneous determination of pesticide and veterinary drug residues in milk by CE-MS.

    Blasco, Cristina; Picó, Yolanda; Andreu, Vicente

    2009-05-01

    This study reports a method based on CE-MS/MS detection developed for the multiresidue determination of seven pesticides (amidosulfuron, cyprodinil, cyromazine, imazaquin, pirimicarb, demethyl pirimicarb, procymidone) and eight residues of veterinary drugs (ciprofloxacin, enrofloxacin, sulfacetamide, sulfabenzamide, sulfachlorpyridazine, sulfaquinoxaline, sulfathiazole, sulfisoxazole), whose contents are regulated by the EU Council Regulations no. 396/2005 and no. 2377/90, in animal edible tissues. Milk samples were extracted with ACN and the extract was cleaned up using an Oasis hydrophilic-lipophilic balance SPE cartridge. The proposed method was validated in accordance with the European Commission Decision 657/2002. MS/MS experiments, using an IT analyzer, operating in multiple reaction monitoring mode, were carried out to achieve the minimum number of required identification points. Recovery data were also satisfactory, with values higher than 78% for most pesticides and veterinary drugs extracted from milk spiked at half the maximum residue limit established for the studied compounds. The RSD% (n = 5) were lower than 13 and 15% for intra-day and inter-day assays, respectively. The method was applied to establish the occurrence of the studied pesticides in 100 milk samples, attaining the determination of pesticide and veterinary drug residues in milk in the low microg/kg range. PMID:19384986

  14. Levels of organochlorine pesticide residues in blood plasma of various species of birds from India.

    Dhananjayan, Venugopal; Muralidharan, Subramanian

    2010-08-01

    Concentrations of organochlorine pesticides (OCPs) were measured in blood plasma of 13 species of birds collected from Ahmedabad, India. Among the various OCPs determined, HCHs and its isomers had higher contribution to the total OCPs. Concentration of summation operatorHCHs varied from 11.4 ng/mL in White ibis Threskiornis melanocephalus to 286 ng/mL in Sarus Crane Grus antigone, while summation operatorDDT ranged between 19 ng/mL in Black Ibis Pseudibis papillosa and 147 ng/mL in Painted Stork Mycteria leucocephala. p,p'-DDE was accounted for more than 50% of total DDT in many of the samples analysed. However, a p,p'-DDT to p,p'-DDE ratio higher than one obtained for many species of birds indicates the recent use of DDT in this study region. The concentrations of cyclodiene insecticides, heptachlor epoxide, dieldrin and total endosulfan ranged from 15.8 to 296.2 ng/mL, below detectable level to 15 and 41.1-153.2 ng/mL, respectively. The pattern of total OCP load generally occurred in the following order: granivores < insectivores < omnivores < piscivores < carnivores. Although, the organochlorine residues detected in blood plasma of birds are not indicative of toxicity, the presence of residues in birds over the years (2005-2007) indicates continued exposure to organochlorine compounds. However, continuous monitoring is recommended to facilitate the early identification of risks to the survival of a species. PMID:20571760

  15. Spectrum of Organochlorine Pesticide Residues in Fish Samples from the Densu Basin

    Samuel Afful

    2010-07-01

    Full Text Available In this study, the levels of organochlorine pesticide residues in the Densu basin have been investigated using fish sam ples as a case study. Six fish species namely Heterotis niloticus, Channa obscura, Hepsetus odoe, Tilapia zilli, Clarias gariepinus and Chrysichthys nigrodigitatus were collected from the sampling towns, Weija and Nsawam along the Densu river basin in the Greater Accra Region of Ghana. Composite samples w ere homogenized, freeze dried and ground to obtain powdered samples. The powdered samples were extracted by soxhlet extraction procedure using (3:1 hexane: acetone mixture. The extracts were cleaned-up using florisil adsorbent and characterized for organochlorine content using Gas Chromatography (GC equipped with Electron Capture Detector (ECD. The GC recoveries of spiked samples were between 80 to 96%. Fourteen organochlorines (OCs namely gamma-HCH, delta-HCH, heptachlor, aldrin, gammachlordane, p,p’-DDE, alpha-endosulfan, dieldrin, endrin, endrin-aldehyde, endosulfan-sufate, p,p’-DDT, endrinketone and methoxychlor were identified and quantified. A 100% incidence was recorded for gamma-HCH, delta-HCH, heptachlor, aldrin, gamma-chlordane, alpha-endosulfan, dieldrin and p,p’-DDT, while 75% incidence was recorded for the metabolites, p,p’-DDE and endosulfan-sulfate. The concentrations of OCs ranged from 0.3 to 71.3 :g/kg and were however, below the Australian Maximum Residue Limits (MRL of 50 to 1000 :g/kg for fresh w ater fish.

  16. Pesticide residues in tomatoes from greenhouses in Souss Massa Valley, Morocco.

    Salghi, R; Luis, G; Rubio, C; Hormatallah, A; Bazzi, L; Gutirrez, A J; Hardisson, A

    2012-03-01

    Eight pesticide residues in tomato samples collected in the area of Souss Massa Valley (Southern Morocco) were analyzed. The detected residue levels ranged from 0.001 to 0.400 mg kg(-1) for dicofol, from 0.003 to 0.170 mg kg(-1) for procymidone, from 0.001 to 0.250 mg kg(-1) for chlorothalonil, from 0.050 to 0.500 mg kg(-1) for bifenthrin, from 0.001 to 0.010 mg kg(-1) for ?-cyhalothrin, from 0.001 to 0.300 mg kg(-1) for cypermethrin, from 0.010 to 1 mg kg(-1) for deltamethrin and from 0.003 to 1.123 mg kg(-1) for endosulfan. European MRL for endosulfan in tomatoes set in 0.500 mg kg(-1), was exceeded in 8 samples, and MRL for deltamethrin set in 0.300 mg kg(-1) for tomatoes was exceeded in 2 samples. PMID:22210446

  17. Development of a procedure for the multiresidue analysis of pesticides in vineyard soils and its application to real samples.

    Pose-Juan, Eva; Herrero-Hernndez, Eliseo; lvarez-Martn, Alba; Snchez-Martn, Mara J; Rodrguez-Cruz, M Sonia

    2014-08-01

    A procedure for multiresidue analysis was developed for the extraction and determination of 17 pesticides, including herbicides, fungicides, and insecticides, as well as certain degradation products, in vineyard soils from La Rioja region (Spain). Different solvents and mixtures were tested in spiked pesticide-free soils, and pesticides were comparatively evaluated by gas chromatography with mass spectrometry and liquid chromatography with mass spectrometry. Recoveries >70%, with relative standard deviations vineyard soil samples, and terbuthylazine and its metabolite desethylterbuthylazine were the most ubiquitous compounds, as they were detected in the 100% of the soils analyzed. The presence of fungicides was also high, and the presence of insecticides was lower than other pesticides. The results confirm the usefulness of the optimized procedure for monitoring residues in vineyard soils. PMID:24910322

  18. Study On The Procedures For Determining Of Pesticide Residues In Green Vegetables

    Researches presented in this work are divided into two main parts. One part embraces the residue analytical methods. The other part comprises applying of these residue analytical methods for analysis of plant material. Part I: Residue analytical methods (Analytical procedures): Determination of Endosulphan in plant material by GC/ECD; Determination of Methamidofos in plant material by GC/FTD; Determination of Deltamethrin, Cyhalothrin, Cyfluthrin in plant material by GC/ECD; Determination of Maneb in plant material by HPLC/UV; Determination of Zineb in plant material by F-AAS; Determination of Organo-Asenic and Mercury in plant material by RNAA; The limits of detection and determination (LOD, LOQ), Recovery, Efficiency, the Calibration curve are validated. Part II: Applying of Residue Analytical Methods for analysis of endosulphan, methamidofos, maneb, zineb, cyhalothrin, deltamethrin, cyfluthrin, metallo-organic compounds in Spinach, Cabbage, Pimento, Japanese Bean, Japanese Pumpkin, Tomato, Potato, Sweet Potato. The results and conclusion are present in this work. (author)

  19. Concentrations of organochlorine pesticides (OCPs) residues in foodstuffs collected from traditional markets in Indonesia.

    Shoiful, Ahmad; Fujita, Hiroyuki; Watanabe, Isao; Honda, Katsuhisa

    2013-02-01

    A total 23 of organochlorine pesticides (OCPs) residues were determined in five groups of foodstuffs, i.e.: vegetables (carrot, potato, cucumber, corn, and onion), rice, pulses (green bean and soybean), nuts (peanut), and fish (milkfish), which collected from traditional markets in three big cities of Indonesia; Jakarta, Bogor, and Yogyakarta. OCPs were only detected in fatty foodstuffs, such as soybean, peanut, and milkfish. The concentration of HCB (expressed as ng g(-1) on a whole basis), ?Drins, ?DDTs, ?Heptachlors, and ?HCHs were in the range of <0.3-0.74 ng g(-1), <0.03-0.42 ng g(-1), <0.02-0.41 ng g(-1), <0.03-0.14 ng g(-1), and <0.03-0.06 ng g(-1), respectively, which were far below the maximum residue limits (MRLs) as established by FAO/WHO. These very low concentrations of OCPs residues in foodstuffs indicated that OCPs were used only in past time and no recent input into the environment. Furthermore, the estimated daily intake (EDI) of HCB, ?DDTs, ?Drins, ?Heptachlors, and ?HCHs in five group foodstuffs, which were 60% of total daily diet of Indonesian, were 0.09 ng kg(-1) bw d(-1), 0.04 ng kg(-1) bw d(-1), 0.01 ng kg(-1) bw d(-1), 0.003 ng kg(-1) bw d(-1), and 0.002 ng kg(-1) bw d(-1), respectively. These results were far below the acceptable daily intake (ADI) as established by FAO/WHO, which indicated that consumption of foodstuffs from Indonesia were at little risk to human health in term of OCPs at present. PMID:23177005

  20. 77 FR 20334 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2012-04-04

    ...-methylbenzene, with number average molecular weight greater than 10,000 daltons, (CAS No. 35297-61-1) under 40...) number and the pesticide petition number (PP) of interest as shown in the body of this document, by one... arrangements should be made for deliveries of boxed information. The Docket Facility telephone number is...

  1. 76 FR 69690 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2011-11-09

    ... production (NAICS code 112). Food manufacturing (NAICS code 311). Pesticide manufacturing (NAICS code 32532...-10 at 2.5 ppm; fruit, pome, group 11-10 at 4.0 ppm; persimmon at 1.9 ppm; and tea at 20 ppm....

  2. 77 FR 43562 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2012-07-25

    ... groups or segments of the population who, as a result of their location, cultural practices, or other... effects from exposure to the pesticides discussed in this document, compared to the general population. II... indoxacarb in various matrices including sweet corn, lettuce, tomato, broccoli, apple, grape,...

  3. 76 FR 20667 - Notice of Withdrawal of Pesticide Petitions for Residues of Pesticide Chemicals in or on Various...

    2011-04-13

    ... (75 FR 60452) (FRL-8837- 2) (EPA-HQ-OPP-2010-0547), which announced the filing of a pesticide petition... propionate). EPA issued a notice in the Federal Register of April 8, 2009 (74 FR 15976) (FRL-8409-4) (EPA-HQ... mosaic tobamovirus). EPA issued a notice in the Federal Register of March 10, 2010 (75 FR 11171)...

  4. A Meta-Analysis of the Willingness to Pay for Reductions in Pesticide Risk Exposure

    Travisi, Chiara M.; Nijkamp, Peter; Florax, Raymond J.G.M.

    2004-01-01

    The use of environmental policy instruments such as eco-labelling and pesticide taxes should preferably be based on disaggregate estimates of the individuals' willingness to pay (WTP) for pesticide risk reductions. We review the empirical valuation literature dealing with pesticide risk exposure and develop a taxonomy of environmental and human health risks associated with pesticide usage. Subsequently, we use meta-analysis to investigate the variation in WTP estimates for reduced pesticide r...

  5. Evaluation of low-pressure gas chromatography-tandem mass spectrometry method for analysis of greater than 140 pesticides in fish

    A multi-residue method for analysis of 143 pesticide residues in fish was developed and evaluated using fast, low pressure gas chromatography triple quadrupole tandem mass spectrometry (LP-GC/MS-MS). The method was based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction with ace...

  6. Rapid Determination Method for 12 Pyrethroid Pesticide Residues in Tea by Stir Bar Sorptive Extraction-Thermal Desorption-Gas Chromatography

    Li, Bin; Zeng, Fangang; Dong, Qichun; Cao, Yang; Fan, Haitao; Deng, Chuanfeng

    The 12 pyrethroid Pesticides residues in tea samples can be rapidly extracted and separated by a noval stir bar sorptive extraction(SBSE)-thermal desorption(TDU)-gas chromatography(GC) method. Impurities and pyrethroid pesticides residues of tea can be seperated by this method.and then use TDU-GC to analyse pyrethroid Pesticides residues. The residues of 12 pyrethroid pesticides at same time can be identified and quantified simultaneously by SBSE-TDU-GC rapidiy with high sensitivity and good reproducibility. This method is simple, rapid, and the average adding standard recovery ratios were 92.89%-105.01%.The correlation coefficient of pyrethroid pesticides in tea samples is >0.9926. Good repeatability(n=6) was obtained in all the cases with The relative standard deviation lower 9.7%.Pyrethroid pesticides residues in 4 real tea samples can be determined rapidly by this method, their pyrethroid pesticide residues are all less than MRL of China and European union.

  7. Reduction in pesticide residue levels in olives by ozonated and tap water treatments and their transfer into olive oil.

    Kırış, Sevilay; Velioglu, Yakup Sedat

    2016-01-01

    The effects of different wash times (2 and 5 min) with tap and ozonated water on the removal of nine pesticides from olives and the transfer ratios of these pesticides during olive oil production were determined. The reliability of the analytical methods was also tested. The applied methods of analysis were found to be suitable based on linearity, trueness, repeatability, selectivity and limit of quantification all the pesticides tested. All tap and ozonated water wash cycles removed a significant quantity of the pesticides from the olives, with a few exceptions. Generally, extending the wash time increased the pesticide reduction with ozonated water, but did not make significant differences with tap water. During olive oil processing, depending on the processing technique and physicochemical properties of the pesticides, eight of nine pesticides were concentrated into olive oil (processing factor > 1) with almost no significant difference between treatments. Imidacloprid did not pass into olive oil. Ozonated water wash for 5 min reduced chlorpyrifos, β-cyfluthrin, α-cypermethrin and imidacloprid contents by 38%, 50%, 55% and 61% respectively in olives. PMID:26565682

  8. Search of Organochlorine Pesticide Residues (Pocs) in Bodies of Water in Cotton-Growing Area of Benin by GC-ECD

    *M. A. N. Gbaguidi; 2L. F. Dovonon; A. Youssao; R. Djibril; 1M. Saizonou; 1Y. I. Mohamed; 1H. H. Soclo; Fayomi, B.

    2014-01-01

    Despite their incontestable services in agriculture, the use of pesticides is not without consequences on the environment. So, in an attempt to access the impacts of pesticides usage in agriculture in Benin, research of some residual organochloride pesticides have been conducted both in rainy and dry seasons in two cotton growing areas: the northern and central part of Benin. The analytical technique used is GC-ECD. During the dry season we notice that the DDT and its metabolites (DDE and DDD...

