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

    Pujeri, U. S.; A.S.Pujari; S. C. Hiremath; M.S.Yadawe

    2010-01-01

    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 fermentativ...

  4. Fast gas chromatography for pesticide residues analysis using analyte protectants.

    Kirchner, Michal; Húsková, Renáta; Matisová, Eva; Mocák, Ján

    2008-04-01

    Fast GC-MS with narrow-bore columns combined with effective sample preparation technique (QuEChERS method) was used for evaluation of various calibration approaches in pesticide residues analysis. In order to compare the performance of analyte protectants (APs) with matrix-matched standards calibration curves of selected pesticides were searched in terms of linearity of responses, repeatability of measurements and reached limit of quantifications utilizing the following calibration standards in the concentration range 1-500 ng mL(-1)(the equivalent sample concentration 1-500 microg kg(-1)): in neat solvent (acetonitrile) with/without addition of APs, matrix-matched standards with/without addition of APs. For APs results are in a good agreement with matrix-matched standards. To evaluate errors of determination of concentration synthetic samples at concentration level of pesticides 50 ng mL(-1) (50 microg kg(-1)) were analyzed and quantified using the above given standards. For less troublesome pesticides very good estimation of concentration was obtained utilizing APs, while for more troublesome pesticides such as methidathion, malathion, phosalone and deltamethrin significant overestimation reaching up to 80% occurred. According to presented results APs can be advantegously used for "easy" pesticides determination. For "difficult" pesticides an alternative calibration approach is required for samples potentially violating MRLs. An example of real sample measurement is shown. In this paper also the use of internal standards (triphenylphosphate (TPP) and heptachlor (HEPT)) for peak areas normalization is discussed in terms of repeatability of measurements and quantitative data obtained. TPP normalization provided slightly better results than the use of absolute peak areas measurements on the contrary to HEPT. PMID:17920613

  5. A perspective on high throughput analysis of pesticide residues in foods

    Kai ZHANG; Jon W WONG; Perry G WANG

    2011-01-01

    The screening of pesticide residues plays a vital role in food safety. Applications of high throughput analytical procedures are desirable for screening a large number of pesticides and food samples in a time-effi- cient and cost-effective manner. This review discusses how sample throughput of pesticide analysis could be improved with an emphasis on sample preparation, instrumentation and data analysis.

  6. 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.

  7. 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

  8. Statistical Analysis of Regularity of Pesticide Residues in Vegetables Produced in Inner Mongoli

    Fujin ZHANG; Dekun HOU; Jiang HE; Tianyun GAO; Hong LUO; Songyan LANG; Xinxin ZHANG; Yiping YAO

    2013-01-01

    [Objective] The paper was to study regularity of pesticide residues in veg-etables produced in Inner Mongolia. [Method] Mathematical statistic analysis was carried out on 6 800 samples of veggies, fruits, leguminous vegetables, nuts and seeds produced in Inner Mongolia. [Result] The dominated vegetables in Inner Mon-golia were green leafy vegetables, solanaceous vegetables and melon vegetables, and their yields accounted for 70% of the total vegetables production. Since 2003, with the rapid increase of detected vegetable numbers, the status of vegetable qual-ity safety had entered into a new stage of sustainable steady after a rapid decline or periodic fluctuation, and the differences in safety levels were obvious, of which the range of exceeding standard rate of pesticide residues in solanaceous vegeta-bles, melon vegetables and leguminous vegetables (about 55% of the total vegeta-bles) was under 2%, with average values of 1.1%, 1.6% and 3.1%, respectively. They belonged to stable type. The exceeding standard rate of pesticide residues in green leafy vegetables and Chinese cabbage group (about 30% of total vegetables) presented a decreasing trend year by year, wondering in the range of 7%-10%. They belonged to main risk type. The time period of exceeding standard of pesticide residues in root vegetables and cole vegetables was under predictable, and its ex-ceeding standard rate in some years was over 5% (amplitude variation is over 15 percentage points). They belonged to random risk type. The kinds of pesticides, which exceeding standard rate in vegetables were relatively intensive, presented vari-ance in different vegetable species. 70% of the pesticides belonged to intermittent over-limits and the probability was below 5%. About 20% tradition pesticides often exceeded standard and their probabilities were over 30%. The exceeding standard of organophosphorus and carbamates pesticides in vegetables presented a decreasing tend, while the risk of some new pesticides

  9. 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)

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

    Lucía Pareja

    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 flame 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.

  11. 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%.

  12. 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)

  13. 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 ...

  14. Blind Analysis of Fortified Pesticide Residues in Carrot Extracts using GC-MS to Evaluate Qualitative and Quantitative Performance

    Unlike quantitative analysis, the quality of the qualitative results in the analysis of pesticide residues in food are generally ignored in practice. Instead, chemists tend to rely on advanced mass spectrometric techniques and general subjective guidelines or fixed acceptability criteria when makin...

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

    Sheheli Islam; Nazneen Afrin; Hossain, Mohammad S.; Nilufar Nahar; Mohammad Mosihuzzaman; Mohammad I.R. Mamun

    2009-01-01

    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 rep...

  16. 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

  17. 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

  18. QuEChERS sample preparation approach for mass spectrometric analysis of pesticide residues in foods

    This chapter describes an easy, rapid, and low-cost sample preparation approach for the determination of pesticide residues in foods using gas and/or liquid chromatographic (GC and/or LC) analytical separation and mass spectrometric (MS) detection. The approach is known as QuEChERS, which stands fo...

  19. 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 μg 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 μg 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

  20. 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 pesticide residues. This method is suitable for the identification and quantification of systemic pesticides with matrix-matched standards in various baby foods. PMID:24861738

  1. 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)

  2. 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.

  3. Analysis of Bioenergy Residues (biochar and digestate) to Study the Fate of Pesticides for Biopurification Systems

    Mukherjee, S.

    2015-12-01

    To overcome the problem of on farm point sources of pollution, environmental friendly and low cost technology filter systems are under development. Processes like sorption-desorption, dissipation behavior of three radiolabeled pesticides (Bentazone, Boscalid and Pyrimethanil) has been investigated at lab scale. Biochar and digestate mixtures with two types of soil (sandy and silt loam) had been used as a biofilter test material for a respiration study (over three month's time period) instead of conventional soil, peat and straw mixtures. The results show that digestate is an easily available C-source leading to highest release of CO2-C. It was found that with the addition of even a small amount (1 % W/W) of biochar there is a profound suppression in the CO2-C release.The driving mechanism for this suppression can be manifold like negative priming, chemisorption of CO2-C on biochar or combinations of all. Further, the fate of applied organic contaminants to biomixtures depends on factors like soil properties as well as biological degradation by soil microbes. To analyze the degradation potential of the different soil/amendment mixtures on pesticides a degradation study was performed. The results from the 14C labelled pesticides study indicated that a mixture of digestate (5%) and biochar (5%) well balanced the mineralization (~20% for bentazone, ~6% for boscalid and ~2% for pyrimethanil) and sorption process (>85% non-extractable residues for all pesticides) resulting in favorable dissipation process. To investigate the sorption-desorption potential of the above pesticides a batch equilibrium study was carried out with selected biomixtures. A higher Kd (>1500 L kg-1), kf (>400 μM1-1/nf L1/nfkg-1) and KL (>40 L kg-1) was obtained for all pesticides for the soil/digestate/biochar mixtures, which had a higher organic matter content. SUVA254 values justified the aromatic character of digestate (5%) and biochar (5%) mixture which showed highest Koc values among all

  4. Pesticide Residues in Food: Your Daily Dose.

    Mott, Lawrie

    1985-01-01

    Extensive use of pesticides during food production has created concerns for certain involuntary risks. Examines these concerns: government role in control and monitoring pesticide use, proposals for reform, and how consumer awareness might be an effective pressure for finding remedies. A table listing produce and pesticide residues is included.…

  5. Evaluation of gas chromatography - electron ionization - full scan high resolution Orbitrap mass spectrometry for pesticide residue analysis.

    Mol, Hans G J; Tienstra, Marc; Zomer, Paul

    2016-09-01

    Gas chromatography with electron ionization and full scan high resolution mass spectrometry with an Orbitrap mass analyzer (GC-EI-full scan Orbitrap HRMS) was evaluated for residue analysis. Pesticides in fruit and vegetables were taken as an example application. The relevant aspects for GC-MS based residue analysis, including the resolving power (15,000 to 120,000 FWHM at m/z 200), scan rate, dynamic range, selectivity, sensitivity, analyte identification, and utility of existing EI-libraries, are assessed and discussed in detail. The optimum acquisition conditions in full scan mode (m/z 50-500) were a resolving power of 60,000 and an automatic-gain-control target value of 3E6. These conditions provided (i) an optimum mass accuracy: within 2 ppm over a wide concentration range, with/without matrix, enabling the use of ±5 ppm mass extraction windows (ii) adequate scan speed: minimum 12 scans/peak, (iii) an intra-scan dynamic range sufficient to achieve LOD/LOQs ≤0.5 pg in fruit/vegetable matrices (corresponding to ≤0.5 μg kg(-1)) for most pesticides. EI-Orbitrap spectra were consistent over a very wide concentration range (5 orders) with good match values against NIST (EI-quadrupole) spectra. The applicability for quantitative residue analysis was verified by validation of 54 pesticides in three matrices (tomato, leek, orange) at 10 and 50 μg/kg. The method involved a QuEChERS-based extraction with a solvent switch into iso-octane, and 1 μL hot splitless injection into the GC-HRMS system. A recovery between 70 and 120% and a repeatability RSD pesticides could be identified according to the applicable EU criteria for GC-HRMS (SANTE/11945/2015). GC-EI-full scan Orbitrap HRMS was found to be highly suited for quantitative pesticide residue analysis. The potential of qualitative screening to extend the scope makes it an attractive alternative to GC-triple quadrupole MS. PMID:27543025

  6. 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)

  7. 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

  8. 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.

  9. 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%.

  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. 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...

  12. Earthworm tolerance to residual agricultural pesticide contamination

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

    2014-01-01

    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...... of soluble glutathione-S-transferases (sGST) and catalase increased with soil pesticide contamination in A. caliginosa. Pesticide stress was reflected in depletion of energy reserves in A. chlorotica. Acute exposure of pre-adapted and naïve A. caliginosa to pesticides (fungicide Opus ®, 0.1 μg active...

  13. Management of pesticide residues in China

    CHEN Zeng-long; DONG Feng-shou; XU Jun; LIU Xin-gang; ZHENG Yong-quan

    2015-01-01

    This paper reviewed management of pesticide residues in China including laws and regulations, the supervision system, the standard system, and the quality and safety of agricultural products. The process of establishment and international-ization of standards for pesticide residues were also discussed. Results indicate that the progress of the management of pesticide residues has been steadily made in China. However, the folowing aspects which refer to updates to regulations, supervising efifciency, standard system, risk assessment, international cooperation and communication, should be further improved. China should draw lessons from international experience, and then establish its own management system, which focuses on pesticides controls by strictly folowing relevant laws and technical standards to ensure the quality and safety of agricultural products.

  14. Contribution of Sample Processing to Variability and Accuracy of the Results of Pesticide Residue Analysis in Plant Commodities.

    Ambrus, Árpád; Buczkó, Judit; Hamow, Kamirán Á; Juhász, Viktor; Solymosné Majzik, Etelka; Szemánné Dobrik, Henriett; Szitás, Róbert

    2016-08-10

    Significant reduction of concentration of some pesticide residues and substantial increase of the uncertainty of the results derived from the homogenization of sample materials have been reported in scientific papers long ago. Nevertheless, performance of methods is frequently evaluated on the basis of only recovery tests, which exclude sample processing. We studied the effect of sample processing on accuracy and uncertainty of the measured residue values with lettuce, tomato, and maize grain samples applying mixtures of selected pesticides. The results indicate that the method is simple and robust and applicable in any pesticide residue laboratory. The analytes remaining in the final extract are influenced by their physical-chemical properties, the nature of the sample material, the temperature of comminution of sample, and the mass of test portion extracted. Consequently, validation protocols should include testing the effect of sample processing, and the performance of the complete method should be regularly checked within internal quality control. PMID:26755282

  15. [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

  16. 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...

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

    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 QuEChE...

  18. Application of zirconium dioxide nanoparticle sorbent for the clean-up step in post-harvest pesticide residue analysis.

    Uclés, Ana; Herrera López, Sonia; Dolores Hernando, Maria; Rosal, Roberto; Ferrer, Carmen; Fernández-Alba, Amadeo R

    2015-11-01

    The use of yttria-stabilized zirconium dioxide nanoparticles as d-SPE clean-up sorbent for a rapid and sensitive liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) method for the determination of post-harvest fungicides (carbaryl, carbendazim, chlorpropham, diphenylamine, ethoxyquin, flutriafol, imazalil, iprodione, methomyl, myclobutanil, pirimiphos-methyl, prochloraz, pyrimethanil, thiabendazole, thiophanate-methyl and tolclofos-methyl) in orange and pear samples has been evaluated and validated. The sample preparation was a modification of the QuEChERS extraction method using yttria-stabilized zirconium dioxide and multi-walled carbon nanotubes (MWCNTs) nanoparticles as the solid phase extraction (d-SPE) clean-up sorbents prior to injecting the ten-fold diluted extracts into the LC system. By using the yttria-stabilized zirconium dioxide extraction method, more recoveries in the 70-120% range were obtained - thus this method was used for the validation. Quantification was carried out using a matrix-matched calibration curve which was linear in the 1-500 µg kg(-1) range for almost all the pesticides studied. The validated limit of quantification was 10 µg kg(-1) for most of the studied compounds, except chlorpropham, ethoxyquin and thiophanate-methyl. Pesticide recoveries at the 10 and 100 µg kg(-1) concentration levels were satisfactory, with values between 77% and 120% and relative standard deviations (RSD) lower than 10% (n=5). The developed method was applied for the determination of selected fungicides in 20 real orange and pear samples. Four different pesticide residues were detected in 10 of these commodities; 20% of the samples contained pesticide residues at a quantifiable level (equal to or above the LOQs) for at least one pesticide residue. The most frequently-detected pesticide residues were: carbendazim, thiabendazole and imazalil-all were below the MRL. The highest concentration found was imazalil at 1175 µg kg

  19. Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables

    This article describes the comparison of different versions of an easy, rapid, and low-cost sample preparation approach for the determination of pesticide residues in fruits and vegetables by concurrent use of gas and liquid chromatography (GC and LC) coupled to mass spectrometry (MS) for detection....

  20. 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)

  1. 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.

  2. Multiplug filtration clean-up with multiwalled carbon nanotubes in the analysis of pesticide residues using LC-ESI-MS/MS.

    Zhao, Pengyue; Fan, Sufang; Yu, Chuanshan; Zhang, Junyan; Pan, Canping

    2013-10-01

    A novel design for a rapid clean-up method was developed for the analysis of pesticide residues in fruit and vegetables followed by LC-ESI-MS/MS. The acetonitrile-based sample extraction technique was used to obtain the extracts, and further clean-up was carried out by applying the streamlined procedure on a multiplug filtration clean-up column coupled with a syringe. The sorbent used for clean-up in this research is multiwalled carbon nanotubes, which was mixed with anhydrous magnesium sulfate to remove water from the extracts. This method was validated on 40 representative pesticides and apple, cabbage, and potato sample matrices spiked at two concentration levels of 10 and 100 μg/kg. It exhibited recoveries between 71 and 117% for most pesticides with RSDs 0.995 for most studied pesticides between concentration levels of 10-500 μg/L. The LOQs for 40 pesticides ranged from 2 to 50 μg/kg. The developed method was successfully applied to the determination of pesticide residues in market fruit and vegetable samples. PMID:23939876

  3. An Innovative Rapid Method for Analysis of 10 Organophosphorus Pesticide Residues in Wheat by HS-SPME-GC-FPD/MSD.

    Du, Xin; Ren, YongLin; Beckett, Stephen J

    2016-03-01

    The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/PDMS fiber increased with increasing spiking levels, yielding significant (R(2) > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity. PMID:26964527

  4. Monitoring of pesticide residues in vegetarian diet.

    Kumari, Beena; Kathpal, T S

    2009-04-01

    Samples (28) of complete vegetarian diet consumed from morning till night i.e. tea, milk, breakfast, lunch, snacks, dinner, sweet dish etc. were collected from homes, hostels and hotels periodically from Hisar and analysed for detecting the residues of organochlorine, synthetic pyrethriod, organophosphate and carbamate insecticides. The estimation was carried out by using multi-residue analytical technique employing gas chromatograph (GC)-electron capture detector and GC-nitrogen phosphorous detector systems equipped with capillary columns. The whole diet sample was macerated in a mixer grinder and a representative sample in duplicate was analyzed for residues keeping the average daily diet of an adult to be 1,300 g. On comparing the data, it was found that actual daily intake (microgram/person/day) of lindane in two and endosulfan in four samples exceeded the acceptable daily intake. Residues of other pesticides in all the diet samples were lower than the acceptable daily intake (ADI) of the respective pesticides. The study concluded that although all the diet samples were found contaminated with one or the other pesticide, the actual daily intake of only a few pesticides was higher than their respective ADI. More extensive study covering other localities of Haryana has been suggested to know the overall scenario of contamination of vegetarian diet. PMID:18386151

  5. Multi-residue analysis of 26 organochlorine pesticides in Alpinia oxyphylla by GC-ECD after solid phase extraction and acid cleanup.

    Zhao, Xiangsheng; Zhou, Yakui; Kong, Weijun; Gong, Bao; Chen, Deli; Wei, Jianhe; Yang, Meihua

    2016-04-01

    A simple and effective multi-residue method was developed and validated for the analysis of 26 organochlorine pesticide residues in Alpinia oxyphylla by a gas chromatography with an electron capture detector (GC-ECD). The target pesticides were extracted by sonication and cleaned up with florisil solid phase extraction and sulphuric acid. Some crucial parameters, including extraction solvent and time, sorbent type, elute solvent and concentration of sulphuric acid were optimized to improve the performance of sample preparation procedure. The optimized method gave high sensitivity with detection limit ranging from 0.1 to 2.0μg/kg. Matrix-matched calibration was employed for the quantification, and a wide linear range (from 1.0 to 1000μg/kg) with r(2) values ranging from 0.9971 to 0.9998 was obtained. For the majority of the tested pesticides, the average recoveries were in acceptable range (between 70% and 110%) with relative standard deviation values below 15.0%. Matrix effect was evaluated for target compounds through the study of ratio of peak area obtained in the solvent and blank matrix. The proposed method was applied to simultaneously analyze 26 pesticides in 55 batches of Alpinia oxyphylla samples. 3 samples were found to be positive with four pesticides (α-BHC, quintozene, trans-chlordane and op'-DDD), which were confirmed by gas chromatography-mass spectrometry (GC-MS) in selective ion monitoring (SIM) mode. PMID:26990736

  6. 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...

  7. 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.

  8. Validation of a QuEChERS-based gas chromatographic method for analysis of pesticide residues in Cassia angustifolia (senna).

    Tripathy, Vandana; Saha, Ajoy; Patel, Dilipkumar J; Basak, B B; Shah, Paresh G; Kumar, Jitendra

    2016-08-01

    A simple multi-residue method based on modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach was established for the determination of 17 organochlorine (OC), 15 organophosphorous (OP) and 7 synthetic pyrethroid (SP) pesticides in an economically important medicinal plant of India, Senna (Cassia angustifolia), by gas chromatography coupled to electron capture and flame thermionic detectors (GC/ECD/FTD) and confirmation of residues was done on gas chromatograph coupled with mass spectrometry (GC-MS). The developed method was validated by testing the following parameters: linearity, limit of detection (LOD), limit of quantification (LOQ), matrix effect, accuracy-precision and measurement uncertainty; the validation study clearly demonstrated the suitability of the method for its intended application. All pesticides showed good linearity in the range 0.01-1.0 μg mL(-1) for OCs and OPs and 0.05-2.5 μg mL(-1) for SPs with correlation coefficients higher than 0.98. The method gave good recoveries for most of the pesticides (70-120%) with intra-day and inter-day precision < 20% in most of the cases. The limits of detection varied from 0.003 to 0.03 mg kg(-1), and the LOQs were determined as 0.01-0.049 mg kg(-1). The expanded uncertainties were <30%, which was distinctively less than a maximum default value of ±50%. The proposed method was successfully applied to determine pesticide residues in 12 commercial market samples obtained from different locations in India. PMID:27153296

  9. Persistent organochlorine pesticide residues in animal feed.

    Nag, Subir Kumar; Raikwar, Mukesh K

    2011-03-01

    Animal products like milk and meat are often found to be contaminated with residues of persistent pesticides and other toxic substances. The major source of entry of these compounds to animal body is the contaminated feed and fodder. So, unless the residues are managed at this stage, it is very difficult to prevent contamination in milk and meat. Therefore, the status of residue level of most persistent organochlorinated pesticides (OCP) in feed and fodder should be monitored regularly. The frequency of occurrence and contamination levels of OCP residues in different kinds of animal concentrate feed and straw samples collected from Bundelkhand region of India were determined. Out of 533 total samples, 301 i.e. 56.47% samples were positive containing residues of different OCPs like hexachlorocyclohexane (HCH) isomers, dichlorodiphenyltrichloroethane (DDT) complex, endosulfan and dicofol. Among different HCH isomers, the mean concentration of β-HCH was highest, and total HCH varied from 0.01 to 0.306 mg kg(-1). In case of DDT complex, i.e. DDD, DDE and DDT, the concentration ranged between 0.016 and 0.118 mg kg(-1) and the pp(|) isomers were more frequently encountered than their op(|) counterparts. Endosulfan was also found in some samples in concentration ranging from 0.009 to 0.237 mg/kg, but dicofol could be recorded in very few samples. Although feed samples were found to contain OC residues, after comparing their levels in positive samples with the limiting values of respective pesticides, only very few were found to exceed the threshold level. Otherwise, they were mostly within safe limits. PMID:20443138

  10. Organochlorine Pesticide Residues in the Processing of Pressed Cheese

    Dorin Ţibulcă; Mirela Jimborean; Dan Sălăgean; Ariana Caraba

    2015-01-01

    The persistence of pesticide residues in food and environment determined UN institutions to track their presence and establish rules of tolerance in foodstuffs of animal origin. Pesticide use leads to their presence as residue in foods. The research objectives were to establish the level of organo-chlorine pesticides in raw milk and their evolution during the process of obtaining pressed cheese.

  11. 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.

  12. 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

  13. Removal of acidic interferences in multi-pesticides residue analysis of fruits using modified magnetic nanoparticles prior to determination via ultra-HPLC-MS/MS

    The authors describe magnetite (Fe3O4) nanoparticles modified with 3-(N,N-diethylamino) propyltrimethoxysilane (Fe3O4-PSA NPs) for use as a sorbent for dispersive solid phase extraction of pesticide residues. The Fe3O4-PSA NPs were prepared by silanizing Fe3O4 NPs and modifying them with 3-(N,N-diethylamino) propyltrimethoxysilane. Field-emission scanning electron microscopy, FTIR and zeta potential measurements were employed to characterize the modified NPs. They were then used as an adsorbent to remove acidic interferences (such as malic acid and succinic acid), which are major interferences in LC-MS/MS analysis in causing ion suppression in the MS spectra of pesticides. In addition, graphitized carbon black (GCB) was used as an adsorbent to eliminate interferences by pigments. The use of Fe3O4-PSA NPs can replace time-consuming centrifugation as used in the so-called QuEChERS (quick, easy, cheap, effective, rugged and safe) method. This improvement is particularly significant in high-throughput analysis. Following the optimization of the quantities of Fe3O4-PSA NPs and GCB, the method was applied to the determination of 56 pesticides in (spiked) fruits (apple, kiwi, orange and pear) by ultra-HPLC-MS/MS. The analytical ranges typically extend from 1 to 200 ng∙mL−1, and recoveries range from 60.2 to 130 % at different concentrations of all four kinds of fruits. The LOQs for the pesticides are 10 ng∙kg−1, which makes the method a viable tool for pesticide monitoring in fruits. (author)

  14. Analysis of Veterinary Drug and Pesticide Residues Using the Ethyl Acetate Multiclass/Multiresidue Method in Milk by Liquid Chromatography-Tandem Mass Spectrometry.

    Imamoglu, Husniye; Oktem Olgun, Elmas

    2016-01-01

    A rapid and simple multiclass, ethyl acetate (EtOAc) multiresidue method based on liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) detection was developed for the determination and quantification of 26 veterinary drugs and 187 total pesticide residues in milk. Sample preparation was a simple procedure based on liquid-liquid extraction with ethyl acetate containing 0.1% acetic acid, followed by centrifugation and evaporation of the supernatant. The residue was dissolved in ethyl acetate with 0.1% acetic acid and centrifuged prior to LC-MS/MS analysis. Chromatographic separation of analytes was performed on an Inertsil X-Terra C18 column with acetic acid in methanol and water gradient. The repeatability and reproducibility were in the range of 2 to 13% and 6 to 16%, respectively. The average recoveries ranged from 75 to 120% with the RSD (n = 18). The developed method was validated according to the criteria set in Commission Decision 2002/657/EC and SANTE/11945/2015. The validated methodology represents a fast and cheap alternative for the simultaneous analysis of veterinary drug and pesticide residues which can be easily extended to other compounds and matrices. PMID:27293962

  15. Analysis of Veterinary Drug and Pesticide Residues Using the Ethyl Acetate Multiclass/Multiresidue Method in Milk by Liquid Chromatography-Tandem Mass Spectrometry

    Husniye Imamoglu

    2016-01-01

    Full Text Available A rapid and simple multiclass, ethyl acetate (EtOAc multiresidue method based on liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS detection was developed for the determination and quantification of 26 veterinary drugs and 187 total pesticide residues in milk. Sample preparation was a simple procedure based on liquid–liquid extraction with ethyl acetate containing 0.1% acetic acid, followed by centrifugation and evaporation of the supernatant. The residue was dissolved in ethyl acetate with 0.1% acetic acid and centrifuged prior to LC-MS/MS analysis. Chromatographic separation of analytes was performed on an Inertsil X-Terra C18 column with acetic acid in methanol and water gradient. The repeatability and reproducibility were in the range of 2 to 13% and 6 to 16%, respectively. The average recoveries ranged from 75 to 120% with the RSD (n=18. The developed method was validated according to the criteria set in Commission Decision 2002/657/EC and SANTE/11945/2015. The validated methodology represents a fast and cheap alternative for the simultaneous analysis of veterinary drug and pesticide residues which can be easily extended to other compounds and matrices.

  16. 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...

  17. Risk assessment and ranking of pesticide residues in Chinese pears

    LI Zhi-xia; LIU Chuan-de; ZHAO Xu-bo; GUO Yong-ze; NIE Ji-yun; YAN Zhen; XU Guo-feng; LI Hai-fei; KUANG Li-xue; PAN Li-gang; XIE Han-zhong; WANG Cheng

    2015-01-01

    The presence of pesticide residues in pears is a serious health concern. This study presents the results from a 2-year investigation (2013–2014) that used gas chromatography, GS/MS and UPLC/MS-MS to measure the levels of 104 pesti-cides in 310 pear samples. In 93.2% of the samples, 43 pesticides were detected, of which the maximum residue levels (MRLs) were exceeded in 2.6% of the samples. Multiple residues (two to eight compounds) were present in 69.7% of the samples; one sample contained nine pesticides and one sample contained 10. Only 6.8% of the samples did not contain residues. To assess the health risks, the pesticide residue data have been combined with daily pear consumption data for children and adult populations. A deterministic model was used to assess the chronic and acute exposures based on the Joint Meeting on Pesticide Residues (JMPR) method. A potential acute risk was demonstrated for children in the case of bifenthrin, which was found to be present at 105.36% of the acute reference dose (ARfD) value. The long-term exposure of the Chinese consumer to pesticide residues through the consumption of raw pears was far below the acceptable daily intake (ADI) criterion. Additionally, the matrix ranking scheme was used to classify risk subgroups of pesticides and pear samples. In general, 95.5% of samples were deemed to be safe and nine pesticides were classiifed as being of a relatively high risk. The ifndings indicated that the occurrence of pesticide residues in pears should not be considered a serious public health problem. Nevertheless, a more detailed study is required for vulnerable consumer groups, especially children. Continuous monitoring of pesticides in pears and tighter regulation of pesticide residue standards are recommended.

  18. 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)

  19. Organochlorine and organophosphorus pesticide residues in fodder and milk samples along Musi river belt, India

    Korrapati Kotinagu; Nelapati Krishnaiah

    2015-01-01

    Aim: The present study was conducted to find the organochlorine pesticide (OCP) and organophosphorus pesticide (OPP) residues in fodder and milk samples along Musi river belt, India. Materials and Methods: Fodder and milk samples collected from the six zones of Musi river belt, Hyderabad India were analyzed by gas chromatography with electron capture detector for OCP residues and pulsated flame photometric detector for the presence of OPP residues. Results: The gas chromatographic analysis of...

  20. Organochlorine Pesticide Residues in the Processing of Pressed Cheese

    Dorin Ţibulcă

    2015-11-01

    Full Text Available The persistence of pesticide residues in food and environment determined UN institutions to track their presence and establish rules of tolerance in foodstuffs of animal origin. Pesticide use leads to their presence as residue in foods. The research objectives were to establish the level of organo-chlorine pesticides in raw milk and their evolution during the process of obtaining pressed cheese.

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

    Francisco Sanchez-Bayo

    Full Text Available 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.

  2. 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; Camões, 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

  3. 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)

  4. 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...

  5. 76 FR 82238 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2011-12-30

    ... AGENCY 40 CFR Part 180 Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals... 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...

  6. 78 FR 13295 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2013-02-27

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

  7. 76 FR 3885 - Notice of Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on...

    2011-01-21

    ... AGENCY Notice of Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on... modification of regulations for residues of pesticide chemicals in or on various commodities. DATES: Comments... 174 or part 180 for residues of pesticide chemicals in or on various food commodities. EPA...

  8. 75 FR 14154 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-03-24

    ... 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...

  9. 76 FR 2110 - Notice of Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on...

    2011-01-12

    ... AGENCY Notice of Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on... modification of regulations for residues of pesticide chemicals in or on various commodities. DATES: Comments... 180 for residues of pesticide chemicals in or on various food commodities. EPA has determined that...

  10. 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...

  11. 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...

  12. 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...

  13. 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...

  14. 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

  15. Dispersive solid-phase extraction followed by liquid chromatography-tandem mass spectrometry for the multi-residue analysis of pesticides in raw bovine milk.

    Dagnac, Thierry; Garcia-Chao, Maria; Pulleiro, Paula; Garcia-Jares, Carmen; Llompart, Maria

    2009-05-01

    A fast multi-residue method based on dispersive solid-phase extraction (DSPE) followed by liquid chromatography-tandem mass spectrometry was developed for the simultaneous determination of 44 pesticides in raw bovine milk. Raw bovine milk samples did not percolate through SPE cartridges usually applied for pesticide extraction from homogenized pasteurized milk samples. Therefore, a DSPE technique was implemented and validated for the first time in this work. Graphitized non-porous carbon and C18 modified silica materials were tested both in combination with magnesium sulfate and bonded silica with ethylenediamine-N-propyl phase. The efficiency of the DSPE process was studied at several concentration levels obtaining the higher recoveries with C18 material. The method performance was also assessed and the limits of quantification reached the ng g(-1) level, complying with the most recent maximum residue levels. The DSPE method was also shown to be suited to both the fatty and skimmed fractions issued from raw milk. Finally, the extraction method was successfully applied to the analysis of raw milk samples collected in 23 farms of dairy cattle from NW Spain (Galicia). PMID:19268955

  16. Multi-walled carbon nanotubes as alternative reversed-dispersive solid phase extraction materials in pesticide multi-residue analysis with QuEChERS method.

    Zhao, Pengyue; Wang, Lei; Zhou, Li; Zhang, Fengzu; Kang, Shu; Pan, Canping

    2012-02-17

    A multi-residue method based on modified QuEChERS sample preparation with multi-walled carbon nanotubes (MWCNTs) as reversed-dispersive solid phase extraction (r-DSPE) material and gas chromatography-mass spectrometry determination by selected ion monitoring (GC/MS-SIM) mode was validated on 30 representative pesticides residues in vegetables and fruits. The acetonitrile-based QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation technique was used to obtain the extracts, and the further cleanup was carried out by applying r-DSPE. It was found that the amount of MWCNTs influenced the cleanup performance and the recoveries. The optimal amount of 10mg MWCNTs was suitable for cleaning up all selected matrices, as a suitable alternative r-DSPE material to primary secondary amine (PSA). This method was validated on cabbage, spinach, grape and orange spiked at concentration levels of 0.02 and 0.2 mg/kg. The recoveries of 30 pesticides were in the range of 71-110%, with relative standard deviations (RSDs, n=5) lower than 15%. Matrix effects were observed by comparing the slope of matrix-matched standard calibration with that of solvent. Good linearity was achieved at the concentration levels of 0.02-0.5 mg/L. The limits of quantification (LOQs) and the limits of detection (LODs) for 30 pesticides ranged from 0.003 to 0.05 mg/kg and 0.001 to 0.02 mg/kg at the signal-to-noise ratio (S/N) of 10 and 3, respectively. The method was successfully applied to analysis real samples in Beijing. In conclusion, the modified QuEChERS method with MWCNTs cleanup step showed reliable method validation performances and good cleanup effects in this study. PMID:22227363

  17. 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

  18. 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

  19. 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)

  20. 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...

