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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. Sampling and sample processing in pesticide residue analysis.

    Science.gov (United States)

    Lehotay, Steven J; Cook, Jo Marie

    2015-05-13

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

  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. [Preparation of samples for proficiency testing of pesticide residue analysis in processed foods].

    Science.gov (United States)

    Okihashi, Masahiro; Osakada, Masakazu; Uchida, Kotaro; Nagayoshi, Haruna; Yamaguchi, Takahiro; Kakimoto, Kensaku; Nakayama, Yukiko; Obana, Hirotaka

    2010-01-01

    To conduct proficiency testing for the analysis of pesticide residues in processed foods, fortified samples of retort curry and pancake were examined. In the case of retort curry, heating and mixing were necessary at the time of preparation to provide a homogenous analytical sample. A mixture of 4 carbamates and 11 organophosphorus pesticides was spiked and 14 of them showed consistent results in the samples. In the case of pancake, 10 kinds of pesticides were added to the pastry. The prepared pastry was them cooked. The relative concentrations of most of the pesticides in the pancake were not affected and all the pesticides showed consistent results in the samples. These results showed that the two tested samples were suitable for proficiency testing. PMID:21071910

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

    Directory of Open Access Journals (Sweden)

    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.

  6. Modelling pesticides residues

    OpenAIRE

    Charles, Raphael

    2004-01-01

    This work is a contribution to the development of a specific method to assess the presence of residues in agricultural commodities. The following objectives are formulated: to identify and describe main processes in environment — plant exchanges, to build of a model to assess the residue concentration at harvest in agricultural commodities, to understand the functioning of the modelled system, to characterise pesticides used in field crops and identify optimisation potentials in phytosanitary...

  7. Uncertainty of the sample size reduction step in pesticide residue analysis of large-sized crops.

    Science.gov (United States)

    Omeroglu, P Yolci; Ambrus, Á; Boyacioglu, D; Majzik, E Solymosne

    2013-01-01

    To estimate the uncertainty of the sample size reduction step, each unit in laboratory samples of papaya and cucumber was cut into four segments in longitudinal directions and two opposite segments were selected for further homogenisation while the other two were discarded. Jackfruit was cut into six segments in longitudinal directions, and all segments were kept for further analysis. To determine the pesticide residue concentrations in each segment, they were individually homogenised and analysed by chromatographic methods. One segment from each unit of the laboratory sample was drawn randomly to obtain 50 theoretical sub-samples with an MS Office Excel macro. The residue concentrations in a sub-sample were calculated from the weight of segments and the corresponding residue concentration. The coefficient of variation calculated from the residue concentrations of 50 sub-samples gave the relative uncertainty resulting from the sample size reduction step. The sample size reduction step, which is performed by selecting one longitudinal segment from each unit of the laboratory sample, resulted in relative uncertainties of 17% and 21% for field-treated jackfruits and cucumber, respectively, and 7% for post-harvest treated papaya. The results demonstrated that sample size reduction is an inevitable source of uncertainty in pesticide residue analysis of large-sized crops. The post-harvest treatment resulted in a lower variability because the dipping process leads to a more uniform residue concentration on the surface of the crops than does the foliar application of pesticides. PMID:23039817

  8. 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)

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

    Science.gov (United States)

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

    2005-01-01

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

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

    Scientific Electronic Library Online (English)

    Lucía, Pareja; Silvina, Niell; Zisis, Vryzas; Joaquín, González; María Verónica, Cesio; Euphemia P., Mourkidou; Horacio, Heinzen.

    2015-04-01

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

  11. Pesticide residues in canned foods, fruits, and vegetables: the application of Supercritical Fluid Extraction and chromatographic techniques in the analysis.

    Science.gov (United States)