  9. Validation of a multi-residue method for the determination of residuals pesticides in cabbage (Brassica Oleracea var. Capitata) for gases chromatography

    This study describes the validation of a multi-residue method for the determination of most used organo chlorine, organophosphorus and organonitrogen pesticides in cabbage in the Cundinamarca Department (Colombia). The extraction process includes blending of small sample quantity with ethyl acetate in presence of Na2SO4 and NaHCO3, filtration and concentration. The clean up steps include GPC and mini-column chromatography using silica gel. Final determination was carried out by gas chromatography with: pulsed splitless injection, HP-5 capillary column, and a parallel detection system with micro electron capture detection (μ - ECD) and Nitrogen-Phosphorus Detection (NPD). The methodology is specific, selective, accurate and robust. Recovery values of majority of pesticides were in the range 70-120% at spiking levels ranging 0.05-10.73 mg/kg. Limits of detection were less than 0.10 mg/kg for most of the studied compounds. The distribution of the analyses in the laboratory sample was evaluated and it was found its homogeneity. The evaluation of pesticide residues was made in a specific area of municipality of Madrid-Cundinamarca, (Colombia). No residues of the studied analyses were founded

  10. Gel Permeation Chromatography Purification and Gas Chromatography-Mass Spectrometry Detection of Multi-Pesticide Residues in Traditional Chinese Medicine

    Zhen-Bin Gong; Wan-E Zhuang

    2012-01-01

    The measurement of 23 organochlorine, organophosphorus, and pyrethroid pesticides in typical traditional Chinese medicine (TCM), flos lonicerae, was made using gel permeation chromatography (GPC) purification and gas chroma- tography-mass spectrometry (GC-MS) detection. The pesticides were extracted with ultrasonic device and 5.0 mL mixture of ethyl acetate and cyclohexane (1:1, v/v). Coextractants from sample matrices which may have interfere to the qualitative and quantitative analysis, suc...

  11. [Determination of eight pesticide residues in tea by liquid chromatography-tandem mass spectrometry and its uncertainty evaluation].

    Hu, Beizhen; Cai, Haijiang; Song, Weihua

    2012-09-01

    A method was developed for the determination of eight pesticide residues (fipronil, imidacloprid, acetamiprid, buprofezin, triadimefon, triadimenol, profenofos, pyridaben) in tea by liquid chromatography-tandem mass spectrometry. The sample was extracted by accelerated solvent extraction with acetone-dichloromethane (1:1, v/v) as solvent, and the extract was then cleaned-up with a Carb/NH2 solid phase extraction (SPE) column. The separation was performed on a Hypersil Gold C, column (150 mm x 2. 1 mm, 5 microm) and with the gradient elution of acetonitrile and 0. 1% formic acid. The eight pesticides were determined in the modes of electrospray ionization (ESI) and multiple reaction monitoring (MRM). The analytes were quantified by matrix-matched internal standard method for imidacloprid and acetamiprid, by matrix-matched external standard method for the other pesticides. The calibration curves showed good linearity in 1 - 100 microg/L for fipronil, and in 5 -200 microg/L for the other pesticides. The limits of quantification (LOQs, S/N> 10) were 2 p.g/kg for fipronil and 10 microg/kg for the other pesticides. The average recoveries ranged from 75. 5% to 115.0% with the relative standard deviations of 2.7% - 7.7% at the spiked levels of 2, 5, 50 microg/kg for fipronil and 10, 50, 100 microg/kg for the other pesticides. The uncertainty evaluation for the results was carried out according to JJF 1059-1999 "Evaluation and Expression of Uncertainty in Measurement". Items constituting measurement uncertainty involved standard solution, weighing of sample, sample pre-treatment, and the measurement repeatability of the equipment were evaluated. The results showed that the measurement uncertainty is mainly due to sample pre-treatment, standard curves and measurement repeatability of the equipment. The method developed is suitable for the conformation and quantification of the pesticides in tea. PMID:23285969

  12. Awareness of pesticide residues in locally available food and condiments among food sellers: a case study of Osun state, Nigeria

    Samson Ayo Deji

    2012-10-01

    Full Text Available The specific objectives are: i to determine the level of awareness of pesticide residue in locally available food among food sellers in Ile Ife area of Osun state, Nigeria; ii to identify the demographic and socio-economic characteristics of food sellers who use pesticides, natural means in preserving their foodstuff from getting spoilt; iii to determine the level of understanding of food sellers who use pesticides about the likely health implications that could result. The design of the study is cross sectional. Structured open-ended questionnaires were administered to 98 randomly selected food sellers in Ile Ife area Osun state, Nigeria. This includes males and female. The inference from the study shows that majority of the food sellers were between ages 21 and 30 years, suggesting that more of the young people are involved in the selling of foodstuff in the area of study. Most of the food sellers used phostozin, an organophosphate compound as preservatives for cereals. The majority of those that were aware of the health hazards associated with the usage of pesticides as preservative were literate school leavers. Among respondents to the questionnaire, it was expected that many of those food sellers likely to demonstrate caution in the usage of pesticide would be the literate school leavers. This is because they are more aware of the possible associated health hazards than their fellow food sellers who are not literate. The level of awareness of health implications associated with use of pesticides on consumable food items is higher among school certificate holders who are food sellers. Phostozin, an organophosphate, is a common preservative pesticide used on cereals foodstuff (e.g., bean, rice, maize in the area of study, especially among the age group between 21 and 30 years.

  13. [Application of a rapid and simple multi-residue method for determination of pesticide residues in drinking water and beverages using liquid chromatography-tandem mass spectrometry].

    Fukui, Naoki; Takatori, Satoshi; Kitagawa, Yoko; Okihashi, Masahiro; Osakada, Masakazu; Nakatsuji, Naoto; Nakayama, Yukiko; Kakimoto, You; Obana, Hirotaka

    2012-01-01

    A rapid and simple multi-residue method for determination of pesticides has been applied to drinking water and beverages. To a disposable polypropylene tube containing 10.0 g sample, 20 mL acetonitrile was added and the mixture was shaken vigorously for 1 min to extract pesticides. Then, 1 g sodium chloride and 4 g magnesium sulfate anhydrous were added, followed by vigorous shaking for 1 min and centrifugation to obtain the organic phase. The organic phase was processed with a graphite carbon black/PSA solid phase column. After concentration and reconstitution with 25% methanol containing aqueous solution, the test solution was analyzed with LC-MS/MS. Recovery tests of 91 pesticides fortified (0.02 ?g/g) in 35 kinds of drinking water and beverages were conducted. The decline of recoveries in alcoholic beverages is considered to be due to the increase of organic phase volume owing to ethanol included in the alcoholic beverages. A simulation study was carried out with simulated alcoholic beverages, which consisted of 50% grape juice, with various amounts of ethanol and water, to examine pesticides recoveries and volume of the organic phase. The results suggested this method would be applicable both to alcoholic beverages containing less than 10% ethanol and to alcoholic beverages containing over 10% ethanol after dilution with water to below 10% ethanol prior to the addition of acetonitrile. A sample could be processed and analyzed by LC-MS/MS within 2 h. Thus, this method should be useful for monitoring and screening pesticide residues in drinking water and various beverages. PMID:23132358

  14. Multi-residue method for the determination of pesticides and pesticide metabolites in honeybees by liquid and gas chromatography coupled with tandem mass spectrometry-Honeybee poisoning incidents.

    Kiljanek, Tomasz; Niewiadowska, Alicja; Semeniuk, Stanisław; Gaweł, Marta; Borzęcka, Milena; Posyniak, Andrzej

    2016-02-26

    A method for the determination of 200 pesticides and pesticide metabolites in honeybee samples has been developed and validated. Almost 98% of compounds included in this method are approved to use within European Union, as active substances of plant protection products or veterinary medicinal products used by beekeepers to control mites Varroa destructor in hives. Many significant metabolites, like metabolites of imidacloprid, thiacloprid, fipronil, methiocarb and amitraz, are also possible to detect. The sample preparation was based on the buffered QuEChERS method. Samples of bees were extracted with acetonitrile containing 1% acetic acid and then subjected to clean-up by dispersive solid phase extraction (dSPE) using a new Z-Sep+ sorbent and PSA. The majority of pesticides, including neonicotionoids and their metabolites, were analyzed by liquid chromatography tandem mass spectrometry (LC-MS/MS) but some of pesticides, especially pyrethroid insecticides, were analyzed by gas chromatography tandem mass spectrometry (GC-MS/MS). The procedure was validated according to the Guidance document SANCO/12571/2013 at four concentration levels: 1, 5, 10 and 100ng/g bees and verified in the international proficiency test. The analysis of bee samples spiked at the limit of quantification (LOQ) showed about 98% mean recovery value (trueness) and 97% of analytes showed recovery in the required range of 70-120% and RSDr (precision) below 20%. Linearity and matrix effects were also established. The LOQs of pesticides were in the range of 1-100ng/g. The developed method allows determination of insecticides at concentrations of 10ng/g or less, except abamectin and tebufenozide. LOQ values are lower than the median lethal doses LD50 for bees. The method was used to investigate more than 70 honeybee poisoning incidents. Data about detected pesticides and their metabolites are included. PMID:26830634

  15. Residual analysis for spatial point processes

    Baddeley, A.; Turner, R.; Møller, Jesper; Hazelton, M.

    We define residuals for point process models fitted to spatial point pattern data, and propose diagnostic plots based on these residuals. The techniques apply to any Gibbs point process model, which may exhibit spatial heterogeneity, interpoint interaction and dependence on spatial covariates. Our...... residuals generalise the well-known residuals for point processes in time, used in signal processing and survival analysis. An important difference is that the conditional intensity or hazard rate of the temporal point process must be replaced by the Papangelou conditional intensity $lambda$ of the spatial...... process. Residuals are ascribed to locations in the empty background, as well as to data points of the point pattern. We obtain variance formulae, and study standardised residuals. There is also an analogy between our spatial residuals and the usual residuals for (non-spatial) generalised linear models...

  16. [Analysis of scientific background of establishing definitions for Maximum Residue Levels (MRLs)].

    Czaja, Katarzyna; Gralczyk, Katarzyna; Struci?ski, Pawe?; Hernik, Agnieszka; Korcz, Wojciech; Snopczy?ski, Tomasz; Ludwicki, Jan K

    2009-01-01

    For each pesticide used in food or feed productions, the legislative authorities have to establish the residue definitions, that mean compounds which need to be taken into account in risk assessment in process of authorization of plant protection products as well as in establishing and enforcing Maximum Residue Levels (MRLs). The residue definition for a given pesticide can be different depending on the aim for which they are used. Inclusion of a compound in such definition results in consequence in its later analysis in different matrices during monitoring and official control. Inclusion of compounds in the definition depends on a number of factors, and the decisions on whether they should be included have to be made for every case separately. The definition should include toxicologically important compounds, and those which contribute into the residue in 10 or more percent of TRR, or those that have been detected in livestock and plants as metabolites different than those found in rats. PMID:20063688

  17. Guidelines for application of the good laboratory practices and quality assurance and control in pesticide residues analysis; Linee guida per l`applicazione delle buone pratiche di laboratorio e l`assicurazione e il controllo della qualita` nell`analisi di residui di prodotti fitosanitari

    Attard Barbini, Danilo [Istituo Superiore di Sanita`, Rome (Italy); Biancardi, Gino [Agenzia Regionale per la Protezione dell`Ambiente, Massa Carrara (Italy); Bove, Bruno [Presiduo Multizonale di Prevenzione, Potenza (Italy)] [and others

    1997-09-01

    The guidelines, particularly aimed at laboratories which carry out studies in the field of pesticide residues in food and environment, are intended to give practical, organizational and operational hints along the lines set up by the Italian Legislative Decree n. 120 of January 27, 1992 and the European standard UNI CEI EN 45001, to which the laboratories dealing with official control and monitoring should conform. The main items discussed include: organization of the laboratory, personnel and equipment, working procedures related to analytical methodology, confirmation criteria for violation of maximum residue limits and quality control.

  18. Distribution of phthalates, pesticides and drug residues in the dissolved, particulate and sedimentary phases from transboundary rivers (France-Belgium).

    Net, Sopheak; Rabodonirina, Suzanah; Sghaier, Rafika Ben; Dumoulin, David; Chbib, Chaza; Tlili, Ines; Ouddane, Baghdad

    2015-07-15

    Various drug residues, pesticides and phthalates are ubiquitous in the environment. Their presence in the environment has attracted considerable attention due to their potential impacts on ecosystem functioning and on public health. In this work, 14 drug residues, 24 pesticides and 6 phthalates have been quantified in three matrices (in the dissolved phase, associated to suspended solid matter (SSM), and in sediment) collected from fifteen watercourses and rivers located in a highly industrialized zone at the cross-border area of Northern France and Belgium. The extractions have been carried out using accelerated solvent extraction (ASE) for solid matrices (SSM and sediment) and using solid phase extraction (SPE) for liquid matrix. The final extract was analyzed using GC-MS technique. Among the three classes of compounds, phthalates have been found at highest level compared to pesticides and drug residues. The Σ6PAE concentrations were ranging from 17.2±2.58 to 179.1±26.9μgL(-1) in dissolved phase, from 2.9±0.4 to 21.1±3.2μgL(-1) in SSM and from 1.1±0.2 to 11.9±1.8μgg(-1)dw in sediment. The Σ14drug residue concentrations were lower than 1.3μgL(-1) in the dissolved phases, lower than 30ngL(-1) associated to SSM and from nondetectable levels to 60.7±9.1ngg(-1)dw in sediment. For pesticides, all compounds were below the LOQ values in dissolved phase and in sediment, and only EPTC could be quantified in SSM. PMID:25829293

  19. Determination of pesticide residues in nonfatty foods by supercritical fluid extraction and gas chromatography/mass spectrometry: collaborative study.