  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. Organochlorine pesticide residues in wheat from Konya region, Turkey.

    Guler, G O; Cakmak, Y S; Dagli, Z; Aktumsek, A; Ozparlak, H

    2010-05-01

    The present study has been carried out to evaluate the organochlorine pesticide contamination in wheat from Konya region. This region is the largest area of cereal production in Turkey. The contamination level has been determined according to the European Community Directives. Different wheat samples (36) were obtained from local farmers and wheat factories in this region. All the wheat samples examined were found to be contaminated by organochlorine pesticide residues of cis-Chlordane and methoxychlor. Chlordane isomers, methoxychlor, DDT and its metabolites, aldrin, beta HCH, heptachlor and lindane have been found to be the highest organochlorine pesticide residues. In some of these samples, various organochlorine pesticide residues have been determined to be higher than European Community maximum residual limits. The residues of aldrin in one sample, trans-Chlordane in one sample, oxy-chlordane in eight samples and methoxychlor in one sample were found to be in excess of EC MRLs. Since most of the samples have been found to be contaminated with residues and some residues exceed EC MRLs, a control of organochlorine pesticide residues in wheat is necessary. PMID:20156519

  3. Proficiency test on incurred and spiked pesticide residues in cereals

    Poulsen, Mette Erecius; Christensen, Hanne Bjerre; Herrmann, Susan Strange

    2009-01-01

    A proficiency test on incurred and spiked pesticide residues in wheat was organised in 2008. The test material was grown in 2007 and treated in the field with 14 pesticides formulations containing the active substances, alpha-cypermethrin, bifentrin, carbendazim, chlormequat, chlorpyrifos......-methyl, difenconazole, epoxiconazole, glyphosate, iprodione, malathion, pirimicarb, prochloraz, spiroxamin and trifloxystrobin. After harvest, the test material was additionally spiked in the laboratory with three pesticides, that where the residues were too low, and axozystrobin. In total, 72 laboratories submitted...... results and z-scores were calculated for all laboratories and pesticides, except for glyphosate where only five laboratories submitted results and summed weighted z-scores were calculated for the laboratories with a sufficient scope. For several pesticides, the submitted results were strongly depending on...

  4. 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

  5. Analysis of Veterinary Drug and Pesticide Residues Using the Ethyl Acetate Multiclass/Multiresidue Method in Milk by Liquid Chromatography-Tandem Mass Spectrometry

    Husniye Imamoglu; Elmas Oktem Olgun

    2016-01-01

    A rapid and simple multiclass, ethyl acetate (EtOAc) multiresidue method based on liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) detection was developed for the determination and quantification of 26 veterinary drugs and 187 total pesticide residues in milk. Sample preparation was a simple procedure based on liquid–liquid extraction with ethyl acetate containing 0.1% acetic acid, followed by centrifugation and evaporation of the supernatant. The residue was dissolved i...

  6. [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

  7. 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)...

  8. 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)...

  9. 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...

  10. 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...

  11. 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

  12. 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)

  13. 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

  14. Assessing Children’s Dietary Pesticide Exposure: Direct Measurement of Pesticide Residues in 24-Hr Duplicate Food Samples

    Schenck, Frank J.; Pearson, Melanie A.; Wong, Jon W.; Lu, Chensheng Alex

    2010-01-01

    Background: The data presented here are a response to calls for more direct measurements of pesticide residues in foods consumed by children and provide an opportunity to compare direct measures of pesticide residues in foods representing actual consumption with those reported by the U.S. Department of Agriculture Pesticide Data Program. Objective: We measured pesticide residues in 24-hr duplicate food samples collected from a group of 46 young children participating in the Children’s Pestici...

  15. GC/MIP/AED method for pesticide residue determination in fruits and vegetables.

    Ting, K C; Kho, P

    1991-01-01

    This research describes the results of a gas chromatography/microwave induced plasma/atomic emission detection (GC/MIP/AED) method performed on a Hewlett-Packard 5921A system for pesticide residue analysis in fruits and vegetables. A total of 6 experiments were conducted: (1) sensitivity and linearity studies for elements S, P, Cl, and N by analyzing dursban; (2) a study of instrument response to Cl concentration in pesticide molecules; (3) organochlorinated pesticide recoveries; (4) organophosphate pesticide recoveries; (5) carbamate pesticide recoveries; and (6) investigation of metallic pesticides with plictran and vendex as standards. The rank according to sensitivity and linearity was found to be as follows: S-181 greater than P-178 greater than Cl-479 greater than N-174. Instrument response to the concentration of chlorine atoms in the pesticide molecule was linear, with a correlation coefficient of 0.89. Recoveries of organochlorinated pesticides were 91.7-109.3%, with the exception of citrus, whose recovery was affected by coeluting interferences. Organophosphate recoveries were 73.2% or higher, except for the cygon oxygen analog, which degraded in the GC system under all circumstances. Carbamate recoveries were inconsistent quantitatively; however, the information generated from elements N and S were useful for qualitative confirmation of other methods, such as LC postcolumn derivatization analysis. Overall, the GC/MIP/AED method is powerful for qualitative confirmation in pesticide residue analysis. The instrument's capability of acquiring multi-elements (Cl and P) selectively and accurately is an alternative method for organochlorinated and organophosphate pesticide residue analyses. In addition, the GC/MIP/AED system is easy to use, simple to maintain, and its chromatograms can be interpreted by any chromatography analyst without much prior training. PMID:1757425

  16. 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

  17. 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

  18. Residues of organochlorinated pesticides in soils from the Czech Republic

    National POPs inventories carried out currently in many countries as a part of the implementation of Stockholm Convention revealed the need for detailed information about a distribution of pollutants in various regions. Screening for the residues of selected organochlorinated pesticides (chlordane, heptachlor, dieldrin, aldrin, endrin, isodrin, endosulfan I, endosulfan II, methoxychlor, mirex) in soil and biotic samples from the Czech Republic was performed. Although these pesticides have never been used in large quantities in this region, results indicate that their residues still persist in the top layer soils more than 20 years after they have been banned. The fact that their soil concentrations in the mountains are generally higher than those in agricultural areas, and detection of the traces of pesticides that have never been used in this region suggest on their occurrence in soils due to the atmospheric redistribution rather than as a result of direct application. - Organochlorinated pesticides persist in soils

  19. 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

  20. Monitoring of pesticide residue in bovine milk from Nadia district, West Bengal.

    Singh, Aruna Kumari; Sar, Tapas Kumar; Mandal, Tapan Kumar

    2013-07-01

    Monitoring of 210 bovine milk samples collected from local markets in the Nadia district of West Bengal during 2011 was performed. Samples were collected in summer and winter seasons. Analysis of pesticides was performed by using a multiresidue method validated in the laboratory. The quantification was performed using GC-ECD. Analysis revealed the presence of lindane in less than 1 % of milk samples. Endosulfan I and II were also detected and were found to exceed MRL recommended by Codex. Overall 1.90 % of the analyzed samples showed trace to measurable amount of pesticide residues. The monitored area provided pesticide residues data of milk, assisting in future scientific assessment on pesticide usage. PMID:23708263

  1. 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.

  2. 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)

  3. 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.

  4. Overall and class-specific scores of pesticide residues from fruits and vegetables as a tool to rank intake of pesticide residues in United States: A validation study.

    Hu, Yang; Chiu, Yu-Han; Hauser, Russ; Chavarro, Jorge; Sun, Qi

    2016-01-01

    Pesticide residues in fruits and vegetables are among the primary sources of pesticide exposure through diet, but the lack of adequate measurements hinder the research on health effects of pesticide residues. Pesticide Residue Burden Score (PRBS) for estimating overall dietary pesticide intake, organochlorine pesticide score (OC-PRBS) and organophosphate pesticide score (OP-PRBS) for estimating organochlorine and organophosphate pesticides-specific intake, respectively, were derived using U.S. Department of Agriculture Pesticide Data Program data and National Health and Nutrition Examination Survey (NHANES) food frequency questionnaire data. We evaluated the performance of these scores by validating the scores against pesticide metabolites measured in urine or serum among 3,679 participants in NHANES using generalized linear regression. The PRBS was positively associated with a score summarizing the ranks of all pesticide metabolites in a linear fashion (p for linear trend vegetables with high vs. low pesticide residues, respectively (p for trend vegetables (p for trend 0.07) than from less contaminated Fruits and vegetables (p for trend 0.63), although neither of the associations achieved statistical significance. The PRBS and the class-specific scores for two major types of pesticides were significantly associated with pesticide biomarkers. These scores can reasonably rank study participants by their pesticide residue exposures from fruits and vegetables in large-scale environmental epidemiological studies. PMID:27128714

  5. 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

  6. 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

  7. 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)

  8. 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

  9. Sub-lethal effects of pesticide residues in brood comb on worker honey bee (Apis mellifera development and longevity.

    Judy Y Wu

    Full Text Available BACKGROUND: Numerous surveys reveal high levels of pesticide residue contamination in honey bee comb. We conducted studies to examine possible direct and indirect effects of pesticide exposure from contaminated brood comb on developing worker bees and adult worker lifespan. METHODOLOGY/PRINCIPAL FINDINGS: Worker bees were reared in brood comb containing high levels of known pesticide residues (treatment or in relatively uncontaminated brood comb (control. Delayed development was observed in bees reared in treatment combs containing high levels of pesticides particularly in the early stages (day 4 and 8 of worker bee development. Adult longevity was reduced by 4 days in bees exposed to pesticide residues in contaminated brood comb during development. Pesticide residue migration from comb containing high pesticide residues caused contamination of control comb after multiple brood cycles and provided insight on how quickly residues move through wax. Higher brood mortality and delayed adult emergence occurred after multiple brood cycles in contaminated control combs. In contrast, survivability increased in bees reared in treatment comb after multiple brood cycles when pesticide residues had been reduced in treatment combs due to residue migration into uncontaminated control combs, supporting comb replacement efforts. Chemical analysis after the experiment confirmed the migration of pesticide residues from treatment combs into previously uncontaminated control comb. CONCLUSIONS/SIGNIFICANCE: This study is the first to demonstrate sub-lethal effects on worker honey bees from pesticide residue exposure from contaminated brood comb. Sub-lethal effects, including delayed larval development and adult emergence or shortened adult longevity, can have indirect effects on the colony such as premature shifts in hive roles and foraging activity. In addition, longer development time for bees may provide a reproductive advantage for parasitic Varroa destructor

  10. Assessment of Organophosphate and Carbamate Pesticide Residues in Cigarette Tobacco with a Novel Cell Biosensor

    Spiridon Kintzios

    2008-04-01

    Full Text Available The conventional analysis of pesticide residues in analytical commodities, such as tobacco and tobacco products is a labor intensive procedure, since it is necessary to cover a wide range of different chemicals, using a single procedure. Standard analysis methods include extensive sample pretreatment (with solvent extraction and partitioning phases and determination by GC and HPLC to achieve the necessary selectivity and sensitivity for the different classes of compounds under detection. As a consequence, current methods of analysis provide a limited sample capacity. In the present study, we report on the development of a novel cell biosensor for detecting organophosphate and carbamate pesticide residues in tobacco. The sensor is based on neuroblastoma N2a cells and the measurement of changes of the cell membrane potential, according to the working principle of the Bioelectric Recognition Assay (BERA. The presence of pesticide residues is detected by the degree of inhibition of acetylcholine esterase (AChE. The sensor instantly responded to both the organophoshate pesticide chlorpyriphos and the carbamate carbaryl in a concentration-dependent pattern, being able to detect one part per billion (1 ppb. Additionally, tobacco leaf samples (in blended dry form were analyzed with both the novel biosensor and conventional methods, according to a double-blind protocol. Pesticide residues in tobacco samples caused a considerable cell membrane hyperpolarization to neuroblastoma cells immobilized in the sensor, as indicated by the increase of the negative sensor potential, which was clearly distinguishable from the sensor’s response against pesticide-free control samples. The observed response was quite reproducible, with an average variation of +5,6%. Fluorescence microscopy observations showed that treatment of the cells with either chlorpyrifos or carbaryl was associated with increased [Ca2+]cyt . The novel biosensor offers fresh

  11. 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

  12. 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

  13. 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

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

    Petersen, Annette; Jensen, Bodil Hamborg; Andersen, Jens Hinge;

    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...

  15. 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

  16. 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...

  17. Impact of toxic heavy metals and pesticide residues in herbal products

    Nema S. Shaban

    2016-03-01

    Full Text Available Medicinal plants have a long history of use in therapy throughout the world and still make an important part of traditional medicine. The World Health Organization (WHO estimates that 65%–80% of the world's populations depend on the herbal products as their primary form of health care. This review is conducted to provide a general idea about chemical contaminants such as heavy metals and pesticide residues as major common contaminants of the herbal medicine, which impose serious health risks to human health. Additionally, we aim to provide different analytical methods for analysis of heavy metals and pesticide residues in the herbal medicine.

  18. Using a Hazard Quotient to Evaluate Pesticide Residues Detected in Pollen Trapped from Honey Bees (Apis mellifera) in Connecticut

    Stoner, Kimberly A.; Brian D Eitzer

    2013-01-01

    Analysis of pollen trapped from honey bees as they return to their hives provides a method of monitoring fluctuations in one route of pesticide exposure over location and time. We collected pollen from apiaries in five locations in Connecticut, including urban, rural, and mixed agricultural sites, for periods from two to five years. Pollen was analyzed for pesticide residues using a standard extraction method widely used for pesticides (QuEChERS) and liquid chromatography/mass spectrometric a...

  19. 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

    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-M...

  20. 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...

  1. Potential and real residues of pesticides in sugar beet

    Šovljanski Radmila A.; Lazić Sanja D.; Vuković Slavica

    2006-01-01

    Crops and their products can be contaminated either by direct application of pesticides for the protection of insects, acarives, agents of plant diseases and/or weeds, i.e. as the result of growing them on the soil containing pesticide residues applied in previous years. For the protection of sugar beet in our country, 23 insectisides, 17 fungicides and 18 herbicides have been registered. The pre-harvest interval (PHI) ranges from 14 to 42 days i.e. they are provided by the time of applicatio...

  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. Bioenergy residues as novel sorbents to clean up pesticide pollution

    Mukherjee, Santanu

    2016-04-01

    Worldwide, water contamination from agricultural use of pesticides has received increasing attention within the last decades. In general, sources of pesticide water pollution are categorized into diffuse (stemming from treated fields) and point sources (stemming from farmyards and spillages). Research has demonstrated that 40 to 90% of surface water pesticide contamination is due to point source pollution. To reduce point pollution from farm yards, where the spray equipment is washed, biobed or biofilter systems are used to treat the washing water. The organic material usually used in these systems is often not environmentally sustainable (e.g. peat) and incorporated organic material such as straw leads to a highly heterogeneous water flow, with negative effects on the retention and degradation behavior of the pesticides. Therefore, the objective of this study was to assess the suitability of alternative materials based on bioenergy residues (biochar and digestate) for use in biofilters. To this aim the sorption-desorption potential of three contrasting pesticides (bentazone, boscalid, and pyrimethanil) on mixtures of soil with digestate and/or biochar were investigated in laboratory batch equilibrium experiments. The results indicate that the mixture of digestate and biochar increased pesticide sorption potential, whereby in all cases, the Kd des / Kf des values were lower than the Kd ads / Kf ads values indicating that the retention of the pesticides was weak. Thus, as Kf des were lower than the Kf ads values and H values were below 1, it can be concluded that the biomixtures presented negative desorption (higher hysteresis) in those cases. A higher Kd (>78 L kg-1), Kf (>400 μM1-1/nf L1/nfkg-1) and KL (>40 L kg-1) was obtained for all pesticides for the digestate and biochar based mixtures, which had a higher organic matter content. However, lower sorption of the pesticides was observed in blank soil compared to the other biomixtures, which was attributed to the

  4. 免疫分析技术在有机磷农药残留检测中应用%Application of immunoassay in organophosphorus pesticide residue analysis

    梁彦

    2013-01-01

    In this review,the harm of organophosphorus pesticide and the commonly used detection methods are introduced,especially that the immunoassay in detection of organophosphorus pesticide residue. The several key factors to affect the immunoassay are reviewed. The main directions of the further development of immunoassay techniques for determining organophosphorus pesticides are also discussed.%  该文简介有机磷农药危害及常用几种检测方法,对免疫分析技术在有机磷农药残留检测中应用进行归纳分析;着重介绍研究最多的酶联免疫分析法,对影响免疫分析方法几个关键因素进行综述,并探讨免疫分析技术在有机磷农药检测领域发展。

  5. Pesticide residue in water--a challenging task in India.

    Agarwal, Akriti; Prajapati, Rajmani; Singh, Om Pal; Raza, S K; Thakur, L K

    2015-02-01

    Modern agriculture practices reveal an increase in use of pesticides to meet the food demand of increasing population which results in contamination of the environment. In India, crop production increased to 100 %, but the cropping area has increased marginally by 20 %. Pesticides have played a major role in achieving the maximum crop production but maximum usage and accumulation of pesticide residues is highly detrimental to aquatic and other ecosystem. Pesticide residues in drinking water have become a major challenge over the last few years. It has been monitored in public water supply resources in National capital territory, i.e., Delhi. Organochlorine pesticides (OCPs), mainly isomers of hexachlorohexane (HCH), dichloro-diphenyl-trichloroethane (DDT), endosulphan, endrin, aldrin, dieldrin, and heptachlore, were identified from potable water samples. Results suggested that continuous consumption of contaminated water can pose severe health threats to local residents of this area. Central Pollution Control Board (CPCB), Delhi, had found α and β isomers of endosulphan residues in the Yamuna river. High concentrations of γ-HCH (0.259 μg/l) and malathion (2.618 μg/l) were detected in the surface water samples collected from the river Ganga in Kanpur, Uttar Pradesh (UP). High concentration of methyl parathion, endosulfan, and DDT were observed in water samples collected from the river at Bhagalpur, Bihar. The Industrial Toxicology Research Centre (ITRC), Lucknow (UP) study also found 0.5671 ppb concentrations of endosulfan in the river at Allahabad, UP. Similar results were found in other water samples in India. PMID:25638058

  6. Sample treatment and determination of pesticide residues in fatty vegetable matrices: a review.

    Gilbert-López, Bienvenida; García-Reyes, Juan F; Molina-Díaz, Antonio

    2009-07-15

    A demanding task in pesticide residue analysis is yet the development of multi-residue methods for the determination of pesticides in vegetables with relatively high fat content (i.e. edible oils and fatty vegetables). The separation of pesticides and other chemical contaminants from high-fat food samples prior to subsequent steps in the analytical process is yet a challenging issue to which much effort in method development has being applied. This review addresses the main sample treatment methodologies for pesticide residue analysis in fatty vegetable matrices. Even with the advent of advanced hyphenated techniques based on mass spectrometry these complex fatty matrices usually require extensive sample extraction and purification. Current methods involve the use of one or the combination of some of the following techniques for both the sample extraction and clean-up steps: liquid-liquid partitioning, solid-phase extraction (SPE), gel-permeation chromatography (GPC), matrix solid-phase dispersion (MSPD), etc. An overview of methods developed for these contaminants in fatty vegetables matrices is presented. Sample extraction and purification techniques are discussed and their most recent applications are highlighted. This review emphasizes that sample preparation is a critical step, but also the determination method is, and cannot be treated separately from sample treatment. In recent years, the appearance and use of new, more polar pesticides has fostered the development of liquid chromatography/mass spectrometry (LC-MS) besides gas chromatography. The main features of LC-MS for the analysis of multi-class pesticides in fatty vegetable samples will be also underlined, with an emphasis on the multi-class, multi-residue strategy and the difficulties associated. PMID:19559852

  7. Organochlorine and organophosphorus pesticide residues in fodder and milk samples along Musi river belt, India

    Korrapati Kotinagu

    2015-04-01

    Full Text Available Aim: The present study was conducted to find the organochlorine pesticide (OCP and organophosphorus pesticide (OPP residues in fodder and milk samples along Musi river belt, India. Materials and Methods: Fodder and milk samples collected from the six zones of Musi river belt, Hyderabad India were analyzed by gas chromatography with electron capture detector for OCP residues and pulsated flame photometric detector for the presence of OPP residues. Results: The gas chromatographic analysis of fodder samples of Zone 5 of Musi river showed the residues of dicofol at concentration of 0.07±0.0007 (0.071-0.077. Among organophosphorus compounds, dimetheoate was present in milk samples collected from Zone 6 at a level of 0.13±0.006 (0.111-0.167. The residues of OCPs, OPPs and cyclodies were below the detection limit in the remaining fodder and milk samples collected from Musi river belt in the present study. Conclusion: The results indicate that the pesticide residues in fodder and milk samples were well below the maximum residue level (MRL values, whereas dicofol in fodder and dimethoate in milk were slightly above the MRL values specified by EU and CODEX.

  8. 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,...

  9. 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...

  10. 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)

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

    Sarah Blankson-Arthur; P. Owiredu Yeboah; Abledze Golow; Anita Osei Tutu; Dzifa Denutsui

    2011-01-01

    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 extra...

  12. A Qualitative Study of Residual Pesticides on Cotton Fibers

    Zameer Ul Hassan, Syed; Militky, Jiri; Krejci, Jan

    2013-01-01

    Two different methods are utilized for this study. The first method covers the measurement of bioelectrical signals caused by enzymatic inhibition of acetyl cholinesterase (AChE) for the detection of pesticides. Biosensor toxicity analyzer (BTA) was used for the testing and the monitoring of changes in bioelectrical signals caused by the interaction of biological substances, and residues were evaluated. The second method is based on measurement of the oxygen level caused by photosynthetic inh...

  13. 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.

  14. Validation and use of a fast sample preparation method and liquid chromatography-tandem mass spectrometry in analysis of ultra-trace levels of 98 organophosphorus pesticide and carbamate residues in a total diet study involving diversified food types.

    Chung, Stephen W C; Chan, Benny T P

    2010-07-16

    This paper reports a comprehensive sensitive multi-residue liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for detection, identification and quantitation of 73 pesticides and their related products, a total of 98 analytes, belonging to organophosphorus pesticides (OPPs) and carbamates, in foods. The proposed method makes use of a modified QuEChERS (quick, easy, cheap, effective, rigged, and safe) procedure that combines isolation of the pesticides and sample clean-up in a single step. Analysis is performed by liquid chromatography-electrospray ionization-tandem mass spectrometry operated in the multiple reaction monitoring (MRM) mode, acquiring two specific precursor-product ion transitions per target compound. Two main fragment ions for each pesticide were obtained to achieve the identification according to the SANCO guidelines 10684/2009. The method was validated with various food samples, including edible oil, meat, egg, cheese, chocolate, coffee, rice, tree nuts, citric fruits, vegetables, etc. No significant matrix effect was observed for tested pesticides, therefore, matrix-matched calibration was not necessary. Calibration curves were linear and covered from 1 to 20 microg L(-1) for all compounds studied. The average recoveries, measured at 10 microg kg(-1), were in the range 70-120% for all of the compounds tested with relative standard deviations below 20%, while a value of 10 microg kg(-1) has been established as the method limit of quantitation (MLOQ) for all target analytes. Similar trueness and precision results were also obtained for spiking at 200 microg kg(-1). Expanded uncertainty values were in the range 21-27% while the HorRat ratios were below 1. The method has been successfully applied to the analysis of 700 food samples in the course of a baseline monitoring study of OPPs and carbamates. PMID:20557892

  15. 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

  16. 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.

  17. Residues levels of organochlorine pesticide in cow's milk from industrial farms in Hidalgo, Mexico.

    Gutierrez, Rey; Ortiz, Rutilio; Vega, Salvador; Schettino, Beatriz; Ramirez, Maria L; Perez, Jose J

    2013-01-01

    A survey was carried out from 2008 to 2010 to determine the concentrations of 16 organochlorine pesticide residues (OPRs) from Tizayuca, Hidalgo, Mexico. Organochlorine residue determinations were made from milk fat, using chromatographic cleanup and analysis by gas chromatography with an electron capture detector. The OPR concentrations found were from below the detection limit (DL) to 0.91 ng g(-1) in 2008, DL to 0.38 ng g(-1) in 2009 and DL to 0.59 ng g(-1) in 2010. In general concentrations of organochlorine pesticides were higher in the wet season (3.37 ng g(-1) and 4.79 ng g(-1)) than the dry season (1.92 ng g(-1) and 2.71 ng g(-1)) for 2009 and 2010, due to control of pests in the pasture and sheds. According to Codex Alimentarius regulations, individual pesticides did not exceed the permissible limits, which for example were 10 μg kg(-)1 for alpha hexachlorocyclohexane (HCH) and endosulfan I, 20 μg kg(-1) for p,p'-DDT, and 6 μg kg(-1) for dieldrin, endrin and heptachlor. A reduction of organochlorine pesticide concentrations in cow's milk was noted, indicating that the Mexican government has achieved reduction or elimination of some organochlorine pesticides in response to global agreements on persistent organic pollutants. PMID:23998305

  18. Multi-residue detection of pesticides using a sensitive immunochip assay based on nanogold enhancement.

    Lan, Meijing; Guo, Yirong; Zhao, Ying; Liu, Yihua; Gui, Wenjun; Zhu, Guonian

    2016-09-28

    This paper describes the development of a new multiplex immunoassay for simultaneous detection of seven pesticides (triazophos, methyl-parathion, fenpropathrin, carbofuran, thiacloprid, chlorothalonil, and carbendazim). Sixteen pairs of pesticide antibodies and antigens were screened for reactivity and cross-reaction. A microarray chip consisting of seven antigens immobilized on a nitrocellulose membrane was then constructed. Nanogold was employed for labeling and signal amplification to obtain a sensitive colorimetric immunoassay. The direct and indirect detection formats were further compared using primary antibody-gold and secondary antibody-gold conjugates as tracers. An integrated 7-plex immunochip assay based on the indirect model was established and optimized. The detection limits for the pesticides were 0.02-6.45 ng mL(-1), which meets detection requirements for pesticide residues. Naked-eye assessment showed the visual detection limits of the assay ranged from 1 to 100 ng mL(-1). Spiked recovery results demonstrated that the immunochip assay had potential for multi-analysis of pesticide residues in vegetables and fruits. The proposed microarray methodology is a flexible and versatile tool, which can be applied to other competitive multiplex immunoassays for small molecular compounds. PMID:27619097

  19. Earthworm tolerance to residual agricultural pesticide contamination: field and experimental assessment of detoxification capabilities.

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

    2014-09-01

    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 conventional cultivation to organic pasture. Soil multiresidual pesticide analysis revealed up to 9 molecules including atrazine up to 2.4 ng g(-1) dry soil. Exposure history of endogeic Aporrectodea caliginosa and Allolobophora chlorotica modified their responses to pesticides. In the field, activities of soluble glutathione-S-transferases (sGST) and catalase increased with soil pesticide contamination in A. caliginosa. Pesticide stress was reflected in depletion of energy reserves in A. chlorotica. Acute exposure of pre-adapted and naïve A. caliginosa to pesticides (fungicide Opus(®), 0.1 μg active ingredient epoxiconazole g(-1) dry soil, RoundUp Flash(®), 2.5 μg active ingredient glyphosate g(-1) dry soil, and their mixture), revealed that environmental pre-exposure accelerated activation of the detoxification enzyme sGST towards epoxiconazole. PMID:24874794

  20. Detection of Residual Levels and Associated Health Risk of Seven Pesticides in Fresh Eggplant and Tomato Samples from Narayanganj District, Bangladesh

    Md. Nur Alam; M. Alamgir Zaman Chowdhury; M. Sabir Hossain; Mohammad Mijanur Rahman; M Abdur Rahman; Siew Hua Gan; Md. Ibrahim Khalil

    2015-01-01

    Residual levels of seven frequently used pesticides were investigated in 140 samples of two common vegetables, eggplants and tomatoes, from agricultural fields in the Narayanganj district of Bangladesh. The analysis of pesticide residues was performed by high-performance liquid chromatography with photodiode array detection. A large percentage of the eggplants (50%) and tomatoes (60%) from the Narayanganj district were contaminated with pesticides, and all of the levels were above the maximum...

  1. Pesticide residue determination in vegetables from western China applying gas chromatography with mass spectrometry.

    Qin, Guofu; Zou, Keting; Li, Yongbo; Chen, Yan; He, Fengrui; Ding, Guirong

    2016-09-01

    In this study,an effort has been made to evaluate the pesticide residues in vegetables from western China. Fifty-one pesticides, including organophosphorus, organochlorine, carbamate and pyrethroid, were detected in 369 commonly used vegetables by GC-MS. Concentrations of organophosphorus pesticides were detected ranging from 0.0008 to 18.8200 mg/kg, among which organophosphorus pesticide concentrations exceeded their maximum residue levels (MRLs) in five samples. Carbamate and organochlorine pesticides were determined to have concentrations in the range of 0.0012-0.7928 mg/kg. The residual concentrations of carbamate pesticides in six samples and organochlorine pesticides in four samples exceeded their MRLs. The residual concentrations of five pyrethroid pesticides were within the range of 0.0016-6.0827 mg/kg and the pyrethroid residues in two samples exceeded their MRLs. The results revealed that pesticide residues in 70.73% of the vegetables samples were not detected, while in the rest of vegetables there were one or more pesticide residues and some even exceeded their MRLs, which would threaten the health of consumers. Our work provides significant information for the food safety regulations to control the excessive use of some pesticides on those kinds of vegetables from western China. Copyright © 2016 John Wiley & Sons, Ltd. PMID:26864471

  2. Modification and re-validation of the ethyl acetate-based multi-residue method for pesticides in produce

    Mol, J.G.J.; Rooseboom, A.; Dam, van R.; Roding, M.; Arondeus, K.; Sunarto, S.

    2007-01-01

    The ethyl acetate-based multi-residue method for determination of pesticide residues in produce has been modified for gas chromatographic (GC) analysis by implementation of dispersive solid-phase extraction (using primary¿secondary amine and graphitized carbon black) and large-volume (20 ¿L) injecti

  3. 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...

  4. 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

  5. 商品奶与原料奶中农药与亚硝酸钠残留分析%Analysis of pesticide residues and sodium nitrite in commercial milk and raw milk

    冷静; 邓斌; 李琦华; 杨舒黎; 苟潇; 毛华明

    2011-01-01

    The gas chromatograph (GC) method was used for analysis of pesticide residues and sodium nitrite residues in commercial milk and raw milk, and also analysis the effect of feeding pattern on pesticide residues in raw milk. The results showed that: Among five pesticides,Methamidophos, Dichlorvos and Malathion had high detection rate of pesticide residue, 45.0%~67.5% with commercial milk, and 46.8%~71.2% with raw milk. The detection rate and the residual quantity of Methamidophos, Dichlorvos, Trichlorfon, Malathion and Fenthion were no significant difference between commercial milk and raw milk (P > 0.05); but the detection rate and the residual quantity of sodium nitrite had significant difference between commercial milk and raw milk (P < 0.01). weighted average of detection rate, weighted average residual quantity and weighted total residual quantity of five pesticides were all large-scale farmers significantly lower than backyard farmers and cooperative breeding farmers (P < 0.05), and the were no significant difference between the later two feeding pattern (P > 0.05).%采用高效气相色谱(GC)分析法对商品奶和原料奶中农药和亚硝酸钠残留进行分析,并分析不同饲养模式对原料奶中农药残留的影响.结果表明:在所测定的5种农药中,甲胺磷、敌敌畏和马拉硫磷等3种农药残留检出率较高,商品奶为45.0%~67.5%,原料奶为46.8%~71.2%.商品奶和原料奶中甲胺磷、敌敌畏、敌百虫、马拉硫磷和倍硫磷检出率和残留量差异不显著(P>0.05);而商品奶和原料奶中亚硝酸钠检出率和残留量差异极显著(P<0.01).原料奶中5种农药加权平均检出率、农药加权平均残留量和加权残留总量均为规模化饲养显著低于农户散养和合作社饲养(P<0.05),后两者之间无显著差异(P>0.05).

  6. Some organochlorine pesticide residues in fish species in Konya, Turkey.

    Kalyoncu, Leyla; Agca, Ihsan; Aktumsek, Abdurrahman

    2009-02-01

    The levels of organochlorine pesticides were measured in 18 fish species from Konya markets, Turkey. These species were selected on the basis of their importance to local human fish consumption. The extracted residues were analyzed on a micro capillary gas chromatograph equipped with an electron capture detector. Total 14 different organochlorine pesticides were determined. These residues were detected in all fish species, except in trout, horse mackerel and bonito. DDT and its metabolites and HCH were the predominant contaminants in fish muscles. The mean concentrations of summation operator DDT were in the range between 0.0008 and 0.0828 microg g(-1). DDT was the predominant residue in Sparus aurata. Detectable levels of HCH, aldrin, and heptachlor were found in most samples. However, dieldrin, endrin, beta endosulfan, p-p' DDT, and p-p' DDD were not found in Salmo trutta. The mean of endrin ranged from 0.0040 microg g(-1) (Triglia lineate) to 0.0326 microg g(-1) (Trachurus trachurus). These results give no indication of important health risks associated with the consumption of these fishes in Konya markets. PMID:19103455

  7. 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

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

    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

  9. 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...

