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Sample records for pesticide residue analysis

  1. QA/QC in pesticide residue analysis

    International Nuclear Information System (INIS)

    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

    International Nuclear Information System (INIS)

    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. Analysis of pesticide residues and metabolites by radioactive tracers

    International Nuclear Information System (INIS)

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

  4. Optimisation of gas chromatography for pesticide residue analysis

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

  6. Application of High Performance Liquid Chromatography to the Analysis of Pesticide Residues in Eggplants

    Directory of Open Access Journals (Sweden)

    S. Islam

    2009-01-01

    Full Text Available A reverse phase high performance liquid chromatographic method with an acetonitrile-water mobile phase gradient and UV/Visible detection is described for the determination of three pesticides, frequently used in agriculture, in eggplant samples. The samples were sprayed with three pesticides namely, Diazinon, Malathion, Sumithion at three different doses and were harvested at two different Pre-Harvest Interval (PHI of days 1 and 5 after the application of the pesticides. Sample preparation involved extraction with ethyl acetate and clean up was accomplished by solid-phase extraction using florisil columns. Calibration curves that were constructed for the analytes with matrix matching followed linear relationships with good correlation coefficients (R2>0.990. The average recoveries of the pesticides which were sensitive to matrix effects ranged from 88-120%. Detection limit of less than 0.02 mg kg-1 showed that the method developed can be used to determine the pesticide residues in concentrations lower than the maximum residue limits. In the analysis of residues, samples treated with Diazinon at all doses, residual amounts above Maximum Residue Limit (MRL (0.02 mg kg-1 were found. Malathion and Sumithion were found above MRL (0.5 mg kg-1 value in only one sample for each pesticide.

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

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    Sheheli Islam

    2009-01-01

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

  8. Solid-phase extraction for multi-residue analysis of pesticides in honey.

    Science.gov (United States)

    Amendola, Graziella; Pelosi, Patrizia; Dommarco, Roberto

    2011-01-01

    A fast and simple multi-residue method for the analysis of 15 organophosphorus (OP), 17 organochlorine (OC), 8 pyrethroids (PYR), 12 N-methyl-carbamate (NMC) pesticide residues and bromopropylate in honey is presented. Ready-to-use EXtrelutNT 20 column, eluted with dichloromethane, was used to extract the pesticide residues from the aqueous-acetone honey sample, obtaining a clean extract directly analyzable. Determination was carried out by gas chromatography (GC) coupled with flame photometric detector (FPD) for OP compounds and by GC coupled with mass spectrometry detector (MSD) for OC and PYR pesticides and bromopropylate. The NMC pesticides were analysed by liquid chromatography-double derivatization coupled with spectrofluorimetric detector (LC/DD/Fl). This method allows the determination of the 53 pesticide residues at low concentrations (0.0005-0.074 mg/kg) and can be used to assess the compliance with the Maximum Residues Levels (MRLs) set by the European Union. The performance of the method was evaluated and specificity, linearity, recovery, repeatability, reproducibility, limit of quantification (LOQ) and limit of detection (LOD) were determined. A good linearity (r(2)? 0.99) was found in the range 0.0005-0.074 mg/kg for the majority of the compounds studied. Most of the pesticides had recoveries in the range 70-103 % and values of relative standard deviation (RSD) pesticides investigated was from 0.0005 to 0.025 mg/kg while the LOD ranged from 0.0002 to 0.008 mg/kg. PMID:20936565

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

    International Nuclear Information System (INIS)

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

  10. [Status of pesticide registration and residue analysis for traditional Chinese medicine in China].

    Science.gov (United States)

    Yang, Yin-Hui; Dou, Xiao-Wen; Kong, Wei-Jun; Yang, Mei-Hua; Chen, Shi-Lin; Xiao, Qiang

    2013-12-01

    The present paper outlined pesticide registration status for traditional Chinese medicines (TCMs) and summarized the characteristics of pesticide contamination in different regions of some widely used TCMs by retrieving last 10 years' literatures. At present, the problems of pesticide residues for TCM include less pesticide registrations, widespread high-residue organochlorine pesticides contamination, pesticide abuse, irregular GAP bases and imperfect pesticide limit standards, etc. According to the current situation, we should adopt some control measures to strengthen the quality control of TCMs so as to ensure the safety of TCMs and related products. PMID:24791523

  11. Matrix effects in pesticide multi-residue analysis by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Kruve, Anneli; Künnapas, Allan; Herodes, Koit; Leito, Ivo

    2008-04-11

    Three sample preparation methods: Luke method (AOAC 985.22), QuEChERS (quick, easy, cheap, effective, rugged and safe) and matrix solid-phase dispersion (MSPD) were applied to different fruits and vegetables for analysis of 14 pesticide residues by high-performance liquid chromatography with electrospray ionization-mass spectrometry (HPLC/ESI/MS). Matrix effect, recovery and process efficiency of the sample preparation methods applied to different fruits and vegetables were compared. The Luke method was found to produce least matrix effect. On an average the best recoveries were obtained with the QuEChERS method. MSPD gave unsatisfactory recoveries for some basic pesticide residues. Comparison of matrix effects for different apple varieties showed high variability for some residues. It was demonstrated that the amount of co-extracting compounds that cause ionization suppression of aldicarb depends on the apple variety as well as on the sample preparation method employed. PMID:18304557

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

    International Nuclear Information System (INIS)

    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)

  13. EVALUATION OF A NEW MICROVOLUME 3HSC ELECTRON CAPTURE DETECTOR AND ANCILLARY DATA SYSTEM FOR PESTICIDE RESIDUE ANALYSIS

    Science.gov (United States)

    The performance of a linearized 3HSc electron capture detector (ECD) and its ancillary data system was evaluated for use in the analysis of pesticide residues. Serial dilutions of pesticide standards were used to determine the maximum linear range and sensitivity of the detector....

  14. 76 FR 3601 - Codex Alimentarius Commission: Meeting of the Codex Committee on Pesticide Residues

    Science.gov (United States)

    2011-01-20

    ...FAO/WHO Meeting on Pesticide Residues (JMPR); considering...methods of sampling and analysis for the determination of pesticide residues in food and feed...Address Methods of Analysis for Pesticide Residues by the CCPR...

  15. 77 FR 3229 - Codex Alimentarius Commission: Codex Committee on Pesticide Residues (CCPR)

    Science.gov (United States)

    2012-01-23

    ...WHO Meeting on Pesticide Residues (JMPR); considering...sampling and analysis for the determination of pesticide residues in food and feed...Revision of the Risk Analysis Principles Applied...Committee on Pesticide Residues...

  16. The role of GC-MS/MS with triple quadrupole in pesticide residue analysis in food and the environment

    OpenAIRE

    Herna?ndez Herna?ndez, Fe?lix; Cervera Vidal, Mari?a Ine?s; Portole?s Nicolau, Tania; Beltra?n Arandes, Joaquim; Pitarch Arquimbau, Mari?a Elena

    2013-01-01

    Gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) using a triple quadrupole (QqQ) analyzer has in the last few years become a powerful technique for the determination of pesticide residues due to its robustness, and excellent sensitivity and selectivity. This review gives an overview of currently published applications of GC-MS/MS with a QqQ analyzer for pesticide residue analysis of different food and environmental sample matrices. This technique allows the reliable quantific...

  17. Multi-residue analysis of polycyclic aromatic hydrocarbons, polychlorobiphenyls, and organochlorine pesticides in marine sediments

    Energy Technology Data Exchange (ETDEWEB)

    Thompson, S.; Budzinski, H.; LeMenach, K.; Letellier, M.; Garrigues, P. [Laboratory of Environmental and Toxicological Chemistry, University of Bordeaux, Talence (France)

    2002-01-01

    A multi-residue analysis procedure using microwave-assisted extraction and pre-purification has been developed for the combined analysis of polycyclic aromatic hydrocarbons (PAH), polychlorobiphenyls (PCB), and organochlorine pesticides (OCP) in marine sediments. This procedure has been validated with certified marine sediment. Several surrogate standards have been employed and the use of octachloronaphthalene (OCN) as a surrogate standard for organochlorine determination in this matrix is discussed. The recoveries of all compounds were high (>70%) and the relative standard deviations are of the same order as the certified values. Different analytical problems are discussed, including DDT degradation in gas chromatography and laboratory PCB background levels. Quantification problems encountered for two pesticides (cis-chlordane and trans-nonachlor) were attributed to PAH interference in the GC-ECD chromatogram. (orig.)

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

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    Jelena Milinovi?

    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%.

  19. Multi-residue analysis of pesticides in tea by online SEC-GC/MS.

    Science.gov (United States)

    Xu, Xiao-Min; Yu, Cun; Han, Jian-Long; Li, Jia-Ping; El-Sepai, Fawzi; Zhu, Yan; Huang, Bai-Fen; Cai, Zeng-Xuan; Wu, Hong-Wei; Ren, Yi-Ping

    2011-01-01

    A multi-residue method for the analysis of pesticides in tea was developed by online size exclusion chromatography (SEC)-GC/MS with full scan mode. The sample was fortified with chlorpyrifos-d(10) isotope internal standard and extracted by acetonitrile. After purification by primary secondary amine sorbent and solvent exchange by SEC mobile phase, the sample was detected by online SEC-GC/MS. The purification result of the online system was evaluated by comparing the correlation between Chinese cabbage and tea matrix. The factors for method optimization included sample preparation, matrix effects and the instrument parameters of each online component. Scatter plot was introduced in this study to directly illustrate the results of the condition optimization and matrix effects in the online system. For most of the pesticides, the average recoveries ranged from 70 to 130% and the RSD were below 15%. The feasibility of the application of full scan mode in multi-residue determination of trace amounts of pesticides (LODs below 0.01 mg/kg) in a complex matrix was discussed. PMID:21246727

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

    OpenAIRE

    Jelena Milinovi?; Mirjana Markovi?; Dragan Markovi?; Rada ?urovi?

    2007-01-01

    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 ...

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

    International Nuclear Information System (INIS)

    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)

  2. Aqueous acetonitrile extraction for pesticide residue analysis in agricultural products with HPLC-DAD.

    Science.gov (United States)

    Watanabe, Eiki; Kobara, Yuso; Baba, Koji; Eun, Heesoo

    2014-07-01

    To reduce hazardous organic solvent consumption during sample preparation procedures as much as possible, an extraction method of smallest feasible sample volume (5g) using aqueous acetonitrile (MeCN) was developed to extract pesticide residues from agricultural samples prior to HPLC-DAD determination. Extraction with MeCN/water (1:1, v/v), and adjustment of the MeCN concentration by diluting with water after extraction recovered successfully most pesticides showing various physicochemical properties. The matrix effects of tested samples on the proposed method developed herein were generally negligibly-small. The average recoveries were in the range 70-120% for all pesticides with the coefficient of variation values below 20%. The reduction rate of organic solvents used for the proposed sample preparation method was up to approximately 60% compared with the Japanese authorised official method for pesticide residue analyses. These results demonstrate the feasibility of the proposed method for pesticides with diverse properties. PMID:24518309

  3. Testing the stability of pesticides during sample processing for the chlorpyrifos and malathion residue analysis in cucumber, including matrix effects.

    Science.gov (United States)

    Tiryaki, Osman; Baysoyu, Dilan; Seçer, Emine; Aydin, Gülizar

    2008-01-01

    This article describes the procedure of the testing the stability of compounds during sample processing for the pesticide residue analysis in cucumber, including matrix matched assessment. To find out significant differences, one-tailed t test was applied to the data at 95% confidence level. Our results showed that the calculated value was bigger than the critical value (t ( calc ) > t ( crit )), which means the pesticides were decomposed under our processing conditions. PMID:17999016

  4. SBSE-GC-ECD/FPD in the analysis of pesticide residues in Passiflora alata dryander herbal teas

    OpenAIRE

    Bicchi, Carlo; Rubiolo, Patrizia; Cordero, Chiara Emilia Irma

    2003-01-01

    Stir bar sorptive extraction (SBSE) in combination with GC-ECD/FPD analysis is here applied to the determination of the residues of 11 pesticides (hexachlorobenzene, lindane, chlorothalonil, parathion methyl, parathion ethyl, fenitrothion, malathion, dieldrin, - and -endosulfan, and tetradifon) in herbal teas prepared with Passiflora alata Dryander spiked leaves. The method was optimized using spiked herbal teas in a range from 0.05 to 1 pg/L for organochlorine pesticides and from 0.15 to 3 p...

  5. Multi-Residue Analysis of Pesticides in Pistachio Using Gas Chromatography-Mass Spectrometry (GC/MS

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    Azadeh Emami

    2014-12-01

    Full Text Available Background: Analysis of pesticide residues in food and other environmental commodities have become an essential requirement for consumers, producers, food inspectors and authorities. This study is focused on validation of an accurate, rapid and reliable method for multi-residual analysis of pesticides in pistachio as a strategic crop for export and one of the main nuts in Iranian food basket. Methods: We developed a "Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS method based on spiking blank samples and used the data for drawing calibration curves instead of standard solutions. Sample preparations were developed for determination of 12 pesticide residues in pistachio by gas chromatography-mass spectrometry (GC/MS. Results: Recovery of pesticides at 5 concentration levels (n=3 was in the range of 81.40% - 93.08 %. The method proved to be repeatable in the majority of samples with relative standard deviation (RSD of lower than 20%. The limits of detection and quantification for all pesticides were 2 ppb and 10 ppb, respectively. Conclusion: The calibration curves of pesticides were linear in the range of 10-500 (ng/g and correlation coefficient of entire pesticides was higher than 0.994. The recovery of pesticides at 5 concentration levels (n=3 was in range of 81.41- 91.80 %. The method was proved to be repeatable with the majority of RSDs being lower than 20%. The limits of detection and quantification for all pesticides were 2 and 10 ppb, respectively. The recoveries and repeatabilities were in accordance with the criteria set by SANCO Guideline (Commission of the European Communities, 2006.

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

    Science.gov (United States)

    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...

  7. 76 FR 6465 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2011-02-04

    ...Petitions Filed for Residues of Pesticide Chemicals in or on...40 CFR part 180 for residues of the herbicide glyphosate...are available for analysis of residues of glyphosate and...GLC), Method I in Pesticides Analytical...

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

    International Nuclear Information System (INIS)

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

  9. Pesticide residue analysis of soil, water, and grain of IPM basmati rice.

    Science.gov (United States)

    Arora, Sumitra; Mukherji, Irani; Kumar, Aman; Tanwar, R K

    2014-12-01

    The main aim of the present investigations was to compare the pesticide load in integrated pest management (IPM) with non-IPM crops of rice fields. The harvest samples of Basmati rice grain, soil, and irrigation water, from IPM and non-IPM field trials, at villages in northern India, were analyzed using multi-pesticide residue method. The field experiments were conducted for three consecutive years (2008-2011) for the successful validation of the modules, synthesized for Basmati rice, at these locations. Residues of tricyclazole, propiconazole, hexconazole, lambda cyhalothrin, pretilachlor chlorpyrifos, DDVP, carbendazim, and imidacloprid were analyzed from two locations, Dudhli village of Dehradun, Uttrakhand and Saboli and Aterna village of Sonepat, Haryana. The pesticide residues were observed below detectable limit (BDL) (Residues were below detection level (Residues of tricyclazole and carbendazim, analyzed from same locations, revealed pesticide residues as BDL (residues of tricyclazole, propioconazole, chlorpyrifos, hexaconazole, pretilachlor, and ?-cyhalothrin were also found as BDL (<0.001-0.05 ?g/g) in 40 samples of Basmati rice grains and soil and 12 water samples (<0.001-0.05 ?g/L) (2010-2011). PMID:25213562

  10. Pesticide residues in locally available cereals and vegetables

    International Nuclear Information System (INIS)

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

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

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    Seema Tahir

    1999-01-01

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

  12. Electrospray ionization matrix effect as an uncertainty source in HPLC/ESI-MS pesticide residue analysis.

    Science.gov (United States)

    Kruve, Anneli; Herodes, Koit; Leito, Ivo

    2010-01-01

    The matrix effects in HPLC/electrospray ionization (ESI)-MS analysis are difficult to compensate for because of their large variability. It is, therefore, often more practical to include uncertainty due to the matrix effect into the uncertainty budget rather than try to compensate. This work presents an empirical approach--the matrix effect graph approach--for estimating the uncertainty due to the matrix effect in HPLC/ESI-MS analysis of pesticide residues in fruits and vegetables. At certain time intervals (1 month), a calibration graph using extracts of different fruits/vegetables as calibration solutions is prepared, and a regression line is fitted through these data. These fruits/vegetables may be either from the commodity group of the samples or from different commodity groups. The relative residuals of the calibration point peak areas are calculated and plotted against the measurement time. We term the resulting graph the matrix effect graph. The root mean square of the relative residuals is calculated and used as the estimate of relative uncertainty of the sample peak areas caused by the matrix effect. The matrix effect graph obtained over fruits/vegetables from different commodity groups can also be used to identify fruits/vegetables with extreme matrix effects. The matrix effect graph approach was used for determination of thiabendazole, aldicarb, imazalil, and methiocarb and was validated with tomato, cucumber, and sweet corn matrixes at the 0.5 mg/kg concentration level. When different commodity groups were used to compile the matrix effect graph, results of analysis of all samples agreed with the spiked concentrations within the expanded uncertainties (at k=2 level). When the matrix effect graph was compiled using fruits from the same commodity group as the analyzed samples (fruiting vegetables in this case), agreement was found in 98% of the cases. PMID:20334192

  13. Matrix effects observed during pesticides residue analysis in fruits by GC.

    Science.gov (United States)

    Freitas, Silvia de Sousa; Lanças, Fernando M

    2009-11-01

    The influence of the sample matrix in the GC-electron-capture detection analysis of the pesticides dimethoate, diazinon, chlorothalonil, parathion methyl and fenitrothion in fruits samples has been studied. Experiments have been carried out where the pesticide responses in standard solutions prepared in selected solvent were compared with their response when present in apple, mango, papaya, banana, pineapple and melon extracts. The presence of matrix effects (MEs) and their extent were shown to be simultaneously influenced by several factors (matrix concentration, matrix type, pesticide concentration, analytical range). Pronounced MEs were observed particularly for dimethoate and diazinon in all matrices tested; in lower concentrations, all pesticides presented significant ME. The other pesticides presented variable ME. Higher ME enhancement was detected at lower pesticide concentration levels of and/or at higher matrix concentration solutions. The ME detected for fenitrothion, in the analytical range evaluated, were dependent on matrix type. For each pesticide, solvent and matrix-matched calibrations were compared for all fruit samples, and it could be concluded that quantitation based on standard solutions prepared in blank matrix extract (matrix-matched calibration) should be used to compensate the MEs and to obtain more accurate results for the pesticides studied. PMID:19877144

  14. Application of Molecularly Imprinted Polymers for the Analysis of Pesticide Residues in Food—A Highly Selective and Innovative Approach

    Directory of Open Access Journals (Sweden)

    Raquel Garcia

    2011-12-01

    Full Text Available The increasing application of pesticides for agricultural purposes involves serious risk to the environment and human health due to either exposure or through residues in food and drinking water. Since food safety is of mandatory importance there is a growing interest on the development of selective, simple, rapid, cost-effective and reliable analytical methodologies in order to ensure that pesticides residues should not be found at levels above the established maximum pesticide residue limits (MRLs. In recent years, a new methodology based on the development of molecularly imprinting polymers (MIPs allows not only pre-concentration and cleaning of the sample but also selective extraction of the target analyte, which is crucial, particularly when the sample is complex and impurities can interfere with quantification. The scope of this review is to provide a general overview on MIPs field, with emphasis on MIP preparation and its use as sorbents for solid-phase extraction. This paper will be focused on the review of the current state of the art in the use of MIPs as selective materials in molecularly imprinted solid-phase extraction (MISPE for the analysis of pesticide residues from food matrices. A review of preparation and application of MIPs in food matrices, will also be discussed.

  15. Pesticide residue analysis in parsley, lettuce and spinach by LC-MS/MS.

    Science.gov (United States)

    Esturk, Okan; Yakar, Yasin; Ayhan, Zehra

    2014-03-01

    In this study, pesticide residues in parsley, lettuce and spinach (120 samples) were analyzed by the application of liquid chromatography-tandem mass spectrometry (LC-MS/MS). All samples of spinach, parsley or lettuce contained residues of three or more active substances. In parsley, carbendazim (100.0%), dichlorvos (100.0%), fenarimol (40.0%), pendimethalin (95.0%), in lettuce, diazinon (30.0%), dichlorvos (100.0%), pendimethalin (92.5%) phenthoate (12.5%), and in spinach, carbendazim (45.0%), cymoxanil (85.0%), dichlorvos (100.0%) and fenarimol (85.0%) were the significant active compounds. The maximum residue limits were exceeded in 28, 20 and 40 samples of parsley, lettuce and spinach, respectively. The results showed that there was a high occurrence of pesticide residues in parsley, lettuce and spinach samples from Hatay province, in which most of them were prohibited from use in Turkey for these vegetables. The contamination levels of these residues may be considered a serious public health problem according to the maximum residue limits (MRLs) of Turkey and the European Union (EU). PMID:24587520

  16. An applicable strategy for improvement recovery in simultaneous analysis of 20 pesticides residue in tea.

    Science.gov (United States)

    Shoeibi, Shahram; Amirahmadi, Maryam; Rastegar, Hossein; Khosrokhavar, Roya; Khaneghah, Amin Mousavi

    2013-05-01

    It is important to have a reliable method to analyze pesticides in tea, a beverage commonly consumed in Iran. A validated method was developed for the determination of 20 pesticides in tea based on QuEChERS sample preparation and capillary gas chromatography-quadrupole mass spectrometry in selective ion monitoring mode (GC-MS/SIM) using triphenyl methane (TPM) solution as an internal standard. We used fortified, extracted, and cleaned-up tea samples instead of calibration standards for quantitation, which substantially reduced adverse matrix-related effects and negative recovery affected by graphite carbon black (GCB) on pesticide analysis. The recovery of pesticides at 3 concentration (40, 60, and 240 ng/g) ranged from 79.5% to 111.4% (n = 3). The method had acceptable repeatability with RSDr pesticides were ?20 ng/g. The analytical results of the proposed method were in good agreement with proficiency test results (FAPAS, 19116). The recoveries and repeatabilities were in accordance with the criteria set by SANCO Guideline. The validated method was suitable for the analysis of pesticides in tea. PMID:23534490

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

    International Nuclear Information System (INIS)

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

  18. Application of Molecularly Imprinted Polymers for the Analysis of Pesticide Residues in Food—A Highly Selective and Innovative Approach

    OpenAIRE

    Raquel Garcia; Maria João Cabrita; Ana Maria Costa Freitas

    2011-01-01

    The increasing application of pesticides for agricultural purposes involves serious risk to the environment and human health due to either exposure or through residues in food and drinking water. Since food safety is of mandatory importance there is a growing interest on the development of selective, simple, rapid, cost-effective and reliable analytical methodologies in order to ensure that pesticides residues should not be found at levels above the established maximum pesticide residue limit...

  19. 78 FR 16243 - Codex Alimentarius Commission: Codex Committee on Pesticide Residues (CCPR)

    Science.gov (United States)

    2013-03-14

    ...considering methods of sampling and analysis for the determination of pesticide residues in food and feed; considering...suitability assessment of methods of analysis for pesticide residues Revision of the Risk Analysis Principles applied by the...

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

    Directory of Open Access Journals (Sweden)

    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.

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

    Science.gov (United States)

    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 <20%. The method was successfully applied to 13 actual samples collected from a local market, and none of the samples were found to contain pesticide residues. This method is suitable for the identification and quantification of systemic pesticides with matrix-matched standards in various baby foods. PMID:24861738

  2. The 2011 European Union Report on Pesticide Residues in Food

    OpenAIRE

    European Food Safety Authority

    2014-01-01

    The report presents the results of the control activities related to pesticide residues in food carried out in 2011 in 29 European countries (27 Member States and 2 EFTA countries). The report also presents a dietary risk assessment. On the basis of the detailed analysis of the results, EFSA derived some recommendations aimed at improving the enforcement of the European pesticide residue legislation. In 2011, more than 79,000 samples of more than 600 food products were tested for pesticide re...

  3. Targeted pesticide residue analysis using triple Quad LC-MS/MS.

    Science.gov (United States)

    Alder, Lutz

    2011-01-01

    The determination of pesticide residues by HPLC-MS/MS requires decisions on a multitude of analytical parameters. This includes the selection of eluents, columns and ion sources, but also the optimization of the tandem mass spectrometer for the selected target analytes. Another aspect is the use of the restricted acquisition time between two chromatographic data points. An appropriate selection of all these parameters as well as the measures to avoid interference by cross talks and wrong quantitative results by matrix effects is discussed in this chapter. PMID:21643908

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

    Directory of Open Access Journals (Sweden)

    Zuin Vânia G.

    2003-01-01

    Full Text Available This paper proposes a method based on matrix solid phase dispersion (MSPD to determine the presence of organochlorine (OC and organophosphorus (OP pesticide residues in species of Passiflora L. (passion fruit leaves by gas chromatography, using an electron capture detector (HRGC-ECD. A comparison with conventional methods, mainly the European Pharmacopoeia method (EP, showed MSPD to be efficient, fast, simple and easy to perform. To date, there are no official methods or limits that take into account Brazil's "real life" conditions in the analysis of pesticides in medicinal plants and phytomedicines, and the MSPD method described herein has proved to be a feasible one for the analysis of Passiflora L-based phytomedicines.

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

    Directory of Open Access Journals (Sweden)

    Jozef Sokol

    2010-07-01

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

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

    International Nuclear Information System (INIS)

    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. Investigation of preconcentration strategies for the trace analysis of multi-residue pesticides in real samples by capillary electrophoresis.

    Science.gov (United States)

    da Silva, Clóvis L; de Lima, Elizabete C; Tavares, Marina F M

    2003-10-01

    In this work, on-line preconcentration strategies were investigated for the multi-residue analysis of pesticides in drinking water and vegetables using micellar electrokinetic chromatography. Among the on-line strategies, sweeping and stacking with reverse migration of micelles (SRMM), with and without the insertion of a plug of water before sample injection, were contrasted. A new version of SRMM was also introduced. The modification consisted of momentarily applying a positive voltage at the inlet vial right after sample has been injected, increasing the efficiency by which the analytes are captured. Nine pesticides from different classes, carbendazim (benzimidazole), simazine, atrazine, propazine and ametryn (triazine), diuron and linuron (urea), carbaryl and propoxur (carbamate), were baseline separated in less than 6 min with a electrolyte composed of 20 mmol l(-1) phosphate buffer at pH 2.5, containing 25 mmol l(-1) sodium dodecyl sulfate and 10% methanol. Limits of detection (LODs) in the order of 2-46 microg l(-1) for the pesticides under investigation were obtained solely using the on-line strategies. Enrichment factors of 3-18-fold were obtained. These factors were computed as the improvement of the concentration LODs with respect to the reference condition (injection of 10 s at 2.5 kPa pressure). The proposed methodologies were applied to the analysis of pesticides in complex matrices such as carrot extracts where the detection of 2.5 microg l(-1) was illustrated. By combining off-line solid-phase extraction and the proposed on-line strategies, the detection of pesticides in drinking water at the 0.1 microg l(-1) level was conceived. PMID:14558617

  8. 75 FR 80489 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2010-12-22

    ...for residues of pesticides in or on food commodities...CFR part 180 for residues of the herbicide...enforcement method for residues of dichlormid in...ACL) of EPA. Analysis is carried out using...a tolerance for residues of 5-chloro...million (ppm) in pesticide formulations....

  9. Pesticide Residues and Bees – A Risk Assessment

    Science.gov (United States)

    Sanchez-Bayo, Francisco; Goka, Koichi

    2014-01-01

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

  10. Benefits and pitfalls of the application of screening methods for the analysis of pesticide residues in fruits and vegetables.

    Science.gov (United States)

    Malato, Octavio; Lozano, Ana; Mezcua, Milagros; Agüera, Ana; Fernandez-Alba, Amadeo R

    2011-10-21

    The goal of this study was to expand knowledge on the performance of screening methods based on accurate mass measurements using a liquid chromatography electrospray quadrupole time-of-flight mass spectrometry (LC-ESI-QTOF-MS) system operating in full scan mode and with automatic identification based on the use accurate-mass databases. The study involved the analysis of 97 pesticides, in five matrices (tomato, pepper, zucchini, orange and leek) and at three concentration levels (20, 50 and 100 ?g kg(-1)). Aspects concerning optimization of the search parameters, sensitivity, matrix effects, efficiency of the algorithm search, usefulness of fragment ions, etc., are evaluated in deep. Sensitivity requirements have been identified as the main obstacle affecting the automatic identification of pesticides, especially in complex matrices, where the ionization suppression reduces the detectability of analytes. In addition, we have detected some failures in the software used for automatic data processing in terms of analysis of isobaric compounds, use of isotopic clusters, spectral deconvolution and data processing speed that hamper the correct identification in some pesticide/matrix combinations. These drawbacks should be improved in the future for its effective implementation in routine residue analysis. PMID:21798548

  11. Radioisotopes in pesticide residues and metabolic studies

    International Nuclear Information System (INIS)

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

  12. Analysis of pesticide residues in rice using matrix solid-phase dispersion (MSPD)

    Scientific Electronic Library Online (English)

    Haroldo S., Dórea; Ledjane, Lima Sobrinho.

    2004-10-01

    Full Text Available SciELO Brazil | Language: English Abstract in portuguese Este trabalho apresenta um método multirresíduo de extração por dispersão da matriz em fase sólida (MSPD) para quantificação de dois inseticidas organofosforados (malation e paration metílico) e um organoclorado (beta-endosulfan) em arroz por cromatografia gasosa de alta resolução com detector por c [...] aptura de elétrons. Experimentos foram realizados com adição de pesticidas na amostra, variando quantidades de amostra e de suporte, tipo de suporte e solvente de eluição. A eficiência do método proposto foi demonstrada pelos valores médios de recuperação entre 75,5% e 116,0%, com valores de desvio padrão relativo entre 0,5% e 10,9%, obtidos nas análises de recuperação com amostras fortificadas nos níveis de 0,5 a 10,0 mg kg-1. Os limites de detecção foram de 20 a 105 pg para os pesticidas estudados. Arroz comercial foi analisado para a aplicação do método. Abstract in english This work reports a multi-residue extraction method based on matrix solid-phase dispersion (MSPD) and capillary gas chromatography - electron capture detection for quantification of two widely used organophosphorus insecticides (malathion and parathion-methyl) and an organochlorine pesticide (beta-e [...] ndosulfan) in rice. A set of experiments was done with a spiked matrix with a standard mix, varying sample and solid phase amounts, solid phase and eluting solvent. Analyses of fortified rice samples were performed at different levels (0.5-10.0 mg kg-1). Mean recoveries from three replicates ranged from 75.5% to 116.0%, with coefficients of variation from 0.5% to 10.9%. The limit of detection was in the range of 20 to 105 pg for the pesticides. Commercial rice was analyzed for method application.

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

    OpenAIRE

    Herna?ndez Herna?ndez, Fe?lix; Beltra?n Arandes, Joaquim; Portole?s Nicolau, Tania; Pitarch Arquimbau, Mari?a Elena; Cervera Vidal, Mari?a Ine?s

    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 (appl...

  14. Decline of Pesticide Residues from Barley to Malt

    OpenAIRE

    Navarro, Simon; Vela, Nuria; Pe?rez, Gabriel; Navarro, Gine?s

    2007-01-01

    Abstract The fate of dinitroaniline herbicides (pendimethalin and trifluralin), organophosphous insecticides (fenitrothion and malathion), and pyrimidine (nuarimol) and triazole (myclobutanil and propiconazole) fungicides from barley to malt has been assessed. Several samples for residue analysis were taken after each stage of malting (steeping, germination, and kilning). Analyses of pesticide residues were carried out by GC/ITMS in SIM mode. Pesticides decline along the process al...

  15. Determination of Pesticide Residues in Cannabis Smoke

    OpenAIRE

    Nicholas Sullivan; Sytze Elzinga; Raber, Jeffrey C.

    2013-01-01

    The present study was conducted in order to quantify to what extent cannabis consumers may be exposed to pesticide and other chemical residues through inhaled mainstream cannabis smoke. Three different smoking devices were evaluated in order to provide a generalized data set representative of pesticide exposures possible for medical cannabis users. Three different pesticides, bifenthrin, diazinon, and permethrin, along with the plant growth regulator paclobutrazol, which are readily available...

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

    Directory of Open Access Journals (Sweden)

    Rada ?urovi?

    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%.

  17. 75 FR 46924 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2010-08-04

    ...01 mg/kg with final analysis by LC-MS/MS for...40 CFR part 180 for residues of the [[Page 46926...are available for the analysis of residues of dicamba and its relevant...livestock commodities. Pesticide Analytical...

  18. 75 FR 28009 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2010-05-19

    ...Petitions Filed for Residues of Pesticide Chemicals in or...CFR part 180 for residues of the insecticide...methodology LC/MS/MS analysis is available to...CFR 180.593 for residues of the miticide...when used as a pesticide inert...

  19. Application of High Performance Liquid Chromatography to the Analysis of Pesticide Residues in Eggplants

    OpenAIRE

    Islam, S.; Hossain, M. S.; Nahar, N.; Mosihuzzaman, M.; Mamun, M. I. R.

    2009-01-01

    A reverse phase high performance liquid chromatographic method with an acetonitrile-water mobile phase gradient and UV/Visible detection is described for the determination of three pesticides, frequently used in agriculture, in eggplant samples. The samples were sprayed with three pesticides namely, Diazinon, Malathion, Sumithion at three different doses and were harvested at two different Pre-Harvest Interval (PHI) of days 1 and 5 after the application of the pesticides. Sample prepara...

  20. Planar solid phase extraction clean-up for pesticide residue analysis in tea by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Oellig, Claudia; Schwack, Wolfgang

    2012-10-19

    Efficient clean-up is indispensable for preventing matrix effects in multi-residue analysis of pesticides in food by liquid and gas chromatography (LC and GC) coupled to mass spectrometry (MS). High-throughput planar solid phase extraction (HTpSPE) was recently introduced as a new clean-up concept in residue analysis of pesticides in fruit and vegetables (C. Oellig, W. Schwack, 2011 [45]). Thin-layer chromatography (TLC) was used to completely separate pesticides from matrix compounds and to focus them into a sharp zone, followed by extraction of the target zone by the TLC-MS interface. As rather challenging matrices, tea samples were chosen in this study. Besides chlorophylls and polyphenols, high amount of caffeine is co-extracted resulting in strong matrix effects both in LC-MS and GC-MS. The former HTpSPE procedure was adapted to initial extracts of green and black tea resulting in colorless extracts nearly free of matrix effects and interferences, as shown for seven chemically representative pesticides (acetamiprid, penconazole, azoxystrobin, chlorpyrifos, pirimicarb, fenarimol, and mepanipyrim). LC-MS/MS calibration curves obtained in the range of 0.002-0.5 mg/kg from matrix-matched standards and solvent standards were nearly identical and demonstrated the effectiveness of clean-up by HTpSPE. Mean recoveries determined by LC-MS/MS against solvent standards at spiking levels of 0.01 and 0.1 mg/kg ranged between 72 and 114% with relative standard deviations (RSDs) of 0.7-4.7% (n=4), while LC-MS measurements of tea samples spiked at 1 mg/kg provided recoveries of 81-104% with RSDs of 1.2-4.9% (n=6). Using LC-MS/MS, the method showed high sensitivity with signal-to-noise ratios>10 for concentrations below 0.002 mg/kg. HTpSPE of one sample was done in a few minutes, while numerous samples were cleaned in parallel at minimal costs with very low sample and solvent consumption. PMID:22981507

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

    Science.gov (United States)

    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

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

    Scientific Electronic Library Online (English)

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

    2003-04-01

    Full Text Available SciELO Brazil | Language: English Abstract in portuguese Neste trabalho é proposto um método baseado na dispersão da matriz em fase sólida (MSPD) para a determinação de resíduos de pesticidas organoclorados (OC) e organofosforados (OP) por cromatografia em fase gasosa com detector de captura de elétrons (HRGC-ECD) em folhas de espécies de Passiflora L. (m [...] aracujá). Em confronto com os métodos convencionais, sobretudo versus o descrito pela Farmacopéia Européia (EP), a MSPD mostrou-se eficiente, rápida, simples e de fácil execução. Até o momento, não existem nem metodologias oficiais e nem limites que considerem a realidade brasileira para a análise de pesticidas em plantas medicinais e medicamentos fitoterápicos em geral, e o método MSPD aqui descrito mostrou ser uma opção viável para a análise de fitoterápicos de Passiflora L. Abstract in english This paper proposes a method based on matrix solid phase dispersion (MSPD) to determine the presence of organochlorine (OC) and organophosphorus (OP) pesticide residues in species of Passiflora L. (passion fruit) leaves by gas chromatography, using an electron capture detector (HRGC-ECD). A comparis [...] on with conventional methods, mainly the European Pharmacopoeia method (EP), showed MSPD to be efficient, fast, simple and easy to perform. To date, there are no official methods or limits that take into account Brazil's "real life" conditions in the analysis of pesticides in medicinal plants and phytomedicines, and the MSPD method described herein has proved to be a feasible one for the analysis of Passiflora L-based phytomedicines.

  3. Determination of pesticide residues in cannabis smoke.

    Science.gov (United States)

    Sullivan, Nicholas; Elzinga, Sytze; Raber, Jeffrey C

    2013-01-01

    The present study was conducted in order to quantify to what extent cannabis consumers may be exposed to pesticide and other chemical residues through inhaled mainstream cannabis smoke. Three different smoking devices were evaluated in order to provide a generalized data set representative of pesticide exposures possible for medical cannabis users. Three different pesticides, bifenthrin, diazinon, and permethrin, along with the plant growth regulator paclobutrazol, which are readily available to cultivators in commercial products, were investigated in the experiment. Smoke generated from the smoking devices was condensed in tandem chilled gas traps and analyzed with gas chromatography-mass spectrometry (GC-MS). Recoveries of residues were as high as 69.5% depending on the device used and the component investigated, suggesting that the potential of pesticide and chemical residue exposures to cannabis users is substantial and may pose a significant toxicological threat in the absence of adequate regulatory frameworks. PMID:23737769

  4. Considerations on the Content of Pesticides Residues in Vegetables

    Directory of Open Access Journals (Sweden)

    Florica Morar

    2011-06-01

    Full Text Available Pesticide contamination of vegetables, today, is more and more questionable. Biodegradability and molecular recalcitrance are two properties expressing the capacity of used substances in plant treatments. Therefore, it is preferred the use of those pesticides that decompose from a treatment to another without accumulating thepollutant residues. It is recommended that, when choosing a pesticide which is used in treatments, to keep in mind: no effect dose, tolerable daily intake, tolerable amount of residues, residues’ limit, the maximum limit allowable, daily dose acceptable for the individual, level of tolerance, maximum limit of contamination allowed and themaximum daily intake acceptable for human. In the Laboratory of pesticide residues determination from plants and plant products in Târgu Mure?, pesticide residues were detected in some species of vegetables; methods of analysis used in the laboratory are multiresidual analysis methods developed in the laboratory (method GC x GC - TOF MS. To be mentioned that the pesticides detected values in vegetables have not exceeded the maximum permissible limits.

  5. Analysis of six organophosphorus pesticide residues in apples and pears using cloud-point extraction coupled with HPLC-UV.

    Science.gov (United States)

    Zhang, Lijin; Chen, Fang; Zhang, Wenhuan; Pan, Canping

    2014-01-01

    A cloud-point extraction (CPE) method with Triton X-114 has been developed for analysis of six organophosphorus pesticides (OPPs) in apples and pears. In this CPE procedure, the effects of the surfactant volume, mass of sodium chloride, equilibrium temperature, equilibrium time, and pH on the extraction procedure were investigated. Under the optimal CPE conditions, the analytes were enriched 20-fold and the LODs dropped to 0.44-5.20 microg/kg. Furthermore, the proposed extraction method was validated by the correlation coefficient (R2) of the calibration curve, repeatability (RSD, n = 6), and fortified recoveries, which were 0.9967-0.9993, 2.7-6.5, and 74.7-104.5%, respectively. Based on these results, it could be concluded that the proposed CPE method with Triton X-114 was suitable for the effective extraction and enrichment of OPP residues in the apple and pear samples. PMID:25145158

  6. Pesticide Instrumental Analysis

    International Nuclear Information System (INIS)

    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.

  7. Simultaneous multiresidue analysis of 41 pesticide residues in cooked foodstuff using QuEChERS: Comparison with classical method.

    Science.gov (United States)

    Park, Ji-Yeon; Choi, Jeong-Heui; Abd El-Aty, A M; Kim, Bo Mi; Oh, Jae-Ho; Do, Jung-Ah; Kwon, Ki Sung; Shim, Ki-Hoon; Choi, Ok-Ja; Shin, Sung Chul; Shim, Jae-Han

    2011-09-01

    The principal objective of this study was to develop a simple multiresidue method involving a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method for the identification and quantification of 41 pesticide residues in cooked foodstuffs including cooked potatoes, radishes, and rice using GC-?ECD. The analytes were subsequently confirmed via GC-MS. The results were then compared using the classical method established by the KFDA. The quantitation of individual pesticides was based on matrix-matched calibration curves with a correlation coefficient in excess of 0.993 for the 41 pesticides selected herein. Using QuEChERS, the mean recoveries ranged between 68.6 and 130.0% for the majority of the tested pesticides; however, the classical method exhibited low recoveries for dichlofluanid, tetraconazole, oxadixyl, fenbuconazloe, and paclobutrazol. After QuEChERS, the LODs and LOQs ranged between 0.004 and 0.3?g/kg and 0.0125 and 1.0?g/kg, respectively. The proposed method was applied successfully to determine the residue levels in cooked foodstuffs, and none of the samples contained detectable amounts of pesticide residues. PMID:25214356

  8. Análise de resíduos de pesticidas em tomates por cromatografia em camada delgada Analysis of residue pesticide in tomatoes by thin layer chromatography

    Directory of Open Access Journals (Sweden)

    Solange Leite Moraes

    2002-05-01

    Full Text Available Pesticide residues are determined by thin layer chromatography (TLC using the Hill reaction as a detection method. Tomatoes samples without pesticide were fortified with atrazine, diuron, chloroxuron and metribuzin, and were applyed in silica gel plates with the help of a microsyringe. The pesticides were elued with ethyl acetate. There was no need of cleaning up because no interference was noticed. After the revelation of the plates, the diameters of the spots were measure by using a rule. The range of the determined concentration for all the pesticides was from 0.1 to1.0 ng/muL. The results obtained through TLC can be used for semi-quantitative analysis.The results obtained were compared to gas and liquid chromatography, showing good agreement between both techniques.

  9. Análise de resíduos de pesticidas em tomates por cromatografia em camada delgada / Analysis of residue pesticide in tomatoes by thin layer chromatography

    Scientific Electronic Library Online (English)

    Solange Leite, Moraes; Maria Olímpia Oliveira, Rezende; Lia Emi, Nakagawa; Luiz Carlos, Luchini.

    2002-05-01

    Full Text Available SciELO Brazil | Language: Portuguese Abstract in portuguese [...] Abstract in english Pesticide residues are determined by thin layer chromatography (TLC) using the Hill reaction as a detection method. Tomatoes samples without pesticide were fortified with atrazine, diuron, chloroxuron and metribuzin, and were applyed in silica gel plates with the help of a microsyringe. The pesticid [...] es were elued with ethyl acetate. There was no need of cleaning up because no interference was noticed. After the revelation of the plates, the diameters of the spots were measure by using a rule. The range of the determined concentration for all the pesticides was from 0.1 to1.0 ng/muL. The results obtained through TLC can be used for semi-quantitative analysis.The results obtained were compared to gas and liquid chromatography, showing good agreement between both techniques.

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

    International Nuclear Information System (INIS)

    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 (?-HCH, ?-HCH, aldrin, heptachlor, ?-chlordane, heptachlor epoxide, ?-endosulfan, p,p'-DDE, endrin, ?-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 ?-HCH, ?-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 poidered 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)

  11. The 2011 European Union Report on Pesticide Residues in Food

    Directory of Open Access Journals (Sweden)

    European Food Safety Authority

    2014-05-01

    Full Text Available The report presents the results of the control activities related to pesticide residues in food carried out in 2011 in 29 European countries (27 Member States and 2 EFTA countries. The report also presents a dietary risk assessment. On the basis of the detailed analysis of the results, EFSA derived some recommendations aimed at improving the enforcement of the European pesticide residue legislation. In 2011, more than 79,000 samples of more than 600 food products were tested for pesticide residues throughout Europe. Nearly 900 pesticides were sought and less than 400 were detected in measurable amounts. In the framework of the EU-coordinated monitoring programme which covered more than 12,000 samples 98.1 % of the tested food samples analysed complied with the legal limits and that 53.4 % of samples contained no measurable residues at all. The dietary risk assessment that was performed to estimate the long-term exposure of consumers confirmed that there was no long-term risk to consumer health through their diets from 99 % of the 171 pesticides assessed. For two pesticides (dieldrin and heptachlor the estimated worst-case exposure exceeded the toxicological reference value, indicating there may be a potential for an impact on consumer health. Neither compound is authorised for use as a pesticide, but due to historical use and the high persistence of the molecules and their capacity to bioaccumulate, they are still present in the food chain. The risk assessment that focussed on the short-term exposure revealed that potential consumer health concerns could not be excluded in 253 instances should the products that contained residues in high concentrations be consumed in high amounts. Finally, an acute risk assessment was carried out for pears that contained multiple residues of pesticides that share the same toxicological effects. Two samples of pears exceeded the toxicological threshold for cumulative effects.