    El-Saeid, Mohamed H

    2003-12-11

    Multiple pesticide residues have been observed in some samples of canned foods, frozen vegetables, and fruit jam, which put the health of the consumers at risk of adverse effects. It is quite apparent that such a state of affairs calls for the need of more accurate, cost-effective, and rapid analytical techniques capable of detecting the minimum concentrations of the multiple pesticide residues. The aims of this paper were first, to determine the effectiveness of the use of Supercritical Fluid Extraction (SFE) and Supercritical Fluid Chromatography (SFC) techniques in the analysis of the levels of pesticide residues in canned foods, vegetables, and fruits; and second, to contribute to the promotion of consumer safety by excluding pesticide residue contamination from markets. Fifteen different types of imported canned and frozen fruits and vegetables samples obtained from the Houston local food markets were investigated. The major types of pesticides tested were pyrethroids, herbicides, fungicides, and carbamates. By using these techniques, the overall data showed 60.82% of the food samples had no detection of any pesticide residues under this investigation. On the other hand, 39.15% different food samples were contaminated by four different pyrethroid residues +/- RSD% ranging from 0.03 +/- 0.005 to 0.05 +/- 0.03 ppm, of which most of the pyrethroid residues were detected in frozen vegetables and strawberry jam. Herbicide residues in test samples ranged from 0.03 +/- 0.005 to 0.8 +/- 0.01 ppm. Five different fungicides, ranging from 0.05 +/- 0.02 to 0.8 +/- 0.1 ppm, were found in five different frozen vegetable samples. Carbamate residues were not detected in 60% of investigated food samples. It was concluded that SFE and SFC techniques were accurate, reliable, less time consuming, and cost effective in the analysis of imported canned foods, fruits, and vegetables and are recommended for the monitoring of pesticide contaminations. PMID:14755112

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

    Science.gov (United States)

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

  13. 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)

  14. 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.

  15. A new analysis method with GC or GC-MS for the quick detection of pesticide residues in vegetables.

    Science.gov (United States)

    Guo, Jianyu; Zhang, Xiangmin

    2005-03-01

    A new analytical method for gas chromatography (GC) or GC-mass spectrometry (MS) using the direct sampling technique is described. This direct sampling technique, which bypasses the conventional complicated sample pretreatment process, is applicable to cases of fast detection of pesticide residues in foods and large-scale screening of samples by portable GC in field detection. By a direct sampling technique, the vegetable sample is ground into paste, and 30 mg is placed directly into the evaporating chamber for GC-MS identification and quantitation (by full-scan mode). The GC column used is an HP-5 (30.0-m x 250-microm x 0.25-microm, 5% phenyl methyl siloxane). Chlorpyrifos, bromophos, fenpropathrin, gamma-666, and pp'-DDT are chosen to represent organophosphorus, pyrethrins, and organochlorine pesticides because they are chief objects of the detection of pesticide residues in vegetables. Rape, a common and mass-consumed vegetable in China, is chosen as the sample in this study. The detection limits for these pesticides by the full-scan mode are all below the maximum pesticide residue limit of vegetables set by the Ministry of Agriculture of China, and the reproducibility of this method is acceptable. This analysis method is proven to be simple, quick, and reliable and is suitable for multipesticide residues analysis of vegetables. It can also be used in the analysis of vegetable components and signal chemicals. PMID:15842755

  16. 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

  17. Impact analysis of IPM programs in Basmati rice by estimation of pesticide residues.

    Science.gov (United States)

    Mukherjee, Irani; Arora, Sumitra

    2011-03-01

    Samples of Basmati rice grain, soil and water were collected, from IPM and non-IPM field trials conducted at four regions of Haryana, Uttar Pradesh and Uttarakhand in India, for pesticide residue analysis. Out of 45 soil samples collected, only four non-IPM samples indicated the presence of chlorpyrifos and endosulfan in the range of ND (<0.001) to 0.05 mg/kg. Carbendazim used at two locations of Dehradun and Kaithal was found below detectable limit (<0.05 mg/kg) in both IPM and non-IPM trials. Out of total 22 samples of water analyzed, chlorpyriphos was detected in samples from Kaithal and Pant Nagar in the range 0.003-0.006 ?L/L, alpha -endosulfan isomer was detected in the range 0.005-0.03 ?L/L and the beta-isomer in the range 0.005-0.02 ?L/L in sample from Pant Nagar and Kaithal. The residues in all the grain sample of paddy were below detectable limit (<0.001-0.05 mg/kg). The insecticides applied in IPM as well as non-IPM trials were found to be below maximum residue level (MRL). PMID:21279627

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

    Science.gov (United States)

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

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

    Directory of Open Access Journals (Sweden)

    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.

  20. 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) (<0.001-0.05 ?g/g) in all 24 samples of rice grains and soil under IPM and non-IPM trials. Residues were below detection level (<0.001-0.05 ?g/L) in irrigation water samples (2008-09). Residues of tricyclazole and carbendazim, analyzed from same locations, revealed pesticide residues as BDL (<0.001-0.05 ?g/g) in all 40 samples of Basmati rice grains and soil. It was also observed as BDL (<0.001-0.05 ?g/L) for 12 water samples (2009-2010). The 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

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

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    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.