  10. 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

  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. Contributions of pesticide residue chemistry to improving food and environmental safety: past and present accomplishments and future challenges.

    Seiber, James N; Kleinschmidt, Loreen A

    2011-07-27

    The principles of modern pesticide residue chemistry were articulated in the 1950s. Early authors pointed out the advantages of systematizing and standardizing analytical methods for pesticides so that they could be widely practiced and the results could be reproduced from one laboratory to the next. The availability of improved methods has led to a much more complete understanding of pesticide behavior and fate in foods and the environment. Using methods based largely upon gas chromatography (GC) and high-performance liquid chromatography (HPLC) coupled increasingly with mass spectrometry (MS) and MS(n) as the detection tool, residues can be measured at parts per billion levels and below in a variety of food and environmental matrices. Development of efficient extraction and cleanup methods, techniques such as ELISA, efficient sample preparation techniques such as QuEChERS, and automated laboratory and field instrumentation has also contributed to the tools available for use in modern pesticide residue analysis. As a result, great strides have been made in improving food and worker safety and in understanding environmental behavior and fate of pesticides. There are many challenges remaining in the field of pesticide residue chemistry that will continue to stimulate analytical chemists. New chemistries are emerging, often patterned on complex natural products. Analyzing for the parent chemicals and potentially multiple breakdown products will require analytical ingenuity. The development of more sensitive bioassays and knowledge of unintended side effects will challenge residue chemistry as well, as in the case of following the fate of environmental endocrine disruptors associated with some pesticides as well as nonpesticide contaminants from packaging materials and other familiar articles. Continued funding and other resources to ensure better training, international cooperation, and accelerated research and development activities will be a constant need in

  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. The analysis method of pesticides residue in Hongkong plant-derived spices%输港植物源性调味品中农药残留检测方法

    刘润珠; 张靖坤; 崔淑华; 周春杨; 王建华

    2014-01-01

    目的:针对2012年5月香港特区政府发布全新的食物中残余除害剂管理制度——《香港食物中残余除害剂的建议规管方案》(简称《规管方案》)中所涉及的共计7大类植物源性调味品中25项农药残留,建立相关样品处理及仪器测定方法。方法样品用含0.1%乙酸乙腈溶液超声提取,经SAX/PSA固相萃取柱净化,分别用气相色谱-质谱联用仪、气相色谱-串联质谱联用仪及液相色谱-串联质谱联用仪进行定性、定量分析。分别对蒜粉、姜粉及辣椒粉基质进行了50µg/kg水平上的添加回收实验,优化了前处理过程及仪器分析过程中几个关键步骤。结果检测结果添加回收率在67.8%~123.7%之间,确立了针对植物源性调味品中25项农药残留的分析和确认方法。结论该方法简单便捷,易于操作,有效地解决了植物源性调味品中复杂基质对测定农药残留的影响。%Objective To establish a method for the related samples’ pretreatment and instrument detection, regarding the 25 pesticide residues in the 7 major categories of plant derived spices which are involved in the new residual pesticides in food management system——“Hongkong foods recommended gauge residual pesticides tube scheme” (referred to as “regulatory scheme”) issued in 2012 May by the Hongkong SAR government.MethodsBy using acetonitrile with 0.1% acetic acid as the solvent, the sample was ultrasonic extracted, cleaned by SAX/PSA, and qualitatively and quantitatively analyzed by gas chromatography-mass (GC-MS), gas chromatography-mass/mass (GC-MS/MS) and liquid chromatography-mass/mass (LC-MS/ MS). In the experiment of recovery test on garlic powder, ginger powder and chilli powder spiked with 50 µg/kg, several key steps were optimized in the pretreatment process and instrument testing.Results The recoveries of those pesticides were from 67.8% and 123.7%. The analysis and confirmation method of plant

  15. Organochlorine and organophosphorus pesticide residues in raw buffalo milk from agroindustrial areas in Assiut, Egypt.

    Shaker, Eman M; Elsharkawy, Eman E

    2015-01-01

    Raw buffalo milk samples from the agroindustrial zone in upper Egypt were analyzed for the presence of organochlorine and organophosphorus pesticides using gas chromatography-mass spectroscopy. Five organochlorine pesticides namely, alachlor, dieldrin, hexachlorobenzene, lindane and methoxychlor and three organophosphorus pesticides chlorpyrifos, malathion, and parathion-methyl were detected in the milk samples. In 44% of the samples, the concentrations of lindane and malathion residues exceeded tolerance levels set by the European Commission (EC) in 2008. In addition, the concentrations of chlorpyrifos, methoxychlor, and hexachlorobenzene residues exceeded the 2008 EC maximum residual limits (MRLs) by 33, 66, and 88% of the examined samples, respectively. However, the levels of alachlor, dieldrin, and parathion-methyl residues were below EC MRLs. The results of this study confirm the risks of pesticide residues exposure that threaten consumer health in Egypt. Thus, we recommend that pesticide residue monitoring programs be instituted in all the developing countries. PMID:25575291

  16. 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.

  17. 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

  18. 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...

  19. 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

  20. Analysis of pesticide residues in strawberries and soils by GC-MS/MS, LC-MS/MS and two-dimensional GC-time-of-flight MS comparing organic and integrated pest management farming

    The issue of pesticide residues in foods is growing in importance due to greater global food trade and increasing public concern. Therefore, appropriate control and monitoring of residues in food must be conducted. In this study, we analyzed 22 strawberry and soil samples after their collection over...

  1. Detection of Residual Levels and Associated Health Risk of Seven Pesticides in Fresh Eggplant and Tomato Samples from Narayanganj District, Bangladesh

    Md. Nur Alam

    2015-01-01

    Full Text Available Residual levels of seven frequently used pesticides were investigated in 140 samples of two common vegetables, eggplants and tomatoes, from agricultural fields in the Narayanganj district of Bangladesh. The analysis of pesticide residues was performed by high-performance liquid chromatography with photodiode array detection. A large percentage of the eggplants (50% and tomatoes (60% from the Narayanganj district were contaminated with pesticides, and all of the levels were above the maximum residual limit (MRL proposed by the EC regulation. Diazinon was the most common (35% pesticide detected in the vegetable samples at a concentration of 45–450 times higher than the MRL. The health risk index for diazinon was highest for both eggplant and tomato samples, which may be due to its physiochemical properties. Fenitrothion and linuron are the two second most common types of pesticides detected in the vegetable samples. Regular monitoring of the use of common pesticides on vegetables should be conducted.

  2. 蔬菜农药残留现状及其潜在风险分析%Present Status of Pesticide Residue in Vegetables and Its Potential Risk Analysis

    叶雪珠; 赵燕申; 王强; 蒋玉根

    2012-01-01

    By detecting the pesticide use and 94 kinds pesticide residues in vegetable production in Zhejiang Province, major pesticide residue types at present and their risks in vegetable were analyzed. The results showed that 78 kinds of pesticides mainly used in vegetable production, including insecticide, fungicide, growth regulator and herbicide were mostly pesticides with high effective and low toxic. The detection of pesticide residues revealed that 28 pesticides got high detectable rate in vegetables, including acetamiprid, carbendazim, dursban, imidacloprid, morpholine, triazophos, propamocarb, pyridaben, etc.. The results also indicated that 46.4% of the detected pesticides with residual in vegetables were not found in using. But methamidophos and other highly toxic pesticides were still checked out. One of the main risks is some pesticide products without label and their component is unclear to customer. In addition, a unified standard testing method has not been established for 28 kinds of pesticides frequently used in vegetable production. Pesticide residue is still a security risk for vegetable consumption.%通过对浙江省蔬菜生产中使用农药情况调查和94种农药的残留检测,分析了目前蔬菜中主要残留农药品种及其潜在风险.结果发现,目前蔬菜生产中主要使用78种农药,包括杀虫剂、杀菌剂、生长调节剂和除草剂,以低毒农药品种为主;蔬菜中主要残留28种农药,检出频率较高的农药依次为啶虫脒、多菌灵、毒死蜱、吡虫啉、烯酰吗啉、三唑磷、霜霉威和哒螨灵等,检出的残留农药品种中,有46.4%在调查中未发现有使用,甲胺磷等高毒农药仍有检出.农药产品标识和农药成分不明是主要风险之一.此外,蔬菜中使用的28种农药尚未建立统一的标准检测方法,蔬菜食用仍存在农药残留安全风险.

  3. Assessment of organochlorine pesticide residues in soils and drinking water sources from cocoa farms in Ghana

    Fosu-Mensah, Benedicta Y.; Okoffo, Elvis D.; Darko, Godfred; Gordon, Christopher

    2016-01-01

    Residues of organochlorine pesticides were determined in soils and drinking water sources in cocoa growing areas in Ghana. Soil samples analysed showed the presence of four organochlorine pesticide residues namely lindane (0.005–0.05 mg/kg), beta-HCH (

  4. Distribution of pesticide residues within homes in central New York State.

    Obendorf, S K; Lemley, A T; Hedge, A; Kline, A A; Tan, K; Dokuchayeva, T

    2006-01-01

    Residues for 17 pesticides were analyzed in 41 households in central New York State that represented farm, rural, and urban houses. Samples were taken in both summer and winter of 2000-2001 from the same households from four locations; family room carpet; adjacent smooth floor; flat tabletop surface; and settled dust collected in a Petri dish on a tabletop. Pesticide residues were analyzed to identity factors that influence both the transport into and the redistribution of pesticides in the indoor environment. Differences were observed between the various pesticides and pesticide classifications relative to location within and between households as well as by season. Variations in the pesticide residues were related to a number of factors. Higher residues were observed in the farm households, particularly in summer, with the highest amount observed for chloropyrifos in carpet (33 microg/m2). For many pesticides, the frequency of detection and the amount of residues were higher in summer, which relates to usage patterns in agriculture and horticulture; however, larger amounts of insecticides such as mecoprop, resmethrin, and tetramethrin were found on flat surfaces in winter, indicating household use and possible redistribution within the home. Distribution patterns suggest that routines within a household may cause high variation in residues; these practices include indoor pets and treatment for fleas and ticks, use of termiticides, and fastidiousness of occupants. Frequency of pesticide detection was highest in carpet for both summer and winter for all households, indicating that carpets hold pesticides over time. Adsorbent fibrous materials such as textiles hold pesticides by macro- and micro-occlusion in their complex structures. Amounts of pesticide residue were higher in carpets than on smooth floors, particularly for rural farm households where the farmer was a certified pesticide applicator. The maximum amount of pesticide residue on a smooth floor surface

  5. 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

  6. Validation of a method for the determination of 120 pesticide residues in apples and cucumbers by LC-MS/MS.

    Ramadan, Gouda; Al Jabir, Muna; Alabdulmalik, Najat; Mohammed, Ali

    2016-05-01

    Most countries have clearly defined regulations governing the use of pesticides in agricultural activity. The application of pesticides in agriculture usually leads to a residual amount of these pesticides on food products such as fruit and vegetables. The presence of pesticide residues on these foods destined for human consumption may pose food safety risks to consumers. To protect consumers, national authorities have established maximum limits for pesticide residues in foods. These limits can only be enforced if there are methods available to detect and monitor their concentrations in the applicable food products. To support the enforcement of this legislation, we have developed a multi-residue liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the analysis of 120 pesticide residues in apples and cucumbers which has been validated and implemented in the routine monitoring and surveillance programme for these pesticides. In this method, apple and cucumber samples are extracted using the QuEChERS method (quick, easy, cheap, effective, rugged, and safe) and the extracts were analyzed directly by LC-MS/MS. The mean recoveries at three different concentrations of 0.01 µg/g , 0.05 µg/g, and 0.1 µg/g over the analytical range varied between 70 and 120%. The repeatability of the method expressed as %RSD was less than 20%. The limit of detection (LOD) of the method ranged between 0.0014 and 0.0110 µg/g for apples and between 0.0012 and 0.0075 µg/g for cucumbers. The limit of quantification (LOQ) of the method was 0.01 µg/g for apples and cucumbers. The method has been used for the analysis of over 600 apple and 550 cucumber samples over the past two years. Copyright © 2016 John Wiley & Sons, Ltd. PMID:27443204

  7. Flexible and Adhesive Surface Enhance Raman Scattering Active Tape for Rapid Detection of Pesticide Residues in Fruits and Vegetables.

    Chen, Jiaming; Huang, Youju; Kannan, Palanisamy; Zhang, Lei; Lin, Zhenyu; Zhang, Jiawei; Chen, Tao; Guo, Longhua

    2016-02-16

    The efficient extraction of targets from complex surfaces is vital for technological applications ranging from environmental pollutant monitoring to analysis of explosive traces and pesticide residues. In our present study, we proposed a proof-of-concept surface enhance Raman scattering (SERS) active substrate serving directly to the rapid extraction and detection of target molecules. The novel substrate was constructed by decorating the commercial tape with colloidal gold nanoparticles (Au NPs), which simultaneously provides SERS activity and "sticky" of adhesive. The utility of SERS tape was demonstrated by directly extracting pesticide residues in fruits and vegetables via a simple and viable "paste and peel off" approach. The obtained strong and easily distinguishable SERS signals allow us to detect various pesticide residues such as parathion-methyl, thiram, and chlorpyrifos in the real samples with complex surfaces including green vegetable, cucumber, orange, and apple. PMID:26810698

  8. 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,

  9. 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...

  10. 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.

  11. 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

    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.

  12. 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

  13. Exploration on risk assessment of pesticide residues in vegetables%蔬菜农药残留风险评估探讨

    黄和勇

    2012-01-01

    Based on the analysis on standard-exceeded reason of pesticide residues in vegetables,this paper elaborated the process of risk assessment of pesticide residues in vegetables,explored the countermeasures to strengthen the task in risk assessment of pesticide residues in vegetables.%分析蔬菜农药残留超标的原因,阐述蔬菜农药残留风险评估的过程,探讨加强蔬菜农药残留风险评估工作的对策。

  14. 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.

  15. 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...

  16. 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.

  17. 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 concentrations±SE 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

  18. Determination of some organochlorine pesticide residues in honeys from Konya, Turkey.

    Yavuz, Halil; Guler, Gokalp O; Aktumsek, Abdurrahman; Cakmak, Yavuz S; Ozparlak, Haluk

    2010-09-01

    In this study, 24 organochlorine pesticide residues in 109 different honey samples collected from stores and open markets in Konya, Turkey were analyzed by gas chromatography-electron capture detection. Aldrin, cis-chlordane, trans-chlordane, oxy-chlordane, 2,4(')-DDE, and 4,4(')-DDE were found in all honey samples. The mean value was 0.0540 microg g(-1) for oxy-chlordane. In the 55 samples of 109, levels of organochlorine pesticide residues of oxy-chlordane were determined as higher than those of Turkish Alimentarius Codex maximum residual limits (MRLs). Other organochlorine pesticide residues also exceeded MRLs except for cis-heptachlor epoxide and alpha-hexachlorocyclohexane. Since all of the honey samples are found contaminated and most of these samples exceeded MRLs, a control of organochlorine pesticide residues in honey is necessary for consumer health. PMID:19685151

  19. 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)

  20. 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

  1. 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.

  2. Health impact from pesticide residues in a desert environment.

    Gomes, James

    1998-01-01

    The amount and frequency of use of pesticides in vegetable farming have been shown to be high in the five farming areas in Al-Ain, UAE. The mean usage of all pesticides was high (6.81 g/m2) while the usage of organophosphorus pesticides (2.11 g/m2) was higher compared to the usage of all the other types of pesticides. A number of pesticides banned from use in the developed countries are still used in vegetable farming. The depletion of erythrocyte acetylcholinesterase (AChE) activity among...

  3. 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

  4. 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...

  5. Proposal for field-based definition of soil bound pesticide residues

    Boesten, J.J.T.I.

    2016-01-01

    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

  6. 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...

  7. 2010年杭州市蔬菜有机磷和氨基甲酸酯农药残留状况分析%Analysis of organophosphorus and carbamate pesticide residues in vegetables collected from Hangzhou in 2010

    何良兴; 张瓅文; 李燕

    2011-01-01

    目的:了解杭州市蔬菜农药残留情况,为蔬菜质量安全的监管和控制工作提供科学依据.方法:采集蔬菜样品446577批次,测定有机磷和氨基甲酸酯农药残留量,并对结果进行分析总结.结果:蔬菜年均农药超标率为0.09%,残留农药以有机磷为主,不同品种蔬菜的超标率与超标农药类型都不同,杭州本地与外地蔬菜农药超标率没有显著不同.结论:杭州市蔬菜农药残留水平较低,质量安全状况良好,但禁用农药还需要进一步加强监管.%Objective: To investigate the conditions of organophosphorus and carbamate pesticide residues in vegetables in Hangzhou in order to provide the basis for surveillance and control of vegetables safety. Methods: The total 446,577 samples of vegetables were collected and their residues of organophosphorus and carbamate were measured. At last, the results were analysised and summaried. Results: The disqualification rate of vegetables is 0.09%. The organophosphorus is the main pesticide residues. The disqualification rate and the type of pesticide residues varies in different kinds of vegetables. There's no difference in the disqualification rate of vegetables between Hangzhou and other places. Conclusion: The level of pesticide residues is low,and vegetable quality of Hangzhou is good, but supervision and administration on the forbidden pesticides should be strengthened.

  8. 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, lady’s 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 lady’s 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.

  9. 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 .

  10. 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 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

  11. 免疫分析法在吡虫啉农药检测中的应用进展%Application of Immunoassay Analysis in Doping Test of Pesticide Residues

    彭方毅; 杨海艳; 姜海蓉; 徐建建

    2011-01-01

    As a low toxicity, low-residue pesticide, imidacloprid has a wide range of applications on a-gainst pests in agriculture. In order to get a more accurate evaluation of environmental safety, detection technique of imidacloprid residue has gradually become a research hotspot. In this paper,the immuno-assay test of pesticide imidacloprid residue has been overviewed.%对吡虫啉残留免疫分析检测方法进行综述.介绍了各种免疫分析方法,比较了这些方法的优劣,在此基础上展望了免疫分析法在吡虫啉农药残留检测的应用前景和发展方向.

  12. Pesticide residues in human breast milk: risk assessment for infants from Punjab, India.

    Bedi, J S; Gill, J P S; Aulakh, R S; Kaur, P; Sharma, A; Pooni, P A

    2013-10-01

    Punjab state in India is an agrarian society, where agriculture is the lifeline of farming community. To keep pace with increasing demands of food for growing population the indiscriminate use of pesticides has led to the contamination of environment and food commodities in this region. Analysis of human breast milk samples (n=53) for pesticide residues revealed the presence of β-, γ-HCH, p,p' DDD, p,p' DDE, p,p' DDT and endrin with mean concentration of 97.9, 101.7, 239.8, 1574.1, 100.3 and 90.7 ng g(-1) lipid wt., respectively. In addition, occurrence of β-endosulfan, endosulfan sulphate, cypermethrin and chlorpyrifos in this study have also been reported for the first time in human breast milk in Punjab, India. With increase in parity, HCH and DDT residue burden in donor's milk decreased. Although levels of HCH and DDT residues in breast milk samples have decreased significantly, yet estimated daily intake values for DDT are higher than the FAO/WHO permissible tolerable daily intake values for few infants. PMID:23850662

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

    Md. Shakhaoat Hossain; Md. Alamgir Hossain; Md. Abdur Rahman; Md Mainul Islam; Md Atiqur Rahman; Tanveer Mehedi Adyel

    2013-01-01

    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 comm...

  14. 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)

  15. Analysis of non-cleaned QuEChERS extracts for the determination of pesticide residues in fruit, vegetables and cereals by gas chromatography-tandem mass spectrometry.

    Norli, Hans Ragnar; Christiansen, Agnethe L; Stuveseth, Kari

    2016-01-01

    This paper investigated the possibility of leaving out the traditional clean-up step in the QuEChERS procedure and analysing non-cleaned extracts from fruit, vegetables and cereals with a combination of gas chromatography-tandem mass spectrometry (GC-MS/MS), back-flush technology and large-volume injection. By using calibration standards in cucumber matrix, recovery and precision were calculated in lettuce, orange and wheat for 109 pesticides at 0.01 and 0.1 mg kg(-1) in two sets of samples: one with and one without clean-up. For both spiking levels, 80-82% of the pesticides in the non-cleaned extracts and 80-84% of the pesticides in the cleaned extracts were within the acceptable recovery range of 70-120%. Precision data for both levels showed that 95% of the pesticides in the non-cleaned extracts and 93-95% of the pesticides in the cleaned extracts had RSDs below 20%. Recovery and precision data were determined using a two tailed t-test (p = 0.05). By using calibration standards in the respective matrix, we studied if the non-cleaned calibration standards gave an extra matrix effect compared with the cleaned standards by using the slope from calibration graphs and plotting the calculated extra matrix effect minus 100 for each compound. The results showed that for 79% of the pesticides, the extra matrix effect minus 100 was within the acceptable range of -20% to 20%. Five European Union proficiency tests on rye, mandarin, rice, pear and barley, respectively, from 2010 to 2012 were reanalysed omitting the clean-up step and showed satisfactory results. At least 70 injections of non-cleaned extracts were made without detecting any increased need for maintenance during the experimental period. Analysing non-cleaned QuEChERS extracts of lettuce, orange and wheat are possible under the conditions described in this paper because recovery, precision and specificity showed satisfactory results compared with samples subjected to traditional dispersive clean-up. PMID

  16. Current status of pesticides application and their residue in the water environment in Ireland

    Zhao, Y.Q.; Singleton, P; Meredith, S.; et al

    2013-01-01

    Pesticides have been listed by the Irish Environmental Protection Agency as potentially dangerous pollutants that may pose a significant risk to the water environment in the Republic of Ireland (ROI). Although this analysis of pesticides data was based on the existing pesticides application survey in ROI, this study aims to produce a geographical information system profile for the amount of pesticides used in agriculture and the distribution of their use in different parts of the country. The...

  17. Analysis of gas chromatography - mass spectrometry in detection of pesticide residues in vegetables%GC-MS检测蔬菜有机磷农药残留的效果分析

    齐志彩

    2012-01-01

    目的:用比较法对气相色谱-质谱法检测蔬菜农药残留的效果进行综合分析.方法:用气相色谱-质谱法对已知的5种农药标准品连续稀释计算出检出限,并随机抽取本地菜农种植的四种蔬菜进行农药残留量检测.同时用气相色谱法同步进行比较试验.结果:两种方法比较,气相色谱-质谱法具有更高的灵敏度和准确度,差异有统计学意义(P<0.05).对蔬菜残留农药的检测结果表明GC-MS在蔬菜农残检测中具有更广泛的用途.结论:GC- MS在检测蔬菜农药残留方面具有更好的效果.%Objective: To analyze the effect of gas chromatography - mass spectrometry in detection of pesticide residues in vegetables. Methods: 5 known pesticide standards were detected by GC - MS continuously after dilution to calculate the detection limit, and 4 kinds of vegetables were randomly selected for pesticide residues detection by GC - MS and GC simultaneously for comparison test. Results: Compared to GC, GC - MS had better sensitivity and accuracy, the difference of the two methods had statistical significance (P < 0. 05). GC - MS was more suitable for detection of pesticide residues in vegetables. Conclusion: Gas chromatography - mass spectrometry in the detection of pesticide residues in vegetables has better effect.

  18. 76 FR 76674 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2011-12-08

    ....940(a) for residues of didecyl dimethyl ammonium carbonate and didecyl ammonium bicarbonate.... Potentially affected entities may include, but are not limited to: Crop production (NAICS code 111). Animal production (NAICS code 112). Food manufacturing (NAICS code 311). Pesticide manufacturing (NAICS code...

  19. 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.

  20. 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 μm), (II) Microaggregate (MA, 20-2 μm) and (III) Colloid phase (COL, 2-0.05 μm). 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.

  1. 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

  2. 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)

  3. 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.

  4. 2006年-2010年某市蔬菜中农药残留情况分析%Investigation and analysis on pesticide residues in vegetables from 2006 to 2010

    陈焕娟

    2012-01-01

    目的:通过某市2006年-2010年蔬菜农药残留情况,探讨造成农药残留的原因和防控措施.方法:用回顾性流行病学方法对某市2006年-2010年蔬菜农药检测资料进行分析.结果:①2006年-2010年用气相色谱法检测95份蔬菜样品,其中不合格蔬菜20份,检出违规使用的农药15种,有机磷酸酯类农药检出率最高为21.1%.②2006年-2010年用速测卡法共检测5790份蔬菜样品,农药检出率在2.8% ~7.4%之间,平均检出率为4.5%.结论:5年间该市均检出蔬菜农药残留,且呈现波动性.%Objective:To explore the causes and control measures of pesticide residue in vegetables by understanding the status of pesticide residues in vegetables from 2006 to 2010. Methods; The detection data of pesticide residues in vegetables from 2006 to 2010 were analyzed with retrospective epidemiological method. Results: 1. 95 vegetable samples were detected by gas chromatography from 2006 to 2010, of which 20 samples were not qualified, and 15 kinds of illegal pesticides were detected with organophosphate pesticide detection rate up to 21. 1%. 2. 5790 vegetable samples were detected by speed test card from 2006 to 2010, pesticide detection rate was between 2. 8% -7.4% , with the average rate of 4.5% . Conclusion; Pesticide residues were detected in vegetables in last 5 years with volatility.

  5. 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.

  6. 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.

  7. 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

    Sapozhnikova, Yelena, E-mail: yelena.sapozhnikova@ars.usda.gov [US Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 193038 (United States); Lehotay, Steven J. [US Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 193038 (United States)

    2013-01-03

    Highlights: Black-Right-Pointing-Pointer A method for analysis of POPs and novel flame retardants in catfish was developed. Black-Right-Pointing-Pointer The method is based on a QuEChERS extraction, d-SPE clean-up and low pressure GC/MS-MS. Black-Right-Pointing-Pointer The method validation demonstrated good recoveries and low detection limits. Black-Right-Pointing-Pointer 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{sup -1} for PCBs, 0.5-10 ng g{sup -1} for PBDEs, 0.5-5 ng g{sup -1} for select pesticides and PAHs and 1-10 ng g{sup -1} for flame retardants. The developed method was successfully applied for analysis of catfish samples

  8. 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.

  9. 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

  10. Analysis of heavy metals and organochlorine pesticide residues in ramulus uncaria cum uncis in Guangxi%广西部分钩藤药材重金属和有机氯农药残留量

    王超英; 黄瑞松; 覃利梅; 肖梅; 陆峥琳

    2012-01-01

    Objective:To investigate the heavy metals and organochlorine pesticide residues in Ramulus Uncaria Cum Uncis in Guangxi, and to evaluate their safety. Methods: The heavy metals (Pb, Cd, As, Hg, Cu) and organochlorine pesticide residues(BHC, PCNB, DDT) in 17 samples of 9 variaties of Ramulus Uncaria Cum Uncis in Guangxi were determined by AAS and GC, respectively. Results: Five heavy metals in 14 samples were all qualified ; but Cd contents in 3 samples exceeded the standard limit; and organochlorine pesticide residues in all samples were all qualified. Conclusion: The organochlorine pesticide residues in all samples and heavy metals in most samples were in the safety range, but' Cd in some samples was in the risk of exceeding the standards.%目的:通过对广西部分钩藤药材重金属和有机氯农药残留量分析,对其安全性进行评价.方法:采用原子吸收分光光度法和气相色谱法分别测定9种钩藤药材17批样品的铅、镉、砷、汞、铜和六六六、滴滴涕、五氯硝基苯含量.结果:14批样品的5种重金属元素含量全部合格,3批样品的镉超标,全部样品的有机氯农药残留量合格.结论:全部样品有机氯类农药残留量和大部分样品重金属含量均在安全范围内,但有部分样品存在镉超标的安全隐患.

  11. Pesticides residues in milks and feedstuff of farm animals drawn from Greece.

    Tsiplakou, E; Anagnostopoulos, C J; Liapis, K; Haroutounian, S A; Zervas, G

    2010-07-01

    The objective of this study was to investigate if milk from dairy sheep and goats, fed mainly with supplementary feed during the winter months, was contaminated with pesticides residues. Tauwo hundred milk samples from sheep and goats were collected from 10 farms of each animals. The sheep and goats farms were selected from those which represent common conventional production and feeding systems in Greece. Milk and feed samples (alfalfa hay, wheat straw, shrubs, pasture and concentrates) were taken from each farm to analyze for pesticides residues. The results showed that the summation operatorendosulfan was the main pesticide residue which was detected in all the concentrates samples at a mean concentration of 5.36 mgkg(-1), which is much higher from the maximum residue level (MRL). In addition, the summation operatorendosulfan was also detected in all the alfalfa hay samples but at a mean concentration of 0.10 mgkg(-1) which is lower than the MRL. The mean concentrations of endosulfan alpha and beta were 2.82 and 2.39 mgkg(-1) in the concentrates samples and 0.08 and 0.02 mgkg(-1) respectively in alfalfa hay samples. In the wheat straw, shrubs and pasture samples no pesticides residues were detected. No pesticide residues were also detected in milk samples of sheep and goats. Thus, this milk from the farms sampled presents no human health risks as far as the contaminants analyzed concerned. PMID:20537679

  12. Gas-liquid chromatographic determination of nonpolar organochlorine pesticide residues in a crude vegetable oil and its refinery by-products.

    Young, S J; Kamps, L R

    1982-07-01

    A crude soybean oil, several of its refinery by-products (described as soapstock, deodorizer distillate, and clabber stock), and the completely refined oil were analyzed for pesticide residues. Fourteen organo-chlorine pesticides and pesticide metabolites were found in the deodorizer distillate; 5 of these were also found in the clabber stock. Levels in these by-products ranged from 0.3 to 8 ppm. Only endrin and dieldrin were detected in the crude oil at levels of 0.01 and 0.05 ppm, respectively. Forty to 150 times these levels were found in the deodorizer distillate and clabber stock. Pesticide residues were not detected in the refined oil or in the soapstock at limits of detection for dieldrin of about 0.01 and 0.1 ppm, respectively. The method used by the Food and Drug Administration to analyze fats and oils for multiple organohalogen pesticide residues was inadequate for the extraction of pesticide residues from vegetable oil refinery by-products. The method used to analyze the crude vegetable oil and the refinery by-products involved dissolution of the oil samples in ethyl acetate-toluene, filtration if necessary, cleanup by gel permeation chromatography, and then Florisil column chromatography. The oil was isolated from aqueous-oil mixtures by extraction with hexane before analysis. The crude soybean oil was fortified with 12 organohalogen pesticides and Aroclor 1254 at levels of 0.5-3.7 ppm. Recoveries ranged from 83 to 102%. PMID:6889594

  13. Pesticide residues in leafy vegetables, stalk and stem vegetables from South Korea: a long-term study on safety and health risk assessment.

    Park, Duck Woong; Kim, Kwang Gon; Choi, Eun Ah; Kang, Gyeong Ri; Kim, Tae Sun; Yang, Yong Shik; Moon, Su Jin; Ha, Dong Ryong; Kim, Eun Sun; Cho, Bae Sik

    2016-01-01

    South Korea has a unique food culture. South Koreans enjoy wrapping meat and eating or making kimchi (traditionally fermented Korean food) and eating using raw leafy vegetables, stalk and stem vegetables. Therefore, there is a high chance of being exposed to pesticide residues of vegetables. The objective of this study was to investigate pesticide residues in leafy vegetables, stalk and stem vegetables from South Korea. A total of 8496 samples were mainly collected from Gwangju and Jeonnam area (the largest production region of leafy vegetables, stalk and stem vegetables) in South Korea from 2010 to 2014. A total of 230 pesticides were used for multi-residue analysis of pesticides. Among 8496 samples, 61 different pesticides (1029 times) were detected in 890 samples, of which 118 samples (1.4%) exceeded the Korea maximum residue limits (MRLs). Samples exceeding the MRLs were mostly found in leafy vegetables (brassica lee ssp. namai, leafy lettuce, spinach, perilla leaves, crown daisy, marsh mallow, aster scaber, pimpinella brachycarpa) and Chinese chive. Procymidone, dimethomorph and azoxystrobin were the most frequently found pesticides. A risk assessment of pesticides exceeding the MRLs was evaluated by calculating the estimated daily intake (EDI) and the acceptable daily intake (ADI). The ratio of EDI to ADI was 0.003-30.4%. PMID:26571090

  14. 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...

  15. Organic amendments for risk mitigation of organochlorine pesticide residues in old orchard soils

    Performance of compost and biochar amendments for in situ risk mitigation of aged DDT, DDE and dieldrin residues in an old orchard soil was examined. The change in bioavailability of pesticide residues relative to an unamended control soil was assessed using Lumbricus terrestris in 4-L soil microcos...

  16. 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...

  17. Bound xenobiotic residues in food commodities of plant and animal origin: IUPAC Reports on Pesticides (40)

    Skidmore, M.W.; Paulson, G.D.; Kuiper, H.A.; Ohlin, B.

    1998-01-01

    In order to assess the dietary risk resulting from the use of pesticides or veterinary drugs the nature of the chemical residues on food commodities needs to be determined. Elucidation of the nature of the chemical residue is carried out using radiolabelled studies where the radiolabelled xenobiotic

  18. 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.