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

    Science.gov (United States)

    Oellig, Claudia; Schwack, Wolfgang

    2014-07-18

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

  13. Assessment of pesticide residues on selected vegetables of Pakistan

    International Nuclear Information System (INIS)

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

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

    OpenAIRE

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

    2003-01-01

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

  15. Practical aspects in gas chromatography-mass spectrometry for the analysis of pesticide residues in exotic fruits.

    Science.gov (United States)

    España Amórtegui, Julio César; Guerrero Dallos, Jairo Arturo

    2015-09-01

    The most relevant parameters of a multimode inlet were optimized to increase the injection volume up to 25?L using solvent vent mode in order to improve the sensitivity of the gas chromatography-mass spectrometry system. Consequently, the implementation of a concurrent backflushing was necessary to largely prevent the expected loss of performance derived from such matrix load out of a general-purpose extraction (EN-15622-QuEChERS). Additionally, four mixtures of compounds used as analyte protectants were tested using spiked physalis to enhance the quality of signals. The chosen mixture remarkably improved sensitivity and yield better peak shapes, significantly more than others also tested. The analysis of pesticide residues in exotic fruits using instruments of limited selectivity is challenging since these complex matrices usually give notably dirty extracts. This scheme included an instrumental optimization and the addition of selected compounds that enabled to selectively reach limits of quantitation of 0.01mgkg(-1) for most analytes. PMID:25842302

  16. Estimation of the uncertainties of extraction and clean-up steps in pesticide residue analysis of plant commodities.

    Science.gov (United States)

    Omeroglu, P Yolci; Ambrus, A; Boyacioglu, D

    2013-01-01

    Extraction and clean-up constitute important steps in pesticide residue analysis. For the correct interpretation of analytical results, uncertainties of extraction and clean-up steps should be taken into account when the combined uncertainty of the analytical result is estimated. In the scope of this study, uncertainties of extraction and clean-up steps were investigated by spiking (14)C-labelled chlorpyrifos to analytical portions of tomato, orange, apple, green bean, cucumber, jackfruit, papaya and starfruit. After each step, replicate measurements were carried out with a liquid scintillation counter. Uncertainties in extraction and clean-up steps were estimated separately for every matrix and method combination by using within-laboratory reproducibility standard deviation and were characterised with the CV of recoveries. It was observed that the uncertainty of the ethyl acetate extraction step varied between 0.8% and 5.9%. The relative standard uncertainty of the clean-up step with dispersive SPE used in the method known as QuEChERS was estimated to be around 1.5% for tomato, apple and green beans. The highest variation of 4.8% was observed in cucumber. The uncertainty of the clean-up step with gel permeation chromatography ranged between 5.3% and 13.1%, and it was relatively higher than that obtained with the dispersive SPE method. PMID:23216411

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

    International Nuclear Information System (INIS)

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

  18. 76 FR 36479 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2011-06-22

    ...make a final determination on this pesticide...regulations for residues of pesticides...regulations for residues of pesticides...part 180 for residues of the insecticide thiamethoxam...procedures and determination by liquid...

  19. 78 FR 79359 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2013-12-30

    ...40 CFR part 180 for residues of pesticide chemicals...EPA can make a final determination on these pesticide...of regulations for residues of pesticides in or...180 for the combined residues of the insecticide spinetoram,...

  20. 78 FR 56185 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2013-09-12

    ...40 CFR part 180 for residues of pesticide chemicals...EPA can make a final determination on these pesticide...of regulations for residues of pesticides in or...40 CFR part 180 for residues of the insecticide diflubenzuron,...

  1. Pesticide residue analysis of fruit juices by LC-MS/MS direct injection. One year pilot survey.

    Science.gov (United States)

    Ferrer, Carmen; Martínez-Bueno, M J; Lozano, Ana; Fernández-Alba, A R

    2011-02-15

    For this work, thirteen types of fruit juices (orange, pineapple, peach, apple, multifruit, mango, strawberry, tomato, pear, mandarin, grape, banana and grapefruit) were selected to develop an analytical method for the analysis of 53 pesticides by direct injection in LC-MS/MS. The preparation of the samples was very simple: an aliquot of the juice was centrifuged and it was ten-times diluted prior to analysis, which allowed reducing considerably the time and cost of the analyses. Besides, dilution of the samples permits reducing the amount of matrix going into the system, and thus, decreasing the matrix effects, so common in this type of commodities, opening the possibility to perform quantification with solvent based standards. Validation of the method was carried out in accordance with EU guidelines. Calibration curves covering three orders of magnitude were performed, and they were linear over the concentration range studied for all the matrices (from 0.1 to 100 ?g L(-1)). Practical limits of quantification were in the low ?g L(-1) range, far below the maximum residue levels (MRLs) of the EU regulations, which do not set specific MRLs for juices, and in this cases of processed food, MRLs of the raw product are applied. Repeatability of the instrumental method was studied in all matrices, obtaining good intra- and inter-day relative standard deviations (RSDs). The proposed method was applied to 106 real fruit juice samples purchased in different local markets during a one-year survey in order to validate the suitability for routine analysis. 43% of the analysed samples gave positive results (higher than the practical limits of quantification). PMID:21238751

  2. Microflow liquid chromatography coupled to mass spectrometry--an approach to significantly increase sensitivity, decrease matrix effects, and reduce organic solvent usage in pesticide residue analysis.

    Science.gov (United States)

    Uclés Moreno, Ana; Herrera López, Sonia; Reichert, Barbara; Lozano Fernández, Ana; Hernando Guil, María Dolores; Fernández-Alba, Amadeo Rodríguez

    2015-01-20

    This manuscript reports a new pesticide residue analysis method employing a microflow-liquid chromatography system coupled to a triple quadrupole mass spectrometer (microflow-LC-ESI-QqQ-MS). This uses an electrospray ionization source with a narrow tip emitter to generate smaller droplets. A validation study was undertaken to establish performance characteristics for this new approach on 90 pesticide residues, including their degradation products, in three commodities (tomato, pepper, and orange). The significant benefits of the microflow-LC-MS/MS-based method were a high sensitivity gain and a notable reduction in matrix effects delivered by a dilution of the sample (up to 30-fold); this is as a result of competition reduction between the matrix compounds and analytes for charge during ionization. Overall robustness and a capability to withstand long analytical runs using the microflow-LC-MS system have been demonstrated (for 100 consecutive injections without any maintenance being required). Quality controls based on the results of internal standards added at the samples' extraction, dilution, and injection steps were also satisfactory. The LOQ values were mostly 5 ?g kg(-1) for almost all pesticide residues. Other benefits were a substantial reduction in solvent usage and waste disposal as well as a decrease in the run-time. The method was successfully applied in the routine analysis of 50 fruit and vegetable samples labeled as organically produced. PMID:25495653

  3. Streamlined pretreatment and GC-FPD analysis of multi-pesticide residues in perennial Morinda roots: a tropical or subtropical plant.

    Science.gov (United States)

    Liu, Hongmei; Kong, Weijun; Qi, Yun; Gong, Bao; Miao, Qing; Wei, Jianhe; Yang, Meihua

    2014-01-01

    In this study, a simple and rapid multi-pesticide residues analytical method has been developed and evaluated for simultaneous identification and quantification of 30 organophosphorus pesticides (OPPs) present at trace levels in perennial Morinda roots. Samples were firstly extracted and cleaned up with a streamlined method (modified QuEChERS), and then detected by gas chromatography with flame photometric detector (GC-FPD). For accurate quantification, representative matrix-matched calibration curves were applied to compensate matrix effects. Reasonable linearity was found in the concentration ranges of 0.04 and 1.28 ?g mL(-1), with correlation coefficients r better than 0.9921 (0.9921-0.9998). The limits of detection (LODs) were between 0.005 and 0.02 ?g mL(-1) for all investigated pesticides, while the limits of quantification (LOQs) were in the range of 0.01-0.04 ?g mL(-1), below the regulatory maximum residue limits (MRL) suggested. Acceptable quantitative recoveries of 75.01-118.89% (96.0% on average) were achieved with relative standard deviations (RSD) varying from 0.89% to 9.80% (5.39% on average) at three different concentration levels of 0.05, 0.1 and 1.0 mg kg(-1). Out of all 40 batches of real samples, only fenitrothion was found in two samples, which was successfully confirmed by GC-MS. Based on these results, this analytical method has been proven to be fast, robust, accurate, selective, sensitive and easy to operate in the analysis of multiple pesticide residues in Morinda roots. Meanwhile, it also draws attention to the need of pesticide monitoring programs in local soils. PMID:24007616

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

    Science.gov (United States)

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

    2008-01-01

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

  5. Pesticides.

    Science.gov (United States)

    Sherma, Joseph

    1989-01-01

    This review is devoted to methods for the determination of residues of pesticides and some related industrial chemicals. Topics include: residue methods, sampling, chromatography, organochlorine pesticides, organophosphorus pesticides, carbamate insecticides, herbicides, fungicides, pyrethrins, fumigants, and related chemicals. (MVL)

  6. Persistent organochlorine pesticide residues in animal feed.

    Science.gov (United States)

    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 ?-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

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

    Science.gov (United States)

    Kwon, Hyeyoung; Lehotay, Steven J; Geis-Asteggiante, Lucía

    2012-12-28

    Gas and liquid chromatography (GC and LC) coupled to mass spectrometry (MS) serve as the most powerful analytical tools commonly used to monitor pesticide residues in food, among other applications. However, both GC-MS and LC-MS are susceptible to matrix effects which can adversely affect quantification depending on the analyte, matrix, sample preparation, instrumentation, and operating conditions. Among the approaches that reduce matrix effects, the most common in pesticide residue applications is matrix-matched calibration because it is relatively inexpensive and simple. Also, it has been shown to work well during method validation when fortified samples are exactly matched with samples used for calibration. However, the quality of matrix-matched results in real-world analyses depends on the consistency of matrix effects among diverse samples. In this study, the variability of matrix effects was measured for 38 representative pesticides in 20 samples each (including different varieties) of rice, orange, apple, and spinach extracted using the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) method for analysis by LC-MS/MS and low-pressure GC-MS. Using LC-MS/MS, only oranges gave >20% matrix effects for a few pesticides. GC-MS exhibited larger matrix effects, but as in LC-MS/MS, the differences were reasonably consistent among the 20 samples tested. Main conclusions of this study are that for the conditions utilized: (1) matrix-matching was not needed for most pesticides in the simpler food matrices; and (2) for the more complex orange matrix, acceptably accurate quantitative results were achieved by using matrix-matching even with a different sample of the same type. However, full confidence cannot be extended to matrix-matched results, and for consequential applications such as regulatory enforcement, confirmatory analyses using alternate quantitative determinations should also be conducted. PMID:23182936

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

    OpenAIRE

    Rada ?urovi?; Jelena Milinovi?; Mirjana Markovi?; Dragan Markovi?

    2007-01-01

    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 differe...

  9. Organophosphate and Carbamate Pesticide Residues in Beans from Markets in Lagos State, Nigeria

    Directory of Open Access Journals (Sweden)

    Ogah C.O

    2011-03-01

    Full Text Available Foods treated with pesticides for protection against destructive pests often contain residues of these chemicals. The levels of pesticide residues in food are often determined as a means of assessing appropriate use as well as the level of human exposure to these chemicals and hence their potential human health hazards. The aim of this study was to determine the concentration of organophosphate and carbamate pesticides in beans samples collected from markets in Lagos State and compare these values with established safety values. Beans (Phaseolus vulgaris L. samples purchased from different markets in Lagos State were analyzed for residues of organophosphate and carbamate pesticides. Analysis was done using gas chromatograph with mass spectrometric detector (GC-MS after careful extraction and cleanup. It was found that all the beans samples contained residues of one or more organophosphate or carbamate pesticides. Mean concentrations ranged from 19.4 to 455.9 ?g/kg. Maximum residue limits (MRL of the various pesticides (except for parathion were exceeded in up to 10% of samples. The estimated total diet intake (ETDI for dichlorvos exceeded its maximum permissible intake (MPI by 131%. Organophosphate and carbamate pesticide residues are present in beans sold in Lagos markets and maximum residue limits for most of the pesticides are exceeded. There is therefore a need for more stringent monitoring of importation and use of these pesticides in agriculture and food storage in Nigeria.

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

    International Nuclear Information System (INIS)

    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.

  11. Análise de resíduos de pesticidas em tomates por cromatografia em camada delgada Analysis of residue pesticide in tomatoes by thin layer chromatography

    OpenAIRE

    Solange Leite de Moraes; Maria Olímpia Oliveira Rezende; Lia Emi Nakagawa; Luiz Carlos Luchini

    2002-01-01

    Pesticide residues are determined by thin layer chromatography (TLC) using the Hill reaction as a detection method. Tomatoes samples without pesticide were fortified with atrazine, diuron, chloroxuron and metribuzin, and were applyed in silica gel plates with the help of a microsyringe. The pesticides were elued with ethyl acetate. There was no need of cleaning up because no interference was noticed. After the revelation of the plates, the diameters of the spots were measure by using a rule. ...

  12. Determination of Pesticide Residues in Fresh and Greenhouse Vegetables

    Directory of Open Access Journals (Sweden)

    M.H. Azizi

    2008-04-01

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

  13. Types of pesticides and determination of their residues

    International Nuclear Information System (INIS)

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

  14. Pesticide Residues Evaluation in Pulp, Juice and Nectar of Fruits

    OpenAIRE

    Claudia Helena Pastor Ciscato; Amir Bertoni Gebara; Claudia Maria Barbosa; Gisele Santos Souza; Hamada, N.; Silva, D. L.

    2012-01-01

    Industrial processing of fruit in order to produce juice and nectar can contribute to over exposure of some contaminants, such as pesticide residues. Thus, this work aimed to check the compliance with the Maximum Residue Levels (MRL). In our research, 162 samples of frozen pulps, 16 of juice and 2 of nectar, were evaluated for pesticide residues, as well as the acceptable dietary intake (ADI). A multi-residue method was employed and almost 140 active ingredients were studied. Positive results...

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

    DEFF Research Database (Denmark)

    Rasmussen, Rie Romme; Poulsen, Mette Erecius

    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 significantly reduced five of the pesticide residues: diazinon, chlorpyrifos, fenitrothion, kresoxim-methyl and tolylfluanid, by 25-69%. Residues of the metabolite endosulfan sulfate were increased by 34% during storage. Boiling significantly reduced residues of fenitrothion and tolylfluanid by 32 and 81%, respectively. Only a few of the observed effects of processing could be explained by the physical or chemical characteristics of the pesticides. No differences in effect of processing due to apple variety were identified.

  16. 76 FR 49396 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2011-08-10

    ...make a final determination on this pesticide...regulations for residues of pesticides...part 180 for residues of the insecticide metaflumizone...to determine residues of metaflumizone...The final determination of...

  17. 75 FR 11171 - Notice of Filing of Several Pesticide Petitions for Residues of Pesticide Chemicals in or on...

    Science.gov (United States)

    2010-03-10

    ...can make a final determination on these pesticide...regulations for residues of pesticides in...a tolerance for residues of the insecticide, Paecilomyces...a tolerance for residues of the insecticide,...

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

    Energy Technology Data Exchange (ETDEWEB)

    Neves Bettencourt da Silva, Ricardo Jorge, E-mail: rjsilva@fc.ul.pt [CCMM-DQB, Faculty of Sciences, University of Lisbon, Campo Grande, 1749-016 Lisbon (Portugal); Gomes Ferreira Crujo Camoes, Maria Filomena [CCMM-DQB, Faculty of Sciences, University of Lisbon, Campo Grande, 1749-016 Lisbon (Portugal)

    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.

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

    International Nuclear Information System (INIS)

    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 ca 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.

  20. Planar solid phase extraction--a new clean-up concept in multi-residue analysis of pesticides by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Oellig, Claudia; Schwack, Wolfgang

    2011-09-16

    Efficient clean-up is indispensable for preventing matrix effects in multi-residue analysis of pesticides in food by liquid and gas chromatography coupled to mass spectrometry. As a completely new approach, highly automated planar chromatographic tools were applied for powerful clean-up, called high-throughput planar solid phase extraction (HTpSPE). Thin-layer chromatography (TLC) was used to completely separate pesticides from matrix compounds and to focus them into a sharp zone, followed by extraction of the target zone by the TLC-MS interface. HTpSPE resulted in extracts nearly free of interference and free of matrix effects, as shown for seven chemically representative pesticides in four different matrices (apples, cucumbers, red grapes, tomatoes). Regarding the clean-up step, quantification by LC-MS provided mean recovery (against solvent standards) of 90-104% with relative standard deviations of 0.3-4.1% (n=5) for two spiking levels of 0.1 and 0.5 mg/kg. Clean-up of one sample was completed in a manner of minutes, while running numerous samples in parallel at reduced costs, with very low sample and solvent volumes. PMID:21794869

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

    Science.gov (United States)

    Sanchez-Bayo, Francisco; Goka, Koichi

    2014-01-01

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

  2. Evaluation of the Potential of GC-APCI-MS for the Analysis of Pesticide Residues in Fatty Matrices

    Science.gov (United States)

    Gómez-Pérez, María Luz; Plaza-Bolaños, Patricia; Romero-González, Roberto; Martínez Vidal, José Luis; Garrido Frenich, Antonia

    2014-05-01

    A method based on gas chromatography-atmospheric pressure chemical ionization-mass spectrometry (GC-APCI-MS) has been developed for the analysis of pesticides in meat by using quadrupole-time of flight mass spectrometry (QTOF-MS). Ionization and MS conditions were studied for 71 compounds, although only 51 showed acceptable performance. The protonated form of the analytes was mainly found ([M + H]+), although some compounds generated the molecular ion (M+•). A fast and generic extraction procedure was applied in sample pretreatment. The analytical method was suitable for qualitative analysis, and it was also evaluated for quantitative analysis, obtaining adequate recovery and precision values for most of the studied analytes at two concentration levels (50 and 150 ?g/kg). Several operational drawbacks were found with this instrument, such as slow stabilization and moderate sensitivity, although the fast switching between LC and GC allows the increase of its applicability.

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

    Science.gov (United States)

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

    2004-04-01

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

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

    Science.gov (United States)

    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 ?g 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 ?g kg(-1), the target method LOQ. For the spike concentrations of 20 and 50 ?g kg(-1), the recoveries and RSDs were even better. The validated LOQ(m) was 10, 20 and 50 ?g kg(-1) for respectively 33, 3 and 6 of the analytes studied. For five compounds, the European Union method performance requirements for the validation of a quantitative method (average recoveries between 70-120% and repeatability RSD ? 20%) were not achieved and 4 problematic pesticides (captan, captafol, folpet and dicofol) could not be detected as their parent compound, but only via their degradation products. Although the matrix effect (matrix-enhanced detector response) was high for all pesticides studied, the matrix interference was minimal, due to the high selectivity obtained with the GC-NCI-MS detection. Matrix-matched calibration for applying the method in routine analysis is recommended for reliable quantitative results. PMID:22771261

  5. Determination of pesticide residues in cereal grains

    International Nuclear Information System (INIS)

    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)

  6. Organochlorine pesticide (OCP) residues in mountain soils from Tajikistan.

    Science.gov (United States)

    Zhao, Zhonghua; Zeng, Haiao; Wu, Jinglu; Zhang, Lu

    2013-03-01

    The concentrations and spatial distribution of organochlorine pesticides (OCPs) in surface soils of different altitudes (570–4656 m) from Tajikistan were determined. OCPs were detected in all samples with concentrations in the range 52.83–247.98 ng g(-1) dry weight (ng g(-1) dw). Aldrins were the most predominant compounds followed by chlordanes, hexachlorocyclohexanes (HCHs) and endosulfans, while dichlorodiphenyltrichloroethanes (DDTs) and methoxychlor were detected at much lower concentrations. Composition analysis indicated that OCPs mainly came from the atmospheric transport of historically used pesticides. OCP residues in the west and northwest parts of Tajikistan were higher than the east and the southeast due to the proximity to the potential sources and anthropogenic activity intensities around. Additionally, correlation analysis between OCPs and altitudes indicated that the more volatile pollutants, such as HCH isomers, seemed to become enriched more easily in regions with higher altitudes relative to the less volatile ones, such as DDTs. PMID:23738359

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

    Science.gov (United States)

    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

  8. Multiresidue method for the analysis of more than 140 pesticide residues in fruits and vegetables by gas chromatography coupled to triple quadrupole mass spectrometry.

    Science.gov (United States)

    Fernández Moreno, José Luis; Garrido Frenich, A; Plaza Bolaños, Patricia; Martínez Vidal, José Luis

    2008-09-01

    A new multiresidue method has been developed and validated for the determination of more than 140 pesticide residues in cucumber and orange by gas chromatography coupled to triple quadrupole mass spectrometry (GC-QqQ-MS/MS) in a single run of 25.50 min. The triple quadrupole (QqQ) analyzer simultaneously operated in the selected reaction monitoring (SRM) and selected ion monitoring (SIM) modes, acquiring two or three transitions per compound. Samples were extracted by the application of a single-phase extraction of 10 g of sample with acetonitrile containing 1% of acetic acid, followed by a liquid-liquid partition formed by the addition of 4 g of MgSO(4) and 1 g of NaOAc. A dispersive solid-phase extraction (D-SPE) with primary secondary amine (PSA) was applied to clean up the extracts. A final concentration step was included in order to increase sensitivity in the instrumental analysis. The method was properly validated in each matrix in a wide dynamic range (10-400 microg kg(-1)): this work relies on a new quantification strategy by the use of two calibration curves to increase the dynamic range, which permitted reduction of sample dilutions and increase in sample throughput. Recovery was studied at three concentration levels (11.5, 50.0, and 150.0 microg kg(-1)), yielding values in the range 70-110% with precision values, expressed as relative standard deviation (RSD), lower than 20 and 25% for the intraday and interday precision, respectively. Limits of quantification (LOQs) were established at 10 microg kg(-1), the lowest maximum residue level (MRL) value set by the European Union in vegetables. The method was successfully applied to the analysis of pesticide residues in real samples from the southeastern Spain. PMID:18383275

  9. Rapid detection of pesticide residue in apple based on Raman spectroscopy

    Science.gov (United States)

    Li, Yongyu; Sun, Yunyun; Peng, Yankun; Dhakal, Sagar; Chao, Kuanglin; Liu, Qiaoqiao

    2012-05-01

    The potential of Raman spectroscopy in the analysis of low concentration organic contaminants on apples' surface was evidenced in this study. Chlorpyrifos, an organophosphorus pesticide, was used as a probe for this purpose. The characteristic peaks of fingerprints of pesticide on an aluminum substrate and apple fruit cuticle without pesticide residue were acquired first. Then a concentration range of chlorpyrifos (commercial products at 40%) solutions were made using deionised and distilled water. Single 100 ?L droplets of the chlorpyrifos solutions were placed gently on apple fruit cuticles and left to dry before analysis. Through comparative analysis of the Raman spectra data collected, 341, 632 and 1237cm-1 were identified to detect the chlorpyrifos pesticide residue on apple surface. Based on the relationship between the Raman intensity of the most prominent peak at around 632cm-1 and the pesticide concentrations, the limit of detection of ordinary Raman spectrum for chlorpyrifos was estimated to be 48ppm.

  10. Evaluation of the QuEChERS Method and Gas Chromatography–Mass Spectrometry for the Analysis Pesticide Residues in Water and Sediment

    OpenAIRE

    Brondi, S. H. G.; Macedo, A. N.; Vicente, G. H. L.; Nogueira, A. R. A.

    2010-01-01

    A method for the determination of pesticide residues in water and sediment was developed using the QuEChERS method followed by gas chromatography – mass spectrometry. The method was validated in terms of accuracy, specificity, linearity, detection and quantification limits. The recovery percentages obtained for the pesticides in water at different concentrations ranged from 63 to 116%, with relative standard deviations below 12%. The corresponding results from the sediment ranged from 48 to...

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

    International Nuclear Information System (INIS)

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

  12. Public Health Implications of Pesticide Residues in Meat

    Directory of Open Access Journals (Sweden)

    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

  13. [Occurrence of pesticide residues in raspberries in 2000-2005].

    Science.gov (United States)

    Sad?o, Stanis?aw; Szpyrka, Ewa; Rogozi?ska, Krystyna; Rupar, Julian; Ku?menko, Arletta

    2007-01-01

    The aim of this paper was to present occurrence of pesticide residues in raspberries in 2000-2005. Gas chromatographic and spectroscopy methods were used. The most frequently found were tolylfluanid residues (43% of the analysed samples), procymidone residues (33%), pyrimethanil residues (15%), ethylenebisdithiocarbamates (EBDC) residues (8%) and iprodione residues (5%), while insecticides (mainly synthetic pyrethroids) cypermethrin residues (6%) and bifenthrin (4%). In 8 % of analysed samples EBDC residues exceeded the national Maximum Residue Level established for raspberries. On relatively the highest level EBDC occurred. PMID:18246655

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

    Science.gov (United States)

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

  15. Rapid analysis of multiple pesticide residues in fruit-based baby food using programmed temperature vaporiser injection–low pressure gas chromatography–high-resolution time-of-flight mass spectrometry

    Science.gov (United States)

    A rapid method using programmed temperature vaporizer injection–low-pressure gas chromatography–high-resolution time-of-flight mass spectrometry (PTV–LP-GC–HRTOFMS) for the analysis of multiple pesticide residues in fruit-based baby food was developed. The fast and inexpensive buffered QuEChERS ext...

  16. Monitoring of pesticide residues on cucumber, tomatoes and strawberries in Gaza Governorates, Palestine.

    Science.gov (United States)

    Safi, J M; Abou-Foul, N S; el-Nahhal, Y Z; el-Sebae, A H

    2002-02-01

    Three techniques of gas chromatography (GC) either with flame photometric-detector (FPD), electron capture detector (ECD), or with mass-spectrometry (MS) were applied for identification and quantification of pesticide residues on 45 samples of cucumber, tomatoes, and strawberries in fifteen locations in Gaza Governorates. GC-FPD analysis showed the presence of four different organo-phosphorus (OP) pesticides, their levels were very low and below maximum residue limits (MRL's). GC-ECD detected ten different pesticides at levels below the MRL's. Using the GC-MS technique, alpha and beta-endosulfan, chlorpyrifos, carbofuran, chlorfluazuron, triadimenol I and II, penconazole, coptafolmetabolite, pyrimethanil and iprodione were detected and confirmed on some samples of cucumber, tomatoes and strawberries. All GC-MS pesticide residues detected on tomato were below the MRL's except chlorfluazuron while on strawberry were below the MRL's except penconazole, chlorfluazuron and pyrimethanil, but on cucumber were slightly higher than the MRL's except alpha and beta-endosulfan. Also, statistical analysis of pesticide residues in all samples showed that most of the detected residues mean were significantly lower than the MRL's (p < 0.05). Generally, tomatoes showed the least number and level of pesticide residues by all the GC-techniques. On the other hand, strawberries showed greater number and levels of pesticide residues, particularly by the GC-MS technique. These results indicate that the protective period to elapse before harvesting should be increased especially on strawberry. The results also can help in risk assessment of consumers exposure to the expected pesticide residues. PMID:11890053

  17. Use of activated charcoal in a solid-phase extraction technique for analysis of pesticide residues in tomatoes

    OpenAIRE

    Kaipper Beatriz I. A.; Madureira Luiz A. S.; Corseuil Henry X.

    2001-01-01

    The present work describes extraction and purification methods that were developed to determine and to monitor the content of organophosphorus pesticides in tomato crops from the agricultural district of Florianópolis, Brazil. SPE technique with activated charcoal was used for purification and recovery of the pesticides methamidophos, acephate, malation and methyl parathion. The solvents used for sample extraction and elution were chosen after several comparative tests. Best results were ach...

  18. Characteristics and alteration of pesticide residues in surface soils of agricultural fields and public parks

    Science.gov (United States)

    Al-Mutlaq, Khalid F.

    2006-12-01

    Organic contents of agricultural soils are major sources of organic compounds and pesticides into atmosphere. Therefore, surface soil samples from different locations in the city of Corvallis, USA were collected over a course of 1 year (2004/2005). The samples were subject to chemical extraction and analysis by gas chromatography-mass spectrometry (GC-MS). The results of the chemical analysis showed pesticide residues were present in soils and varied seasonally. For example, the highest total relative concentration of pesticide residues in Canola field was 0.16% in January 2005, and was 0.56% in Wheat Field in August 2005, and was 0.14% in the River Front Park in December 2004 and was 0.33 in Rose Garden. Sometimes in the year, these pesticide residues were not detected in the same sites.

  19. Application of magnetic nanoparticles to residue analysis of organochlorine pesticides in water samples by GC/MS.

    Science.gov (United States)

    Ozcan, Senar; Tor, Ali; Aydin, Mehmet Emin

    2012-01-01

    This paper describes a novel magnetic-SPE method for the determination of organochlorine pesticides (OCPs) in environmental water samples by use of Fe3O4-magnetic nanoparticles (MNPs) coated with oleic acid followed by GC/MS. The chemisorption of oleic acid onto Fe3O4-MNPs provides reusability of the developed sorbent materials several times. The effects of different parameters such as pH, desorption solvent, contact time, temperature, ionic strength, and sorbent dosage on the efficiency of magnetic-SPE were investigated. The optimized SPE method involved shaking 50 mL of water sample (pH 4) with 50 mg oleic acid coated Fe3O4(-) MNPs for 1 h, isolating the sorbent with an Nd-Fe-B magnet, and eluting the OCPs with methanol. An ionic strength of 0.1 M and temperature of 15 degrees C provided the maximum extraction efficiency. The LOQs were in the range of 0.006 to 0.048 microg/L. For three fortification levels, recoveries were in the range of 44-108%, with RSD <5%. The developed SPE method was successfully applied to real water samples, and it is viable, rapid, and easy to use for analysis of OCPs in water samples. PMID:23175964

  20. 78 FR 6274 - Withdrawal of Pesticide Petitions for Residues of Pesticide Chemicals in or on Various Commodities

    Science.gov (United States)

    2013-01-30

    ...Petitions for Residues of Pesticide Chemicals in or on Various Commodities...regulations for residues of pesticide chemicals in or on various commodities...petition summary. You may also reach each contact person by mail...180 for residues of pesticide chemicals in or on various food...

  1. 76 FR 20667 - Notice of Withdrawal of Pesticide Petitions for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2011-04-13

    ...Petitions for Residues of Pesticide Chemicals in or on Various Commodities...regulations for residues of pesticide chemicals in or on various commodities...petition summary. You may also reach each contact person by mail...180 for residues of pesticide chemicals in or on various food...

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

    DEFF Research Database (Denmark)

    Poulsen, Mette Erecius; Christensen, Hanne Bjerre

    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 the extraction procedure and consequently the assigned values were calculated based on part of the results. Acceptable z-scores were obtained by 56-97% of the participants.

  3. Ultrahigh-performance liquid chromatography electrospray ionization Q-Orbitrap mass spectrometry for the analysis of 451 pesticide residues in fruits and vegetables: method development and validation.

    Science.gov (United States)

    Wang, Jian; Chow, Willis; Chang, James; Wong, Jon W

    2014-10-22

    This paper presents an application of ultrahigh-performance liquid chromatography electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry (UHPLC/ESI Q-Orbitrap MS) for the determination of 451 pesticide residues in fruits and vegetables. Pesticides were extracted from samples using the QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure. UHPLC/ESI Q-Orbitrap MS in full MS scan mode acquired full MS data for quantification, and UHPLC/ESI Q-Orbitrap Full MS/dd-MS(2) (i.e., data-dependent scan mode) obtained product ion spectra for identification. UHPLC/ESI Q-Orbitrap MS quantification was achieved using matrix-matched standard calibration curves along with the use of isotopically labeled standards or a chemical analogue as internal standards to achieve optimal method accuracy. The method performance characteristics include overall recovery, intermediate precision, and measurement uncertainty evaluated according to a nested experimental design. For the 10 matrices studied, 94.5% of the pesticides in fruits and 90.7% in vegetables had recoveries between 81 and 110%; 99.3% of the pesticides in fruits and 99.1% of the pesticides in vegetables had an intermediate precision of ?20%; and 97.8% of the pesticides in fruits and 96.4% of the pesticides in vegetables showed measurement uncertainty of ?50%. Overall, the UHPLC/ESI Q-Orbitrap MS demonstrated acceptable performance for the quantification of pesticide residues in fruits and vegetables. The UHPLC/ESI Q-Orbitrap Full MS/dd-MS(2) along with library matching showed great potential for identification and is being investigated further for routine practice. PMID:25265038

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

    Science.gov (United States)

    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

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

    Science.gov (United States)

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

  6. 77 FR 66781 - Notice of Filing of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2012-11-07

    ...make a final determination on these...regulations for residues of pesticides...residues of the insecticide chlorantraniliprole...part 180 for residues of the herbicide...available for the determination of linuron...628 for residues of the insecticide...

  7. [Evaluation of QuEchERS methods for the analysis of 66 organophosphorus pesticide residues in vegetables by liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Wang, Lianzhu; Zhou, Yu; Chen, Yong; Wang, Ruilong; Lin, Zixu; Lin, Dejuan; Zheng, Shaohui

    2012-02-01

    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 microg/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 > or = 10) were 0.1 - 8 microg/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. PMID:22679828

  8. Dissipation behavior of organophosphorus pesticides during the cabbage pickling process: residue changes with salt and vinegar content of pickling solution.

    Science.gov (United States)

    Lu, Yuele; Yang, Zhonghua; Shen, Luyao; Liu, Zhenmin; Zhou, Zhiqiang; Diao, Jinling

    2013-03-01

    In this experiment, the behavior of 10 pesticides in three different cabbage pickling treatments has been studied. The brine used for pickling was made up with different salt and vinegar contents to determine the influence of different pickling solutions on pesticide dissipation and distribution. A modified QuECHERS and SPE method was established for the analysis of the pesticides in the cabbage and brine. It was found that different pesticides showed different dissipation patterns and finally represented dissimilar residue levels in the cabbage and brine. Statistical analysis was performed to compare the distinctions of these pesticides between each treatment and proved that salt content and pH value had certain influence on the dissipation and distribution of these pesticides during the pickling process. The data from this experiment would help to control pesticide residues in pickled cabbage and prevent potential risk to human health and environmental safety. PMID:23402557

  9. Pesticide residues in artichokes: effect of different head shape.

    Science.gov (United States)

    Cabras, P; Angioni, A; Garau, V L; Melis, M; Pirisi, F M; Cabitza, F; Cubeddu, M; Minelli, E

    1996-11-01

    Residues of three pesticides (dimethoate, parathion, and pyrazophos) in two artichoke cultivars, Masedu and Spinoso sardo, were investigated. The amount of pesticides in artichokes was greatly affected by the head shape. In the case of the calix-shaped Masedu artichoke, the residues in whole heads at commercial ripening were on average about twice higher than those of the pagoda-shaped Spinoso sardo artichoke. In the heart this ratio was 4 to 42 times greater. Residue decay rates were very fast, mainly owing to the dilution effect due to head growth. PMID:8896357

  10. Extraction of pesticide residues from biological and environmental samples

    International Nuclear Information System (INIS)

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

  11. An optical instrument to test pesticide residues in agricultural products

    Science.gov (United States)

    Qiu, Zhengjun; Zheng, Wenzhong; Fang, Hui; He, Yong

    2005-10-01

    Pesticide is one of the indispensability materials in modern agricultural management, however the excessive use of pesticides has threatened the ecological environment and people's health. This paper introduced an optical instrument to test the pesticide residues in agricultural products based on the inhibition rate of organophosphates against acrtyl-cholinesterase (AchE). The instrument consists mainly of a solid light source with 410nm wavelength, a sampling container, an optical sensor, a temperature sensor, and a MCU based data acquisition board. The light illuminated through the liquid in the sampling container, and the absorptivity was determined by the amount of the pesticide residues in the liquid. This paper involves the design of optical testing system, the data acquisition and calibration of the optical sensor, the design of microcontroller-based electrical board. Tests were done to reveal the affection of temperature and reacting time on AchE, to establish the relationship between the amount of methamidophos and dichlorvos with AchE. The results showed that the absorption rate was related to the pesticide residues and it could be concluded that the pesticide residues exceeded the normal level when the inhibition rate was over 50 percent. The instrument has potential application in vegetable markets.

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

    International Nuclear Information System (INIS)

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

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

    DEFF Research Database (Denmark)

    Poulsen, Mette Erecius; Naef, A.

    2009-01-01

    Seven pesticide application strategies were investigated to control apple scab (Venturia inaequalis) and powdery mildew (Podosphaera leucotricha) and, at the same time.. fulfil the new quality standards implemented by some German retailers. These demand that pesticide residues should be below 80% of European Maximum Residue Levels (EU MRL) and that the number of residues present at levels above 0.01 mg kg(-1) should be limited to a maximum of four. The strategies fulfilled the requirement to use combinations of different active substances in order to prevent the emergence of resistance to pesticides. The trials were conducted at two sites in Switzerland, in 2007, and all strategies and applications were in accordance with actual practice. Four replicates of apple samples from each strategy were then analysed for pesticide residues. The incidence of infection with apple scab and powdery mildew were monitored during the season in order to evaluate the efficacy of the different strategies. The efficacies of the different strategies against apple scab and powdery mildew were between 84% and 100% successful. In general, the level of pesticide residues found correlated with application rate and time, and no measured residue level exceeded the EU-MRL. The numbers of residues present at > 0.01 mg kg(-1) were between two and five.

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

    Directory of Open Access Journals (Sweden)

    Neff Roni A

    2012-01-01

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

  15. Use of activated charcoal in a solid-phase extraction technique for analysis of pesticide residues in tomatoes

    Directory of Open Access Journals (Sweden)

    Kaipper Beatriz I. A.

    2001-01-01

    Full Text Available The present work describes extraction and purification methods that were developed to determine and to monitor the content of organophosphorus pesticides in tomato crops from the agricultural district of Florianópolis, Brazil. SPE technique with activated charcoal was used for purification and recovery of the pesticides methamidophos, acephate, malation and methyl parathion. The solvents used for sample extraction and elution were chosen after several comparative tests. Best results were achieved using ethyl acetate for extraction and dichloromethane - ethyl acetate (7:3 for elution. Average recoveries from the matrices fortified with 0.20 to 0.60 mug g-1 ranged from 85.2 to 100 % with overall coefficients of variation of 1.3 to 6.3 %. The limits of detection of the method varied between 0.04 and 0.12 ng g-1. Activated charcoal demonstrated to be efficient for tomato matrix purification and for quantitative recovery of the analytes.

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

    Science.gov (United States)

    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

  17. Development and validation of a multiresidue method for the analysis of 151 pesticide residues in strawberry by gas chromatography coupled to a triple quadrupole mass analyzer.

    Science.gov (United States)

    Bolaños, Patricia Plaza; Moreno, José Luis Fernández; Shtereva, Deyana D; Frenich, Antonia Garrido; Vidal, José Luis Martínez

    2007-01-01

    A new method was developed and validated for the simultaneous determination of 151 pesticide residues in strawberry by gas chromatography coupled to a triple quadrupole mass analyzer (GC/QqQ-MS/MS), mainly using the selected reaction monitoring (SRM) mode. The list of target compounds included various classes of pesticides such as organochlorine (OCPs), organophosphorus (OPPs), carbamates, pyrethroids, triazoles and dicarboximides. A single extraction of 10 g of sample with acetonitrile followed by liquid-liquid partition formed by the addition of 4 g of MgSO4 and 1 g of NaCl was applied in sample preparation. Cleanup of the extracts was carried out by applying dispersive solid-phase extraction (D-SPE) with primary secondary amine (PSA). The analysis time was 21 min. The method was subjected to a thorough validation procedure. The recovery data were obtained by spiking blank samples at two concentration levels (11.5 and 50 microg/kg), yielding recoveries in the range 70-110%. Precision values expressed as relative standard deviation (RSD) were lower than 18% and 22% for the intraday and interday precision, respectively. Linearity was studied in the range 10-200 microg/kg and determination coefficients (R(2)) were higher than 0.98% for all compounds. Limits of detection (LODs) and limits of quantification (LOQs) were established as 4 and 10 microg/kg, respectively. The overall uncertainty of the method was estimated at two different concentrations (11.5 and 50 microg/kg), being lower than 25% in both cases. According to the validation data and performance characteristics as well as the high sample throughput and low cost, the proposed method is suitable for routine application. PMID:17577875

  18. The Organochlorine Pesticides Residue Levels in Karun River Water

    OpenAIRE

    Behrooz Jannat; Abdolazim Behfar; Zahra Nazari; Mohammad Hassan Rabiee; Gholamreza Raeesi; Mohammad Reza Oveisi; Nafiseh Sadeghi

    2013-01-01

    Background: The organochlorine pesticides (OCPs) are among the most commonly used in water streams around the world. Most of these contaminants are highly hydrophobic and persist in sediments of rivers and lakes. Studies have suggested that OCPs may affect the normal function of the human and wildlife endocrine systems.Objectives: The aim of this study is to determine the concentrations of selected organochlorine pesticides residues [OP'DDT, PP'DDT, alderin, dieldrin, heptachlor, (?,ß,?,?...

  19. Exposure to pesticide residues from consumption of Italian blood oranges

    OpenAIRE

    Fallico, Biagio; D Urso, Mary Giuseppina; Chiappara, Elena

    2009-01-01

    Abstract The paper reports findings concerning a five years study aimed to evaluate pesticides levels, deriving from orchards activities, on the Italian most common orange cultivar (Citrus Sinensis, L. Osbeck, cv. Tarocco). The study, using a Bayesian approach, allowed obtaining both the qualitative (the number) and quantitative distributions (the amount) of pesticides with its own probability value. Multi residues analyses of the 460 analysed samples highlighted the presence o...

  20. Monitoring and Risk Assessment of Pesticide Residues in Commercially Dried Vegetables

    OpenAIRE

    Seo, Young-ho; Cho, Tae-hee; Hong, Chae-kyu; Kim, Mi-sun; Cho, Sung-ja; Park, Won-hee; Hwang, In-sook; Kim, Moo-sang

    2013-01-01

    We tested for residual pesticide levels in dried vegetables in Seoul, Korea. A total of 100 samples of 13 different types of agricultural products were analyzed by a gas chromatography-nitrogen phosphate detector (GC-NPD), an electron capture detector (GC-?ECD), a mass spectrometry detector (GC-MSD), and a high performance liquid chromatography-ultraviolet detector (HPLC-UV). We used multi-analysis methods to analyze for 253 different pesticide types. Among the selected agricultural products...

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

    International Nuclear Information System (INIS)

    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)

  2. Amine modified graphene as reversed-dispersive solid phase extraction materials combined with liquid chromatography-tandem mass spectrometry for pesticide multi-residue analysis in oil crops.

    Science.gov (United States)

    Guan, Wenbi; Li, Zhuonan; Zhang, Hongyan; Hong, Huijie; Rebeyev, Natalie; Ye, Yong; Ma, Yongqiang

    2013-04-19

    Amine modified graphene is successfully synthesized via a one-pot solvothermal reaction between graphene oxide and ammonia water, methylamine or n-butyl amine. The presence of amine groups in graphene is identified by Fourier-transform infrared spectrometry, X-ray photoelectron spectroscopy and an X-ray diffractometer. The ability of amine modified graphene to cleanup fatty acids and other interfering substances from acetonitrile extracts of oil crops has been evaluated. It is found that the resulting CH3NH-G exhibits the best performance in interfering substances removal. Meanwhile, a multi-residue method is validated on 28 representative pesticide residues in four oil crops (rapeseed, peanut, sesame seeds and soybean). This method is based on modified QuEChERS sample preparation with CH3NH-G as reversed-dispersive solid phase extraction material and liquid chromatography-tandem mass spectrometry. Use of matrix-matched standards provides acceptable results for most pesticides with overall average recoveries between 70.5 and 100% and consistent RSDsthidiazuron and diuron. In any case, this method still meets the 0.1-8.3 ?g/kg detection limit needs for most pesticides and may be used for qualitative screening applications, in which any identified pesticides can be quantified and confirmed by a more intensive method that achieves >70% recovery. PMID:23489497

  3. Comparison of QuEChERS official methodologies for the analysis of pesticide residues on Colombian fruit by GC-MS.

    Science.gov (United States)

    España Amórtegui, Julio C; Guerrero Dallos, Jairo A

    2014-04-01

    Surveys of pesticide residues in fruit are important to demonstrate conformity with strict regulations of newly open markets for export of exotic fruit. Multi-residue methods are tools to ensure compliance with regulations and both the CEN and the AOAC have versions of QuEChERS that are used effectively as mainstream methods. The aim of this study was to assess their performance and pick the optimum one for this particular application using GC-MS. The use of graphitised carbon black (GCB) to improve clean-up was assessed. Optimisation of large volume injection (LVI) and implementation of concurrent back-flushing was needed in order to improve sensitivity at a low concentration levels for 33 pesticides (0.01 mg kg(-1)). Cleaner total ion current (TIC) profiles were obtained with the CEN method. Recoveries of most of the pesticides showed statistical differences (? = 0.05) when GCB was used in the AOAC method, unlike the CEN method. In general, GCB/no GCB use for CEN clean-up gave good, very similar results for all fruit, though some pesticides showed some adsorption on the GCB surface. The CEN general method was preferred since acceptable recoveries (> 80%) and RSD (< 20%) can be achieved for all analytes. PMID:24499126

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

    International Nuclear Information System (INIS)

    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)

  5. Studies on organochlorine pesticide residue in fishes from the Densu river basin, Ghana.

    Science.gov (United States)

    Kuranchie-Mensah, Harriet; Yeboah, Philip O; Nyarko, Elvis; Golow, Abledze A

    2013-04-01

    The study was carried out to determine the levels of organochlorine pesticide residue in five fish species Chrysichthys nigrodigitatus, Hepsetus odoe, Tilapia zilli, Heterotis niloticus and Oreochromis niloticus from the Densu river basin (Weija) in Ghana. The fishes sampled from the Weija fish landing site were selected on the basis of their importance to local human fish consumption. The detectable organochlorine pesticides were ?-Hexachlorocyclohexane (HCH), ?-Hexachlorocyclohexane, aldrin and dieldrin. Others investigated were alpha endosulfan, endosulfan sulfate, p,p'-DDT and its metabolite p,p'-DDE, endrin and its metabolite endrin aldehyde and endrin ketone. The total contamination levels of the individual fishes varied in the decreasing order of 9.19 ng g(-1) (O. niloticus), 4.16 ng g(-1) (T. zilli), 3.69 ng g(-1) (C. nigrodigitatus), 3.68 ng g(-1) (H. odoe) and 3.09 ng g(-1) (H. niloticus). The highest organochlorine pesticide residue recorded in the study was alpha-endosulfan while dieldrin was the least pesticide observed. Analysis of variance indicated significant statistical differences for most organochlorine pesticide residues in the samples. The levels of organochlorine pesticides found in fish samples in the study were below maximum residue limit for food safety stipulated by EU, US FDA, FAO, Italy and Australia and thus safe for human consumption. PMID:23283531

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

    Directory of Open Access Journals (Sweden)

    Sarah Blankson-Arthur

    2011-06-01

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

  7. Pesticide Residues Evaluation in Pulp, Juice and Nectar of Fruits

    Directory of Open Access Journals (Sweden)

    Claudia Helena Pastor Ciscato

    2012-04-01

    Full Text Available Industrial processing of fruit in order to produce juice and nectar can contribute to over exposure of some contaminants, such as pesticide residues. Thus, this work aimed to check the compliance with the Maximum Residue Levels (MRL. In our research, 162 samples of frozen pulps, 16 of juice and 2 of nectar, were evaluated for pesticide residues, as well as the acceptable dietary intake (ADI. A multi-residue method was employed and almost 140 active ingredients were studied. Positive results were detected only in pulps, corresponding to 40% of the amount of samples. According to the Brazilian and the Codex Alimentarius legislation, none of the pesticide residues found were above the MRL. The most frequently found compounds were: pyridaphenthion, azinphos-methyl and carbendazim in peach and endosulfan in strawberry samples. Multiple findings were found in strawberry (29.6% and peach (7.8%. Chronic dietary intake was not exceeded. The results demonstrated the necessity of pesticide residue control in fruit.