    Lehotay, Steven J

    2002-01-01

    A collaborative study was conducted to determine multiple pesticide residues in apple, green bean, and carrot by using supercritical fluid extraction (SFE) and gas chromatography/mass spectrometry (GC/MS). Seventeen laboratories from 7 countries participated in the final study, and a variety of different instruments was used by collaborators. The procedure simply entails 3 steps: (1) mix 1.1 g drying agent (Hydromatrix) per 1 g frozen precomminuted sample, and load 4-5.5 g of this mixture into a 7-10 mL extraction vessel; (2) perform SFE for 20-30 min with a 1-2 mL/min flow rate of carbon dioxide at 0.85 g/mL density (320 atm, 60 degrees C); and (3) inject the extract, which was collected on a solid-phase or in a liquid trap, into the gas chromatograph/mass spectrometer, using either an ion-trap instrument in full-scan mode or a quadrupole-type instrument in selected-ion monitoring mode. The ability of GC/MS to simultaneously quantitate and confirm the identity of the semivolatile analytes at trace concentrations is a strong feature of the approach. The selectivity of SFE and GC/MS avoids the need for post-extraction cleanup steps, and the conversion of the CO2 solvent to a gas after SFE eliminates the solvent evaporation step common in traditional methods. The approach has several advantages, but its main drawback is the lower recoveries for the most polar analytes, such as methamidophos and acephate, and the most nonpolar analytes, such as pyrethroids. Recoveries for most pesticides are >75%, and recoveries of nonpolar analytes are still >50%. The (within-laboratory) repeatability relative standard deviation (RSDr) values of the recoveries are generally metalaxyl in carrot (75-500 ng/g), 89% recovery, 8% RSDr, 12% RSDR; parathion-methyl in carrot (75-500 ng/g), 84% recovery, 14% RSDr, 15% RSDR; chlorpyrifos in carrot (50-300 ng/g), 77% recovery, 13% RSDr, 19% RSDR; and bifenthrin in carrot (90-600 ng/g), 63% recovery, 12% RSDr, and 25% RSDR. All analytes except for the nonpolar compounds trifluralin, p,p'-DDE, and bifenthrin gave average Horwitz ratios of residue analysis, and the Study Director recommends that it be adopted Official First Action. PMID:12374416

  20. A rapid, solid phase extraction (SPE) technique for the extraction and gas chromatographic determination lindane pesticide residue in tissue and milk

    Yuningsih; Sri Yuliastuti

    2012-01-01

    Organochlorine pesticide contamination in feed can cause residue in animal product (tissue and milk), so its become a problem in food safety. Solid phase extraction (SPE) has been carried out for determination organochlorine pesticide residues in food animal production. The technique was rapid, not costly and produce limited amount of hazardous-waste. Samples were homogenized with acetonitrile trough cartridge C18, eluted in fluorocyl column with 2% ether-petroleum or acetonitrile fortissue a...

  1. Residues in Food and Feed Topic Area at the 13th IUPAC International Congress of Pesticide Chemistry.

    Lehotay, Steven J; Riter, Leah S; Saha, Manasi

    2015-05-13

    The organizers of two symposia in the "Residues in Food and Feed" topic area held at the 13th IUPAC International Congress of Pesticide Chemistry introduce the papers that were contributed to this special section in the Journal. The symposia were titled "Taking Advantage of Advanced Analytical Tools" and "Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods". The oral and poster sessions generated much interest and discussion among the attendees, and some highlights are described in this introductory paper. PMID:25660997

  2. Pesticide residues in tropical coastal lagoons: Use of 14C labelled compounds to study the cycling and fate of agrochemicals

    Organophosphorus and organochlorine pesticide residues present in tropical coastal lagoons originate from the use of agrochemicals in the surrounding fields. A study of the early stages in the cycling and fate of chlorpyrifos, parathion and DDT in this type of ecosystem was conducted using 14C labelled compounds in microcosm and large outdoor tank experiments. Organophosphates in water were shown to be degraded by chemical hydrolysis and microbial action. The effect of temperature was investigated and it was found that increased temperature enhanced the degradation rates of these compounds. However, the rapid association of pesticides with sediments increased their persistence in the aquatic environment. Microbial biomass associated with the sediments contributed significantly to the degradation of these compounds, but the action of microbes did not compensate for the increase in pesticide persistence afforded by sorption to sediment. Preliminary results from outdoor tank experiments indicate that sediment associated pesticides remain biologically available at least partially to tropical benthic organisms. (author). 16 refs, 4 figs, 3 tabs

  3. Honey bees (Apis mellifera) reared in brood combs containing high levels of pesticide residues exhibit increased susceptibility to Nosema (Microsporidia) infection.

    Wu, Judy Y; Smart, Matthew D; Anelli, Carol M; Sheppard, Walter S

    2012-03-01

    Nosema ceranae and pesticide exposure can contribute to honey bee health decline. Bees reared from brood comb containing high or low levels of pesticide residues were placed in two common colony environments. One colony was inoculated weekly with N. ceranae spores in sugar syrup and the other colony received sugar syrup only. Worker honey bees were sampled weekly from the treatment and control colonies and analyzed for Nosema spore levels. Regardless of the colony environment (spores+syrup added or syrup only added), a higher proportion of bees reared from the high pesticide residue brood comb became infected with N. ceranae, and at a younger age, compared to those reared in low residue brood combs. These data suggest that developmental exposure to pesticides in brood comb increases the susceptibility of bees to N. ceranae infection. PMID:22285445

  4. Organo chlorine pesticide residues in the major rivers of Southern Thailand

    Environmental contaminations by organo chlorine pesticides (OCPs) of inland water have been a global issues, since most of these compounds are very persistent, bio accumulative and toxic compounds. Due to the widespread use of DDT for malaria vector eradication programs in the past and no comprehensive works have been conducted to assess trace organic pollutants in river waters, this work is the first effort to assess the contamination levels of OCPs in the major rivers of Southern Thailand. The objectives of this study were to determine the concentration levels of OCPs and oil and grease in the 3 major rivers and to compare the present results with surrounding regions for further assessment of OCPs contamination status in inland waters of Southern Thailand. Ther water samples were collected along the 3 major rivers (Saiburi, Patani and Tiba River) during July 2006-February 2007. Water samples were solid phase extracted with Supelco C-18 cartridge (1 g/ 6 mL) and quantified by gas chromatograph (GC-ECD). The concentration of oil and grease was determined by gravimetric method and reported as hexane extractable material (HEM) and silica gel treated hexane extractable material (SGT-HEM). Severla parameters of waters such as total suspended solid, pH, turbidity and conductivity were measured. The commonly found OCP residues in these rivers were β-HCH, γ-HCH, heptachlor epoxide, endosulfan 1, p,p'-DDE and endrin aldehyde. The overall results showed that Saiburi River was more polluted with OCPs than Patani and Tiba River, especially p, p'-DDE which was detected in the wide range concentration of 9.6 to 203.1 ng/ mL. For oil and grease contamination, Tiba River waters were found to be more polluted than either Patani or Saiburi River. The experimental procedures and analytical results together with the possible sources of OCPs and its environmental impacts are presented. (author)

  5. [Comparison of the performances of gas chromatography-quadrupole time of flight mass spectrometry and gas chromatography-tandem mass spectrometry in rapid screening and confirmation of 208 pesticide residues in fruits and vegetables].

    Cao, Xinyue; Pang, Guofang; Jin, Linghe; Kang, Jian; Hu, Xueyan; Chang, Qiaoying; Wang, Minglin; Fan, Chunlin

    2015-04-01

    The performances of gas chromatography-tandem mass spectrometry (GC-MS/MS) and gas chromatography quadrupole time of flight mass spectrometry (GC-QTOF/MS) for the determination of 208 pesticide residues in fruit and vegetable samples, including apple, orange, tomato and cucumber, were compared comprehensively. Based on the differences of the two instruments, their respective characteristics and scopes of application in the detection of the pesticide residues were presented, which provided the reference for the analysis of pesticide residues. The performance parameters of the two instruments, such as overall recoveries, precisions, limits of detection, linear ranges, identification points and matrix effects, were evaluated according to a designed experiment. At three spiked levels (5.0, 10.0 and 20.0 µg/kg), the average recoveries for the majority of pesticides (93.0%) ranged from 70% to 120% in the four matrices with relative standard deviations below 20%. The limits of detection for most of the pesticides by GC-MS/MS and GC-Q-TOF/MS were less than 5.0 µg/kg. Compared with GC-QTOF/MS, GC-MS/MS showed relatively lower limits of detection and wider linear ranges, and its performance was more satisfactory in accurate quantitative analysis due to its superior sensitivity. On the other hand, GC-QTOF/MS provided accurate mass measurement, which was proved to be an efficient analytical tool on the rapid screening and confirmation of a large number of pesticides and non-target compounds. PMID:26292409

  6. Spatio-temporal patterns of pesticide residues in the Turia and Jcar Rivers (Spain).

    Ccanccapa, Alexander; Masi, Ana; Andreu, Vicente; Pic, Yolanda

    2016-01-01

    A study was conducted on the occurrence of 50 pesticides in water and sediments of Turia and Jcar Rivers (Valencian Community, Eastern Spain) for a period of two consecutive years each, 2010/2011 and 2012/2013, respectively to assess the contribution of agriculture and urban activities on pesticide pollution. The results showed that mean concentrations of pesticides ranged from agricultural practices and rainfall. Contrarily, in the abrupt part of the rivers of difficult access the contamination is low. Other quality parameters monitored in this study also corroborate the worst water quality in the alluvial plains that coincides with higher anthropic pressure. The temporal variations also indicated a strong relation of pesticide concentrations with hydrology, the higher the river flow, the higher number and frequency of pesticides but at lower concentrations. On the contrary, at lower river flows higher pesticide concentrations were detected. The risk assessment for aquatic biota pointed out that organophosphorus and fungicides are a threat to fish and daphnia and herbicides and fungicides are hazards for algae. Thus, the strict control of pesticide concentrations is important to preserve the aquatic ecosystems health. PMID:26118860

  7. Tank 12H residuals sample analysis report

    Oji, L. N. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Shine, E. P. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Diprete, D. P. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Coleman, C. J. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Hay, M. S. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2015-06-11

    The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) to provide sample preparation and analysis of the Tank 12H final characterization samples to determine the residual tank inventory prior to grouting. Eleven Tank 12H floor and mound residual material samples and three cooling coil scrape samples were collected and delivered to SRNL between May and August of 2014.

  8. Combining solid-phase microextraction and on-line preconcentration-capillary electrophoresis for sensitive analysis of pesticides in foods.

    Hernández-Borges, Javier; Cifuentes, Alejandro; García-Montelongo, Francisco J; Rodríguez-Delgado, Miguel A

    2005-02-01

    The combined use of solid-phase microextraction (SPME) and different on-line preconcentration strategies for ultrasensitive capillary electrophoresis-ultraviolet (CE-UV) analysis of five pesticides in a single run is investigated. Normal stacking mode (NSM), field-enhanced sample injection (FESI), and stacking with matrix removal (SWMR) are explored to increase the sensitivity of the CE-UV analysis of a selected group of pesticides (cyprodinil, cyromazine, pyrifenox, pirimicarb, and pyrimethanil). It could be observed that reverse polarity-stacking with matrix removal (RP-SWMR) provided the best results in terms of sensitivity (enhancement was up to 272-fold compared with normal injection). The separation buffer consisted of 0.4 mM cetyltrimethylammonium chloride (CTAC), 0.4 M acetic acid at pH 4 containing 5% v / v 2-propanol. This approach was then combined with SPME to determine the pesticides in water, apple, and orange juice. The combination of both preconcentration procedures allowed the determination of these pesticides at concentrations down to 2.5 microg / L in water and 3.1 microg / L in juices (i.e., levels well below the maximum residue limits allowed for these compounds). To our knowledge, this is the first report showing the great possibilities of the combined use of SPME, on-line sample preconcentration, and CE for pesticide analysis. PMID:15714540

  9. QuEChERS sample preparation for the determination of pesticides and other organic residues in environmental matrices: a critical review.

    Bruzzoniti, Maria Concetta; Checchini, Leonardo; De Carlo, Rosa Maria; Orlandini, Serena; Rivoira, Luca; Del Bubba, Massimo

    2014-07-01

    Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) is an extraction and clean-up technique originally developed for recovering pesticide residues from fruits and vegetables. Since its introduction, and until December 2013, about 700 papers have been published using the QuEChERS technique, according to a literature overview carried out using SciFinder, Elsevier SciVerse, and Google search engines. Most of these papers were dedicated to pesticide multiresidue analysis in food matrices, and this topic has been thoroughly reviewed over recent years. The QuEChERS approach is now rapidly developing beyond its original field of application to analytes other than pesticides, and matrices other than food, such as biological fluids and non-edible plants, including Chinese medicinal plants. Recently, the QuEChERS concept has spread to environmental applications by analyzing not only pesticides but also other compounds of environmental concern in soil, sediments, and water. To the best of our knowledge, QuEChERS environmental applications have not been reviewed so far; therefore, in this contribution, after a general discussion on the evolution and changes of the original QuEChERS method, a critical survey of the literature regarding environmental applications of conventional and modified QuEChERS methodology is provided. The overall recoveries obtained with QuEChERS and other extraction approaches (e.g., accelerated solvent extraction, ultrasonic solvent extraction, liquid/solid extraction, and soxhlet extraction) were compared, providing evidence for QuEChERS higher recoveries for various classes of compounds, such as biopesticides, chloroalkanes, phenols, and perfluoroalkyl substances. The role of physicochemical properties of soil (i.e., clay and organic carbon content, as well as cation exchange capacity) and target analytes (i.e., log KOW, water solubility, and vapor pressure) were also evaluated in order to interpret recovery and matrix effect data. PMID:24770804

  10. Organophosphorus and Carbamate Pesticide Residues Detected in Water Samples Collected from Paddy and Vegetable Fields of the Savar and Dhamrai Upazilas in Bangladesh

    Nurul Karim

    2012-09-01

    Full Text Available Several types of organophosphorous and carbamate pesticides have been used extensively by the farmers in Bangladesh during the last few decades. Twenty seven water samples collected from both paddy and vegetable fields in the Savar and Dhamrai Upazilas in Bangladesh were analyzed to determine the occurrence and distribution of organo-phosphorus (chlorpyrifos, malathion and diazinon and carbamate (carbaryl and carbofuran pesticide residues. A high performance liquid chromatograph instrument equipped with a photodiode array detector was used to determine the concentrations of these pesticide residues. Diazinon and carbofuran were detected in water samples collected from Savar Upazila at 0.9 μg/L and 198.7 μg/L, respectively. Malathion was also detected in a single water sample at 105.2 μg/L from Dhamrai Upazila. Carbaryl was the most common pesticide detected in Dhamrai Upazila at 14.1 and 18.1 μg/L, while another water sample from Dhamrai Upazila was contaminated with carbofuran at 105.2 μg/L. Chlorpyrifos was not detected in any sample. Overall, the pesticide residues detected were well above the maximum acceptable levels of total and individual pesticide contamination, at 0.5 and 0.1 μg/L, respectively, in water samples recommended by the European Economic Community (Directive 98/83/EC. The presence of these pesticide residues may be attributed by their intense use by the farmers living in these areas. Proper handling of these pesticides should be ensured to avoid direct or indirect exposure to these pesticides.

  11. 77 FR 50661 - Notice of Filing of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2012-08-22

    ... determination of imazapyr residues in milk. Contact: Hope Johnson, (703) 305-5410, email address: johnson.hope... nuts (group 14, except almond hulls) at 0.3 ppm; and almond, hulls (group 12) at 20 ppm. An adequate... for milk and juices, and 0.01 ppm for all other substrates. Contact: Julie Chao, (703) 308-...

  12. 75 FR 5790 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-02-04

    ... tolerances in 40 CFR part 180 for residues of the insecticide fluazifop-p-butyl, in or on potato, tuber at 1.1 ppm; potato, peel (wet) at 1.1 ppm; potato, chips at 3.0 ppm; and potato, granules/flakes at...

  13. 78 FR 11126 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2013-02-15

    ... using capillary gas liquid chromatography (GLC) with flame ionization detector (FID). Contact: Andrew... to detect either the phenyl or the triazole ring would be appropriate for the measurement of residues. However, because of the natural occurrence of compounds that interfere with the measurement of...

  14. 78 FR 13295 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2013-02-27

    ... degradates, in or on corn, sweet, kernel plus cob with husks removed at 0.01 ppm; corn, sweet, forage at 15 ppm; and corn, sweet, stover at 30 ppm. Based upon the metabolism of acetamiprid in plants and the... ethyl acetate. The residue method for wheat straw is similar, except that a C 18 solid phase...