  19. 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)

  20. Codex Committee on Pesticide Residues--a plan for improved participation by governments.

    Wessel, J R

    1992-10-01

    The Codex Committee on Pesticide Residues (CCPR), which is responsible for establishing maximum residue limits (MRLs) for pesticides on food, has a vital role in protecting the public health and facilitating international trade. Codex MRLs are based on scientific evaluations by expert panels that constitute the Joint FAO/WHO Meeting on Pesticide Residues (JMPR). These panelists estimate an acceptable daily intake for a pesticide and expected level of residue remaining in food when the pesticide is used according to good agricultural practice. The goals of the CCPR are not being fully achieved. Governments are generally not accepting Codex MRLs; instead, technical and procedural aspects of the JMPR and CCPR process are being criticized. The CCPR is responding to valid criticisms of the process; however, governments may still lack the will to seek harmonization of pesticide limits for food in international trade. Overcoming this problem will be difficult, but not impossible. A plan of action is proposed that allows countries to selectively accept Codex MRLs, increase the number of chemicals in the JMPR/CCPR system for evaluation, and be responsive to both their consumers and their food producers without compromising national health and safety standards and competitive trade advantages. PMID:1438994

  1. Multi-residue analysis of veterinary drugs, pesticides and mycotoxins in dairy products by liquid chromatography-tandem mass spectrometry using low-temperature cleanup and solid phase extraction.

    Xie, Jie; Peng, Tao; Zhu, Ailing; He, Jianli; Chang, Qiaoying; Hu, Xueyan; Chen, Hui; Fan, Chunlin; Jiang, Wenxiao; Chen, Min; Li, Jiancheng; Ding, Shuangyang; Jiang, Haiyang

    2015-10-01

    A multi-class multi-residue analysis method for determination of veterinary drugs, pesticides and mycotoxins in dairy products by liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been established. These 17 classes, a total of 40 kinds of target compounds were chosen because their administration to food-producing animals is banned or regulated in China and may be potentially abused or misused. Samples were extracted with acetonitrile-ethyl acetate-acetic acid (49.5+49.5+1, v/v/v). Most of lipids in the extract were removed by low-temperature cleanup, prior to solid phase extraction on HLB cartridges. The quantification and confirmation of the 40 analytes were performed by LC-MS/MS with electro-spray ionization (ESI) interface in multiple reaction monitoring (MRM) mode. The limits of detection (LODs) and limits of quantification (LOQs) were 0.006-0.3μg/kg and 0.02-1.0μg/kg, respectively. The spiked recoveries in milk, yogurt, milk powder and cheese samples were from 67.3% to 106.9%. The repeatability and the within-laboratory reproducibility were less than 12.7% and 13.9%. Applying this method, our results revealed the presences of chloramphenicol, cimeterol, and flunixin at the concentration of 0.027-0.452μg/kg in some samples. PMID:26298066

  2. 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.

  3. Quantitative Structure activity relationship and risk analysis of some pesticides in the cattle milk

    Faqir Muhammad*, Ijaz Javed, Masood Akhtar1, Zia-ur-Rahman, Mian Muhammad Awais1, Muhammad Kashif Saleemi2 and Muhammad Irfan Anwar3

    2012-10-01

    Full Text Available Milk of cattle was collected from various localities of Faisalabad, Pakistan. Pesticides concentration was determined by HPLC using solid phase microextraction. The residue analysis revealed that about 40% milk samples were contaminated with pesticides. The mean±SE levels (ppm of cyhalothrin, endosulfan, chlorpyrifos and cypermethrin were 0.38±0.02, 0.26±0.02, 0.072±0.01 and 0.085±0.02, respectively. Quantitative structure activity relationship (QSAR models were used to predict the residues of unknown pesticides in the milk of cattle using their known physicochemical properties such as molecular weight (MW, melting point (MP, and log octanol to water partition coefficient (Ko/w as well as the milk characteristics such as pH, % fat, and specific gravity (SG in this species. The analysis revealed good correlation coefficients (R2 = 0.91 for cattle QSAR model. The coefficient for Ko/w for the studied pesticides was higher in cattle milk. Risk analysis was conducted based upon the determined pesticide residues and their provisional tolerable daily intakes. The daily intake levels of pesticide residues including cyhalothrin, chlorpyrifos and cypermethrin in present study were 3, 11, 2.5 times higher, respectively in cattle milk. This intake of pesticide contaminated milk might pose health hazards to humans in this locality.

  4. Safety Trap Analysis of NationaI Standard of MaximumResidue Limits for Pesticide in Food%我国农药残留国家标准的安全隐患探析

    李太平

    2011-01-01

    [目的]农药残留国家标准GB 2763-2005是判别食品安全的重要依据,研究标准本身是否存在安全隐患,对保障食品安全具有重要现实意义.[方法]利用农药最大残留限量(MRLs)、日允许摄入量(ADI)与被测食品每日最大理论摄人量(TDI)三者数量关系,计算了GB 2763-2005的439项指标的TDI值,并与消费者每日实际摄人量(RDI)进行了比较.[结果]发现35项指标的食品有不同比例消费者的RDI超过TDI,占总指标的7.3%.[结论]我国现行农药残留国家标准存在较大安全隐患.%[Aims] The national standard of maximum residue limits for pesticides in food GB 2763-2005 is the key base of food safety risk identification. Discussing the dependability of pesticide residue standards is very important for controlling food safety risk. [Methods] The national standard's theory daily intake (TDI) related with foods of 439 residue indexes of GB 2763-2005 was calculated with the quantity relation between MRLs, ADI and TDI, and compared with the customer's real daily intake (RDI) related with foods. [Results] There were 35 residue indexes related with foods which TDI were over their RDI with different proportion customers, accounted for 7.3% of total indexes in it. [Conclusions] It showed that there is a big potential safety risk in the present national standard of pesticide residue.

  5. A review on the fermentation of foods and the residues of pesticides-biotransformation of pesticides and effects on fermentation and food quality.

    Regueiro, Jorge; López-Fernández, Olalla; Rial-Otero, Raquel; Cancho-Grande, Beatriz; Simal-Gándara, Jesús

    2015-01-01

    Residues of pesticides in food are influenced by processing such as fermentation. Reviewing the extensive literature showed that in most cases, this step leads to large reductions in original residue levels in the fermented food, with the formation of new pesticide by-products. The behavior of residues in fermentation can be rationalized in terms of the physical-chemical properties of the pesticide and the nature of the process. In addition, the presence of pesticides decrease the growth rate of fermentative microbiota (yeasts and bacterias), which provokes stuck and sluggish fermentations. These changes have in consequence repercussions on several aspects of food sensory quality (physical-chemical properties, polyphenolic content, and aromatic profile) of fermented food. The main aim of this review is to deal with all these topics to propose challenging needs in science-based quality management of pesticides residues in food. PMID:24915365

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

    Poulsen, Mette E.; Wenneker, Marcel; Withagen, Jacques;

    2012-01-01

    versus coarse spray quality application on residue levels. The applications included boscalid, bupirimate, captan, fenoxycarb, indoxacarb, pirimicarb, pyraclostrobin and thiophanate-methyl. Apples were collected from four zones in the tree and pesticide residues were detected in the individual apples...... fine and coarse spray quality, except for carbendazim, the degradation product of thiophanate-methyl, where fine spray quality resulted in higher carbendazim residue levels than coarse spray quality. To examine the relationship between individual results and average results from ten apples, 20...

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

    Poulsen, Mette Erecius; Hansen, H.K.; Sloth, Jens Jørgen;

    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...

  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;

    2007-01-01

    , 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, the exposure were...

  9. MONITORING OF PESTICIDE RESIDUES IN AGRICULTURAL PRODUCTS IN THE YEARS 2003 AND 2004 IN SLOVENIA

    Helena BAŠA ČESNIK

    2006-10-01

    Full Text Available Agricultural Institute of Slovenia was performing national monitoring for pesticide residues in agricultural products according to the Decree on Monitoring of Pesticides in Foodstuffs and in Agricultural Products (Offi cial Gazette of the Republic of Slovenia No. 13/99. Constant measurements are necessary due to intensive agricultural production and use of chemical substances for plant protection. Due to the nutrition characteristic for the Slovenians pesticide residues are monitored each year in the samples of potato, lettuce and apples; the choice of other agricultural products and active substances analysed are adapted to the guidelines indicated in the EU recommendations. In the years 2003 and 2004 we analysed the presence of pesticide residues in 361 samples of agricultural products: caulifl ower, head cabbage, grapes, apples, strawberries, potatoes, peppers, tomatoes, wheat and lettuce from eight different growing areas of Slovenia. All agricultural products were analysed in 2003 for the presence of 51 active substances and in 2004 for the presence of 57 active substances. The maximum residue level (MRL was exceeded by 6.6 % samples inspected. Potato contributed a major share to this, since in 5.0 % of samples exceeded values of dithiocarbamate residues were determined, however, they were the only active substance found in potato. In 39.1 % of analysed samples residues lower than MRL were determined, in 54.3 % of samples residues were not found or they were below the level of detection method. The greatest number of pesticide residues which did not exceed MRLs was found in fruit, f. ex.: eight in apples and six in strawberries. Residues of dithiocarbamates were the most frequently found active substance in agricultural products.

  10. 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.

  11. Matrix-Matching as an Improvement Strategy for the Detection of Pesticide Residues.

    Giacinti, Géraldine; Raynaud, Christine; Capblancq, Sophie; Simon, Valérie

    2016-05-01

    More than 90% of the pesticides residues in apples are located in the peel. We developed a gas chromatography/ion trap tandem mass spectrometry method for investigating all detectable residues in the peel of 3 apple varieties. Sample preparation is based on the use of the Quick Easy Cheap Effective Rugged and Safe method on the whole fruit, the flesh, and the peel. Pesticide residues were quantified with solvent-matched and matrix-matched standards, by spiking apple sample extracts. Matrix effects dependent on the type of extract (fruit, flesh, or peel) and the apple variety were detected. The best data processing methods involved normalizing matrix effect rates by matrix-matched internal/external calibration. Boscalid, captan, chlorpyrifos, fludioxonil, and pyraclostrobin were the most frequently detected pesticides. However, their concentrations in the whole fruit were below European maximum residue levels. Despite negative matrix effects, the residues in peel were detected at concentrations up to 10 times higher than those in whole fruits. Consequently, other pesticide residues present at concentrations below the limit of quantification in the whole fruit were detected in the peel. PMID:27095394

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

    Anita Osei Tutu; P.O. Yeboah, A.A. Golow, D. Denutsui and S. Blankson-Arthur

    2011-01-01

    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, end...

  13. Determination of Organophosphorous and Carbamat Pesticides Residue in Drinking Water Resources of Hamadan in 2007

    A Allahresani

    2010-02-01

    Full Text Available "n "nBackgrounds and Objectives: Water contamination by pesticides is considered as an environmentalproblem today. In terms of agricultural development and diversity of plant pests, the use of pesticides has been increasing. Hamedan province has a suitable agricultural condition, it has enjoyed significant development in this respect. Among all the cities of Hamedan province, Hamedan city has the highest rank in tiller crops. Therefore, yearly use of pesticides is increasing in this area; which could be a serious threat to water resources of the city. The aim of this survey was determinaton of Organophosphorous and Carbamat pesticides residue in drinking water resources of Hamadan in 2007."nMaterials and Methods: In this survey, 126 water samples were collected from 7 drinking water resources of Hamedan during 12 consecutive months in 2007. for determination of these pesticides,two methods (solid- phase extraction and Liquid-Liquid extraction were adopted .and samples were analyzed by means of HPLC and GC/MS applying standard methods."nResults: Final results showed that the most concentration of Chlorpyrifos and Carbaryl pesticides were found to be about 3.85 ppb (part per billion and 1.8 ppb in spring and June respectively; the maximum concentration of Diazinon was about 36.5ppb in October (autumn.The minimum concentration of the three pesticides was detected in winter. According to the statistical test Two - Way ANOWA there were significant differences among pesticides concentrations in the water samples in different seasons (p<0.05 . However, there wasn't a significant difference in pesticides concentrations in surface and ground water samples(p>0.05. "nConclusion: Different studies have shown that pesticides residue concentration in water samples have a relationship with the amount of pesticides used in an area, physical and chemical refractory properties of pesticides; and environmental conditions. Thus, using resistant pollutants such

  14. 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...

  15. 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.)

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

    Crentsil Kofi Bempah; Archibold Buah-Kwofie; Dzifa Denutsui; Jacob Asomaning; Anita Osei Tutu

    2011-01-01

    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 elec...

  17. 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

  18. Pesticide Residues and Bees – A Risk Assessment

    Francisco Sanchez-Bayo; Koichi Goka

    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...

  19. 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)

  20. 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

  1. 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)

  2. Monitoring of some organochlorine pesticide residues of butter in Konya, Turkey.

    Nizamlioglu, Ferhan; Aktumsek, Abdurrahman; Kara, Huseyin; Dinc, Iffet

    2005-06-01

    Some organochlorine pesticide residues were investigated in the samples of all local commercial butter brands sold in the supermarket in Konya (Turkey). Some of the samples were found to have the DDT complex (DDT, DDD, DDE and isomers), total HCH complex (alpha-HCH, beta-HCH, gamma-HCH), aldrin, dieldrin and endosulfan (I and II). Nearly 94% of the butter samples were found to be contaminated. Endrin and heptachlorine were detected in three and two samples, respectively, while 87% of samples were contaminated by one or more HCH isomers. 78% of the organochlorine pesticide was DDT and/or its metabolites. These results confirmed that butters sold in Konya presented organochlorine pesticide residues indicating a human exposure. PMID:16334269

  3. Using a hazard quotient to evaluate pesticide residues detected in pollen trapped from honey bees (Apis mellifera in Connecticut.

    Kimberly A Stoner

    Full Text Available Analysis of pollen trapped from honey bees as they return to their hives provides a method of monitoring fluctuations in one route of pesticide exposure over location and time. We collected pollen from apiaries in five locations in Connecticut, including urban, rural, and mixed agricultural sites, for periods from two to five years. Pollen was analyzed for pesticide residues using a standard extraction method widely used for pesticides (QuEChERS and liquid chromatography/mass spectrometric analysis. Sixty pesticides or metabolites were detected. Because the dose lethal to 50% of adult worker honey bees (LD50 is the only toxicity parameter available for a wide range of pesticides, and among our pesticides there were contact LD50 values ranging from 0.006 to >1000 μg per bee (range 166,000X, and even among insecticides LD50 values ranged from 0.006 to 59.8 μg/bee (10,000X; therefore we propose that in studies of honey bee exposure to pesticides that concentrations be reported as Hazard Quotients as well as in standard concentrations such as parts per billion. We used both contact and oral LD50 values to calculate Pollen Hazard Quotients (PHQ = concentration in ppb ÷ LD50 as μg/bee when both were available. In this study, pesticide Pollen Hazard Quotients ranged from over 75,000 to 0.01. The pesticides with the greatest Pollen Hazard Quotients at the maximum concentrations found in our study were (in descending order: phosmet, Imidacloprid, indoxacarb, chlorpyrifos, fipronil, thiamethoxam, azinphos-methyl, and fenthion, all with at least one Pollen Hazard Quotient (using contact or oral LD50 over 500. At the maximum rate of pollen consumption by nurse bees, a Pollen Hazard Quotient of 500 would be approximately equivalent to consuming 0.5% of the LD50 per day. We also present an example of a Nectar Hazard Quotient and the percentage of LD50 per day at the maximum nectar consumption rate.

  4. 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 ...

  5. Safe apples for baby food production:search for pesticide preparations leaving minimum residues

    Ticha, Jana; Hajslova, Jana; Kovalczuk, Tomas; Jech, Martin; Honzicek, Jiri; Kocourek, Vladimir; Lansky, Miroslav; Kloutvorova, Jana; Falta, Vladan

    2007-01-01

    Abstract Altogether 19 pesticide preparations were used according to agriculture practise within 6 trials in apple orchards. Using gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods, premature Golden Delicious apples collected 64, 50, 36 days before harvest and matured fruit were examined for residues of active ingredients. No residues of triflumuron, triazamate, chlorpyrifos, etofenprox, fenoxycarb, kresoxim-methyl, c...

  6. Qualitative aspects in the analysis of pesticide residues in fruits and vegetables using fast, low-pressure gas chromatography - time-of-flight mass spectrometry

    Assessment of qualitative results in analytical methods is needed to estimate selectivity and devise criteria for chemical identification, particularly for mass spectrometric analysis. Low-pressure gas chromatography - mass spectrometry (LP-GC/MS) has been demonstrated to increase the speed of anal...

  7. Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: A review.

    Masiá, Ana; Suarez-Varela, Maria Morales; Llopis-Gonzalez, Agustin; Picó, Yolanda

    2016-09-14

    Monitoring of pesticides and veterinary drug residues is required to enforce legislation and guarantee food safety. Liquid chromatography-mass spectrometry (LC-MS) is the prevailing technique for assessing both types of residues because LC offers a versatile and universal separation mechanism suitable for non-gas chromatography (GC) amenable and the majority of GC-amenable compounds. This characteristic becomes more relevant when LC is coupled to MS because the high sensitivity and specificity of the detector allows to apply generic sample preparation procedures, which simultaneously extract a wide variety of residues with different physico-chemical properties. Determination of metabolites and degradation products, non-target suspected screening of an increasing number of residues, and even unknowns identification are also becoming inherent LC-MS advantages thanks to the latest advances. For routine analysis and, in particular, for official surveillance purposes in food control, analytical methods properly validated following strict guidelines are needed. After a brief introduction and an outline of the legislation applicable around the world, aspects such as improvement of specificity of high-throughput methods, resolution and mass accuracy of identification strategies and quantitative accuracy are critically reviewed in this article. In them, extraction, separation and determination are emphasized. The main objective is to offer an assessment of the state of the art and identify research needs and future trends in determining pesticide and veterinary drug residues in food by LC-MS. PMID:27566339

  8. 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...

  9. 77 FR 3229 - Codex Alimentarius Commission: Codex Committee on Pesticide Residues (CCPR)

    2012-01-23

    ... [Federal Register Volume 77, Number 14 (Monday, January 23, 2012)] [Notices] [Pages 3229-3230] [FR... Washington, DC, on January 17, 2012. Karen Stuck, U.S. Manager for Codex Alimentarius. [FR Doc. 2012-1160... No. FSIS-2011-0035] Codex Alimentarius Commission: Codex Committee on Pesticide Residues...

  10. 牛奶中有机磷农药残留的气相色谱法测定%Analysis of Organophosphate Pesticide Residues in Milk by Gas Chromatograph

    冷静; 邓斌; 李琦华; 杨舒黎; 苟潇; 毛华明

    2011-01-01

    提出同时测定牛奶中敌百虫、甲胺磷、敌敌畏、马拉硫磷、倍硫磷五种有机磷农药残留的检测方法.在选定的色谱条件下,添加浓度在0.5~10.0μg/mL之间时5种农药的检测限分别为0.031μg/mL、0.013μg/mL、0.023μg/mL、0.019μg/mL和O.014μg/mL,回收率范围分别达81.0%~85.5%、84.5%~89.4%、79.0%~81.8%、77.3%~82.5%和77.9%~89.5%,变异系数在0.29%~3.96%之间.本方法对牛奶中有机磷农药残留的检测分析准确可靠.%Five kinds(Trichlorfon, Methamidophos, Dichlorvos, Malathion and Fenthion) of organophosphate pesticide residues in milk were detected by gas chromatograph(GC). With the selected chromatographic conditions, the lowest detection limit of five kinds of organophosphate pesticide residues were 0.031μg/mL, 0.013μg/mL, 0.023μg/mL, 0.019μg/mL and 0.014μg/mL,respectively,within the linear concentration ranging of 0.5~10.0μm/mL. The recovery(n=3) of five kinds of organophosphate pesticide were 81.0%~85.5%, 84.5%~89.4%, 79.0%~81.8%, 77.3%~82.5% and 77.9%~89.5%, respectively, and the relative standard deviations were 0.29%~3.96%. The method is effective and accurate for determining organophosphate pesticide residues in milk.

  11. 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...

  12. [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

  13. Pesticides

    ... rodents, noxious weeds, and insects. Pesticides help prevent crop loss and, potentially, human disease. According to the ... pesticides. DO NOT mix pesticides. DO NOT set traps or place bait in areas where children or ...

  14. 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

  15. Focused microwave assistance for extracting some pesticide residues from strawberries into water before their determination by SPME/HPLC/DAD.

    Falqui-Cao, C; Wang, Z; Urruty, L; Pommier, J J; Montury, M

    2001-11-01

    A novel and simple method for the determination of some pesticide residues in strawberries using both focused microwave-assisted extraction (FMAE) and solid-phase micro extraction (SPME), coupled with high-performance liquid chromatography (HPLC), has been developed. The pesticides were first extracted from strawberries with water and the assistance of focused microwaves at 30 W for 7 min. Then, an aliquot of the resulting aqueous extract was subjected to SPME with a 60-microm thick poly(dimethylsiloxane)/divinylbenzene (PDMS/DVB) fiber for 45 min at room temperature, with the solution being stirred at 1000 rpm. The extracted pesticides on the SPME fiber were desorbed into the SPME/HPLC interface for quantitative analysis with a diode array detector (DAD). The whole sample pretreatment procedure before chromatographic analysis did not use any organic solvents or involve any blending or centrifugation steps. The five compounds (carbendazim, diethofencarb, azoxystrobine, napropamide, and bupirimate) were chosen because they cannot be analyzed easily by GC. The efficiency of this relatively fast procedure was comparable to that of previously reported methods, with detection limits at low microg/kg levels and linear responses in the range from 0.05 to 1 mg/kg of pesticide in strawberries, with RSDs between 3 and 7.3%, depending on the analyte. In all but one case results obtained by this method for field-incurred samples were comparable to those obtained with traditional methods. PMID:11714287

  16. 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... high and adverse human health impacts or environmental effects from exposure to the pesticides... analysis of milk eliminated the initial extraction step in the tissue method. Contact: Rosemary...

  17. 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.

  18. 宁波市镇海区蔬菜中农药残留状况分析%Analysis on pesticide residues in vegetables in Zhenhai district of Ningbo

    丁坚强; 蔡曦; 钟良康; 谢益君; 陈米娜

    2011-01-01

    目的:了解镇海区不同季节不同蔬菜中农药残留情况,为确保蔬菜食用安全提供监管依据.方法:通过对镇海区蔬菜生产基地和散户生产和镇海各菜场中销售的叶菜类、果菜类、茎菜类、根菜类、花菜类等的农药残留量按季节进行抽样,用气相色谱法对14种有机磷农药和6种拟除虫菊酯类农药进行检测.结果:抽查样本中农药残留量检出率为7.85%,残留量超标率为3.78%.其中蔬菜生产基地农药残留量检出率为3.27%,超标率为0.65%,显著低于散户和菜场中蔬菜的检出率(分别为8.20%和11.54%)和超标率(分别为4.92%和6.92%).在20种检测的农药中,毒死蟀和氯氰菊醋的检出率明显高于其它农药.叶菜类的检出率为11.34%,超标率为8.24%,明显高于其他品种的蔬菜.从时.间上看,农药残留并无明显的季节变化.结论:应采取有效措施,加强蔬菜的监督管理,从源头禁止高毒农药的使用,加大蔬菜种植、销售环节的监测,确保市民食用蔬菜的安全.%Objective:To investigate the conditions of pesticide residues in different seasons in Zhenhai district in order to provide inspection basis for assuring the safety of vegetable intake. Methods: In 2010 year, 344 samples of vegetables were randomly collected from vegetable production base, production of vegetables around the famers and vegetables market in Zhenhai district.The vegetables were random sampling in accordance with leafy vegetables, stem vegetables, root vegetables, cauliflower classes and fruit vegetables categories in different seasons, and measured 14 organophosphorus pesticides and 6 pyrethriod pesticides by GC. Results: The detection rate of pesticide residues in all vegetables was 7.85%, and over - standard rate was 3.78%. The detection rate of Vegetable Production Base was 3. 27%, which was lower than famers (8.20%) and vegetable market ( 11.54% ), and over - standard rate was 0.65% which also was

  19. Pesticide residues in drinking water and associated risk to consumers in Ethiopia.

    Mekonen, Seblework; Argaw, Roba; Simanesew, Aklilu; Houbraken, Michael; Senaeve, David; Ambelu, Argaw; Spanoghe, Pieter

    2016-11-01

    Access to safe and reliable drinking water is vital for a healthy population. However, surface water may be contaminated with pesticides because of the nearby agricultural areas as well as from household application. Water samples were collected from water sources in Jimma zone and Addis Ababa, Ethiopia. The extraction and clean up of the samples were undertaken using liquid-solid and liquid-liquid methods. Human exposure was assessed by calculating the estimated daily intake (EDI) of pesticides in water and compared with the acceptable daily intake (ADI) and the acute reference dose (ARfD). The mean concentrations of 2,4-D, malathion, diazinon and fenpropimorph were 1.59-13.90 μg/l and 0.11-138 µg/l in Jimma and Addis Ababa water sources, respectively. The residue level of some of the pesticides were above the European drinking water guide line values, which is an indication of an illegal use of pesticides in the study areas. Concerning human health risk estimation, there was no acute risk (EDI  ADI) for Jimma and Addis Ababa populations, respectively. A comprehensive monitoring is required to reduce the level of pesticide residues in the water and to minimize particularly the long term human health risks. PMID:27501312

  20. Quantitative structure activity relationship and risk analysis of some pesticides in the goat milk.

    Muhammad, Faqir; Awais, Mian Muhammad; Akhtar, Masood; Anwar, Muhammad Irfan

    2013-01-01

    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. PMID:23369514

  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. Australian national residue survey – closing the loop on pesticide residue risk management for Australian grain

    Reichstein, I.; Healy, K; James, A.; Murray, B.

    2010-01-01

    Australia exports a major proportion of its agricultural production and is highly dependent on maintaining and developing access to, and competitiveness in, export markets. To preserve Australia’s status as a provider of high quality grain, the majority of Australian primary producers rely on pesticides to protect their crops from pests and diseases, particularly in post-harvest situations. The Australian Pesticides and Veterinary Medicines Authority (APVMA) supports Australian agriculture by...

  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. 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.

  5. 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.

  6. Occurrence and estimation of pesticide residues in edible minor crops in southeastern Poland in 2013-2014.

    Podbielska, Magdalena; Szpyrka, Ewa; Matyaszek, Aneta; Słowik-Borowiec, Magdalena; Rupar, Julian; Kurdziel, Anna

    2016-07-01

    This paper presents the results of official control of pesticide residues in minor crops collected in southeastern Poland in 2013-2014. Compliance of used pesticides with applicable law was also verified, and determined residues were compared to maximum residue levels (MRLs) provided for in Regulation (EC) No. 395/2005. A total of 583 samples of 25 different types of fresh fruit and vegetables were analyzed for pesticide residues. Pesticide residues were detected in 158 samples (27.1 % of the analyzed samples). According to the European Commission Health & Consumer Protection Directorate-General (SANCO) guidelines document, MRL violations were understood as cases where a residue level exceeded the MRL after the uncertainty of the method (50 %) was considered. MRL violations were found in four samples. The usage of unauthorized pesticides was detected in 5.8 % of analyzed samples. Substances banned in Poland were found in two samples. Fungicides were the most frequently detected group of pesticides. Pesticide residues were most commonly found in fruit samples (19.4 % of all analyzed samples), mainly in gooseberry, redcurrant, and huckleberry. The majority of samples were compliant with MRLs, which means that they were suitable for trade. PMID:27251221

  7. 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

  8. Determination and Analysis of Residues of Organochlorine Pesticides in Ophiopogon japonicus from Sichuan Province%川麦冬残留有机氯农药含量的测定与分析

    徐作英; 严伟; 刘菲; 燕旎

    2011-01-01

    [Objective]The aim was to determine residues of organochlorine pesticides in geo-authentic crude drugs Ophiopogon japonicus from Sichuan Province, and judge the quality of 0. Japonicus, so as to provide experimental data for the establishment of quality standard. [Method] With 0. Japonicus from Santai County of Sichuan Province as material, the contents of BHC, DDT and PCNB were determined by gas chromatog-raphy. [ Result ] The contents of residues of organochlorine pesticides in O. Japonicus from Santai County were all under the standards. [Conclusion] It was proved the superiority of 0. Japonicus as Sichuan Province geo-authentic crude drug from residues of organochlorine pesticides, which was accordance with CAP standard and food standard.%[目的]测定四川道地药材—“川麦冬”中残留有机氯农药的含量,以评判川麦冬作为四川道地药材的质量情况,为川麦冬药材质量标准的制定提供了试验数据,也为三台县所产麦冬作为四川道地药材的用药质量提供了依据.[方法]以四川三台县所产川麦冬为材料,采用气相色谱法测定其总六六六(BHC)、总滴滴涕(DDT)和五氯硝基苯(PCNB)的含量.[结果]三台县所产川麦冬中残留有机氧农药含量均低于限量标准.[结论]从有机氯农药残留含量方面印证了川麦冬作为四川道地药材的优越性,符合国家中药材GAP标准和食品标准.

  9. 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

  10. 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

  11. 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)

  12. 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.

  13. 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 ...

  14. 生鲜乳中农兽药残留限量分析比对%Comparison and analysis study of veterinary and pesticide residue limits standard in raw milk

    王建军; 黄菲菲; 赵嘉胤; 楼飞; 刘永琦

    2011-01-01

    Food standards about maximum residue limits (MRLs)of veterinary drug and pesticide were collected in this paper, which analyzed the differences among CAC ,America,Canada,EU,Japan,New Zealand,Australia and Chinese standards. some measures and advices were proposed for improving national standards.%整理了国际食品法典(CAC)、美国、加拿大、欧盟、日本、新西兰、澳大利亚以及我国生鲜乳中农兽药残留限量,分析了我国与其他国家或组织生鲜乳中农兽药残留限量标准存在的差异,并提出了完善我国生鲜乳中农兽药残留限量标准的措施和建议.

  15. Current mass spectrometry strategies for the analysis of pesticides and their metabolites in food and water matrices.

    Botitsi, Helen V; Garbis, Spiros D; Economou, Anastasios; Tsipi, Despina F

    2011-01-01

    Analysis of pesticides and their metabolites in food and water matrices continues to be an active research area closely related to food safety and environmental issues. This review discusses the most widely applied mass spectrometric (MS) approaches to pesticide residues analysis over the last few years. The main techniques for sample preparation remain solvent extraction and solid-phase extraction. The QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) approach is being increasingly used for the development of multi-class pesticide residues methods in various sample matrices. MS detectors-triple quadrupole (QqQ), ion-trap (IT), quadrupole linear ion trap (QqLIT), time-of-flight (TOF), and quadrupole time-of-flight (QqTOF)-have been established as powerful analytical tools sharing a primary role in the detection/quantification and/or identification/confirmation of pesticides and their metabolites. Recent developments in analytical instrumentation have enabled coupling of ultra-performance liquid chromatography (UPLC) and fast gas chromatography (GC) with MS detectors, and faster analysis for a greater number of pesticides. The newly developed "ambient-ionization" MS techniques (e.g., desorption electrospray ionization, DESI, and direct analysis in real time, DART) hyphenated with high-resolution MS platforms without liquid chromatography separation, and sometimes with minimum pre-treatment, have shown potential for pesticide residue screening. The recently introduced Orbitrap mass spectrometers can provide high resolving power and mass accuracy, to tackle complex analytical problems involved in pesticide residue analysis. PMID:24737632

  16. 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.

  17. Organic amendments for risk mitigation of organochlorine pesticide residues in old orchard soils.

    Centofanti, Tiziana; McConnell, Laura L; Chaney, Rufus L; Beyer, W Nelson; Andrade, Natasha A; Hapeman, Cathleen J; Torrents, Alba; Nguyen, Anh; Anderson, Marya O; Novak, Jeffrey M; Jackson, Dana

    2016-03-01

    Performance of compost and biochar amendments for in situ risk mitigation of aged DDT, DDE and dieldrin residues in an old orchard soil was examined. The change in bioavailability of pesticide residues to Lumbricus terrestris L. relative to the unamended control soil was assessed using 4-L soil microcosms with and without plant cover in a 48-day experiment. The use of aged dairy manure compost and biosolids compost was found to be effective, especially in the planted treatments, at lowering the bioavailability factor (BAF) by 18-39%; however, BAF results for DDT in the unplanted soil treatments were unaffected or increased. The pine chip biochar utilized in this experiment was ineffective at lower the BAF of pesticides in the soil. The US EPA Soil Screening Level approach was used with our measured values. Addition of 10% of the aged dairy manure compost reduced the average hazard quotient values to below 1.0 for DDT + DDE and dieldrin. Results indicate this sustainable approach is appropriate to minimize risks to wildlife in areas of marginal organochlorine pesticide contamination. Application of this remediation approach has potential for use internationally in areas where historical pesticide contamination of soils remains a threat to wildlife populations. PMID:26716732

  18. Organic amendments for risk mitigation of organochlorine pesticide residues in old orchard soils

    Centofantia, Tiziana; McConnell, Laura L.; Chaney, Rufus L.; Beyer, W. Nelson; Andradea, Natasha A.; Hapeman, Cathleen J.; Torrents, Alba; Nguyen, Anh; Anderson, Marya O.; Novak, J. M.; Jackson, Dana

    2015-01-01

    Performance of compost and biochar amendments for in situ risk mitigation of aged DDT, DDE and dieldrin residues in an old orchard soil was examined. The change in bioavailability of pesticide residues to Lumbricus terrestris L. relative to the unamended control soil was assessed using 4-L soil microcosms with and without plant cover in a 48-day experiment. The use of aged dairy manure compost and biosolids compost was found to be effective, especially in the planted treatments, at lowering the bioavailability factor (BAF) by 18–39%; however, BAF results for DDT in the unplanted soil treatments were unaffected or increased. The pine chip biochar utilized in this experiment was ineffective at lower the BAF of pesticides in the soil. The US EPA Soil Screening Level approach was used with our measured values. Addition of 10% of the aged dairy manure compost reduced the average hazard quotient values to below 1.0 for DDT + DDE and dieldrin. Results indicate this sustainable approach is appropriate to minimize risks to wildlife in areas of marginal organochlorine pesticide contamination. Application of this remediation approach has potential for use internationally in areas where historical pesticide contamination of soils remains a threat to wildlife populations.