  8. 78 FR 43115 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2013-07-19

    ...of regulations for residues of pesticides in or...40 CFR part 180 for residues of the herbicide linuron...available for the determination of linuron in plant...40 CFR part 180 for residues of the insecticide...

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

    Directory of Open Access Journals (Sweden)

    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 perspectives for ultra-rapid, sensitive and low-cost monitoring of pesticide residues in tobacco as well as other food and agricultural commodities.

  10. 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

    International Nuclear Information System (INIS)

    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

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

    DEFF Research Database (Denmark)

    Hjorth, Karen; Johansen, K.

    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 samples contained pesticide residues at or below MRL, and 8.4% of samples contained pesticide residues above MRL. Thiabendazole, imazalil and chlorpyrifos were the pesticide most frequently found. Thirty-seven pesticides were found with frequencies higher that 1% in the samples. The results emphasize the need for continuous monitoring of pesticide residues, especially in imported fruits and vegetables.

  12. Pesticide residues in vegetable samples from the Andaman Islands, India.

    Science.gov (United States)

    Swarnam, T P; Velmurugan, A

    2013-07-01

    Vegetable samples of brinjal, okra, green chilli, crucifers, and cucurbits collected from farmers' field were tested for the presence of organochlorine (OC), organophosphorus (OP), and synthetic pyrethroid (SP) compounds using a gas chromatograph equipped with electron capture and flame thermionic detectors. Of the samples tested, 34.0% were found to have pesticide residues. Among the OC compounds, ?-endosulfan, ?-endosulfan, and endosulfan sulfate were detected in 14.5% of the samples with residues. These were taken from crucifer, okra, green chilli, and cucurbit samples. SP compound residues, such as ?-cypermethrin, fenvalerate I, fluvalinate I, deltamethrin, and ?-cyhalothrin were detected in 32% of the samples with residues. OP compound residues such as chlorpyrifos, profenofos, monocrotophos, triazophos, ethion, dimethoate, and acephate were found in 54% of the samples with residues, which were taken from all vegetable samples. Of the positive samples, 15.3% were found to contain residues exceeding the prescribed maximum residue limit. The average pesticide residue content across all the vegetable samples was 0.108 ppm, with values ranging from 0.008 to 2.099 ppm. Multiple residues of more than one compound were detected in 34.1% of samples containing residues. PMID:23208759

  13. Organophosphorus pesticide residues in the total diet of Kuwait

    International Nuclear Information System (INIS)

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

  14. MSPD sample preparation approach for reversed-phase liquid chromatographic analysis of pesticide residues in stem of coconut palm.

    Science.gov (United States)

    Ferreira, Jordana Alves; Santos, Luís Fabrício Santana; Souza, Nicaellen Roberta da Silva; Navickiene, Sandro; de Oliveira, Frederico Alberto; Talamini, Viviane

    2013-08-01

    A method was developed using matrix solid-phase dispersion, together with liquid chromatography with ultraviolet diode array detector for determination of carbofuran, difenoconazole, ?-cyfluthrin, spirodiclofen and thiophanate-methyl in stem of coconut palm. The best results were obtained using 2.0 g of stem, 1.6 g of Florisil as sorbent and cyclohexane:acetone mixture (4:1). The method was validated using stem samples spiked with pesticides at four concentration levels (0.05-2.0 ?g/g). Average recoveries ranged from 70 % to 114.3 %, with relative standard deviations between 1.2 % and 19.2 %. Detection and quantification limits were in the ranges 0.02-0.03 and 0.05-0.1 ?g/g, respectively. PMID:23722654

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

    Science.gov (United States)

    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 ? and ? isomers of endosulphan residues in the Yamuna river. High concentrations of ?-HCH (0.259 ?g/l) and malathion (2.618 ?g/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

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

    Directory of Open Access Journals (Sweden)

    David Adeyemi

    2008-01-01

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

  17. Pesticide Residues and Bees – A Risk Assessment

    OpenAIRE

    Sanchez-bayo, Francisco; Goka, Koichi

    2014-01-01

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

  18. Improved gas chromatography–tandem mass spectrometry determination of pesticide residues making use of atmospheric pressure chemical ionization

    OpenAIRE

    Herna?ndez Herna?ndez, Fe?lix; Beltra?n Arandes, Joaquim; Portole?s Nicolau, Tania; Cherta Cucala, Laura

    2012-01-01

    The capabilities of a recently launched atmospheric pressure chemical ionization (APCI) source for mass spectrometry (MS) coupled to gas chromatography (GC) have been tested in order to evaluate its potential in pesticide residue analysis in fruits and vegetables. Twenty-five pesticides were selected due to their high fragmentation under electron ionization (EI), making that the molecular ion (M+) is practically absent in their spectra. The fragmentation of these pesticides under APCI conditi...

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

    OpenAIRE

    Stoner, Kimberly A.; Eitzer, Brian D.

    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...

  20. Use of activated charcoal in a solid-phase extraction technique for analysis of pesticide residues in tomatoes

    Scientific Electronic Library Online (English)

    Beatriz I. A., Kaipper; Luiz A. S., Madureira; Henry X., Corseuil.

    2001-08-01

    Full Text Available SciELO Brazil | Language: English Abstract in portuguese No presente trabalho foram desenvolvidos métodos de extração e purificação a fim de determinar e monitorar as concentrações dos pesticidas organofosforados mais utilizados em tomates na grande Florianópolis. A técnica de EFS com carvão ativo foi utilizada para a purificação e recuperação dos pestici [...] das metamidofós, acefato, malation e paration metílico. Os solventes para a extração e eluição foram escolhidos após diversas análises, sendo que os melhores resultados foram alcançados através da extração dos pesticidas com acetato de etila e eluição com CH2Cl2 - acetato de etila (7:3). A média recuperada dos analitos das matrizes fortificadas com 0,20 - 0,60 mig g-1 variou entre 85,2 e 100 %, com coeficientes de variação entre 1,3 e 6,3 %. Os limites de detecção foram de 0,04 a 0,12 ng g-1. O adsorvente carvão ativo mostrou-se eficiente para a purificação da matriz de tomate e para a recuperação quantitativa dos analitos, especialmente os mais polares. Abstract in english The present work describes extraction and purification methods that were developed to determine and to monitor the content of organophosphorus pesticides in tomato crops from the agricultural district of Florianópolis, Brazil. SPE technique with activated charcoal was used for purification and recov [...] ery of the pesticides methamidophos, acephate, malation and methyl parathion. The solvents used for sample extraction and elution were chosen after several comparative tests. Best results were achieved using ethyl acetate for extraction and dichloromethane - ethyl acetate (7:3) for elution. Average recoveries from the matrices fortified with 0.20 to 0.60 mug g-1 ranged from 85.2 to 100 % with overall coefficients of variation of 1.3 to 6.3 %. The limits of detection of the method varied between 0.04 and 0.12 ng g-1. Activated charcoal demonstrated to be efficient for tomato matrix purification and for quantitative recovery of the analytes.

  1. Guidelines for predicting the dietary intake of pesticide residues*

    OpenAIRE

    1988-01-01

    These guidelines have been developed to describe procedures for predicting the dietary intake of pesticide residues, and will assist national authorities in their considerations of the acceptability of the Codex maximum residue limits (MRLs). The relevant authorities are invited to consider the basic approaches described in these guidelines, which have been designed to provide reasonable assurance that such MRLs would not result in dietary intakes that exceed the acceptable daily intake (ADI)...

  2. Radiotracer studies of pesticide residues in stored products

    International Nuclear Information System (INIS)

    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

  3. Effects of different washing methods on pesticide organophosphorus residues

    Directory of Open Access Journals (Sweden)

    WANG Xiao-Wei

    2013-02-01

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

  4. Analysis of the residues of 20 organochlorine pesticides in Herba epimedii, a Chinese herbal medicine, by solid-phase extraction with gas chromatography/negative chemical ionization-mass spectrometry.

    Science.gov (United States)

    Guo, Qing; Deng, Ming; Yu, Boyang; Tan, Li

    2010-01-01

    A multiresidue analytical method has been developed to simultaneously determine the residues of 20 organochlorine pesticides in Herba epimedii, a traditional Chinese medicine. The 20 pesticides are included in the list of regulated substances by the Food and Environmental Hygiene Department in Hong Kong. The method consists of solid-phase extraction for cleanup of samples and GC coupled on-line with negative chemical ion-MS to analyze the target pesticides. The chromatographic separation of the compounds was carried out on a DB-1701 column by using an optimal temperature program, and the quantitative analysis was conducted by selected ion monitoring. The LOD and LOQ values fell in the range of 0.0555-5.8821 and 0.1241-17.9333 ng/g, respectively. The average recoveries were between 75.4 and 90.7% (n=5) for the 20 organochlorine pesticides. The developed method proved to be reliable and accurate, and permits rapid determination of the 20 organochlorine pesticides in one run. PMID:20334191

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

    Science.gov (United States)

    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

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

    Directory of Open Access Journals (Sweden)

    Jasbir Singh Bedi

    2015-01-01

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

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

    OpenAIRE

    David Adeyemi; Grace Ukpo; Chimezie Anyakora; JohnPaul Unyimadu

    2008-01-01

    The organochlorine pesticide (OCPs) residues were measured in three species of fish Tilapia zilli (Red belly Tilapia), Ethmalosa fimbriata (Bonga Shad) and Chrysichthys nigrodigitatus (Catfish). These fish species are a significant part of the diet of residents of Lagos Nigeria. The organochlorine pesticides analyzed include DDT(pp'1,1,1-trichloro-2,2-bis-(4-chlorophenyl) ethane), DDD, DDE (pp 1,1-dichloro-2, 2-bis-(4-chlorophenyl) ethylene, HCH (gamma 1,2,3,4,5,6-hexachlorocylohexane, HCB (h...

  8. Potential and real residues of pesticides in sugar beet

    OpenAIRE

    Šovljanski Radmila A.; Lazi? Sanja D.; Vukovi? 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...

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

    OpenAIRE

    Wen Li; Ming Sun; Minzan Li

    2013-01-01

    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 ...

  10. Quantification of Organochlorine Pesticide Residues in the Buffalo Milk Samples of Delhi City, India

    Directory of Open Access Journals (Sweden)

    Mohd Aslam

    2013-08-01

    Full Text Available The ill effects of green revolution include residues of extensively used chemical pesticides in various environmental components. The present study was designed to analyze the levels of organochlorine pesticide residues along with chemical composition in buffalo milk samples collected from different localities of Delhi. Milk monitoring can yield information about the kinds and quantities of pesticides in the environment as well as in our daily diet. In this study, the residue of three different organochlorine pesticides, namely Hexachlorocyclohexane (HCH, Dichlorodiphenyltrichloroethane (DDT and Endosulfan have been reported. Residues of Lindane exceeded the Maximum Residual Limit values in 50% of the samples is a cause of serious concern. The p,p’-DDT was detected in 70% of the samples with p,p’-DDE (dichlorodiphenyldichloroethylene in 80% of the milk samples of different parts of Delhi state. DDD (Dichlorodiphenyldichloroethane another metabolite of p,p’-DDT was detected in 65% of the milk samples. The analysis indicates that DDT is the major contaminants in different parts of Delhi state. ? and ? endosulfan were detected in 35% and 40% of the samples analyzed. The statistical correlation shows no significant correlation between chemical compositions of the samples. The presence of multiple chemicals in virtually all samples of buffalo milk raises new questions about the possible toxicological impacts of chemical mixtures on an infant’s developing nervous and immune systems and reproductive organs.

  11. 75 FR 13277 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2010-03-19

    ...make a final determination on these...regulations for residues of pesticides...residues of the insecticide flubendiamide...part 180 for residues of the herbicide...for the determination of triflusulfuron methyl residues in garden...residues of the insecticide...

  12. Determination of organochlorine pesticide residue in sediment and water from the Densu river basin, Ghana.

    Science.gov (United States)

    Kuranchie-Mensah, Harriet; Atiemo, Sampson Manukure; Palm, Linda Maud Naa-Dedei; Blankson-Arthur, Sarah; Tutu, Anita Osei; Fosu, Paul

    2012-01-01

    The distribution of organochlorine pesticides in the aquatic ecosystem from the Densu river revealed varying levels of concentration in water and the sediment samples. Three locations were sampled along the river to evaluate the levels of organochlorine pesticide residue in the river. Sediment and surface water samples were extracted by soxhlet and liquid-liquid extraction respectively and analyzed using Gas Chromatograph coupled with electron capture detector. The detectable organochlorine pesticides were gamma-hexachlorocyclohexane (HCH), delta-hexachlorocyclohexane, heptachlor, aldrin and dieldrin. The other pesticides that were investigated are gamma-chlordane, alpha endosulfan, endosulfan sulfate, p,p'-DDT and its metabolite p,p'-DDE, methoxychlor, endrin and its metabolite endrin aldehyde and endrin ketone. The order of increasing frequency of detection of samples was higher in sediment than water. In sediment, the mean concentration ranged from 0.030 ?g kg(-1) dry weight (endrin) to 10.98 ?g kg(-1) dry weight (aldrin). The highest detected concentration of organochlorine in water was endosulfan sulfate with mean concentration of 0.185 ?g L(-1). Analysis of variance indicated significant differences for most organochlorine pesticide residue in the sediment sampled from the various locations. Some of the levels of organochlorine pesticides detected in water were relatively high compared to guideline values set by World Health Organization and Australia and thus could be harmful if the trend is not checked. PMID:22123529

  13. Bioavailability of nonextractable (bound) pesticide residues to earthworms.

    Science.gov (United States)

    Gevao, B; Mordaunt, C; Semple, K T; Piearce, T G; Jones, K C

    2001-02-01

    There is an ongoing debate regarding whether nonextractable (bound) pesticide residues in soils are occluded or may remain bioavailable in the long term in the environment. This study investigated the release of 14C-labeled residues, which were previously nonextractable after exhaustive extraction with organic solvents in soils, and their uptake by earthworms (Aporrectodea longa). After a 100-day incubation of soils treated with 14C-labeled atrazine, isoproturon, and dicamba and exhaustive Soxhlet extractions with methanol and dichloromethane, nonextracted 14C-labeled residues remaining in the soils were 18, 70, and 67%, respectively. Adding clean soil in the ratio of 7:1 increased the volumes of these extracted soils. After earthworms had lived in these previously extracted soils for 28 days, 0.02-0.2% of previously bound 14C activity was absorbed into the earthworm tissue. Uptake by earthworms was found to be 2-10 times higher in soils containing freshly introduced 14C-labeled pesticides as compared to soils containing nonextractable 14C-labeled residues. The differential bioavailability observed between freshly introduced 14C-labeled pesticides and those previously nonextractable may be related to the ease of transfer of the 14C activity into the solution phase. By the end of the 28-day incubation period, 3, 23, and 24% of previously nonextractable 14C-labeled isoproturon, dicamba, and atrazine residues, respectively, were extracted by solvents or mineralized to 14CO2. The amounts of 14C activity released were not significantly different in the presence or in the absence of earthworms in soils containing previously nonextractable residues. However, the formation of bound residues was 2, 2, and 4 times lower for freshly introduced 14C-labeled isoproturon, dicamba, and atrazine, respectively, suggesting that the presence of earthworms retarded bound residue formation. PMID:11351720

  14. EFSA’s contribution to the implementation of the EU legislation on pesticide residues in food

    Directory of Open Access Journals (Sweden)

    Reich H

    2012-10-01

    Full Text Available

    The active involvement of EFSA in the area of pesticide residues assessment started in 2006 following the adoption of new legislation on maximum residue levels (MRLs of pesticides in food (Regulation (EC No 396/2005. EFSA took on a new role as an independent risk assessment body in the process of MRL setting, providing important contributions in the EU-wide harmonisation of MRLs. With the development of a risk assessment model (EFSA PRIMo the risk assessment process has become more transparent. EFSA is now involved in all routine MRL setting processes by giving advice to the risk managers and, so far, has given recommendations on ca. 1 200 MRLs. EFSA also provides other scientific assessments, in many cases where urgent advice is needed due to unexpected incidences which require immediate risk management action. Currently, high priority is given to the systematic MRL review, which involves making a comprehensive inventory of the scientific studies and performing risk assessments for the pesticides covered by this programme. Another major task for EFSA is the drafting of the Annual Report on Pesticide Residues, which gives an overview of the pesticide residues in food available to European consumers. EFSA has revised the data collection of monitoring results to allow more powerful data analysis to identify potential consumer risks and weak points in the food production system, and to develop strategies for improvements. EFSA places major emphasis on risk communication on topics related to pesticide residues, which is an integral part of EFSA’s tasks as risk assessor. Building on the achievements of the last six years, future challenges for EFSA include the continued improvement of risk assessment methodologies (updating risk assessment models, developing new methodologies for cumulative risk assessment and the timely provision of risk assessments for MRL applications and MRL reviews.

  15. The Organochlorine Pesticides Residue Levels in Karun River Water

    Directory of Open Access Journals (Sweden)

    Behrooz Jannat

    2013-01-01

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

  16. Evaluation of pesticide residues in fruit from Poland and health risk assessment

    Directory of Open Access Journals (Sweden)

    B. ?ozowicka

    2013-05-01

    Full Text Available In the present study an effort has been made to evaluate the residues of insecticides, fungicides and herbicides in fruit fromPolandand their health risks assessed. Accredited multiresidue methods based on gas and liquid chromatography, and spectroscopic technique were used to determine the concentrations above 160 pesticides. A total of 392 samples of 15 different fruit were collected during the May 2010 to October 2012. In 48.2% of samples no residues were found, 45.9% of samples contained pesticide residues at or below the EU MRL, and 5.9% of samples contained pesticide residues above MRL. Sour cherries (66% and apples (63% were the commodities in which pesticide residues the most frequently occurred. Thirty one different pesticides were detected in total. Dithiocarbamate, captan, cyprodinil and boscalid were the pesticide most frequently found. Multiple pesticides ( > 1 pesticide were detected in about 30.1% samples. The dietary intake of residues of some pesticides can pose acute hazards. Data obtained were used for estimating the potential health risks associated with the exposures to these pesticides. The highest estimated daily intakes (EDIs for children were: 22% for dimethoate and 112% for diazinone of the ADI. The most critical commodity was apple, contributing 1.30 to the acute Hazard Index for flusilazole. The results show that despite a high occurrence of pesticide residues in fruit it could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring of pesticide residues in fruit is recommended.

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

    OpenAIRE

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

    2010-01-01

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

  18. Pesticide residues in grapes from integrated production of the Slovene origin The CORRECTED TITLE is: Pesticide residues in grapes from vineyards included in integrated pest management in Slovenia.

    OpenAIRE

    Bas?a C?esnik, Helena; Gregorc?ic?, Ana; C?us?, Franc

    2008-01-01

    Abstract Although the list of pesticides used in integrated pest management (IPM) in grape growing and their annual application rates are limited, we are still confronted with the problem of pesticide residues in grapes. The paper presents the results of pesticide monitoring in 47 samples of wine grapes (Vitis vinifera L.) of the 2006 vintage from the vineyards included in IPM. The grape samples were analysed for the presence of 67 pesticides. Among them, 20 were allowed in IPM in ...

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

    International Nuclear Information System (INIS)

    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)

  20. Alternative calibration techniques for counteracting the matrix effects in GC-MS-SPE pesticide residue analysis - a statistical approach.

    Science.gov (United States)

    Rimayi, Cornelius; Odusanya, David; Mtunzi, Fanyana; Tsoka, Shepherd

    2015-01-01

    This paper investigates the efficiency of application of four different multivariate calibration techniques, namely matrix-matched internal standard (MMIS), matrix-matched external standard (MMES), solvent-only internal standard (SOIS) and solvent-only external standard (SOES) on the detection and quantification of 20 organochlorine compounds from high, low and blank matrix water sample matrices by Gas Chromatography-Mass Spectrometry (GC-MS) coupled to solid phase extraction (SPE). Further statistical testing, using Statistical Package for the Social Science (SPSS) by applying MANOVA, T-tests and Levene's F tests indicates that matrix composition has a more significant effect on the efficiency of the analytical method than the calibration method of choice. Matrix effects are widely described as one of the major sources of errors in GC-MS multiresidue analysis. Descriptive and inferential statistics proved that the matrix-matched internal standard calibration was the best approach to use for samples of varying matrix composition as it produced the most precise average mean recovery of 87% across all matrices tested. The use of an internal standard calibration overall produced more precise total recoveries than external standard calibration, with mean values of 77% and 64% respectively. The internal standard calibration technique produced a particularly high overall standard deviation of 38% at 95% confidence level indicating that it is less robust than the external standard calibration method which had an overall standard error of 32% at 95% confidence level. Overall, the matrix-matched external standard calibration proved to be the best calibration approach for analysis of low matrix samples which consisted of the real sample matrix as it had the most precise recovery of 98% compared to other calibration approaches for the low-matrix samples. PMID:24968235

  1. Determination of Pesticides Residues in Selected varieties of Mango

    OpenAIRE

    Saqib Hussain; Tariq Masud; Karam Ahad

    2002-01-01

    The present study was undertaken to access the residue of commonly used pesticides viz Cypermethrin, Methamedophos, Monocrotophos, Cyfluthrin, Dialdrin and Methyl Parathian respectively in three varieties of Mango being collected from the grower fields in Multan division. The samples were treated with organic solvent Cyclohexane and ethylacetate (1:1), cleaned on Gel Permeation Chromatograph (GPC) and analyzed on auto system Gas Chromatograph (GC) with electron capture detector (ECD). All the...

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

    OpenAIRE

    Sarah Blankson-Arthur; Owiredu Yeboah, P.; 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 ((?-HCH) and ?-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 ext...

  3. Design of a novel noninvasive spectrometer for pesticide residues monitor

    Science.gov (United States)

    Ren, Zhong; Liu, Guodong; Huang, Zhen

    2014-11-01

    Although the gas or liquid chromatography had been widely used into pesticide residues monitoring, some drawbacks such as time-consuming, complicated operation and especially the destructivity for samples were existed. To overcome the limits of destructive detection methods, the noninvasive detection method based on spectroscopy was used to detect the pesticide residues in this paper. To overcome low resolution and light-efficiency due to the drawbacks of the classical plane and holography concave gratings, a novel noninvasive spectrometer for pesticide residues monitor (PRM) based on volume holography transmission (VHT) grating was designed. Meanwhile, a custom-built splitting light system for PRM based on the VHT grating was developed. In addition, the linear charge coupled device (CCD) with combined data acquisition (DAQ) card and the virtual-PRM based on LabVIEW were respectively used as the spectral acquisition hardware and software-platform. Experimental results showed that the spectral resolution of this spectrometer reached 2nm, and the VHT grating's diffraction efficiency was gotten via the simulation experiment.

  4. 76 FR 68750 - Final National Pollutant Discharge Elimination System (NPDES) Pesticide General Permit for Point...

    Science.gov (United States)

    2011-11-07

    ...biological pesticides and chemical pesticide residues to Waters of the United States...permit that all chemical pesticides have a residue, and, therefore would need...analysis, titled, ``Economic Analysis of the Pesticide General Permit (PGP)...

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

    Science.gov (United States)

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

    2015-06-01

    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

  6. Evaluation of two sample treatment methodologies for large-scale pesticide residue analysis in olive oil by fast liquid chromatography-electrospray mass spectrometry.

    Science.gov (United States)

    Gilbert-López, Bienvenida; García-Reyes, Juan F; Fernández-Alba, Amadeo R; Molina-Díaz, Antonio

    2010-06-11

    In this study, a comprehensive evaluation of two simple sample treatment methodologies has been carried out for the development of large-scale multi-residue methods for pesticide testing in olive oil. The proposed methodologies are based on (a) liquid-liquid partitioning with acetonitrile followed by dispersive solid-phase extraction clean-up using graphitized carbon black, primary-secondary amine and C(18) sorbents; (b) liquid partitioning with acetonitrile saturated with petroleum ether followed by matrix solid-phase dispersion (MSPD) using aminopropyl as sorbent material and a Florisil cartridge for final clean-up in the elution step. To evaluate the proposed sample treatment methodologies, 105 representative multi-class pesticides were studied using fast liquid chromatography-electrospray time-of-flight mass spectrometry (LC-TOFMS). For validation purposes, recoveries studies were carried out at 10 and 100microgkg(-1) levels, yielding recovery rates in the range 70-130% for 72% of analytes using liquid-liquid procedure and for 57% analytes using MSPD procedure. The LC-MS method provided good linearity, precision and accuracy. The limits of detection obtained were lower than 10microgkg(-1) for more than 85% analytes using both sample treatment methodologies. In addition, minor matrix effects (i.e. signal suppression or enhancement pesticide testing in olive oil samples, showing the ability to quickly detect trace amount of over one hundred target species with different physicochemical properties, without requiring expensive instrumentation for sample treatment step and involving relatively low amounts of solvent consumption and waste generation. PMID:20447638

  7. Adverse Effects of Pesticides Residues on Biochemical Markers in Pakistani Tobacco Farmers

    OpenAIRE

    Khan, Dilshad A.; Bhatti, Mahwish M.; Khan, Farooq A.; Naqvi, Syed T.; Karam, A.

    2008-01-01

    Tobacco is an important cash crop of Pakistan and tremendous amount of irrational pesticides are being used to control insect growth. The frequency of plasma pesticide residues above acceptable daily intake (ADI) and its correlation with biochemical markers for assessment of adverse health effects in the tobacco farmers at district Sawabi, Pakistan was determined. Total 109 adult males consisting of 55 tobacco farmers exposed to pesticides and 54 controls were included. Pesticides residues in...

  8. 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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Cabras, P; Angioni, A

    2000-04-01

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

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

    Science.gov (United States)

    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 ?g kg(-)1 for alpha hexachlorocyclohexane (HCH) and endosulfan I, 20 ?g kg(-1) for p,p'-DDT, and 6 ?g 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

  11. Earthworm tolerance to residual agricultural pesticide contamination : Field and experimental assessment of detoxification capabilities

    DEFF Research Database (Denmark)

    Givaudan, Nicolas; Binet, Françoise

    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 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 ?g active ingredient epoxiconazole g-1 dry soil, RoundUp Flash®, 2.5 ?g active ingredient glyphosate g-1 dry soil, and their mixture), revealed that environmental pre-exposure accelerated activation of the detoxification enzyme sGST towards epoxiconazole. © 2014 Elsevier Ltd. All rights reserved.

  12. The comparison of dispersive solid phase extraction and multi-plug filtration cleanup method based on multi-walled carbon nanotubes for pesticides multi-residue analysis by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Qin, Yuhong; Zhao, Pengyue; Fan, Sufang; Han, Yongtao; Li, Yanjie; Zou, Nan; Song, Shuangyu; Zhang, Yuan; Li, Fangbing; Li, Xuesheng; Pan, Canping

    2015-03-13

    In this study, dispersive-Solid Phase Extraction (d-SPE) cleanup and multi-plug filtration cleanup (m-PFC) methods were compared for 25 representative pesticides in six matrices (wheat, spinach, carrot, apple, citrus and peanut) by QuEChERS-LC-ESI-MS/MS detection. The type of sorbents in dispersive-SPE (d-SPE) was optimized for the above matrices. Multi-walled carbon nanotubes (MWCNTs), which mixed other materials like PSA (Primary Secondary Amines), GCB (Graphitized Carbon Black) and C18 (Octadecyl-silica), showed brilliant cleanup performance in multi residue monitoring (MRM) pesticide residue analysis. Cleanup effects with d-SPE and m-PFC methods were examined. When spiked at 3 concentration levels of 10, 100, 500?g/kg in above matrices, for both d-SPE and m-PFC methods, the recoveries ranged from 70 to 110% with relative standard deviations (RSDs) lower than 20%. Limits of quantification (LOQs) for both cleanup methods ranged from 1 to 25?g/kg. Matrix-matched calibrations were performed with the coefficients of determination more than 0.99 between concentration levels of 10-1000?g/kg. It was found that m-PFC was more convenient and effective than d-SPE with the same sorbents, due to the increased contact time and contact area between the extracts and compressed sorbents. The study demonstrated that m-PFC method could be used as a rapid, convenient and high-throughput cleanup method for analysis of pesticide residues. PMID:25660523

  13. Potential and real residues of pesticides in sugar beet

    Directory of Open Access Journals (Sweden)

    Šovljanski Radmila A.

    2006-01-01

    Full Text Available 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 application (PTA whereas the pre-harvest interval for herbicides ranges from 30 to 91 days and is ensured by the application period. Based on the results from the literature and on their own studies, the authors are of the opinion that the residues of the applied pesticides in sugar beet protection in accordance with the principles of good agricultural practice will be significantly lower than the maximum tolerable ammounts and that at the level from 1/4 to 1/10 of MRL. IT is necessary to emphasize the necessity of MRL determination both in leaves and in sugar loaf.in case they are used as animal feed.

  14. [Trial for estimating the concentration of pesticide residues in the ingredients of processed foods].

    Science.gov (United States)

    Fukui, Naoki; Takatori, Satoshi; Kitagawa, Yoko; Okihashi, Masahiro; Kajimura, Keiji; Obana, Hirotaka

    2013-01-01

    If pesticide residues are detected at over the uniform limit (0.01 ppm) in processed foods, the maximum residue limits of pesticides in each ingredient should be considered. For that purpose, analysis of pesticide residues in the ingredients would be required, but in many cases it is difficult to obtain ingredients from the same lot, or the processed foods may have been manufactured overseas. Thus, a means of estimating pesticide concentrations in ingredients before processing would be important. In this study, we estimated the concentration of paclobutrazol, which was detected in LM pickles (LMPs), that would have been present in Takana (LM; mustard leaf) before processing. The LMPs mainly consisted of LM and seasoning liquid (SL), and other ingredients (sesame seeds or red pepper) accounted for less than 0.2% (w/w) of the LMPs. The LM and SL were separated and their paclobutrazol concentrations were determined. The concentration of paclobutrazol in the SL was approximately 1/10 of that detected in LM. Loss of water from LM during processing was taken into account to calculate the content of paclobutrazol in LM before processing, based on the analytical result of processed LM. PMID:24389469

  15. 75 FR 57942 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2010-09-23

    ...modified Monier-Williams method, which is the official method of analysis approved by the Association...pesticide inert ingredient in pesticide formulations applied to growing...after harvest. An analytical method has not been proposed...

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

    OpenAIRE

    Benbrook, Charles M.; Baker, Brian P.

    2014-01-01

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

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

    OpenAIRE

    Claeys, Wendie Liliane; Voghel, Simon; Schmit, Jean-franc?ois; Vromman, Vale?rie; Pussemier, Luc

    2008-01-01

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

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

    International Nuclear Information System (INIS)

    Cocoa is a major cash crop and contributes significantly to Ghana's economy. Majority of this contribution is as a result of foreign earnings in foreign trade partnership. Cocoa products are consumed locally aside it generating foreign income for the country. Pesticide residues above allowable limits in cocoa beans have potential detrimental effects on human health, depending on the frequency of exposure and/or the potency or toxicity of the pesticide. Pesticide residues on cocoa also attract trade sanctions from international trading partners. The approved pesticides, which are used to control pests in the growing cocoa in Ghana, are: Diazinon, Cypermethrin, Deltamethrin, Acetamiprid, Imidicloprid and Pyrethrums; nevertheless some unapproved pesticides on cocoa such as Pirimiphos-methyl, Chlorpyrifos, Endosulfan, Fenitrotion, Fenvalerate, Permethrin and others find their way for use on cocoa in Ghana. The main objective of this study was to determine the levels of pesticide residues in fermented dried cocoa beans produced and ready for export in Ghana, using gas chromatography mass spectrometry. It also seeks to provide the baseline information on contamination levels of pesticide residues in semi-finished and selected finished fermented dried cocoa beans products. Fermented dried cocoa beans were sampled at random in the two main COCOBOD warehouses located in Tema and Takoradi. Semi-finished and finished cocoa products were obtained from processing industries in Temobtained from processing industries in Tema. Two extraction methods were used. The second extraction method was as by the QuEChERS method for vegetable oils which was used for the cocoa butter samples only, after being liquefied in water bath at 40 degrees celsius. The investigated pesticides consisted of fifteen organochlorine pesticides, thirteen organophosphorous pesticides and nine synthetic pyrethroids pesticides. Percentage recoveries ranged from 70-110 percent, with instrumental detection limits of 0.3ug/kg, 0.15ug/g and 0.15ug/g for the organochlorine, organophosphorous and synthetic pyrethroids pesticides respectively. Multivariate analysis on the residue data obtained from fermented dried cocoa beans in R-mode and Q-mode grouped the detected pesticides into currently used, previously used and drift from neighbouring crops pesticides applications. It also grouped sampled cocoa beans into four major clusters based on similarities in crop storage and farm practices. Beta-HCH (18.7 ?g/kg), Gamma-chlordane (152.0 ?g/kg), Methamidophos (18.5 ?g/kg), Profenofos (31.8 ?g/kg), Allethrin (10.5 ?g/kg), Cypermethrin (32.0 ?g/kg) and Fenvalerate (14.6 ?g/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

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

    International Nuclear Information System (INIS)

    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

  20. Pesticide residues in conventional, integrated pest management (IPM)-grown and organic foods: insights from three US data sets.

    Science.gov (United States)

    Baker, B P; Benbrook, C M; Groth, E; Lutz Benbrook, K

    2002-05-01

    An analysis of pesticide residue data was performed to describe and quantify differences between organically grown and non-organic fresh fruits and vegetables. Data on residues in foods from three different market categories (conventionally grown, integrated pest management (IPM)-grown/no detectable residues (NDR), and organically grown) were compared using data from three test programmes: The Pesticide Data Program of the US Department of Agriculture; the Marketplace Surveillance Program of the California Department of Pesticide Regulation; and private tests by the Consumers Union, an independent testing organization. Organically grown foods consistently had about one-third as many residues as conventionally grown foods, and about one-half as many residues as found in IPM/NDR samples. Conventionally grown and IPM/NDR samples were also far more likely to contain multiple pesticide residues than were organically grown samples. Comparison of specific residues on specific crops found that residue concentrations in organic samples were consistently lower than in the other two categories, across all three data sets. The IPM/NDR category, based on data from two of the test programmes, had residues higher than those in organic samples but lower than those in conventionally grown foods. PMID:12028642

  1. 40 CFR 158.2082 - Experimental use permit biochemical pesticides residue data requirements table.

    Science.gov (United States)

    2010-07-01

    ...biochemical pesticides product chemistry and are referenced...section. 1. Residue chemistry data requirements...biochemical product chemistry data requirements...premises, to livestock drinking water, or to...

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

    Science.gov (United States)

    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 ?g/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 ?g/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

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

    Directory of Open Access Journals (Sweden)

    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.

  4. Exposure assessment of fruit contaminated with pesticide residues from Valencia, 2001-2003

    OpenAIRE

    Berrada, Houda; Ferna?ndez, Mo?nica; Ruiz, Maria Jose; Molto?, Juan Carlos; Man?ez, Jordi

    2006-01-01

    Abstract A total of 634 samples of oranges, tangerines, peaches, nectarines, khakis, and watermelons were collected from an Agricultural Valencia Community Cooperative during May 2001 to April 2003 campaigns and analyzed for fifteen pesticides among those recommended for their pest treatment. A conventional multi-residue analytical procedure based on a ethyl acetate extraction was used followed by gas chromatography coupled to nitrogen phosphorus detector for routine analysis and ...

  5. 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.

    Science.gov (United States)

    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

  6. Levels of organochlorine pesticide residue in grasscutter (Thryonomys swinderianus) tissues

    International Nuclear Information System (INIS)

    Organochlorine pesticide residues have been determined in the muscle, liver and kidney tissues from a total of 45 grasscutter (Thryonomys swinderianus) meat samples obtained from the Gomoa district, a vegetable farming area in the Central Region of Ghana. All samples were analyzed for their residue content of the following organochlorine pesticides; DDT, DDE, hexachlorocyclohexane isomers, lindane (?-HCH) and ?-HCH, dieldrin, aldrin, endrin, endrin aldehyde, endrin ketone, alpha endosulfan, endosulfan sulfate, chlordane, heptachlor and methoxychlor. The results indicated that all the analyzed samples were contaminated with the studied organochlorine pesticides. Aldrin and heptachlor were the principal contaminants in all the samples. The muscle had the highest pollutant load. All organochlorine pesticides investigated were detected in the muscle tissues of the grasscutter at the following mean concentrations; aldrin 1.833?g /kg, heptachlor 0.695?g /kg, ?-HCH 0.283?g /kg, ?-HCH 0.108?g /kg, dieldrin 0.040 ?g /kg, p,p'-DDT 0.019?g /kg. p,p'-DDE 0.014?g /kg, endrin 0.018?g /kg, endrin aldehyde 0.090?g /kg, endrin ketone 0.340?g /kg, ?-endosulfan 0.162?g /kg, endosulfan sulfate 0.183?g /kg, gamma-chlordane 0.174?g /kg and methoxychlor 0.101?g /kg wet weight. The organochlorine pesticide residues were detected in the liver tissues at the following mean concentrations; aldrin 1.315?g /kg, heptachlor 0.530?g /kg, dieldrin 0.050?g /kg, ?-HCH 0.233?g /k, ?-HCH 0.233?g /kg, ?-HCH 0.070?g /kg, p,p'-DDT 0.123?g /kg. p,p'-DDE 0.043?g /kg endrin aldehyde 0.110?g /kg, endrin ketone 0.115?g /kg, gamma-chlordane 0.093?g /kg and methoxychlor 0.128?g /kg wet weight. No endrin was however detected in the liver. The highest concentrations of ?-HCH, ?-HCH, endrin ketone and endrin aldehyde were measured in the kidney. The mean concentrations of ?-HCH and ?-HCH in the kidney were 0.435?g /kg and 0.107?g /kg respectively. Endrin aldehyde was detected at 0.135?g /kg in the kidney. The level of endrin ketone was higher than endrin aldehyde in all the tissues analyzed. The mean concentration of endrin ketone was 0.347 ?g /kg in the kidney. The mean concentration of ?-endosulfan was 0.140?g /kg wet weight. Endosulfan sulfate was detected at 0.033 ?g /kg in the kidney. The mean concentration of gamma-chlordane was 0.020 ?g /kg kidney. Methoxychlor was detected at 0.183?g /kg, wet weight in the kidney. The levels of organochlorine pesticides residues detected in all the tissues were below the accepted maximum residue limits (MRL), as adopted by the WHO/FAO Codex Alimentarius Commission.

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

    Science.gov (United States)

    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

  8. Reduction of hazardous organic solvent in sample preparation for hydrophilic pesticide residues in agricultural products with conventional liquid chromatography.

    Science.gov (United States)

    Watanabe, Eiki; Kobara, Yuso; Baba, Koji; Eun, Heesoo

    2013-05-22

    An original extraction method using water as an extractant has been established for environmentally friendly sample preparation procedures for hydrophilic pesticides (acetamiprid, clothianidin, dinotefuran, flonicamid, imidacloprid, methomyl, pymetrozine, thiacloprid, and thiamethoxam) in agricultural samples with conventional HPLC. Water-based extraction and cleanup with two solid-phase extraction cartridges can recover target hydrophilic pesticides quantitatively. The matrix effects of tested samples on the proposed method developed herein were negligibly small. Under the optimized conditions, the recoveries of almost all tested pesticides were 70-120% with satisfactory precision (%CV < 20%). The analytical data are in good accordance with Japanese or European Union guidelines for pesticide residue analysis. The reduction rate of hazardous organic solvents used for the proposed method and by reducing the sample size for extraction was about 70% compared with the Japanese authorized reference method used in this work. The results demonstrate the feasibility of the proposed sample preparation procedures for hydrophilic pesticides. PMID:23614723

  9. Organophosphate and Carbamate Pesticide Residues in Beans from Markets in Lagos State, Nigeria

    OpenAIRE

    Ogah C.O; Coker H.B; Adepoju-Bello A.A

    2011-01-01

    Foods treated with pesticides for protection against destructive pests often contain residues of these chemicals. The levels of pesticide residues in food are often determined as a means of assessing appropriate use as well as the level of human exposure to these chemicals and hence their potential human health hazards. The aim of this study was to determine the concentration of organophosphate and carbamate pesticides in beans samples collected from markets in Lagos State and compare these v...

  10. Present situation of pesticide residues and biological suppression of pests and diseases in Chinese tea gardens

    OpenAIRE

    Han, B.; Dong, W.; Cui, L.

    2004-01-01

    Several insecticides, germicides and herbicides which, are now prohibited, are still used in Chinese common tea gardens. Applied amounts of the pesticides with high toxicity and long time residues, such as methomyl, cannot bypass certain limits in A-grade green food tea gardens. Pesticides are forbidden to be used in AA-grade green food tea gardens and organic tea gardens. Pesticide residues in a large number of merchant teas exceeded the national standard during 1998 - 2001. According to nat...

  11. Health risk for children and adults consuming apples with pesticide residue.

    Science.gov (United States)

    Lozowicka, Bozena

    2015-01-01

    The presence of pesticide residues in apples raises serious health concerns, especially when the fresh fruits are consumed by children, particularly vulnerable to the pesticide hazards. This study demonstrates the results from nine years of investigation (2005-2013) of 696 samples of Polish apples for 182 pesticides using gas and liquid chromatography and spectrophotometric techniques. Only 33.5% of the samples did not contain residues above the limit of detection. In 66.5% of the samples, 34 pesticides were detected, of which maximum residue level (MRL) was exceeded in 3%. Multiple residues were present in 35% of the samples with two to six pesticides, and one sample contained seven compounds. A study of the health risk for children, adults and the general population consuming apples with these pesticides was performed. The pesticide residue data have been combined with the consumption of apples in the 97.5 percentile and the mean diet. A deterministic model was used to assess the chronic and acute exposures that are based on the average and high concentrations of residues. Additionally, the "worst-case scenario" and "optimistic case scenario" were used to assess the chronic risk. In certain cases, the total dietary pesticide intake calculated from the residue levels observed in apples exceeds the toxicological criteria. Children were the group most exposed to the pesticides, and the greatest short-term hazard stemmed from flusilazole at 624%, dimethoate at 312%, tebuconazole at 173%, and chlorpyrifos methyl and captan with 104% Acute Reference Dose (ARfD) each. In the cumulative chronic exposure, among the 17 groups of compounds studied, organophosphate insecticides constituted 99% acceptable daily intake (ADI). The results indicate that the occurrence of pesticide residues in apples could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring and tighter regulation of pesticide residues is recommended. PMID:25260164

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

    Science.gov (United States)

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

    2013-04-01

    The use and application of pesticides in vineyard is a common practice, which is important to prevent pest and diseases and improve the crop health and production, but on the other hand it could involve a potential risk for humans and the environment. For this reason, it is important to develop and validate a simple and fast multiresidue method to determine the presence of these compounds in soils. La Rioja region (Spain) is one of the most important wine-growing regions in Spain, which also entails that could be an important area of pesticide pollution. The objective of this work is to assess the temporal distribution of the possible pesticide pollution in soils from different areas of La Rioja (Spain). The pesticides selected in this study included fungicides (metalaxyl, and its metabolite CGA62826, pyrimethanil, tebuconazole, myclobutanil, kresoxim-methyl, triadimenol and flutriafol); herbicides (fluometuron, terbuthylazine and its metabolites desethylterbuthylazine and hydroxyterbuthylazine, lenacil, ethofumesate and acetochlor) and insecticides (methoxyfenozide and pirimicarb). The pesticide residues were evaluated by two analytical techniques, gas chromatography and liquid chromatography (GC-MS and LC-MS). The extraction procedure of pesticides from soils was optimized using two soil samples (blank soils) with different texture and characteristics collected from areas without pesticide application. Recoveries were studied in soil samples fortified with all pesticides at two levels of concentrations (the agronomic dose, 0.1 mg kg-1, and ten times this dose, 1 mg kg-1). Different extraction solvents were tested. The best results were obtained with methanol:acetone (50:50) mixture or methanol:CaCl2 0.01 M (50:50) mixture for hydroxyterbuthylazine and CGA62826. The accuracy (average recovery) and precision (reproducibility and repeatability) of the method were assessed using six replicates and the limits of detection (LODs) and quantification (LOQs) were estimated. Recoveries were above 70% for all pesticides. Good linear relationships of the calibration curves (0.01-1 ?g 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 studied. After the development and validation of an analytical method, the study of the temporal variability of the pesticide pollution in different periods of time (September 2011, and March, June and October 2012) were performed. Herbicide 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.