  15. 75 FR 14154 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-03-24

    ... residues of alkyl polyglucoside esters (AGEs) group, formed by D- Glucopyranose, oligomeric, 6-(dihydrogen... salts (CAS No. 1079993-97-7); D- Glucopyranose, oligomeric, 6-(hydrogen sulfobutanedioate), 1- (C 8 -C 20 linear and branched alkyl) ethers, sodium salts (CAS No. 1079993-92-2);...

  16. 75 FR 9596 - Notice of Filing of a Pesticide Petition for Residues of a Aspergillus flavus AF36 on Corn Food...

    2010-03-03

    ... From the Federal Register Online via the Government Publishing Office ENVIRONMENTAL PROTECTION AGENCY Notice of Filing of a Pesticide Petition for Residues of a Aspergillus flavus AF36 on Corn Food... residues of the antifungal ] agent, Aspergillus flavus AF36, in or on corn food and feed commodities....

  17. Monitoring Pesticide Residues in Surface and Ground Water in Hungary: Surveys in 1990–2015

    András Székács; Mária Mörtl; Béla Darvas

    2015-01-01

    Over 2000 surface, ground and raw drinking water samples have been analyzed in the frame of different monitoring projects in Hungary and watercourses in neighboring countries between 1990 and 2015. Effects of pesticide contamination on ecological farming and drinking water supply have been assessed. Main water pollutant ingredients of agricultural origin in Hungary are herbicides related to maize production. After EU pesticide re-registration, diazinon, atrazine, and trifluralin gradually dis...

  18. Comparison of pesticide residues in surface water and ground water of agriculture intensive areas

    Lari, Summaiya Z; Khan, Noor A; Gandhi, Kavita N; Meshram, Tejal S; Thacker, Neeta P

    2014-01-01

    The organochlorines (OClPs) and organophosphates (OPPs) pesticides in surface and ground water having intensive agriculture activity were investigated to evaluate their potential pollution and risks on human health. As per USEPA 8081 B method, liquid-liquid extraction followed by Gas-Chromatographic technique with electron capture detector and mass selective detector (GC-MS) were used for monitoring of pesticides. Among organochlorines, α,β,γ,δ HCH’s, aldrin, dicofol, DDT and its derivatives,...

  19. Consumers’ Willingness to Pay for Cabbage with Minimized Pesticide Residues in Southern Benin

    Faustin Vidogbéna; Anselme Adégbidi; Rigobert Tossou; Françoise Assogba-Komlan; Thibaut Martin; Mathieu Ngouajio; Serge Simon; Laurent Parrot; Zander, Kerstin K.

    2015-01-01

    Cabbage (Brassicaceae) is one of the most frequently consumed exotic vegetables in Benin and also the most affected by insects. To meet growing food demand, farmers rely heavily on synthetic pesticides that are harmful for themselves, consumers and the environment. Integrated pest management has been proposed as the means to improve vegetable productivity and quality in many developing countries. One approach is to substitute pesticides with physical barriers to insects, like nets. Here, we a...

  20. Organochlorine pesticides residues and PCBs in benthic organisms of the inner shelf of the São Sebastião Channel, São Paulo, Brazil

    Rosângela Gorni; Rolf Roland Weber

    2004-01-01

    Thirty seven benthic samples of the inner shelf area of São Sebastião, Brazil, were collected between April 1994 and August 1998 and analysed for seventeen chlorinated pesticide residues and PCBs congeners. Pesticide residues and PCBs congeners levels were low (ng/g) and predominantly found in the crustacean samples. DDE was the most frequently residue with a maximum of 9,7 ng/g followed by HCHs with maximum of 17,1ng/g. As for the PCBs, the heavier congeners predominate: CB 138,153,170, 180 ...

  1. Organochlorine pesticide residues in human breast milk and placenta in Tohoku, Japan

    Nakai, K.; Suzuki, K.; Oka, T.; Sugawara, N.; Ohba, T.; Kameo, S.; Satoh, H. [Environmental Heath Sciences, Tohoku Univ. Graduate School of Medicine, Sendai (Japan); Nakamura, T.; Saitoh, Y. [Miyagi Prefectural Inst. of Piblic Health and Environment (Japan); Okamura, K. [Dept. of Obstetrics, Tohoku Univ. Graduate School of Medicine, Sendai (Japan)

    2004-09-15

    Recently, we have started a birth cohort study to examine the effects of exposure to persistent organochemical pollutants and heavy metals on neurodevelopment in Japanese children, The Tohoku Study of Child Development. In this cohort study, biological samples, including maternal peripheral blood, cord blood, placenta, cord tissue, and breast milk have been collected from more than six hundred mother-infant pairs for chemical determinations. The growth of infants has been monitored using neurodevelopmental tests, including the Brazelton Neonatal Behavioral Assessment Scale, the Bayley Scale of Infant Development, the Kyoto Scale of Psychological Development, and others. Exposures to dioxin and related compounds, polychlorinated biphenyls, methylmercury, and several heavy metals were assessed. Additionally, since perinatal exposure to organochlorine pesticides may affect the neurodevelopment of children, we examined the effects of those pesticides in the cohort study. In the present study, several organochlorine pesticides were analyzed in human breast milk and placenta from 20 mothers to identify the major pesticide compounds found in the cohort subjects. The relationship between pesticides in breast milk and the placenta was analyzed to examine the utilization of the placenta as the material for exposure assessment. Some information regarding the factors affecting the contamination of breast milk and the placenta with organochlorine pesticides are also discussed.

  2. Influence of different planting seasons of six leaf vegetables on residues of five pesticides.

    Fan, Sufang; Deng, Kailin; Yu, Chuanshan; Zhao, Pengyue; Bai, Aijuan; Li, Yanjie; Pan, Canping; Li, Xuesheng

    2013-09-25

    To investigate the influence of different planting seasons on the dissipation of pesticides, field experiments of thiophanate-methyl, metalaxyl, fluazifop-P-butyl, chlorpyrifos, and λ-cyhalothrin on six crops including pakchoi, rape, crown daisy, amaranth, spinach, and lettuce were designed and conducted. In this study, a high-performance liquid chromatography and electrospray ionization-tandem mass spectrometer with multiple reaction monitoring was used to simultaneously determine thiophanate-methyl and its metabolite carbendazim, metalaxyl, and fluazifop-P-butyl in various samples; gas chromatography with an electron capture detector was used to detect chlorpyrifos and λ-cyhalothrin. The limits of quantitation (LOQs) of these six pesticides were in the range of 0.001-0.01 mg kg(-1) for all samples, and the average recoveries of all pesticides ranged from 60.1 to 119.1% at 0.01 and 0.1 mg kg(-1) spiked levels. The relative standard deviation (RSD) ranged from 1.1 to 13.9%. All maximal concentrations of the six pesticides in six leaf vegetables in autumn were higher than in summer in Beijing. For most pesticides half-lives in autumn were longer than in summer. The results showed that the initial concentration, maximal concentration, and half-lives of pesticides were influenced not only by environmental factors such as light, heat, moisture, and rainy climate but also by plant matrices. PMID:23978278

  3. Residual analysis for spatial point processes

    Waagepetersen, Rasmus Plenge

    2005-01-01

    Discussion of the paper "Residual analysis for spatial point processes" by A. Baddeley, M. Hazelton, J. Møller and R. Turner. Journal of the Royal Statistical Society, Series B, vol. 67, pages 617-666, 2005.......Discussion of the paper "Residual analysis for spatial point processes" by A. Baddeley, M. Hazelton, J. Møller and R. Turner. Journal of the Royal Statistical Society, Series B, vol. 67, pages 617-666, 2005....

  4. Pesticide residues in Nile tilapia (Oreochromis niloticus) and Nile perch (Lates niloticus) from Southern Lake Victoria, Tanzania

    Henry, L. [Chemistry Department, University of Dar es Salaam. PO Box 35061, Dar es Salaam (Tanzania); Kishimba, M.A. [Chemistry Department, University of Dar es Salaam. PO Box 35061, Dar es Salaam (Tanzania)]. E-mail: kishimba@chem.udsm.ac.tz

    2006-03-15

    Nile tilapia (Oreochromis niloticus) and Nile perch (Lates niloticus) samples were collected from fish landing stations in nine riparian districts on the Tanzanian side of Lake Victoria and screened for residues of 64 organochlorine, organophosphorus, carbamate, and pyrethroid pesticides. The residue levels in the fish fillet were up to 0.003, 0.03 and 0.2 mg/kg fresh weight (0.7, 3.8 and 42 mg/kg lipid weight) of fenitrothion, DDT and endosulfan, respectively. Mean levels within sites were up to 0.002, 0.02 and 0.1 mg/kg fresh weight (0.5, 0.5 and 16 mg/kg lipid weight), respectively. The detection of higher levels of p,p'-DDT than the degradation products (p,p'-DDD and p,p'-DDE), and higher levels of endosulfan isomers ({alpha} and {beta}) than the sulphate, in fish samples, implied recent exposure of fish to DDT and endosulfan, respectively. Generally, most of the fish samples had residue levels above the average method detection limits (MDLs), but were within the calculated ADI. - Fish from Lake Victoria had relatively low pesticide levels.

  5. Pesticide residues in Nile tilapia (Oreochromis niloticus) and Nile perch (Lates niloticus) from Southern Lake Victoria, Tanzania

    Nile tilapia (Oreochromis niloticus) and Nile perch (Lates niloticus) samples were collected from fish landing stations in nine riparian districts on the Tanzanian side of Lake Victoria and screened for residues of 64 organochlorine, organophosphorus, carbamate, and pyrethroid pesticides. The residue levels in the fish fillet were up to 0.003, 0.03 and 0.2 mg/kg fresh weight (0.7, 3.8 and 42 mg/kg lipid weight) of fenitrothion, DDT and endosulfan, respectively. Mean levels within sites were up to 0.002, 0.02 and 0.1 mg/kg fresh weight (0.5, 0.5 and 16 mg/kg lipid weight), respectively. The detection of higher levels of p,p'-DDT than the degradation products (p,p'-DDD and p,p'-DDE), and higher levels of endosulfan isomers (? and ?) than the sulphate, in fish samples, implied recent exposure of fish to DDT and endosulfan, respectively. Generally, most of the fish samples had residue levels above the average method detection limits (MDLs), but were within the calculated ADI. - Fish from Lake Victoria had relatively low pesticide levels

  6. New platform of biosensors for prescreening of pesticide residues to support laboratory analyses.

    Buonasera, Katia; Pezzotti, Gianni; Scognamiglio, Viviana; Tibuzzi, Arianna; Giardi, Maria Teresa

    2010-05-26

    Millions of tons of pesticides are applied worldwide annually in agriculture. Among them, herbicides such as triazines and ureas, originating from agricultural runoff, can contaminate soils and surface and ground waters with severe toxic effects on humans. Nowadays, different analytical techniques are available for the detection of these chemicals; however, most of them are expensive and time-consuming, especially in the case of routine analyses. For this reason, on the basis of results collected through many years of experience in the field of photosynthetic organisms, we designed a biosensor platform intended for the easy, low-cost, and fast prescreening of photosynthetic herbicides. The platform combines the possibilities of amperometric and optical transduction systems, which have proven to be highly sensitive (limits of detection = 10(-10)-10(-8) M). The use of genetically modified algae strengthens the power of the platform, allowing different subclasses of herbicides to be recognized. The system has been validated for the analysis of environmental water and is proposed to support laboratories involved in the control of water pollution. PMID:20020685

  7. 76 FR 38158 - Withdrawal of Pesticide Petitions for Residues of Pesticide Chemicals in or on Various Commodities

    2011-06-29

    ...-pyrrolidone (Agsolex 8) (CAS Reg No. 2687-94- 7) and N-(n-dodecyl)-2-pyrrolidone (Agsolex 12) (CAS Reg. No... commodities, or to animals. EPA also issued a Notice of Filing on September 2, 1999 (64 FR 48165) (FRL-6094-5... proposed to amend 40 CFR Part 180 for residues of N-(n-octyl)- 2-pyrrolidone (Agsolex 8) (CAS Reg. No....

  8. Non-destructive detection of pesticide residues in cucumber using visible/near-infrared spectroscopy.

    Jamshidi, Bahareh; Mohajerani, Ezeddin; Jamshidi, Jamshid; Minaei, Saeid; Sharifi, Ahmad

    2015-01-01

    The feasibility of using visible/near-infrared (Vis/NIR) spectroscopy was assessed for non-destructive detection of diazinon residues in intact cucumbers. Vis/NIR spectra of diazinon solution and cucumber samples without and with different concentrations of diazinon residue were analysed at the range of 450-1000 nm. Partial least squares-discriminant analysis (PLS-DA) models were developed based on different spectral pre-processing techniques to classify cucumbers with contents of diazinon below and above the MRL as safe and unsafe samples, respectively. The best model was obtained using a first-derivative method with the lowest standard error of cross-validation (SECV = 0.366). Moreover, total percentages of correctly classified samples in calibration and prediction sets were 97.5% and 92.31%, respectively. It was concluded that Vis/NIR spectroscopy could be an appropriate, fast and non-destructive technology for safety control of intact cucumbers by the absence/presence of diazinon residues. PMID:25789964

  9. Determination of pesticide residues in high oil vegetal commodities by using various multi-residue methods and clean-ups followed by liquid chromatography tandem mass spectrometry.