  19. 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

  20. Rapid detection of pesticides not amenable to multi-residue methods by flow injection-tandem mass spectrometry

    Mol, J.G.J.; Dam, van R.C.J.

    2014-01-01

    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 includ

  1. LITERATURE REVIEW AND EVALUATION OF THE EPA FOOD-CHAIN (KENAGA) NOMOGRAM, AN INSTRUMENT FOR ESTIMATING PESTICIDE RESIDUES ON PLANTS

    The Kenaga nomogram is a simple device developed by the U.S. Environmental Protection Agency (EPA) in the early 1980s and is currently used to predict the maximum potential pesticide residue levels in the food chain of wildlife before pesticide registration. o evaluate the accura...

  2. 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...

  3. Quantitative Structure activity relationship and risk analysis of some pesticides in the cattle milk

    Faqir Muhammad*, Ijaz Javed, Masood Akhtar1, Zia-ur-Rahman, Mian Muhammad Awais1, Muhammad Kashif Saleemi2 and Muhammad Irfan Anwar3

    2012-01-01

    Milk of cattle was collected from various localities of Faisalabad, Pakistan. Pesticides concentration was determined by HPLC using solid phase microextraction. The residue analysis revealed that about 40% milk samples were contaminated with pesticides. The mean±SE levels (ppm) of cyhalothrin, endosulfan, chlorpyrifos and cypermethrin were 0.38±0.02, 0.26±0.02, 0.072±0.01 and 0.085±0.02, respectively. Quantitative structure activity relationship (QSAR) models were used to predict the residues...

  4. 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...

  5. Organochlorine pesticide residues in paddy fish in Malaysia and the associated health risk to farmers*

    Chen, Donald F.; Meier, Peter G.; Hilbert, Morton S.

    1984-01-01

    Paddy fish (Trichogaster pectoralis Regan) were collected from five sampling locations in a major paddy-growing area of Malaysia and analysed for organochlorine residues. During the same period, ten farming families, chosen at random from each of the five sampling sites, were interviewed. Information was obtained about the quantity of paddy fish consumed, the amount and type of pesticide used on the paddy-field, and the frequency of application.

  6. 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 ...

  7. 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...

  8. Assessment of Pesticide and Heavy Metal Residues in Tilapia Fish From Machakos and Kiambu Counties, Kenya.

    Omwenga, Isaac Mokaya

    2013-01-01

    Exposure to pesticides, heavy metals and other chemical residues cause harmful effects; they can cause injury to human health as well as to the environment. Humans take up these chemicals through skin absorption, respiration and ingestion of contaminated food. Among all foods, fish is one of the main sources of chemical contaminants although fish products account only for about 10% of diet or less. The present study was conducted in Kiambu and Machakos counties with objectives of determining ...

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

    Abong'o, D.A.; Wandiga, S.O.; Jumba, I.O.; Brink, van den, R.B.A.; 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...

  10. 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...

  11. Organophosphorus pesticide residues in raw milk and infant formulas from Spanish northwest.

    Melgar, M J; Santaeufemia, M; Garcia, M A

    2010-10-01

    Residue levels of seven organophosphorus pesticides (OPPs), widely used as dairy cattle ectoparasiticides or in crops used for animal feed, were determined in raw milk and infant formulas. A total of 312 samples were collected (70 from infant formulas and 242 from raw milk) biweekly during a 24-month period. Pesticides were extracted by means of a solid phase system into acetone. An extract aliquot of acetone was injected into a gas chromatograph (GC) with a nitrogen-phosphorus detector. Recoveries of pesticides spiked in milk samples were 62.2 - 97.2 %. The frequency of total samples containing detectable levels of OPP residues was 6.73 % in total milk and 8.67 % in raw milk. The highest percentage incidence measured was for dichlorvos (5.78 %), followed by coumaphos (2.06 %), and parathion methyl (0.83 %). The range of positive results was calculated to be between 0.005 and 0.220 mg kg(- 1). No residue was detected in the final product (infant formulas), so any risk to consumer health, especially to children's health, would be limited. PMID:20803361

  12. 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)

  13. 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.

  14. The effect of pesticide residue on caged mosquito bioassays.

    Barber, J A S; Greer, Mike; Coughlin, Jamie

    2006-09-01

    Wind tunnel experiments showed that secondary pickup of insecticide residue by mosquitoes in cage bioassays had a significant effect on mortality. Cage bioassays using adult Ochlerotatus taeniorhynchus (Wiedemann) investigated the effect of exposure time to a contaminated surface. Cages were dosed in a wind tunnel using the LC50 for naled (0.124 mg a.i./ml) and an LC25 (0.0772 mg a.i./ml) for naled. Half of the bioassay mosquitoes were moved directly into clean cages with the other half remaining in the sprayed, hence contaminated, cage. Treatment mortality was assessed at 8, 15, 30, 60, 120, 240, and 1,440 min postapplication. Cage contamination had a significant effect on mosquito mortality for both the LC25 and LC50 between 15 and 30 min postapplication. PMID:17067048

  15. Safe apples for baby-food production: survey of pesticide treatment regimes leaving minimum residues.

    Ticha, Jana; Hajslova, Jana; Kovalczuk, Tomas; Jech, Martin; Honzicek, Jiri; Kocourek, Vladimir; Lansky, Miroslav; Kloutvorova, Jana; Falta, Vladan

    2007-06-01

    A total of 19 pesticide preparations were used according to agricultural practice in six trials in apple orchards. Using gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS), premature Golden Delicious apples collected 64, 50, 36 days before harvest and mature fruit were examined for residues of active ingredients. No residues of triflumuron, triazamate, chlorpyrifos, etofenprox, fenoxycarb, kresoxim-methyl, cyprodinyl, difenoconazole or thiram were detected in the first sampling. Also, the levels of chlorpyrifos-methyl, penconazole, tebuconazole and tolylfluanid dropped during the pre-harvest interval. Detectable residues of pyridaben, thiacloprid, trifloxystrobin and tetraconazole in harvested fruits were below 0.01 mg kg(-1), which is the maximum concentration of residues acceptable by baby-food producers in any raw material. The only residues exceeding this concentration were captan and teflubenzuron. Based on the data, farmers can choose pesticides for optimal treatment of plants, while enabling growth of a safe crop suitable for baby-food production. PMID:17487602

  16. 78 FR 56185 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2013-09-12

    ..., filtration, partition, and cleanup with analysis by high performance liquid chromatography (HPLC...), and citrus, oil at 32.0 ppm. Residues of the individual analytes are detectable and quantifiable using three separate analytical methods. Residues of diflubenzuron (DFB) were quantitated by...

  17. 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

  18. Detection of Pesticide Residues in Organic and Conventional Fruits and Vegetables Available in Ireland Using Gas Chromotography/Tandem Mass Spectrometry (GC-MS/MS and Liquid Chromotography/Tandem Mass Spectrometry (LC-MS/MS Detection

    Rachel Tobin

    2014-02-01

    Full Text Available Irish organic consumers believe that organic foods are a healthier choice due to the lack of synthetic pesticides used in organic agricultural practices; however, few scientific studies have shown that organic samples are void of any pesticide residues. Nine different fruit and vegetable types of organic and conventional origin were sampled from large supermarkets. Analysis for 465 pesticide residues was carried out using GC-MS/MS and LC-MS/MS analysis. Of the 27 organic samples tested, 15 contained one or more detected pesticide residues, with one of these being above the limit of quantification (LOQ for the method, imazalil in organic onion, 11.13 ng/g. Of the conventional samples 17 of the 27 samples contained one or more residues. Twelve of the residues detected in conventional samples were above the LOQ with concentrations ranging from 9.84 to 154.10 ng/g. A similar number of organic (15 and conventional (17 samples tested positive for detectable residues, however the number of residues detected was higher in conventional (43 than in organic (29, and the concentration of these residues were higher. It is concluded that it cannot be said that organic fruits and vegetables are void of pesticides based on the results of this study.

  19. Concentrations of pesticide residues in tissues of fish from Kolleru Lake in India.

    Amaraneni, S R; Pillala, R R

    2001-01-01

    Kolleru Lake is the largest natural freshwater lake of Andhra Pradesh in India. It is situated between latitudes 16 degrees 32' and 16 degrees 47'N and longitudes 81 degrees 05' and 81 degrees 27'E. The use of pesticides for agricultural purposes is widespread in the Kolleru Lake region. The biological indicators like fish help in the studies of aquatic pollution by pesticides. Fish species Channa striata and Catla catla and water samples were collected from Kolleru Lake in each of three seasons over a period of three years. Fish samples were analyzed according to a modified method which is proposed for the gas chromatographic determination for the pesticides viz., alpha-BHC, gamma-BHC, malathion, chloirpyrifos, isodrin, endosulfan, dieldrin, and p,p-DDT. Water samples were analyzed for selected physico-chemical parameters. The extraction efficiency for the selected pesticides is between 82.8% and 91.2%. The maximum concentrations of pesticide residues in Kolleru Lake fish on wet weight basis are 123.8 micrograms/g for alpha-BHC, 98.7 micrograms/g for gamma-BHC, 2.5 micrograms/g for malathion, 88.6 micrograms/g for chlorpyrifos, 0.91 microgram/g for isodrin, 76.5 micrograms/g for endosulfan, 1.98 micrograms/g for dieldrin, and 157.4 micrograms/g for p,p'-DDT. These analyses were used to evaluate the baseline data and the pesticide pollution in the lake's ecosystem. PMID:11769254

  20. 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

  1. Ecological risk analysis of pesticides used on irrigated rice crops in southern Brazil.

    Vieira, Danielle Cristina; Noldin, José Alberto; Deschamps, Francisco C; Resgalla, Charrid

    2016-11-01

    Based on studies conducted in the past decade in the southern region of Brazil to determine residue levels of the pesticides normally used on irrigated rice crops, changes can be observed in relation to the presence of pesticides in the waters of the main river basins in Santa Catarina State. In previous harvests, the presence of residues of 7 pesticides was determined, with the herbicide bentazon and the insecticide carbofuran being the products showing highest frequency. Following toxicological tests conducted with 8 different test organisms, deterministic and probabilistic risk analysis was performed to assess the situation of the river basins in areas used for the production of irrigated rice. Of the species tested, the herbicide bentazon showed greatest toxicity toward plants, but did not present an ecological risk because in the worst-case scenario the highest concentration of this pesticide in the environment is 37 times lower than the lowest EC50/LC50 value obtained in the tests. The insecticide carbofuran, which had the highest toxicity toward the organisms used in the tests, presented an ecological risk in the deterministic analysis, but without any associated probability. The results highlight the need for increased efforts in training farmers in crop management practices and for the continual monitor of water bodies for the presence of pesticide residues. PMID:27479455

  2. Solid-phase microextraction coupled with high performance liquid chromatography: a complementary technique to solid-phase microextraction-gas chromatography for the analysis of pesticide residues in strawberries.

    Wang, Z; Hennion, B; Urruty, L; Montury, M

    2000-11-01

    Solid-phase microextraction coupled with high performance liquid chromatography has been studied for the analysis of methiocarb, napropamide, fenoxycarb and bupirimate in strawberries. The strawberries were blended and centrifuged. Then, an aliquot of the resulting extracting solution was subjected to solid-phase microextraction (SPME) on a 60 microns polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre for 45 min at room temperature. The extracted pesticides on the SPME fibre were desorbed into SPME/high performance liquid chromatography (HPLC) interface for HPLC analysis with diode-array detection (DAD). The method is organic solvent-free for the whole extraction process and is simple and easy to manipulate. The detection limits were shown to be at low microgram kg-1 level and the linear response covered the range from 0.05 to 2 mg kg-1 of pesticides in strawberries with a regression coefficient larger than 0.99. A good repeatability with RSDs between 2.92 and 9.25% was obtained, depending on compounds. PMID:11271705

  3. A smartphone-readable barcode assay for the detection and quantitation of pesticide residues.

    Guo, Juan; Wong, Jessica X H; Cui, Caie; Li, Xiaochun; Yu, Hua-Zhong

    2015-08-21

    In this paper, we present a smartphone-readable barcode assay for the qualitative detection of methyl parathion residues, a toxic organophosphorus pesticide that is popularly used in agriculture worldwide. The detection principle is based on the irreversible inhibition of the enzymatic activity of acetylcholinesterase (AchE) by methyl parathion; AchE catalytically hydrolyzes acetylthiocholine iodine to thiocholine that in turn dissociates dithiobis-nitrobenzoate to produce a yellow product (deprotonated thio-nitrobenzoate). The yellow intensity of the product was confirmed to be inversely dependent on the concentration of the pesticide. We have designed a barcode-formatted assay chip by using a PDMS (polydimethylsiloxane) channel plate (as the reaction reservoir), situated under a printed partial barcode, to complete the whole barcode such that it can be directly read by a barcode scanning app installed on a smartphone. The app is able to qualitatively present the result of the pesticide test; the absence or a low concentration of methyl parathion results in the barcode reading as "-", identifying the test as negative for pesticides. Upon obtaining a positive result (the app reads a "+" character), the captured image can be further analyzed to quantitate the methyl parathion concentration in the sample. Besides the portability and simplicity, this mobile-app based colorimetric barcode assay compares favorably with the standard spectrophotometric method. PMID:26087169

  4. A micro-machined thin film electro-acoustic biosensor for detection of pesticide residuals

    Jing-jing WANG; Wei-hui LIU; Da CHEN; Yan XU; Lu-yin ZHANG

    2014-01-01

    Increasing awareness concerning food safety problems has been driving the search for simple and efficient bio-chemical analytical methods. In this paper, we develop a portable electro-acoustic biosensor based on a film bulk acoustic reso-nator for the detection of pesticide residues in agricultural products. A shear mode ZnO film bulk acoustic resonator with a mi-cro-machining structure was fabricated as a mass-sensitive transducer for the real-time detection of antibody-antigen reactions in liquids. In order to obtain an ultra-low detection level, the artificial antigens were immobilized on the sensing surface of the resonator to employ a competitive format for the immunoassays. The competitive immunoreactions can be observed clearly through monitoring the frequency changes. The presence of pesticides was detected through the diminution of the frequency shift compared with the level without pesticides. The limit of detection for carbaryl (a widely used pesticide for vegetables and crops) is 2´10-10 M. The proposed device represents a potential alternative to the complex optical systems and electrochemical methods that are currently being used, and represents a significant opportunity in terms of simplicity of use and portability for on-site food safety testing.

  5. 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

  6. 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).

  7. 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 Σ 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 (ΣDDT and ΣOCs) 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

  8. 农药残留检测方法及光谱技术在生菜农残检测中的应用%Study on Methods of Detecting Pesticide Residues and Application of Spectrum Technique in the Detection of Pesticide Residues in Lettuce

    孙俊; 董梁; 张梅霞; 刘枭; 邬婷; 高洪燕

    2014-01-01

    蔬菜农药残留给人们健康饮食带来很大安全隐患。为此,综述了几大类农药残留检测方法:活体测定法、理化检测法、快速检测法和光谱检测法,分析了它们各自特点。同时,基于光谱技术对生菜叶片上的农残进行了检测试验,比较了有农残叶片光谱与无农残叶片光谱,并通过PCA算法进行光谱特征提取,结合学习向量量化神经网络建立农残鉴别模型,取得了较好的鉴别结果。%Pesticide residues in vegetables bring the great hidden dangers to the health of people .This paper reviews sev-eral kinds of pesticide residue detection methods , including bioassay method , chemical method , rapid detection method and spectral analysis method , and analyses their characteristics .In this paper , the pesticide residue in lettuce leaves were detected based on spectral techniques , and the spectra of the blades having pesticide residues were compared with the ones of the blades without pesticide residues .PCA algorithm was used for spectral feature extraction , and LVQ ( Learn-ing Vector Quantization ) neural network was used to set up model of identification of pesticide residues , and the identifi-cation result was good .

  9. Prediction of the processing factor for pesticides in apple juice by principal component analysis and multiple linear regression.

    Martin, L; Mezcua, M; Ferrer, C; Gil Garcia, M D; Malato, O; Fernandez-Alba, A R

    2013-01-01

    The main objective of this work was to establish a mathematical function that correlates pesticide residue levels in apple juice with the levels of the pesticides applied on the raw fruit, taking into account some of their physicochemical properties such as water solubility, the octanol/water partition coefficient, the organic carbon partition coefficient, vapour pressure and density. A mixture of 12 pesticides was applied to an apple tree; apples were collected after 10 days of application. After harvest, apples were treated with a mixture of three post-harvest pesticides and the fruits were then processed in order to obtain apple juice following a routine industrial process. The pesticide residue levels in the apple samples were analysed using two multi-residue methods based on LC-MS/MS and GC-MS/MS. The concentration of pesticides was determined in samples derived from the different steps of processing. The processing factors (the coefficient between residue level in the processed commodity and the residue level in the commodity to be processed) obtained for the full juicing process were found to vary among the different pesticides studied. In order to investigate the relationships between the levels of pesticide residue found in apple juice samples and their physicochemical properties, principal component analysis (PCA) was performed using two sets of samples (one of them using experimental data obtained in this work and the other including the data taken from the literature). In both cases the correlation was found between processing factors of pesticides in the apple juice and the negative logarithms (base 10) of the water solubility, octanol/water partition coefficient and organic carbon partition coefficient. The linear correlation between these physicochemical properties and the processing factor were established using a multiple linear regression technique. PMID:23281800

  10. 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.

  11. 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

  12. Multiresidue Method for Determination of 183 Pesticide Residues in Leeks by Rapid Multiplug Filtration Cleanup and Gas Chromatography-Tandem Mass Spectrometry.

    Zou, Nan; Han, Yongtao; Li, Yanjie; Qin, Yuhong; Gu, Kejia; Zhang, Jingru; Pan, Canping; Li, Xuesheng

    2016-08-10

    This study reports the development of a novel multiplug filtration cleanup (m-PFC) procedure for analysis of pesticide residues in leek samples followed by gas chromatography-tandem mass spectrometry detection. The leek samples were initially purified following the dispersive solid-phase extraction with different sorbents to determine the most suitable proportioning of sorbent materials; then, the m-PFC method was carried out by applying the streamlined procedure with syringes. Average recoveries of most pesticides were in the range from 70.2 to 126.0% with the relative standard deviation market samples. In that analysis, 35 pesticides were detected in 29 samples, with values ranging from 2.0 to 9353.1 μg kg(-1). PMID:26651870

  13. 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

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

    Kästner, M.; Nowak, K. M.; Miltner, A.;

    2015-01-01

    .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......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...... 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...

  15. 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...

  16. 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...

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

    Skretteberg, L. G.; Lyrån, B.; Holen, B.;

    2015-01-01

    Fruits and vegetables from Souteast Asia were analysed for the presence of pesticide residues. A total of 721 samples of 63 different commodities were collected in 2011. The products were imported to Denmark, Finland, Norway and Sweden from ten countries; about 80% were imported from Thailand...... 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...

  18. 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)

  19. 脐橙和蜜桔农药残留调查及风险评估%Pesticide Residue Investigation and Risk Assessment of Navel Orange and Orange

    吕蓉

    2015-01-01

    调查江西省脐橙和蜜桔的农药残留情况并进行风险评估. 对江西省2013年脐橙和蜜桔的144个送检样品中的36种农药残留进行定量检测分析.2013年9月至12月江西省的脐橙和蜜桔质量安全较为稳定,农药残留超标率为0.毒死蜱、啶虫脒、杀扑磷、抑霉唑4种农药有检出,12月份抑霉唑的检出率最高.3个月的农药安全指数均小于1,说明检测的36种农药均在可接受的风险程度内,没有安全风险.本研究可为江西省脐橙和蜜桔质量安全监管提供参考.%The aim was to investigate and estimate risk of pesticide residue in navel orange and orange in Jiangxi province. 36 pesticides residues in 144 samples of navel orange and orange in Jiangxi province were determined by quantitative analysis. The results showed that the quality of navel orange and orange in Jiangxi province is stable and safety from september to october in 2013. Pesticide residues over standard in navel orange and orange were zero. Chlorpyrifos,acetamiprid,methidathion,imazalil were checked out,the detection rate of imazalil is highest in December. Safety indexes of all pesticides were lower than 1 in each sample during three month,showing that 36 pesticide residues were safe. The paper provides a theoretical basis for supervising navel orange and orange safety in Jiangxi province.

  20. Pesticide residues in fruit samples: comparison of different QuEChERS methods using liquid chromatography-tandem mass spectrometry.

    Christia, C; Bizani, E; Christophoridis, C; Fytianos, K

    2015-09-01

    Acetate- and citrate-buffered quick, easy, cheap, effective, rugged, safe (QuEChERS) pretreatment methods were evaluated for the determination of various pesticides in peaches, grapes, apples, bananas, pears, and strawberries from various regions of Greece, using LC-MS/MS. The purposes of this study were (i) to evaluate which type of QuEChERS method was the most appropriate and effective for each matrix; (ii) to apply the selected QuEChERS method for each matrix, in order to detect and quantify pesticide residues in various fruit samples using UPLC-MS/MS; (iii) to examine the concentration distribution of pesticide classes among fruit originating from various areas; and (iv) to assess pesticide concentration distribution between peel and flesh of fruit in order to evaluate the penetration of pesticide residues in the fruit flesh. Acetate-buffered QuEChERS was found to be the most suitable technique for most of the fruit matrices. According to the recovery values at two different concentration levels, peaches should preferably be treated by the citrate-buffered type, whereas grapes, bananas, apples, pears, and strawberries are best treated by the acetate-buffered version, although the differences in efficiency were small. The addition of graphitized carbon black significantly decreases the recovery of specific pesticides in all matrices except for strawberries. The majority of values do not exceed the official maximum residue levels set by the European Commission. Organophosphates proved to be the most commonly detected category along with triazines-triazoles-conazoles group and by carbamates. Apples and pears seem to be the most contaminated fruit matrices among those tested. Distribution of pesticide classes shows variations between different regions, suggesting different pesticide application practices. In the case of peaches and pears, there is an equal distribution of detected pesticides between peel and flesh, indicating penetration of contaminants into the

  1. 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)

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

    Luo, Yuzhou; Zhang, Minghua

    2009-12-01

    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. PMID:19616876

  3. Pyrotechnic reaction residue particle analysis.

    Kosanke, Kenneth L; Dujay, Richard C; Kosanke, Bonnie J

    2006-03-01

    Pyrotechnic reaction residue particle (PRRP) production, sampling and analysis are all very similar to that for primer gunshot residue. In both cases, the preferred method of analysis uses scanning electron microscopy to locate suspect particles and then uses energy dispersive x-ray spectroscopy to characterize the particle's constituent chemical elements. There are relatively few times when standard micro-analytical chemistry performed on pyrotechnic residues may not provide sufficient information for forensic investigators. However, on those occasions, PRRP analysis provides a greatly improved ability to discriminate between materials of pyrotechnic origin and other unrelated substances also present. The greater specificity of PRRP analysis is the result of its analyzing a large number of individual micron-sized particles, rather than producing only a single integrated result such as produced using standard micro-analytical chemistry. For example, PRRP analyses are used to demonstrate its ability to successfully (1) discriminate between pyrotechnic residues and unrelated background contamination, (2) identify that two different pyrotechnic compositions had previously been exploded within the same device, and (3) establish the chronology of an incident involving two separate and closely occurring explosions. PMID:16566762

  4. Pesticides and other chemical residues in infant and toddler total diet samples: i. august 1974-july 1975

    Johnson, R.D.; Manske, D.D.; New, D.H.; Podrebarac, D.S.

    1979-12-01

    Results of a program conducted by FDA to monitor chemical and pesticide levels in food processed for consumption by infants and toddlers are presented. In infant foods, 306 residues of 28 different coumpounds were found in the August 1974-July 1975 period; 468 residues of 30 different compounds were present in toddler food. Residues found included heavy metals, dieldrin, DDE, and hexachlorobenzene. (12 references, 6 tables)

  5. 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

  6. 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

  7. 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

  8. Pesticide adsorptivity of aged particulate matter arising from crop residue burns.

    Yang, Yaning; Sheng, Guangyao

    2003-08-13

    Particulates (ashes) arising from the burning of crop residues are potentially effective adsorbents for pesticides in agricultural soils. To determine the long-term adsorptive sustainability of ashes, a wheat (Triticum aestivum L.) ash was aged under environmentally relevant conditions (in CaCl(2) solution at room temperature and pH 7) in soil extract for 1 month and in a soil (1% ash) for a period of up to 12 months. The aged ash and ash-amended soil were used to sorb diuron from water. The diuron sorption was also measured in the presence of atrazine as a competing pesticide. There was no observed microbial impact on the stability of the wheat ash in soil. All isotherms with the ash were nonlinear type-I curves, suggestive of the surface adsorption. On a unit mass basis, the ash in soil extract was 600-10000 times more effective than the soil in sorbing diuron. Adsorption of dissolved soil organic matter (DOM) during aging on the ash surfaces reduced the diuron adsorption by 50-60%. Surface competition from the atrazine adsorption also reduced the ash adsorption of diuron by 10-30%. A total of 55-67% reduction in diuron sorption by the ash-amended soil was observed. Due to its high initial adsorptivity, the ash fraction of the aged ash-amended soil contributed >50% to the total diuron sorption. Thus, the wheat ash aged in the soil remained highly effective in adsorbing diuron. As crop residues are frequently burned in the field, pesticides in agricultural soils may be highly immobilized due to the presence of ashes. PMID:12903968

  9. Simultaneous determination of pyrethroids from pesticide residues in porcine muscle and pasteurized milk using GC.

    Khay, Sathya; Abd El-Aty, A M; Choi, Jeong-Heui; Shin, Eun-Ho; Shin, Ho-Chul; Kim, Jin-Suk; Chang, Byung-Joon; Lee, Chi-Ho; Shin, Sung-Chul; Jeong, Ji Yoon; Shim, Jae-Han

    2009-01-01

    The principal goal of this work was to develop an efficient method for the simultaneous determination of four pyrethroid (PYR) insecticides, cyfluthrin, cyhalothrin, cypermethrin, and deltamethrin, in porcine muscle and pasteurized milk using liquid-liquid extraction (LLE). Sample extraction was carried out with and without additional column cleanup procedures, and the final determination was made using GC with electron-capture detector (ECD). The pesticide identity was confirmed using GC-MS in the SIM mode. Since there were minor differences between the extraction procedures, extraction without the additional cleanup procedure was used throughout the work. The method was validated by fortifying blank samples with half, two, and four times the maximum residue limit (MRL) of each PYR. The average recoveries (n = 6) ranged from 83.5 to 99.2% and 82.9 to 109% in porcine muscle and pasteurized milk, respectively. The repeatability of measurements expressed as RSDs, was in the range of 1.7-11.9 and 1.5-10.3% in porcine muscle and pasteurized milk, respectively. The LODs ranged from 3.3 to 9 and 3 to 8.1 ppm, whereas the LOQs ranged from 10 to 27.4 and 9 to 24.6 ppm, in porcine muscle and pasteurized milk, respectively. The applicability of the method was demonstrated by analyzing real samples collected from major cities in the Republic of Korea. No residues of the selected pesticides were detected in any of the samples. PMID:19107766

  10. 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.

  11. 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....

  12. 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

  13. 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...

  14. 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

  15. 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

  16. Decontamination of organochlorine pesticides residue and heavy metal in Rehmannia glutinosa Libosch by SFE.

    Zhao, Chunjie; Bai, Lu; Ou, Yingfu; Li, Dan; Xin, Chunhong

    2009-01-01

    A method involving the simultaneous extraction and decontamination of 12 organochlorine pesticides (OCPs) and seven heavy metals (HM) from Rehmannia glutinosa Libosch was established using supercritical fluid extraction (SFE). A gas chromatography (GC) method with electron capture detection was employed for the determination of the OCPs. The quantitative determination of active constituents (iridoid glycoside and catalpol) in Rehmannia glutinosa Libosch was detected by high-performance liquid chromatography (HPLC). An atomic absorption spectrometry (AAS) was designed for the determination of seven HM, including lead (Pb), cadmium (Cd), copper (Cu), iron (Fe), zinc (Zn), arsenic (As), and mercury (Hg) in Rehmannia glutinosa Libosch. Recovery of the determination of the 12 organochlorine pesticides in Rehmannia glutinosa Libosch sample was 85.9%-101.4% by GC, and relative standard deviation (RSD) was 1.9%-6.0%. Catalpol determination with HPLC in a Rehmannia glutinosa Libosch sample was 0.2486 and 0.2559 mg/mL before and after decontaminating OCPs by SFE, respectively. Those were 0.2486 and 0.2632 mg/mL before and after decontaminating HM by SFE, respectively. After a series of experiments to optimize the final SFE, the following conditions were used to determine the OCPs: pure CO(2), extraction pressure of 15 Mpa, extraction temperature of 60 degrees C, extraction time of 30 min, flow rate at 35 kg/h, and the final SFE conditions of HM was pure CO(2), extraction pressure of 18 Mpa, extraction temperature of 50 degrees C, extraction time of 20 min, modifier at 2.5 mL/50 g. The SFE was used to remove the 12 OCP residues and seven HM residues from Rehmannia glutinosa Libosch with less residue left and negligible loss of the active constituent catalpol. PMID:19930806

  17. 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

  18. Residual Characteristics of Organochlorine Pesticides in Lou Soils with Different Fertilization Modes

    2006-01-01

    Soil samples with three fertilization treatments (no fertilizer, corn straw and farm manure) collected from a Lou soil(Eum-orthic Anthrosol classfied using Chinese Soil Taxonomy) in northwestern China were analysed for residual levels and their characteristics of organochlorine pesticides (α-HCH,β-HCH, γ-HCH, δ-HCH, HCB, o, p'-DDT, p, p'-DDT, o, p'-DDE, p, p'-DDE, p, p'-DDD, α-endosulfan, dieldrin and endrin). Organochlorine pesticides (OCPs) were detected in all soil samples except δ-HCH and their total concentrations ranged from 159.31 ± 9.00 to 179.77 ± 2.58 ng g-1 with an order of HCHs > DDTs > (dieldrin + endrin) > HCB >α-endosulfan. Among all the compounds, γ-HCH had the highest concentration followed by p, p'-DDE. The residual levels of HCH isomers and DDT as well as their metabolites in soil with different fertilization treatments were in the order of γ-HCH >β-HCH ≈α-HCH >δ-HCH and p, p'-DDE >p, p'-DDT > o, p'-DDT > p, p'-DDD ≈ o, p'-DDE, respectively. DDE/DDT ratios ranged from 1.59 ± 0.13 to 3.35 ±0.16and endrin/dieldrin ratios from 1.40 ± 0.06 to 9.20 ± 4.05, both indicating no new occurrence of these pesticides in these soils, while α-HCH/γ-HCH ratios of 0.04 indicated a new input of lindane (almost pure γ-HCH) in the past several years.The farm manure treatments showed lower DDT residues than samples without fertilizer. Also addition of corn straw and farm manure increased soil organic matter content and decreased the soil pH which could retard the degradation of DDT in the soil.

  19. 苹果农药残留风险评估%Risk Assessment of Pesticide Residues in Apples

    聂继云; 闫震; 李志霞; 刘传德; 方金豹; 王成; 郭永泽; 雷绍荣; 李海飞; 徐国锋

    2014-01-01

    修订或制定苹果中矮壮素等18种农药的MRLs。%[Objective]Risk assessment of pesticide residues in apples will provide a scientific basis for apple consumption, apple pesticide residue supervision, and establishment of maximum residue limits (MRLs) for pesticides in apple. [Method]Residues of 102 pesticides in 200 apple samples from main producing areas in China were detected. Chronic dietary intake risk and acute dietary intake risk of pesticide residues in these samples were assessed, respectively, by%ADI and%ARfD. Estimated maximum residue limits (eMRLs) of 26 pesticides with detectable residues were calculated by ADIs, large portion of apple, and body weight of consumer. The Matrix Ranking developed by the Veterinary Residues Committee of the United Kingdom was referred to rank the risk of pesticides and apple samples.[Result]25.5% of pesticides (26/102) and 89.5% of apple samples (179/200) had detectable residues. 0.5% of apple samples contained residue above the MRL (of omethoate). For 26 pesticides with detectable residues, their chronic dietary intake risks expressed as%ADI were 0.00%-1.07%with an average of 0.13%, and their acute dietary intake risks expressed as %ARfD were 0.18%-22.41% with an average of 4.12%. These 26 pesticides were divided into 3 groups by risk score, i.e. high risk group (8 pesticides), medium risk group (10 pesticides), and low risk group (8 pesticides). Apple samples studied were ranked by risk index, 1.5%of which had high pesticide residue risk, and 98.5%of which had medium, low, or lower pesticide residue risk. Among 26 pesticides with detectable residues, it is unnecessary for chlorbenzuron to establish MRL in apple, MRLs of 6 pesticides (e.g. flusilazole) are overly strict, MRLs of 5 pesticides (e.g. dimethoate) are overly loose, and MRLs of 18 pesticides (including chlormequat, difenoconazole, tebufenozide, diazinon, flusilazole, thiophanate-methyl, dimethoate, bifenthrin, cyhalothrin, fenvalerate, propargite

  20. 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

  1. 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

  2. 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.