  13. Pesticide residues in sediments and aquatic species in Lake Nokoué and Cotonou Lagoon in the Republic of Bénin.

    Science.gov (United States)

    Yehouenou A Pazou, Elisabeth; Aléodjrodo, Patrick Edorh; Azehoun, Judicaël P; van Straalen, Nico M; van Hattum, Bert; Swart, Kees; van Gestel, Cornelis A M

    2014-01-01

    Lake Nokoué and Cotonou Lagoon are the most important and most productive continental freshwaters in Bénin, with an estimated fish production of over 2 tonnes per hectare in Lake Nokoué. Organochlorine pesticides are used in agriculture and to repel tsetse flies, malaria mosquitoes and other diseases raised. Sediment, fish, shrimp and oyster species were collected in Lake Nokoué and Cotonou Lagoon for pesticide residues analysis. The main pesticides identified in sediment were pp'-DDT and its metabolites pp-DDE and pp'-DDD, with residue levels between the detection limit and 24.4 ?g/kg dry weight. Fish species commonly consumed such as Elops lacerta, Podamasys jubelini, Gobbienellus occidentalis, Ethmalosa fimbriata, Mugil cephalus and Hemichromis fasciatus were contaminated with residues of seven to nine pesticides, including pp-DDE, op'-DDD, pp'-DDD, op'-DDT, pp'-DDT, ?-endosulfan, aldrin, dieldrin and ?-hexachlorocyclohexane. The levels ranged from detection limit to 289 ng/g lipid. The same pesticides were also detected in other aquatic species, such as shrimp and oysters. A summed risk assessment, comparing pesticide intake levels through fish consumption with tolerable daily intake levels proposed by the World Health Organization, showed in all cases a low risk for human health. PMID:23942697

  14. [Survey of pesticide residues in imported tea (1992.4-2010.3)].

    Science.gov (United States)

    Kobayash, Maki; Ohtsuka, Kenji; Tamura, Yasuhiro; Tomizawa, Sanae; Kinoshita, Teruaki; Kamijo, Kyoko; Iwakoshi, Keiko; Sato, Chizuko; Nagayama, Toshihiro; Takano, Ichiro

    2013-01-01

    A survey of pesticide residues in 116 imported tea samples on the Tokyo market from April 1992 to March 2010 was carried out. Twenty-two kinds of pesticides, including organophosphorus, organochlorine, pyrethroid and others, were detected at levels between trace (below 0.01 ppm) and 4.0 ppm in 76 samples. The rate of detection was 90% in non-fermented tea, 89% in semi-fermented tea, and 49% in fermented tea. Organophosphorus pesticide was not detected in puer tea, which is fermented with bacteria. The pesticide residues tended to be decreased by a fermentation process. However, organochlorine and pyrethroid pesticides appeared to be chemically stable, so they were still detected in fermented teas. Residue levels of these pesticides were calculated as less than 1% of ADI, except for ethion (45% of ADI) based on the daily intake of tea. Therefore, these teas should be safe when drunk in customary amounts. PMID:23863368

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

    International Nuclear Information System (INIS)

    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 sts. 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, ? -HCH, DDT, aldrin, dieldrin, DDE, endosulfan sulphate, ?-chlordane, endrin and ?-HCH were detected in fish, water and sediment samples. Aldrin and dieldrin levels detected were above the recommended limit of 0.03 ?L-1 with endosulfan, endrin and chlordane registering levels above their recommended limits of 20.0?L-1 and 0.2 ?L-1 respectively for drinking water. Pesticide residues in fish samples varied between 0.10 ?gKg-1 to 30.90 ?gKg-1. The highest level was detected in Hepsetus odoe (HO-N). Contamination pattern of pesticide residues in fish samples was generally in the order of p'p'-DDE > heptachlor > ?- HCH > p'p'-DDT > endosulfan Sulphate > ?-endosulfan > ?- HCH > ?-chlordane > dieldrin > endrin ketone > methoxychlor > endrin > aldrin > endrin aldehyde. Data obtained from the field survey regarding safe use of pesticides, toxicity awareness and symptoms among farmers indicated that a very high proportion of farmers were at high risk of pesticide poisoning from occupational exposure. More than 90% of farm workers did not practice safety precaution during pesticide formulation and application leading to considerable prevalence of pesticide related illness in this agricultural community. The presence of pesticide residues in fish was of further concern because fish is the main protein diet for humans in the basin. The estimated dose for aldrin, methoxychlor, ?-chlordane, endrin aldehyde, endrin ketone, endrin, p'p'-DDT and ?-HCH do not pose a direct hazard to human health, although present in fish samples since the values registered were lower than the reference doses. However, ?- HCH, heptachlor, ?-endosulfan, endosulfan sulphate, p'p'-DDE and dieldrin levels exceeded the reference dose, indicating a great potential for systemic toxicity in children who are considered to be the most vulnerable population subgroup. In children, between the ages of 0 - 1year, the hazard indices of 2.64, 1.720, 1.736 and 0.792 were computed for ?-endosulfan, heptachlor, endosulfan sulphate and dieldrin respectively while for children between the ages 1 -11years, hazard indices for heptachlor, ?-endosu

  16. Health risk assessment of pesticides residue in maize and cowpea from Ejura, Ghana.

    Science.gov (United States)

    Akoto, O; Andoh, H; Darko, G; Eshun, K; Osei-Fosu, P

    2013-06-01

    Low productivity in agriculture due to damage cause by pests has led to the application of pesticides to control pest infestation. Residues of pesticides applied on crops are often found in the food which can cause chronic effect on the health of humans who consume such products. The aim of this study is to measure pesticides residues in maize and cowpea and compare the values with stablished safety limits. A total of 37 pesticides comprising 15 organochlorines, 13 organophosphorus and 9 pyrethroids pesticides were identified in maize and cowpea samples obtained from farms in Ejura. Analytical methods included solvent extraction of the pesticide residues and their subsequent quantification using gas chromatograph equipped with Electron Capture Detector and Pulse Flame Photometric Detector after clean-up on alumina/activated charcoal column. The results showed that the mean concentration of pesticides in maize ranged from 0.001 to 0.103 mg kg(-1) for organochlorine pesticides, 0.002-0.019 mg kg(-1) for organophosphorus pesticides and 0.002-0.028 mg kg(-1) for pyrethroids pesticides. In cowpea the mean concentration ranged from 0.001 to 0.108 mg kg(-1) for organochlorine pesticides, 0.002-0.015 mg kg(-1) for organophosphorus pesticides and 0.001-0.039 mg kg(-1) for pyrethroids pesticides. Maximum Residue Limits for ?-HCH, ?-endosulfan, p,p'-DDE and p,p'-DDD were exceeded in both maize and cowpea samples. Health risk estimation revealed that residues of heptachlor, dieldrin, endrin, ?-endosulfna, ?-chlordane and chlorfenvinphos found in maize exceeded the Acceptable Daily Intake. Similarly the levels of heptachlor and p,p'-DDD found in cowpea also exceeded the Acceptable Daily Intake. This suggests a great potential for chronic toxicity to consumers of these food items. PMID:23557726

  17. Pesticide Residues in Conventional, IPM-grown and Organic Foods: Insights from Three U.S. Data Sets

    Science.gov (United States)

    Baker, Brian P., 1958-

    The above mentioned report by Brian P. Baker, Charles M. Benbrook, Edward Groth III, and Karen Lutz Benbrook was published in the May 2002 edition of Food Additives and Contaminants, Volume 19, No. 5. The Consumers Union (an independent nonprofit testing, educational, and information organization) has released a summary of this report for Internet viewers. According to the Consumer Union (CU), this report is the first detailed analysis of pesticide residue data in foods grown organically and conventionally. The report reveals that consumers who purchase organic fruits and vegetables are exposed to only one-third as many residues as in conventionally grown foods. The authors gathered and analyzed test data on pesticide residues in organic and non-organic foods from three independent sources: tests done on selected foods by CU in 1997; surveys of residues in foods in the US market conducted by the Pesticide Data Program of the US Department of Agriculture in 1994 through 1999; and surveys of residues in foods sold in California, tested by the California Department of Pesticide Regulation in 1989 through 1998. The combined residue data sets covered more than 94,000 food samples from more than 20 different crops of which 1,291 were organically grown. A complete copy of the paper may be purchased from the publishers of Food Additives and Contaminants.

  18. [Survey of pesticide residues in imported fruit products (1994.4-2006.3)].

    Science.gov (United States)

    Kobayash, Maki; Ohtsuka, Kenji; Tamura, Yasuhiro; Tomizawa, Sanae; Sakai, Naoko; Kamijo, Kyoko; Kageyama, Yuriko; Takano, Ichiro; Nagayama, Toshihiro

    2009-10-01

    A survey of pesticide residues in 600 imported fruit products on the Tokyo market from April 1994 to March 2006 was carried out. Thirty kinds of pesticides, including organophosphorus, organochlorine, carbamate, and pyrethroid, were detected between levels of Tr (below 0.01 ppm) to 0.37 ppm from 75 samples. Residual pesticides were detected from fruit products, dried fruits and pressed juice. A high frequency of pesticide residues was observed in peels, whole body of fruits and products which contained them. Residue levels of these pesticides were calculated as between less than 0.1 and 3.9% of their ADI values according to the daily intake of fruit products. Therefore, these fruit products should be safe when eaten in customary amounts. PMID:19897954

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

    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.

  1. Pesticide residues in fruits and vegetables from the Aegean region, Turkey.

    Science.gov (United States)

    Bak?rc?, Gözde Türköz; Yaman Acay, Dilek Bengü; Bak?rc?, Fatih; Ötle?, Semih

    2014-10-01

    The purpose of this study was to investigate pesticide residues in fruits and vegetables from the Aegean region of Turkey. A total of 1423 samples of fresh fruit and vegetables were collected from 2010 to 2012. The samples were analysed to determine the concentrations of 186 pesticide residues. The analyses utilized ultrahigh performance liquid chromatography coupled with tandem mass spectrometry (UPLC/MS/MS) and gas chromatography with an electron capture detector (GC-ECD) confirmed by gas chromatography with mass spectrometry (GC-MS) after a multi-residue extraction procedure (the QuEChERS method). The results were evaluated according to maximum residue limits (MRLs) for each commodity and pesticide by Turkish Regulation. All pomegranate, cauliflower and cabbage samples were pesticides-free. A total of 754 samples contained detectable residues at or below MRLs, and 48 (8.4%) of the fruit samples and 83 (9.8%) of the vegetable samples contained pesticide residues above MRLs. MRL values were most often exceeded in arugula, cucumber, lemon, and grape commodities. All detected pesticides in apricot, carrot, kiwifruit and leek were below the MRLs. Acetamiprid, chlorpyriphos and carbendazim were the most detected pesticide residues. PMID:24799252

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

    OpenAIRE

    Mol, J. G. J.; Rooseboom, A.; Dam, 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) injection. The same extract, before clean-up and after a change of solvent, was also analyzed by liquid chromatography with tandem mass spectrometry (LC¿MS¿MS). All aspects related to sample preparati...

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Science.gov (United States)

    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

  5. Pesticide residue legal standards for beverages: risk regulation and public perception

    DEFF Research Database (Denmark)

    Grieger, Khara Deanne; Trapp, Stefan

    2007-01-01

    Exposure to pesticide residues in dietary sources is a major concern of Europeans. Meanwhile, drinking water and food safety authorities establish and implement maximum residue levels (MRLs) for pesticides in drinking water and food. This study compares MRLs between EU, US and Codex authorities for both drinking water and other beverages, i.e. milk, juice and wine, investigating differences between authorites as well as between beverage types. These results were confronted with public perceptions towards pesticide residues in beverages, based on a consumer survey conducted in Copenhagen, Denmark. Seven frequently-occurring pesticides were selected for this study. Results show that since no specific MRLs for juice and wine exist, MRLs for the raw products were used instead. Furthermore, established MRLs are significantly greater for pesticides in beverages when compared to legal standards for drinking water. Maximum levels in drinking water, if available, are generally low (0.0001 mg/L in the EU), while MRLs for pesticides in milk, juice and wine range from 0.05 to 60 mg/L. At the same time, questionnaire participants were equally concerned about their exposure to pesticide residues in drinking water and other beverage types. These findings reveal some inconsistencies in setting legal maximum concentrations for pesticide residues in different dietary sources as well as between different drinking water and food safety authorities.

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

    International Nuclear Information System (INIS)

    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)

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

    Directory of Open Access Journals (Sweden)

    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 (?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 ?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 ?g g-1 in analyzed fruits were above 90% with relative standard deviations (RSD less than 6

  8. Limitations in the determination of maximum residue limits and highest residues of pesticides: Part I.

    Science.gov (United States)

    Horváth, Zsuzsanna; Sali, Judit; Zentai, Andrea; Dorogházi, Enik?; Farkas, Zsuzsa; Kerekes, Kata; Ambrus, Árpád

    2014-01-01

    The pesticide usages are controlled by comparing residue concentrations in treated commodities to legally permitted maximum levels (MRLs) determined based on supervised trials designed to reflect likely maximum residues occurring in practice following authorised use. The number of trials available may significantly affect the accuracy of estimated maximum residues. We conducted a study with synthetic lognormal distributions with mean of 1 and standard deviations of 0.8 and 1.0, which reflect the residue distributions observed in practice. The likely residues in samples were modelled by drawing random samples of size 3, 5, 10 and 25 from the synthetic populations. The results indicate that the estimations of highest residues (HR), used for calculation of short-term intake, and the MRLs, serving as legal limits, are very uncertain based on 3-5 trials indicated by the calculated HR0.975/HR0.025 and MRL0.975/MRL0.025 ratios of 12 and 9, and 13 and 10, respectively, which question the suitability of such trials for the intended purpose. As the 95% range of HR and MRL rapidly decreases with number of trials, ideally ?15 but minimum 6-8 trials should be used for estimation of HR and MRL according to the current typical practice of Codex Alimentarius. PMID:24380614

  9. 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.

    Science.gov (United States)

    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

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

    Science.gov (United States)

    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, ?-endosulfan, ?-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 ?g l(-1) in water for isoprothiolane and up to 521 ?g kg(-1) dm in sediment for buprofezin. Annual average concentrations ranged up to 3.34 ?g l(-1) in water and up to 135 ?g 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

  11. Preparation of mesoporous ZrO2-coated magnetic microsphere and its application in the multi-residue analysis of pesticides and PCBs in fish by GC-MS/MS.

    Science.gov (United States)

    Peng, Xi-Tian; Jiang, Li; Gong, Yan; Hu, Xi-Zhou; Peng, Li-Jun; Feng, Yu-Qi

    2015-01-01

    A novel mesoporous ZrO2 immobilized magnetic Fe3O4 microsphere (m-ZrO2@Fe3O4) was successfully synthesized and characterized by transmission electron microscope (TEM), X-ray diffractometer (XRD), nitrogen adsorption measurement (NAM), energy-dispersive X-ray analysis (EDX), vibrating sample magnetometer (VSM). Then the resultant m-ZrO2@Fe3O4 and an n-octadecylphosphonic acid modified magnetic microsphere (Fe3O4-OPA) were employed as clean-up co-adsorbents of QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) method for the analysis of 42 pesticides and 7 polychlorinated biphenyls (PCBs) in fish samples. Lipid co-extractives such as fatty acids in QuEChERS extracts could be efficiently removed through the Lewis acid-Lewis base interaction between m-ZrO2@Fe3O4 and carboxylic groups, while some other apolar interferents could be adsorbed through hydrophobic interaction by Fe3O4-OPA. Meanwhile, the magnetic property of adsorbents endows the clean-up procedure with manipulative convenience. Several parameters affecting the clean-up performance were investigated. Under the optimal conditions, the modified QuEChERS method combined with gas chromatography-tandem mass spectrometry (GC-MS/MS) for the multi-class, multi-residue analysis of pesticides and PCBs in fish samples was validated according to linearility, recovery and precision. Good linearities were obtained for all analytes with R(2) larger than 0.9903. Limits of detection (LODs) were found to be in the range of 0.02-4.40 ng/g. The method recoveries of all analytes spiked at three concentration levels in blank fish samples were from 69.8% to 117.1%, with the intra-day and inter-day relative standard deviations (RSDs) less than 13.4% and 16.5%, respectively. PMID:25476287

  12. Gas chromatographic determination of pesticide residues in white mustard.

    Science.gov (United States)

    S?owik-Borowiec, Magdalena; Szpyrka, Ewa; Walorczyk, Stanis?aw

    2015-04-15

    A new analytical method employing gas chromatography coupled to electron capture and nitrogen phosphorus detection (GC-ECD/NPD) has been developed and validated for the screening and quantification of 51 pesticides in a matrix of high chlorophyll content - white mustard (Sinapis alba L.). For preparation of the sample extract, the citrate buffered QuEChERS procedure was followed. However certain changes were made to adapt the method to our needs and available laboratory resources. The sample size was reduced to 5 g, 10 mL water was added and exchange of solvent before GC analysis was done. The samples spiked with the target pesticides at the concentration level 0.01 mg/kg and a higher level (depending on the compound) yielded average recoveries in the range of 70-120% with relative standard deviations (RSDs) 0-19% except for HCB, S-metolachlor and teflubenzuron, and displayed very good linearity (R(2)>0.99) for nearly all the analytes. Limit of quantification was 0.01 mg/kg for the majority of the analytes. The expanded measurement uncertainties were estimated employing a "top-down" empirical model as being between 6% and 32% and yielding an average value of 18% (coverage factor k=2, confidence level 95%). PMID:25466117

  13. Effect of Cooking Process on the Residues of Three Carbamate Pesticides in Rice

    OpenAIRE

    Shoeibi, Shahram; Amirahmadi, Maryam; Yazdanpanah, Hassan; Pirali-hamedani, Morteza; Pakzad, Saied Reza; Kobarfard, Farzad

    2011-01-01

    A gas chromatography mass spectrometry with spike calibration curve method was used to quantify three carbamate pesticides residue in cooked white rice and to estimate the reduction percentage of the cooking process duration.

  14. 40 CFR 158.2040 - Biochemical pesticides residue data requirements table.

    Science.gov (United States)

    2010-07-01

    ...biochemical pesticides product chemistry and are in the last...section. 1. Residue chemistry data requirements...biochemical product chemistry data requirements...premises, to livestock drinking water, or to crops used...

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

    OpenAIRE

    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...

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

    International Nuclear Information System (INIS)

    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)

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

    Directory of Open Access Journals (Sweden)

    Maryam Amirahmadi

    2013-01-01

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

  18. Measurement Residue of Two Current Used Pesticides (Endosulfan and Fosalon in Colorado Potato Beetle Control

    Directory of Open Access Journals (Sweden)

    2007-01-01

    Full Text Available In our country high amount of insecticides are been consumed to fight agricultural pest that can severely contaminate environment and arable crops. Phosphoric and chlorine toxins, are from important one`s for high toxicity and long-term persistence in the environment, respectively. These toxins directly or indirectly enter environment and enter crops and through it enter nutrition cycle of organisms. Determining of these toxins residue consistency and comparing with world standards will help us in management of correct use of pesticides. In present research effects of different consistency of toxin and crop-dusting time on the rest of two toxins [Endosulfan (Thiodan and Fosalon (Zolone] that frequently used in control of Colorado potato beetle were been evaluated. The procedure includes sampling stage, condensation, concentrating and analysis. Analysis was been performed by GC machine and FTD, ECD detectors. According to result, it is specified that using of different consistency with applying of different consistency, residue of these toxins weren`t higher than standard, again it is specified that residue of Fosalon was more than Endosulfan. Results showed that there was no meaningful difference between different consistencies and different using time, from the viewpoint of residue of toxins. Sampling with one month interval showed that with lapse of time toxin`s residue has been reduced as 0.008 PPM.

  19. The Concept of Withholding Period and Pesticide Residue in Grain Storage

    Directory of Open Access Journals (Sweden)

    Adegbola, J. A.

    2012-12-01

    Full Text Available This review focuses on pesticides, their unquantifiable benefits to agriculture, pesticide residue, maximum pesticide residue limit, and withholding period in grain storage. It delved into the origin of synthetic pesticide and its introduction to Nigeria in the 1950s, it maintained that pesticide have posed major health and social challenges, and have had negative, unintended, catastrophic, fatal consequences to man, animals, and even the environment especially when instructions on their labels are not adhered to. Again, it maintained that withholding periods are often stipulated on the labels of genuine pesticides, it reiterated that not adhering to the stipulated withholding period can have catastrophic consequences on consumers of grain and grain products. Furthermore, it dwelt on the activities of Nigerian stored Products Research Institute (NSPRI and National Food Drug Administration and Control (NAFDAC, their mandates and quest to nip pesticide poisoning in the bud. Finally, recommendations were put forward to check the seeming ignorance and dearth of information about pesticide residue limit and withholding period, and dangers that are concomitants of not adhering to these.

  20. Identification of the main pesticide residue mixtures to which the French population is exposed.

    Science.gov (United States)

    Crépet, A; Tressou, J; Graillot, V; Béchaux, C; Pierlot, S; Héraud, F; Leblanc, J Ch

    2013-10-01

    Owing to the intensive use of pesticides and their potential persistence in the environment, various pesticide residues can be found in the diet. Consumers are therefore exposed to complex pesticide mixtures which may have combined adverse effects on human health. By modelling food exposure to multiple pesticides, this paper aims to determine the main mixtures to which the general population is exposed in France. Dietary exposure of 3337 individuals from the INCA2 French national consumption survey was assessed for 79 pesticide residues, based on results of the 2006 French food monitoring programmes. Individuals were divided into groups with similar patterns of co-exposure using the clustering ability of a Bayesian nonparametric model. In the 5 groups of individuals with the highest exposure, mixtures are formed by pairs of pesticides with correlations above 0.7. Seven mixtures of 2-6 pesticides each were characterised. We identified the commodities that contributed the most to exposure. Pesticide mixtures can either be components of a single plant protection product applied together on the same crop or be from separate products that are consumed together during a meal. Of the 25 pesticides forming the mixtures, two--DDT and Dieldrin--are known persistent organic pollutants. The approach developed is generic and can be applied to all types of substances found in the diet in order to characterise the mixtures that should be studied first because of their adverse effects on health. PMID:23777638

  1. [Residual pesticide concentrations after processing various types of tea and tea infusions].

    Science.gov (United States)

    Kondo, Takahide; Watanabe, Ayaka; Shitara, Hiroshi; Kaburagi, Yasuo; Shibata, Masahisa; Kanda, Noriko; Kurokawa, Chieko; Inoue, Yutaka; Miyazaki, Motonobu; Togawa, Masayuki; Ozawa, Akihito; Uchiyama, Toru; Koizumi, Yutaka; Nakamura, Yoriyuki; Masuda, Shuichi; Maitani, Tamio

    2013-01-01

    The effects of processing to produce various types of tea or infusion on the levels of pesticide residues in tea were investigated for three insecticides (chlorfenapyr, pyrimiphos-methyl, and clothianidin). Tea plants were sprayed with one of the three pesticides and cultivated under cover. The levels of pesticide residues in tea decreased after processing according to the time and temperature of heating, as well as fermentation. Although significant differences were not observed among the three pesticides in the ratio of decreased of pesticide concentration after processing to green tea, clothianidin, which is a neonicotinoid insecticide and has a lower log Pow value, tended to be transferred more than the other two insecticides into infusions. However, no significant difference in the ratios of clothianidin transferred to infusions was observed among green tea with three different leaf sizes. PMID:24025203

  2. Pesticide residue levels in soils and crops from 37 states, 1972--National Soils Monitoring Program (IV).

    Science.gov (United States)

    Carey, A E; Gowen, J A; Tai, H; Mitchell, W G; Wiersma, G B

    1979-03-01

    Residue data from the 1972 (FY--73) National Soils Monitoring Program are summarized. Composite samples of agricultural soil and mature crops were collected from 1,483 of the 1,533 selected 4-hectare sites in 37 states. Analyses were performed for organochlorine and organophosphorus compounds, trifluralin and polychlorinated biphenyls (PCBs); analysis for atrazine was performed only when pesticide application data indicated current-year use. Organochlorine pesticides were detected in 45 percent of the soil samples. The most frequently detected compound was dieldrin, found in 27 percent of all soil samples. Other compounds detected, in order of frequency, included DDT, aldrin, chlordane, and heptachlor epoxide, found, respectively, in 21, 9, 8, and 7 percent of all soil samples. Crop samples were collected from 727 sites. All were analyzed for organochlorines; analyses were performed for organophosphates and atrazine only when pesticide application data indicated current-year use. For all crops, 40 percent of the samples contained detectable levels of organochlorines and 10 percent contained detectable levels of organophosphates. Atrazine was not detected. PMID:461116

  3. 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

    International Nuclear Information System (INIS)

    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 deviith 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.

  4. 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

    Energy Technology Data Exchange (ETDEWEB)

    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 from the market.

  5. [Survey of pesticide residues in imported spices and herbs (1997.4-2011.3)].

    Science.gov (United States)

    Kobayashi, Maki; Ohtsuka, Kenji; Tamura, Yasuhiro; Tomizawa, Sanae; Kinoshita, Teruaki; Kamijo, Kyoko; Iwakoshi, Keiko; Sato, Chizuko; Nagayama, Toshihiro; Takano, Ichiro

    2013-01-01

    A survey of pesticide residues in 313 samples of imported spices and herbs on the Tokyo market from April 1997 to March 2011 was carried out. Thirty-seven kinds of pesticides, including organophosphorus, organochlorine, pyrethroid, carbamate and others, were detected between levels of trace (below 0.01 ppm) and 3.3 ppm from 64 samples. The rate of detection was highest in peel (100%) followed by stem (66.7%), fruit (34.5%), bark (33.3%), flower (31.3%) and leaf (14.7%). No residues were detected in root, seed or whole grass. Organochlorine pesticides were detected in all plant parts. The insecticides were detected in products from all production areas, suggesting that their use is common. Residue levels of these pesticides were calculated as less than 1% of their ADI values, based on the daily intake of spices and herbs. Therefore, these spices and herbs should be safe when consumed in customary amounts. PMID:24025211

  6. Monitoring of pesticide residues levels in fresh vegetable form Heibei Province, North China.

    Science.gov (United States)

    Li, Weihao; Tai, Lingyu; Liu, Jianxia; Gai, Zikuan; Ding, Guotao

    2014-10-01

    In this study, 226 samples of seven types of domestic vegetables collected from several vegetable-growing regions in Hebei Province of China were tested for the presence of 38 different agricultural pesticides using a gas chromatograph equipped with electron capture and nitrogen phosphorus detectors. The aim of this study was to investigate the distribution of pesticides in main vegetables from Hebei Province. Results showed that, in 65.93% of the samples, no residues were found, 31.42% of the samples contained pesticide residues at or below the maximum residue levels (MRLs), and 2.65% of the samples contained pesticide residues above MRL. The most frequently detected pesticides were acephate (31), followed by cyhalothrin (15), bifenthrin (8), omethoate (6), isazophos (6), dimethoate (5), chlorpyrifos (2), and malathion (1). Some (1.33%) of the samples contained multiple residues. The results provide useful information on the current contamination status of a key agricultural area in North China, and points to the continuous monitoring and strict regulation of pesticide use on vegetables are necessary. PMID:24869955

  7. Determination of pesticide residue in selected fruits and vegetable

    International Nuclear Information System (INIS)

    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)

  8. Potential Transport and Degradation of “Aged” Pesticide Residues in Soil

    Science.gov (United States)

    Increased pesticide residence time in soil, or “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 coefficie...

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

    Science.gov (United States)

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

    2014-01-01

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

  10. [Identification of pesticide residues in common fruits and vegetables by gas chromatography-quadrupole time-of-flight mass spectrometry].

    Science.gov (United States)

    Li, Xiaoying; Zhang, Hongyi; Chang, Qiaoying; Fan, Chunlin; Spang, Guofang; Cao, Zhe; Wang, Wenwen

    2014-03-01

    A new screening method was developed for the determination of 152 pesticide multi-residues in different chemical species with a Carbon NH2 column using solid-phase extraction (SPE) coupled with gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF MS). In the first stage (MS1) accurate mass database, up to three-five ions of the pesticides were monitored. The presence of at least three ions and the accomplishment of the intensity ratio (Q/q(i)) within the established tolerances were used as the confirmation of intensity criteria. The pesticides which have less characteristic ions or the peaks of the characteristic ions detected were up the tolerance were determined in the second stage (MS2) and the spectral difference was evaluated using MS2 library for the identified. Cabbage, tomato, pear were selected as typical fruits and vegetables to spike and detected all the 152 pesticides at two concentration levels of 5.0 and 10.0 microg/kg. The recoveries in the range of 70%-120% at two concentration levels were 91.45% and 94.08% for cabbage, 88.20% and 88.80% for tomato, 86.84% and 92.10% for pear respectively. Using the established 152 pesticide MS2 library some suspected pesticides were identified, and at the same time the analysis scope was expanded. PMID:24984467

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

    International Nuclear Information System (INIS)

    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 reseaced 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

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

    Directory of Open Access Journals (Sweden)

    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.

  13. Pesticides residues in okra (non-target crop) grown close to a watermelon farm in Ghana.

    Science.gov (United States)

    Essumang, D K; Asare, E A; Dodoo, D K

    2013-09-01

    The study looked at the levels of pesticides in okra grown close to a watermelon farm herein referred to as a non-target crop. The watermelon received some pesticide application in the course of its cultivation, and the okra which was not meant to be sprayed was also affected by the pesticide. About 500 okra samples were collected for a period of 6 weeks and pesticides extracted with 1:1 n-hexane and dichloromethane which was analysed with Agilent 2222 GC/MS coupled with 389 auto-sampler. The results confirmed accumulation of significant levels of pesticides in the non-target crop (okra grown close to watermelon farm). Levels of organochlorine pesticides ranged from 3.10 to 7.60 ?g/kg whilst the organophosphorus pesticides had levels ranging from 2.80 to 2016.80 ?g/kg. The synthetic pyrethroid pesticide mean levels also ranged from 0.10 to 4.10 ?g/kg and were below World Health Organization/Food and Agriculture Organization-recommended residue levels, and though not appearing to constitute a grave threat to life, their occurrence is a concern, and pre-emptive techniques must be developed to thwart the contaminations. Though the non- target crop was not treated directly with the pesticides, some level of contamination with organochlorine and organophosphorus pesticides persisted in the crops. It can be inferred that application of pesticides affected the adjoining crops, meaning that inter-cropping and mix-cropping might not be acceptable when one of the crops requires pesticide application. It is important for the farmers to be trained to ensure proper application of pesticide to minimise its impact on the health of consumers. PMID:23404549

  14. 77 FR 42433 - Difenoconazole; Pesticide Tolerances

    Science.gov (United States)

    2012-07-19

    ...food-use pesticide, if a toxicological...CSFII). As to residue levels in food...unrefined acute analysis for food and...of pesticide residues in food and...actual levels of pesticide residues that have been...dietary exposure analysis and risk...

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

    Directory of Open Access Journals (Sweden)

    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 ?-HCH, ?-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.

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

    Directory of Open Access Journals (Sweden)

    D.K. Essumang

    2009-04-01

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

  17. Organophosphorus pesticide residues in milled rice (Oryza sativa) on the Chinese market and dietary risk assessment.

    Science.gov (United States)

    Chen, Chen; Li, Yun; Chen, Mingxue; Chen, Zhijun; Qian, Yongzhong

    2009-03-01

    The present study investigates the occurrence of acetylcholinesterase (AChE)-inhibiting organophosphorus (OP) pesticide residues in milled rice samples obtained form local markets in China during the period 2004-2006 and estimates their cumulative exposure. Concentrations of OP pesticides were determined by gas chromatography with flame photometric detection (GC-FPD). The results showed that 9.3% of the samples contained detectable residues of at least one of the seven target OP pesticides (chlorpyrifos, dichlorvos, omethoate, methamidophos, parathion-methyl, parathion and triazophos) mainly used for agriculture in China, with concentrations ranging 0.011-1.756 mg kg(-1). Rice consumption data was obtained from an individual food consumption survey. Relative potency factors (RPFs) for each pesticide were calculated with methamidophos as the index compound (IC), using 1- or 2-year chronic non-observed adverse effect levels (NOAEL) for AChE inhibition, mostly in rat brain, obtained from international evaluations of pesticides. Exposure to AChE-inhibiting pesticides for the population above 7 years old at P99.9 represented 52-94.5% of the acceptable daily intake (ADI) expressed as methamidophos. Estimated exposure for children aged 2-4 and 4-7 years at P99.9 were 119 and 104.3% of the ADI level, respectively. This study suggests that a yearly monitoring program for OP pesticide residues and strict implementation of the national safety standard for milled rice is necessary. PMID:19680907

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

    International Nuclear Information System (INIS)

    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)

  19. Monitoring of Pesticide Residues in Commonly Used Fruits in Hyderabad Region, Pakistan

    Directory of Open Access Journals (Sweden)

    Yawar Latif

    2011-12-01

    Full Text Available A market based survey was carried out to evaluate the level of 26 pesticides in some commonly used fruits in Hyderabad region, Pakistan. Gas chromatography coupled with micro electron capture detector was used to assess the levels of pesticide residues. Gas chromatography-mass spectrometry (GC-MS was also applied for the confirmation of results. Out of total 131 analyzed samples, 53 (40% were found contaminated with pesticide residues while only 3 (2% samples were exceeded the MRLs of some pesticides. Chlorpyrifos and dieldrin were detected in almost all analyzed samples. Residues of chlorpyrifos (1256 µg/kg and endosulfan sulfate (1236 µg/kg were found higher in orange and apple samples, respectively. The findings of this study provided important data about contamination of pesticide residue in some fruits sold in Hyderabad, Pakistan, and recommended that monitoring studies should be expanded to other fruits grown in different agro climatic regions, which may serve as basis for future policy about the standards and quality control of pesticides.

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

    Directory of Open Access Journals (Sweden)

    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.

  1. Recent Advances in the Synthesis of Artificial Antigen and Its Application in the Detection of Pesticide Residue

    Directory of Open Access Journals (Sweden)

    Tong Dewen

    2007-01-01

    Full Text Available Recent advances in the research of artificial antigen have shown that artificial antigens can be valuable approach for the treatment of some diseases as well as the detection of pesticide residues. By directly/indirectly coupling hapten to an appropriated carrier (macromolecule, artificial antigen can induce animals to produce hapten-specific antibody. Based on this principle, various vaccines have been developed. More impotently, new analytical method, immunological analysis has also been established. Comparing the conventional technologies, such as chromatographic methods, this promising method offers an alternative with high specificity, sensitivity, simplicity and suitability for the analysis of a large number of samples in a short period of time. In this review, we describe the recent advances in the synthesis of artificial antigen and its application in the detection of pesticide residues.

  2. 77 FR 59106 - Glufosinate Ammonium; Pesticide Tolerances

    Science.gov (United States)

    2012-09-26

    ...chronic dietary analysis for crops that...Anticipated residue and percent crop...residue levels of pesticide residues in food...tolerance-level residues. The chronic dietary exposure analysis was performed using anticipated residues from field trial...chronic dietary pesticide exposures...

  3. Development of a multi-residue enantiomeric analysis method for 9 pesticides in soil and water by chiral liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Li, Yuanbo; Dong, Fengshou; Liu, Xingang; Xu, Jun; Chen, Xiu; Han, Yongtao; Liang, Xuyang; Zheng, Yongquan

    2013-04-15

    A novel and sensitive chiral liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method was developed and validated for simultaneous measuring individual enantiomers of 9 pesticides including herbicides, insecticides, and fungicides in soil and water. The separation and determination were performed using reversed-phase chromatography on an amylose chiral stationary phase, a Chiralpak AD-RH column, under gradient elution using a mixture of ACN-2mM ammonium acetate in water as the mobile phase at 0.45 mL/min flow rate. The effects of three cellulose-based columns and three amylose-based columns on the separation were also investigated. The QuEChERS (acronym for Quick, Easy, Cheap, Effective, Rugged and Safe) method and solid-phase extraction (SPE) were used for the extraction and clean-up of the soil and water samples, respectively. Parameters including the matrix effect, linearity, precision, accuracy and stability were undertaken. Under optimal conditions, the mean recoveries for all enantiomers from the soil and water samples were ranged from 77.8% to 106.2% with the relative standard deviations (RSD) less than 14.2%. Good linearity (at least R(2) ? 0.9986) was obtained for all studied analytes in the soil and water matrix calibration curves over the range from 2.0 to 125 ?g/L. The limits of detection (LOD) for all enantiomers in the soil and water were less than 1.8 ?g/kg or ?g/L, whereas the limit of quantification (LOQ) did not exceed 5.0 ?g/kg or ?g/L. The results of the method validation confirm that this proposed method is convenient and reliable for the enantioselective determination of the enantiomers of 9 chiral pesticides in soil and water. PMID:23434475

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

    Science.gov (United States)

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

    2014-06-15

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

  5. Recent Advances in the Synthesis of Artificial Antigen and Its Application in the Detection of Pesticide Residue

    OpenAIRE

    Tong Dewen; Hesheng Yang; Wang Jinyi

    2007-01-01

    Recent advances in the research of artificial antigen have shown that artificial antigens can be valuable approach for the treatment of some diseases as well as the detection of pesticide residues. By directly/indirectly coupling hapten to an appropriated carrier (macromolecule), artificial antigen can induce animals to produce hapten-specific antibody. Based on this principle, various vaccines have been developed. More impotently, new analytical method, immunological analysis has also been e...

  6. Pesticide and plasticizer residues in citrus essential oils from different countries.

    Science.gov (United States)

    Di Bella, Giuseppa; Lo Turco, Vincenzo; Rando, Rossana; Arena, Gabriella; Pollicino, Donatella; Luppino, Rosario Rocco; Dugo, Giacomo

    2010-08-01

    Residue analyses are very important in the quality control of citrus essential oils. Organophosphorus and organochlorine pesticides, phosphorated plasticizers and chloroparaffins contamination were investigated by HRGC with FPD and ECD detectors in 120 citrus essential oils produced in Italy and in 70 from other countries in the crop year 2006-2007. Results showed that the largest pesticide quantities were found in oils from Brazil and Spain. The presence of such residues might be the result of an improper use of pesticide in citrus growing or of previous contamination of the extractors. However, the pesticide levels showed a measurable decrease in relation to past production years. The absence of phosporated plasticizers and chloroparaffins can be the result of either improvement of the procedures used during the production cycle or in the storage of the essential oils compared with previous years. PMID:20839646

  7. [Survey of pesticide residues in imported frozen vegetables and fruits (1989.4~2008.3)].

    Science.gov (United States)

    Kobayashi, Maki; Ohtsuka, Kenji; Tamura, Yasuhiro; Tomizawa, Sanae; Kamijo, Kyoko; Iwakoshi, Keiko; Kageyama, Yuriko; Nagayama, Toshihiro; Takano, Ichiro

    2011-01-01

    A survey of pesticide residues in 595 imported frozen products on the Tokyo market from April 1989 to March 2008 was carried out. Forty three kinds of pesticides, including organophosphorus, organochlorine, carbamate, pyrethroid and others, were detected between levels of trace (below 0.01 ppm) and 4.6 ppm from 162 samples. Chlorpyrifos, cypermethrin and omethoate were frequently detected in green vegetables (komatsuna leaf and spinach), cypermethrin and methamidophos were detected in pods and seeds (green soybean and string pea), chlorpropham (CIPC) was detected in potato, and captan and carbaryl were detected in berries (blueberry, raspberry and strawberry). The hydrophilic pesticide methamidophos was detected in flesh of lychee. Residue levels of these pesticides were calculated as between less than 0.5% and 30% of their ADI values according to the daily intake of frozen products. Therefore, these frozen products should be safe when they were eaten in customary amounts. PMID:21515967

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

    International Nuclear Information System (INIS)

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

  9. Residual Component Analysis

    OpenAIRE

    Kalaitzis, Alfredo A.; Lawrence, Neil D.

    2011-01-01

    Probabilistic principal component analysis (PPCA) seeks a low dimensional representation of a data set in the presence of independent spherical Gaussian noise, Sigma = (sigma^2)*I. The maximum likelihood solution for the model is an eigenvalue problem on the sample covariance matrix. In this paper we consider the situation where the data variance is already partially explained by other factors, e.g. covariates of interest, or temporal correlations leaving some residual varia...

  10. Organochlorine Pesticides Residues in Soil of Cocoa Farms in Ondo State Central District, Nigeria

    OpenAIRE

    Aiyesanmi, Ademola F.; Idowu, Gideon A.

    2012-01-01

    Ondo State being the highest producer of Cocoa in Nigeria constitutes the most probable area with the highest use of chemical pesticides to enhance cocoa production. As effective as these chemicals may be in achieving this goal, the incidence of their residues on non-targeted substances and the total environment, with the attendant adverse effects have being of serious concerns. Our objective in this paper is to assess contamination of farm soils by organochlorine pesticides applied on cocoa ...

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

    OpenAIRE

    Crentsil Kofi Bempah; Jacob Asomaning; Juliana Boateng

    2012-01-01

    A study was conducted to investigate the organochlorine, organophosphorus and synthetic pyrethroid pesticide residues in fruits and vegetables from markets in Ghana. For this purpose, a total of 309 fruits and vegetable samples, were collected and analyzed by gas chromatography with electron capture detector. The obtained results showed that the predominance of organochlorine followed by organophosphorus and synthetic pyrethroid pesticides in most of the analyzed samples. The detected concent...

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

    International Nuclear Information System (INIS)

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

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

    Science.gov (United States)

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

    2015-03-01

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

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

    Science.gov (United States)

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

    2014-08-01

    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.

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

    Science.gov (United States)

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

    2013-01-01

    The dynamics of pesticide residues in strawberries that involved quantification of pesticide residues in ripe fruits after model treatment was evaluated in repeated field trials conducted over 3 years. Sixteen commercial pesticide formulations in various combinations were employed in applications from 7 to 44 days before harvest. Altogether 21 active ingredients and some of their metabolites were determined in treated strawberries using LC-MS and GC-MS methods. Except for propargite, the concentrations of all active ingredients declined below the respective MRLs (Regulation (EC) No. 396/2005); nevertheless, most of the tested fungicides often persisted above the 0.01 mg kg?¹ limit required by baby food producers to avoid the risk of exceeding the 'baby food limit' established in Commission Directive 2006/141/EC. On the other hand, residues of the majority of tested insecticides, namely spinosad, pymetrozine, deltamethrin, lambda-cyhalothrin and azadirachtin, declined below this limit. PMID:24303788

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

    OpenAIRE

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

    2004-01-01

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

  17. Assessment of sample cleanup and matrix effects in the pesticide residue analysis of foods using postcolumn infusion in liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Kittlaus, Stefan; Schimanke, Julia; Kempe, Guenther; Speer, Karl

    2011-11-18

    Matrix effect profiles can be used to visualize the effect of the sample matrix to the data signals occurring in a chromatogram. In the present study these profiles were generated by postcolumn infusion of a standard pesticide mix with extracts of different food matrices prepared by the QuEChERS method. Complete raw extracts as well as individual clean-up steps were analyzed. This allowed for a detailed comparison of the interferences caused by the matrix effects from various food samples. It also gave an idea about the efficiency of matrix reduction processes. When analyzing the individual clean-up extracts of the QuEChERS method just a slight reduction of matrix effects could be observed from step to step. Matrices causing strong signal effects in the results of the raw extracts also have strong effects after the final clean-up step. Some of the components responsible for the matrix effects show an extremely high retention time. After the injection of extracts from rocket or different types of tea, significant ion suppressions occurred even after rinsing the analytical column for a long time. The experiments have shown that similar matrices can produce different matrix effect profiles. For example, for black teas and green teas significantly different matrix effect profiles were obtained, while the matrix effects of teas within one of these groups were exactly the same. Analogous results could be found for citrus fruits. In order to overcome interfering matrix effects, analytical systems equipped with different electrospray ion sources were tested. Furthermore, profiles of diluted food extracts were generated. Dilution led to a significant decrease in the matrix effects. PMID:21999915

  18. Guidelines for the validation of qualitative multi-residue methods used to detect pesticides in food

    OpenAIRE

    Mol, J. G. J.; Reynolds, S. L.; Fussell, R. J.; Stajnbaher, D.

    2012-01-01

    There is a current trend for many laboratories to develop and use qualitative gas chromatography–mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS) based multi-residue methods (MRMs) in order to greatly increase the number of pesticides that they can target. Before these qualitative MRMs can be used for the monitoring of pesticide residues in food, their fitness-for-purpose needs to be established by initial method validation. This paper sets out to assess the per...

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

    OpenAIRE

    Anita Osei Tutu; P O Yeboah, A. A. Golow

    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,...

  20. Residues of organochlorine pesticides in fruits, vegetables and tubers from Nigerian markets.

    Science.gov (United States)

    Adeyeye, A; Osibanjo, O

    1999-07-01

    Residue levels of organochlorine pesticides have been determined in raw fruits, vegetables and tubers from markets in Nigeria. In the fruits, total HCH, aldrin and total DDT were detected in 77, 38 and 30% of all samples, respectively. In the vegetables, total HCH, HCB, total DDT and aldrin were detected from 95, 53, 50 and 30%, respectively, of all samples. Aldrin + dieldrin, total HCH, and total DDT were detected from 98, 79 and 49%, respectively, of all tuber samples. Other pesticides were below their detection limits. The average levels were generally low and none were above the FAOs maximum residue limits. PMID:10472135

  1. 78 FR 13295 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2013-02-27

    ...filtration and finally analysis by a Liquid Chromotagraphy...LC/ MS/MS) method. Contact: Andrew...filtration and finally analysis by a LC/MS/MS method. Contact: Andrew...limitations in pesticide formulations...no analytical method is needed...

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

    OpenAIRE

    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...

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

    International Nuclear Information System (INIS)

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

  4. Compound specific isotope analysis of organophosphorus pesticides.

    Science.gov (United States)

    Wu, Langping; Yao, Jun; Trebse, Polonca; Zhang, Ning; Richnow, Hans H

    2014-09-01

    Compound-specific isotope analysis (CSIA) has been established as a tool to study the environmental fate of a wide range of contaminants. In this study, CSIA was developed to analyse the stable carbon isotope signatures of the widely used organophosphorus pesticides: dichlorvos, omethoate and dimethoate. The linearity of the GC-C-IRMS system was tested for target pesticides and led to an acceptable isotope composition within the uncertainty of the instrument. In order to assess the accuracy of the developed method, the effect of the evaporation procedure on measured carbon isotope composition (?(13)C) values was studied and showed that concentration by evaporation of solvents had no significant isotope effect. The CSIA was then applied to investigate isotope fractionation of the hydrolysis and photolysis of selected pesticides. The carbon isotope fractionation of tested pesticides was quantified by the Rayleigh model, which revealed a bulk enrichment factor (?) of -0.2±0.1‰ for hydrolysis of dichlorvos, -1.0±0.1‰ and -3.7±1.1‰ for hydrolysis and photolysis of dimethoate respectively. This study is a first step towards the application of CSIA to trace the transport and degradation of organophosphorus pesticides in the environment. PMID:24997952

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

    Science.gov (United States)

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

    2015-03-01

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

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

    OpenAIRE

    Faqir Muhammad, Ijaz Javed

    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 res...