    Rajski, ?ukasz; Lozano, Ana; Ucls, Ana; Ferrer, Carmen; Fernndez-Alba, Amadeo R

    2013-08-23

    Several extraction methods were evaluated in terms of recoveries and extraction precision for 113 pesticides in avocado: QuEChERS with various d-SPE clean-ups (Z-Sep, Z-Sep+, PSA+C18 and silica), miniLuke and ethyl acetate. Extracts were analysed using liquid chromatography coupled with triple quadrupole mass spectrometer working in multi-reaction monitoring mode. Z-Sep and Z-Sep+ are new types of material for high lipid matrices - these two sorbents contain ZrO2, which improves fat removal from the extracts. The QuEChERS protocol with Z-Sep provided the highest number of pesticides with recoveries in the 70-120% range along with the lowest amount of coextracted matrix compounds. Subsequently, this method was validated in two matrices - avocado and almonds. In the validation recoveries at two levels - 10 and 50?g/kg - limit of quantitation, linearity, matrix effects, as well as the inter- and intraday precision were studied. In the avocado samples, 107 analytes had LOQs equal to 10?g/kg (signal to noise of quantitative transition was equal 20 or more). In the almond samples, 92 pesticides had LOQs equal to 10?g/kg (S/N?20) and 2 pesticides at 50?g/kg. The validated method was employed in the analysis of real avocado and almond samples. PMID:23871559

  10. Development and validation of a cellular biosensor detecting pesticide residues in tomatoes.

    Flampouri, Kelly; Mavrikou, Sophie; Kintzios, Spiridon; Miliadis, George; Aplada-Sarlis, Pipina

    2010-03-15

    Two of the most important categories of pesticides used in agricultural practice are organophosphates and dithiocarbamates. Their extensive and inappropriate use has rendered their reliable monitoring at trace levels more and more necessary. This study presents the construction of a rapid and sensitive cellular biosensor test based on the measurement of changes of the cell membrane potential of immobilized cells, according to the working principle of the Bioelectric Recognition Assay (BERA). The cells were immobilized by entrapment in a sodium alginate bead and directly applied in different pesticide dilutions and agricultural samples. The pesticides used were the organophosphate insecticide diazinon and the dithiocarbamate fungicide propineb. Two different cell types, N2a (neuroblastoma) and Vero (fibroblast) were used as the biosensory elements in order to investigate their differential response against the pesticides. In this way, we hoped to increase the selectivity of the assay. Based on the observed patterns of response, we demonstrate that the sensor can be used for the qualitative and, in some concentrations, quantitative detection of the pesticides with a high degree of reproducibility. The lowest detected concentration was 3nM. Finally, for the investigation of the effects of different pesticides on the accumulation of cytosolic Ca(2+), we conducted a fluorescent assay on N2a cells treated with tomato sample extracts, which were replicates of the E.U. proficiency test sample. The tomato samples were either organically grown or contained 14 different pesticides. The experimental results showed a higher increase of the intracellular Ca(2+) concentration in cells treated with non-organic samples compared to the cells treated with organic samples. PMID:20152413

  11. Pesticide formulation analysis by gas chromatography flame ionization detector

    Gas liquid chromatography system equipped with flame ionization detector was used in the analysis of pesticides formulation. A series of organophosphorus pesticides formulation (Cypermethrin and Dursban) were investigated under different conditions. The samples under study were consisting of 20 blank formulated sample (without active ingredient) and 5 formulated samples with active ingredients. Three capillary columns were used; 10 meter fused silica thick film containing a non-polar methyl silicone, 20- meter thin film methyl silicone and 50-m (0.25 ?m x 0.32 mm. i. d.) methyl silicone, thin film. The three types of columns were used to assess and achieve a simple and practical way for quantitative measurement with RSD within 1% for a series of organophosphours pesticide formulations. 10 meter fused silica thick film also used to separate and determine the four stereo isomers of Cypermethrin present in such formulations. Mixtures with relatively short retention times, as well as Dursban. The 10-meter column, although of high quality, only partially resolved the Cypermethrin isomers into three overlapping peaks instead of the expected four. As a consequence, the 10-meter capillary column produced the largest errors in the quantitative analysis and was unsatisfactory, especially with regard to the Cypermethrin content. The performance of the 10-meter column could not be improved even when conditions were varified however, both columns (20 m, 50 m) showed good performance and solved the Cypermethrin isomers completely. (author)

  12. Residual stress concerns in containment analysis

    The manufacturing of steel containment vessels starts with the forming of flat plates into curved plates. A steel containment structure is made by welding individual plates together to form the sections that make up the complex shaped vessels. The metal forming and welding process leaves residual stresses in the vessel walls. Generally, the effect of metal forming residual stresses can be reduced or virtually eliminated by thermally stress relieving the vesseL In large containment vessels this may not be practical and thus the residual stresses due to manufacturing may become important. The residual stresses could possibly tiect the response of the vessel to internal pressurization. When the level of residual stresses is significant it will affect the vessel's response, for instance the yielding pressure and possibly the failure pressure. The paper will address the effect of metal forming residual stresses on the response of a generic pressure vessel to internal pressurization. A scoping analysis investigated the effect of residual forming stresses on the response of an internally pressurized vessel. A simple model was developed to gain understanding of the mechanics of the problem. Residual stresses due to the welding process were not considered in this investigation

  13. Studying of specific disintegrative characteristic for pesticide residues that used in green vegetables in the environment of Dalat city

    After pesticides are used, the disintegration occurs due to light, temperature, alkaline materials and bio-microorganism in soil and water. The disintegration rate depends on chemical properties of each pesticide and environmental conditions. In this work, use of the method enable plant material to be extracted and cleaned up for gas chromatographic determination of residues of 4 compounds of the organophosphorus and pyrethroid groups as dimethoat, clopyrifos, methidathion and cypermethrin compounds by one or the same procedure. Limit of detection and limit of quantitation are determined in range of 5-10 ng and 0.01-0.05 ppm. Recovery is in range 80-98%. The transformation and disintegration rate in vegetables such as: Nozawana, Perilla and Spinach depends on the stability of pesticides used, the activities of enzyme in soil and water and weather conditions. Their process occurs fast when vegetables are in the interval of growth and in the condition of high temperature, moisture and light intensity. The disintegration rate of 4 compounds of the organophosphorus and pyrethroid groups in vegetables occurs faster in dry season than rainy season (author)

  14. Accumulative characteristics of pesticide residues in organs of bivalves (Anodonta woodiana and Corbicula leana) under natural conditions.

    Uno, S; Shiraishi, H; Hatakeyama, S; Otsuki, A; Koyama, J

    2001-01-01

    Accumulative characteristics of pesticide residues in the gill, midgut gland, gonad, and the remaining tissues of the bivalve mollusks Anodonta woodiana and Corbicula leana were examined during the rice planting seasons of 1992 and 1994. Although seven pesticides, except thiobencarb, were accumulated all at ppb levels in the midgut gland (liver) and gonad of both bivalves during their application period, thiobencarb was accumulated in C. leana at extremely high levels of 15.70 microg g(-1) in 1992 and 12.45 microg g(-1) in 1994 in the midgut gland and 15.80 microg g(-1) in 1992 and 16.40 microg g(-1) in 1994 in the gonad, respectively. These levels were about 100 times higher than those in A. woodiana. Thiobencarb and molinate in A. woodiana and chlornitrofen (CNP) and molinate in C. leana remained in the gonad and midgut gland longer than in the gill and remaining tissues, while thiobencarb in organs of C. leana remained at ppm levels until the end of the experiments. The present study suggests that these interspecies differences can be attributed to differences between the two species in their ability to eliminate pesticides. PMID:11116339

  15. A lysimeter experiment to investigate temporal changes in the availability of pesticide residues for leaching

    Leaching of three pesticides (isoproturon, chlorotoluron and triasulfuron) and a tracer (bromide) were determined in four contrasting soils ranging in texture from sandy loam to clay. The compounds were applied to undisturbed columns of soil and four columns for each soil were randomly selected and leached with 24-mm equivalent of water at prescribed time intervals (3, 9, 24, 37 and 57 d after application). A rapid decline in leached loads of isoproturon and chlorotoluron as time from application to irrigation increased was observed in all soils. In contrast, triasulfuron and bromide loads only decreased rapidly in the clay soil. Bromide losses decreased with decreasing clay contents of the soil and therefore with a decrease in structural development. Magnitudes of pesticide losses varied from soil to soil, depending on structural development and the organic carbon content. Pesticide degradation experiments on disturbed and undisturbed soil samples showed that the rapid decline of leached loads with time was faster than could be explained by degradation alone. Five physico-chemical processes are put forward to explain the different patterns of pesticide leached loads observed in the soils: (1) relative extent of preferential flow, (2) sorption capacity of the compounds to the different soils, (3) extent of degradation of the compounds in the soil, (4) variation in sorption kinetics between compounds associated with pesticide diffusion into soil aggregates, and (5) protection of the compounds by a combination of intra-aggregate diffusion and the presence of preferential flow pathways

  16. Multiresidue analytical procedures for pesticides residues in vegetable products; Metodi mutiresiduo per l`analisi di residui di antiparassitari in prodotti vegetali

    Gruppo di lavoro per i residui di antiparassitari della Commissione permanente di coordinamento interregionale per i problemi relativi al controllo ufficiale dei prodotti alimentari

    1997-09-01

    Multiresidue methods for pesticide residues in vegetable products, most frequently used by laboratories of the Italian national health service, by the regional and provincial agencies for environmental protection and by the National health institute. The analytical behaviour is presented for 249 pesticides through the different steps of extraction and cleanup, along with data for the gas chromatography (GC), gas chromatography coupled to mass spectrometry (GC/MS) and high performance liquid chromatography coupled to spectrophotometric detector (HPL/UV).

  17. Evaluation of Quechers Sample Preparation and GC Mass Spectrometry Method for the Determination of 15 Pesticide Residues in Tomatoes Used in Salad Production Plants

    JAHANMARD, Elham; ANSARI, Fatemeh; Mansour FEIZI

    2016-01-01

    Background: The present study was the first attempt for determination and measurement of pesticide residues in tomatoes used in salad production plants in Isfahan, central Iran. Methods: A multiresidue method based on modified QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation, followed by Gas Chromatography Mass Spectrometry (GC–MS) was developed and validated for the determination of 15 pesticides (permethrin, primicarb, dichlorvos, diazinone, fenpropathrin, carbar...

  18. Analysis of Endocrine Disrupting Pesticides by Capillary GC with Mass Spectrometric Detection

    Svetlana Hrouzková

    2012-09-01

    Full Text Available Endocrine disrupting chemicals, among them many pesticides, alter the normal functioning of the endocrine system of both wildlife and humans at very low concentration levels. Therefore, the importance of method development for their analysis in food and the environment is increasing. This also covers contributions in the field of ultra-trace analysis of multicomponent mixtures of organic pollutants in complex matrices. With this fact conventional capillary gas chromatography (CGC and fast CGC with mass spectrometric detection (MS has acquired a real importance in the analysis of endocrine disrupting pesticide (EDP residues. This paper provides an overview of GC methods, including sample preparation steps, for analysis of EDPs in a variety of matrices at ultra-trace concentration levels. Emphasis is put on separation method, mode of MS detection and ionization and obtained limits of detection and quantification. Analysis time is one of the most important aspects that should be considered in the choice of analytical methods for routine analysis. Therefore, the benefits of developed fast GC methods are important.

  19. Residual stress analysis in thick uranium films

    Residual stress analysis was performed on thick, 1-25 μm, depleted uranium (DU) films deposited on an Al substrate by magnetron sputtering. Two distinct characterization techniques were used to measure substrate curvature before and after deposition. Stress evaluation was performed using the Benabdi/Roche equation, which is based on beam theory of a bi-layer material. The residual stress evolution was studied as a function of coating thickness and applied negative bias voltage (0, -200, -300 V). The stresses developed were always compressive; however, increasing the coating thickness and applying a bias voltage presented a trend towards more tensile stresses and thus an overall reduction of residual stresses

  20. Residual stress analysis in thick uranium films

    Hodge, A. M.; Foreman, R. J.; Gallegos, G. F.

    2005-06-01

    Residual stress analysis was performed on thick, 1-25 μm, depleted uranium (DU) films deposited on an Al substrate by magnetron sputtering. Two distinct characterization techniques were used to measure substrate curvature before and after deposition. Stress evaluation was performed using the Benabdi/Roche equation, which is based on beam theory of a bi-layer material. The residual stress evolution was studied as a function of coating thickness and applied negative bias voltage (0, -200, -300 V). The stresses developed were always compressive; however, increasing the coating thickness and applying a bias voltage presented a trend towards more tensile stresses and thus an overall reduction of residual stresses.

  1. Study on diminution of pesticide residues in citrus fruits by {gamma}-irradiation

    Yang, Hee Sun; Park, Yong Dae; Jin, Chang Hyun; Choi, Dae Seong; Jeong, Il Yun [Korea Atomic Energy Research Institte, Jeongeup (Korea, Republic of)

    2009-03-15

    The citrus fruits were irradiated at different doses(25 {approx} 200 kGy) to remove pesticides such as diuron, dichlorbenil, trifluralin, chlorothalonil, fenitrothion, bromacil, phenthoate and norflurazon, and the rates of degradation were detected by using gas chromatography electron capture detector (GC-ECD). The limit of detection (LOD) was in the range of 0.007 {approx} 0.105ppm. The limit of quantification (LOQ) was in the range of 0.024 {approx} 0.352 ppm, and the recoveries of 9 pesticides were in the range of 71.5 {approx} 106.5%. The results demonstrated that the {gamma}-irradiation was effective method to remove pesticides such as diuron, dichlorbenil, trifluralin, dimetoate, chlorothalonil, fenitrothion, and norflurazon. However, the bromacil and phenthoate showed lower removal rates in the rate of 40.5 and 54.8%, respectively, at 200 kGy irradiation.

  2. Study on diminution of pesticide residues in citrus fruits by ?-irradiation

    The citrus fruits were irradiated at different doses(25 ? 200 kGy) to remove pesticides such as diuron, dichlorbenil, trifluralin, chlorothalonil, fenitrothion, bromacil, phenthoate and norflurazon, and the rates of degradation were detected by using gas chromatography electron capture detector (GC-ECD). The limit of detection (LOD) was in the range of 0.007 ? 0.105ppm. The limit of quantification (LOQ) was in the range of 0.024 ? 0.352 ppm, and the recoveries of 9 pesticides were in the range of 71.5 ? 106.5%. The results demonstrated that the ?-irradiation was effective method to remove pesticides such as diuron, dichlorbenil, trifluralin, dimetoate, chlorothalonil, fenitrothion, and norflurazon. However, the bromacil and phenthoate showed lower removal rates in the rate of 40.5 and 54.8%, respectively, at 200 kGy irradiation

  3. Scientific support for preparing an EU position in the 46th Session of the Codex Committee on Pesticide Residues (CCPR

    European Food Safety Authority

    2014-07-01

    Full Text Available In accordance with Article 43 of Regulation (EC No 396/2005, EFSA received a request from the European Commission to provide support for the preparation of the EU position for 46th session of the Codex Committee on Pesticide Residues (CCPR. In 2013, JMPR evaluated 10 active substances regarding the setting of toxicological reference values to be used in consumer risk assessment (diquat, chlorfenapyr, picoxystrobin, benzovindiflupyr, bixafen, fenamidone, fluesulfone, isoxaflutole, tolfenpyrad, and trinexapac and 31 active substances regarding the setting of Maximum Residue Limits (MRLs (diquat, malathion, chlorpyrifos methyl, triazophos, glyphosate, propiconazole, bentazone, dithianon, fenpyroximate, fenbuconazole, flutriafol, cyprodinil, fludioxonil, indoxocarb, difenoconazole, pyrimethanil, azoxystrobin, chlorantraniliprole, mandipropamid, spirotetramate, cyproconazole, dicamba, sulfoxaflor, penthiopyrad, cyantraniliprole, imazapic, imazapyr, isoxaflutole, tolfenpyrad and trinexapac.

  4. Scientific support for preparing an EU position for the 45th Session of the Codex Committee on Pesticide Residues (CCPR

    European Food Safety Authority

    2013-07-01

    Full Text Available In accordance with Article 43 of Regulation (EC No 396/2005, EFSA received a request from the European Commission to provide support for the preparation of the EU position for the 45th session of the Codex Committee on Pesticide Residues (CCPR. In 2012, JMPR evaluated 12 active substances regarding the setting of toxicological reference values to be used in consumer risk assessment, 7 new compounds (ametoctradin, chlorfenapyr, dinotefuran, fluxapyroxad, MCPA, picoxystrobin, sedaxane and 4 part of periodic reevaluation (benzoate, fenpropathrin, fenvalerate, glufosinate-ammonium. Regarding the setting of Maximum Residue Limits (CXLs, JMPR assessed 26 substances (ametoctradin, azoxystrobin, buprofezin, carbofuran, chlorfenapyr, chlorothalonil, cycloxydim, cyfluthrin, cyromazine, dichlorvos, dicofol, dinotefuran, fenvalerate, fludioxonil, fluopyram, fluxapyroxad, glufosinate-ammonium, imidacloprid, MCPA, methoxyfenozide, penthiopyrad, phorate, picoxystrobin, sedaxane, spinetoram and trifloxystrobin. EFSA derived comments on the JMPR evaluations regarding the acceptability of the proposed draft Codex MRLs and the toxicological reference values.