  3. 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 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

  4. Comparison pesticide residue levels in the surface of Bertam River in Cameron Highlands, Pahang

    Haron, S. H., E-mail: ismail@ukm.edu.my; Ismail, B. S., E-mail: sthumaira@yahoo.com [School of Environmental and Natural Resource Sciences, Faculty of Science and Technology, Universiti Kebangsaan Malaysia 43600 UKM, Bangi, Selangor (Malaysia)

    2015-09-25

    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.

  5. 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

  6. 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.

  7. Determination of Trichlorfon Pesticide Residues in Milk via Gas Chromatography with μ-Electron Capture Detection and GC-MS

    Hem, Lina; Khay, Sathya; Choi, Jeong-Heui; Morgan, E. D.; El-Aty, A.M. Abd; Shim, Jae-Han

    2010-01-01

    The pesticide trichlorfon is readily degraded under experimental conditions to dichlorvos. A method has therefore been developed by which residues of trichlorfon in milk are determined as dichlorvos, using gas chromatography with μ-electron capture detection. The identification of dichlorvos was confirmed by mass spectrometry. Milk was extracted with acetonitrile followed by centrifugation, freezing lipid filtration, and partitioning into dichloromethane. The residue after partitioning of dic...

  8. Monitoring of pesticide residues in apples, lettuce and potato of the Slovene origin in the years 2001 to 2004

    Baša Česnik, Helena; Gregorčič, Ana; 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 (...

  9. 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

  10. 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

  11. 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

  12. 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...

  13. 76 FR 6465 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2011-02-04

    ... disproportionately high and adverse human health impacts or environmental effects from exposure to the pesticides... address: kearns.rosemary@epa.gov . 6. PP 0F7796. (EPA-HQ-OPP-2010-0905). Interregional Research...

  14. Monitoring of pesticide residues in human breast milk from Punjab, India and its correlation with health associated parameters.

    Sharma, Anupama; Gill, J P S; Bedi, J S; Pooni, P A

    2014-10-01

    This study was undertaken to determine the present status of pesticide residues in breast milk from Punjab. A total of 127 breast milk samples were analyzed and pesticide residues were detected in 25 % of the milk samples. Residues of cyfluthrin, fenvalerate, cypermethrin, profenophos, γ-HCH, β-HCH, chlorpyriphos, monocrotophos, p,p' DDE and phosalone were detected with mean levels of 63.04, 11.69, 3.63, 2.66, 2.64, 2.29, 1.91, 1.63, 0.56 and 0.29 ng g(-1), respectively. Cyfluthrin was leading pesticide detected in breast milk contributing 31.28 % to the total residue load. It was observed that the residue levels were decreasing with increase in parity and age of mother and cyfluthrin had highest mean concentration of 90.63 ng g(-1) in the first parity and 21.11 ng g(-1) in youngest age group. Residue levels were higher in urban population than the rural population although, statistically non-significant difference was found between the two (p > 0.05). PMID:25011502

  15. Discussion on Safety Evaluation Model of Several Kinds of Pesticide Residues in Ram%山药中几种农药残留安全评价模式的探讨

    康燕玉

    2015-01-01

    Through the analysis of pesticide residues in Fujian province exists some phenomenon of Chinese yam.Put forward the mode and measures of safety evaluation and risk assessment system of pesticide residues in yam.Aims to explore how to improve the safety level of pesticide residues in Fujian province yam.To promote the healthy development of Chinese yam industry in Fujian Province.%通过分析福建省山药中农药残留的现象,提出开展山药中农药残留安全系统评价和风险评估的模式及措施。旨在探讨如何提高福建省山药农药残留安全水平,促进福建省山药产业的健康发展。

  16. Multiresidue Analysis of 86 Pesticides Using Gas Chromatography Mass Spectrometry: II-Nonleafy Vegetables

    M. H. EL-Saeid

    2013-01-01

    Full Text Available A total of 1057 samples of fresh vegetables from import and domestic production were analyzed (cold pepper, egg plant, carrot, cucumber, potato, hot pepper, cultivation tomato, squash, beans, okra, onions, cauliflower, and green house tomato. The aim of this study was to investigate pesticide residues in market foods in Riyadh, which have been collected from Riyadh Development Company (Al-Tamer Vegetables Market. Pesticide residues were determined by gas chromatography with mass selective detector (GC-MSD. A multiresidue method was developed and described for simultaneous determination of 86 pesticides commonly used in crop protection. This method used to determine 86 pesticide residues with a broad range of physicochemical properties in fresh vegetables related to organophosphorus (OPP, organochlorines (OCP, pyrethroids, and carbamates mainly used in agriculture. Sample extract was cleaned up by using AOAC method. Pesticide residues above the maximum residue limits (MRL were detected in 15.89% of the total samples (168 from 1057 samples, but 83.90% of the total samples (887 from 1057 samples has no residues or contained pesticide residues at or below MRL. The detected and most frequently found pesticide residues were permethrin (45 times and endosulfan (34 times followed by deltamethrin (27 times. The findings of this study pointed to the following recommendations: the need for a monitoring program for pesticide residues in imported food crops.

  17. 基于供求理论的农药最大残留限量标准过严的风险探讨%Risk Analysis of Excessively Rigorous Maximum Residue Limits for Pesticides Based on the Supply and Demand Theory

    李太平

    2012-01-01

    The standards of maximum residue limits for pesticides in food are bases to recognize food safety. It is very important for scientifically drafting pesticide residue limits standards, ensuring customers' food safety and protecting ecosystem to research the risk of excessively rigorous deviation of the Chinese national standards of pesticide residues in food. This paper applied the supply and demand theory to deeply analyze possible risk of excessively rigorous pesticide residue standards from the view of fanners seeking economic profit. It was concluded that the excessively rigorous pesticide residue standards could not protect customers' health and ecosystem, on the contrary, could encourage farmers to abuse pesticides when the quality information of agri-food was not full and the market supervision was not effective. Therefore our government should set up the program of food safety assessment and scientifically evaluate the rationality of the national standards of pesticide residue limits in food in order to clear up the trouble of food safety management.%农药最大残留限量标准是判别食品安全性的基础.研究农药最大残留限量标准制定过严可能产生的风险,对科学制定我国农药残留标准、保证食品安全和保护生态环境具有十分重要的现实意义.运用经济学的供求理论,从农户追求利润角度对农药残留标准制定过严可能产生的风险进行了深入分析.研究表明,在农产品质量信息不对称、市场监管不到位的情况下,农药最大残留限量标准制定过严,不但不能保护消费者身体健康和农业生态环境,反而有可能加剧农产品的农药残留问题泛滥.因此建议政府要尽快启动食品安全标准风险评估程序,合理评价农药最大残留限量标准的科学性,以消除食品安全管理隐患.

  18. 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.

  19. 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

  20. 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 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.

  1. 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

  2. Seasonal trends in organochlorine pesticide residues in raw bovine milk from rural areas of Haryana, India.

    Kaushik, C P; Kaushik, A; Sharma, H R

    2014-01-01

    Seasonal trends in organochlorine pesticides residues namely, 1,2,3,4,5,6-hexachlorocyclohexane (HCH) isomers, 1,1,1-trichloro-2,2-bis (p-chlorophenyl) ethane (DDT) and its metabolites and endosulfan stereo isomers were investigated in raw bovine milk samples from rural areas of Ambala, Gurgaon and Hisar districts of the state of Haryana for winter, summer, and post-monsoon seasons. Highest concentration of HCH and DDT was found in 43 % and 53 % milk samples, respectively in post-monsoon season whereas highest values of endosulfan was reported in 36 % samples during winter season. During the study period only 2 % milk samples exceeded the maximum residue limit recommended by WHO for ΣHCH, 1 % samples each for α-HCH and γ-HCH, 9 % samples for β-HCH as recommended by PFAA and 30 % samples for ΣDDT as prescribed by FAO. No statistical difference in the mean concentration of ∑HCH and ∑Endosulfan could be observed in any of the three districts. However, ∑DDT concentration showed marked difference [F(2, 25) = 12.42, p = 0.00018)] among the three districts. PMID:24154613

  3. Pesticide residues in bovine milk from a predominantly agricultural state of Haryana, India.

    Sharma, H R; Kaushik, A; Kaushik, C P

    2007-06-01

    One hundred forty seven samples of bovine milk were collected from 14 districts of Haryana, India during December 1998-February 1999 and analysed for the presence of organochlorine pesticide (OCPs) residues. summation operator HCH, summation operator DDT, summation operator endosulfan and aldrin were detected in 100%, 97%, 43% and 12% samples and with mean values of 0.0292, 0.0367, 0.0022 and 0.0036 microg/ml, respectively. Eight percent samples exceeded the maximum residue limit (MRL) of 0.10 mg/kg as recommended by WHO for summation operator HCH, 4% samples of 0.05 mg/kg for alpha-HCH, 5% samples of 0.01 mg/kg for gamma-HCH, 26% samples of 0.02 mg/kg for beta-HCH as recommended by PFAA and 24% samples of 0.05 mg/kg as recommended by FAO for summation operator DDT. Concentrations of beta-HCH and p,p'-DDE were more as compared to other isomers and metabolites of HCH and DDT. PMID:17180431

  4. 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

  5. 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)

  6. Flesh residue concentrations of organochlorine pesticides in farmed and wild salmon from British Columbia, Canada.

    Kelly, Barry C; Ikonomou, Michael G; Higgs, David A; Oakes, Janice; Dubetz, Cory

    2011-11-01

    The present study reports measured levels of organochlorine pesticides (OCPs) in commercial salmon feed (n = 8) and farmed Atlantic, coho, and chinook salmon (n = 110), as well as wild coho, chinook, chum, sockeye, and pink salmon (n = 91). Flesh residue concentrations (ng/g wet weight) of dichlorodiphenyltrichloroethanes (DDTs), hexachlorocyclohexanes (HCHs), chlordanes, chlorobenzenes (CBz) and cyclodiene pesticides (e.g., dieldrin, mirex) were 2 to 11 times higher (p flesh lipid levels. Farmed Atlantic salmon (12-15% lipid) typically exhibited the greatest OCP burdens compared with other salmon species. However, when expressed on a lipid weight basis, concentrations of OCPs (ng/g lipid weight) in wild salmon, in many cases, exceeded those levels in farmed salmon. Observed interspecies and site-specific variations of OCP concentrations in farmed and wild salmon may be attributed to divergent life history, prey/feed characteristics and composition, bioenergetics, or ambient environmental concentrations. Calculated biomagnification factors (BMF = C(F)/C(D), lipid wt) of OCPs in farmed salmon typically ranged between two and five. Biomagnification of chemicals such as DDTs, chlordanes, and mirex was anticipated, because those compounds tend to exhibit high dietary uptake and slow depuration rates in fish because of relatively high octanol-water partition coefficients (K(OW)s > 10⁵). Surprisingly, less hydrophobic pesticides such as hexachlorocyclohexanes and endosulfans (K(OW) s  5). This is contrary to previous laboratory and field observations demonstrating fish BMFs less than 1 for low K(OW) chemicals, because of efficient respiratory elimination of those compounds via gills. The results suggest that ambient seawater concentrations and bioconcentration-driven accumulation may play a key role in the bioaccumulation of these relatively more water-soluble contaminants in farmed salmon. Finally, OCP exposure through consumption of British

  7. 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)...

  8. 75 FR 32463 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-06-08

    ..., e-mail address: austin.lisa@epa.gov . 2. PP 0E7699. (EPA-HQ-OPP-2010-0275). Croda Inc., EPA Company....gov . 4. PP 9E7538. (EPA-HQ-OPP-2009-0066). Croda Inc., 315 Cherry Lane, New Castle, DE 19720... glycerides used to formulate pesticides applied to growing crops or to raw commodities after harvest....

  9. 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... Rm. S- 4400, One Potomac Yard (South Bldg.), 2777 S. Crystal Dr., Arlington, VA. The hours of... formulations of the active ingredients potassium iodide and potassium thiocyanate. On September 9, 2011,...

  10. 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; 1A. Youssao; 1R. Djibril; M. Saizonou; 1Y. I. Mohamed; H. H. Soclo; B. Fayomi

    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...

  11. 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

  12. 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

  13. 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...

  14. 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.

  15. [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

  16. Part II: temporal and spatial distribution of multiclass pesticide residues in lake sediments of northern Greece: application of an optimized MAE-LC-MS/MS pretreatment and analytical method.

    Kalogridi, Eleni-Chrysoula; Christophoridis, Christophoros; Bizani, Erasmia; Drimaropoulou, Garyfallia; Fytianos, Konstantinos

    2014-06-01

    The development and application of an analytical methodology for the pretreatment and determination of 253 multiclass pesticides, in lake sediment samples, using liquid chromatography coupled with mass spectrometry (LC-MS/MS) are described in this work. Sediments of lakes Volvi, Doirani, and Kerkini, located in northern Greece, were collected in two-time periods (fall/winter 2010 and spring/summer 2011) and analyzed, applying the developed analytical methodology. Microwave-assisted extraction (MAE) was applied to extract the pesticide residues from lake sediment samples. Analytical results were stored, categorized, and visualized using geographical information systems, in order to assess and observe spatial and temporal variations of the pollution. Main pesticides that were detected included the following: amitrole, tebuconazole, phoxim, diniconazole, sethoxydim, temephos, tetrachlorvinphos, pendimethalin, boscalid, disulfoton sulfone, lenacil, propiconazole, cycloxydim, pyridaben, and terbuthylazine. Amitrole, diniconazole, and tebuconazole were found to be common in all three lakes. Lakes Kerkini and Doirani exhibited increased concentrations during the first sampling period (winter 2010) with predominant pesticide classes, triazines/triazoles and organophosphates. Pollution is mainly located near the populated villages of the lakes and the nearby cultivations. During the second sampling period, pesticide concentrations appear lower and located in sediments near the center of the lake. Lake Volvi exhibits increased pesticide concentrations during the second sampling period, temporal and spatial variations and different pesticide profile pattern. Increased pollution occurs near the center of the lake during the first sampling period, mainly comprised by triazines/triazoles and organophosphates. During the second sampling period, the majority of the sediment samples demonstrated a different pesticide profile dominated by unclassified pesticides and triazines

  17. 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...

  18. 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 100 ng/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 1-100 ng/g. The developed method allows determination of insecticides at concentrations of 10 ng/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

  19. 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

  20. Heterogeneity Index of Trade and Actual Heterogeneity Index - the case of maximum residue levels (MRLs) for pesticides

    Burnquist, L.H.; Shutes, K.; Rau, M.L.; Souza, de, H.R.; DE Faria

    2011-01-01

    Non-tariff measures (NTMs) beyond traditional trade policy instruments define the requirements that importing countries imposed on foreign products. Due to differences across countries, requirements for supplying foreign markets can lead to trade costs and thus hamper international trade. In this paper, we introduce two regulatory heterogeneity indexes which are subsequently applied to the case maximum residue levels (MRLs) of pesticides. The Heterogeneity Index of Trade (HIT) reflects the re...

  1. Residues of organochlorine pesticides in intertidal flat surface sediments from coastal zone of Jiangsu Province, China

    Han, Xiumei; Zheng, Rong; Zhao, Jiale; Ma, Chao; Gao, Xiaojiang

    2014-09-01

    Sixteen surface sediment samples were collected and analysed to evaluate the residues of organochlorine pesticides (OCPs) from intertidal flat in Jiangsu Province. Overall, 22 OCPs were detected with total concentrations of OCPs ranging widely from 0.96 to 12.14 ng/g (dry wt). Total hexachlorocyclohexane (HCH) and total dichlorodiphenyltrichloroethane (DDT) levels varied from <0.01 to 0.67 ng/g and from 0.23 to 4.85 ng/g, respectively. DDTs were the predominant compounds. The dominance of β-HCH indicated a history of HCH pollution. According to the ratios of ( p, p'-DDD+ p, p'-DDE)/ p, p'-DDT and o,p'-DDT/ p, p'-DDT, new input of DDTs did not occur in most sites, and the main sources were historical usage of technical DDTs. OCPs such as dieldrin, endrin, p, p'-DDD, and p, p'-DDT exceeded the effects range low, showing adverse biological effects that would occasionally occur at some sites of the study area.

  2. Persistent organochlorine pesticides residues in cow and goat milks collected from different regions of Ethiopia.

    Deti, Habtewold; Hymete, Ariaya; Bekhit, Adnan A; Mohamed, Abdel Maaboud I; Bekhit, Alaa El-Din A

    2014-07-01

    The present study investigated the bioaccumulation of organochlorines in two milk-producing animals (goats and cows) grazed on the same feed to explore the extent of organochlorines availability in milk and any species effect on the bioaccumulation pattern. Six organochlorine pesticides: aldrin, α-endosulfan, β-endosulfan, p,p'-DDE, o,p'-DDT and p,p'-DDT were determined in samples collected from four regions in Ethiopia. Aldrin (11.6μgkg(-1)) was detected only in one cow milk sample and α-endosulfan was detected in one goat milk sample at a level of 142.1μgkg(-1), and in one cow milk sample (47.8μgkg(-1)) from the same region. p,p'-DDE was detected in 40% of the milk samples analyzed while o,p'-DDT and p,p'-DDT were found in high amounts in almost all samples. The average total DDT (excluding DDD) in the samples was 328.5μgkg(-1). Regions known for their malaria epidemics were the most contaminated with DDT residue. The accumulation pattern in both species was not clear under natural sampling. PMID:24630448

  3. 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

  4. 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.

  5. A rapid, solid phase extraction (SPE) technique for the extraction and gas chromatographic determination lindane pesticide residue in tissue and milk

    Yuningsih; Sri Yuliastuti

    2006-01-01

    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...

  6. HPLC 法测定不同产地赤芍中芍药苷的含量及重金属和残留农药的分析%Analysis of Paeoniflorin,Residual Pesticide and Heavy Metal Content Determination in Radix Paeoniae Rubra from Different Habitats by HPLC

    陈述

    2014-01-01

    目的:建立一种测定赤芍中芍药苷含量的高效液相色谱法,测定不同产地赤芍中芍药苷的含量并分析赤芍中重金属含量及农药的残留量。方法:色谱柱:Kromasil C18柱(5μm,4.6 mm ×250 mm);流动相:甲醇-0.05 mol/L 磷酸二氢钾(30∶70);波长:230 nm;柱温:25℃;流速:1.0 mL/min;进样量:10μL。采用原子吸收分光光度法对赤芍药材中的重金属铅、砷、铜、镉、汞进行分析,同时采用气相色谱法对有机氯类农药残留量进行测定。结果:芍药苷在0.1~1.0 mg/mL 范围内,浓度与峰面积的线性关系良好(R2=0.9996),样品的平均加样回收率为98.8%,RSD 为0.29%。17个不同产地的赤芍药材中芍药苷的含量为2.17%~4.17%;赤芍中检出铅、砷、铜、镉、汞的残留量分别为0.19~0.39、0.19~0.72、0.87~8.17、0.11~0.29和0.08~0.14 mg/kg;部分赤芍药材中有检出有机氯类,DHC、DDT、PCNB 的残留量分别为0.021~0.063、0.039~0.121和0.024~0.050 mg/kg。结论:17个产地的赤芍药材中芍药苷的含量均符合中国药典要求;药材存在一定量的重金属和有机氯类农药残留,除1份药材 DDT 含量超标外,其他药材的重金属及农药残留量均符合《药用植物及制剂进出口绿色行业标准》中的限量规定,赤芍药材总体质量较好。%Objective:To establish a HPLC method to determine the content of paeoniflorin as well as residual pesticide and heavy metal in Radix Paeoniae Rubra in different areas.Methods:Chromatographic column was Kromasil C18 column (5 μm,4.6 mm ×250 mm);mobile phase was methanol -0.05mol/L potassium dihydrogen phosphate (30:70);wavelength was 230 nm;column temperature was 25℃;flow rate was 1 mL/min;sample size was 10 L.Analysis of heavy metal lead,arsenic,copper,cadmium,mercury in Paeonia lacti-flora were determined by atomic absorption spectrophotometry,and gas

  7. 77 FR 20334 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2012-04-04

    ... extract (red ginseng extract and ginseng extract) at 0.5 ppm. An adequate analytical method, gas... the extract is purified through a solid phase extraction cartridge. The residues are then derivatized... tolerance for residues of the antimicrobial gaseous chlorine dioxide, on tomato. EPA Method 300,...

  8. Simultaneous determination of 70 pesticide residues in leek, leaf lettuce and garland chrysanthemum using modified QuEChERS method with multi-walled carbon nanotubes as reversed-dispersive solid-phase extraction materials.

    Han, Yongtao; Zou, Nan; Song, Le; Li, Yanjie; Qin, Yuhong; Liu, Shaowen; Li, Xuesheng; Pan, Canping

    2015-11-15

    Leek, leaf lettuce and garland chrysanthemum are troublesome vegetables containing large amount of pigments which may bring serious matrix interferences in mass spectrometry analysis. Multi-walled carbon nanotubes (MWCNTs) have a good effect for the cleanup of troublesome matrix. So the study was designed to develop a multi-residue method for the determination of 70 pesticide residues in leek, leaf lettuce and garland chrysanthemum based on a modified QuEChERS procedure using MWCNTs as reversed-dispersive solid phase extraction (r-DSPE) materials to remove the interferences of pigments. PSA and GCB were used as comparison. LC-MS/MS was used to identify and quantify the residue levels of multi-pesticides. The clean-up performance of MWCNTs was demonstrated to be obviously superior to GCB and PSA. This method was validated on leek, leaf lettuce and garland chrysanthemum spiked at the concentration of 10, 50 and 100μgkg(-1) with five replicates. The recoveries of 70 pesticides ranged from 74% to 119%, with relative standard deviations (RSDs) lower than 14.2%. Good linearity (R(2)≥0.9903) was obtained at the range of 10-1000μg/L for all pesticides in the selected matrices. The limit of quantification (LOQs) and limit of detection (LODs) of the 70 pesticides for the selected matrices ranged from 0.3 to 7.9μgkg(-1) and from 0.1 to 2.4μgkg(-1) respectively. The method was successfully applied to the routine monitoring of pesticide residues in market samples. PMID:26513135

  9. The potential for using ozone to decrease pesticide residues in honey bee comb

    As a strong oxidizer, ozone is known to breakdown some organic pesticides, and we evaluated the potential for using a gaseous fumigation of ozone to decontaminate honeycomb and empty honey bee hives. Honey bees are inadvertently exposed to pesticides when they forage for nectar and pollen in agricul...

  10. 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)

  11. [Determination of 213 pesticide residues in milk and milk power by gas chromatography-triple quadrupole tandem mass spectrometry].

    Wang, Jing; Ai, Lianfeng; Ma, Yusong; Zhang, Haichao; Li, Wei; Yu, Meng

    2015-11-01

    On the basis of the optimization of solid phase extraction adsorbent, eluting solvent types and amounts, a gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS) method was established for the determination of 213 pesticide residues in milk and milk power. The samples were extracted by acetonitrile, cleaned-up with an ENVI-Carb/NH2 solid-phase extractant, and determined by GC-MS/MS using external standard method. The linear ranges were from 10 to 1 000 μg/L for 197 pesticides, from 50 to 1 000 μg/L for the other 16 pesticides with the correlation coefficients higher than 0.99. The limits of detection (LODs, S/N = 3) varied over the range of 0.03 to 7.59 μg/kg, and limits of quantification (LOQs, S/N = 10) ranged from 0.10 to 21.94 μg/kg. The average recoveries in different matrices were in the range of 66.9% - 120.1% with the relative standard deviations (RSDs) of 1.23% - 17.6%. This method is simple, rapid, sensitive and reliable for meeting the requirements for the simultaneous identification and quantification of the multi-residues in milk and milk power. PMID:26939364

  12. [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

  13. Risk A nalysis of Pesticide Residues in Seven Categories of Vegetables%7类重要蔬菜中农药残留风险分析

    赵小中; 魏小春; 朱香玲; 董森森

    2013-01-01

    Pesticide residues in vegetables were monitored in order to comprehensively investigate the current status in Zhengzhou ,Henan province ,in 2010-2012 ,and to provide the basis for its manage-ment .We carried the pesticide residue analysis of 21 kinds of vegetables ,belonging to seven categories in Zhengzhou vegetable production base .The results showed that among 32 pesticides monitored ,30 kinds were detected from the vegetable samples ,and the pesticides with detection rate of more than 5% were deltamethrin ,chlorothalonil ,triadimefon ,procymidone and PCNB .The exceeding rate of pesticide residues had a tendency of Sinusoidal line with seasons ,whose tendency from higher to lower was bulb vegeta-bles ,green leafy vegetables ,brassica vegetables ,bean-like vegetables ,melon-like vegetables ,tuber-like vegetables and eggplant-like vegetables .Meanwhile ,the risk factor of omethoate residue was more than 2 .5 in vegetables ,which was thought high risk ;and that of chlorpyrifos and phorate was between 1 .5 and 2 .5 ,which were thought middle risk ;the risk factor of the rest pesticide residues was lower than 1.5 ,which were thought low risk .%为全面了解和掌握郑州市蔬菜农药残留现状,为政府和相关部门的管理提供依据,2010-2012年对郑州市蔬菜生产基地七大类21种蔬菜开展了农药残留监测工作,采用危害物风险系数法评估农药残留的风险性。结果表明:所检测的32种农药中有30种农药被检出,检出率大于5%的农药有溴氰菊酯、百菌清、三唑酮、腐霉利及五氯硝基苯。农药残留超标率随季节呈“正弦线”的变化趋势,不同类蔬菜农药残留平均超标率大小表现为鳞茎类>绿叶菜类>芸薹类>豆类>瓜类>根茎类>茄果类。蔬菜中氧化乐果的风险系数大于2.5,为高度风险;毒死蜱、甲拌磷的风险系数介于1.5~2.5,为中度风险;其余检测的农药残留风险系数均小于1.5,为低度风险。

  14. Simple, specific analysis of organophosphorus and carbamate pesticides in sediments using column extraction and gas chromatography

    Belisle, A.A.; Swineford, D.M.

    1988-01-01

    A simple, specific procedure was developed for the analysis of organophosphorus and carbamate pesticides in sediment. The wet soil was mixed with anhydrous sodium sulfate to bind water and the residues were column extracted in acetone:methylene chloride (1:l,v/v). Coextracted water was removed by additional sodium sulfate packed below the sample mixture. The eluate was concentrated and analyzed directly by capillary gas chromatography using phosphorus and nitrogen specific detectors. Recoveries averaged 93 % for sediments extracted shortly after spiking, but decreased significantly as the samples aged.

  15. 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.

  16. Tank 12H residuals sample analysis report

    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.

  17. Residual analysis for spatial point processes

    Baddeley, A.; Turner, R.; Møller, Jesper;

    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....... The conditional intensity $lambda$ plays the role of the mean response. Elaborating this analogy gives us recommendations for diagnostic plots and model criticism using these residuals. A plot of smoothed residuals against spatial location, or against a spatial covariate, is effective in diagnosing spatial trend...

  18. 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

  19. 75 FR 57942 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-09-23

    ... developed and used to quantitate residues of oxytetracycline by using liquid chromatography mass...,4,2-dioxazin-3-yl)methanone O- methyloxime, in or on raw agricultural commodities listed under crop... chromatography/mass spectroscopy/mass spectrometry (HPLC/MS/MS) detection is available for enforcement...

  20. 78 FR 33785 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2013-06-05

    ... enforcement analytical methods for determining flutriafol in/on appropriate raw agricultural commodities and... liquid-liquid partition. The final sample solution is quantitated using liquid chromatography (LC... metabolites. Residues are quantified by high performance liquid chromatography (HPLC) with MS/MS...

  1. 77 FR 50661 - Notice of Filing of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2012-08-22

    ..., subgroup 13-07G at 3.0 ppm. A practical analytical method, high pressure liquid chromatography (HPLC) with... analytical method for detecting residues of imazapyr in canola and sunflower raw agricultural commodities (RACs) and processed commodity samples is an liquid chromatography/mass spectrometry (LC/MS/ MS)...

  2. 76 FR 17374 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2011-03-29

    ... commodities (RACs) published in the Federal Register of April 19, 2000 (65 FR 20972) (FRL-6554-3). Contact... residues of concern, followed by addition of an internal standard to the extract. The extract is then...; citrus, oil; citrus, dried pulp; tomato, puree; tomato, paste. The petitioner believes no...

  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...) for pre-harvest uses, in or on all agricultural commodities. Pear Ester is the naturally occurring... from the requirement of a tolerance for residues of the biochemical potato sprout inhibitor,...

  4. 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....

  5. Chronic dietary exposure to pesticide residues and associated risk in the French ELFE cohort of pregnant women.

    de Gavelle, Erwan; de Lauzon-Guillain, Blandine; Charles, Marie-Aline; Chevrier, Cécile; Hulin, Marion; Sirot, Véronique; Merlo, Mathilde; Nougadère, Alexandre

    2016-01-01

    Dietary exposure to pesticide residues may present a risk to public health, especially for sensitive populations such as pregnant women. To characterize this risk, this study assessed chronic dietary exposure to pesticide residues based on the French ELFE cohort. A self-administered food frequency questionnaire (FFQ) about the last three months of pregnancy filled in by pregnant women in 2011 was used in combination with occurrence data from French Total Diet Studies completed by the results of national monitoring programs on pesticide residues in food. The dietary intake of pesticides (μg/kg of body weight/day) was estimated for 14,099 pregnant women with a complete FFQ, for 317 substances under two occurrence scenarios to handle left-censored data: a lower-bound scenario (LB), where undetected results were set to zero, and an upper-bound scenario (UB), where undetected results were set to the detection limit if the substance was expected to be found in food and zero if it was not. The risk was assessed for 284 substances with a toxicological reference value (TRV) and a good coverage level of the diet potentially contributing to pesticide intake. The cumulative risk was also assessed for seven effects on nervous and thyroid systems using the hazard index and the Cumulative Assessment Groups defined by EFSA. Substances with the highest exposure levels under the LB scenario were, in decreasing order, imazalil, piperonyl butoxide, chlorpropham, thiabendazole, iprodione and propargite. Under the LB scenario, only for lindane did women have a statistically significant probability of exceeding the TRV (2.4%). Under the UB scenario, risk could not be excluded for nine other substances. A better management of left-censored data and more sensitive analyses of the main food contributors might help to refine the UB exposure and risk assessments. A statistically significant cumulative risk was found for neurochemical effects related to high intake levels of three

  6. 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

  7. 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.

  8. 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.

  9. 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 (α and β) 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

  10. Residues of organochlorine pesticides and PCBs in some Brazilian municipal solid waste compost.

    Lourencetti, Carolina; Favoreto, Rodrigo; Marchi, Mary R R; Ribeiro, Maria L

    2007-08-01

    Persistent organic pollutants (POPs), organochlorine pesticides and polychlorinated biphenyls (PCBs), listed as per the Stockholm Convention (alpha -HCH, beta -HCH, gamma -HCH, p,p'-DDT, o,p'-DDT, p,p'-DDD, p,p'-DDE, aldrin, endrin, dieldrin, PCBs 28, 52, 118, 138, 153, and 180), were analyzed in municipal solid waste (MSW) compost samples from three different Brazilian composting plants located in three São Paulo State cities: Araras, Araraquara and São Paulo (Vila Leopoldinha). Quantitative and qualitative analyses were carried out using gas chromatography electron capture detection (GC-ECD) and gas chromatography mass spectrometry (GC-MS) (Ion Trap, electron impact ionization), respectively. The samples were analyzed in triplicate and the target POPs were not detected by GC-ECD. Twelve pollutants were identified in two samples when qualitative analysis (GC-MS) was used (beta -HCH, gamma -HCH, p,p'-DDT, o,p'-DDT, p,p'-DDD, and p,p'-DDE, PCBs 28, 118, 138, 153 and 180). The composting process has advantages such as urban solid waste reduction and landfill life-span increase, however the MSW compost quality, which can be utilized for agricultural purposes, should be evaluated and be controlled. This kind of study is the first step in making available information to answer questions regarding MSW compost for sustainable agricultural use, such as the pollutants accumulation in soil and in groundwater, and plants uptake. PMID:17701705

  11. 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....