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

    International Nuclear Information System (INIS)

    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 reporte was still lower than levels reported worldwide. For example, at the Gulf of Mexico (range DDT<0.02-454.00 ng/g, dry weight), Arabian Sea (range DDT 7.4-179.1 ng/g), Gulf of Bengal (range DDT<0.22-720.0 ng/g, dry weight) and Colombian Caribbean (range DDT 38.0-266.0 ng/g, dry weight). Being aware of the sensitivity of marine life, especially crustacean to organochlorines and ensuring the sustainability of rice production in the Muda area, continued monitoring of the level of pesticides residues of the coastal water of the Muda granary area should be undertaken, lack of which could be damaging to the marine ecosystem as the compounds are persistent in the environment. (Author)

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

    DEFF Research Database (Denmark)

    Poulsen, Mette Erecius; Hansen, H.K.

    2007-01-01

    The differences in residue pattern between Italy and South Africa, the main exporters of table grapes to the Danish market, were investigated. The results showed no major differences with respect to the number of samples with residues, with residues being found in 54-78% of the samples. Exceedances of the European Union maximum residue limit (MRL) were found in five samples from Italy. A number of samples were rinsed to study the possible reduction of residues. For copper, iprodione, procymidone and dithiocarbamates a significant effect of rinsing was found (20-49% reduction of residues). 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, the exposure were approximately 0.5% for Italian samples and 1% for South African samples.

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

    Directory of Open Access Journals (Sweden)

    Crentsil Kofi Bempah

    2012-12-01

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

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

    Science.gov (United States)

    Stoner, Kimberly A.; Eitzer, Brian D.

    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 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 ?g per bee (range 166,000X), and even among insecticides LD50 values ranged from 0.006 to 59.8 ?g/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 ?g/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. PMID:24143241

  11. Analysis of pesticide residues in fresh peppermint, Mentha piperita L., using the quick easy cheap effective rugged and safe method (QuEChERS) followed by gas chromatography with electron capture and nitrogen phosphorus detection.

    Science.gov (United States)

    S?owik-Borowiec, Magdalena; Szpyrka, Ewa; Walorczyk, Stanis?aw

    2012-09-01

    A new analytical method for the determination of 14 pesticide residues in fresh peppermint was developed based on the QuEChERS sample preparation technique followed by gas chromatography coupled to electron capture and nitrogen phosphorus detectors (GC/ECD/NPD). The validation study clearly demonstrated suitability of the method for its intended application. The overall recoveries of the pesticides from peppermint, at the three spiking levels of 0.01, 0.1 and 1.0 mg kg(-1), were 100% ± 10% with relative standard deviations of 6% ± 5% on average. The limit of quantification was 0.01 mg kg(-1) for all the pesticides. The expanded uncertainties were in the range between 7% and 30% (14% on average), which was distinctively less than a maximum default value of ±50%. Compared with our previous method, that entailed dichloromethane/acetone extraction and florisil column cleanup with collection of four fractions, the new method was more straightforward, less time and labour intensive as well as more sensitive, selective and accurate, simultaneously. PMID:22752220

  12. [Occurrence of some pesticides residues in peppermint Mentha piperita L. in 2003-2005].

    Science.gov (United States)

    Sad?o, Stanis?aw; Szpyrka, Ewa; Rogozi?ska, Krystyna; Rupar, Julian

    2006-01-01

    The aim of this paper was to present occurrence of pesticides residues in peppermint Mentha Piperita in 2003-2005 and to estimate of their intakes by consumer. Gas chromatographic and spectroscopy methods were used. The most frequently found were chlorpyrifos residues (16% analysed samples) followed by terbacil (11%), dithiocarbamates (10%) and diazinon (5%). Residues in 14% analysed samples exceeded the European Union Maximum Residue Levels established for tea. Assuming consumption of peppermint on the level of 4.5 g (three bags) per day, short-term intake by adult and child consumer was a few times lower then Acceptable Daily Intake. PMID:17193741

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

    International Nuclear Information System (INIS)

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

  14. 78 FR 13264 - Acetochlor; Pesticide Tolerances

    Science.gov (United States)

    2013-02-27

    ...the dietary exposure analysis and risk assessment...water models used in pesticide exposure assessment...Acetochlor parent residue exposure is generally...concentrations using the PRZM (Pesticide Root Zone Model) and EXAMS (Exposure Analysis Modeling...

  15. 75 FR 29441 - Novaluron; Pesticide Tolerances

    Science.gov (United States)

    2010-05-26

    ...the dietary exposure analysis and risk assessment...water models used in pesticide exposure assessment...were used to assess residues of concern in drinking water: The Pesticide Root Zone Model/Exposure Analysis Modeling...

  16. Simultaneous and rapid detection of multiple pesticide and veterinary drug residues by suspension array technology.

    Science.gov (United States)

    Liu, Nan; Gao, Zhixian; Ma, Hongwei; Su, Pu; Ma, Xinhua; Li, Xiaoli; Ou, Guorong

    2013-03-15

    Suspension array technology is proposed for the simultaneous quantitative determination of seven kinds of pesticide and veterinary drug residues, namely, atrazine, chloramphenicol, carbaryl, clenbuterol, 17-?-estradiol, imidacloprid, and tylosin. The assay is simple and can be accomplished within 2h without repeated pumping and washing steps unlike conventional suspension arrays. The hapten-protein conjugate-coated beads bind to their complementary biotinylated antibodies using a competitive immunoassay format. The coefficients of determination R(2) for six targets were greater than 0.992, whereas that for atrazine was 0.961, which indicate good logistic correlations. The dynamic ranges for the seven targets in the 7-plex assay ranged from 2 log units to 4 log units(1.60×10(0)-1.64×10(3), 5.12×10(-2)-1.60×10(2), 1.00×10(0)-3.13×10(3), 4.00×10(-1)-4.10×10(2), 4.00×10(-1)-4.10×10(2), 5.12×10(-2)-1.60×10(2), and 2.00×10(0)-4.00×10(2)ngmL(-1)). The minimum detection concentrations of chloramphenicol, carbaryl, clenbuterol and 17-?-estradiol in the suspension array (0.05, 1.00, 0.40 and 0.40 ng mL(-1)) were lower than the corresponding limits of detection (0.25, 6.60, 24.23 and 13.96 ng mL(-1)) of using an indirect competitive enzyme-linked immunosorbent assay. Environmental scanning electron microscope was employed to characterize the bead surface, which directly confirmed the reactions on the beads. The suspension array is more flexible and feasible than ELISA for the fast quantitative analysis of pesticide and veterinary drug residues. PMID:23084755

  17. Acetylcholinesterase Based Detection of Residual Pesticides on Cotton

    OpenAIRE

    Jiri Militky; Syed Zameer Ul Hassan

    2012-01-01

    This study describes the measurement of bio-electrical signals caused by enzymatic inhibition of acetylcholinesterase (AChE) for the detection of organophosphorous and carbamate pesticides which are the strong inhibitors of AChE and prevents its normal function of the rapid removal of acetylcholine (Ach). Biosensor Toxicity Analyzer (BTA) was used for the testing and enzyme activity was determined by acetylthiocholine chloride (ATCCl) as enzyme substrate. The monitoring of changes in bio-elec...

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

    International Nuclear Information System (INIS)

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

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

    Directory of Open Access Journals (Sweden)

    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.

  20. Health risks associated with pesticide residues in sediments, fish, and plants from the Ouémé Valley in the Republic of Bénin.

    Science.gov (United States)

    Yehouenou A Pazou, Elisabeth; Azehoun, Judicaël P; Aléodjrodo, Patrick Edorh; van Straalen, Nico M; van Hattum, Bert; van Gestel, Cornelis A M

    2013-08-01

    To determine possible human and environmental health risks, organochlorine pesticide residues were determined in vegetables grown in floodplains along the Ouémé River near Lowé in Bénin. Testing of vegetables found 13 pesticides with ?DDT, ?-endosulfan, ?drin, and lindane being most important. The same pesticides were also detected in plants eaten by bovine cattle, sheep, and herbivorous fish. Human pesticide intake by vegetable consumption was compared with tolerable daily intake (TDI) values reported by the World Health Organization. Pesticide intake by fish consumption was estimated from residue levels in whole fish collected from the Ouémé River in 2004 and reported earlier. Fish consumption does not pose a risk for human health, but consuming vegetables that contain pesticide residues may lead to exceedance of TDI values. Based on these findings, concerns are warranted, and more work is needed to understand the full exposure profile for the local population. PMID:23535941

  1. Evaluation of pesticide residues in fruit from Poland and health risk assessment

    OpenAIRE

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

    2013-01-01

    In the present study an effort has been made to evaluate the residues of insecticides, fungicides and herbicides in fruit fromPolandand their health risks assessed. Accredited multiresidue methods based on gas and liquid chromatography, and spectroscopic technique were used to determine the concentrations above 160 pesticides. A total of 392 samples of 15 different fruit were collected during the May 2010 to October 2012. In 48.2% of samples no residues were found, 45.9% of samples contained...

  2. MACRO AND MICRO APPROACHES TO THE DETERMINATION OF PESTICIDE RESIDUES IN HUMAN AND ANIMAL TISSUES

    Science.gov (United States)

    Analytical approaches to the determination of pesticides and metabolites in human and animal tissues will take many forms. Several factors must be considered in choosing an analytical scheme if the results are to be meaningful. Whenever possible the residue chemist will use stand...

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

    Science.gov (United States)

    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...

  4. Assessment of organochlorine pesticide residues in Indian flue-cured tobacco with gas chromatography-single quadrupole mass spectrometer.

    Science.gov (United States)

    Ghosh, Rakesh Kumar; Khan, Zareen S; Rao, C V N; Banerjee, Kaushik; Reddy, D Damodar; Murthy, T G K; Johnson, Nalli; Ray, Deb Prasad

    2014-08-01

    Presence of pesticide residues in tobacco increases health risk of both active and passive smokers, apart from the imminent potential health problems associated with it. Thus, monitoring of pesticide residue is an important issue in terms of formulating stringent policies, enabling global trade and safeguarding the consumer's safety. In this study, a gas chromatography-single quadrupole mass spectrometry (GC-MS) method based upon quantifier-qualifier ions (m/z) ratio was employed for detecting and assessing ten organochlorine pesticide residues (?-HCH, ?-HCH, ?-HCH, ?-HCH, 2,4-DDT, 4,4-DDT, endrin, ?-endosulfan, ?-endosulfan and endosulfan sulphate) in 152 flue-cured (FC) tobacco leave samples from two major tobacco growing states, Karnataka and Andhra Pradesh, of India. In the majority of samples, pesticide residue levels were below the limit of quantification (LOQ). In few samples, pesticide residues were detected and they found to comply with the guidance residue levels (GRL) specifications of the Cooperation Center for Scientific Research Relative to Tobacco (CORESTA). Detection of the phase out pesticides like DDT/HCH might be due to transfer of persistent residues from the environmental components to the plant. This is the first report on these ten organochlorine pesticide residues in Indian FC tobacco. PMID:24687692

  5. Multi-residue determination of pesticides in tropical fruits using liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Botero-Coy, A M; Marín, J M; Ibáñez, M; Sancho, J V; Hernández, F

    2012-03-01

    Monitoring pesticide residues in tropical fruits is of great interest for many countries, e.g., from South America, that base an important part of their economy on the exportation of these products. In this work, a LC-MS/MS multi-residue method using a triple quadrupole analyzer has been developed for around 30 pesticides in seven Colombian tropical fruits of high commercial value for domestic and international markets (uchuva, tamarillo, granadilla, gulupa, maracuya, papaya, and pithaya). After sample extraction with acetonitrile, an aliquot of the extract was diluted with water and directly injected into the HPLC-MS/MS system (electrospray interface) without any cleanup step. The formation of sodium adducts-of poor fragmentation-was minimized using 0.1% formic acid in the mobile phase, which favored the formation of the protonated molecule. However, the addition of ammonium acetate made the formation of the ammonium adducts in some particular cases possible, avoiding the presence of the sodium adducts. The highest sensitivity was observed in positive electrospray ionization for the wide majority of pesticides, with a few exceptions for acidic compounds that gave better response in the negative mode (e.g., 2,4-D, fluazinan). Thus, simultaneous acquisition on the positive/negative mode was applied. Two MS/MS transitions were acquired for each compound to ensure a reliable quantification and identification of the compounds detected in samples, although for malathion a third transition was acquired due to the presence of interfering isobaric compounds in the sample extracts. A detailed study of matrix effects was made by a comparison of standards in solvent and in matrix. Both ionization suppression and ionization enhancement were observed depending on the analyte/matrix combination tested. Correction of matrix effects was made by the application of calibration in matrix. Three matrices were selected (uchuva, maracuya, gulupa) to perform matrix calibration in the analysis of all seven fruit varieties studied. The method was validated by recovery experiments in samples spiked at two levels (0.05 and 0.5 mg/kg). The data were satisfactory for the wide majority of analyte/matrix combinations, with most recoveries between 70% and 110% and the RSD below 15%. Several samples collected from the market were finally analyzed. Positive findings were confirmed by evaluating the experimental Q/q ratios and retention times, and comparing them with those of reference standards. PMID:21983979

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

    International Nuclear Information System (INIS)

    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.y.

  7. Pesticide residues in apples grown under a conventional and integrated pest management system.

    Science.gov (United States)

    Mladenova, R; Shtereva, D

    2009-06-01

    This paper describes method validation for determination of more than 40 pesticides in apples using a GC technique. Target compounds belonged to the organochlorine, organophosphorus, carbamates, pyrethroids, triazoles, dicarboximides and strobilurins groups, among others. Sample preparation consisted of acetone extraction and subsequent cleanup/concentration by SPE with a polymer-based sorbent. Single quadrupole GC-MS operating in SIM mode and electron impact ionization was used for identification and quantification of the pesticides. Average recoveries for analytes ranged between 70 and 110% at three fortification levels - 0.01, 0.1 and 0.2 mg kg(-1). Relative standard deviations were lower than 20% for all tested compounds. Calculated limits of detection and limits of quantification were below 0.01 mg kg(-1), which were sufficiently low compared to the maximum residue levels (MRLs) established by European legislation. The proposed method was applied for determination of pesticide residue in four selected apple varieties after harvesting. Whole and processed fruits (peel and peeled fruits) were analyzed from different treatment systems: two conventional, one based on integrated pest management (IPM) and two variants based on organic production (controls). Higher levels of pesticide residues were found in apple fruits under conventional conditions. Fenitrothion and chlorpyrifos residues were detected frequently in apple peel at concentrations up to 0.45 and 0.77 mg kg(-1), respectively. The levels found in the whole fruits of the same samples were much lower than in peel and below the respective MRLs (0.5 mg kg(-1) for both pesticides). Measurable residues of triadimenol only, up to 0.05 mg kg(-1), concentrated in the peel, were found in the apples from IPM. PMID:19680960

  8. Comparative study of pesticide multi-residue extraction in tobacco for gas chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Lee, Jeong-Min; Park, Jin-Won; Jang, Gi-Chul; Hwang, Keon-Joong

    2008-04-11

    This study was performed to apply the more rapid and accurate sample preparation, and the high selectivity and sensitivity of the analyte detection by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). We compared with the three-sample preparation methods of pesticide residues in tobacco such as the conventional liquid-liquid extraction (LLE), pressurized liquid extraction (PLE) and QuEChERS (quick, easy, cheap, effective, rugged and safe) methods. These methods were validated for 49 pesticides in the CORESTA Agrochemical Advisory Committee guide and amenable to GC-MS/MS determination. LLE with acetonitrile, and PLE with acetone were followed by solid-phase extraction (SPE) and analyzed by GC-MS/MS. In QuEChERS method, the effects of sorbents, such as primary secondary amine (PSA), octadecylsilane (C(18)) and graphitized carbon black (GCB), and matrix of the analytes in tobacco types, such as flue-cured, burley and oriental were investigated. MS/MS acquisition provided high specificity and selectivity for pesticides and low limit of detection and quantification. QuEChERS by using PSA alone and the matrix-matched standards gave good recoveries and RSD values in three types of tobaccos. The method yielded higher and more consistent recoveries of these analytes than LLE and PLE. QuEChERS method was no needed to be complex clean-up procedure and would be used to rapid and sensitive analysis of pesticides as an alternative to LLE and PLE methods. PMID:18304556

  9. Rapid detection of chlorpyrifos pesticide residue concentration in agro-product using Raman spectroscopy

    Science.gov (United States)

    Dhakal, Sagar; Peng, Yankun; Li, Yongyu; Chao, Kuanglin; Qin, Jianwei; Zhang, Leilei; Xu, Tianfeng

    2014-05-01

    Different chemicals are sprayed in fruits and vegetables before and after harvest for better yield and longer shelf-life of crops. Cases of pesticide poisoning to human health are regularly reported due to excessive application of such chemicals for greater economic benefit. Different analytical technologies exist to detect trace amount of pesticides in fruits and vegetables, but are expensive, sample destructive, and require longer processing time. This study explores the application of Raman spectroscopy for rapid and non-destructive detection of pesticide residue in agricultural products. Raman spectroscopy with laser module of 785 nm was used to collect Raman spectral information from the surface of Gala apples contaminated with different concentrations of commercially available organophosphorous (48% chlorpyrifos) pesticide. Apples within 15 days of harvest from same orchard were used in this study. The Raman spectral signal was processed by Savitzky-Golay (SG) filter for noise removal, Multiplicative Scatter Correction (MSC) for drift removal and finally polynomial fitting was used to eliminate the fluorescence background. The Raman spectral peak at 677 cm-1 was recognized as Raman fingerprint of chlorpyrifos. Presence of Raman peak at 677 cm-1 after fluorescence background removal was used to develop classification model (presence and absence of pesticide). The peak intensity was correlated with actual pesticide concentration obtained using Gas Chromatography and MLR prediction model was developed with correlation coefficient of calibration and validation of 0.86 and 0.81 respectively. Result shows that Raman spectroscopy is a promising tool for rapid, real-time and non-destructive detection of pesticide residue in agro-products.

  10. Organochlorine Pesticides Residues in Soil of Cocoa Farms in Ondo State Central District, Nigeria

    Directory of Open Access Journals (Sweden)

    Ademola F. Aiyesanmi

    2012-05-01

    Full Text Available Ondo State being the highest producer of Cocoa in Nigeria constitutes the most probable area with the highest use of chemical pesticides to enhance cocoa production. As effective as these chemicals may be in achieving this goal, the incidence of their residues on non-targeted substances and the total environment, with the attendant adverse effects have being of serious concerns. Our objective in this paper is to assess contamination of farm soils by organochlorine pesticides applied on cocoa farms within the Central Senatorial District of Ondo State, Nigeria. Soil samples were collected from selected cocoa farms and analysed for organochlorine pesticides residues using GC-MS. Some soil physicochemical properties including pH, particle size and organic matter that may influence the dynamics of the pollutants were also determined. Organochlorine compounds detected at varied concentrations include Endosulfan I and Endosulfan II occurring most frequently with highest concentrations of 350.10 mg/kg and 3.55 mg/kg respectively. Other organochlorine compounds detected were Heptachlor, Heptachlor epoxide, Aldrin, Deldrin,, isomers of Benzene hexachloride: ?-BHC, ?-BHC, ?-BHC, and ?-BHC (lindane. The concentrations of the organochlorine pesticides (mg/kg measured in the soil samples showed significant (p<0.05 correlation with the total organic matter contents of the soil. Findings from this research thus, provide information on the current and health risk residue levels of organochlorine pesticides in soil from this region with which future environmental performance on the use of pesticides on cocoa farms could be progressively monitored.

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

    Science.gov (United States)

    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.

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

    Directory of Open Access Journals (Sweden)

    B Shabankhani

    2006-01-01

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

  13. Residual gas analysis

    International Nuclear Information System (INIS)

    Determination of the residual gas composition in vacuum systems by a special mass spectrometric method was presented. The quadrupole mass spectrometer (QMS) and its application in thin film technology was discussed. Results, partial pressure versus time curves as well as the line spectra of the residual gases in case of the vaporization of a Ti-Pd-Au alloy were demonstrated together with the possible construction schemes of QMS residual gas analysers. (Sz.J.)

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

    International Nuclear Information System (INIS)

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

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

    Science.gov (United States)

    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

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

    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 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

  18. Rapid and simple analysis of pesticides persisting on green pepper surfaces swabbing with solvent-moistened cotton.

    Science.gov (United States)

    Watanabe, Eiki; Kobara, Yuso; Yogo, Yasuhiro

    2012-09-12

    A rapid and simple nondestructive extraction (NDE) method that includes wiping off of systemic neonicotinoid insecticides has been developed to streamline sample pretreatment procedures conducted before chromatographic determination. Pesticide residues were extracted from green pepper surfaces by swabbing them with absorbent cotton moistened with acetone or acetonitrile. After spraying of pesticides, the extraction rate decreased gradually, except for thiacloprid. Presumably, extraction rates depend on the physicochemical properties of pesticides, especially water solubility. It was thought that the applicability of the proposed method greatly depended on the systemic speed of each pesticide, and water solubility was placed as the index that was important to making certain. Direct analysis of some insecticides persisting on sample surfaces has been possible only by extraction before chromatographic determination. These findings indicate strongly that the proposed NDE method has collateral conditions, but it appears promising for on-site pretreatment for pesticide residue analysis. PMID:22908857

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

    International Nuclear Information System (INIS)

    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)

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

    International Nuclear Information System (INIS)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Luo Yuzhou [University of California, Davis, CA 95616 (United States); Wenzhou Medical College, Wenzhou 325035 (China); Zhang Minghua, E-mail: mhzhang@ucdavis.ed [University of California, Davis, CA 95616 (United States); Wenzhou Medical College, Wenzhou 325035 (China)

    2009-12-15

    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.

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

    Directory of Open Access Journals (Sweden)

    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 :?g/kg fats. With the exception of Endosulphan Sulphate whose mean concentration (99.052 :?g/kg was above the Australian Maximum Residue Limit (MRL of 20 :?g/kg for milk, the mean concentrations for all the other organochlorines detected were below their respective limits.

  3. Análise de resíduos de agrotóxicos em tomates empregando dispersão da matriz em fase sólida (DMFS e cromatografia gasosa Analysis of pesticide residue in tomato using matrix solid-phase dispersion (MSPD and gas chromatography

    Directory of Open Access Journals (Sweden)

    Gevany P. Pinho

    2009-01-01

    Full Text Available This work was aimed on optimization of the matrix solid-phase dispersion (MSPD technique using gas chromatography for analyzing residues of chlorpyriphos, ?-cyhalothrin, cypermethrin and deltamethrin in tomatoes. The results showed that silica was more efficient for the clean up of extracts, but florisil provided the highest recovery rates. A 2³ complete factorial design was carried out to evaluate the absorbent/sample ratio, presence of co-column (silica and ultrasonic bath on the extraction rate. The percentage of extraction of the pesticides chlorpyriphos, ?-cyhalothrin, cypermethrin and deltamethrin were 64.7, 88.3, 99.2 and 89.2%, respectively, with relative standard deviations below 5%.

  4. Análise de resíduos de agrotóxicos em tomates empregando dispersão da matriz em fase sólida (DMFS) e cromatografia gasosa / Analysis of pesticide residue in tomato using matrix solid-phase dispersion (MSPD) and gas chromatography

    Scientific Electronic Library Online (English)

    Gevany P., Pinho; Antônio A., Neves; Maria Eliana L. R., Queiroz.

    Full Text Available SciELO Brazil | Language: Portuguese Abstract in portuguese [...] Abstract in english This work was aimed on optimization of the matrix solid-phase dispersion (MSPD) technique using gas chromatography for analyzing residues of chlorpyriphos, ?-cyhalothrin, cypermethrin and deltamethrin in tomatoes. The results showed that silica was more efficient for the clean up of extracts, but fl [...] orisil provided the highest recovery rates. A 2³ complete factorial design was carried out to evaluate the absorbent/sample ratio, presence of co-column (silica) and ultrasonic bath on the extraction rate. The percentage of extraction of the pesticides chlorpyriphos, ?-cyhalothrin, cypermethrin and deltamethrin were 64.7, 88.3, 99.2 and 89.2%, respectively, with relative standard deviations below 5%.

  5. [Multi-residue method for screening of pesticides in crops by liquid chromatography with tandem mass spectrometry].

    Science.gov (United States)

    Tanizawa, Haruna; Shima, Mikie; Ikehara, Chieko; Kobata, Masakazu; Sato, Motoaki

    2005-10-01

    A simple and rapid method was developed for the screening of 82 pesticides/metabolites in a wide variety of crops, using solid-phase extraction and liquid chromatography with tandem mass spectrometry (LC/MS/MS). After extraction with methanol, the filtered extracts were made up to 100 mL and a 2 mL aliquot was subjected to solid-phase extraction. Co-extractives were removed with a C18 mini-column, while pesticides were retained on 3 kinds of mini-columns (HLB, SAX, activated carbon), and then eluted with acetonitrile. Analysis was performed by LC/MS/MS, and MS acquisition parameters were established in positive and negative ESI modes. The utility of the method was demonstrated by the analysis of 6 crops (carrot, cabbage, onion, spinach, lemon, brown rice) and one mixed vegetable juice. Of 82 compounds tested, 75 in carrot and 62 in lemon were obtained with recoveries ranging from 70-120%. For all samples tested, 75 compounds could be obtained with recoveries of over 50%, and the detection limits of most compounds were lower than 0.01 microg/g. This method provides acceptable performance for analysis of these 75 compounds. Further, by using aliquots of the extracts with small-scale mini-columns, purified samples could be obtained. This proposed method with small matrix effects, is effective and suitable for screening of multiple residual pesticides by using LC/MS/MS. PMID:16305173

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

    Science.gov (United States)

    Flores-García, Mery Elisa; Molina-Morales, Yuri; Balza-Quintero, Alirio; Benítez-Díaz, Pedro Rafael; Miranda-Contreras, Leticia

    2011-12-01

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

  7. Selective extraction of pyrethroid pesticide residues from milk by solid-matrix dispersion.

    Science.gov (United States)

    Di Muccio, A; Pelosi, P; Barbini, D A; Generali, T; Ausili, A; Vergori, F

    1997-03-21

    A rapid procedure has been developed that allows a single-step, selective extraction and clean-up of pyrethroid (PYR) pesticide residues from milk dispersed on solid-matrix diatomaceous material filled into disposable cartridges and eluted by means of light petroleum saturated with acetonitrile and ethanol. The extract was cleaned up by high-performance size-exclusion chromatography. Determinations were carried out by gas chromatography with electron-capture detection. Recovery experiments were carried out on homogenized commercial milk (3.6% fat content) that was spiked with solutions of 14 PYR pesticides, viz., tefluthrin, tetramethrin, cyphenothrin, cyfluthrin, flucythrinate, fluvalinate, deltamethrin, bioallethrin, fenpropathrin, lambda-cyhalothrin, permethrin, alpha-cypermethrin, esfenvalerate and tralomethrin, at levels ranging from 0.04 to 0.41 mg/kg for the different PYR pesticides. Average recoveries were in the range 60-119% for the different PYR pesticides, with relative standard deviations from ca. 2.5 to 14.4%. Coextracted fatty material amounted to an average of ca. 5 mg/ml of milk. The sole extraction step requires about 30 min. The main advantages of the procedure are that extraction of PYR pesticides (with a minimum carry over of fat) is performed in a single step, emulsions do not occur, several samples can be run in parallel by a single operator, reusable glassware is not needed and simple operations are required. PMID:9129301

  8. Determination of pesticide residues in animal origin baby foods by gas chromatography coupled with triple quadrupole mass spectrometry.

    Science.gov (United States)

    Amendola, Graziella; Pelosi, Patrizia; Attard Barbini, Danilo

    2015-01-01

    A simple, fast and multiresidue method for the determination of pesticide residues in baby foods of animal origin has been developed in order to check the compliance with the Maximum Residue Levels (MRLs) set at a general value of 0.01 mg/kg by Commission Directive 2006/125/EC for infant foods. The main classes of organochlorine, organophosphorus and pyrethroid compounds have been considered, which are mainly fat soluble pesticides. The analytical procedure consists in the extraction of baby food samples by acetonitrile (ACN) followed by a clean up using C18 solid-phase extraction column eluted with ACN. The compounds were determined by gas chromatography-triple quadrupole mass spectrometry equipped with a Programmed Temperature Vaporizer (PTV) injection and a backflush system. In order to compensate for matrix effects PTV and matrix matched standard calibrations have been used. The method has been fully validated for 57 pesticides according to the Document SANCO/12571/2013. Accuracy and precision (repeatability) have been studied by recoveries at two spiking levels, the Limit of Quantitation (LOQ) (0.003-0.008 mg/kg) and 10 time greater (0.03-0.08 mg/kg), and the results were in the acceptable range of 70-120% with Relative Standards Deviations (RSD) ?20%. Selectivity, linearity, LOQ and uncertainty of measurement were also determined for all the compounds. The method has been also applied for the analysis of 18 baby food animal origin samples, bought form the local market in Rome (Italy), and no pesticide in the scope of the method has been found above the MRL or the LOQ. PMID:25587780

  9. Agricultural pesticide residues in farm ditches of the Lower Fraser Valley, British Columbia, Canada.

    Science.gov (United States)

    Wan, Michael T; Kuo, Jen-ni; McPherson, Brad; Pasternak, John

    2006-01-01

    Transient and permanent farm ditches flowing to the Lower Fraser River tributary fish streams of British Columbia, Canada, were sampled at several locations in 2003-2004 to determine the occurrence and concentration of residues of selected pesticides, their transformation products, and soluble/extractable Cu++ ions. Of the 43 compounds analyzed, 28 and 22 pesticides were detected in transient farm ditch water and sediments, respectively. About 34% fewer pesticides, however, were found in both matrices of permanent farm ditches. Average concentrations (microg L(-1)) of those most frequently detected in permanent farm ditch water were atrazine (0.20), alpha -chlordane (0.06), desethylatrazine (0.13), diazinon (0.55), dieldrin (0.28), endosulfan sulfate (0.16), glyphosate (6), metalaxyl (0.27); and soluble Cu++ ions (25). Those most often found in ditch sediments (microg kg(-1)) were aminomethylphosphonic acid (AMPA) (2,300), 1,1,1-trichloro-2,2-bis-(4-chlorophenyl)ethane (DDT) (250), endosulfan sulfate (500), glyphosate (1,225); and extractable Cu++ ions (58,000). The risk potential of these pesticide residues to non-target aquatic organisms inhabiting Fraser River tributary fish streams contiguous to permanent farm ditches is evaluated and discussed. PMID:16785173

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

    Directory of Open Access Journals (Sweden)

    VALENTINA L. CHRISTOVA-BAGDASSARIAN

    2014-07-01

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

  11. 40 CFR 158.2081 - Experimental use permit biochemical pesticides product chemistry data requirements table.

    Science.gov (United States)

    2010-07-01

    ...particular biochemical pesticide product. Notes that...are required for all pesticide products and are not...active ingredient; Residue of concern=the...use permit biochemical pesticides product chemistry... TGAI and EP 4 Analysis and Certified...

  12. 40 CFR 158.2150 - Microbial pesticides nontarget organisms and environmental fate data requirements table.

    Science.gov (United States)

    2010-07-01

    ...tests for microbial pesticides: i. Avian acute...tests for microbial pesticides: i. Estuarine...Required if, after an analysis of the microbial pesticide's...or expected field residue exposure levels...

  13. 40 CFR 180.7 - Petitions proposing tolerances or exemptions for pesticide residues in or on raw agricultural...

    Science.gov (United States)

    2010-07-01

    ...it shall be accompanied by an accurate and complete English translation. The petition shall be accompanied by an advance deposit...or other endocrine effects. (13) Information regarding exposure to the pesticide chemical residue due to any tolerance...

  14. Quantification, nature and bioavailability of bound 14C-pesticide residues in soil, plants and food

    International Nuclear Information System (INIS)

    The Joint FAO/IAEA co-ordinated research programme on isotopic tracer aided studies of unextractable or bound pesticide residues in soil, plants and food was initiated in 1980. The first meeting was held in 1981 and the second meeting was held in 1983. The current programme was designed to assist scientists of developing countries to make safe and effective use of nuclear techniques for studying pesticide interactions with various components of the agricultural ecosystem. The third and final research co-ordination meeting was held in March 1985, and the papers presented there by the scientists participating in this programme are published in these Proceedings. The book also contains a report on the results of a collaborative study using a model protocol for the determination of bound residues in soil and an appraisal of the overall programme accomplishments. A separate abstract was prepared for each of these papers

  15. 77 FR 23625 - Quizalofop Ethyl; Pesticide Tolerances

    Science.gov (United States)

    2012-04-20

    ...anticipated residue and/or PCT...Tolerance level residues and/or 100...dietary exposure analysis and risk assessment...models used in pesticide exposure assessment...levels based on analysis of the residue field trial...for Setting Pesticide...

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

    International Nuclear Information System (INIS)

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

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

    OpenAIRE

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

    2014-01-01

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

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

    International Nuclear Information System (INIS)

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Mordaunt, Catriona J.; Gevao, Bondi; Jones, Kevin C.; Semple, Kirk T

    2005-01-01

    Six major use pesticides (Atrazine, Dicamba, Isoproturon, Lindane, Paraquat and Trifluralin) with differing physico-chemical properties were evaluated for the significance of 'bound' or non extractable residue formation. Investigations were carried out in purpose-built microcosms where mineralization, volatilisation, 'soil water' extractable and organic solvent extractable residues could be quantified. Extractable residues were defined as those accessible by sequential extraction where the solvent used became increasingly non-polar. Dichloromethane was the 'harshest' solvent used at the end of the sequential extraction procedure. {sup 14}C-labelled volatilised and {sup 14}CO{sub 2} fractions were trapped on exit from the microcosm. The pesticides were categorised into 3 classes based on their behaviour. (i) Type A (Atrazine, Lindane and Trifluralin) in which ring degradation was limited as was the formation of non-extractable residues; the remainder of the {sup 14}C-activity was found in the extractable fraction. (ii) Type B (Dicamba and Isoproturon) in which approximately 25% of the {sup 14}C-activity was mineralised and a large portion was found in the non-extractable fraction after 91 days. Finally, Type C (Paraquat) in which almost all of the {sup 14}C-activity was quickly incorporated into the non-extractable fraction. The implications of the data are discussed, with respect to the variability and significance of regulatory aspects of non-extractable residues.

  20. Examination of Some Pesticide Residues in Surface Water, Sediment and Fish Tissue of Elechi Creek, Niger Delta, Nigeria

    Directory of Open Access Journals (Sweden)

    F. Upadhi

    2012-11-01

    Full Text Available An investigation into the levels of selected pesticides in surface waters, sediment and fish (Mudskipper in the Elechi creek was carried out in two seasons and at three pre-determined sites. A higher concentration of 2, 4-diamine was observed in all stations and matrixes, while propoxur was least observed. Pesticide concentration in sediment is significantly different from that of water and fish tissue, which had the highest residual concentration. Concentration of pesticides ranged from 0.01 to 0.04 ?g/L in water, 0.01 to 0.06 ?g/gdw in sediment and 0.01 to 0.07 ?g/gdw in fish, respectively. There was bioaccumulation of pesticides in fish samples. Observed residues are generally higher than stipulated limit of 0.01 ?g/L by USEPA for pesticides of aquatic life, therefore, possess an ecological risk to the ecosystem and consequently human health.

  1. Analysis of Coupling the Pesticide Use Reduction with Environmental Policy for Agricultural Sustainability in Taiwan

    Directory of Open Access Journals (Sweden)

    Wen-Tien Tsai

    2013-03-01

    Full Text Available As Taiwan has a dense population and only limited natural resources, the government began actively establishing a Taiwan’s sustainable development indicators (TSDI system in 2003 to evaluate the progress towards sustainability. Commonly used pesticides could pose a risk of causing adverse effects to food sanitation, human health and the environment. Thus, the pesticide usage rate per hectare of farmland and the area of organic cultivation have been selected as agricultural sustainability indicators. The objective of this paper was to describe an analysis of current status of pesticide use and regulatory policy for environmental sustainability in Taiwan. Furthermore, it can be connected with the regulatory infrastructure, which has been established by the joint-venture of the central competent authorities (i.e., Council of Agriculture, Environmental Protection Administration, Department of Health, Ministry of Economic Affairs, and Council of Labor Affairs for controlling and/or preventing pesticide distribution in the environment. The significant progress is that the residual pesticides have notably declined in the past decade, which was in parallel with the pesticide usage rate decreased and organic farming area increased. For example, total area of organically certified cropping in Taiwan has been increased from 900 hectares (ha in 2001 to about 4,500 ha in 2010. Finally, some recommendations for the pollution prevention and toxicity reduction of pesticide use were also addressed to progress towards a sustainable agriculture in Taiwan.

  2. Dietary exposure of Hong Kong adults to pesticide residues: results of the first Hong Kong Total Diet Study.

    Science.gov (United States)

    Wong, Waiky W K; Yau, Arthur T C; Chung, Stephen W C; Lam, Chi-ho; Ma, Stephanie; Ho, Y Y; Xiao, Ying

    2014-01-01

    The use of pesticides and other chemicals has become a common practice in modern agriculture to enhance and stabilise crop yield, protect the nutritional integrity of food, facilitate food storage to assure year-round supplies, and provide attractive and appealing food products. With the adoption of strict good agricultural practice (GAP), only minimal amounts of pesticide residues should remain on the crops or in connected foods of animal origin up the food chain. To assess their associated health risk to local people, the dietary exposure of Hong Kong adults to residues of four groups of pesticides or their metabolites - organophosphorus pesticides (OPPs), carbamates, pyrethrins and pyrethroids, and dithiocarbamate (DTC) metabolites - is estimated in the first Hong Kong Total Diet Study (TDS). A total of 150 commonly consumed food items were collected and prepared "as consumed". A total of 600 composite food samples were analysed for 85 pesticides or their metabolites by liquid chromatography-tandem mass spectrometry (LC-MS/MS). These pesticides were primarily found at low levels (highest mean = 350 ?g kg?¹) in food samples of plant origin such as vegetables and fruits. Dietary exposures to pesticide residues were estimated based on the analytical results and the food consumption data of the local residents. The estimated dietary exposures of Hong Kong adults to all individual pesticides were well below their respective acceptable daily intakes (ADIs). The percentage contributions of the estimated mean and 95th percentile dietary exposures to the ADIs of individual pesticides were pesticide residues analysed in this study were unlikely to pose unacceptable health risks to the Hong Kong population. PMID:24588687

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

    International Nuclear Information System (INIS)

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

  4. Residues of organochlorine and synthetic pyrethroid pesticides in honey, an indicator of ambient environment, a pilot study.

    Science.gov (United States)

    Malhat, Farag M; Haggag, Mohamed N; Loutfy, Naglaa M; Osman, Mohamed A M; Ahmed, Mohamed Tawfic

    2015-02-01

    Samples of honey were screened to monitor residues of organochlorine and pyrethroid pesticides. The study meant to examine the quality of honey, and to use honey as a bioindicator of environmental contamination. Residue levels were determined by gas chromatography (GC-?ECD). Samples had a wide spectrum of organochlorine and synthetic pyrethroids pesticides, with hexachlorobenzene (HCB) as the most frequently detected organochlorine, followed by permethrin, heptachlor epoxide. Only one sample had a concentration of ?-HCH higher than maximum residue limit of honey (0.01 mg kg(-1)). Residues of organochlorines detected, indicate the presence of some fresh supplies, despite the ban imposed on their use. The study confirmed that honey bee and beehive matrices could be used as gauge for monitoring environment contamination. From public health point of view, the observed levels of pesticide residues in honey do not pose a serious health risk to the consumers, but raises questions of the source of organochlorines. PMID:25243805

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

    Science.gov (United States)

    Cassigneul, Ana; Alletto, Lionel; Chuette, Delphine; Le Gac, Anne-Laure; Hatier, Jules; Etievant, Veronique; Bergheaud, Valérie; Baumberger, Stéphanie; Méchin, Valérie; Justes, Eric; Benoit, Pierre

    2013-04-01

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

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

    International Nuclear Information System (INIS)

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

  7. 75 FR 60113 - Pesticide Science Policy; Notice of Withdrawal

    Science.gov (United States)

    2010-09-29

    ...the preferred method, but recommended...understanding of methods of analysis. For a time...exposure to pesticide residues in...vary for each pesticide- commodity...Assessment Analysis EPA's evaluation...methodology to a method known as...

  8. Resíduos de agrotóxicos em alimentos: uma preocupação ambiental global - Um enfoque às maçãs Residues of pesticides in food: a global environmental preoccupation - Focussing on apples

    Directory of Open Access Journals (Sweden)

    Isabel Cristina Sales Fontes Jardim

    2009-01-01

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

  9. 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

    International Nuclear Information System (INIS)

    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

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

    DEFF Research Database (Denmark)

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

  11. Pesticide residues in soils, sediments, and vegetables in the Red River Delta, northern Vietnam.

    Science.gov (United States)

    Nishina, Takuro; Kien, Chu Ngoc; Noi, Nguyen Van; Ngoc, Ha Minh; Kim, Chul-Sa; Tanaka, Sota; Iwasaki, K?z?

    2010-10-01

    This study assessed pesticide residues in soils, sediments, and vegetables in the Xuan Khe and Hop Ly communes located along the Chau Giang River in the Red River Delta, northern Vietnam. Samples were collected from agricultural areas within and outside of embankments built to prevent flooding. In Xuan Khe, the soils outside of the embankment were more clayey with higher organic matter contents compared with the inside, due to selective deposition during river flooding. Many of the soils contained significant amounts of pesticides including dichlorodiphenyltrichloroethane (DDT), dicofol, isoprothiolane, and metalaxyl although their levels were below the maximum allowable concentration set by the Vietnamese government. The spectrum of DDT derivatives found suggested that the source of DDTs was not contaminated dicofol. Soils in Hop Ly resembled soils in Xuan Khe but were relatively sandy; one field showed appreciable contents of DDT derivatives. The ratios of (p,p(')-dichlorodiphenyldichloroethylene + p,p(')-dichlorodiphenyldichloroethane)/ summation operatorDDT in the surface and subsurface soils in Hop Ly were 0.34 and 0.57, suggesting that the DDTs originated from recent application. Pesticide residues in soils were not likely to translocate into vegetable crops, except for metalaxyl. High concentrations of cypermethrins in kohlrabi leaves could be ascribed to foliar deposition. PMID:19757109

  12. Residues of organochlorine pesticides in soils from the southern Sonora, Mexico.

    Science.gov (United States)

    Cantu-Soto, E U; Meza-Montenegro, Maria Mercedes; Valenzuela-Quintanar, A I; Félix-Fuentes, A; Grajeda-Cota, P; Balderas-Cortes, J J; Osorio-Rosas, C L; Acuña-García, G; Aguilar-Apodaca, M G

    2011-11-01

    Although, the Yaqui and Mayo valleys are the most important agricultural areas in Sonora, there is only limited data of the pesticides residue in soils in these valleys. This study measured the organochlorine pesticides (OCPs) in 234 soil samples (residential and agricultural) from 24 communities. The global results (mean, range) indicated that benzene hexachloride (19.2, ND-938.5 ?g g(-1)), endrin (6.6, ND-377.3 ?g g(-1)) and DDTs (36.45, ND-679.7 ?g g(-1)) were the dominant contaminants. Soil is one of the most important routes of exposure to OCPs in the population of southern Sonora and this study can be used to establish background levels of OCPs. PMID:21761173

  13. Organochlorine pesticide residues in human blood samples collected from Haryana, India and the changing pattern.

    Science.gov (United States)

    Kaushik, C P; Sharma, Neetu; Kumar, Surender; Kaushik, A

    2012-09-01

    Blood samples were collected during August 1992 and August 2002 from various hospitals of Haryana state and analyzed for the presence of HCH and DDT residues and the change in concentration of pesticide residues was calculated in terms of % reduction. The study revealed that the mean residue levels of total HCH in human blood samples have declined by 87.6% while those of total DDT have decreased by 98.9% during a gap of 10 years. The obtained results reveal that during 1992 p,p'-DDT was the major component with the mean value of 6.125 mg/L followed by p,p'-DDE, ?-HCH, ?-HCH and ?-HCH while in 2002, ?-HCH and p,p'-DDE were comparable with mean value of 0.053 and 0.052 mg/L, respectively followed by p,p'-DDT, ?-HCH and p,p'-DDD. PMID:22772832

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

    Science.gov (United States)

    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

  15. Realistic approach of pesticide residues and French consumer exposure within fruit & vegetable intake.

    Science.gov (United States)

    Drouillet-Pinard, Peggy; Boisset, Michel; Periquet, Alain; Lecerf, Jean-Michel; Casse, Francine; Catteau, Michel; Barnat, Saida

    2011-01-01

    The increase of fruit and vegetable (F&V) intake contributes to the prevention of chronic diseases, but could also significantly increase pesticide exposure and may thus be of health concern. Following a previous pesticide exposure assessment study, the present study was carried out to determine actual levels of pesticides within 400 g of F&V intake and to evaluate consumer risk. Forty-three Active Substances (AS) exceeding 10 % of the Acceptable Daily Intake (ADI) in balanced menus established for our previous theoretical study were considered. Fifty-six pooled food samples were analyzed: 28 fruit samples and 28 vegetable samples. Pesticide values were compared to Maximum Residue Levels (MRL) and to the "toxicological credit" derived from ADI. It was observed that 23 out of the 43 retained AS were never detected, 5 were detected both in F&V samples, 12 only in fruits and 3 only in vegetables. The most frequently detected AS were carbendazim, iprodione and dithiocarbamates. When detected, AS were more frequently found in fruit samples (74 %) than in vegetable samples (26 %). A maximum of 3 AS were detected at once in a given sample. Overall, we observed 8 and 14 overruns of the MRL in 1204 measures in pooled vegetable and fruit samples, respectively (0.7 % and 1.2 % of cases, respectively). Chronic exposure for adults was the highest for dithiocarbamates but did not exceed 23.7 % of the ADI in F&V. It was concluded that raising both F&V consumption up to 400 g/day (~5 F&V/day) according to recommendations of the national health and nutrition plan, does not induce pesticide overexposure and should not represent a risk for the consumer. PMID:21191868

  16. Organochlorine pesticides residues and PCBs in benthic organisms of the inner shelf of the São Sebastião Channel, São Paulo, Brazil

    OpenAIRE

    Rosângela Gorni; Rolf Roland Weber

    2004-01-01

    Thirty seven benthic samples of the inner shelf area of São Sebastião, Brazil, were collected between April 1994 and August 1998 and analysed for seventeen chlorinated pesticide residues and PCBs congeners. Pesticide residues and PCBs congeners levels were low (ng/g) and predominantly found in the crustacean samples. DDE was the most frequently residue with a maximum of 9,7 ng/g followed by HCHs with maximum of 17,1ng/g. As for the PCBs, the heavier congeners predominate: CB 138,153,170, 18...