  5. Search of Organochlorine Pesticide Residues (Pocs in Bodies of Water in Cotton-Growing Area of Benin by GC-ECD

    *M. A. N. Gbaguidi

    2014-06-01

    Full Text Available Despite their incontestable services in agriculture, the use of pesticides is not without consequences on the environment. So, in an attempt to access the impacts of pesticides usage in agriculture in Benin, research of some residual organochloride pesticides have been conducted both in rainy and dry seasons in two cotton growing areas: the northern and central part of Benin. The analytical technique used is GC-ECD. During the dry season we notice that the DDT and its metabolites (DDE and DDD represent 36% of all organochlorine pesticides (POCs against 64 % of cyclodiens. Endosulfan comes first representing 57% of all organochlorine pesticides (POCs, then follows DDT with 17 %. During the rainy season these two types of organochlorine pesticides (POCs represent 73% for cyclodiens and 23% for DDT and its by-products. Endosulfan comes first by representing 47% of all organochlorine pesticides (POCs followed by DDT representing 12%. In the sediments and regardless of the season, the cyclodiens come first by representing 70% of all organochlorine pesticides (POCs and then follows the DDT and its by-products which represent 30%. Since in the water column, the sediments are more contaminated in rainy season than in dry season (25273 ppb of all organochlorine pesticide (POCs in rainy season against 2.256 ppb in dry season, it is derived from this study that northern areas are more contaminated than the central areas. Also a strong correlation has been established between the content of different moleculars of organochlorine pesticide (POCs. This means that the famers still use prohibited pesticides in the two areas despite existing laws like “Stockholm convention” which strictly ban the usage of those moleculars.

  6. Search of Organochlorine Pesticide Residues (Pocs in Bodies of Water in Cotton-Growing Area of Benin by GC-ECD

    M. A. N. Gbaguidi

    2014-06-01

    Full Text Available Despite their incontestable services in agriculture, the use of pesticides is not without consequences on the environment. So, in an attempt to access the impacts of pesticides usage in agriculture in Benin, research of some residual organochloride pesticides have been conducted both in rainy and dry seasons in two cotton growing areas: the northern and central part of Benin. The analytical technique used is GC-ECD. During the dry season we notice that the DDT and its metabolites (DDE and DDD represent 36% of all organochlorine pesticides (POCs against 64 % of cyclodiens. Endosulfan comes first representing 57% of all organochlorine pesticides (POCs, then follows DDT with 17 %. During the rainy season these two types of organochlorine pesticides (POCs represent 73% for cyclodiens and 23% for DDT and its by-products. Endosulfan comes first by representing 47% of all organochlorine pesticides (POCs followed by DDT representing 12%. In the sediments and regardless of the season, the cyclodiens come first by representing 70% of all organochlorine pesticides (POCs and then follows the DDT and its by-products which represent 30%. Since in the water column, the sediments are more contaminated in rainy season than in dry season (25273 ppb of all organochlorine pesticide (POCs in rainy season against 2.256 ppb in dry season, it is derived from this study that northern areas are more contaminated than the central areas. Also a strong correlation has been established between the content of different moleculars of organochlorine pesticide (POCs. This means that the famers still use prohibited pesticides in the two areas despite existing laws like Stockholm convention which strictly ban the usage of those moleculars.

  7. Organochlorine pesticide residues in different Indian cereals, pulses, spices, vegetables, fruits, milk, butter, Deshi ghee, and edible oils.

    Kaphalia, B S; Takroo, R; Mehrotra, S; Nigam, U; Seth, T D

    1990-01-01

    A total of 244 samples of cereals (wheat flour, rice, and maize), pulses (arhar, moong, gram, lentil, and black gram), spices (turmeric, chili, coriander, and black pepper), vegetables (potato, onion, spinach, cabbage, brinjal, and tomato), fruits (mango, guava, apple, and grape), milk, butter, Deshi ghee, and edible oils (vegetable, mustard, groundnut, and sesame) collected from different cities of Northern Province (Utter Pradesh) were analyzed by gas liquid chromatography for the presence of organochlorine pesticide residues. Residues of hexachlorocyclohexane (HCH) and 2,2-bis(p-chlorophenyl)-1,1,1-trichloroethane (DDT) were detected in about 85% of the total samples of cereals, spices, milk, butter, Deshi ghee, and edible oils analyzed in the present study. However, the residue levels were either very small (less than 0.06 ppm) or not detected at all in pulses, vegetables, and fruits as compared with very high concentrations in wheat flour (4.42 and 0.12 ppm), butter (1.19 and 4.85 ppm), mustard oil (1.26 and 2.42 ppm), Deshi ghee (1.10 and 3.84 ppm), vegetable oil (1.02 and 0.59 ppm), groundnut oil (0.51 and 1.49 ppm), and chili (0.48 and 1.92 ppm). The levels of HCH and DDT residues detected in rice, maize, turmeric, corlander, black pepper, and all the vegetables and fruits were also lower than those found in wheat flour, oil, and fat samples analyzed in the present study. These findings suggest that a restricted and controlled use of such persistent pesticides may be useful for decreasing their contamination levels in different food items. PMID:1698760

  8. Simultaneous multi-determination and transfer of eight pesticide residues from green tea leaves to infusion using gas chromatography.

    Cho, Soon-Kil; Abd El-Aty, A M; Rahman, Md Musfiqur; Choi, Jeong-Heui; Shim, Jae-Han

    2014-12-15

    A method for determining eight pesticide (cyhalothrin, flufenoxuron, fenitrothion, EPN, bifenthrin, difenoconazole, triflumizole, and azoxystrobin) residues in made green tea as well as a tea infusion (under various brewing water temperatures; 60, 80, and 100°C) using gas chromatography (GC) micro-electron capture detector (μECD) was developed and validated. The extraction method adopted the relatively commonly used approach of solid sample hydration, with the green tea hydrated before being extracted through salting out with acetonitrile followed by a cleanup procedure. The analytes were confirmed using GC-coupled to tandem mass spectrometry (GC/MS/MS) with a triple quadrupole. The linearity of the calibration curves yielded determination coefficients (R(2)) >0.995. Recoveries were carried out using blank samples spiked with all analytes at two levels. The results demonstrated that all pesticides were recovered within the range of 77-116% with a relative standard deviation (RSD) ⩽14%. The quantification limits of 0.015-0.03 mg/kg were lower than the maximum residue limits (MRLs) set by the Korea Food and Drug Administration (KFDA) for all analytes (0.05-10mg/kg). The infusion study indicated that cyhalothrin, flufenoxuron, and bifenthrin did not infuse into the tea brew from the made tea. Increases in brewing time resulted in increased transfer of azoxystrobin, fenitrothion, and difenoconazole from the made tea to the brew; however, this was not the case with triflumizole or EPN. We conclude that transfer of pesticides appeared to be dependent on their water solubilities and drinking a cup of tea is recommended to be at a water temperature of 60°C. PMID:25038708

  9. Monitoring of Certain Pesticide Residues and Some Heavy Metals in Fresh Cow`s Milk at Gharbia Governorate, Egypt

    I.N. Nasr

    2007-01-01

    Full Text Available This monitoring study of 40 samples of cow`s milk collected from different locations at Gharbia Governorate during the four different seasons of the years 2005-2006, was conducted to determine the contamination levels of seven pesticide residues including four organophosphorus (chlorpyrifos, diazinon, dimethoate and malathion and three synthetic pyrethroides (cypermethrin, deltamethrin and fenvelerate, as well as five heavy metals (copper, iron, cadmium, zinc and lead. The results showed that there were no contamination with investigated pesticide residues found in all analyzed samples, except for malathion, which was detected in a single sample with a negligible existence (0.018 mg kg-1, by ratio of (0.02% of all samples. In relation to heavy metals detection, data revealed that all milk samples were contaminated with heavy metals all year around. The contamination with heavy metals was generally dominated at summer season. Level of lead was higher than other metals. The mean levels of Cu, Fe, Cd, Zn and Pb were 0.251, 0.607, 0.159, 0.371 and 2.462 mg kg-1, respectively. Cu, Fe and Zn level were under the permissible limits, while the Cd and Pb were exceeded the permissible limits, indicating serious heavy metals pollution in the region.

  10. Monitoring of Certain Pesticide Residues and Some Heavy Metals in Fresh Cow`s Milk at Gharbia Governorate, Egypt

    Nasr, I. N.; Sallam, A. A. A.; Abd El-Khair, A. A.

    This monitoring study of 40 samples of cow's milk collected from different locations at Gharbia Governorate during the four different seasons of the years 2005-2006, was conducted to determine the contamination levels of seven pesticide residues including four organophosphorus (chlorpyrifos, diazinon, dimethoate and malathion) and three synthetic pyrethroides (cypermethrin, deltamethrin and fenvelerate), as well as five heavy metals (copper, iron, cadmium, zinc and lead). The results showed that there were no contamination with investigated pesticide residues found in all analyzed samples, except for malathion, which was detected in a single sample with a negligible existence (0.018 mg kg-1), by ratio of (0.02%) of all samples. In relation to heavy metals detection, data revealed that all milk samples were contaminated with heavy metals all year around. The contamination with heavy metals was generally dominated at summer season. Level of lead was higher than other metals. The mean levels of Cu, Fe, Cd, Zn and Pb were 0.251, 0.607, 0.159, 0.371 and 2.462 mg kg-1, respectively. Cu, Fe and Zn level were under the permissible limits, while the Cd and Pb were exceeded the permissible limits, indicating serious heavy metals pollution in the region.

  11. Studies on organochlorine pesticide residues in human breast milk of primparae mothers from selected areas in the Greater Accra Region

    A study was conducted to determine the types and levels of organochlorine pesticide residuals in the human milk samples of 42 nursing mothers from Ada and Accra. The milk samples were analyzed for 14 different organochlorine pesticides residue (Aldrin, Dieldrin, p,p'-DDT, p,p'-DDE, Endrin, Endrin Aldehyde, Endrin Ketone, Endosulphan sulfate,' Alpha Endosulphan, Gamma-HCH, Delta-HCH, Gamma Chlordane, Heptachlor and Methoxychlor) using Gas chromatography with electron capture detector. The mean concentrations for the organochlorine pesticide residues detected in the human milk samples from Accra are; Gamma-HCH (4.207µg/kg fat), Delta-HCH (13.855µg/kg fat), Heptachlor (11.791µg/kg fat), Aldrin (2.962µg/kg fat), Gamma- Chlordane (1.839µg/kg fat), Alpha-Endosulfan (4.740µg/kg fat), p,p'-DDE (23.367µg/kg fat), Dieldrin (2.407µg/kg fat), p,p'-DDT (3.085µg/kg fat), Endrin (7.669µg/kg fat), Endrin Aldehyde (7.769µg/kg fat), Endosulfan-Sulphate (99.052µg/kg fat), Endrin Ketone (63.846µg/kg fat), and Methoxychlor (20.116µg/kg fat). The mean concentrations of the various organochlorine pesticide residues detected in the human milk samples from Ada are; Gamma-HCH (5.438µg/kg fat), DeIta-HCH (6.728µg/kg fat), Heptachlor (0.682µg/kg fat), Aldrin (2.38µg/kg fat), Gamma- Chlordane (1.304µg/kg fat), Alpha-Endosulfan (2.588µg/kg fat), p,p'-DDE (24.165µg/kg fat), Dieldrin (2.222µg/kg fat), p,p'-DDT (3.468µg/kg fat), Endrin (6.339 µg/kg fat), Endosulfan-Sulphate (63.803)µg/kg fat), Endrin Ketone (11.167)µg/kg fat), and Methoxychlor (0.703µg/kg fat). The mean concentration of Endosulfan Sulfate was (99.052Iµ g/kg fat) was highest for the milk samples from Accra. Gamma chlordane recorded the least mean concentration (1.839 µg/kg fat) in the milk samples from Accra. The mean concentration of Endosulfan sulfate (63.803 µg/kg fat) was still the highest as compared to the other organochlorines analyzed for in the milk samples from Ada. Endrin Aldehyde was not detected in the milk samples from Ada even though it was detected in the milk samples from Accra. p,p'-DDE was recorded in all the individual milk samples from Accra. p,p'-DDE was detected in 90.5% of the milk samples from Ada. Gamma -HCH was detected in 95.2% of the milk samples from Ada. With the exception of the mean concentrations of endosulfan sulfate from Accra and Ada which are 99.052 µg/kg fat and 63.803 µg/kg fat respectively. The mean concentrations of all the other organochlorine pesticides detected were below the internationally recognized maximum residue limit. (author)

  12. FUNGUS INDEX AND RESIDUAL EFFECTS OF PESTICIDES IN ACID AND ALKALINE SOILS

    Soil applied pesticides have profound effects on the population density and diversity of fungi, however, such information is lacking in tropical soils of the Amazon region. Field experiments were implemented at two experimental farms ("El Choclito", "Bello Horizonte”) of Tropical Crop Institute (ICT...

  13. Adaptation of TLC detection method for the determination of pesticide residues in grains

    In this study the retention factor (Rf), relative retention factor (RRf) and minimum detectable quantities (MDQ) of some pesticide active ingredients were determined with various TLC detection methods. The MDQs of the compounds were verified with grain extracts after subjecting them to cleanup procedure with the KL-SX-3 GPC gel chromatograph. The limits of detection (LOD) of compounds were calculated. (author)

  14. Potential transport and degradation of “Aged” pesticide residues in soil

    “Aging” has been shown to affect the sorption-desorption of pesticides in the soil, which in turn can control transport and degradation processes. Aging effects have been characterized by batch sequential extraction methods, in which sorption coefficients (i.e. Kd) are determined for the chemical re...

  15. Organochlorine pesticides residues in feed and muscle of farmed Nile tilapia from Brazilian fish farms.

    Botaro, Daniele; Torres, João Paulo Machado; Malm, Olaf; Rebelo, Mauro Freitas; Henkelmann, Bernhard; Schramm, Karl-Werner

    2011-09-01

    Organochlorine pesticide (OCP) concentrations were determined in fish muscle and feed collected from four different fish farms in Brazil. Nile tilapia from two growth stages, juveniles and adults, collected at two intensive tanks farms (IT1 and IT2) and two net cage farms (NC1 and NC2), were analyzed by High Resolution Gas Chromatography/High Resolution Mass Spectrometry. Pesticides were detected in almost all samples, but no samples exceeded international maximum limits for safe fish consumption. ΣDDT was the predominant pesticide in fish muscle, found in all fish samples, and endosulfan was the most predominant pesticide in feed, found in all feed samples. No significant correlation (p>0.05) was observed between the different growth stages and OCP concentrations, although slightly higher OCP concentrations were observed in adults. Among the rearing systems, NC farmed fish presented higher lipid levels and, consequently, higher OCP concentrations than fish from IT farms. Some OCPs (ΣHCH, aldrin, dieldrin and endrin) presented strong positive correlations (pcontaminants found in most of the feed samples may explain the low contaminant levels in fish tissue. PMID:21664942

  16. DETERMINATION OF PESTICIDE RESIDUES IN BIOLOGICAL EXTRACTS BY RETENTION TIME LOCKING CAPILLARY GAS CHROMATOGRAPHY MASS SPECTROMETRY

    The widespread use of pesticides in agricultural and urban areas (golf course and residential lawn applications) is largely responsible for the presence of these compounds in many water bodies. Transported by storm-waters, irrigation runoffs, wind, and treated and untreated sewag...