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

    Science.gov (United States)

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

    2015-04-01

    The feasibility of the production of a reference material for pesticide residue analysis in a cucumber matrix was investigated. Cucumber was spiked at 0.075 mg/kg with each of the 15 selected pesticides (acetamiprid, azoxystrobin, carbendazim, chlorpyrifos, cypermethrin, diazinon, (??+??)-endosulfan, fenitrothion, imazalil, imidacloprid, iprodione, malathion, methomyl, tebuconazole and thiabendazole) respectively. Three different strategies were considered for processing the material, based on the physicochemical properties of the vegetable and the target pesticides. As a result, a frozen spiked slurry of fresh cucumber, a spiked freeze-dried cucumber powder and a freeze-dried cucumber powder spiked by spraying the powder were studied. The effects of processing and aspects related to the reconstitution of the material were evaluated by monitoring the pesticide levels in the three materials. Two separate analytical methods based on LC-MS/MS and GC-MS/MS were developed and validated in-house. The spiked freeze-dried cucumber powder was selected as the most feasible material and more exhaustive studies on homogeneity and stability of the pesticide residues in the matrix were carried out. The results suggested that the between-unit homogeneity was satisfactory with a sample intake of dried material as low as 0.1 g. A 9-week isochronous stability study was undertaken at -20 °C, 4 °C and 18 °C, with -70 °C designated as the reference temperature. The pesticides tested exhibited adequate stability at -20 °C during the 9-week period as well as at -70 °C for a period of 18 months. These results constitute a good basis for the development of a new candidate reference material for selected pesticides in a cucumber matrix. PMID:25627789

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

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    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.

  4. 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

  5. ANALYSIS OF PESTICIDE RESIDUES IN HUMAN AND ENVIRONMENTAL SAMPLES: A COMPILATION OF METHODS SELECTED FOR USE IN PESTICIDE MONITORING PROGRAMS

    Science.gov (United States)

    This manual provides the pesticide chemist with methodology useful in determining human exposure to pesticides and related industrial chemicals. Methods are also presented for measuring the extent of environmental contamination with these compounds. This manual has been compiled ...

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

    International Nuclear Information System (INIS)

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

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

    Scientific Electronic Library Online (English)

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

    2014-04-01

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

  8. 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

  9. 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)

  10. Alternative QuEChERS-based modular approach for pesticide residue analysis in food of animal origin.

    Science.gov (United States)

    Lichtmannegger, Karolina; Fischer, Roman; Steemann, Franz Xaver; Unterluggauer, Hermann; Masselter, Sonja

    2015-05-01

    The approach for pesticide residue analysis in food of animal origin differs strongly from the one established for food of plant origin, as laboratories mainly focus on conventional methods for the analysis of non-polar pesticides known to accumulate in fatty tissues. However, these group-specific methods are very laborious and cost intensive and typically require extraction of fat components followed by extensive clean-up steps to remove matrix constituents. This work highlights the development and validation of a straightforward QuEChERS-derived clean-up procedure enabling facile, precise, and reliable identification and quantitation of pesticide residues in food of animal origin, which can be extended to various other commodities with moderate fat content and applied to replace traditional group-specific methods. Two additional methods for lean and highly fatty commodities complete this well-established "simplified modular system". The proposed method was in-house validated in terms of accuracy and precision, recovery and linearity as well as specificity and sensitivity on two representative commodities for food of animal origin (egg and meat). For the majority of the more than 80 pesticides investigated, satisfactory results were obtained. Procedural matrix calibration was applied for screening purposes in conjunction with GC-MS/MS or LC-MS/MS as integral part of the approach. Apparent recoveries for most of the compounds ranged from 70 to 120 % (RSD?

  11. 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

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

    Science.gov (United States)

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

  13. 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)

  14. Liquid-phase micro-extraction techniques in pesticide residue analysis.

    Science.gov (United States)

    Lambropoulou, Dimitra A; Albanis, Triantafyllos A

    2007-03-10

    Modern trends in analytical chemistry are towards the simplification and miniaturization of sample preparation, as well as the minimization of organic solvent used. In view of this aspect, several novel micro-extraction techniques are being developed in order to reduce the analysis step, increase the sample throughput and to improve the quality and the sensitivity of analytical methods. One of the emerging techniques in this area is liquid-phase micro-extraction (LPME). It is a miniaturized implementation of conventional liquid/liquid extraction (LLE) in which only microliters of solvents are used instead of several hundred milliliters in LLE. It is quick, inexpensive and can be automated. In the last few years, LPME has been combined with liquid chromatography (LC) and capillary electrophoresis (CE), besides the generally used coupling to gas chromatography (GC), and has been applied to various matrices, including biological, environmental, and food samples. This work is aimed at providing an overview of the major developments of LPME, coupled with chromatography and CE, as reported in the literature. The paper will focus on the application of the technique to different matrices and the aim is to reveal the panorama of opportunities and to try to indicate the potential of LPME in pesticide analysis. A critical review of the first applications to pesticide analyses is presented in the main part of the manuscript. The optimization of LPME as well as advantages and disadvantages are discussed. It is concluded that, because of its high pre-concentration factor, LPME can be introduced with benefit into water analysis for several pesticide groups. In particular, the application of LPME to non-polar pesticides in environmental analysis appears to be promising. However, similar to other micro-extraction techniques, such as solid phase micro-extraction (SPME), serious limitations still remain when analyzing semi-solid and solid environmental, food or biological matrices and/or highly polar compounds. Thus, other pre-concentration techniques may be a good alternative if an analytical problem cannot be sufficiently dealt with LPME. PMID:17161462