  17. Comparison of solvent extraction and solid-phase extraction for the determination of organochlorine pesticide residues in water.

    Science.gov (United States)

    Tan, G H

    1992-07-01

    Solid-phase extraction (SPE) of organochlorine pesticide residues from environmental water samples was evaluated using octadecyl (C18)-bonded porous silica. The efficiency of SPE of these pesticide residues from reagent water samples at 1-5 micrograms dm-3 levels was compared with those obtained by solvent extraction with hexane and Freon TF (trichlorotrifluoroethane). Average recoveries exceeding 80% for these organochlorine pesticides were obtained via the SPE method using small cartridges containing 100 mg of 40 microns C18-bonded porous silica. The average recovery by solvent extraction with hexane and Freon TF exceeded 90% in both instances. It was concluded that the recoveries and precision for the SPE of organochlorine pesticides were poorer than those for the solvent extraction method. Organochlorine pesticide residue levels in environmental water samples from two major rivers flowing through predominantly rice-growing areas were monitored by gas chromatography using the solvent extraction method with hexane. Exceptionally high levels of organochlorine pesticide residues such as BHC, DDT, heptachlor, endosulfan and dieldrin were found in these water samples. PMID:1524230

  18. Influence of novel lignocellulosic residues in a biobed biopurification system on the degradation of pesticides applied in repeatedly high doses

    Scientific Electronic Library Online (English)

    M. Cristina, Diez; Gonzalo R, Tortella; Gabriela, Briceño; Maria del Pilar, Castillo; Jorge, Díaz; Graciela, Palma; Carolina, Altamirano; Carolina, Calderón; Olga, Rubilar.

    2013-11-15

    Full Text Available Background: The biobed is a simple biopurification system used to prevent the point-source pesticide contamination that occurs at farm level. The typical composition of the biomixture used in this system is soil, peat and straw in volumetric proportions of 1:1:2. The principal component is straw due [...] to its positive effects on biological activity and thus pesticide degradation. However, access to straw can be limited in some regions, so it must be replaced by other more readily available lignocellulosic residues. Results: Therefore, two alternate lignocellulosic materials (barley husks and pine sawdust) were evaluated as partial substitutes for straw. The degradation of a repeatedly applied mixture of six pesticides by these alternates was assessed. The microbial respiration and fluorescein diacetate (FDA) hydrolysis activity were also assessed. The results showed that the highest degradation efficiency was found in mixtures containing straw and barley husks. Each biomixtures tested achieved a high degradation (50 to 90%) of all the pesticides used except iprodione. Repeated applications of pesticides resulted in a slowing of the degradation rate of all pesticide types in all biomixtures. FDA activity and microbial respiration were higher in the biomixtures containing barley husks and straw compared to the mixture with pine sawdust, a result consistent with the pesticide degradations observed. Conclusions: This paper demonstrates that the straw in the traditional biomixture can be partially replaced by other lignocellulosic materials to efficiently degrade a mixture of pesticides, even when the pesticides are added in successive applications and high concentrations.

  19. Effectiveness of pressurized liquid extraction and solvent extraction for the simultaneous quantification of 14 pesticide residues in green tea using GC.

    Science.gov (United States)

    Cho, Soon-Kil; Abd El-Aty, A M; Choi, Jeong-Heui; Jeong, Yang-Mo; Shin, Ho-Chul; Chang, Byung-Joon; Lee, Chitto; Shim, Jae-Han

    2008-06-01

    A simultaneous multiresidue method to determine 14 different pesticides, namely: flufenoxuron, fenitrothion, chlorfluazuron, chlorpyrifos, hexythiazox, methidathion, chlorfenapyr, tebuconazole, EPN, bifenthrin, cyhalothrin, spirodiclofen, difenoconazole, and azoxystrobin in green tea using pressurized liquid extraction (PLE) is described and compared with that of liquid-liquid extraction (LLE). For PLE, the extraction conditions were not optimized. Rather they were selected based upon previous successful investigations published by our laboratory. Analysis was performed by GC with electron capture detector (GC-ECD), and the pesticide identity of the positive samples was confirmed by GC-MS in a selected ion-monitoring (SIM) mode. Calibration curves showed an excellent linearity for concentrations ranging from 0.006 to 36.049 ppm, with r(2) >0.995. Green tea spiked at each of the two fortification levels, yielded average recoveries in the range of 87-112% and 71-109% for PLE and LLE, respectively. Precision values, expressed as RSDs, were below 6% at various spiking levels. With respect to the existing procedures, both methods gave LOQs that were lower than the maximum residue limits (MRLs) established by the Korea Food and Drug Administration (KFDA). Both methods have been successfully applied to the analysis of real samples, and bifenthrin was the only pesticide residue quantified in incurred green tea samples, with concentrations ranging from 0.093 ppm (LLE) to 0.1 ppm (PLE). These concentration levels were relatively low compared to KFDA-MRL (0.3 ppm). According to the validation data and performance characteristics, both methods are appropriate for multiresidue analysis of pesticide residues in green tea. PLE methodology showed superiority in recoveries of some pesticides, acceptable accuracy and precision while minimizing environmental concerns, time, and labor, and can be applied in routine analytical laboratories. PMID:18481329

  20. Comparison of Simple and Rapid Extraction Procedures for the Determination of Pesticide Residues in Fruit Juices by Fast Gas Chromatography–Mass Spectrometry

    OpenAIRE

    Cherta Cucala, Laura; Beltra?n Arandes, Joaquim; Pitarch Arquimbau, Mari?a Elena; Herna?ndez Herna?ndez, Fe?lix

    2013-01-01

    Three sample treatment methods, based on QuEChERS, solid-phase extraction (SPE) and solid-phase microextraction (SPME), were compared and evaluated in order to obtain the best conditions to determine pesticide residues in fruit juice by fast gas chromatography–mass spectrometry (single quadrupole GC-MS). Analysis were performed under selected ion monitoring, acquiring the three most abundant and/or specific ions for each analyte and using their relative intensity ratios as a confirmatory pa...

  1. Stir Bar Sorptive Extraction (SBSE) in Sample Preparation from Heterogeneous Matrices: Determination of Pesticide Residues in Pear Pulp at ppb Level

    OpenAIRE

    Bicchi, Carlo; Rubiolo, Patrizia; Cordero, Chiara Emilia Irma

    2002-01-01

    Chlorpyriphos methyl, chlorpyriphos ethyl, chlorthalonil, parathion methyl, parathion ethyl, fenitrothion, f-endosulfan, g-endosulfan and tetradifon residues were analysed in pear pulp (an heterogeneous matrix) by extraction on polydimethylsiloxane (PDMS) stir bar (SBSE) followed by recovery through thermodesorption (TD) and cGC-MS analysis. The levels of pesticides ranged from 10 to 100 ng/g (ppb). The results were compared to those obtained by a conventional method, namely SPMD-SPE cGC-ECD ...

  2. Monitoring multi-class pesticide residues in fresh grape by hollow fibre sorptive extraction combined with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Li, Jia; Zhang, Hong-Fei; Shi, Yan-Ping

    2011-07-15

    A fast and sensitive multi-residue analysis method is reported for simultaneous determination of 25 pesticides of chemical classes which are spiked into fresh grape. The sample pretreatment method involves extraction and clean-up in one step with SiO(2) hollow fibre from 1.0mL fresh grape slurry to minimise the matrix effects, and determination by gas chromatography-mass spectrometry with selective ion monitoring mode. The validation of the optimised method in terms of linearity, precision, recovery and repeatability showed that the proposed procedure is sensitive (the limits of detection were in the range of 0.0009-0.0084?gmL(-1) for 25 pesticides), precise and repeatable (average recoveries were between 61% and 108% with relative standard deviations from 4.0% to 12.4 %). The proposed method was also applied to the analysis of these groups of pesticides in fresh grape sample purchased from the local markets of Lanzhou (China), while no residues of the selected pesticides were detected in the sample. PMID:23140736

  3. [Simple preprocessing method for multi-determination of 235 pesticide residues in cooked ingredients of foods by GC/MS and LC/MS/MS].

    Science.gov (United States)

    Matsumoto, Naeo; Yoshikawa, Mayumi; Eda, Kuniaki; Kobayashi, Ayumi; Yokoshima, Masumi; Murakami, Masato; Kanekita, Hirofumi

    2008-06-01

    A simple preprocessing method was developed for multiresidue determination of pesticides in processed agricultural products. Residues were extracted from homogenized samples with acetonitrile in a glass centrifuge tube, followed by salting-out and partitioning with n-hexane. Co-extractives were removed by means of mini-column clean up. Analysis was performed by GC/MS and LC/MS/MS. The prepared sample solutions were examined for matrix effects. Matrix effects had both positive and negative effects on quantitative value. Calibration was achieved by preparing matrix-matched calibration standards to counteract the matrix effects. Of the 235 pesticides spiked at 0.05 or 0.10 microg/g (Method GC), 0.025 or 0.05 microg/g (Method LC) into 8 foods (garlic paste, diced green sweet pepper, green peas paste, celery paste, sweet potato paste, dried adzuki beans, boiled bamboo shoots, tomato paste), recoveries of 214 pesticides were between 50 and 100% and the coefficient of variation was below 20%. This method is useful as a multi-residue analysis method for screening of pesticides in foods. PMID:18633206

  4. Validation and application of micro flow liquid chromatography-tandem mass spectrometry for the determination of pesticide residues in fruit jams.

    Science.gov (United States)

    Reichert, Bárbara; Pizzutti, Ionara Regina; Costabeber, Ijoni Hilda; Uclés, Ana; Herrera, Sonia; Fernández-Alba, Amadeo R

    2015-03-01

    In this study, a very sensitive method was validated to determine pesticides residues in fruit jams using micro flow liquid chromatography-tandem mass spectrometry (µLC-MS/MS). A slurry of the fruit jams and water was prepared to yield homogeneous samples. Because of the high sensitivity achieved with the µLC-MS/MS equipment and to minimize matrix effects, the QuEChERS extracts were diluted 30-fold before the analysis. The validation was performed analyzing spiked samples at 9 and 45 µg kg(-1) (n=5). The method met validation criteria of 70-120% recovery and RSD?20% for 92% of the 107 pesticides evaluated. The reporting limit (RL) was 9 and 45 µg kg(-1) for respectively 66% and 26% of the analytes, 5% of the compounds did not fulfill the requirements for validation and 3% were not detected at the studied concentrations. The validated method was applied to the analysis of 51 different fruit jam samples from Brazil and Spain and pesticide residues were detected in 41 samples, 26 of which contained at least one pesticide at concentration >10 µg kg(-1). PMID:25618688

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

    International Nuclear Information System (INIS)

    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)

  6. [Research on rapid and quantitative detection method for organophosphorus pesticide residue].

    Science.gov (United States)

    Sun, Yuan-Xin; Chen, Bing-Tai; Yi, Sen; Sun, Ming

    2014-05-01

    The methods of physical-chemical inspection is adopted in the traditional pesticide residue detection, which require a lot of pretreatment processes, are time-consuming and complicated. In the present study, the authors take chlorpyrifos applied widely in the present agricultural field as the research object and propose a rapid and quantitative detection method for organophosphorus pesticide residues. At first, according to the chemical characteristics of chlorpyrifos and comprehensive chromogenic effect of several colorimetric reagents and secondary pollution, the pretreatment of the scheme of chromogenic reaction of chlorpyrifos with resorcin in a weak alkaline environment was determined. Secondly, by analyzing Uv-Vis spectrum data of chlorpyrifos samples whose content were between 0. 5 and 400 mg kg-1, it was confirmed that the characteristic information after the color reaction mainly was concentrated among 360 approximately 400 nm. Thirdly, the full spectrum forecasting model was established based on the partial least squares, whose correlation coefficient of calibration was 0. 999 6, correlation coefficient of prediction reached 0. 995 6, standard deviation of calibration (RMSEC) was 2. 814 7 mg kg-1, and standard deviation of verification (RMSEP) was 8. 012 4 mg kg-1. Fourthly, the wavelengths whose center wavelength is 400 nm was extracted as characteristic region to build a forecasting model, whose correlation coefficient of calibration was 0. 999 6, correlation coefficient of prediction reached 0. 999 3, standard deviation of calibration (RMSEC) was 2. 566 7 mg kg-1 , standard deviation of verification (RMSEP) was 4. 886 6 mg kg-1, respectively. At last, by analyzing the near infrared spectrum data of chlorpyrifos samples with contents between 0. 5 and 16 mg kg-1, the authors found that although the characteristics of the chromogenic functional group are not obvious, the change of absorption peaks of resorcin itself in the neighborhood of 5 200 cm-' happens. The above-mentioned experimental results show that the proposed method is effective and feasible for rapid and quantitative detection prediction for organophosphorus pesticide residues. In the method, the information in full spectrum especially UV-Vis spectrum is strengthened by chromogenic reaction of a colorimetric reagent, which provides a new way of rapid detection of pesticide residues for agricultural products in the future. PMID:25095434

  7. Residual gas analysis device

    Science.gov (United States)

    Thornberg, Steven M. (Peralta, NM)

    2012-07-31

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

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

    Directory of Open Access Journals (Sweden)

    Mário Sérgio Galhiane

    2012-01-01

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

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

    Scientific Electronic Library Online (English)

    Mário Sérgio, Galhiane; Sandra Regina, Rissato; Lucídio de Sousa, Santos; Gilberto Orivaldo, Chierice; Marcos Vinícius de, Almeida; Terezinha, Fumis; Inês, Chechim; Aloísio Costa, Sampaio.

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

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

    Science.gov (United States)

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

    2015-05-01

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

  11. Assessment of pesticide residues in flesh of Catla catla from Ravi River, Pakistan.

    Science.gov (United States)

    Akhtar, Mobeen; Mahboob, Shahid; Sultana, Salma; Sultana, Tayyaba; Alghanim, Khalid Abdullah; Ahmed, Zubair

    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; however, DDT and DDE concentrations were more than the maximum residue limits (MRLs) about food standards, while endosulfan sulfate and cartap were not detected. Pesticide concentrations in the fish flesh were ranged from 3.240 to 3.389 for DDT, 2.290 to 2.460 for DDE, 0.112 to 0.136 for endosulfan, and 0.260 to 0.370 ?g g(-1) for carbofuran. The findings revealed that the pesticide concentrations in the fish flesh decreased in the order: DDT > DDE > carbofuran > endosulfan. After Degh fall and After Hudiara nulla fall river sampling sites were found severely contaminated. It is proposed that a constant monitoring programs are needed to be initiated to overcome the present alarming situation. PMID:25003148

  12. Fate of 14C-ethion insecticide in the presence of deltamethrin and dimilin pesticides in cotton seeds and oils, removal of ethion residues in oils, and bioavailability of its bound residues to experimental animals.

    Science.gov (United States)

    Abdel-Gawad, Hassan; Mahdy, Fathia; Hashad, Adly; Elgemeie, Galal H

    2014-12-24

    Ethyl-1-(14)C-ethion and some of its degradation products have been prepared for comparison purposes. Cotton plants were treated with (14)C-ethion alone and in the presence of deltamethrin and dimilin pesticides under conditions simulating local agricultural practice. (14)C-Residues in seeds were determined at harvest time; about 47.5% of (14)C-activity was associated with oil. After further extraction of seeds with ethanol, the ethanol-soluble (14)C-residues accounted for 10.6% of the total seed residues, whereas the cake contained about 37.3% of the total residues as bound residues in the case of ethion only. The bound residues decreased in the presence of deltamethrin and dimilin pesticides and amounted to 8.1 and 10.4% of the total residues, respectively. About 95% of the (14)C-activity in the crude oil could be eliminated by simulated commercial processes locally used for oil refining. Chromatographic analysis of crude cotton oil revealed the presence of ethion monooxon, O,O-diethyl phosphorothioate, and O,O-diethyl phosphoric acid in addition to one unknown compound in the case of ethion alone or ethion and dimilin. The same degradation products are found in the case of ethion and deltamethrin in addition to ethion dioxon, whereas ethanol extract revealed the presence of ethion dioxon and O,O-diethyl phosphoric acid as free metabolites. Acid hydrolysis of the conjugated metabolites in the ethanol extract yielded O,O-diethyl S-hydroxymethyl phosphorodithioate. The bound residues were quite readily bioavailable to the rats. After feeding rats with the cake containing ethion-bound residues, a substantial amount (60%) of (14)C-residues was eliminated in the urine, whereas the (14)C-residues excreted in expired air and feces were 10 and 9%, respectively. About 11% of the radioactive residues were distributed among various organs. PMID:25420216

  13. Assessment of dietary intakes of nineteen pesticide residues among five socioeconomic sections of Hyderabad--a total diet study approach.

    Science.gov (United States)

    Betsy, Agatha; Vemula, Sudershan Rao; Sinha, Sn; Mendu, Vishnu Vardhana Rao; Polasa, Kalpagam

    2014-01-01

    Total diet study approach was used to assess the dietary intakes of pesticide residues among the select population in Hyderabad. When assessed by a food frequency questionnaire, it was found that the food intakes varied among five socioeconomic sections (SES). Therefore, we intended to compare the intakes of pesticide residues through these foods among the five SES. A total of 195 foods from different markets were collected and analyzed for 19 pesticides. The residues were analyzed with a gas chromatograph and were confirmed with mass spectrometry. About 51 % of the samples were detected with one or more residues. Thirteen out of the 19 residues were present in levels above detection limits in various concentrations. The median concentrations of the residues in all the samples tested, ranged from 0.00010 to 0.33 mg/kg. Highest median concentration was for ?-HCH in water samples. Exposures to all the residues were below the respective ADIs at both mean and 95th percentile levels of food intakes with highest estimated dietary intakes (EDIs) of ?-HCH in both the cases. The EDIs of ?-HCH were the highest among all the residues at both the intake levels among all the SES. The EDIs of ?-HCH were significantly higher in lower SES than higher SES possibly due to the consumption of rice cooked in water contaminated with ?-HCH. EDIs for other residues did not differ significantly among the five SES. PMID:23996645

  14. 77 FR 30402 - Acibenzolar- S -methyl; Time-Limited Pesticide Tolerances

    Science.gov (United States)

    2012-05-23

    ...CSFII. As to residue levels in food...dietary exposure analysis for the general...Tolerance level residues and 100 crop...residue levels of pesticide residues in food...drinking water. The residues of concern for...models used in pesticide exposure assessment...Model/Exposure Analysis Modeling...

  15. Residues of currently and never used organochlorine pesticides in agricultural soils from Zhejiang Province, China.

    Science.gov (United States)

    Zhang, Anping; Fang, Li; Wang, Junliang; Liu, Weiping; Yuan, Hejin; Jantunen, Liisa; Li, Yi-Fan

    2012-03-28

    Studies on residues of currently and never used organochlorine pesticides (OCPs) facilitate the assessment of the contamination level, distribution, sources, transportation, and trend of these selected OCPs in China. In this work we investigated the concentration levels of endosulfans and chlordane, which are currently used, and the never used aldrin and dieldrin in the province of Zhejiang, a rainy, and hilly tea-growing province in eastern China. The average/mean residue levels of OCPs was in the order ?endosulfan > ?chlordane > aldrin > dieldrin. The residue level was in good agreement with the usage of OCPs in Zhejiang. The spatial distribution showed that the residues of OCPs in soils from the mountain area were always higher than those in soils from the plains. The distribution characteristics were related to usage for current-use OCPs and temperature for never used OCPs. The isomeric ratios and enantiomeric fractions are useful tools to identify the degradation preference of contaminants. The wide range of ratios between trans-chlordane (TC) and cis-chlordane (CC) indicated that the degradation of the two isomers of chlordane was different at different sites. Nonracemic residues of TC and CC were observed in most soils; this is significant since the enantiomers have different toxicities. PMID:22404818

  16. Pyrotechnic reaction residue particle analysis.

    Science.gov (United States)

    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

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

    Science.gov (United States)

    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?gkg(-1)) and triadimenol (26.1?gkg(-1)), the herbicides fluometuron (174.6?gkg(-1)) and terbuthylazine (403.3?gkg(-1)), and the insecticide methoxyfenozide (4.61?gkg(-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

  18. Changing patterns of organochlorine pesticide residues in raw bovine milk from Haryana, India.

    Science.gov (United States)

    Kaushik, C P; Sharma, Hardeep Rai; Gulati, Deepak; Kaushik, Anubha

    2011-11-01

    Bovine milk samples were collected and analyzed during 1992 and 1998 from rural areas of 14 different districts of Haryana state for the presence of HCH and DDT residues. The study revealed that the mean residues of ?HCH in raw bovine milk have declined by 67.5% while mean levels of ?DDT have decreased by 92.8% during six years gap. The obtained results reveal that during 1992 p,p'-DDT was the main component followed by p,p'-DDD, ?-HCH and ?-HCH while in 1998, p,p'-DDE and ?-HCH followed by p,p'-DDT were relatively more as compared to other isomers and metabolites of these pesticides. PMID:21331758

  19. [Multiresidue analysis of nitrogen-containing and sulfur-containing pesticides in agricultural products using dual-column GC-NPD/FPD].

    Science.gov (United States)

    Ueno, Eiji; Oshima, Harumi; Saito, Isao; Matsumoto, Hiroshi

    2002-04-01

    We investigated simultaneous analytical methods for pesticide residues in large numbers of agricultural products samples. Extraction of each sample with acetonitrile was followed by a salting-out step using a graduated cylinder. The test solution was cleaned up with gel permeation chromatography (GPC), which separated the pesticide eluate into 2 fractions, and then with a tandem mini-column. Analysis was done with a dual-column GC equipped with a dual NPD and FPD (S mode) detector. Use of the Siltek-deactivated liner, guard column, and Y connector, and Silcosteel-treated NPD jet was effective for preventing the breakdown of sulfur-containing pesticides. Recoveries of 87 nitrogen-containing and sulfur-containing pesticides from fortified spinach, tomato, apple, strawberry and brown rice, ranged from 71 to 127% with RSD values of 1-24%, except for recoveries of aldicarb, amitraz, ethiofencarb, imazalil, propamocarb and triflumizole. Detection limits of pesticides were very good (0.3-5 ppb (NPD) and 2-20 ppb (FPD)) for routine analysis of pesticide residues in foods. Surveillance of pesticides in agricultural products was carried out by using the present method. From 22 out of 33 samples, 21 pesticides (43 in total) were detected. The results indicated that the present method can be applied as an efficient and reliable means for monitoring pesticide residues in agricultural products. PMID:12092417

  20. Distribution, fate and effects of pesticide residues in tropical coastal lagoons of northwestern Mexico.

    Science.gov (United States)

    Carvalho, F P; Gonzalez-Farias, F; Villeneuve, J P; Cattini, C; Hernandez-Garza, M; Mee, L D; Fowler, S W

    2002-11-01

    Analyses of pesticide residues in sediments, water and biota of the Altata-Ensenada del Pabellon coastal lagoon system in Sinaloa, Mexico, showed the presence of organochlorine and organophosphorus compounds. For all the compounds analysed, concentrations in sediments were higher near the points of water discharge from ponds and drainage from the agricultural area. Among the organochlorines, total DDTs displayed the largest sedimentary reservoir, followed by total endosulfans and chlorpyrifos. In sediments, as well as in biota, pp'-DDT concentrations were lower than those of DDT metabolites, which confirms the reduction in the previous massive use of this compound in agriculture. Endosulfan is currently used in the region and endosulfan residues in lagoon sediments attained levels considered to be toxic to meiofauna, therefore constituting an ecological risk to lagoon ecosystems. There was a large sedimentary reservoir of chlorpyrifos but its ecotoxicological risk is difficult to assess due to lack of adequate comparative data. Nevertheless, concentrations of chlorpyrifos which approach acute toxic levels for shrimp were recorded in lagoon water. This suggests that drainage from agricultural fields during high runoff may, on occasion, cause mass mortality of shrimp and fish Organophosphorus pesticides are widely regarded to degrade very rapidly in aquatic systems. Experimental research performed with 14C-labelled chlorpyrifos and parathion has shown that they may be stabilised for relatively long periods of time through sediment-water partitioning. This extension of their environmental half-lives increases their potential for impacting on coastal ecosystems. Since organophosphorus pesticides are highly toxic for aquatic organisms at concentrations generally lower than organochlorines, their presence in the lagoon water and sediment is a matter for much concern. The increased use of tropical coastal lagoons for shrimp and fish farming requires the implementation of environmental management practices to protect these ecosystems from the impact of agricultural activities. Environmental management aims to preserve the ecosystem integrity of these coastal lagoons and, through improving the water quality, to allow the development of aquaculture and reduce human exposure to pesticide residues in food. PMID:12472156

  1. Are pesticide residues associated to rice production affecting oyster production in Delta del Ebro, NE Spain?

    Science.gov (United States)

    Ochoa, Victoria; Riva, Carmen; Faria, Melissa; Köck-Schulmeyer, Marianne; de Alda, Miren López; Barceló, Damià; Fernandez Tejedor, Margarita; Roque, Ana; Ginebreda, Antoni; Barata, Carlos

    2012-10-15

    Pesticide usage in Delta del Ebro (NE Spain) during the rice growing season has been associated with oyster episodes of mortality that occur early in summer. However, there are no studies that have directly evaluated pesticide levels and effects in oysters (Crassotrea gigas) cultured in Ebro's Bays. In this study pesticide levels in water, metal body burdens and up to 12 different biochemical markers were monitored in gills and digestive glands of oysters transplanted from May to June in 2008 and 2009. Biochemical responses evidenced clear differences in oysters from 2008 and 2009. Oysters transplanted in 2009 showed their antioxidant defenses unaffected from May to June and consequently increased levels of tissue damage measured as lipid peroxidation and DNA strand breaks and of mortality rates. Conversely oysters transplanted in 2008 increase their antioxidant defenses from May to June, had low levels of lipid peroxidation and DNA damage and low mortality rates. Some pesticides in water such as bentazone and propanil together with high temperatures and salinity levels were related with tissue damage in oyster transplanted in 2008 but the observed large differences between years indicate that abiotic factors alone could not explain the high mortalities observed in 2009. An analysis of recent reported studies pointed out in the direction that in addition to abiotic factors the use of oysters sensitive to diseases may explain the observed responses. PMID:22940045

  2. Influence of alternating soil drying and wetting on the desorption and distribution of aged 14C-labeled pesticide residues in soil organic fractions

    Science.gov (United States)

    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 ?m) 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 ?g kg-1 soil (dry/wet) and 10.7 ?g kg-1 soil (wet/wet), accounting for 3.45 and 1.35% of total parent compound initially applied after a total of 10 water extractions, respectively. MBT was detected but not quantified, whereas its metabolite MABT (2-methylamino-benzothiazole) was detected (0.8 vs 0.3 ?g kg-1, in dry/wet vs wet/wet soil water extracts, respectively) after 10 water extractions. These results demonstrate the long-term persistence of ETD and MBT and metabolites and their remobilization potential facilitated by soil drying and rewetting. For all samples, the DOC content was significantly higher for the water extracts obtained after dry/wet cycles compared to values obtained from the constantly moistened soil samples. The DOC and water extracted residual 14C activity correlated positively. This result indicates that pesticide residues are associated with DOC which might function as a shuttle for the distribution of pesticide residues. This molecular association can be released into solution where it might be degraded co-metabolically. Overall, the results suggest that intermittent soil drying and rewetting alters the disaggregation of soil aggregates, resulting in a release of entrapped organic carbon and pesticide molecules. Furthermore, analysis of the organic fractions obtained from the 14C pesticide residues containing soil revealed that 14C residues were mainly associated with the humin fraction. The analysis of the organic fractions revealed that extractable residual 14C activity of ETD was more associated with the fulvic acid fraction compared to the residual pesticide 14C activity of MBT, being more associated with the humic acid fraction. For 14C MBT residues, the distribution of the 14C residues in the organic fractions remained rather equal throughout the water extraction cycles. This observation can be supported by the non-mobile character of MBT in soil and its higher KOC value of 247-587 compared to the rather mobile pesticide ETD with a KOC value of 37.1-149. However, for both pesticides a decrease of residual 14C activity in the humic and fulvic acid fractions throughout the water extractions cycles was observed. This observation was more pronounced

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

    Science.gov (United States)

    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

  4. Residuos de plaguicidas organofosforados en muestras de tomate / Organophosphate pesticide residues in samples of tomato

    Scientific Electronic Library Online (English)

    Paola A., Castro; Juan Pablo, Ramos; Sandra L, Estévez; Andrea, Rangel.

    2004-11-01

    Full Text Available SciELO Colombia | Language: Spanish Abstract in spanish Se estudió la presencia de residuos de diez plaguicidas organofosforados (POPs) en tomates adquiridos en la central de abastos y en una cadena de supermercados de Bogotá, usando extracción líquido-líquido (LLE) y determinación analítica mediante un equipo de Cromatografía de Gases de Alta Resolución [...] (HRGC) - Detector Fotométrico de Llama (FPD). Los plaguicidas analizados fueron: Clorfevinfos, Clorpirifos, Demeton O, Demeton S, Diclorofentión, Dimetoato, Famfur, Leptofos, Metilparation y Triclorfon. Se analizaron diez muestras obtenidas en la central mayoritaria de abastos y ocho muestras de una cadena de supermercados de las cuales el 55% presentó contaminación con Dimetoato, aunque ninguna sobrepasó el límite máximo de residuos (LMR) de 1 mg/kg establecido por el Codex alimentario. También se encontraron residuos de Metilparatíon y Clorfevinfos, en ambos casos dentro de los límites permitidos. Abstract in english The presence of ten organophosphorus pesticides was studied in tomatoes acquired from markets in Bogotá (Colombia), using Liquid-liquid Extraction (LLE) and High Resolution Gas Chromatography (HRGC) with flame photometric detector (FPD). The pesticides analyzed were: Chlorfevinphos, Chlorpyrifos, De [...] meton O, Demeton S, Dichlofenthion, Dimethoate, Famphur, Leptophos and Trichlorfon. Eighteen samples were analyzed in which fifty five percent were contaminated with Dimethoate. Dimethoate levels in the contaminated samples were below the maximun residue levels (MRL) of 1 mg/kg established by the Codex alimentarius. Residues of Methyl parathion and Chlorfevinphos were also found, below the MRL.

  5. Effects of organic and conventional rice on protein efficiency ratio and pesticide residue in rats

    Directory of Open Access Journals (Sweden)

    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.

  6. Improved gas chromatography-tandem mass spectrometry determination of pesticide residues making use of atmospheric pressure chemical ionization.

    Science.gov (United States)

    Portolés, Tania; Cherta, Laura; Beltran, Joaquim; Hernández, Félix

    2012-10-19

    The capabilities of a recently launched atmospheric pressure chemical ionization (APCI) source for mass spectrometry (MS) coupled to gas chromatography (GC) have been tested in order to evaluate its potential in pesticide residue analysis in fruits and vegetables. Twenty-five pesticides were selected due to their high fragmentation under electron ionization (EI), making that the molecular ion (M+) is practically absent in their spectra. The fragmentation of these pesticides under APCI conditions was studied, with the result that M+ was not only present but also highly abundant for most compounds, with noticeable differences in the fragmentation patterns in comparison with EI. Moreover, the addition of water as modifier was tested to promote the formation of protonated molecules ([M+H]+). Under these conditions, [M+H]+ became the base peak of the spectrum for the majority of compounds, thus leading to an increase of sensitivity in the subsequent GC-MS/MS method developed using triple quadrupole analyzer (QqQ). Highly satisfactory sensitivity and precision, in terms of repeatability, were reached and linearity was satisfactory in the range 0.01-100 ng/mL. The developed methodology was applied to apple, orange, tomato and carrot QuEChERS fortified extracts in order to evaluate the matrix effects. In summary, the soft and reproducible ionization in the APCI source has greatly favored the formation of [M+H]+ oppositely to EI where abundant fragmentation occurs and where the molecular ions have low abundance or are even absent in the mass spectrum. In this way, the use of APCI has facilitated the development of tandem MS methods based on the selection of abundant [M+H]+ as precursor ion. PMID:22959847

  7. Determination of Pesticide Residues in Soil by Modified Matrix Solid-Phase Dispersion and Gas Chromatography

    International Nuclear Information System (INIS)

    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

  8. Screening and quantification of pesticide residues in fruits and vegetables making use of gas chromatography-quadrupole time-of-flight mass spectrometry with atmospheric pressure chemical ionization.

    Science.gov (United States)

    Cervera, M I; Portolés, T; López, F J; Beltrán, J; Hernández, F

    2014-11-01

    An atmospheric pressure chemical ionization source has been used to enhance the potential of gas chromatography coupled with quadrupole time-of-flight (QTOF) mass spectrometry (MS) for screening and quantification purposes in pesticide residue analysis. A screening method developed in our laboratory for around 130 pesticides has been applied to fruit and vegetable samples, including strawberries, oranges, apples, carrots, lettuces, courgettes, red peppers, and tomatoes. Samples were analyzed together with quality control samples (at 0.05 mg/kg) for each matrix and for matrix-matched calibration standards. The screening strategy consisted in first rapid searching and detection, and then a refined identification step using the QTOF capabilities (MS(E) and accurate mass). Identification was based on the presence of one characteristic m/z ion (Q) obtained with the low collision energy function and at least one fragment ion (q) obtained with the high collision energy function, both with mass errors of less than 5 ppm, and an ion intensity ratio (q/Q) within the tolerances permitted. Following this strategy, 15 of 130 pesticides were identified in the samples. Afterwards, the quantitation capabilities were tested by performing a quantitative validation for those pesticides detected in the samples. To this aim, five matrices were selected (orange, apple, tomato, lettuce, and carrot) and spiked at two concentrations (0.01 and 0.1 mg/kg), and quantification was done using matrix-matched calibration standards (relative responses versus triphenyl phosphate used as an internal standard). Acceptable average recoveries and relative standard deviations were obtained for many but not all pesticide-matrix combinations. These figures allowed us to perform a retrospective quantification of positives found in the screening without the need for additional analysis. Taking advantage of the accurate-mass full-spectrum data provided by QTOF MS, we searched for a higher number of compounds (up to 416 pesticides) in a second stage by performing extra data processing without any new sample injection. Several more pesticides were detected, confirmed, and/or tentatively identified when the reference standard was unavailable, illustrating in this way the potential of gas chromatography-QTOF MS to detect pesticides in addition to the ones targeted in quantitative analysis of pesticides in food matrices. PMID:24828980

  9. Occurrence and possible fate of organochlorine pesticide residues at Manzala Lake in Egypt as a model study.

    Science.gov (United States)

    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

  10. Selected pesticide residues or metabolites in blood and urine specimens from a general population survey.

    OpenAIRE

    Murphy, R. S.; Kutz, F. W.; Strassman, S. C.

    1983-01-01

    The National Center for Health Statistics collaborated with the National Human Monitoring Program of the U.S. Environmental Protection Agency (EPA) in a four-year study to assess the exposure of the general population to selected pesticides through analysis of blood serum and urine specimens. Specimens were collected on a national probability half sample of persons 12-74 years of age from 64 locations across the United States comprising the sample areas in the Second Health and Nutrition Exam...

  11. Headspace solid-phase microextraction of pesticide residues in Cannabis samples

    OpenAIRE

    Ilias, Yara; Rudaz, Serge; Christen, Philippe; Veuthey, Jean-luc

    2006-01-01

    A headspace solid-phase microextraction method combined with gas chromatography–mass spectrometry was evaluated for the extraction and analysis of selected pesticides, namely alachlor, ?-hexachlorocyclohexane, bromopropylate, carbaryl, diazinon, linuron, polychlorobiphenyl 209, permethrine and simazine in cannabis samples. Using a 100 ?m PDMS fibre, compounds were directly extracted in the headspace mode at 150 °C for 5 min and desorption was performed in the GC injector in the splitless...

  12. Pesticide analysis with the pulsed-flame photometer detector and a direct sample introduction device.

    Science.gov (United States)

    Jing, H; Amirav, A

    1997-04-01

    New methods for fast, sensitive, and informative pesticide analysis in food products are described. These methods are based on sampling with a novel direct sample introduction device (DSI), gas chromatographic analysis, and pesticide detection with the pulsed flame photometric detector (PFPD). Sampling with the DSI is based on introduction of blended fruit or vegetable in a small glass vial that retains the harmful nonvolatile residue and is disposed of after the analysis. The DSI-GC-PFPD combination provides several new features that are demonstrated and discussed:? (a) Extract-free analysis is achieved with the DSI, which serves as an effective alternative to sample extraction and cleanup methods. (b) Faster analysis is achieved through the use of the DSI due to the reduction of the upper GC program temperature, since the low-volatility compounds are retained in the sample vial. (c) Relatively efficient and uniform DSI thermal extraction and PFPD detection can be achieved, allowing the use of internal standards for pesticide calibration. (d) Higher sensitivity is provided by the PFPD as well as through the use of the DSI for sampling larger volumes of extract solutions. (e) Sulfur interference is eliminated with the PFPD in its phosphorus-selective detection mode, using software exploiting differences in S and P delayed pulsed flame emission time dependence. (f) Sulfur pesticides are effectively analyzed by the PFPD in its sulfur-selective detection mode at the usual required levels and with less matrix interference than with NPD in the nitrogen mode. (g) Simultaneous sulfur and phosphorus pesticide analysis is demonstrated, including heteroatom identification and the provision of P and S atom ratio information in the analyzed pesticide. PMID:21639348

  13. 77 FR 59578 - Notice of Filing of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2012-09-28

    ...residues of the insecticide acetamiprid...determine toxic residues. As a result...part 180 for residues of the fungicide...procedure with final determination by HPLC with...tolerance for residues of the insecticide...

  14. 78 FR 33785 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2013-06-05

    ...residues of the insecticide metaflumizone...determine residues of metaflumizone...The final determination of metaflumizone...quantification of residues by liquid...spectrometric determination (LC/MS...part 180 for residues of the insecticide,...

  15. Residuos de plaguicidas organoclorados en 4 tipos de aceites vegetales / Organochlorine pesticide residues in 4 types of vegetable oils.

    Scientific Electronic Library Online (English)

    María, Piñero González; Pedro, Izquierdo Córser; María, Allara Cagnasso; Aiza, García Urdaneta.

    2007-12-01

    Full Text Available SciELO Venezuela | Language: Spanish Abstract in spanish Esta investigación tuvo como objetivos identificar y cuantificar residuos de los plaguicidas organoclorados (POC) hexaclorobenceno (HCB), lindano, cis-clordano, heptacloro, aldrín, dieldrín, endrín y o,p’-diclorodifeniltricloroetano (o,p’-DDT) en aceites de maíz, soya, girasol y mezclas de aceites, [...] que se expenden en la ciudad de Maracaibo, Venezuela. Se analizaron 30 muestras de 4 tipos de aceites de 10 marcas comerciales. La extracción de residuos de POC se realizó según la técnica de la AOAC. Para la identificación y cuantificación se utilizó un cromatógrafo de gases con detector de captura electrónica (GC-ECD), y para la confirmación, un cromatógrafo de gases acoplado a un espectrómetro de masas (GCMS). Todos los residuos de POC investigados fueron detectados en las muestras analizadas. Se detectaron en mayor concentración (mg/ g) aldrín (0,0088), lindano (0,0054) y o,p’-DDT (0,0035). El análisis estadístico demostró diferencias significativas (P Abstract in english The present study had as objectives to identify and to quantify organochlorine pesticide residues (OCP) hexachlorobenzene (HCB), lindane, cis-chlordane, heptachlor, aldrín, dieldrín, endrín and o,p’-DDT in vegetable oils of corn, soybean, sunflower and mixtures of oils, sold in the city of Maracaibo [...] , Venezuela. 30 samples of 4 types of vegetable oils of 10 commercial brands were analyzed. The extraction of OCP residues was done according to the Official Method of AOAC. A gas chromatograph with an electronic capture detector (GC-ECD) was used for identification and quantification of OCP residues and confirmation was done with a gas chromatograph coupled with a mass spectrometer (GC-MS). All the OCP residues investigated were detected in the analyzed samples. Aldrin (0.0088), lindane (0.0054) and o,p’-DDT (0.0035) were the OCP residues detected in higher concentrations (mg/g). The statistical analysis showed significant differences (P

  16. Multiresidue analysis of pesticides in olive oil by gel permeation chromatography followed by gas chromatography-tandem mass-spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez, Andres Garcia [Department of Physical and Analytical Chemistry, E.P.S. of Linares, University of Jaen, E-23700 Linares, Jaen (Spain); Martos, Natividad Ramos [Department of Physical and Analytical Chemistry, Faculty of Sciences, University of Jaen, E-23071 Jaen (Spain); Ballesteros, Evaristo [Department of Physical and Analytical Chemistry, E.P.S. of Linares, University of Jaen, E-23700 Linares, Jaen (Spain)]. E-mail: eballes@ujaen.es

    2006-02-03

    A method for the multiresidue analysis of olive oil samples for 26 pesticides is proposed. Residual pesticides are extracted from oil using an n-hexane/acetonitrile mixture, extracts being cleaned-up by gel permeation chromatography (GPC) for analysis by gas chromatography-tandem mass spectrometry (GC-MS/MS). Electron ionization and chemical ionization are employed in a single analysis for the determination of pesticides. Pesticide recoveries from virgin and refined olive oil spiked with 10, 100 and 250 {mu}g/kg concentrations of the pesticides ranged from 83.8 to 110.3%. The proposed method features good sensitivity: its limits of quantification are low enough to allow pesticide residues to be determined at concentrations below the maximum residue levels legally accepted. The precision, expressed as relative standard deviation, ranges from 4.93 to 8.11%. Applicability was tested on 40 olive oil samples. Several pesticides were detected in most of the virgin olive oil samples. By contrast, refined olive samples contained few pesticides, and only endosulfan sulphate was detected in all.

  17. Organochlorine pesticide residues in sediments from the Uganda side of Lake Victoria.

    Science.gov (United States)

    Wasswa, John; Kiremire, Bernard T; Nkedi-Kizza, Peter; Mbabazi, Jolocam; Ssebugere, Patrick

    2011-01-01

    Organochlorine (OC) residues were analysed in 117 sediment samples collected from four bays of the Uganda side of Lake Victoria. The sediments were collected with a corer at a depth of 0-20 cm, and extracted for OC residues using a solid dispersion method. The extracts were cleaned using gel permeation chromatography and analysed for pesticide residues using a gas chromatograph (GC) equipped with an electron capture detector. The results were confirmed using a GC equipped with a mass spectrometer (MS). A total of 16 OC residues, most of them persistent organic pollutants (POPs) were identified and quantified. The OC residue levels were expressed on an oven dry weight (d.w.) basis. Endosulphan sulphate, in the range of 0.82-5.62 ?g kg?¹ d.w., was the most frequently detected residue. Aldrin and dieldrin were in the ranges of 0.22-15.96 and 0.94-7.18 ?g kg?¹ d.w., respectively. DDT and its metabolites lay between 0.11-3.59 for p,p'-DDE, 0.38-4.02 for p,p'-DDD, 0.04-1.46 for p,p'-DDT, 0.07-2.72 for o,p'-DDE and 0.01-1.63 ?g kg?¹ d.w. for o,p'-DDT. The levels of ?-HCH varied from 0.05 to 5.48 ?g kg?¹ d.w. Heptachlor was detected only once at a level of 0.81 ?g kg?¹ d.w., while its photo-oxidation product, heptachlor epoxide, ranged between non-detectable (ND) to 3.19 ?g kg?¹ d.w. Chlordane ranged from ND to 0.76 ?g kg?¹ d.w. Based on the threshold effect concentration (TEC) for fresh water ecosystems, aldrin and dieldrin were the only OCs that seemed to be a threat to the lake environment. PMID:20947127

  18. Validation of pestice multi residue analysis method on cucumber

    International Nuclear Information System (INIS)

    In this study we aimed to validate the method of multi pesticide residue analysis on cucumber. Before real sample injection, system suitability test was performed in gas chromatography (GC). For this purpose, a sensitive pesticide mixture was used for GC-NPD and estimated the performance parameters such as number of effective theoretical plates, resolution factor, asymmetry, tailing and selectivity. It was detected that the system was suitable for calibration and sample injection. Samples were fortified at the level of 0.02, 0.2, 0.8 and 1 mg/kg with mixture of dichlorvos, malathion and chloropyrifos pesticides. In the fortification step 14C-carbaryl was also added on homogenized analytical portions to make use of 14C labelled pesticides for the determining extraction efficiency. Then the basic analytical process, such as ethyl acetate extraction, filtration, evaporation and cleanup, were performed. The GPC calibration using 14C- carbaryl and fortification mixture (dichlorvos, malathion and chloropyrifos) showed that pesticide fraction come through the column between the 8-23 ml fractions. The recovery of 14C-carbaryl after the extraction and cleanup step were 92.63-111.73 % and 74.83-102.22 %, respectively. The stability of pesticides during analysis is an important factor. In this study, stability test was performed including matrix effect. Our calculation and t test results showed that above mentioned pesticides were not stabile during sample processing in our laboratory conditions and it was found that sample comminution with dry ice may improve stability. In the other part of the study, 14C-chloropyrifos was used to determine homogeneity of analytical portions taken from laboratory samples. Use of 14C labelled pesticides allows us for quick quantification analyte, even with out clean-up. The analytical results show that after sample processing with waring blender, analytical portions were homogenous. Sample processing uncertainty depending on quantity of analytical portions was calculated from sampling constant equation (Ks=WxCVsp2). CVsp for 50 g was 4.539% and 8.033% for 5 g analytical portions.

  19. [Determination of the trace residues of four organochlorine pesticides in agricultural products by high performance liquid chromatography with modified multi-walled carbon nanotubes as solid phase extraction adsorbent].