  17. Assessment of organochlorine pesticide residues in Atlantic Rain Forest fragments, Rio de Janeiro, Brazil

    Soares Quinete, Natalia, E-mail: nataliaquinete@yahoo.com.br [Instituto Nacional de Tecnologia, Departamento de Quimica Analitica, Laboratorio de Quimica Analitica e Metrologia em Quimica, Av. Venezuela, 82 - Rio de Janeiro, RJ 20081-312 (Brazil); Santos de Oliveira, Elba dos [Instituto Nacional de Tecnologia, Departamento de Energia, Av. Venezuela, 82 - Rio de Janeiro, RJ 20081-312 (Brazil); Fernandes, Daniella R. [Universidade Federal do Rio de Janeiro, Instituto de Quimica, Departamento de Quimica Analitica, CT - Bloco A, Cidade Universitaria, 21941-909 - Rio de Janeiro (Brazil); Souza Avelar, Andre de [Universidade Federal do Rio de Janeiro, Departamento de Geografia, Instituto de Geociencias, CCMN, Bloco F, Cidade Universitaria, 21941-919 - Rio de Janeiro (Brazil); Erthal Santelli, Ricardo [Universidade Federal do Rio de Janeiro, Instituto de Quimica, Departamento de Quimica Analitica, CT - Bloco A, Cidade Universitaria, 21941-909 - Rio de Janeiro (Brazil)

    2011-12-15

    A superficial water quality survey in a watershed of the Paraiba do Sul River, the main water supply for the most populated cities of southeastern Brazil, was held in order to assess the impact of the expansion of agricultural activity in the near border of the Atlantic Rain Forest. The aim of this study was to investigate the presence of priority organochlorine pollutants in soils and superficial waters of Atlantic rainforest fragments in Teresopolis, Rio de Janeiro State. Soil sample preparations were compared by using ultrasound, microwave assisted extraction and Soxhlet extraction. Recoveries of matrix spiked samples ranged from 70 to 130%. Analysis of a certified soil material showed recoveries ranging from 71 to 234%. Although low concentrations of organochlorine residues were found in water and soil samples, this area is of environmental importance and concern, thus demanding a monitoring program of its compartments. - Highlights: > The organochlorine pollutants occurrence in the Atlantic Rain Forest was investigated. > PARNASO was considered a control area of environmental quality. > Extractions methods were compared for typical C-rich soils samples from Brazil. > Low concentrations of organochlorine residues were found in water and soil samples. > A monitoring program is demanded due to the environmental importance of the area. - The occurrence of organochlorine pollutants in soils of the Atlantic rainforest fragments in Rio de Janeiro, Brazil demands a monitoring program of its compartments.

  18. Assessment of organochlorine pesticide residues in Atlantic Rain Forest fragments, Rio de Janeiro, Brazil

    A superficial water quality survey in a watershed of the Paraiba do Sul River, the main water supply for the most populated cities of southeastern Brazil, was held in order to assess the impact of the expansion of agricultural activity in the near border of the Atlantic Rain Forest. The aim of this study was to investigate the presence of priority organochlorine pollutants in soils and superficial waters of Atlantic rainforest fragments in Teresopolis, Rio de Janeiro State. Soil sample preparations were compared by using ultrasound, microwave assisted extraction and Soxhlet extraction. Recoveries of matrix spiked samples ranged from 70 to 130%. Analysis of a certified soil material showed recoveries ranging from 71 to 234%. Although low concentrations of organochlorine residues were found in water and soil samples, this area is of environmental importance and concern, thus demanding a monitoring program of its compartments. - Highlights: → The organochlorine pollutants occurrence in the Atlantic Rain Forest was investigated. → PARNASO was considered a control area of environmental quality. → Extractions methods were compared for typical C-rich soils samples from Brazil. → Low concentrations of organochlorine residues were found in water and soil samples. → A monitoring program is demanded due to the environmental importance of the area. - The occurrence of organochlorine pollutants in soils of the Atlantic rainforest fragments in Rio de Janeiro, Brazil demands a monitoring program of its compartments.

  19. Organochlorine pesticide residues in sardinella aurita from the coastal waters of Accra-Tema, Ghana and their potential health risks

    Sardinella aurita and seawater samples from the Accra-Tema coast of Ghana were analysed for organochlorine (OC) pesticides using gas chromatography (GC) with electron capture detection (ECD). Residues of DDTs (p,p'-DDT, p'p'-DDE,p,p'-DDD), hexachlorocyclohexane (HCHs - α-HCH, β-HCH and γ-HCH), endosulfan (α-endosulfan, β-endosulfan, endosulfan sulphate) and heptachlor were detected in fish at average concentrations ranging from 3.0 to 1235.0 μg/kg wet wt. These residues were, however, below the detection limit in seawater samples. Significant differences (p < 0.05) in residue levels were also observed across sites, decreasing from Chorkor to Kpone for seven (7) of the residues that were detected in S. aurita. Evaluation of hazard ratios (HRs) and the health risk associated with OC exposure from consumption of sardinellas revealed a probability of adverse health effect due to p,p'-DDT, γ-HCH and heptachlor. Hence, p,p'-DDT, γ-HCH and heptachlor may be of particular health concern. (au)

  20. Detecting Pesticide Residue by Using Modulating Temperature Over a Single SnO2-Based Gas Sensor

    Zengliang Yu

    2003-09-01

    Full Text Available A new rapid detecting method (called dynamic measurements was reported to detect and distinguish the presence of two pesticide gases in the ambient atmosphere. The method employed only a single SnO2-based gas sensor in a rectangular temperature mode to perform the qualitative analysis of a binary gas mixture (acephate and trichlorphon in air. Polar plots was used for quantitative analysis which the feature extraction was performed by FFT. Experimental results showed that high selectivity of the sensor achieved in the range of 250~3000C and modulating frequency 20mHz, one can easily observe the qualitative difference among the response to pure acephate and trichlorphon gases of the same concentration and to the mixture, and the concentration of pesticide gases can be obtained based on the changes of polar plots.

  1. Pesticide residue concentration in soil following conventional and Low-Input Crop Management in a Mediterranean agro-ecosystem, in Central Greece.

    Karasali, Helen; Marousopoulou, Anna; Machera, Kyriaki

    2016-01-15

    The present study was focused on the comparative evaluation of pesticide residues, determined in soil samples from Kopaida region, Greece before and after the implementation of Low-Input Crop Management (LCM) protocols. LCM has been suggested as an environmental friendly plant protection approach to be applied on crops growing in vulnerable to pollution ecosystems, with special focus on the site specific problems. In the case of the specific pilot area, the vulnerability was mainly related to the pollution of water bodies from agrochemicals attributed to diffuse pollution primarily from herbicides and secondarily from insecticides. A total of sixty-six soil samples, were collected and analyzed during a three-year monitoring study and the results of the determined pesticide residues were considered for the impact evaluation of applied plant protection methodology. The LCM was developed and applied in the main crops growing in the pilot area i.e. cotton, maize and industrial tomato. Herbicides active ingredients such as ethalfluralin, trifluralin, pendimethalin, S-metolachlor and fluometuron were detected in most samples at various concentrations. Ethalfluralin, which was the active ingredient present in the majority of the samples ranged from 0.01 μg g(-1) to 0.26 μg g(-1) soil dry weight. However, the amount of herbicides measured after the implementation of LCM for two cropping periods, was reduced by more than 75% in all cases. The method of analysis was based on the simultaneous extraction of the target compounds by mechanical shaking, followed by liquid chromatography mass spectrometric and gas chromatography electron capture (LC-MS/MS and GC-ECD) analysis. PMID:26406107

  2. FREQUENCY ANALYSIS OF PESTICIDE CONCENTRATIONS FOR RISK ASSESSMENT (FRANCO MODEL)

    This report describes a method for statistically characterizing the occurrence and duration of pesticide concentrations in surface waters receiving runoff from agricultural lands. The characterization bridges the gap between simulated instream pesticide modeling and the risk asse...

  3. 77 FR 15012 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2012-03-14

    ... in the Federal Register for comment on March 10, 2010 (75 FR 11171)(FRL-8810- 8), with a 30 day..., milk, animal tissues, and environmental samples. The extraction methodology has been validated using... analytical methods for analysis of cottonseed, pome fruit, nutmeats, almond hulls, and fruiting...

  4. Multi-residue pesticide analysis (gas chromatography-tandem mass spectrometry detection)-Improvement of the quick, easy, cheap, effective, rugged, and safe method for dried fruits and fat-rich cereals-Benefit and limit of a standardized apple purée calibration (screening).

    Rasche, Claudia; Fournes, Britta; Dirks, Uwe; Speer, Karl

    2015-07-17

    Some steps of the QuEChERS method for the analysis of pesticides with GC-MS/MS in cereals and dried fruits were improved or simplified. For the latter, a mixing vessel with stator-rotor-system proved to be advantageous. The extraction procedure of dried fruits is much easier and safer than the Ultra Turrax and results in excellent validation data at a concentration level of 0.01mg/kg (116 of 118 analytes with recoveries in the range of 70-120%, 117 of 118 analytes with RSD 7%), predominantly organochlorines showed recoveries of pepper, sour cherries, dried apples, black currant powder, raisins, wheat flour, rolled oats, wheat germ). The analyte protectants leveled the differences in the matrix-induced protection effect of the analyzed extracts over a wide range. The majority of the pesticides were analyzed with good analytical results (recoveries in the range of 70-120% and RSD <20%). PMID:26044382

  5. Terminal residues of the organophosphorus pesticides, malathion and dimethoate, in tea

    A study on the fate of 14C malathion and 14C dimethoate applied under field conditions to tea was made. The aqueous infusion of tea extracted ca. 50% of the total radioactivity of either pesticide. In the case of malathion this activity was mainly due to the presence of the parent compound and its oxygen analogue while dimethoate was metabolized to a considerable extent and the oxygen analogue was the major component found. (author)

  6. Interpretation of data on pesticide residues in surface water in France, by grouping data within homogeneous spatial units

    Gauroy C.

    2011-02-01

    Full Text Available In France, the SOeS? manages a database which contains more than eight million analyses of pesticide concentrations in surface water. In order to interpret these analyses better, we tested methods based on a geographic grouping of data within homogeneous units, the hydro-ecoregions (HER. Our objectives were to find suitable descriptors and methods, and test them in order to describe the contamination and highlight explanatory factors. In the case of the examples studied, calculating the 90th percentile of analysis results for each 15-day period allowed us to identify the seasonal and inter-annual contamination patterns associated with the analytes. We observed differences between regions and years, which are consistent with the agricultural use of pesticides (application period and registration. Moreover, differences in contamination levels between areas and products can be partly explained by the type of crop on which the products are applied.

  7. Organophosphate Pesticide Residues in Okra and Brinjal Grown in Peri-Urban Environment of Big Cities of Punjab

    Peri urban farming system is main supplier of vegetables to urban population and organophosphate pesticides exposure due to consumption of okra and brinjal to urban population has been estimated in this study. Okra and brinjal samples (90 samples for each vegetable) were collected from peri-urban farming area of Faisalabad, Multan and Gujranwala and were analysed by GC-ECD for quantification of chlorpyrifos, profenophos and triazophos residues. Data were statistically analyzed to calculate, mean and standard deviation. Quantification of pesticides residues revealed that 85 (47.22 percentage) samples were contaminated and 15 (8.33 percentage of total samples and 17.64 percentage of contaminated) samples showed residues value higher than MRL'S. Out of 85 contaminated samples 27 (31.76 percentage) samples were contaminated with chlorpyrifos, 30 (35.29 percentage) samples with profenofos and 29 (34.11) were contaminated with triazophos. The mean concentration of chlorpyrifos in okra was 0.192 mg Kg-1 and brinjal 0.197 mg Kg-1. The mean concentration for profenofos in okra was 0.02 mg Kg-1 and brinjal 0.035 mg Kg-1. Similarly mean concentration for triazophos in okra was 0.009 mg Kg-1 and brinjal 0.01 mg Kg-1. Overall, 6.67 percentage samples of okra and 6.66 percentage samples of brinjal contaminated with chlorpyrifos exceeded EU MRL of 0.05 mg kg-1. Okra samples were found contaminated at frequency of 4.44 percentage and brinjal samples at frequency of 5.56 percentage with higher profenofos residues level than MRL of 0.05 mg kg-1. Approximately, 6.67 percentage samples of okra and 5.6 percentage samples of brinjal had profenofos residue level above MRL of 0.01 mg kg-1. This study may be helpful for building database regarding regional exposure of urban population and facilitate in estimation of possible risk to their health in our daily life. (author)

  8. Assessment of health risk from organochlorine pesticides residues in high-fat spreadable foods produced in Poland.

    Witczak, Agata; Abdel-Gawad, Hassan

    2014-01-01

    Currently, butter and margarine are food products attracting wide customer interest. Every day, consumers around the world buy these products for human consumption. Butter is obtained from milk fat, while margarine is derived from vegetable oils. The content of organochlorine pesticide (OCP) residues was examined in both types of these high fatty products. A gas chromatograph with MSD (HP 5973) detector was used for the determination of pesticides such as α-HCH, β-HCH, γ-HCH, DDT, DDD, DDE, aldrin, dieldrin, endrin, heptachlor and heptachlor epoxide. The examined products had diverse concentrations of the analyzed compounds. Visible was the division based on the origin of the product, which might be composed of animal or vegetable fats. The research has revealed the presence of OCP residues in all examined spreads. Quantities of organochlorine compounds did not pose an immediate danger to the consumers' health. Human and environmental health risk assessment was carried out by the estimation of lifetime average daily dose (LADD) and non-carcinogenic health hazard quotient (HQ). Total estimated LADD ranged between 1.3 × 10(-5) and 3.1 × 10(-5) mg kg(-1) d(-1) for butter, and 1.9 × 10(-6) and 4.6 × 10(-6) mg kg(-1) d(-1) for margarine and mix spread. The HQ ranged between 1.1 × 10(-4) and 3.7 × 10(-4) for butter, and 1.4 × 10(-5) and 9.0 × 10(-6) for margarine and mix spread for adults. These estimated HQs were within the safe acceptable limits, indicating a negligible risk to the residents of the study area. PMID:25310807

  9. Lead, cadmium and organochlorine pesticide residues in hunted red deer and wild boar from northern Italy.

    Chiari, Mario; Cortinovis, Cristina; Bertoletti, Marco; Alborali, Loris; Zanoni, Mariagrazia; Ferretti, Enrica; Caloni, Francesca