  12. 农药残留问题的过去、现在和将来%Overview on the Problem of Pesticide Residues

    陈宗懋

    2011-01-01

    Pesticide residue in agricultural products is an important aspect in food safety. The application of chemical pesticide in the agriculture was begun since 1938 and the pesticide residue problem was emerged in the end of 1950's. The publication of the "Silent Spring" written by Rachal Carson in 1962 revealed the prologue of pesticide residue. It was paid more attention in the world with the development of pesticide toxicology. The MRL of pesticide residue in food was decreased around 100 times in the 60 years period between the sixties of last century and 2010. The new challenge of pesticide residue in the future was discussed by the author from the aspects of the adoption of acute reference dose (ARID) in the toxicity assessment, the development of pesticide toxicology, the accumulative toxicology of various pesticides and the difference of toxicology in chiral compounds of pesticide. The risk assessment, the revealing of contamination source and the cleaning production were put forward by the author as the major techniques in controlling of pesticide residue in agricultural products.%农产品中的农药残留是食品安全的一个重要方面.化学农药自1938年开始在世界上推广应用,20世纪50年代末农药残留问题凸现.1962年出版的Silent Spring一书揭开了农药残留问题的序幕.随着农药毒理学的发展,食品中农药残留也越来越引起社会的重视.食品中最大农药残留限量(MRL)标准,从20世纪60年代到21世纪10年代的60年间下降了100倍.本文从急性参考剂量(ARfD)毒性评估标准的出现、农药毒理学的发展、同类农药的累积毒性、农药手性化合物的毒性差异等方面,讨论未来农药残留面临的新挑战.提出风险评估、探明污染源、清洁化生产、无公害治理等可作为农产品中农药残留的主要阻控技术.

  13. 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

  14. 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

  15. Evaluation of low-pressure gas chromatography-tandem mass spectrometry method for the analysis of >140 pesticides in fish.

    Sapozhnikova, Yelena

    2014-04-30

    A multiresidue method for the 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 acetonitrile and dispersive solid-phase extraction (d-SPE) cleanup with zirconium-based sorbent. The developed method was evaluated at four spiking levels (1, 5, 50, and 100 ng/g) and further validated by analysis of NIST Standard Reference Materials (SRMs) 1974b and 1947 for selected pesticides with certified concentrations. Acceptable recoveries (70-120%) and standard deviations below 20% were achieved for the majority of pesticides from fortified samples. The measured values for both SRMs agreed with certified values (71-115% accuracy, 4-14% relative standard deviations) for all pesticides, except for p,p-DDD + o,p-DDT (45%) and heptachlor (133%) in SRM 1974b and except for mirex (58%) and trans-chlordane (136%) in SRM 1947. The developed method is fast, simple, and inexpensive with detection limits of 0.5-5 ng/g. Residues of dimethoate, hexachlorobenzene, BHC, lindane, nonachlor, chlorpyrifos, trifluralin, p,p-DDE, p,p-DDD, o,p-DDD, o,p-DDT, p,p-DDD, and chlordane were measured in catfish samples from the market. PMID:24387765

  16. 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)

  17. 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).

  18. 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...

  19. 食品中农药残留筛查系统的构建%Construction of pesticide residues screening system in foods

    杨永坛; 陈士恒; 史晓梅

    2015-01-01

    ABSTRACT:This article reviewed the kinds and damage of common pesticides, latest detection technique and pretreatment methods about pesticide residues in complex food matrix. Solid phase extraction, gel permeation chromatography, microwave assisted extraction and dispersive solid phase extraction technologies were mainly summarized. The detection technology of pesticide residues mainly used chromatography methods. This paper focused on the gas chromatography, liquid chromatography methods and the corresponding mass spectrometry method. The development of high resolution mass spectrometry technology can provide strong support for the establishment of pesticide residue detection and monitoring system. The pesticide residues monitoring system, software system and database based on the main pesticide residues concerned in grain and oil food were proposed, which can be used in the pesticide residues risk screening system. This pesticide residues screening system can be used for government and industry to master the pollution situation of pesticide residues in agricultural products and to propose the practical solution.%对常见农药的种类、农药残留的危害及有关农药残留的最新检测技术和复杂基质样品的前处理技术进行概述,主要总结固相萃取、凝胶渗透色谱、微波辅助消解以及分散固相萃取技术。农药残留检测主要使用色谱学方法,文中重点概述气相色谱、液相色谱方法以及相应的质谱联用技术,高分辨质谱技术的发展可以为农药残留筛查系统的建立提供有力支撑。在此基础上提出基于粮油食品中重点关注的农药残留种类并建立农药残留的监测系统、软件系统及数据库,进而建立农药残留的风险筛查系统,为政府部门及产业部门掌握农产品农药污染情况提出切实可行的解决方案。

  20. 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.

  1. 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.

  2. 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

  3. 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 extraction was carried out analogous to the QuEChERS method, however, without the addition of water. With this simple modification, the problematic lipophilic pesticides, which had been strongly affected by the fat content of the commodities, could be determined with recoveries above 70% even at a concentration level of 0.01mg/kg. Moreover, a GC-MS/MS screening method for 120 pesticides at a concentration level of 0.01mg/kg was established by employing analyte protectants (ethylglycerol, gulonolactone, and sorbitol). The use of only one standardized calibration, made of an apple purée extract in combination with analyte protectants, allowed for a qualitative and quantitative analysis of 120 pesticides in different matrix extracts (tomato, red 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

  4. 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.

  5. 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.

  6. 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

  7. 76 FR 3601 - Codex Alimentarius Commission: Meeting of the Codex Committee on Pesticide Residues

    2011-01-20

    ... Codex Alimentarius Commission (Codex), which will be held in Beijing, P.R. China April 4-9, 2011. The... items or groups of food. The Committee is hosted by China. Issues To Be Discussed at the Public Meeting.... Department of Agriculture (USDA), and the Office of Pesticide Programs, U.S. Environmental Protection...

  8. Pesticide residues in fruit and vegetables from Africa - a Nordic Project

    Petersen, Annette

    . Most of the samples came from South Africa (249), followed by Egypt (129), Morocco (92) and Kenya (88). In total 45 different commodities were analyzed, oranges (162) being the largest group, followed by beans with pods (80) and table grapes (71). In the analytical scope 220 to 345 pesticides and...

  9. 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...

  10. 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...

  11. 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.

  12. 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.

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

    Poulsen, Mette Erecius; Hansen, Hanne Kyhnau; Sloth, Jens Jørgen; Christensen, Hanne Bjerre; Andersen, Jens Hinge

    2007-01-01

    Abstract The differences in residue pattern between the main exporters of table grapes to the Danish market, Italy and South Africa, were investigated. The results showed no major differences with respect to the number of samples with residues, where residues were found in 54-78% of the samples. Excedances of EU-MRL were found in five samples from Italy. A number of samples were rinsed to study possible reduction of residues. For copper, iprodione, procymidone and dithiocarbamates ...

  14. The maximum residue limits and determination of pesticide residues in asparagus%芦笋中农药最大残留限量及检测方法研究进展

    宋欢; 车兰兰; 林勤保; 王蓉珍

    2012-01-01

    总结了芦笋中常用农药及欧盟、日本、美国和我国对其最大残留限量规定,并对农药残留相关检测方法在芦笋等果蔬中的应用进行综述,以期为我国芦笋中农药残留检测和控制提供参考。%Common pesticides used in asparagus planting and the maximum residue limits (MRLs) of those in European Union,Japan,USA and China were summarized,and also the application of relevant determination methods of pesticide residues to asparagus ,vegetables and fruit were reviewed. The paper is aimed at providing reference for pesticide residue determination and controlling in Chinese asparagus field.

  15. Utilizing a novel sorbent in the solid phase extraction for simultaneous determination of 15 pesticide residues in green tea by GC/MS.

    Huo, Feifei; Tang, Hua; Wu, Xue; Chen, Dazhou; Zhao, Tan; Liu, Pei; Li, Lei

    2016-06-15

    Pesticide residues exceeding standard in green tea is a widespread problem of the world's attention, containing organochlorine pesticides (OCPs), organophosphorus pesticides (OPPs), and pyrethroids. In this research, three dimensionally honeycomb Mg-Al layered double oxide (TDH-Mg-Al-LDO) combined with graphitized carbon black (GCB), packed as a column, was used as a novel solid phase extraction sorbent, applying in simultaneous determination of 15 pesticide residues in green tea coupled with GC-MS. Compared with different type of SPE column, it showed that TDH-Mg-Al-LDO exhibited great advantages in the extraction of 15 pesticide residues from green tea, which was seldom reported before. Different experiment conditions, such as combination order of Mg-Al-LDO and GCB, dosage of sorbents, type and volume of eluting solvent were thoroughly studied and optimized. The limits of detection (LODs) of 15 pesticides ranged from 0.9 to 24.2ng/g and the limits of quantifications (LOQs) were ranging from 3.0 to 80.0ng/g. The recoveries using this method at three spiked concentration levels (10, 100 and 500ng/g for Fenthion, P,P'-DDE, O,P'-DDT, P,P'-DDD and Bifenthrin, 100, 500 and 2000ng/g for the others) range from 71.1 to 119.0%. The relative standard deviation (RSD) was from 0.1 to 7.6% in all case. The result indicated that the proposed analytical method had been successfully applied for the simultaneous determination of 15 pesticide residues in commercial green tea. PMID:27183089

  16. Determination of Trichlorfon Pesticide Residues in Milk via Gas Chromatography with μ-Electron Capture Detection and GC-MS.

    Hem, Lina; Khay, Sathya; Choi, Jeong-Heui; Morgan, E D; Abd El-Aty, A M; Shim, Jae-Han

    2010-06-01

    The pesticide trichlorfon is readily degraded under experimental conditions to dichlorvos. A method has therefore been developed by which residues of trichlorfon in milk are determined as dichlorvos, using gas chromatography with μ-electron capture detection. The identification of dichlorvos was confirmed by mass spectrometry. Milk was extracted with acetonitrile followed by centrifugation, freezing lipid filtration, and partitioning into dichloromethane. The residue after partitioning of dichloromethane was dissolved in ethyl acetate for gas chromatography. Recovery concentration was determined at 0.5, 1.0, and 2.0 of times the maximum permitted residue limits (MRLs) for trichlorfon in milk. The average recoveries (n = 6) ranged from 92.4 to 103.6%. The repeatability of the measurements was expressed as relative standard deviations (RSDs) ranging from 3.6%, to 6.7%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.7 and 11.1 μg/l, respectively. The accuracy and precision (expressed as RSD) were estimated at concentrations from 25 to 250 μg/l. The intra- and inter-day accuracy (n = 6) ranged from 89.2%to 91% and 91.3% to 96.3%, respectively. The intra- and inter-day precisions were lower than 8%. The developed method was applied to determine trichlorfon in real samples collected from the seven major cities in the Republic of Korea. No residual trichlorfon was detected in any samples. PMID:24278518

  17. Assessment of organochlorine pesticide residues in Atlantic Rain Forest fragments, Rio de Janeiro, Brazil.

    Quinete, Natalia Soares; de Oliveira, Elba dos Santos; Fernandes, Daniella R; Avelar, Andre de Souza; Santelli, Ricardo Erthal

    2011-12-01

    A superficial water quality survey in a watershed of the Paraíba 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 Teresópolis, 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. PMID:21864959

  18. Research progress of overview on sample pretreatment of pesticides residue in milk%牛奶中农药残留前处理研究进展

    刘慧玲

    2014-01-01

    由于牛奶在食物营养链中又处于较高级,所以其含有的农药残留量相对较高。随着人们对食品安全重视程度的提升,牛奶中含有的各种有害物质残留的检测方法受到了消费者的极大关注。牛奶中农药残留检测是一项关系食品安全的重要问题,而样品前处理是检测的关键步骤。本文综述了近年来牛奶中农药残留的提取,净化的前处理方法,对液液萃取,固相萃取,固相微萃取,基质分散固相萃取,凝胶渗透色谱,浊点萃取, QuEChERS等方法进行了详细阐述。文章综述了牛奶中农药残留前处理检测方法进展,旨在为进一步开展牛奶农残残留检测提供参考。%The level of pesticide residues in milk is relatively quite high as milk is close to the top of food chain. So the harmful substance in milk had attracted much attention of consumer. With the increase of public attention to food safety, detection of pesticide and veterinary drug residues in milk has become a hot topic of food safety in today’s China. Meanwhile, sample preparation is a very critical step in the determination process and it determines the analysis accuracy and precision. This article makes a brief summary of liquid-liquid ex-traction, solid phase extraction, solid phase microextraction, matrix solid-phasedispersion extraction, Gel Per-meation Chromatography, cloud point extraction, and QuEChERS. This article reviewed the new research progress of sample preparation of pesticide residues in milk, aimed to supply some reference to the further re-search in this area.

  19. Spatial and temporal analysis of pesticides concentrations in surface water: Pesticides atlas

    Vijver, M.G.; Zelfde, van 't M.; Tamis, W.L.M.; Snoo, de G.R.

    2008-01-01

    Dutch water boards have a well-established program for monitoring pesticide contamination of surface waters. These monitoring data have been processed into a graphic format accessible online and designed to provide insight into pesticide presence in Dutch surface waters and trends over time: the Pes

  20. 75 FR 48667 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-08-11

    ... homogenization, filtration, partition, and cleanup with analysis by high performance liquid chromatography (HPLC... with triple quadrupole mass spectrometric detection (LC-MS/MS). Contact: Heather Garvie, (703) 308-0034... chromatography with either ultraviolet (UV) or mass spectrometry (MS) detections. The limit of detection...

  1. 77 FR 66781 - Notice of Filing of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2012-11-07

    .... Adequate enforcement methodology (liquid chromatography/mass spectrometry/mass spectrometry--(LC/MS/MS)) is... analysis by high performance liquid chromatography (HPLC) using tandem mass spectrometric detection (HPLC... ppm; dillweed, dried leaves at 7.1 ppm; dillweed, fresh leaves at 1.5 ppm; dill oil at 4.8 ppm;...

  2. 75 FR 66092 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-10-27

    ... of analysis included extraction and liquid chromatography (LC)/MS/MS quantitation. The limit of..., millet, sorghum) at 0.2 ppm; corn, field, sweet, pop at 0.01 ppm; corn, refined oil at 0.03 ppm; cereal...), in or on orange at 0.80 ppm; and its processed commodities: Orange, juice at 0.025 ppm; orange,...

  3. Pesticide Flow Analysis to Assess Human Exposure in Greenhouse Flower Production in Colombia

    Binder, Claudia R.; Camilo Lesmes-Fabian

    2013-01-01

    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 ...

  4. Assessment of Pesticide Residues in Flesh of Catla catla from Ravi River, Pakistan

    2014-01-01

    The levels of dichlorodiphenyltrichloroethane (DDT), dichlorodiphenyldichloroethylene (DDE), endosulfan, endosulfan sulfate, carbofuran, and cartap which were estimated in the flesh of Catla catla sampled from ten sites of Ravi River between its stretches from Shahdara to Head Balloki were studied to know the level of contamination of the selected pesticides by GC-ECD method. All fish samples were found contaminated with different concentrations of DDT, DDE, endosulfan, and carbofuran; howeve...

  5. 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)

  6. 2012年曲靖市蔬菜中农药残留情况%Investigation on pesticide residues in vegetables in Qujing City during 2012

    黄智文; 方双勇; 李荣发; 成珍

    2013-01-01

    [Objective]To investigate the situation of pyrethroid and organophosphorus pesticide residues in vegetables on the markets of Qujing, [Methods]80 samples of vegetable were randomly selected, and the pesticide residues were detected by the method of GB/T 5009.145-2003 and GB/T 5009.146-2003. All the samples were evaluated according to the Maximum residue limits for pesticides in food (GB 2763-2005). [ Results] 13 kinds of pesticide residues were detected, 4 kinds of pesticides, which exceeded the standard, were cyhalothrin, dichlorvos, methamidophos and chlorpyrifos. The total detection rate of pyrethroid and organophosphorus were respectively 52. 5% and 23. 75% , and the over standard rate of them was 2. 5% and 6. 25% respectively. [Conclusion]The situation of pesticide residues in vegetables in Qujing City is serious, and the detection rate of pyrethroid pesticides is higher. In order to ensure the safety of vegetables consumption, it is necessary to strengthen the surveillance of pesticide residues.%目的 了解曲靖市市售蔬菜中拟除虫菊酯类、有机磷类农药的残留现状.方法 随机抽取80份蔬菜样品,按照国家标准检测方法GB/T 5009.145-2003和GB/T 5009.146-2003进行农药残留检测;依据GB 2763-2005《食品中农药最大残留限量》进行限量值评价.结果 检出阳性农药13种,4种超标,分别为氯氟氰菊酯、敌敌畏、甲胺磷、毒死蜱.拟除虫菊酯总检出率52.5%,超标率2.5%;有机磷类农药总检出率23.75%,超标率6.25%.结论 该市蔬菜农药残留现象不容乐观,拟除虫菊酯类农药检出率较高,应加强农药残留监测,保证市民食用蔬菜的安全.

  7. A sensitive multi-residue method for the determination of 35 micropollutants including pharmaceuticals, iodinated contrast media and pesticides in water.

    Valls-Cantenys, Carme; Scheurer, Marco; Iglesias, Mònica; Sacher, Frank; Brauch, Heinz-Jürgen; Salvadó, Victoria

    2016-09-01

    A sensitive, multi-residue method using solid-phase extraction followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed to determine a representative group of 35 analytes, including corrosion inhibitors, pesticides and pharmaceuticals such as analgesic and anti-inflammatory drugs, five iodinated contrast media, β-blockers and some of their metabolites and transformation products in water samples. Few other methods are capable of determining such a broad range of contrast media together with other analytes. We studied the parameters affecting the extraction of the target analytes, including sorbent selection and extraction conditions, their chromatographic separation (mobile phase composition and column) and detection conditions using two ionisation sources: electrospray ionisation (ESI) and atmospheric pressure chemical ionisation (APCI). In order to correct matrix effects, a total of 20 surrogate/internal standards were used. ESI was found to have better sensitivity than APCI. Recoveries ranging from 79 to 134 % for tap water and 66 to 144 % for surface water were obtained. Intra-day precision, calculated as relative standard deviation, was below 34 % for tap water and below 21 % for surface water, groundwater and effluent wastewater. Method quantification limits (MQL) were in the low ng L(-1) range, except for the contrast agents iomeprol, amidotrizoic acid and iohexol (22, 25.5 and 17.9 ng L(-1), respectively). Finally, the method was applied to the analysis of 56 real water samples as part of the validation procedure. All of the compounds were detected in at least some of the water samples analysed. Graphical Abstract Multi-residue method for the determination of micropollutants including pharmaceuticals, iodinated contrast media and pesticides in waters by LC-MS/MS. PMID:27382969

  8. 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...

  9. Detection of Organophosphorus Pesticides with Colorimetry and Computer Image Analysis.

    Li, Yanjie; Hou, Changjun; Lei, Jincan; Deng, Bo; Huang, Jing; Yang, Mei

    2016-01-01

    Organophosphorus pesticides (OPs) represent a very important class of pesticides that are widely used in agriculture because of their relatively high-performance and moderate environmental persistence, hence the sensitive and specific detection of OPs is highly significant. Based on the inhibitory effect of acetylcholinesterase (AChE) induced by inhibitors, including OPs and carbamates, a colorimetric analysis was used for detection of OPs with computer image analysis of color density in CMYK (cyan, magenta, yellow and black) color space and non-linear modeling. The results showed that there was a gradually weakened trend of yellow intensity with the increase of the concentration of dichlorvos. The quantitative analysis of dichlorvos was achieved by Artificial Neural Network (ANN) modeling, and the results showed that the established model had a good predictive ability between training sets and predictive sets. Real cabbage samples containing dichlorvos were detected by colorimetry and gas chromatography (GC), respectively. The results showed that there was no significant difference between colorimetry and GC (P > 0.05). The experiments of accuracy, precision and repeatability revealed good performance for detection of OPs. AChE can also be inhibited by carbamates, and therefore this method has potential applications in real samples for OPs and carbamates because of high selectivity and sensitivity. PMID:27396650

  10. Baseline study of pesticide residues and toxic contaminants in environmental samples in Thailand by neutron activation technique

    The technique of neutron activation, both instrumental and radiochemical, is used for the investigation of pesticide residues and contaminants, viz. Hg, Se, As, Cd, Cu, Br, Co and Zn in rice and marine fish in Thailand. More than 500 samples of 6 species including squid of fish caught from polluted and non (less)-polluted areas in Thai waters, and of 17 varieties of non-glutinous rice and 6 varieties of glutinous rice of both brown and milled collected from 21 different rice experiment stations throughout the Kingdom are analyzed. The results of this study positively indicate that there is no contamination in fish and rice in Thailand. Additionally, the baseline concentration of studies trace toxic elements is established. (author)

  11. 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

  12. 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

  13. 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.

  14. Residues of organochlorine pesticides in surface soils from college school yards in Beijing, China

    WANG Xiaofei; WANG Dianzhong; QIN Xiaofei; XU Xiaobai

    2008-01-01

    Organochlorine pesticides (OCPs) have been a major environmental issue, attracting much scientific concern because of their nature of toxicity, persistence, and endocrine disrupting effects. Soil samples were collected from ten college school yards in Beijing in 2006 and analyzed to determine fifteen OCPs. Dichlorodiphenyltrichloroethanes (DDTs) were found to be the main pollutants, accounting for 93.70% of total OCPs, followed by hexachlorohexanes (HCHs) (2.25%) and hexachlorobenzene (HCB) (1.82%). Content of chlordanes (CHLs), heptachlors (HEPTs), and endosulfans comprised 0.51%, 1.05%, and 0.79% of fifteen OCPs, respectively. The preliminary pollution assessment indicated that DDTs have caused high OCPs levels in some schools. Source identification showed that HCHs in soils were originated from an old mixed source of technical HCHs and lindsne. And DDTs were mainly from mixed use of technical DDTs and dicofol containing DDT impurities. According to GB 15618-1995 (guidelines of Chinese environmental quality standards for soils), HCHs and DDTs levels might be categorized as little and low polluting pesticides. This study indicated that the environmental quality of college school yards with large green land were not as good as was expected and there existed potential exposure risk of college population to OCPs.

  15. Effects of processing on pesticide residues in peaches intended for baby food

    Balinova, Anna; Mladenova, Rosica; Shtereva, Deyana

    2006-01-01

    Abstract ABSTRACT Peaches containing incurred residues of chlorpyrifos-methyl, fenitrothion, procymidone and vinclozolin were submitted to simulated industrial processing to baby food puree. The residues were determined in raw material, in intermediate products at crucial steps of the processing procedures and in final products. The determination was performed by an analytical method distinguished by high sensitivity based on acetone extraction, 2 steps clean-up/preconcentration...

  16. Residues of polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and organochlorine pesticides in organically-farmed vegetables.

    Zohair, Azza; Salim, Abou-Bakr; Soyibo, Adeola A; Beck, Angus J

    2006-04-01

    The residues of polyaromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) in soils from organic farms and their uptake by four varieties of organic-produced potatoes and three varieties of organic carrots from England were investigated. Samples of the soils, crop peels and cores were all Soxhlet-extracted in triplicate, cleaned up by open-column chromatography and analysed by a multi-residue analytical method using gas chromatography with mass selective detection. The concentrations of PAHs, PCBs and OCPs in soils from organic farms ranged from 590+/-43 to 2301+/-146 microg/kg, 3.56+/-0.73 to 9.61+/-1.98 microg/kg and 52.2+/-4.9 to 478+/-111 microg/kg, respectively. Uptake by different crop varieties were 8.42+/-0.93 to 40.1+/-4.9 microg/kg sigmaPAHs, 0.83+/-0.19 to 2.68+/-0.94 microg/kg sigmaPCBs and 8.09+/-0.83 to 133+/-27 microg/kg sigmaOCPs. Residue uptake from soils depended on plant variety; Desiree potato and Nairobi carrot varieties were more susceptible to PAH contamination. Likewise, uptake of PCBs and OCPs depended on potato variety. There were significant positive correlations between the PCB and OCP concentrations (Ppotatoes. Peeling carrots and potatoes was found to remove 52-100% of the contaminant residues depending on crop variety and the properties of the contaminants. Soil-crop bioconcentration factors (BCFs) decreased with increasing logK(ow) for PAHs up to about 4.5 and for PCBs up to about 6.5, above which no changes were discernible for either class of contaminants. No relationship was observed between soil-crop BCFs and logK(ow) for OCPs, most likely because their concentrations were low and variable. PMID:16297429

  17. 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

  18. 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

  19. Study on Carrier Material of Immobilization Acetylcholinesterase For Biosensor in Detectionof Organophosphorus Pesticide Residues

    Sun, Xia; Wang, Xiangyou; Jia, Chuandong

    A comparison between several immobilization materials of AChE on surface of glassy carbon electrode(GCE) was presented. The immobilization methods employed crosslinking method with glutaraldehyde as a cross-linking agent and bovine serum albumin(BSA) as a protectant, AChE was immobilized on different membranes including nylon membrane, cellulose nitrate membrane and chitosan membrane respectively. The enzyme membrane was then fixed on the surface of glassy carbon electrode(GCE) with O-ring to prepare an amperometric biosensor for the detection of organophosphorus pesticides. The activity of immobilization AChE was detected by measuring the oxidation current of thiocholine, the results showed that the activity of immobilization AChE were all different with different membrane as carrier material.Compared with nylon membrane and cellulose nitrate membrane, chitosan membrane was obviously good. So chitosan membrane can be selected as immobilized AChE carrier material.

  20. 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

  1. 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

  2. Radiotracer studies of pesticide residues in edible oil seeds and related products

    Ten papers were presented in which chemical pollution due to insecticides was examined in edible oil seeds and their products. They include hexachlorocyclohexane residues in groundnut; carbaryl in groundnut; maize and cotton seed products, and in lactating goats; propoxur in cocoa beans; and leptophos residues in cotton seed and its products and in lactating goats. Eight of these papers constitute separate INIS entries. Egypt, Ghana, India, Korea, Lebanon, Pakistan, the Philippines, Poland, and the Sudan participated under the coordinated research programme. The progress of the programme is reviewed, and problems and priorities for future development of the programme are identified. A number of recommendations are addressed to the Joint FAO/IAEA Secretariat

  3. Estimating shadow prices and efficiency analysis of productive inputs and pesticide use of vegetable production

    Singbo, Alphonse G.; Lansink, Alfons Oude; Emvalomatis, Grigorios

    2015-01-01

    This paper analyzes technical efficiency and the value of the marginal product of productive inputs vis-a-vis pesticide use to measure allocative efficiency of pesticide use along productive inputs. We employ the data envelopment analysis framework and marginal cost techniques to estimate technic

  4. QuEChERS样品前处理-液相色谱-串联质谱法测定蔬菜中66种有机磷农药残留量方法评估%Evaluation of QuEChERS methods for the analysis of 66 organophosphorus pesticide residues in vegetables by liquid chromatography-tandem mass spectrometry

    王连珠; 周昱; 陈泳; 王瑞龙; 林子旭; 林德娟; 郑少惠

    2012-01-01

    A comparison was made between the two versions of QuEChERS sample preparation method for the extraction of 66 organophosphorus pesticides (OPPS) in vegetables. The two QuEChERS methods were the original method without buffer published in 2003, and the AOAC Official Method 2007. 01 with acetate buffer. The adsorption behaviors of primary secondary amine (PSA) sorbent and C18 sorbent on the OPPS were studied. The method of after-extraction addition was used to evaluate matrix effects for OPPS in matrix of broccoli, tomato, green soybean, radish and shallot during liquid chromatography-tandem mass spectrometry (LC-MS/ MS) analysis. As a result, the QuEChERS method with acetate buffer gave higher and more consistent recoveries for some of OPPS. The PSA sorbent and C18 sorbent can adsorb dibrom, so the QuEChERS method was not suitable for the analysis of dibrom. The maximum matrix effects were in the extracts of broccoli during LC-MS/MS analysis. In this article, OPPS were extracted using the QuEChERS method with acetate buffer, and analysed by LC-MS/MS under the optimized conditions with monitoring 132 MS/MS transitions of precursor ions (two for each pesticide) in one single run. Recoveries for all but dibrom at fortification levels of 10, 40,80 μg/kg in broccoli, tomato, green soybean, radish and shallot ranged from 55% to 122% with relative standard deviations of 1. 6% - 18%. The limits of quantification (S/N≥10) were 0. 1 -8 μg/kg. Based on these results, the analytical method was proven to be highly efficient, robust and sensitive, and suitable for the monitoring of the maximum residue limits (MRLs) of 66 OPPS in vegetables.%比较了两种版本QuEChERS方法(即发表于2003年未加缓冲盐的原创QuEChERS方法及加乙酸盐缓冲液的AOAC 2007.01方法)提取蔬菜中66种有机磷农药(OPPS)的有效性;考察了乙二胺-N-丙基硅烷(PSA)及C18吸附剂对66种OPPS的吸附作用;以提取后添加法评估了青花菜、番茄、枝豆、

  5. 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

  6. Development and validation of a multiresidue method for the determination of neonicotinoid and macrocyclic lactone pesticide residues in milk, fruits, and vegetables by ultra-performance liquid chromatography/MS/MS.

    Kamel, Alaa; Qian, Yaorong; Kolbe, Elizabeth; Stafford, Charles

    2010-01-01

    A multiresidue method was developed and validated for the determination of 13 neonicotinoid pesticides and metabolites, and nine macrocyclic lactone pesticides and veterinary drugs using SPE and ultra-performance liquid chromatography/MS/MS. The method was validated in milk, orange, spinach, apple, plum, watermelon, green bean, zucchini, broccoli, strawberry, grape, and tomato by analyzing replicates of residue-free control samples fortified with a mixture of 22 target analytes at three concentration levels. The recoveries of the analytes from the fortified matrixes were mostly within 70-120%, except for some of the neonicotinoid metabolites. The LOD values varied by analyte and matrix and ranged between 0.001-2 ng/g. The developed method was successful in combining two widely different classes of compounds into a single analysis. PMID:20480883

  7. 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...

  8. Bats at risk? Bat activity and insecticide residue analysis of food items in an apple orchard.

    Stahlschmidt, Peter; Brühl, Carsten A

    2012-07-01

    Although bats are reported as being threatened by pesticides, they are currently not considered in European Union pesticide risk assessments. The reason for that contradiction is probably related to the scarcity of information on bat activity in pesticide-treated fields and the pesticide residues on their food items. The authors recorded bat activity and measured pesticide residues on bat-specific food items following applications of two insecticides in an apple orchard. High activity levels of the common pipistrelle bat, a foraging habitat generalist, were detected. Airborne foragers and bats that take part of their food by gleaning arthropods from the vegetation were recorded frequently. The initial value and the decline of pesticide residues were found to depend on the arthropod type, their surface to volume ratio, their mobility, and the mode of action of the applied pesticide. The highest initial residue values were measured on foliage-dwelling arthropods. By following the toxicity-exposure ratio approaches of the current pesticide risk assessment, no acute dietary risk was found for all recorded bat species. However, a potential reproductive risk for bat species that include foliage-dwelling arthropods in their diet was indicated. The results emphasize the importance of adequately evaluating the risks of pesticides to bats, which, compared to other mammals, are potentially more sensitive due to their ecological traits. PMID:22505289

  9. Variability of pesticide residues in cauliflower units collected from a field trial and market places in Greece.

    Prodhan, M D H; Papadakis, Emmanouil-N; Papadopoulou-Mourkidou, Euphemia

    2016-09-01

    To estimate the variability of pesticide residue levels present in cauliflower units, a total of 142 samples were collected from a field trial of a cooperative farmer, and 120 samples were collected from different market places in Thessaloniki, Greece. The collected samples were extracted using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction technique, and the residues were determined by liquid chromatography-tandem mass spectrometry. The developed method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD), and limit of quantification (LOQ). The average recoveries for all the analytes, derived from the data of control samples fortified at 0.01, 0.05, 0.1, and 0.2 mg/kg, ranged from 74 to 110% with a relative standard deviation of ≤8%. The correlation coefficient (R(2)) was ≥0.997 for all the analytes using matrix-matched calibration standards. The LOD values ranged from 0.001 to 0.003 mg/kg, and the LOQ was determined at 0.01 mg/kg for all the sought analytes. The matrix effect was found to be at a considerable level, especially for cypermethrin and deltamethrin, amounting to +90% and +145%, respectively. For the field samples, the unit-to-unit variability factors (VFs) calculated for cypermethrin and deltamethrin were 2.38 and 2.32, respectively, while the average VF for the market basket samples was 5.11. In the market basket samples, residues of cypermethrin, deltamethrin, chlorpyrifos, and indoxacarb were found at levels ≥LOQ and their respective VFs were 7.12, 5.67, 5.28, and 2.40. PMID:27229457

  10. The Present Situation of Pesticide Residues in Vegetables and Fruits and the Progress of Detection Technique%果蔬中农药残留现状及检测技术的研究进展

    刘建慧; 孙鑫; 刘希光; 张升晓

    2014-01-01

    Pesticide residues do harm to people's health and lives. The article reviewed the present situation and detection technique research progress of pesticide residues in vegetables and fruits. At the same time , some new pesticide residue fast test technologies were discussed.%综述了果蔬中的农药残留现状、农药残留检测技术的研究进展和应用状况,探讨了近年发展起来的一些农药残留快速检测新技术。

  11. Applications of isotopic tracer in analysis of residual sulfonylurea herbicide

    The analysis technique of the agrochemical residue by isotopic tracer is significantly increased, and obtained substantial development. The progress of the isotopic analysis in four kinds of sulfonylurea herbicide residues was reviewed in this paper. (authors)

  12. Comparative Analysis on Pesticide Management System between America and China

    Cunzheng; ZHANG; Yong; GONG; Weili; SHAN; Xianjin; LIU

    2013-01-01

    The production and usage amount of pesticides in US rank the leading position in the world. On the basis of protecting the environment and human health, US government has enacted a series of laws and regulations to normalize and manage the production and use of pesticides so as to ensure the development of modern agriculture. In this paper, US pesticide management system is briefly reviewed and compared with the pesticide management system of China, which may provide good reference for china in establishing its own management system and make steps towards the international standard.