    Science.gov (United States)

    Peng, Xiaojun; Pang, Jinshan; Deng, Aihua; Liang, Weihua; Liang, Youzhen; Wen, Qijing

    2012-09-01

    A novel method for the simultaneous determination of the trace residues of four organochlorine pesticides such as p,p'-DDD, p,p'-DDT, o,p'-DDT and p,p'-DDE in agricultural products by multi-walled carbon nanotubes (MWNTs) modified by acid oxidation on the surface as solid phase extraction (SPE) adsorbent coupled with high performance liquid chromatography (HPLC) was developed. The effects of the surface acid oxidation, SPE operations and HPLC conditions on the determination of the four pesticide residues were investigated. Under the optimized experimental conditions, the novel method provided wide linear ranges for the pesticides with correlation coefficients of 0. 997 8 - 0. 999 5, the detection limit was 0.050 mg/L for each pesticides. The recoveries from the samples spiked with the pesticide standards at three concentration levels of 0.10, 2.0 and 50 mg/L were in the range of 78% - 104% with the relative standard deviations (RSDs) of 2.7% -7.6%. This study indicated the MWNTs SPE was an efficient clean-up method to agricultural products (included dried orange peel, ginseng, cabbage and tea). The proposed method showed the advantages of accuracy and sensitivity, and can meet the requirements for the determination of low residue pesticide in agricultural products. The study provides a useful method for the analysis of trace substance of agricultural products. PMID:23285982

  20. [Determination of five pyrethroid pesticides residues in Anoectochilus roxburghii by cloud point extraction-back extraction and GC-MS].

    Science.gov (United States)

    Liu, Hong-Bo; Zhao, Xiao-Fang; Shi, Gui-Ying; Shao, Qing-Song; Li, Mine-Van

    2014-08-01

    A method for residual determination of 5 pyrethroid pesticides in Anoectochilus roxburghii by cloud point extraction-back extraction-GC-MS was established. PEG 6000 was used as extraction agent and isooctane was used for back-extractant. The con- tent was calculated by external standard method. The linear range was from 15 to 2 000 ?g x kg(-1) with the good correlation coefficients (0.955-0.999). The recoveries at spiked concentrations of 50-500 ?g x kg(-1) ranged from 85.12% to 101.6%. The limit of detection and quantification of 5 pyrethroid pesticides were in the range of 0.63-3.10 ?g x kg(-1) and 2.10-10.31 ?g x kg(-1), respectively. The proposed method can be applied to the determination of pyrethroid pesticides residues in A. roxburghii. PMID:25507544

  1. Residual levels and identify possible sources of organochlorine pesticides in Korea atmosphere

    Science.gov (United States)

    Park, Jin Soo; Shin, Sun Kyoung; Kim, Woo Il; Kim, Byung Hoon

    2011-12-01

    The nationwide monitoring program was established in 2008 to monitor of persistent organic pollutants (POPs) in Korea. Under this program, it was observed air concentrations of organochlorine pesticides (OCPs) at 37 sites from January to October of 2008, to determine the residue levels and identify possible sources in Korea atmosphere. Samples of OCPs including HCB, aldrin, dieldrin, endrin, p, p'-DDT, o, p'-DDT, p, p'-DDE, o, p'-DDE, p, p'-DDD, o, p'-DDD, trans-chlordane, cis-chlordane, trans-nonachlor, cis-nonachlor, oxychlordane, heptachlor, heptachlor epoxide were collected with high volume air sampler and analyzed by HRGC/HRMS. The concentrations were in the range of 41.2-344.3 pg m -3 for HCB, ND-47.55 pg m -3 for DDTs (sum of p, p'-DDT, o, p'-DDT, p, p'-DDE, o, p'-DDE, p, p'-DDD, o, p'-DDD), ND-38.97 pg m -3 for chlordanes (sum of trans-chlordane, cis-chlordane, trans-nonachlor, cis-nonachlor, oxychlordane), ND-9.19 pg m -3 for heptachlors (sum of heptachlor and heptachlor epoxide) and ND-4.32 pg m -3 for dieldrin. The predominant compound in air was HCB. However, HCB itself has not ever been registered and used as a pesticide in Korea. The elevated concentration of HCB in Korea might be contributed to geographical location and long range transport. For DDTs, it was found that no more fresh input occurred recently and technical type DDTs was prevailing in Korea. Higher concentration of chlordane was observed in winter, which was contributed to the fresh input technical chlordane and long range transport. Relatively lower levels of heptachlor and dieldrin despite much more consumption than other pesticides were resulted from shorter half-lives in environment.

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

    OpenAIRE

    Bas?a C?esnik, Helena; Gregorc?ic?, Ana; Velikonja Bolta, S?pela; 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 (...

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

    OpenAIRE

    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 ?-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 di...

  4. Validation of an Efficient Method for the Determination of Pesticide Residues in Fruits and Vegetables Using Ethyl Acetate for Extraction

    Science.gov (United States)

    In this study, a version of the “quick, easy, cheap, effective, rugged, and safe” (QuEChERS) method was modified to use ethyl acetate (EtOAc) rather than acetonitrile (MeCN) for extraction in the determination of multiple pesticide residues in fruits and vegetables. EtOAc is better suited than MeCN...

  5. Development and validation of methodology for the determination of residues of organophosphorus pesticides in tomatoes

    Scientific Electronic Library Online (English)

    Anagilda B., Gobo; Márcia H. S., Kurz; Ionara R., Pizzutti; Martha B., Adaime; Renato, Zanella.

    2004-12-01

    Full Text Available SciELO Brazil | Language: English Abstract in portuguese Os pesticidas organofosforados são freqüentemente aplicados no cultivo de tomate no Brasil. No presente trabalho uma metodologia analítica foi desenvolvida e validada para a quantificação de resíduos dos pesticidas organofosforados acefato, chlorpyrifós, malation, metamidofós and paration metílico e [...] m tomate, empregando Cromatografia Gasosa com Detector de Nitrogênio e Fósforo (GC-NPD). A possibilidade de ocorrência de efeito matriz foi estudada. As curvas analíticas, preparadas nos extratos da matriz, foram lineares de 0,006 até 0,80 mg L-1. Os estudos de precisão forneceram resultados com RSD Abstract in english The organophosphorus pesticides are frequently applied in tomato cultivation in Brazil. In the present work an analytical methodology for quantification of the organophosphorus pesticides: acephate, chlorpyrifos, malathion, methamidophos and parathion-methyl residues in tomatoes was developed and va [...] lidated using Gas Chromatography with a Nitrogen-Phosphorus Detector (GC-NPD). The possibility of a matrix effect was studied. Analytical curves prepared in an extract of the matrix were linear from 0.006 to 0.80 mg L-1. The precision studies supplied results with RSD

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

    Science.gov (United States)

    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, ?-HCH, ?-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

  7. Intra uterine growth retardation: association with organochlorine pesticide residue levels and oxidative stress markers.

    Science.gov (United States)

    Pathak, Rahul; Mustafa, M D; Ahmed, Tanzeel; Ahmed, Rafat S; Tripathi, A K; Guleria, Kiran; Banerjee, B D

    2011-05-01

    Intra uterine growth retardation (IUGR) is a major complication of pregnancy, affecting ?5% to 10% of newborns. Hexachlorocyclohexane (HCH) is an organochlorine pesticide that consists of eight stereoisomers and ?-isomer is the only isomer that possesses insecticidal activity. The aim of the present study was to analyze the OCP residues in maternal and cord blood of women and to assess the level of oxidative stress markers as well as to establish correlation with OCP levels. Fifty women delivering neonates with low birth weight (IUGR) and equal number of women delivering normal birth weight babies (control) were recruited. We have observed higher levels of ?-HCH and T-HCH and increased oxidative stress markers in IUGR subjects versus control subjects. Significant correlations were also found between HCH isomers and oxidative stress markers in IUGR subjects. In conclusion, our results suggest that higher levels of HCH isomers may be associated with IUGR and increased oxidative stress. PMID:21338667

  8. Study of the effect of gamma irradiation on phenolic compounds and pesticides residues

    International Nuclear Information System (INIS)

    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

  9. The determination of pesticide residues in local vegetables by means of neutron activation technique

    International Nuclear Information System (INIS)

    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

  10. Effect of ?- ray, Microwave Heating and Solar Irradiation of Apple Juice on Organochlorinated Pesticides Residues

    Directory of Open Access Journals (Sweden)

    K. Al-Ismail

    2009-01-01

    Full Text Available This study was conducted to evaluate the effect of solar radiation, microwave heating and ?-irradiation on the Organochlorinated Pesticide (OCP's in apple juice. The solar radiation caused a destruction of 20% after 20 hr exposure to sunlight compared to 12% reduction for the tested OCP's after microwave heating for 10 min. On the other hand, the use of ?- irradiation leads to a degradation percentage of 30% after treatment with 25 kGray, while the irradiation with 5 kGray was found to produce insignificant effect on OCP?s residues when compared with the control treatments. The degradation was found to increase with increasing exposure time and all treatments were found to be not effective in complete destruction of OCP?s.

  11. 77 FR 15012 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2012-03-14

    ...validated. The method involves solvent extraction followed by liquid- liquid partitioning...0.01 ppm. Aqueous organic solvent extraction, column clean up, and quantitation...the biochemical pesticide polyoxin D zinc salt when used as a fungicide for...

  12. Development of a fieldable rapid pesticide exposure analysis sensing system

    Science.gov (United States)

    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.

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

    DEFF Research Database (Denmark)

    Uthuppu, Basil; Kostesha, Natalie

    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 haptens and compared the affinity constants of the antibody towards this library. Furthermore, since regeneration of the BAM-hapten surface is a prerequisite for the development of a real-time electrochemical sensor with immunoassay-based detection, studies on regeneration of surfaces, modified with the newly synthesized BAM-haptens has been preformed and compared and correlated to the measured affinity constants. By using conventional ELISA we were able to indicate that one of the immobilized BAM haptens with an intermediate affinity towards the anti-BAM antibody was better in terms of regeneration. Design and fabrication of a fully automated microfluidic based on this immunoassay and electrochemical detection are in progress.

  14. Disposal and Treatment Methods for Pesticide Containing Wastewaters: Critical Review and Comparative Analysis

    Directory of Open Access Journals (Sweden)

    Mariam T. Al Hattab

    2012-05-01

    Full Text Available Pesticides provide the primary means for controlling organisms that compete with man for food and fibre or cause injury to man, livestock and crops. They played a vital role in the economic production of wide ranges of vegetable, fruit, cereal, forage, fibre and oil crops which now constitute a large part of successful agricultural industry in many countries. After application to the target areas, pesticide residues are removed from applicators by rinsing with water which results in the formation of a toxic wastewater that represents a disposal problem for many farmers. Pesticides can adversely affect people, pets, livestock and wildlife in addition to the pests they are intended to destroy. The phenomenon of biomagnification of some pesticides has resulted in reproductive failure of some fish species and egg shell thinning of birds such as peregrine falcons, sparrow hawk and eagle owls. Pesticide toxicity to humans include skin and eye irritation and skin cancer. Therefore, care must be exercised in the application, disposal and treatment of pesticides. Currently, disposal of pesticide wastewater is carried out by: 1 land cultivation, 2 dumping in soil pits, plastic pits and concrete pits or on land and in extreme cases in streams near the rinsing operation, 3 use of evaporation beds and 4 land filling. These methods of disposal are unsafe as the surface run off will reach streams, rivers and lakes and the infiltration of the wastewater into the local soil will eventually reach ground water. The treatment methods currently used for pesticide wastewater include: 1 incineration (incinerators and open burning, 2 chemical treatments (O3/UV, hydrolysis, Fenton oxidation and KPEG, 3 physical treatments (inorganic, organic absorbents and activated carbon and 4 biological treatments (composting, bioaugmentation and phytoremediation. Therefore, the choice of safe, on farm disposal techniques for agricultural pesticides is very important. A comparative analysis was performed on 18 methods of pesticide disposal/treatment using six criteria: containment, detoxification ability, cost, time, suitability for on farm use, size and evaporation efficiency. The results indicated that of the 18 methods evaluated, 9 scored above 80/100 and can be used on farm. They were organic absorbents (97, composting (94, bioaugmentation (92, inorganic absorbents (90, Fenton oxidation (86, O3/UV (83, activated carbon (82, hydrolysis (82, and land cultivation (80. The other methods are not suitable for on farm use as they suffered from containment problems, high cost and variability of effectiveness.

  15. 76 FR 10584 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2011-02-25

    ...for residues of the insecticide etoxazole, 2...CFR part 180 for residues of the insecticide thiamethoxam (CAS...cleanup procedures and determination by liquid chromatography...CFR 180.441 for residues of the...

  16. 78 FR 63938 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2013-10-25

    ...40 CFR part 180 for residues of the fungicide trifloxystrobin...cleanup procedures and determination by GC-NPD. A newer...40 CFR part 180 for residues of the herbicide saflufenacil...is established for residues of the insecticide prallethrin,...

  17. 75 FR 14154 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2010-03-24

    ...available for residue data collection...CFR part 180 for residues of the insecticide thiamethoxam...procedures and determination by liquid chromatography...CFR part 180 for residues of the insecticide amitraz, in...

  18. 75 FR 32463 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2010-06-08

    ...at 25 ppm. Residues of flutolanil...LC/MS Determination of Flutolanil...part 180 for residues of the insecticide spiromesifen...part 180 for residues of the insecticide thiamethoxam...procedures and determination by...

  19. Distribution of pesticide residues in rice grain and in its coproducts

    Scientific Electronic Library Online (English)

    Giniani C., Dors; Ednei G., Primel; Carlos A. A., Fagundes; Carlos H. P., Mariot; Eliana, Badiale-Furlong.

    1921-19-01

    Full Text Available Os agrotóxicos são usados em muitas culturas para prevenir e preservar os grãos de possíveis ataques de pragas. O objetivo deste trabalho foi avaliar a distribuição dos agrotóxicos bispiribaque de sódio, carbofurano, clomazona e tebuconazol nas diferentes frações do arroz beneficiado (arroz branco, [...] farelo de arroz, arroz com casca, arroz parboilizado beneficiado, farelo de arroz parboilizado e arroz parboilizado com casca), o qual foi cultivado em campos experimentais sob condições controladas de aplicação. Para tanto, o método QuEChERS foi otimizado para a extração dos agrotóxicos e validou-se um método utilizando CLAE-DAD para quantificação e CL-EM para confirmação. O método QuEChERS modificado foi adequado na extração dos agrotóxicos, bem como as condições cromatográficas para identificação e quantificação, conforme os indicativos de eficiência determinados: LOD de 0,07 mg kg-1 e LOQ de 0,2 mg kg-1 para a mistura dos agrotóxicos, e recuperação para arroz e farelo de arroz de 119 e 116%, 84 e 119%, 113 e 96%, 103 e 97% para carbofurano, bispiribaque de sódio, clomazona e tebuconazol, respectivamente. O método desenvolvido foi aplicado nas frações do beneficiamento e o farelo apresentou maior concentração de resíduo dos agrotóxicos, quando comparado ao arroz beneficiado, sendo 8,0, 2,3, 2,2 e 1,6 vezes mais contaminado, em média, para tebuconazol, clomazona, carbofurano e bispiribaque de sódio, respectivamente. Apenas o clomazona e o tebuconazol apresentaram concentrações dentro do limite aceitável estabelecidos pelo Codex Alimentarius (0,1 mg kg-1) para o arroz beneficiado nas safras analisadas. Abstract in english Pesticides are used to prevent pests from attacking grains in order to preserve the crops. This paper aims at evaluating the distribution of the pesticides bispyribac-sodium, carbofuran, clomazone and tebuconazole in different fractions of milled rice (white rice, rice bran, husked rice, parboiled r [...] ice, parboiled rice bran, and husked parboiled rice) which is planted on experimental fields under controlled conditions. The QuEChERS method was adapted to the extraction of pesticides and validated by using HPLC-DAD for quantification and LC-MS for confirmation. The analytical method of extracting pesticides, as well as the chromatographic conditions for identification and quantification, were suitable, according to certain efficiency indicators: 0.07 mg kg-1 LOD and 0.2 mg kg-1 LOQ for the mixture of pesticides and rice and rice bran recoveries of 119 and 116%, 84 and 119%, 113 and 96%, 103 and 97% for carbofuran, bispyribac-sodium, clomazone and tebuconazole, respectively. The method under development was applied to rice fractions: bran had the highest residue concentration of the studied pesticides, when compared to milled rice, showing 8.0, 2.3, 2.2 and 1.6 times more contamination, in average, with tebuconazole, clomazone, carbofuran and bispyribac-sodium, respectively. Only clomazone and tebuconazole were in the acceptable limits established by Codex Alimentarius (0.1 mg kg-1) for milled rice.

  20. [Survey of PCB and organochlorine pesticide residues in meats and processed meat products collected in Osaka, Japan].

    Science.gov (United States)

    Matsumoto, Hisashi; Kuwabara, Katsuyoshi; Murakami, Yasuyuki; Murata, Hiroshi

    2006-06-01

    Residues of PCB and organochlorine pesticides in meats (beef, pork and poultry) and processed meat products collected in Osaka, Japan were surveyed. For 35 years from 1970 to 2004, the concentrations of PCB, HCH isomers, DDT analogues and dieldrin in all meats appeared to decline with each passing year. The concentration of each isomer of HCH in all meats declined rapidly from the early to the late 1970's and showed a gentle decline thereafter; beta-HCH showed the highest residue rate of the isomers in all the time periods surveyed, except for pork and poultry samples in the early 1980's. The concentrations of DDT analogues in all meats also showed sharp declines from the late 1970's to the early 1980's, followed by a smaller decrease thereafter; the main residues were pp'-DDD, p,p'-DDE and p,p'-DDT, and the residue rate of p,p'-DDE increased over the years. The residue levels of organochlorine pesticides in processed meat products (raw materials: beef, pork, poultry and mixture of ground beef and pork) were surveyed for 15 years (from 1990 to 2004) and there were no significant differences in the values among the materials. The concentrations of each pesticide in processed meat products tended to be lower than those of the corresponding meat samples, respectively. PMID:16862991

  1. Pesticide residues in fruits and vegetables from Pakistan: a review of the occurrence and associated human health risks.

    Science.gov (United States)

    Syed, Jabir Hussain; Alamdar, Ambreen; Mohammad, Ashiq; Ahad, Karam; Shabir, Zunera; Ahmed, Haroon; Ali, Syeda Maria; Sani, Syed Gul Abbas Shah; Bokhari, Habib; Gallagher, Kevin D; Ahmad, Iftikhar; Eqani, Syed Ali Musstjab Akber Shah

    2014-12-01

    The main objective of the review is to document, assess and analyze the results of the previously reported data on levels of different pesticides in selected fruits and vegetables from Pakistan. The findings of the previous studies clearly indicated that more than 50 % of the samples were contaminated with organophosphate, pyrethroids and organochlorine pesticides. Many studies reported that among fresh fruits and vegetables tomato, apple, melon, mango, grapes, and plum crossed the FAO/WHO permissible limits for these contaminants residual levels. The comparison of other regions showed that observed levels were found above maximum residue limits (MRLs) in 50 % of the samples but were in agreement with the studies from neighboring countries like China and Bangladesh. Higher hazard risk index (HRI) values were calculated for dieldrin, methamidophos, o,p'-DDT, diazinon and p,p'-DDT in apple, mango, banana, melon, potato and onion. The review also highlights that data on pesticide residues in foodstuff is scarce which should be overcome by further extending studies from different areas of Pakistan. In order to ascertain the provision of food suitable for human consumption, it is imperative to monitor pesticides in food commodities by the country's authorities and enforce guidelines based on permissible limits. PMID:24958529

  2. Use of simultaneous dual-probe microdialysis for the determination of pesticide residues in a jade plant (Crassula ovata).

    Science.gov (United States)

    Zhou, Simon Ningsun; Oakes, Ken D; Servos, Mark R; Pawliszyn, Janusz

    2009-04-01

    A microdialysis application for the sampling of plant pesticide residues has been developed utilizing two probes with differing perfusate rates simultaneously inserted into symmetric components of a sampling system. A simple empirical equation is proposed to calculate analyte concentrations in a semi-solid matrix using two different dialysate concentrations. In vitro application yielded excellent correlations between the calculated and spiked concentrations. Subsequent in vivo application of this technique for the determination of pesticide distributions in leaves of a jade plant (Crassula ovata) indicated the utility of this approach in complex living matrices. PMID:19305926

  3. Evaluation of low-pressure gas chromatography-tandem mass spectrometry method for analysis of greater than 140 pesticides in fish

    Science.gov (United States)

    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...

  4. Spectrum of Organochlorine Pesticide Residues in Fish Samples from the Densu Basin

    Directory of Open Access Journals (Sweden)

    Samuel Afful

    2010-07-01

    Full Text Available In this study, the levels of organochlorine pesticide residues in the Densu basin have been investigated using fish sam ples as a case study. Six fish species namely Heterotis niloticus, Channa obscura, Hepsetus odoe, Tilapia zilli, Clarias gariepinus and Chrysichthys nigrodigitatus were collected from the sampling towns, Weija and Nsawam along the Densu river basin in the Greater Accra Region of Ghana. Composite samples w ere homogenized, freeze dried and ground to obtain powdered samples. The powdered samples were extracted by soxhlet extraction procedure using (3:1 hexane: acetone mixture. The extracts were cleaned-up using florisil adsorbent and characterized for organochlorine content using Gas Chromatography (GC equipped with Electron Capture Detector (ECD. The GC recoveries of spiked samples were between 80 to 96%. Fourteen organochlorines (OCs namely gamma-HCH, delta-HCH, heptachlor, aldrin, gammachlordane, p,p’-DDE, alpha-endosulfan, dieldrin, endrin, endrin-aldehyde, endosulfan-sufate, p,p’-DDT, endrinketone and methoxychlor were identified and quantified. A 100% incidence was recorded for gamma-HCH, delta-HCH, heptachlor, aldrin, gamma-chlordane, alpha-endosulfan, dieldrin and p,p’-DDT, while 75% incidence was recorded for the metabolites, p,p’-DDE and endosulfan-sulfate. The concentrations of OCs ranged from 0.3 to 71.3 :g/kg and were however, below the Australian Maximum Residue Limits (MRL of 50 to 1000 :g/kg for fresh w ater fish.

  5. Resíduos de agrotóxicos em frutos de tomate / Pesticide residues in tomato fruits

    Scientific Electronic Library Online (English)

    Leslie Maria Segura, Zavatti; Rosângela Blotta, Abakerli.

    1999-03-01

    Full Text Available SciELO Brazil | Language: Portuguese Abstract in portuguese 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 du [...] rante 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. Abstract in english 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 in [...] gredient residues and evaluating the contamination level of the fruits. The components analised were: methamidophos, chlorpyrifos, captan, chlorothalonil, endosulfan, lambda-cyhalothrin and copper oxychloride. In order to evaluate the contamination level, a multiresidue method was validated. The residues found were from fungicides and insecticides used during the frutification and maturation stages of the crop: captan, 0.35 mg/kg, at Farm 2; chlorothalonil, 0.16 mg/kg and 0.95 mg/kg, at Farms 1 and 2, respectively; lambda-cyhalothrin, 0.03 mg/kg, at Farm 2; copper, 2.03 mg/kg, 3.75 mg/kg and 1.44 mg/kg, at Farms 1, 2 and 3, respectively, and 0.95 mg/kg, 1.70 mg/kg and 2.31 mg/kg, at Farm 4. Residues of organophosphorous components applied mainly during the vegetative growing were not found. There was no contamination in the tomatos. The residues to be monitored are those from the pesticides used in the crop maturation stage.

  6. Resíduos de agrotóxicos em frutos de tomate Pesticide residues in tomato fruits

    Directory of Open Access Journals (Sweden)

    Leslie Maria Segura Zavatti

    1999-03-01

    Full Text Available O uso intensivo de agrotóxicos em culturas de tomates tem causado preocupações quanto à provável contaminação do produto final. Este trabalho teve como objetivo monitorar, por dois anos consecutivos, em quatro propriedades de uma área altamente tecnificada, o uso de agrotóxicos em tomate irrigado durante seu desenvolvimento, quantificar os resíduos dos principais princípios ativos utilizados, e avaliar o grau de contaminação dos frutos colhidos. Foram analisados metamidofós, clorpirifós, captan, clorotalonil, endosulfan, lambda-cialotrina, e cobre. Para avaliar o grau de contaminação dos frutos foi validado um método de análise de resíduos múltiplos capaz de quantificar esses compostos. Os resíduos encontrados foram de fungicidas e inseticidas aplicados nas fases de frutificação e maturação: captan, 0,35 mg/kg, na Fazenda 2; clorotalonil, 0,16 mg/kg e 0,95 mg/kg, nas Fazendas 1 e 2, respectivamente; lambda-cialotrina, 0,03 mg/kg, na Fazenda 2; cobre, 2,03 mg/kg, 3,75 mg/kg e 1,44mg/kg, nas Fazendas 1, 2 e 3, respectivamente, e 0,95 mg/kg, 1,70 mg/kg e 2,31 mg/kg, na Fazenda 4. Não ocorreram resíduos dos inseticidas organofosforados, aplicados principalmente durante o desenvolvimento vegetativo da cultura. Não houve contaminação dos tomates pelos agrotóxicos analisados. Os resíduos que devem ser monitorados são os dos agrotóxicos aplicados na fase de maturação da cultura.The intensive use of pesticide in tomato crops have been causing concern about a possible contamination of the final product. This work aimed at monitoring, for two years, in four farms located in a high technology area, the use of pesticides in irrigated tomato crops, quantifying the main active ingredient residues and evaluating the contamination level of the fruits. The components analised were: methamidophos, chlorpyrifos, captan, chlorothalonil, endosulfan, lambda-cyhalothrin and copper oxychloride. In order to evaluate the contamination level, a multiresidue method was validated. The residues found were from fungicides and insecticides used during the frutification and maturation stages of the crop: captan, 0.35 mg/kg, at Farm 2; chlorothalonil, 0.16 mg/kg and 0.95 mg/kg, at Farms 1 and 2, respectively; lambda-cyhalothrin, 0.03 mg/kg, at Farm 2; copper, 2.03 mg/kg, 3.75 mg/kg and 1.44 mg/kg, at Farms 1, 2 and 3, respectively, and 0.95 mg/kg, 1.70 mg/kg and 2.31 mg/kg, at Farm 4. Residues of organophosphorous components applied mainly during the vegetative growing were not found. There was no contamination in the tomatos. The residues to be monitored are those from the pesticides used in the crop maturation stage.

  7. Statistical assessment of organochlorine pesticides residues in surface water penetrated into caspian sea

    International Nuclear Information System (INIS)

    Multivariate statistical techniques, such as factor analysis (FA) and discriminant analysis (DA) were used for evaluation of temporal/spatial variations and interpretation of organochlorine pesticides (OCPs) data from Shiroud River (Iran). Eight sites were selected along the river and fifteen OCPs components were measured. FA was applied to determine the interrelationship between various variables and also to identify any possible pollution sources. FA has identified six factors were responsible for explaining 73.39 % of the total variance in OCPs data. DA has identified tour discriminant functions (DFs) responsible for spatial variations and two DFs were responsible for temporal variations. It has provided important information about allocation of all observations, since more than 80 % correct assignations in spatial analysis and 76 % correct assignations in temporal analysis DA indicates that some parameters contribute highly in discriminating the eight sites and also in discriminating the four seasons for both spatial/temporal and OCPs variations. (author)

  8. Study On The Procedures For Determining Of Pesticide Residues In Green Vegetables

    International Nuclear Information System (INIS)

    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)

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

    Science.gov (United States)

    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?salmon compared with wild salmon. Concentrations were positively correlated with 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?>?10?). Surprisingly, less hydrophobic pesticides such as hexachlorocyclohexanes and endosulfans (K(OW) s?salmon species (BMFs?>?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 Columbian salmon is found to be low relative to United States national average per capita total exposure levels and provisional tolerable daily intakes. PMID:21898562

  10. Optimization of analitycal control over residues of active ingridients of modern pesticides in reservoirs water

    Directory of Open Access Journals (Sweden)

    Semenenko V.M.

    2013-10-01

    Full Text Available A highly sensitive and selective method of pyraclostrobin, boscalid, tebufenpyrad and prohexadione-calcium determination under their combined presence in water sample, using high-performance liquid chromatography was developed. On the base of mentioned active ingredients (combined fungicide Bellis, insecto-acaricide Masai and plant growth regulator Regalis pesticides may be used in one vegetation season for fruit trees protection. Method of co-determination of these substances is based on the preparation of water samples for extraction, extraction of pyraclostrobin, boscalid, tebufenpyrad and prohexadione-calcium, concentrating of extract of substances mixtures and chromatographic determination with ultraviolet detection. A distinctive feature of this method is changing of ratio of components of mobile phase (mixture of acetonitrile and 0,1 % aqueous solution of phosphoric acid in the process of chromatographic analysis, which allowed to clearly visualize test substances in case of their joint presence in one sample. Implementation of developed and patented method into practice optimizes control over application of pesticides in agriculture and their monitoring in reservoirs water by significant acceleration of analysis and reduction of expenses in its carying out.

  11. 76 FR 82238 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2011-12-30

    ...pesticide petitions filed under section 408 of the Federal Food, Drug, and Cosmetic Act (FFDCA), 21 U.S.C. 346a, requesting...chromatography/tandem mass spectrometry (LC/MS/MS) with an electrospray interface, operated in a positive ion mode. Contact:...

  12. Validation of a multi-residue method for the determination of residuals pesticides in cabbage (Brassica Oleracea var. Capitata) for gases chromatography

    International Nuclear Information System (INIS)

    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 (? - 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. Awareness of pesticide residues in locally available food and condiments among food sellers: a case study of Osun state, Nigeria

    Directory of Open Access Journals (Sweden)

    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.

  14. Organophosphorus pesticide residues in vegetables from farms, markets, and a supermarket around Kwan Phayao Lake of Northern Thailand.

    Science.gov (United States)

    Sapbamrer, Ratana; Hongsibsong, Surat

    2014-07-01

    This study investigated organophosphorus (OP) residues in vegetables from 27 farms, 106 markets, and 1 supermarket around Kwan Phayao Lake, Northern Thailand, between August and September 2013. Types of vegetables sampled were all vegetables cultivated or sold around the study site. The most common OP pesticides detected in farm samples were chlorpyrifos (50 %), malathion (31.8 %), monocrotophos (31.8 %), diazinon (13.6 %), omethoate (13.6 %), and dicrotophos (9.1 %). The most common OP pesticides detected in market samples were chlorpyrifos (33.9 %), diazinon (18.6 %), parathion-methyl (3.4 %), profenofos (3.4 %), primiphos-ethyl (3.4 %), and fenitrothion (1.7 %). The OP pesticides detected in supermarket samples were chlorpyrifos (33.3 %), and diazinon (66.7 %). Among the compounds detected, chlorpyrifos was detected in most of the vegetable samples from all sources. The highest chlorpyrifos level in farm samples were found in lemon balm (2.423 mg/kg) followed by Vietnamese coriander (0.835 mg/kg), and cowpea (0.027 mg/kg). The highest level in markets samples were found in garlic (7.785 mg/kg) followed by Chinese cabbage (2.864 mg/kg) and Vietnamese coriander (1.308 mg/kg). Residues from supermarket samples were found only in parsley (0.027 mg/kg). The findings showed that 16 samples (59.3 %) from farms and 14 samples (13.2 %) from markets contained OP residues at or above the maximum residue limits established by the European Union. It is concluded that awareness, safety education, and strict regulation of pesticide use are necessary. PMID:24609615

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

    OpenAIRE

    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 ?-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) obtai...

  16. 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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  17. Organochlorine pesticide residue levels and oxidative stress in preterm delivery cases.

    Science.gov (United States)

    Pathak, Rahul; Suke, Sanvidhan G; Ahmed, Tanzeel; Ahmed, Rafat S; Tripathi, A K; Guleria, Kiran; Sharma, C S; Makhijani, S D; Banerjee, B D

    2010-05-01

    A number of studies have focused attention on various biochemical abnormalities evoked due to exposure to organochlorine pesticides (OCPs). The aim of the present study was to analyze the OCP residues in maternal and cord blood of women and assess the levels of different non-enzymatic oxidative stress markers as well as to establish correlation with OCP levels, if any. Thirty women in each group of full-term delivery (FTD; > or =37 weeks of gestation) and preterm delivery (PTD; Levels of OCPs like Hexachlorocyclohexane (HCH), endosulfan, p,p(') Dichlorodiphenyldichloroethylene (DDE) and p,p' Dichlorodiphenyltrichloroethane (DDT) were analyzed by gas chromatography. Non-enzymatic oxidative stress was measured by the quantification of malondialhyde (MDA), protein carbonyl, reduced glutathione (GSH) and ferric-reducing ability of plasma (FRAP). MDA and protein carbonyl levels were increased significantly, while the levels of GSH and FRAP were decreased in PTD in comparison to FTD cases. We have observed higher levels of beta-HCH and alpha-endosulfan and increased oxidative stress in PTD than FTD cases. In PTD cases, a significant positive correlation was observed between maternal blood levels of beta-HCH and MDA (r = .78), beta-HCH and GSH (r = -.65), gamma-HCH and MDA (r = .89), gamma-HCH and GSH (r = -.74) and alpha-endosulfan and MDA (r = .54) in PTD cases. We also found significant correlations between cord blood levels of beta-HCH and MDA (r = .59), beta-HCH and GSH (r = -.69), gamma-HCH and MDA (r = .62) and alpha-endosulfan and MDA (r = .54) in PTD cases. In conclusion, our results suggest that higher levels of some of the OCP residues may be associated with PTD and increased oxidative stress. PMID:20385707

  18. Residue levels of organochlorine pesticides in cattle meat and organs slaughtered in selected towns in West Shoa Zone, Ethiopia.

    Science.gov (United States)

    Letta, Bayessa D; Attah, Louis E

    2013-01-01

    Residue levels of organochlorine pesticides (OCP) in a total of 90 cattle samples comprising meat, liver and kidney collected from carcasses slaughtered in six towns in West Shoa Zone, Ethiopia, (Ambo, Guder, Ginchi, Gedo, Holeta and Tikur Inchini), have been determined. The pesticides were extracted by solid phase extraction (SPE) and quantification was carried out using gas chromatography-mass spectrometry (GC-MS). A good linearity (r(2) > 0.998) was found in the range 0.001-7.00 mg/kg for the samples studied. Most of the pesticides had recoveries in the range 81-99% and values of relative standard deviation (RSD) level of the studied organochlorines followed the order: p, p' dichloro-diphenyl-trichloroethane (DDT) > endosulfan>o,p'-DDT >lindane>dieldrin>endrin>aldrin>chlorothanolin while the order of contamination in the analyzed organs was liver > kidney > meat. Heat treatment of the meat, kidney and liver samples (boiling for 90 min.) produced an overall reduction of 62.2%, 44.5%, 37.7%, 29%, 31%, 34.3% and 30.8% in lindane, o, p'-DDT, endosulfan, p, p'-DDT, chlorothanolin, aldrin, dieldrin, and endrin, respectively. Although the residual contents of the organochlorines detected in all the contaminated samples analyzed from the six cities were below the respective maximal permissible levels set by international organizations, samples from Holeta town were more contaminated and may necessitate effective monitoring as bioaccumulation of these residues may pose health problems in human beings. PMID:23030437

  19. Study on Biodegradation of Pesticide Residue in Environment by Bacterial Consortiam

    International Nuclear Information System (INIS)

    The microbial consortium isolated from soil samples of paddy fields in Japan and were shown to have capability in degrading both carbendazim fungicide (methyl-2-benzimidazole; MBC) and 2,4D herbicide (2,4-dichlorophenoxyacetic acid) were determined for its ability to degrade both chemicals accumulated in water samples collected from paddy fields in the Central part of Thailand. It was found that the consortium was able to degrade 10 ? MBC and 1 mM 2,4-D in those samples. Two isolates from the group of bacterial strains purified from this consortium could degrade approximately 99% of 1 mM 2,4-D within 7 days. Identification by using 16S rDNA sequencing method revealed that both isolates are Achrobobacter xylosoxidans. Improvement of their 2,4-D biodegradation ability was carreid degrading ability in water and soil samples collected from paddy fields in Thailand. The preliminary results showed that the microbial consortium from paddy field in Japan and the mutant strains could be applied for biodegradation of pesticide residues accumulated in paddy fields in our country.

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

    Science.gov (United States)

    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 ?-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.

  1. Residues and Characteristics of Organochlorine Pesticides in the Surface Water in the Suburb of Beijing

    Science.gov (United States)

    CHEN, Jiawei; LIU, Chen; YANG, Zhongfang; WANG, Jiyuan

    Organochlorine Pesticides (OCPs), such as DDT and HCH, have stable chemical properties and less biodegradability. As a kind of persistent organic pollutants, they have high risk to the environment and human health. Although DDT and HCH have been prohibited in China since 1983, they are still found in some soil and water nowadays. Water resource is very important in natural environment and essential for agriculture. The existence of OCPs in some surface water in Beijing has been detected with different levels according to previous investigations. In recent years, many measures have been taken to control the pollution and to monitor the environment, and more attention has been paid to the status of surface water today. In this study, the water samples were collected from the Wenyu, Beiyun, Yanqing, Fangshan, Changping, and Shunyi Rivers in the suburb of Beijing, and the residues and characteristics of DDT and HCH were studied. The results showed that the contents of DDTs and HCHs were ND-13.98 ng/L and 3.87-146.42 ng/L, respectively. According to the indicators of the ratio values of (DDD+DDE)/DDT and ?-HCH/?-HCH, the source of pollution and its potential risk are also discussed in this article.

  2. Estimation of sampling uncertainty for pesticide residues in root vegetable crops.

    Science.gov (United States)

    Farkas, Zsuzsa; Horváth, Zsuzsanna; Kerekes, Kata; Ambrus, Árpád; Hámos, András; Szabó, Mária Szeitzné

    2014-01-01

    The sampling uncertainty for pesticide residues in carrots, parsley leaves and selected medium size crops was estimated with simple random sampling by applying range statistics. The primary samples taken from treated fields consisted of individual carrots or a handful of parsley leaves. The samples were analysed with QUEChERs extraction method and LCMS/MS detection with practical LOQ of 0.001 mg/kg. The results indicate that the average sampling uncertainties estimated with simple random sampling and range statistics were practically the same. The confidence interval for the estimated sampling uncertainty decreased with the number of replicate samples taken from one lot and the number of lots sampled. The estimated relative ranges of sampling uncertainty are independent from the relative standard deviation of the primary samples. Consequently the conclusions drawn from these experiments are generally applicable. There is no optimum for sample size and number of lots to be tested for estimation of sampling uncertainty. Taking a minimum of 6 replicate samples from at least 8-12 lots is recommended to obtain a relative 95% range of sampling uncertainty within 50%. The cost of sampling/analyses, the consequences of wrong decision should also be taken into account when a sampling plan is prepared. PMID:24138463

  3. Pesticide, PCB, and lead residues and necropsy data for bald eagles from 32 states-1978-81.

    Science.gov (United States)

    Reichel, W L; Schmeling, S K; Cromartie, E; Kaiser, T E; Krynitsky, A J; Lamont, T G; Mulhern, B M; Prouty, R M; Stafford, C J; Swineford, D M

    1984-12-01

    In 1978-81, 293 bald eagles (Haliaeetus leucocephalus) from 32 states were necropsied and analyzed for organochlorine pesticides, polychlorinated biphenyls (PCB), and lead residues. DDE was found in all carcasses; PCB, DDD, trans-nonachlor, dieldrin and oxychlordane were next in order of percent frequency of detection. The median levels of DDE and PCB have declined when compared with previous collections. Five specimens contained high levels of dieldrin in their brains which may have contributed to their deaths. Seventeen eagles contained liver lead residues greater than 10 ppm and probably died of lead poisoning. Trauma and shooting are the most common causes of death. PMID:24257866

  4. Pesticide, PCB, and lead residues and necropsy data for bald eagles from 32 states - 1978-81

    Science.gov (United States)

    Reichel, W.L.; Schmeling, S.K.; Cromartie, E.; Kaiser, T.E.; Krynitsky, A.J.; Lamont, T.G.; Mulhern, B.M.; Prouty, R.M.; Stafford, C.J.; Swineford, D.M.

    1984-01-01

    In 1978?81, 293 bald eagles (Haliaeetus leucocephalus) from 32 states were necropsied and analyzed for organochlorine pesticides, polychlorinated biphenyls (PCB), and lead residues. DDE was found in all carcasses; PCB, DDD, trans-nonachlor, dieldrin and oxychlordane were next in order of percent frequency of detection. The median levels of DDE and PCB have declined when compared with previous collections. Five specimens contained high levels of dieldrin in their brains which may have contributed to their deaths. Seventeen eagles contained liver lead residues greater than 10 ppm and probably died of lead poisoning. Trauma and shooting are the most common causes of death.

  5. Pesticide, PCB, and lead residues and necropsy data for bald eagles from 32 states, 1978-81

    Science.gov (United States)

    Reichel, W.L.; Schmeling, S.K.; Cromartie, E.; Kaiser, T.E.; Krynitsky, A.J.; Lamont, T.G.; Mulhern, B.M.; Prouty, R.M.; Stafford, C.J.; Swineford, D.M.

    1984-01-01

    In 1978a??81, 293 bald eagles (Haliaeetus leucocephalus) from 32 states were necropsied and analyzed for organochlorine pesticides, polychlorinated biphenyls (PCB), and lead residues. DDE was found in all carcasses; PCB, DDD, trans-nonachlor, dieldrin and oxychlordane were next in order of percent frequency of detection. The median levels of DDE and PCB have declined when compared with previous collections. Five specimens contained high levels of dieldrin in their brains which may have contributed to their deaths. Seventeen eagles contained liver lead residues greater than 10 ppm and probably died of lead poisoning. Trauma and shooting are the most common causes of death.

  6. Hair decontamination procedure prior to multi-class pesticide analysis.

    Science.gov (United States)

    Duca, Radu-Corneliu; Hardy, Emilie; Salquèbre, Guillaume; Appenzeller, Brice M R

    2014-06-01

    Although increasing interest is being observed in hair analysis for the biomonitoring of human exposure to pesticides, some limitations still have to be addressed for optimum use of this matrix in that specific context. One main possible issue concerns the need to differentiate chemicals biologically incorporated into hair from those externally deposited on hair surface from contaminated air or dust. The present study focuses on the development of a washing procedure for the decontamination of hair before analysis of pesticides from different chemical classes. For this purpose, three different procedures of artificial contamination (with silica, cellulose, and aqueous solution) were used to simulate pesticides deposition on hair surface. Several washing solvents (four organic: acetone, dichloromethane, methanol, acetonitrile; and four aqueous: water, phosphate buffer, shampoo, sodium dodecylsulfate) were evaluated for their capacity to remove artificially deposited pesticides from hair surface. The most effective washing solvents were sodium dodecylsulfate and methanol for aqueous and organic solvents, respectively. Moreover, after a first washing with sodium dodecylsulfate or methanol, the majority of externally deposited pesticides was removed and a steady-state was reached since significantly lower amounts were removed by additional second and third washings. Finally, the effectiveness of a decontamination procedure comprising washing with sodium dodecylsulfate and methanol was successively demonstrated. In parallel, it was determined that the final procedure did not affect the chemicals biologically incorporated, as hair strands naturally containing pesticides were used. Such a procedure appears to remove in one-shot the fraction of chemicals located on hair surface and does not require repeated washing steps. PMID:24817049

  7. Determination of pesticide residues in fish tissues by modified QuEChERS method and dual-d-SPE clean-up coupled to gas chromatography-mass spectrometry.

    Science.gov (United States)

    Molina-Ruiz, Juan Manuel; Cieslik, Ewa; Cieslik, Iwona; Walkowska, Izabela

    2015-01-01

    The aim of this research was to modify the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method for the determination of organochlorine and organophosphate pesticides in fatty animal matrices such as fish muscle tissues of carp and sturgeon collected from Carp Valley, Lesser Poland. Pesticides extraction effectiveness was evaluated at 0.030 mg kg(-1) spiking level and efficiency of the dispersive-solid-phase extraction (d-SPE) clean-up step was evaluated by comparison testing two different d-SPE clean-up stages, first the addition of the d-SPE sorbent combination (PSA?+?SAX?+?NH2), and secondly the addition of C18 after extracts enrichment with the d-SPE sorbent combination (PSA?+?SAX?+?NH2), introducing a novel concept of clean-up named dual-d-SPE clean-up. Analysis of pesticide residues was performed by Gas Chromatography Quadrupole Mass Spectrometry (GC/Q-MS) working in selected-ion monitoring (SIM) mode. Linear relation was observed from 0 to 200 ng mL(-1) and determination coefficient R(2)?>?0.997 in all instances for all target analytes. Better recoveries and cleanliness of extracts in both samples, carp and sturgeon tissues, were obtained after C18 addition during the dual-d-SPE clean-up step. Recoveries were in the range 70-120%, with relative standard deviation lower than 10% at 0.030 mg kg(-1) spiking level for most pesticides. LODs ranged 0.001-0.003 mg kg(-1), while LOQs ranged 0.004-0.009 mg kg(-1). The proposed method was successfully applied analyzing pesticide residues in real carp and sturgeon muscle samples; detectable pesticide residues were observed, but in all of the cases contamination level was lower than the default maximum residue levels (MRLs) set by the European Union (EU), Regulation (EC) N 396/2005. PMID:25074831

  8. Results from the monitoring of pesticide residues in fruit and vegetables on the Danish market 1998-99

    DEFF Research Database (Denmark)

    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 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 grown. Of the samples, 35% were of Danish origin, with 65% originating from other countries. Three accredited laboratories performed analyses of the samples using capillary gas chromatography, liquid chromatography and spectrophotometric methods. Results were registered online into a central database. 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.