    2015-01-01

    The objectives of the present study were to assess heavy metal cadmium (Cd), lead (Pb) and organochlorine pesticide concentrations in tissues of red deer (Cervus elaphus) and wild boar (Sus scrofa) from nine hunting areas and to evaluate related risk factors for the host animal. Over a period of 2 years, a total of 1055 and 210 masseters, 424 and 201 livers, 642 and 152 kidneys were collected from wild boar and red deer, respectively, and concentrations of Cd, Pb and organochlorine pesticides were determined. Comparing the two species, Cd concentration in the kidney (3.72 mg/kg), liver (0.67 mg/kg) and muscle (0.02 mg/kg) of wild boar was found to be significantly higher than in the organs of red deer (1.02 mg/kg in the kidneys, 0.07 mg/kg in the liver and 0.006 mg/kg in muscle). Mean Pb concentrations were found to be similar in both animals, with 0.39, 0.52 and 2.60 mg/kg detected in the wild boar kidney, liver and muscle, respectively, and 0.24, 0.21 and 2.04 mg/kg in the respective organs of the red deer. No difference in concentrations were found based on age class, location of tissue sample or contaminant in the case of wild boar. By contrast, a significantly lower Cd concentration was found in the kidney of the young red deer. The search for organochlorine pesticides in both red deer and wild boar produced negative results with values below the limits of detection. Due to the high levels of renal Cd and muscle Pb detected in wild boar and red deer, further research needs to be carried out in an effort to identify the source of contamination and preserve the health of animals and humans. PMID:26365428

  10. Persistence of pesticide residues in Brazilian soil samples related to organic matter and microbiological activity

    Studies on the fate of the pesticides lindane, parathion, malathion and carbaryl in two Brazilian soils, one rich (Soil 1), the other poor (Soil 2) in organic matter were made in the laboratory by using gas chromatography and radiometric techniques. In order of decreasing persistence were lindane, parathion and malathion. Lindane was lost faster from Soil 2 than from Soil 1, but malathion was lost more slowly from Soil 2 than Soil 1. Parathion degraded faster to 14CO2 in the soil richer in organic matter. Carbaryl was more completely extracted from autoclaved soils than from non-autoclaved soils. (author)

  11. Report on repetition analyses for pesticide residues: 1988-1995; Rapporto sulle revisioni di analisi per residui di antiparassitari-1995

    Di Muccio, A.; Attard Barbini, D.; De Merulis, G.; Vergori, L.; Girolimetti, S.; Sernicola, L.; Dommarco, R. [Ist. Superiore di Sanita`, Rome (Italy). Lab. di Tossicologia Applicata

    1995-12-01

    From 1988 to 1995, 1,254 analyses were carried out on samples of fruits (61%), vegetables (29%), cereals and derived products (3%). The analyses were for 80 different pesticides, of which 51% were fungicides, 31% insecticides, 8% diphenylamine and ethoxiquin (post-harvest antioxidans agents for protection of fruits), and 5% antigermogliants and herbicides. Regions that mostly contributed with samples were: Emilia-Romagna (35%), Piedmont (15%), Liguria (11%), Tuscany (10%). Global rate of confirmation between first analysis and repetition analysis was 64% for all the samples analysed.

  12. High-throughput simultaneous analysis of pesticides by supercritical fluid chromatography coupled with high-resolution mass spectrometry.

    Ishibashi, Megumi; Izumi, Yoshihiro; Sakai, Miho; Ando, Takashi; Fukusaki, Eiichiro; Bamba, Takeshi

    2015-05-13

    Recently, a generally applicable screening method for multiresidue pesticide analysis, which is simple, quick, and accurate and has a reliable performance, is becoming increasingly important for food safety and international trade. This paper proposes a high-throughput screening methodology that enables the detection of multiresidue pesticides using supercritical fluid chromatography coupled to a high-performance benchtop quadrupole Orbitrap mass spectrometry (SFC/Q Exactive) and an automated library-based detection. A total of 444 chemicals covering a wide polarity range (logPow from -4.2 to 7.7) and a wide molecular weight range (from 99.0 to 872.5) were analyzed simultaneously through a combination of high mass resolution (a value of m/?m = 70000), high mass accuracy (SFC. A total of 373 pesticides were detected in QuEChERS spinach extracts without dispersive solid phase extraction at the 10 ?g kg(-1) level (provisional maximum residue limits in Japan). In conclusion, the developed analytical system is a potentially useful tool for practical multiresidue pesticide screening with high throughput (time for data acquisition, 72 samples per day; and time for data processing of 72 samples, approximately 45 min). PMID:25547162

  13. Residual gas analysis in ISX-A

    A computer-controlled mass analyzer was utilized to observe the residual gases in the ISX-A tokamak. This residual gas analysis (RGA) system enabled time resolved measurements of preselected m/e peak heights to be made during and after tokamak discharges. Routine mass scans were also made and displayed in the form of semilogarithmic plots of partial pressure (torr) versus m/e. Wall conditioning of the stainless steel torus consisted of hydrogen discharge cleaning and titanium gettering, which ultimately produced gage pressures on the order of 10-8 and 10-9 torr, respectively. The dominant plasma impurities, carbon and oxygen, were observed by the RGA as light hydrocarbons and water vapor. Entrapment of deuterium by the walls was investigated by monitoring the residual D2 content after the working gas was changed to H2. The effective nuclear charge (Z/sub eff/) was found to be proportional to the residual contaminants measured by the RGA immediately following a discharge

  14. A Comparative Analysis of Pesticides Production, Consumption, and Foreign Trade

    Koltsov, A.

    1990-01-01

    The production, consumption and foreign trade of pesticides are important sectors of the chemical industry in particular, and of the national economy as a whole. The pesticides sector has a positive impact on increasing crop yields and a negative effect on the environment as a pollutant hazardous to plants, humans, etc. To analyze the place and role of pesticides in the national economy, we gathered a large amount of data from sources including national and international statistical yearbooks...

  15. QuEChERS GC-MS validation and monitoring of pesticide residues in different foods in the tomato classification group.

    Ramírez Restrepo, Andrés; Gallo Ortiz, Andrés Fernando; Hoyos Ossa, Duvan Esteban; Peñuela Mesa, Gustavo Antonio

    2014-09-01

    The objective of this study was to validate (SANCO/12495/2011 and NTC-ISO/IEC 17025) multi-residue multi-class methods using QuEChERS sample preparation and GC-MS for the analysis of regulated pesticides in tomatoes (Solanum lycopersicum), tamarillos (Solanum betaceum) and goldenberries (Physalis peruviana). These Latin American products are representative and widely produced in Antioquia (Colombia). Sample preparation followed the UNE-EN 15662 method (150 mg MgSO4, 25mg primary secondary amines and 25mg of octadecylsiloxane for cleanup; graphitized carbon black was added for tomatoes). Extracts were injected using a programmed temperature-vaporizing injector. The residues were validated over a range from 0.02 mg/kg to 0.20 mg/kg, with 24 analytes validated in tomatoes, 33 in tamarillos and 28 in goldenberries. An initial risk assessment was enabled by monitoring 24 samples in the municipalities of El Peñol, Marinilla and San Vicente Ferrer. Risks were found for tomatoes, but no significant risks were found for tamarillos or goldenberries. PMID:24731326

  16. Predicting pesticide removal efficacy of vegetated filter strips: A meta-regression analysis.

    Chen, Huajin; Grieneisen, Michael L; Zhang, Minghua

    2016-04-01

    Vegetated Filter Strips (VFS's) are widely used for alleviating agricultural pesticide loadings to surface water bodies. However, effective tools are lacking to quantify the performance of VFS's in reducing off-site pesticide transport. In this study, we applied meta-regression to develop a model for predicting VFS pesticide retention efficiency based on hydrologic responses of VFS's, incoming pollutant characteristics and the interaction within and between these two factor groups (R(2)=0.83). In cross-validation analysis, our model (Q(2)=0.81) outperformed the existing pesticide retention module of VFSMOD (Q(2)=0.72) by explicitly accounting for interaction effect and the categorical effect of pesticide adsorption properties. Based on the 181 data points studied, infiltration had a leading, positive influence on pesticide retention, followed by sedimentation and interaction between the two. Interaction between infiltration and pesticide adsorption properties was also prominent, as the influence of infiltration was significantly lower for strongly adsorbed pesticides. In addition, the clay content of incoming sediment was negatively associated with pesticide retention. Our model is not only valuable in predicting VFS performance, but also provides a quantitative characterization of the interacting VFS processes, thereby facilitating a deeper understanding of the underlying mechanisms. PMID:26802340

  17. Genotoxicity of chlororganic pesticides

    In Kazakhstan there are the warehouses of the obsolete pesticides and their container which should be buried in special burial grounds or neutralized to minimize dangerous genetic and ecological risks. The results of two yr of research were identification of substances stored in 64 former warehouses of pesticides. 64 former warehouses (in the 10 areas of Almaty oblast) are on distance of 250 km from a large city of Almaty (the former capital of Kazakhstan). A total of 352,6 ton of obsolete pesticides and 250 ton of their container were disposed. We determined the residues of DDT metabolites (dichlorodiphenyltrichloroethane) and HCH isomers (hexachlorocyclohexane) in soil around pesticides warehouses where their concentrations exceed MAC (maximum concentration limit) in tens - hundreds times. To analyze a genotoxicity of chlororganic pesticides we used their concentrations that were found in soil from former warehouses. The analysis of structural mutations of chromosomes was carried out by metaphase method in I mitoses meristem cells of barley seeds (Hordeum vulgare L.). It was ascertained that HCH isomers and DDT metabolites have genotoxic effect exceeding spontaneous mutation in 5-7 times. High contaminations by pesticides on soil around of warehouses and their ability to induce chromosome aberrations in plant cells indicate that warehouses are a new centre of contamination by POP's (proof organic pollutants). (author)

  18. Residues, sources and tissue distributions of organochlorine pesticides in dog sharks (Mustelus griseus) from Zhoushan Fishing Ground, China.

    Zhou, Shanshan; Tong, Lu; Tang, Qiaozhi; Gu, Xiaoting; Xue, Bin; Liu, Weiping

    2013-08-15

    Ten dog sharks (Mustelus griseus) collected from Zhoushan Fishing Ground, China, were analysed for organochlorine pesticides in various tissues, including muscle, liver, skin, gill and fin, with the aim to study the residues, sources and tissue distributions of these chemicals in high trophic level marine fishes. The concentrations of DDTs, HCHs, and chlordanes varied from 7.27-26.62, 2.67-3.35, and 0.54-0.61 ng/g wet weight, respectively, with the estimated daily intake far below the acceptable daily intake and Chinese edible hygienic criteria. Data from the tissue distribution suggested a tendency of DDTs and chlordanes to accumulate in the liver, but for HCHs, direct gill penetration may be an important means of entrance. In addition, the compositional profiles indicated that the residues of HCHs and chlordanes mainly originated from the historical usage of these chemicals. However, the predominant maternal compounds and the o,p'-DDT/p,p'-DDT ratios reflected a recent use of dicofol. PMID:23768978

  19. Resíduos de agrotóxicos em frutos de tomate Pesticide residues in tomato fruits

    Leslie Maria Segura Zavatti

    1999-03-01

    Full Text Available O uso intensivo de agrotóxicos em culturas de tomates tem causado preocupações quanto à provável contaminação do produto final. Este trabalho teve como objetivo monitorar, por dois anos consecutivos, em quatro propriedades de uma área altamente tecnificada, o uso de agrotóxicos em tomate irrigado durante seu desenvolvimento, quantificar os resíduos dos principais princípios ativos utilizados, e avaliar o grau de contaminação dos frutos colhidos. Foram analisados metamidofós, clorpirifós, captan, clorotalonil, endosulfan, lambda-cialotrina, e cobre. Para avaliar o grau de contaminação dos frutos foi validado um método de análise de resíduos múltiplos capaz de quantificar esses compostos. Os resíduos encontrados foram de fungicidas e inseticidas aplicados nas fases de frutificação e maturação: captan, 0,35 mg/kg, na Fazenda 2; clorotalonil, 0,16 mg/kg e 0,95 mg/kg, nas Fazendas 1 e 2, respectivamente; lambda-cialotrina, 0,03 mg/kg, na Fazenda 2; cobre, 2,03 mg/kg, 3,75 mg/kg e 1,44mg/kg, nas Fazendas 1, 2 e 3, respectivamente, e 0,95 mg/kg, 1,70 mg/kg e 2,31 mg/kg, na Fazenda 4. Não ocorreram resíduos dos inseticidas organofosforados, aplicados principalmente durante o desenvolvimento vegetativo da cultura. Não houve contaminação dos tomates pelos agrotóxicos analisados. Os resíduos que devem ser monitorados são os dos agrotóxicos aplicados na fase de maturação da cultura.The intensive use of pesticide in tomato crops have been causing concern about a possible contamination of the final product. This work aimed at monitoring, for two years, in four farms located in a high technology area, the use of pesticides in irrigated tomato crops, quantifying the main active ingredient residues and evaluating the contamination level of the fruits. The components analised were: methamidophos, chlorpyrifos, captan, chlorothalonil, endosulfan, lambda-cyhalothrin and copper oxychloride. In order to evaluate the contamination level, a multiresidue method was validated. The residues found were from fungicides and insecticides used during the frutification and maturation stages of the crop: captan, 0.35 mg/kg, at Farm 2; chlorothalonil, 0.16 mg/kg and 0.95 mg/kg, at Farms 1 and 2, respectively; lambda-cyhalothrin, 0.03 mg/kg, at Farm 2; copper, 2.03 mg/kg, 3.75 mg/kg and 1.44 mg/kg, at Farms 1, 2 and 3, respectively, and 0.95 mg/kg, 1.70 mg/kg and 2.31 mg/kg, at Farm 4. Residues of organophosphorous components applied mainly during the vegetative growing were not found. There was no contamination in the tomatos. The residues to be monitored are those from the pesticides used in the crop maturation stage.

  20. Pesticide Flow Analysis to Assess Human Exposure in Greenhouse Flower Production in Colombia

    Claudia R. Binder

    2013-03-01

    Full Text Available Human exposure assessment tools represent a means for understanding human exposure to pesticides in agricultural activities and managing possible health risks. This paper presents a pesticide flow analysis modeling approach developed to assess human exposure to pesticide use in greenhouse flower crops in Colombia, focusing on dermal and inhalation exposure. This approach is based on the material flow analysis methodology. The transfer coefficients were obtained using the whole body dosimetry method for dermal exposure and the button personal inhalable aerosol sampler for inhalation exposure, using the tracer uranine as a pesticide surrogate. The case study was a greenhouse rose farm in the Bogota Plateau in Colombia. The approach was applied to estimate the exposure to pesticides such as mancozeb, carbendazim, propamocarb hydrochloride, fosetyl, carboxin, thiram, dimethomorph and mandipropamide. We found dermal absorption estimations close to the AOEL reference values for the pesticides carbendazim, mancozeb, thiram and mandipropamide during the study period. In addition, high values of dermal exposure were found on the forearms, hands, chest and legs of study participants, indicating weaknesses in the overlapping areas of the personal protective equipment parts. These results show how the material flow analysis methodology can be applied in the field of human exposure for early recognition of the dispersion of pesticides and support the development of measures to improve operational safety during pesticide management. Furthermore, the model makes it possible to identify the status quo of the health risk faced by workers in the study area.