  13. 坚果中185种农药残留的气相色谱-串联质谱法测定%Determination of 185 Pesticide Residues in Nuts by Gas Chromatography Tandem Mass Spectrometry

    李南; 石志红; 庞国芳; 范春林

    2011-01-01

    accurate, and could be used for the routine analysis of pesticide residues in nuts.

  14. 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.

  15. QuEChERS—HPHPLC联用法检测蔬菜中有机磷农药多残留分析%Detection of Organophosphorus Pesticide Residues in Vegetable Using QuEChERS-HPLC

    胡井荣

    2012-01-01

    建立了QuEchERS—HPLC联用法检测蔬菜中有机磷农药多残留的方法。改进了QuEchERS前处理方法,提高回收率及结果准确性,然后运用HPLC进行分析检测,根据有机磷农药的差异,得出其最小检出限在0.02-55.75μg/kg之间,定量限0.1-189.23μg/kg,18种有机磷农药要在定量限浓度和四倍定量限浓度2个加标水平的回收率均在70-120%范围,相对标准偏差低于20%,试验表明本方法适用于蔬菜中有机磷农药的多残留检测分析。%This article reported that the method of detected Organophosphorus Pesticide Residues in Vegetable Using QuEChERS-HPLC. Through improvement of the QuEchERS pretreatment methods, recovery and accuracy as been well improved, and then use HPLC analysis detection, according to the difference of organophosphorus pesticide, and obtain the minimum detection limit is between 0.02-55.75μg/kg, LOQ is between 0.1-189.23μg/kg, 18 organophosphorus pesticide in LOQ concentration and four times the concentration of LOQ two labeled level of recovery are at 70 to 120% range, the relative standard deviation less than 20%, test shows that this method is applicable to vegetables of organophosphorus pesticide residue detection more analysis.

  16. 茶叶农药残留降解过程及方式的研究进展%he Research Review about the Process and the Modes of Degradation of Pesticide Residues in Tea

    单治国; 张春花; 张乃明

    2011-01-01

    Pesticide residue is an important issue about Quality and safety of tea, in the current large - scale production of tea, the use of pesticides is still inevitable. Based on natural degradation of pesticide residues of tea, it has important practical significance for quality and safety of tea which use biological, chemical and physical methods to reduce the pesticide residues of tea. This paper about degradation processes and degraded dation of pesticide residues in tea. modes of pesticide residues in tea, sums up the situation of research and look into the future of degradation of pesticide residues in tea.%农药残留是影响茶叶质量安全的重要问题,在当前茶叶大规模生产中,农药的使用仍不可避免。在茶叶农药残留自然降解的基础上,采用生物、化学和物理的农残降解方法来降低茶叶农残,对于茶叶质量安全具有重要的现实意义。通过研究,概述了茶叶农药残留降解过程及方式的研究情况,并展望了茶叶农残降解技术的发展。

  17. Comparative voltammetric study and determination of carbamate pesticide residues in soil at carbon nanotubes paste electrodes

    THOMMANDRU RAVEENDRANATH BAB

    2014-02-01

    Full Text Available In this investigation, the persistence of carbamate pesticides in soil samples was investigated. A simple and selective differential pulse adsorptive stripping voltammetry was selected for this investigation. Carbon nanotubes paste electrodes were used as working electrodes for differential pulse adsorptive stripping voltammetry and cyclic voltammetry. A symmetric study of the various operational parameters that affect the stripping response was carried out by differential pulse voltammetry. Peak currents were linear over the concentration range of 10-5 to 10-10 M with an accumulation potential of -0.6 V and a 70 s accumulation time with lower detection limits of 1.09 x 10-7 M, 1.07 × 10-7M, 1.09×10-7 M for chlorphropham, thiodicarb, aldicarb. The relative standard deviation (n=10 and correlation coefficient values were 1.15 %, 0.988; 1.13 %, 0.978; and 1.14 %, 0.987, respectively. Universal buffer with pH range 2.0 - 6.0 was used as sup­porting electrolyte. The solutions with uniform concentration (10-5 M were used in all deter­minations. Calculations were made by standard addition method.

  18. 四川省食品中农药残留状况%Study on Pesticide Residues Level of Food in Sichuan Province

    许毅; 林黎; 郭艳; 赵年华; 兰真; 颜玲

    2012-01-01

    目的 了解、分析四川省食品中农药残留状况,为制定相应控制措施提供依据.方法 2009年在四川省4个城市采集蔬菜、水果、鲜食用菌、茶叶共232份食品,进行有机磷、拟除虫菊酯类农药残留监测.结果 食品中农药总检出率为6.13%,总超标率为0.91%.结论 四川省蔬菜水果等食品中农药残留的总体水平不高,但部分食品存在较突出的农药污染问题,对此应进一步加大监管力度.%Objective To understand and analyze the status of pesticide residues contamination of food in Sichuan province, provide evidence for formulating appropriate control measures. Methods In 2009, totally 232 samples of vegetables, fruits, fresh edible mushroom and tea products in 4 cities of Sichuan province had been collected and tested for organophosphorus and pyrethroid pesticide residues monitoring. Results The total pesticide positive rate of food was 6. 13% , 99. 09% of food samples accorded with the National Standards. Conclusion Pesticide residues level of food in Sichuan is not high, but there is prominent pesticide pollution in some food products which should further intensify supervision.

  19. Validation and application of a multi-residue method, using accelerated solvent extraction followed by gas chromatography, for pesticides quantification in soil.

    Leyva-Morales, J B; Valdez-Torres, J B; Bastidas-Bastidas, P J; Betancourt-Lozano, M

    2015-01-01

    A multi-residue method was developed to determine different types of pesticides in soils. An extraction with pressure and temperature, through accelerated solvent extraction (dichloromethane:acetone, 50:50, v/v). The pesticides were determined by gas chromatography with several selective detectors: electron capture detector, pulsed flame photometric detector and thermionic specific detector. The following parameters were determined: limit of detection, limit of quantification, equipment linearity (working interval), method linearity as well as, method accuracy and precision. The average recoveries ranged between 76 and 106%, with the exception of chlorothalonil, which had an average recovery of 46%. Additionally, detection limits from 0.9 to 7.6ng g -: (1) and the quantification limits from 3.00 to 25.47ng g -: (1) were estimated. In terms of linearity and precision, the results obtained were in the ranges considered adequate (R(2) ≥ 0.98 and coefficient of variation (CV) ≤ 20%), with the exception of aldrin (R(2) = 0.946, CV = 35.79%), lindane (R(2) = 0.917, CV = 32.91%) and chlorothalonil (R(2) = 0.8184, CV = 81.35%). The proposed method was used to evaluate pesticides in real soil samples, detecting concentrations over 1000ng g -: (1) for some pesticides. The method was correctly validated and provided for the rapid determination of pesticides in soil. PMID:26041247

  20. Residue levels of organochlorine pesticides in some ecosystem components of Manzala Lake.

    Azab, M M; Darwish, A A; Mahmoud, Hend A; Sdeek, Fayza A

    2013-12-01

    To evaluate the organochlorine pesticide (OCP) contamination of Manzala Lake, its ecosystem was investigated during the winter season (December to March). The studied ecosystem components were water, sediment, aquatic weeds, and fishes in four locations. The samples were analyzed by gas chromatography with electron capture detector. Pollutant levels of total OCPs showed significantly high levels in the water areas of Round road (46.253 ng/ml), Port-Said Damietta road (19.301 ng/ml), followed by Bughas El-Rasoah (5.539 ng/ml), then Ashtoum El Gamel (natural reserve area now) (0.289 ng/ml). Organochlorines were detected in sediment only in Round road (3.359 μg/kg) and Port-Said Damietta road (0.171 μg/kg) by significant order while they were undetectable in Ashtoum El Gamel and Bughas El-Rasoah. Total OCPs in aquatic weeds ranged between 0.194 μg/kg in Port-Said Damietta and 0.026 μg/kg in Ashtoum El Gamel. While OCPs were 0.160 and 0.153 μg/kg in Round road and Bughas El-Rasoah, respectively. Concerning fish muscles OCPs were significantly higher in the Round road area (0.397 μg/kg) followed by the Port-Said Damietta road (0.258 μg/kg), and finally, Ashtoum El Gamel samples (0.126 μg/kg). The results revealed the direct relation for the accumulation of OCPs between studied ecosystem parameters at the Manzala Lake during the winter season. Results also demonstrated that fish samples collected from the Manzala Lake in the studied areas were contaminated with levels of organochlorines, not higher than the maximum permissible level recorded by FAO/WHO, and that the public is not at risk with fish consumption. PMID:23884913

  1. QuEChERS-HPHPLC联用法检测蔬菜中有机磷农药多残留分析%DETECTION OF ORGANOPHOSPHORUS PESTICIDE RESIDUES IN VEGETABLE USING QUECHERS-HPLC

    胡井荣

    2012-01-01

    建立了QuEchERS- HPLC联用法检测蔬菜中有机磷农药多残留的方法.改进了QuEchERS前处理方法,提高回收率及结果准确性,然后运用HPLC进行分析检测,根据有机磷农药的差异,得出其最小检出限在0.02μg/kg~55.75 μg/kg之间,定量限0.1μg/kg~189.23μg/kg,18种有机磷农药要在定量限浓度和四倍定量限浓度2个加标水平的回收率均在70%~120%范围,相对标准偏差低于20%,试验表明本方法适用于蔬菜中有机磷农药的多残留检测分析.%The method of detected Organophosphorus Pesticide Residues in Vegetable Using QuEChERS — HPLC was established. Through improvement of the QuEchERS pretreatment methods, recovery and accuracy was improved well. Then by using HPLC analysis detection, according to the difference of organophosphorus pesticide, the minimum detection limit was obtained as between 0. 02—55. 75/ng/kg, LOQ as between 0.1—189.23/ag/kg. At two labeled level of LOQ concentration and four times the concentration of LOQ, recovery of 18 organophosphorus pesticide was from 70% to 120%, and the relative standard deviation was less than 20%. It shows that this method is applicable to detect organophosphorus pesticide residue of vegetables.

  2. Bonding Analysis of Amino Resin Wood Adhesive with Pesticide Using Response Surface Method

    Bono, Awang; Rajin, Mariani; Siambun, Nancy Julius

    Wood base industries are among the dominant players in Malaysia economic activities. In this research, by using Response Surface Method (RSM), studies of bonding between Disodium Tetraborate Decahydrate (DTD) pesticide and various formulation of wood adhesive i.e., Melamine-Urea-Formaldehyde (MUF) resin is carried out. The RSM formulated twenty-five MUF formulations, consisting combination of different amount of formaldehyde, melamine, urea added in stage-1 and stage-2 of resin synthesis and DTD pesticide. The liquid products of resin are then hardened and tested using Fourier Transformation Infra-Red (FTIR) and visible spectrophotometer (VIS), to analyse the bonding of the resin and pesticide. The data from the FTIR and VIS analysis were then compiled and analysed using Response Surface Method. The results show that, different amount of the formaldehyde, melamine, urea and DTD pesticide, gives specific impact to the strength of MUF resin-pesticide bonding.

  3. 食品中农药残留检测前处理技术进展%A Review of Pretreatment Methods for Determination of Pesticide Residues in Food

    熊琳; 杨博辉; 牛春娥; 郭婷婷

    2012-01-01

    Sample preparation is the key part of determination of pesticide residues in food. All kinds of pretreatment methods for the determination of pesticide residues in food keep popping up to improve the accuracy and precision of determination, and improve greatly the efficiency of the determation of pesticide residues in food. This paper summarizes the pretreatment methods for determination of pesticide residues in food.%样品前处理是检测食品中农药残留的关键部分,为提高食品中农药残留检测的准确度和精确度,各种农药残留检测前处理技术不断地出现,极大地提高了食品中农药残留检测的效率,综述了食品中农药残留检测的样品前处理技术.

  4. Determination of organochlorine pesticide residue levels in chewable parts of the khat (Catha edulis) plant.

    Ligani, Shemsu; Hussen, Ahmed

    2014-11-01

    In this study, the levels of DDT and its metabolite residues were determined in chewable parts of Catha edulis plants grown in the southern part of Ethiopia. The levels of p,p'-DDT and p,p'-DDE were found to be in the range of 10.8-19.7 and 3.5-18.6 μg/kg, respectively. These data revealed that the residue being detected is from recent applications. The estimated daily intake of total DDT from C. edulis consumption was calculated to be in the range between 0.0278 and 0.0747 μg/kg, which is significantly lower than the FAO/WHO guideline. However, this may not guarantee safety, as the application of DDT extends to vegetables as well. Even though the use of DDT was banned in Ethiopia for agriculture purposes, detectable levels are still being observed. The results of the study necessitate the need for awareness creation among the people in the community. PMID:25260995

  5. Isolation and Identification of Specific Pathogens, Presence of Antibiotics, Aflatoxins, Pesticide Residues and Industrial Contaminants in Supply Chain of Milk in Selected Coastal Districts of Andhra Pradesh

    Appalanaidu Kalla; Sunitha Raju Kutcharlapati; Sai Bramari Gannavarapu; Anitha Layam

    2015-01-01

    A research study was undertaken to carry out isolation and identification of specific pathogens, presence of antibiotics, aflatoxins, pesticide residues and industrial contaminants in supply chain of milk in selected coastal districts of Andhra Pradesh. The milk is a whole food; it is categorized under perishable foods as it is biologically nutrient liquid that supports the growth of wide variety of microorganisms and is susceptible to spoilage. The quality of milk can be affected by the pres...

  6. Determination of organophosphorus pesticide residues in vegetables by an enzyme inhibition method using α-naphthyl acetate esterase extracted from wheat flour*

    WANG, JUN-LIANG; Xia, Qing; Zhang, An-Ping; Hu, Xiao-Yan; Lin, Chun-mian

    2012-01-01

    The widespread use of organophosphorus pesticides (OPs) poses a great threat to human health and has made the detection of OP residues in food an important task, especially in view of the fact that easy and rapid detection methods are needed. Because OPs have inhibitory effects on the activity of α-naphthyl acetate esterase (ANAE) in plants, in this work we evaluated the possibility of detecting OPs in vegetables with ANAE extracted from commercial flour. The limits of detection (LODs) obtain...

  7. Residues of Organochlorine Pesticides (OCPs) in Agricultural Soils of Zhangzhou City, China

    YANG Dan; CHEN Wei; YANG Jun-Hua; XU Mei-Hui; QI Shi-Hua; ZHANG Jia-Quan; TAN Ling-Zhi; ZHANG Jun-Peng; ZHANG Yuan; XU Feng; XING Xin-Li; HU Ying

    2012-01-01

    A soil survey was conducted in Zhangzhou City,an important agricultural region in south of the Fujian Province,China.93 surface soil samples were collected in the paddy fields,vegetable lands,orchards and tea plantations from Zhangzhou City.An additional soil profile was sampled in a paddy field as previous research had indicated high concentrations of organochlorine pesticides (OCPs) in the paddy fields.Dichlorodiphenyltrichloroethanes (DDTs) ranged from 0.64-78.07 ng g-1 dry weight and hexachlorocyclohexanes (HCHs) ranged from 0.72-30.16 ng g-1 dry weight in the surface soil of the whole study region.Ratios of α-HCH/γ-HCH < 4 and o,p'-DDT/p,p'-DDT > 1 in all soil samples suggested that lindane and dicofol were widely applied in this region in the past.Concentrations of HCHs and DDTs in soils from the four land use types followed the orders:paddy fields > vegetable lands > tea plantations > orchards and tea plantations > orchards > paddy fields > vegetable lands,respectively.Analyses of the data showed no correlation (r < 0.1) between elevation and OCPs contents in paddy fields,orchards and vegetable lands,indicated no significantly different features in distribution of HCHs and DDTs in the soils from low lying plains and mountains and the unsystematic usage of OCPs,and highlighted the fragmented nature of agricultural production in Zhangzhou,as well as the reemission of OCPs from the soils,where high OCPs concentrations were found,in Longhai of Zhangzhou.In addition,no obvious relationship between the OCPs and total organic carbon (TOC) (r < 0.3) was observed in the soil profile.The mean contribution of dicofol in total DDTs was 66% in the whole Zhangzhou region.The approximate burdens of HCHs and DDTs in the surface layer of 0-20 cm were 0.44 and 1.55 t,respectively.The storage of both HCHs and DDTs in soil surface layer (0-20 cm) accounts for 40% burden of the soil layer of 0-50 cm (1.10 t HCHs and 3.87 t DDTs),in which the highest

  8. Searching for a more sensitive earthworm species to be used in pesticide homologation tests – A meta-analysis.

    Joimel, Sophie; MAKOWSKI, DAVID; Makowski, Daniel

    2013-01-01

    Pesticide risk assessments include experiments designed to measure the effect of pesticides on earthworms using the Eisenia fetida fetida or Eisenia fetida andrei species. There is no clear consensus in the literature on the sensitivity of different earthworm species to pesticides. We performed a meta-analysis on the sensitivity of several earthworm species to pesticides to determine the most sensitive species, and to discuss their suitability for European homologation tests. A dataset i...

  9. Pesticides and health: A review of evidence on health effects, valuation of risks, and benefit‐cost analysis

    Andersson, Henrik; Tago, Damian; Treich, Nicolas

    2014-01-01

    In this paper, we provide reviews of recent scientific findings on health effects and preference valuation of health risks related to pesticides, and the role of benefit‐cost analysis in policies related to pesticides. Our reviews reveal that whereas the focus of the health literature has been on individuals with direct exposure to pesticides, e.g. farmers, the literature on preference elicitation has focused on those with indirect exposure, e.g. consumers. Our discussion of pesticides polici...

  10. Cytogenetic analysis of Pakistani individuals occupationally exposed to pesticides in a pesticide production industry.

    Bhalli, Javed A.; Khan, Q. M.; Haq, M. A.; Khalid, A. M.; Nasim, A

    2006-01-01

    Biomarkers of exposure & early effects: field studiesBiomarker:Liver enzymes, serum cholinesterase (SChE), micronucleus assay and some haematological parametersExposure/effect represented:pesticides(organophosphates and pyrethroids)Study design:case- control studyStudy size:29 exposed and 35 unexposedAnalytical technique:haematological assay, spectrophotometric method, MN measurementTissue/biological material/sample size:10 ml blood samplesRelationship with exposure or effect of interest (inc...

  11. A simple and efficient multi-residue method based on QuEChERS for pesticides determination in palm oil by liquid chromatography time-of-flight mass spectrometry.

    Sobhanzadeh, Elham; Abu Bakar, Nor Kartini; Bin Abas, Mhd Radzi; Nemati, Keivan

    2012-09-01

    In this study, a rapid, specific and sensitive multi-residue method based on acetonitrile extraction followed by dispersive solid-phase extraction (d-SPE) clean-up was implemented and validated for multi-class pesticide residues determination in palm oil for the first time. Liquid-liquid extraction followed by low-temperature precipitation procedure was evaluated in order to study the freezing-out clean-up efficiency to obtain high recovery yield and low co-extract fat residue in the final extract. For clean-up step, d-SPE was carried out using a combination of anhydrous magnesium sulphate (MgSO(4)), primary secondary amine, octadecyl (C(18)) and graphitized carbon black. Recovery study was performed at two concentration levels (10 and 100 ng g(-1)), yielding recovery rates between 74.52% and 97.1% with relative standard deviation values below 10% (n = 6) except diuron. Detection and quantification limits were lower than 5 and 9 ng g(-1), respectively. In addition, soft matrix effects (≤±20%) were observed for most of the studied pesticides except malathion that indicated medium (20-50%) matrix effects. The proposed method was successfully applied to the analysis of suspected palm oil samples. PMID:21989900

  12. Study of enzyme biosensor based on carbon nanotubes modified electrode for detection of pesticides residue

    Shu Ping Zhang; Lian Gang Shan; Zhen Ran Tian; Yi Zheng; Li Yi Shi; Deng Song Zhang

    2008-01-01

    The paper describes a controllable layer-by-layer (LBL) self-assembly modification technique of multi-walled carbon nanotubes(MWNTs) and poly(diallyldimethylammonium chloride) (PDDA) towards glassy carbon electrode (GCE), Acetylcholinesterase(ACHE) was immobilized directly to the modified GCE by LBL self-assembly method, the activity value of AChE was detected byusing i-t technique based on the modified Ellman method. Then the composition of carbaryl were detected by the enzyme electrodewith 0.01U activity value and the detection limit of carbaryl is 10-12 g L-1 so the enzyme biosensor showed good properties forpesticides residue detection.2008 Shu Ping Zhang. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.

  13. Research on a pesticide residue screening platform in botanical food%植物源性食品中农药残留筛选平台研究

    冯超; 徐骞; 金玉娥; 卢大胜; 陈冲; 熊丽蓓; 汪国权

    2015-01-01

    目的:针对植物源性食品中的未知农药残留,在原农药残留筛选平台的基础上,采用气相色谱-三重四极杆质谱联用仪和UPLC-Q-Orbitrap两种色质技术并配合商业和自建农药筛查库建立共1200多个农药及其降解产物的筛选平台,满足未知农残的快速筛选要求。方法建立筛选平台相关筛选方法和准则,并通过两次欧盟国际比对(EUPT)对该平台进行验证评估。结果该平台在24 h内可完成农残筛选,筛选方法基于农药数据库和空白基质,两次能力验证中阳性化合物的检出率均在90%以上且结果无假阳性。结论该平台利用串联质谱和高分辨质谱的高选择性,结合农药数据库和智能筛选软件,在无标准参考物质的情况下实现非靶向农药的快速筛查。%Objective To establish a rapid non-targeted pesticide residue screening platform involving more than 1200 pesticides residues and their degradation products by using gas chromatography tandem mass spectrometry/mass-spectrometry and ultra performance liquid chromatography-Q-Orbitrap technology for unknown pesticide residue in botanical food, on the basis of original screening platform. Methods The principal and criterion of pesticides screening platform were established, and the platform was evaluated through twice proficient tests from Europe Union Reference Lab. Results The platform successfully completed the tests based on comprehensive database and blank matrix in 24 h with 90% screening rate and without false positive. Conclusion The platform achieved rapid screening of non-targeted pesticide residue without reference of standard materials by using the properties of high selectivity of triple quadrupole and high-resolution mass spectrometer combined with comprehensive pesticides database and advanced compound screening software.

  14. Determination of pyrethroids pesticide residues in the roots of Zanthoxylum nitidum (Roxb.) DC%两面针中7种拟除虫菊酯农药残留分析

    莫遗盛; 冯洁; 周劲帆; 赖茂祥

    2013-01-01

    目的:分析两面针中拟除虫菊酯类农药残留,为两面针的安全用药及质量控制和标准制定提供科学依据.方法:应用GC-MS法、选择离子监测模式(SIM)对两面针中7种拟除虫菊酯农药残留进行检测.样品经石油醚-丙酮(4∶1,v/v)混合溶剂超声提取,无水硫酸钠-无水硫酸镁-PSA-石墨化碳固相萃取小柱净化,外标法定量,测定两面针中7种拟除虫菊酯类农药残留.结果:应用所建立的色谱方法,可成功地对两面针中7种拟除虫菊酯类农药准确定量和确证.在检测的12批次两面针中,除1号和4号样品含少量的联苯菊酯、8号和9号样品含少量氰戊菊酯和3号、4号、5号样品含少量溴氰菊酯外,其余样品均检测不到7种拟除虫菊酯类农药.结论:12批次两面针样品中7种拟除虫菊酯类农药均未超标.该方法可用于两面针中拟除虫菊酯类微量农药残留的检测,可以推广应用.%Objective:To analyze the pyrethroid pesticide residues in the roots of Zanthoxylum nitidum and provide the scientific foundation for medication safety,quality control and standard establishment.Methods:A GC-MS method with selected ion monitoring (SIM) mode was applied to determine pyrethroid pesticide residues in the roots of Zanthoxylum nitidum.The samples were extracted with the mixture solution of petroleum ether-acetone (4∶ 1,v/v) and ultrasonic vibrations,and the analytical samples were purified by anhydrous sodium sulfate-anhydrous magnesium sulfate-PSA-PestiCarb-phase extraction (SPE) cartridge.The samples were respectively injected into the GC-MS analytical system for simultaneous analysis of the pyrethroid pesticid residues in the roots of Zanthoxylum nitidum,with external standard method.Results:Accurate quantitation and confirmation of seven pyrethroid pesticide residues were obtained by the established GC-MS method.As a result,samples 1 and 4 were detected with small amounts of bifenthrin,samples 8 and 9 with

  15. The PERICLES research program: An integrated approach to characterize the combined effects of mixtures of pesticide residues to which the French population is exposed

    Due to the broad spectrum of pesticide usages, consumers are exposed to mixtures of residues, which may have combined effects on human health. The PERICLES research program aims to test the potential combined effects of pesticide mixtures, which are likely to occur through dietary exposure. The co-exposure of the French general population to 79 pesticide residues present in the diet was first assessed. A Bayesian nonparametric model was then applied to define the main mixtures to which the French general population is simultaneously and most heavily exposed. Seven mixtures made of two to six pesticides were identified from the exposure assessment. An in vitro approach was used for investigating the toxicological effects of these mixtures and their corresponding individual compounds, using a panel of cellular models, i.e. primary rat and human hepatocytes, liver, intestine, kidney, colon and brain human cell lines. A set of cell functions and corresponding end-points were monitored such as cytotoxicity, real-time cell impedance, genotoxicity, oxidative stress, apoptosis and PXR nuclear receptor transactivation. The mixtures were tested in equimolar concentrations. Among the seven mixtures, two appeared highly cytotoxic, five activated PXR and depending on the assay one or two were genotoxic. In some experiments, the mixture effect was quantitatively different from the effect expected from the addition concept. The PERICLES program shows that, for the most pesticides mixtures to which the French general population is exposed, the toxic effects observed on human cells cannot be easily predicted based on the toxic potential of each compound. Consequently, additional studies should be carried on in order to more accurately define the mixtures of chemicals to which the consumers are exposed, as well as to improve the investigation, prediction and monitoring of their potential human health effects

  16. Evaluation of QuEChERS sample preparation and liquid chromatography-triple-quadrupole mass spectrometry method for the determination of 109 pesticide residues in tomatoes.

    Golge, Ozgur; Kabak, Bulent

    2015-06-01

    A multiresidue method based on modified QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation, followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed and validated for the determination of 109 selected multiclass pesticides in tomatoes. The recovery yields ranged from 77.1% to 113.2%, with repeatabilities of 4.4-19.2% and within-laboratory reproducibilities of 7.1-18.4%. The limit of detections (LODs) for target analytes in tomato extract were between 0.5 and 10.8μgkg(-1), and the limit of quantifications (LOQs) were between 1.3 and 30.4μgkg(-1). The expanded measurement uncertainty was not higher than 30% for all target analytes. The method has been successfully applied to the analysis of 345 tomato samples obtained from local markets and tomato traders. Residues of acetamiprid, azoxystrobin and triadimefon were identified and measured in 9.6% of tomato samples, ranging from 0.015 to 0.37mgkg(-1). PMID:25624240

  17. Application of elevated temperature-dispersive liquid-liquid microextraction for determination of organophosphorus pesticides residues in aqueous samples followed by gas chromatography-flame ionization detection.

    Farajzadeh, Mir Ali; Afshar Mogaddam, Mohammad Reza; Rezaee Aghdam, Samaneh; Nouri, Nina; Bamorrowat, Mahdi

    2016-12-01

    In the present study, an elevated temperature, dispersive, liquid-liquid microextraction/gas chromatography-flame ionization detection was investigated for the determination, pre-concentration, and extraction of six organophosphorus pesticides (malathion, phosalone, dichlorvos, diazinon, profenofos, and chlorpyrifos) residues in fruit juice and aqueous samples. A mixture of 1,2-dibromoethane (extraction solvent) and dimethyl sulfoxide (disperser solvent) was injected rapidly into the sample solution heated at an elevated temperature. Analytical parameters, including enrichment factors (1600-2075), linearity (r>0.994), limits of detection (0.82-2.72ngmL(-1)) and quantification (2.60-7.36ngmL(-1)), relative standard deviations (<7%) and extraction recoveries (64-83%), showed the high efficiency of the method developed for analysis of the target analytes. The proposed procedure was used effectively to analyse selected analytes in river water and fruit juice, and diazinon was found at ngmL(-1) concentrations in apple juice. PMID:27374524

  18. Organochlorine pesticide residuals in chickens and eggs at a poultry farm in Beijing, China

    Tao, S. [Laboratory for Earth Surface Processes, College of Urban and Environmental Sciences, Peking University, Beijing 100871 (China); Department of Geosciences and Center for Applied Environmental Research, University of Missouri, Kansas City, MO 64110-2499 (United States)], E-mail: taos@urban.pku.edu.cn; Liu, W.X.; Li, X.Q.; Zhou, D.X.; Li, X.; Yang, Y.F.; Yue, D.P. [Laboratory for Earth Surface Processes, College of Urban and Environmental Sciences, Peking University, Beijing 100871 (China); Coveney, R.M. [Department of Geosciences and Center for Applied Environmental Research, University of Missouri, Kansas City, MO 64110-2499 (United States)

    2009-02-15

    Chicken organs, animal feed, droppings, and ambient air were sampled at a farm in Beijing to determine the concentrations of hexachlorocyclohexane isomers (HCHs) and dichlorodiphenyltrichloroethane and metabolites (DDTs). Mean fresh weight concentrations of HCHs and DDTs were 0.122 {+-} 0.061 ng/g and 0.051 {+-} 0.038 ng/g in the muscles. These values are 1-2 orders of magnitude lower than those reported in China in 1980. Contaminated feed was the main source of HCHs and DDTs. Only 12.8% of HCH and 3.3% of DDT of the amount consumed were excreted. Accumulated quantities of HCHs and DDTs increased during growth. However, concentrations of HCHs and DDTs did not increase because of dilution from rapid growth. Based on the observed residual levels in mature chicken and the average diet of residents of China, the contributions from chicken and egg consumption to per capita daily intake of HCHs and DDTs were 487% and 88% of those of fish consumption. - Ingestion of chicken and eggs is an important pathway of HCHs and DDTs exposure.

  19. Organochlorine pesticide residuals in chickens and eggs at a poultry farm in Beijing, China

    Chicken organs, animal feed, droppings, and ambient air were sampled at a farm in Beijing to determine the concentrations of hexachlorocyclohexane isomers (HCHs) and dichlorodiphenyltrichloroethane and metabolites (DDTs). Mean fresh weight concentrations of HCHs and DDTs were 0.122 ± 0.061 ng/g and 0.051 ± 0.038 ng/g in the muscles. These values are 1-2 orders of magnitude lower than those reported in China in 1980. Contaminated feed was the main source of HCHs and DDTs. Only 12.8% of HCH and 3.3% of DDT of the amount consumed were excreted. Accumulated quantities of HCHs and DDTs increased during growth. However, concentrations of HCHs and DDTs did not increase because of dilution from rapid growth. Based on the observed residual levels in mature chicken and the average diet of residents of China, the contributions from chicken and egg consumption to per capita daily intake of HCHs and DDTs were 487% and 88% of those of fish consumption. - Ingestion of chicken and eggs is an important pathway of HCHs and DDTs exposure

  20. Pesticide exposure - Indian scene

    Use of pesticides in India began in 1948 when DDT was imported for malaria control and BHC for locust control. India started pesticide production with manufacturing plant for DDT and benzene hexachloride (BHC) (HCH) in the year 1952. In 1958, India was producing over 5000 metric tonnes of pesticides. Currently, there are approximately 145 pesticides registered for use, and production has increased to approximately 85,000 metric tonnes. Rampant use of these chemicals has given rise to several short-term and long-term adverse effects of these chemicals. The first report of poisoning due to pesticides in India came from Kerala in 1958 where, over 100 people died after consuming wheat flour contaminated with parathion. Subsequently several cases of pesticide-poisoning including the Bhopal disaster have been reported. Despite the fact that the consumption of pesticides in India is still very low, about 0.5 kg/ha of pesticides against 6.60 and 12.0 kg/ha in Korea and Japan, respectively, there has been a widespread contamination of food commodities with pesticide residues, basically due to non-judicious use of pesticides. In India, 51% of food commodities are contaminated with pesticide residues and out of these, 20% have pesticides residues above the maximum residue level values on a worldwide basis. It has been observed that their long-term, low-dose exposure are increasingly linked to human health effects such as immune-suppression, hormone disruption, diminished intelligence, reproductive abnormalities, and cancer. In this light, problems of pesticide safety, regulation of pesticide use, use of biotechnology, and biopesticides, and use of pesticides obtained from natural plant sources such as neem extracts are some of the future strategies for minimizing human exposure to pesticides