  9. Determination of Pesticide Residues in Banana by Using High Performance Liquid Chromatography and Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    R. Paranthaman

    2012-01-01

    Full Text Available Problem statement: The occurrence of endosulfan, carbendazim, chloropyripos in 10 banana samples in southern area of Tamilnadu, India (hill banana, karpuravalli, monthan, nendran, ney poovan, pachanadan, poovan, rasthali, red banana, robusta was investigated. Approach: In 7 samples, Carbendazim was found at concentrations ranging from 0.002-0.11 mg kg-1. In three samples, carbendazim was not found, whereas endosulfan, chloropyripos was not detected in any sample. Results: Analysis was carried out using HPLC-UV and samples were confirmed by GC-MS. The seven samples contained carbendazim that not exceeded the FAO/WHO codex alimentarius standards for MRLs (Maximum Residue Limit values of carbendazim pesticide on banana (whole is 1.0 mg kg-1. Conclusion/Recommendations: Based on the HPLC results carbendazim is finding in Hill banana (0.007 mg kg-1, Monthan (0.019 mg kg-1, Nendran (0.002 mg kg-1, Pachanadan (0.007 mg kg-1, Poovan (0.016 mg kg-1, Rasthali (0.017 mg kg-1 and Robusta (0.11 mg kg-1 and carbendazim is not finding Karpuravalli, Ney poovan and Red banana. Endosulfan, Chloropyrifos and Carbendazim in Robusta Banana sample are identified by matching their retention times and characteristic ion. TIC chromatogram for a positive Robusta Banana sample.

  10. [Violations of mrls for pesticide residues in food reported for risk assessment according to RASFF procedures in Poland].

    Science.gov (United States)

    Ludwicki, Jan Krzysztof; Kostka, Grazyna

    2008-01-01

    The results of risk assessment to evaluate the potential risk from food products of plant origin in cases of violations of maximum residue limits for pesticides (MRLs) have been presented. According to the rules set in the RASFF any violation of legally established limit should undergo the risk assessment to allow quantitative approach in hazard evaluation for consumers. The basis of risk assessment have been presented as tool for risk management in the official food control. In case of MRLs violations the risk was assessed for general population as well as for small children as the most vulnerable part of the population. Since beginning of the RASFF in Poland--since mid of 2003 till the end of 2007--148 notifications of MRLs violations underwent risk assessment procedures. This means 2.5% of the overall number of analyzed samples. However, as much as 0.39% of the samples taken for analysis posed a real, considerable risk for consumers health, and the small children seem to be the group at greatest risk. PMID:19227249

  11. Ultra performance liquid chromatography atmospheric pressure photoionization high resolution mass spectrometric method for determination of multiclass pesticide residues in grape and mango juices.

    Science.gov (United States)

    Deme, Pragney; Upadhyayula, Vijayasarathi V R

    2015-04-15

    A novel analytical method was developed for determination of organochlorine, synthetic pyrethroid, organophosphate and carbamate pesticide residues in fruit juices using ultra performance liquid chromatography-atmospheric pressure photoionization-high resolution mass spectrometry (UPLC-APPI-HRMS). The analytes were extracted from fruit juices by dispersive solid-phase extraction using multi-walled carbon nanotubes (MWCNTs). The analysis was carried out in full scan mode using dual ionization mode of APPI in the mass range of 100-650 units. The limit of detection and limit of quantification values for the pesticides were in the range of 0.025-0.15 ng mL(-1) and 0.1-0.5 ng mL(-1) respectively. The matrix effect of the method was found to be low and extraction recoveries were in the range of 60-110%. Some of the real fruits juice samples showed the presence of some pesticides in the range of 6.5-24.8 ng L(-1). PMID:25466136

  12. Ionic-liquid-based dispersive liquid-liquid microextraction combined with high-performance liquid chromatography for the determination of multiclass pesticide residues in water samples.

    Science.gov (United States)

    Tadesse, Bezuayehu; Teju, Endale; Gure, Abera; Megersa, Negussie

    2015-03-01

    Ionic-liquid-based dispersive liquid-liquid microextraction in combination with high-performance liquid chromatography and diode array detection has been proposed for the simultaneous analysis of four multiclass pesticide residues including carbaryl, methidathion, chlorothalonil, and ametryn from water samples. The major experimental parameters including the type and volume of ionic liquid, sample pH, type, and volume of disperser solvent and cooling time were investigated and optimum conditions were established. Under the optimum experimental conditions, limits of detection and quantification of the method were in the range of 0.1-1.8 and 0.4-5.9 ?g/L, respectively, with satisfactory enrichment factors ranging from 10-20. The matrix-matched calibration curves, which were constructed for lake water, as a representative matrix were linear over wide range with coefficients of determination of 0.996 or better. Intra- and interday precisions, expressed as relative standard deviations, were in the range of 1.1-9.7 and 3.1-7.8%, respectively. The relative recoveries of the spiked environmental water samples at one concentration level were in the range of 77-102%. The results of the present study revealed that the proposed method is simple, fast, and uses environmentally friendly extraction solvent for the analysis of the target pesticide residues in environmental water samples. PMID:25641819

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

    Science.gov (United States)

    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.

  14. Pesticide residues in tropical coastal lagoons: Use of 14C labelled compounds to study the cycling and fate of agrochemicals

    International Nuclear Information System (INIS)

    Organophosphorus and organochlorine pesticide residues present in tropical coastal lagoons originate from the use of agrochemicals in the surrounding fields. A study of the early stages in the cycling and fate of chlorpyrifos, parathion and DDT in this type of ecosystem was conducted using 14C labelled compounds in microcosm and large outdoor tank experiments. Organophosphates in water were shown to be degraded by chemical hydrolysis and microbial action. The effect of temperature was investigated and it was found that increased temperature enhanced the degradation rates of these compounds. However, the rapid association of pesticides with sediments increased their persistence in the aquatic environment. Microbial biomass associated with the sediments contributed significantly to the degradation of these compounds, but the action of microbes did not compensate for the increase in pesticide persistence afforded by sorption to sediment. Preliminary results from outdoor tank experiments indicate that sediment associated pesticides remain biologically available at least partially to tropical benthic organisms. (author). 16 refs, 4 figs, 3 tabs

  15. 75 FR 60452 - Notice of Filing of Several Pesticide Petitions for Residues of Pesticide Chemicals in or on...

    Science.gov (United States)

    2010-09-30

    ...achieve environmental justice, the fair treatment and meaningful involvement of any...for residues of the antifungal agent Aspergillus flavus NRRL 21882 in or on cotton...and would be present irrespective of treatment. Shanaz Bacchus, (703)...

  16. 78 FR 11126 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2013-02-15

    ...for residues of castor oil, polymer with adipic acid, linoleic acid, oleic acid, and ricinoleic acid, (CAS No. 1357486-09-9...petitioning that castor oil, polymer with adipic acid, linoleic acid, oleic acid and ricinoleic acid be exempt...

  17. Análise de resíduos de agrotóxicos em tomates empregando dispersão da matriz em fase sólida (DMFS) e cromatografia gasosa Analysis of pesticide residue in tomato using matrix solid-phase dispersion (MSPD) and gas chromatography

    OpenAIRE

    Pinho, Gevany P.; Neves, Anto?nio A.; Queiroz, Maria Eliana L. R.

    2009-01-01

    This work was aimed on optimization of the matrix solid-phase dispersion (MSPD) technique using gas chromatography for analyzing residues of chlorpyriphos, ?-cyhalothrin, cypermethrin and deltamethrin in tomatoes. The results showed that silica was more efficient for the clean up of extracts, but florisil provided the highest recovery rates. A 2³ complete factorial design was carried out to evaluate the absorbent/sample ratio, presence of co-column (silica) and ultrasonic bath on the ex...

  18. Organo chlorine pesticide residues in the major rivers of Southern Thailand

    International Nuclear Information System (INIS)

    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 ?-HCH, ?-HCH, heptachlor epoxide, endosulfan 1, p,p'-DDE and endrin aldehyde. The overall results showed that Saibue. 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)

  19. Residual analysis for spatial point processes

    DEFF Research Database (Denmark)

    Baddeley, A.; Turner, R.

    2004-01-01

    We define residuals for point process models fitted to spatial point pattern data, and propose diagnostic plots based on these residuals. The techniques apply to any Gibbs point process model, which may exhibit spatial heterogeneity, interpoint interaction and dependence on spatial covariates. Our residuals generalise the well-known residuals for point processes in time, used in signal processing and survival analysis. An important difference is that the conditional intensity or hazard rate of the temporal point process must be replaced by the Papangelou conditional intensity $lambda$ of the spatial process. Residuals are ascribed to locations in the empty background, as well as to data points of the point pattern. We obtain variance formulae, and study standardised residuals. There is also an analogy between our spatial residuals and the usual residuals for (non-spatial) generalised linear models. 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 or covariate effects. Q-Q plots of the residuals are effective in diagnosing interpoint interaction. Some existing ad hoc statistics of point patterns (quadrat counts, scan statistic, kernel smoothed intensity, Berman's diagnostic) are recovered as special cases.

  20. Multi-residue method for determination of 238 pesticides in Chinese cabbage and cucumber by liquid chromatography-tandem mass spectrometry: comparison of different purification procedures.

    Science.gov (United States)

    Zhao, Mei-Ai; Feng, Ya-Nan; Zhu, Yong-Zhe; Kim, Jeong-Han

    2014-11-26

    This paper describes the comparison of five sample cleanup procedures for the determination of 238 pesticides via triple quadrupole liquid chromatography-tandem mass spectrometry (LC-MS/MS, with only 10 min of chromatographic running time) in Chinese cabbage and cucumber. Samples were extracted with a quick, easy, cheap, effective, rugged, and safe (QuECHERS) preparation method and cleanup with different sorbents, including primary secondary amine (PSA), multi-walled carbon nanotubes (MWCNTs), and polystyrene (PLS), to find out the most suitable cleanup methods for Chinese cabbage and cucumber. The recovery and matrix effect were evaluated by monitoring the main parameters in one group of 238 pesticides at the spiked level of 8 and 40 ?g/kg. In Chinese cabbage, when PSA dispersive solid-phase extraction (D-SPE) was applied, recoveries of 183 pesticides ranged between 70 and 120% with relative standard deviation (RSD) values lower than 20% at a spiked level of 40 ?g/kg, indicating the effectiveness of the purification step. In cucumber, 203 pesticides were in the 70-120% recovery range with good reproducibility by PSA mini-cartridge column cleanup at a spiked level of 40 ?g/kg and RSD values were generally below 20%. The limits of quantitation [LOQs; signal-to-noise (S/N) = 10] were in the range of 0.16-10.20 ?g/kg for Chinese cabbage and 0.06-21.06 ?g/kg for cucumber, while the limits of detection (LODs; S/N = 3) were between 0.05 and 3.06 ?g/kg and between 0.02 and 6.32 ?g/kg in Chinese cabbage and cucumber, respectively. The proposed methods that might be applied for the multi-residue analysis in Chinese cabbage and cucumber are contributed to their rapid speed and good recoveries. PMID:25380470

  1. QuEChERS sample preparation for the determination of pesticides and other organic residues in environmental matrices: a critical review.

    Science.gov (United States)

    Bruzzoniti, Maria Concetta; Checchini, Leonardo; De Carlo, Rosa Maria; Orlandini, Serena; Rivoira, Luca; Del Bubba, Massimo

    2014-07-01

    Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) is an extraction and clean-up technique originally developed for recovering pesticide residues from fruits and vegetables. Since its introduction, and until December 2013, about 700 papers have been published using the QuEChERS technique, according to a literature overview carried out using SciFinder, Elsevier SciVerse, and Google search engines. Most of these papers were dedicated to pesticide multiresidue analysis in food matrices, and this topic has been thoroughly reviewed over recent years. The QuEChERS approach is now rapidly developing beyond its original field of application to analytes other than pesticides, and matrices other than food, such as biological fluids and non-edible plants, including Chinese medicinal plants. Recently, the QuEChERS concept has spread to environmental applications by analyzing not only pesticides but also other compounds of environmental concern in soil, sediments, and water. To the best of our knowledge, QuEChERS environmental applications have not been reviewed so far; therefore, in this contribution, after a general discussion on the evolution and changes of the original QuEChERS method, a critical survey of the literature regarding environmental applications of conventional and modified QuEChERS methodology is provided. The overall recoveries obtained with QuEChERS and other extraction approaches (e.g., accelerated solvent extraction, ultrasonic solvent extraction, liquid/solid extraction, and soxhlet extraction) were compared, providing evidence for QuEChERS higher recoveries for various classes of compounds, such as biopesticides, chloroalkanes, phenols, and perfluoroalkyl substances. The role of physicochemical properties of soil (i.e., clay and organic carbon content, as well as cation exchange capacity) and target analytes (i.e., log KOW, water solubility, and vapor pressure) were also evaluated in order to interpret recovery and matrix effect data. PMID:24770804

  2. Organophosphorus and Carbamate Pesticide Residues Detected in Water Samples Collected from Paddy and Vegetable Fields of the Savar and Dhamrai Upazilas in Bangladesh

    Directory of Open Access Journals (Sweden)

    Nurul Karim

    2012-09-01

    Full Text Available Several types of organophosphorous and carbamate pesticides have been used extensively by the farmers in Bangladesh during the last few decades. Twenty seven water samples collected from both paddy and vegetable fields in the Savar and Dhamrai Upazilas in Bangladesh were analyzed to determine the occurrence and distribution of organo-phosphorus (chlorpyrifos, malathion and diazinon and carbamate (carbaryl and carbofuran pesticide residues. A high performance liquid chromatograph instrument equipped with a photodiode array detector was used to determine the concentrations of these pesticide residues. Diazinon and carbofuran were detected in water samples collected from Savar Upazila at 0.9 ?g/L and 198.7 ?g/L, respectively. Malathion was also detected in a single water sample at 105.2 ?g/L from Dhamrai Upazila. Carbaryl was the most common pesticide detected in Dhamrai Upazila at 14.1 and 18.1 ?g/L, while another water sample from Dhamrai Upazila was contaminated with carbofuran at 105.2 ?g/L. Chlorpyrifos was not detected in any sample. Overall, the pesticide residues detected were well above the maximum acceptable levels of total and individual pesticide contamination, at 0.5 and 0.1 ?g/L, respectively, in water samples recommended by the European Economic Community (Directive 98/83/EC. The presence of these pesticide residues may be attributed by their intense use by the farmers living in these areas. Proper handling of these pesticides should be ensured to avoid direct or indirect exposure to these pesticides.

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

    Science.gov (United States)

    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

  4. Determination of pesticide residues in nonfatty foods by supercritical fluid extraction and gas chromatography/mass spectrometry: collaborative study.

    Science.gov (United States)

    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 analysis of 6 blind duplicates at 3 concentrations for each pesticide are as follows: carbofuran in apple (75-500 ng/g), 89% recovery, 7% RSDr, 9% reproducibility relative standard deviation (RSDR); diazinon in apple (60-400 ng/g), 83% recovery, 13% RSDr, 17% RSDR; vinclozolin in apple (6-400 ng/g), 97% recovery, 13% RSDr, 18% RSDR; chlorpyrifos in apple (50-300 ng/g), 105% recovery, 11% RSDr, 13% RSDR; endosulfan sulfate in apple (150-1000 ng/g), 95% recovery, 15% RSDr, 17% RSDR; trifluralin in green bean (30-200 ng/g), 58% recovery, 11% RSDr, 27% RSDR; dacthal in green bean (60-400 ng/g), 88% recovery, 11% RSDr, 17% RSDR; quintozene in green bean (60-400 ng/g), 79% recovery, 13% RSDr, 18% RSDR; chlorpyrifos in green bean (50-300 ng/g), 84% recovery, 11% RSDr, 17% RSDR; p,p'-DDE in green bean (45-300 ng/g), 64% recovery, 14% RSDr, 27% RSDR; atrazine in carrot (75-500 ng/g), 90% recovery, 11% RSDr, 15% RSDR; metalaxyl in carrot (75-500 ng/g), 89% recovery, 8% RSDr, 12% RSDR; parathion-methyl in carrot (75-500 ng/g), 84% recovery, 14% RSDr, 15% RSDR; chlorpyrifos in carrot (50-300 ng/g), 77% recovery, 13% RSDr, 19% RSDR; and bifenthrin in carrot (90-600 ng/g), 63% recovery, 12% RSDr, and 25% RSDR. All analytes except for the nonpolar compounds trifluralin, p,p'-DDE, and bifenthrin gave average Horwitz ratios of analysis, and the Study Director recommends that it be adopted Official First Action. PMID:12374416

  5. 77 FR 48902 - S-Metolachlor; Pesticide Tolerances

    Science.gov (United States)

    2012-08-15

    ...and chronic analyses assume tolerance-level residues on all crops...used in the analyses. i. Acute...food-use pesticide, if a toxicological...Tolerance level residues and 100 PCT...exposure analysis and risk...models used in pesticide...

  6. DETERMINATION OF PYRETHROID PESTICIDE RESIDUES FROM RAT TISSUE USING TWO-DIMENSIONAL LCMS

    Science.gov (United States)

    Pyrethroids are a synthetic class of pesticides that elicit neurobehavioral effects in mammals. They are applied occupationally and residentially creating the potential for human exposure. Determining relationships between parent pyrethroid tissue concentrations and neurotoxic ...

  7. 75 FR 35801 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2010-06-23

    ...NAICS code 111). Animal production (NAICS...ppm; potato, wet peel at 0.2 ppm...demonstrated the ability to extract aged clothianidin...at 0.01 ppm; pomegranates at 0.01 ppm...picoxystrobin residues in animal tissues including...picoxystrobin in the animal matrices at...

  8. 76 FR 17374 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2011-03-29

    ...ecirc]S,[ecirc]S']zinc], in or on apple, fruit...large animal tissues includes extraction of the residues of concern...was developed that involves extraction of acetamiprid from composite...ecirc]S, [ecirc]S']zinc], in or on apple,...

  9. 75 FR 48667 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2010-08-11

    ...residues of the insecticide avermectin B 1 (a mixture of avermectins containing greater than or equal to 80% avermectinB 1a...and the limit of quantification (LOQ) is 0.005 ppm for milk and juices, and 0.01 ppm for all other substrates....

  10. Comparison of pesticide residues in surface water and ground water of agriculture intensive areas

    OpenAIRE

    Lari, Summaiya Z.; Khan, Noor A.; Gandhi, Kavita N.; Meshram, Tejal S.; Thacker, Neeta P.

    2014-01-01

    The organochlorines (OClPs) and organophosphates (OPPs) pesticides in surface and ground water having intensive agriculture activity were investigated to evaluate their potential pollution and risks on human health. As per USEPA 8081 B method, liquid-liquid extraction followed by Gas-Chromatographic technique with electron capture detector and mass selective detector (GC-MS) were used for monitoring of pesticides. Among organochlorines, ?,?,?,? HCH’s, aldrin, dicofol, DDT and its deriva...

  11. Comparison of pesticide residues in surface water and ground water of agriculture intensive areas

    Science.gov (United States)

    2014-01-01

    The organochlorines (OClPs) and organophosphates (OPPs) pesticides in surface and ground water having intensive agriculture activity were investigated to evaluate their potential pollution and risks on human health. As per USEPA 8081 B method, liquid-liquid extraction followed by Gas-Chromatographic technique with electron capture detector and mass selective detector (GC-MS) were used for monitoring of pesticides. Among organochlorines, ?,?,?,? HCH’s, aldrin, dicofol, DDT and its derivatives, ?,? endosulphan’s and endosulphan-sulphate were analysed; dichlorovos, ethion, parathion-methyl, phorate, chlorpyrifos and profenofos were determined among organophosphates. As compared to ground water, higher concentrations of OClPs and OPPs were found in surface water. Throughout the monitoring study, ??-?HCH (0.39 ?g/L in Amravati region),??-?endosulphan (0.78 ?g/L in Yavatmal region), chlorpyrifos (0.25 ?g/L in Bhandara region) and parathion-methyl (0.09 ?g/L in Amravati region) are frequently found pesticide in ground water, whereas ?,?,?-HCH (0.39 ?g/L in Amravati region), ?,??-?endosulphan (0.42 ?g/L in Amravati region), dichlorovos (0.25 ?g/L in Yavatmal region), parathion-methyl (0.42 ?g/L in Bhandara region), phorate (0.33 ?g/L in Yavatmal region) were found in surface water. Surface water was found to be more contaminated than ground water with more number of and more concentrated pesticides. Among pesticides water samples are found to be more contaminated by organophosphate than organochlorine. Pesticides in the surface water samples from Bhandara and Yavatmal region exceeded the EU (European Union) limit of 1.0 ?g/L (sum of pesticide levels in surface water) but were within the WHO guidelines for individual pesticides. PMID:24398360

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

    OpenAIRE

    Essumang, D. K.; Togoh, G. K.; Chokky, L.

    2009-01-01

    This study was to ascertain the presence and subsequent amount of four organochlorine pesticides: dichlorodiphenyl dichloroethylene (2,4’-DDE), 4,4’-dichlorodiphenyldichloroethane (4,4’-DDD), p,p’-dichloro- diphenyltrichloroethane [p,p’-DDT (r) (i) (f)] and Propiconazol (f); and four organophosphorous pesticides: Fenitrothion (i), Chlorpyrifos (i), Dichlorvos (a) (i) and Diazinon (a) (i) in Chemu lagoon (Tema), Korle lagoon (Accra), Fosu lagoon (Cape Coast) and the Etsii lagoon (Aba...

  13. Pesticide residues in Nile tilapia (Oreochromis niloticus) and Nile perch (Lates niloticus) from Southern Lake Victoria, Tanzania

    Energy Technology Data Exchange (ETDEWEB)

    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.

  14. Pesticide residues in Nile tilapia (Oreochromis niloticus) and Nile perch (Lates niloticus) from Southern Lake Victoria, Tanzania

    International Nuclear Information System (INIS)

    Nile tilapia (Oreochromis niloticus) and Nile perch (Lates niloticus) samples were collected from fish landing stations in nine riparian districts on the Tanzanian side of Lake Victoria and screened for residues of 64 organochlorine, organophosphorus, carbamate, and pyrethroid pesticides. The residue levels in the fish fillet were up to 0.003, 0.03 and 0.2 mg/kg fresh weight (0.7, 3.8 and 42 mg/kg lipid weight) of fenitrothion, DDT and endosulfan, respectively. Mean levels within sites were up to 0.002, 0.02 and 0.1 mg/kg fresh weight (0.5, 0.5 and 16 mg/kg lipid weight), respectively. The detection of higher levels of p,p'-DDT than the degradation products (p,p'-DDD and p,p'-DDE), and higher levels of endosulfan isomers (? and ?) than the sulphate, in fish samples, implied recent exposure of fish to DDT and endosulfan, respectively. Generally, most of the fish samples had residue levels above the average method detection limits (MDLs), but were within the calculated ADI. - Fish from Lake Victoria had relatively low pesticide levels

  15. Influence of different planting seasons of six leaf vegetables on residues of five pesticides.

    Science.gov (United States)

    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 ?-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 ?-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

  16. Organochlorine pesticide residues in human breast milk and placenta in Tohoku, Japan

    Energy Technology Data Exchange (ETDEWEB)

    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.

  17. Gel Permeation Chromatography Purification and Gas Chromatography-Mass Spectrometry Detection of Multi-Pesticide Residues in Traditional Chinese Medicine

    Directory of Open Access Journals (Sweden)

    Zhen-Bin Gong

    2012-01-01

    Full Text Available The measurement of 23 organochlorine, organophosphorus, and pyrethroid pesticides in typical traditional Chinese medicine (TCM, flos lonicerae, was made using gel permeation chromatography (GPC purification and gas chroma- tography-mass spectrometry (GC-MS detection. The pesticides were extracted with ultrasonic device and 5.0 mL mixture of ethyl acetate and cyclohexane (1:1, v/v. Coextractants from sample matrices which may have interfere to the qualitative and quantitative analysis, such as pigments, were removed using GPC purification. Simultaneous full scan and selective ion monitor (scan/SIM mode for GC-MS was used for qualitative and quantitative analysis, which pro- vided retention time and characteristic fragments ratio for each pesticide so as to positively identify each analyte. Rela- tive standard deviations (RSDs were within 7.7% (5.0 - 22.5 µg/kg, n = 3. The recoveries of pesticide standards at the spiked concentration of 5.0 - 22.5 µg/kg were between 87.1% and 110.9%. Limits of detection (LODs for the analytes were 0.16 - 3.2 µg/kg, which could meet the demand of routine analysis and TCM quality control.

  18. Analysis of endocrine disrupting pesticides by capillary GC with mass spectrometric detection.

    Science.gov (United States)

    Matisová, Eva; Hrouzková, Svetlana

    2012-09-01

    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. PMID:23202677

  19. Levels of organochlorine pesticide residues in some organs of the Ganges perch, Lates calcarifer, from the Ganges-Brahmaputra-Meghna Estuary, Bangladesh

    Energy Technology Data Exchange (ETDEWEB)

    Jabber, Sardar Md Abdul; Khan, Yusuf Sharif Ahmed [Chittagong Univ., Inst. of Marine Sciences, Chittagong (Bangladesh); Rahman, M. Saifur [Atomic Energy Research Establishment, Inst. of Food and Radiation Biology (IFRB), Dhaka, (Bangladesh)

    2001-07-01

    Levels of organochlorine pesticide residues (p,p' DDT, DDD, DDE, Aldrin, Dieldrin, Lindane, Heptachlor and BHC) were analysed in the dry and wet seasons in four organs (muscle, liver, gut and egg samples) of Granges Perch, Lates calcarifer, collected during October-November-December, 1996 and May-June-July, 1997 from the Ganges-Brahmaputtra-Meghna estuary. The residues were analysed by using gas-chromatography (GC) in electron capture detector (ECD) mode and were verified by thin layer chromatography (TLC). Among the four organs analysed, the residues were found in the order egg>gut>muscle>liver. The pesticide residues were found in the order {sigma}DDT>Heptachlor>Dieldrin>Aldrin. Higher levels of residues were found during the dry season due to high lipid content in fishes. A positive correlation was observed between the pesticide residues ({sigma}DDT and {sigma}OCs) and lipid contents of fish, and the correlation was found to be linear. The concentrations of pesticide residues in muscle, liver and gut were below the FAO/WHO (1993) recommended permissible limit except in eggs. (Author)

  20. Determination of pesticide residues in high oil vegetal commodities by using various multi-residue methods and clean-ups followed by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Rajski, ?ukasz; Lozano, Ana; Uclés, Ana; Ferrer, Carmen; Fernández-Alba, Amadeo R

    2013-08-23

    Several extraction methods were evaluated in terms of recoveries and extraction precision for 113 pesticides in avocado: QuEChERS with various d-SPE clean-ups (Z-Sep, Z-Sep+, PSA+C18 and silica), miniLuke and ethyl acetate. Extracts were analysed using liquid chromatography coupled with triple quadrupole mass spectrometer working in multi-reaction monitoring mode. Z-Sep and Z-Sep+ are new types of material for high lipid matrices - these two sorbents contain ZrO2, which improves fat removal from the extracts. The QuEChERS protocol with Z-Sep provided the highest number of pesticides with recoveries in the 70-120% range along with the lowest amount of coextracted matrix compounds. Subsequently, this method was validated in two matrices - avocado and almonds. In the validation recoveries at two levels - 10 and 50?g/kg - limit of quantitation, linearity, matrix effects, as well as the inter- and intraday precision were studied. In the avocado samples, 107 analytes had LOQs equal to 10?g/kg (signal to noise of quantitative transition was equal 20 or more). In the almond samples, 92 pesticides had LOQs equal to 10?g/kg (S/N?20) and 2 pesticides at 50?g/kg. The validated method was employed in the analysis of real avocado and almond samples. PMID:23871559

  1. 77 FR 26462 - Dimethomorph; Pesticide Tolerances

    Science.gov (United States)

    2012-05-04

    ...unnecessary. iv. Anticipated residue and PCT information...not use anticipated residue and/or PCT information...dimethomorph. Tolerance level residues and/or 100 PCT were...the dietary exposure analysis and risk assessment...water models used in pesticide exposure...

  2. 75 FR 80346 - Flutolanil; Pesticide Tolerances

    Science.gov (United States)

    2010-12-22

    ...unnecessary. iv. Anticipated residue and percent crop treated...not use anticipated residue and/or PCT information...flutolanil. Tolerance level residues and/or 100% CT were...the dietary exposure analysis and risk assessment...water models used in pesticide exposure...

  3. Validation of Analysis Method of pesticides in fresh tomatoes by Gas Chromatography associated to a liquid scintillation counting

    International Nuclear Information System (INIS)

    Pesticides are nowadays considered as toxic for human health. The maximum residues levels (MRL) in foodstuff are more and more strict. Therefore, selective analytical techniques are necessary for their identification and their quantification. The aim of this study is to set up a multi residue method for the determination of pesticides in tomatoes by gas chromatography with ?ECD detector (GC/?ECD) associated to liquid scintillation counting. A global analytical protocol consisting of a QuECHERS version of the extraction step followed by purification step of the resulting extract on a polymeric sorbent was set up. The 14C-chloropyrifos used as an internal standard proved excellent to control the different steps needed for the sample preparation. The method optimized is specific, selective with a recovery averaged more than 70 pour cent, repetitive and reproducible. Although some others criteria need to be checked regarding validation before its use in routine analysis, the potential of the method has been demonstrated.

  4. Multiresidue analytical procedures for pesticides residues in vegetable products; Metodi mutiresiduo per l`analisi di residui di antiparassitari in prodotti vegetali

    Energy Technology Data Exchange (ETDEWEB)

    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).

  5. Studying of specific disintegrative characteristic for pesticide residues that used in green vegetables in the environment of Dalat city

    International Nuclear Information System (INIS)

    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)

  6. Detecting Pesticide Residue by Using Modulating Temperature Over a Single SnO2-Based Gas Sensor

    OpenAIRE

    Zengliang Yu; Zongxin Pi; Jinhuai Liu; Xingjiu Huang

    2003-01-01

    A new rapid detecting method (called dynamic measurements ) was reported to detect and distinguish the presence of two pesticide gases in the ambient atmosphere. The method employed only a single SnO2-based gas sensor in a rectangular temperature mode to perform the qualitative analysis of a binary gas mixture (acephate and trichlorphon) in air. Polar plots was used for quantitative analysis which the feature extraction was performed by FFT. Experimental results showed that high selectivity o...

  7. Determination of pesticide residues in tomato using dispersive solid-phase extraction and gas chromatography/ion trap mass spectrometry

    Scientific Electronic Library Online (English)

    Graziela C. R. Moura, Andrade; Rosana M. O, Freguglia; Regina P. Z, Furlani; Nádia H, Torres; Valdemar L, Tornisielo.

    1701-17-01

    Full Text Available A cultura do tomate é frequentemente afetada por pragas, doenças e estresses abióticos, resultando em menor produtividade e perda de qualidade dos frutos. O uso intensivo de pesticidas em tomates sem utilização das boas práticas agrícolas tem causado grande preocupação quanto à provável contaminação [...] do produto final. O método QuEChERS foi utilizado para a determinação de seis pesticidas (buprofezina, carbofurano, ?-endosulfan, ?-endosulfan, sulfato de endosulfan e monocrotofós) em amostras de tomate coletadas em supermercados. O método envolveu a extração líquido-líquido com acetonitrila, adição de MgSO4 e NaCl seguida de extração em fase sólida dispersiva com PSA (amina primária secundária) e as análises foram realizadas com cromatografia gasosa/espectrometria de massa ion trap. O estudo de recuperação para os pesticidas variou de 71 a 111% e o desvio padrão relativo foi inferior a 15%. Não foram detectados resíduos de pesticidas (> LOD) nas trinta e três amostras de tomate analisadas. Abstract in english Tomato crop is frequently damaged by diseases, pests and abiotic stresses, resulting in lower yielding and loss of fruit quality. The intensive use of pesticides in tomatoes without observation of good agriculture practices and regulations has caused great concern with a probable final product conta [...] mination. The QuEChERS method of sample preparation was used for the determination of six pesticides (buprofezin, carbofuran, endosulfan-?, endosulfan-?, endosulfan sulfate and monocrotophos) in thirty three tomato samples collected from local market retailers. The method involved extraction with acetonitrile, liquid-liquid partition with addition of MgSO4 and NaCl followed by dispersive solid phase extraction using primary secondary amine sorbent and the analyses were carried out with a gas chromatography/mass spectrometry equipment by ion trap. Recovery studies for different pesticides ranged from 71 to 111% and the relative standard deviation (RSD) was below 15%. No pesticide residue was detected (> LOD) among the thirty three tomato samples analysed.

  8. Scientific support for preparing an EU position in the 46th Session of the Codex Committee on Pesticide Residues (CCPR

    Directory of Open Access Journals (Sweden)

    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.

  9. Comparison of methods of preserving tissues for pesticide analysis

    Science.gov (United States)

    Stickel, W.H.; Stickel, L.F.; Dyrland, R.A.; Hughes, D.L.

    1984-01-01

    Formalin preservation, freezing, spoiling followed by freezing, and phenoxyethanol were compared in terms of concentrations of DDT, DDD, DDE, endrin, and hepatachlor epoxide measured in brain, liver and carcass of birds fed dietary dosages of pesticides and in spiked egg homogenate. Phenoxyethanol proved to be an unsatisfactory preservative; the amount of 'extractable lipid' was excessive, and measurements of concentrations in replicates were erratic. Concentrations of residues in formalin-preserved and frozen samples did not differ significantly in any tissue. Percentage lipid in brains and eggs, however, were significantly lower in formalin-preserved samples. Samples of muscle and liver that had been spoiled before freezing yielded less DDD, and muscle samples yielded more DDT than formalin-preserved samples. The authors conclude that formalin preservation is a satisfactory method for preservation of field samples and that the warming and spoiling of samples that may occur unavoidably in the field will not result in misleading analytical results.

  10. Monitoring of organochlorine pesticide residue levels in adipose tissue of Veracruz, Mexico inhabitants.

    Science.gov (United States)

    Waliszewski, Stefan M; Caba, M; Herrero-Mercado, M; Saldariaga-Noreña, H; Meza, E; Zepeda, R; Martínez-Valenzuela, C; Infanzon, R; Hernández-Chalate, F

    2011-11-01

    The objective of the present study was to monitor the levels of organochlorine pesticides HCB, ?-?-?-HCH, pp'DDE, op'DDT and pp'DDT in 150 adipose tissue samples of Veracruz, Mexico inhabitants. In analyzed samples, the following pesticides were detected: p,p'-DDE in 100% of the samples at mean 1.643 mg/kg; p,p'-DDT in 99.3.% of the samples at mean 0.227 mg/kg; ?-HCH in 97.3% of the samples at mean 0.063 mg/kg; and op'DDT in 93.3% of the samples at mean 0.022 mg/kg. Comparing mean, median and geometric mean concentrations of organochlorine pesticides shows a decrease in values from mean to median and to geometric mean which points out a prevalence of lower concentrations among the total samples and the existence of occasional cases of extreme exposure expressed in range values. The pooled samples divided according to sex, showed only significant differences of pp'DDE median concentrations between sexes. The other organochlorine pesticides indicated no statistical differences between sexes, including the pp'DDE/pp'DDT ratio. The samples grouped according to age, showed that the third tertile was more contaminated for both sexes, indicating age as a positively associated factor with organochlorine pesticide levels in adipose tissue of Veracruz inhabitants. Comparing organochlorine pesticide levels between 2008 and 2010 years, a decreased tendency for ?-HCH, pp'DDE, ?-DDT and pp'DDE/pp'DDT ratio levels was observed. PMID:21681398

  11. Occurrence, distribution and possible sources of organochlorine pesticide residues in tropical coastal environment of India: an overview.

    Science.gov (United States)

    Sarkar, S K; Bhattacharya, B D; Bhattacharya, A; Chatterjee, M; Alam, A; Satpathy, K K; Jonathan, M P

    2008-10-01

    Organochlorine pesticides (OCPs) are an important potential component of chemical pollutants used extensively for agriculture and sanitation purposes in India as these are comparatively cheap and effective. These persistent organic compounds such as HCH isomers, DDT and its metabolites are the predominant chemical contaminants found along the Indian coast and thus constitute both alluring and grave areas of scientific research. Our objective in the paper is to provide a comprehensive account of the distribution of organochlorine pesticides in biotic and abiotic compartments of the Indian coastal environment, make some comments on their environmental sources, their movement through the food chain and possible ecotoxicological risk of health in biota including humans. The prevalent HCH, DDT and HCB concentrations differ markedly in eastern and western coast of India reflecting differing agricultural and other usage and their ultimate input into the coastal environment by several rivers and the bioturbation activities of macrozoobenthos (bivalve mollusks, polychaetous annelids, etc.). In several cases, the DDT levels exceeded the effects range-low (ER-L) and could thus cause acute biological impairments, in comparison with the sediment quality guidelines. Contributions of DDT metabolites (DDT, DDD and DDE residues) vary in different Indian coastal regions predominated by pp'-DDT and pp'-DDD. Measured concentrations of HCHs were lower than DDTs that might be due to higher water solubility, vapor pressure and biodegradability of the latter. HCH and DDT residues in fish in India were lower than those in the temperate countries indicating a lower accumulation in tropical fish, which might be related to rapid volatilization of this insecticide in the tropical environment. The concentrations of other chlorinated pesticides (aldrin, dieldrin, eldrin, methoxychlor, endosulfan sulphate) were lower and not generally of great concern. PMID:18423595

  12. Simultaneous multi-determination and transfer of eight pesticide residues from green tea leaves to infusion using gas chromatography.

    Science.gov (United States)

    Cho, Soon-Kil; Abd El-Aty, A M; Rahman, Md Musfiqur; Choi, Jeong-Heui; Shim, Jae-Han

    2014-12-15

    A method for determining eight pesticide (cyhalothrin, flufenoxuron, fenitrothion, EPN, bifenthrin, difenoconazole, triflumizole, and azoxystrobin) residues in made green tea as well as a tea infusion (under various brewing water temperatures; 60, 80, and 100°C) using gas chromatography (GC) micro-electron capture detector (?ECD) was developed and validated. The extraction method adopted the relatively commonly used approach of solid sample hydration, with the green tea hydrated before being extracted through salting out with acetonitrile followed by a cleanup procedure. The analytes were confirmed using GC-coupled to tandem mass spectrometry (GC/MS/MS) with a triple quadrupole. The linearity of the calibration curves yielded determination coefficients (R(2)) >0.995. Recoveries were carried out using blank samples spiked with all analytes at two levels. The results demonstrated that all pesticides were recovered within the range of 77-116% with a relative standard deviation (RSD) ?14%. The quantification limits of 0.015-0.03 mg/kg were lower than the maximum residue limits (MRLs) set by the Korea Food and Drug Administration (KFDA) for all analytes (0.05-10mg/kg). The infusion study indicated that cyhalothrin, flufenoxuron, and bifenthrin did not infuse into the tea brew from the made tea. Increases in brewing time resulted in increased transfer of azoxystrobin, fenitrothion, and difenoconazole from the made tea to the brew; however, this was not the case with triflumizole or EPN. We conclude that transfer of pesticides appeared to be dependent on their water solubilities and drinking a cup of tea is recommended to be at a water temperature of 60°C. PMID:25038708

  13. Monitoring of Certain Pesticide Residues and Some Heavy Metals in Fresh Cow`s Milk at Gharbia Governorate, Egypt

    Directory of Open Access Journals (Sweden)

    I.N. Nasr

    2007-01-01

    Full Text Available This monitoring study of 40 samples of cow`s milk collected from different locations at Gharbia Governorate during the four different seasons of the years 2005-2006, was conducted to determine the contamination levels of seven pesticide residues including four organophosphorus (chlorpyrifos, diazinon, dimethoate and malathion and three synthetic pyrethroides (cypermethrin, deltamethrin and fenvelerate, as well as five heavy metals (copper, iron, cadmium, zinc and lead. The results showed that there were no contamination with investigated pesticide residues found in all analyzed samples, except for malathion, which was detected in a single sample with a negligible existence (0.018 mg kg-1, by ratio of (0.02% of all samples. In relation to heavy metals detection, data revealed that all milk samples were contaminated with heavy metals all year around. The contamination with heavy metals was generally dominated at summer season. Level of lead was higher than other metals. The mean levels of Cu, Fe, Cd, Zn and Pb were 0.251, 0.607, 0.159, 0.371 and 2.462 mg kg-1, respectively. Cu, Fe and Zn level were under the permissible limits, while the Cd and Pb were exceeded the permissible limits, indicating serious heavy metals pollution in the region.

  14. Interlaboratory comparison for the determination of five residual organochlorine pesticides in ginseng root samples by gas chromatography.

    Science.gov (United States)

    Kong, Mei-Fung; Chan, Serena; Wong, Yiu-Chung; Wong, Siu-Kay; Sin, Della Wai-Mei

    2007-01-01

    An interlaboratory comparison study for the determination of 5 residual organochlorine pesticides (hexachlorobenzene and 4 hexachlorocyclohexane isomers) in ginseng root was performed. This program [Asia Pacific Laboratory Accreditation Cooperation (APLAC) T049] was the first of its kind for an herbal matrix and involved the participation of 70 laboratories from 26 countries worldwide. Consensus mean values were computed statistically from the reported results, which were eventually used to assess the performance of individual laboratories in terms of the z-scores. The distribution of analytical data was found to be widespread, with standard deviation ranging from 43.9 to 55.9%, and the result patterns obtained were similar to those residue pesticide programs using other matrixes. Although the estimation of measurement uncertainty is a crucial requirement for all quantitative tests for laboratories that meet the requirements of International Organization for Standardization/International Electrotechnical Commisssion (ISO/IEC) 17025, some laboratories in this program had difficulties and showed unfamiliarity with respect to that quality criterion. It was recommended that laboratories review and rectify the situation promptly so that they would have a better understanding of measurement uncertainty or the test service provided. PMID:17760352

  15. Pesticide reducing instruments : an interdisciplinary analysis of effectiveness and optimality

    DEFF Research Database (Denmark)

    Jacobsen, Lars-Bo; Jensen, JØrgen Dejgård

    2005-01-01

    For decades the concerns about the impact of modern agriculture’s use of pesticides have been one of the most debated issues within Danish environmental politics. Several action plans have aimed at reducing the use of pesticides, but the scientific basis of these has not been well justified. The aim of this paper is to analyze the effectiveness of different instruments targeting unilateral pesticide reductions in Danish agriculture as well as whether the benefit from further reductions exceeds the social costs. The last issue is a novel feature of this paper since it requires the collaboration and linkage of very different research disciplines and modeling tools. In the paper we combine several analytical tools in search of an effective pesticide instrument and an optimal application of such an instrument. The tools under considerations are firstly a CGE model used for evaluating the cost and to calculate general economic and sectoral consequences. This CGE model is linked to an agricultural sector model calculating the optimal use of land, and the agricultural sector model is then linked to a biological agent based simulation model (ABM) calculating changes in the population of a key species of farmland bird, caused to changes in production and landscape. The results from the agricultural sector model are also used in evaluation of pesticide usage and the leaching of pesticides to ground water. First we analyze the implication of three different scenarios in all of the above-mentioned models and tools. All three scenarios are constructed such that they result in the same welfare implication (measured by national consumption in the CGE model). The scenarios are: 1) pesticide taxes resulting in a 25 percent overall reduction; 2) use of unsprayed field margins, resulting in the same welfare loss as in scenario 1; and finally 3) increased conversion to organic farming also resulting in the same welfare loss as in scenario 1. Biological and geological results from the first part of our analysis suggest that theuse of unsprayed field margins is the most cost-effective instrument for improving bio-diversity and securing drinking water. That is, combining economic modeling with physical biological modeling and geological evaluation allows us to select unsprayed field margins as the most effective instrument. Sensitivity analysis conducted on bio-diversity suggest that this result is globally stable Having concluded that unsprayed field margins are the most effective instrument, we proceed by including valuation studies of increased bio-diversity which allows us to estimate the total value of increased biodiversity in the field margins scenario and thus contributes to an actual cost-benefit analysis. But further more we also address the question of the optimal size of field margins. Combining the valuation studies, with a series of analysis from both the biodiversity model (ABM) and the CGE model enables us to obtain the total abatement cost and benefit curves. From these curves we can then deduce the marginal benefit and cost curves, which allow us to determine the optimal size of unsprayed field margins.

  16. Studies on organochlorine pesticide residues in human breast milk of primparae mothers from selected areas in the Greater Accra Region

    International Nuclear Information System (INIS)

    A study was conducted to determine the types and levels of organochlorine pesticide residuals in the human milk samples of 42 nursing mothers from Ada and Accra. The milk samples were analyzed for 14 different organochlorine pesticides residue (Aldrin, Dieldrin, p,p'-DDT, p,p'-DDE, Endrin, Endrin Aldehyde, Endrin Ketone, Endosulphan sulfate,' Alpha Endosulphan, Gamma-HCH, Delta-HCH, Gamma Chlordane, Heptachlor and Methoxychlor) using Gas chromatography with electron capture detector. The mean concentrations for the organochlorine pesticide residues detected in the human milk samples from Accra are; Gamma-HCH (4.207µg/kg fat), Delta-HCH (13.855µg/kg fat), Heptachlor (11.791µg/kg fat), Aldrin (2.962µg/kg fat), Gamma- Chlordane (1.839µg/kg fat), Alpha-Endosulfan (4.740µg/kg fat), p,p'-DDE (23.367µg/kg fat), Dieldrin (2.407µg/kg fat), p,p'-DDT (3.085µg/kg fat), Endrin (7.669µg/kg fat), Endrin Aldehyde (7.769µg/kg fat), Endosulfan-Sulphate (99.052µg/kg fat), Endrin Ketone (63.846µg/kg fat), and Methoxychlor (20.116µg/kg fat). The mean concentrations of the various organochlorine pesticide residues detected in the human milk samples from Ada are; Gamma-HCH (5.438µg/kg fat), DeIta-HCH (6.728µg/kg fat), Heptachlor (0.682µg/kg fat), Aldrin (2.38µg/kg fat), Gamma- Chlordane (1.304µg/kg fat), Alpha-Endosulfan (2.588µg/kg fat), p,p'-DDE (24.165µg/kg fat), Dieldrin (2.222µg/kg fat), p,p'-DDT (3.468µg/kg fat), Endrin (6.339 µg/kg fat), Endosulfan-Sulphate (63.803)µg/kg fat), Endrin Ketone (11.167)µg/kg fat), and Methoxychlor (0.703µg/kg fat). The mean concentration of Endosulfan Sulfate was (99.052Iµ g/kg fat) was highest for the milk samples from Accra. Gamma chlordane recorded the least mean concentration (1.839 µg/kg fat) in the milk samples from Accra. The mean concentration of Endosulfan sulfate (63.803 µg/kg fat) was still the highest as compared to the other organochlorines analyzed for in the milk samples from Ada. Endrin Aldehyde was not detected in the milk samples from