  15. 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...

  16. 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...

  17. 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...

  18. 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%.

  19. QuEChERS Adaptability for the Analysis of Pesticide Residues in Beehive Products Seeking the Development of an Agroecosystem Sustainability Monitor.

    Science.gov (United States)

    Niell, Silvina; Jesús, Florencia; Pérez, Cecilia; Mendoza, Yamandú; Díaz, Rosana; Franco, Jorge; Cesio, Verónica; Heinzen, Horacio

    2015-05-13

    Beehive products could be powerful monitors of pesticide residues originating in agroecosystems during production cycles. Their ready availability provides enough samples to perform analytical determinations, but their chemical complexity makes residue analysis a real challenge. Taking advantage of the plasticity of QuEChERS coupled to LC-MS/MS, validated methodologies were developed for bees, honey, beeswax, and pollen and applied to real samples for the simultaneous determination of 19 of the most employed pesticides in intensive cropping fields. Beehives placed in Uruguayan agroecosystems accumulated the pesticides thiacloprid, imidacloprid, methomyl, carbaryl, hexythiazox, azoxystrobin, pyraclostrobin, tebuconazole, and haloxyfop-methyl at 0.0001-0.01 mg/kg levels. The oscillations on the amount and occurrence of residue findings for specific apiaries were correlated statistically with the sampling season and the agroecosystem where the beehives were located, showing the potential of bees and bee products to record relevant information to survey the chemicals applied in their surroundings. PMID:25880394

  20. Decline of pesticide residues from barley to malt.

    Science.gov (United States)

    Navarro, S; Pérez, G; Navarro, G; Vela, N

    2007-08-01

    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 was determined. Several samples for residue analysis were taken after each stage of malting (steeping, germination and kilning). Pesticide residue analysis was carried out by GC/ITMS in selected ion monitoring mode. Pesticides decline along the process, although in different proportions. The carryover of residues after steeping was 45-85%. A good correlation (r > 0.92) was observed between percentages removed after steeping and the P(OW) values of pesticides. The amount remaining after malting ranged from 13 to 51% for fenitrothion and nuarimol, respectively. Steeping was the most important stage in the removal of pesticide residues (52%) followed by germination (25%), and kilning (drying and curing, 23%). During malt storage (3 months) the fall in pesticide residues was not significant. Applying the standard first-order kinetics equation (r > 0.95), the half-lives obtained for the pesticides during malt storage varied from 244 to 1533 days for myclobutanil and nuarimol, respectively. PMID:17613072

  1. 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

  2. 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)

  3. 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

  4. 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 [...] 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.

  5. 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)

  6. 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

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

    Science.gov (United States)

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

  8. 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 0.01 mg kg(-1) for most analytes. PMID:25842302

  9. Pesticide residues in chicken eggs - A sample preparation methodology for analysis by gas and liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Hildmann, Fanny; Gottert, Christina; Frenzel, Thomas; Kempe, Guenther; Speer, Karl

    2015-07-17

    A sample preparation method was developed for the analysis of chicken eggs to determine 97 GC and 81 LC amenable residues, including organophosphates, organochlorines, pyrethroids, triazoles, carboxyl-containing compounds, and the indicator PCBs. Hereby, considerations were given to the recoveries of the analytes, the method's suitability for routine analysis, and the assessment of the clean-up effect, for which a simple thin layer chromatography was implemented to visualize the most important lipid classes. The procedure consisted of (I) the extraction by matrix solid phase dispersion, and the clean-up by means of (II) small-scale gel permeation chromatography (GPC) and (III) two different solid phase extractions (SPE) for GC and LC amenable analytes, as well as (IV) the quantification using GC-MS/MS and LC-MS/MS. Cyclohexane/ethyl acetate was chosen as extraction solvent due to its suitability for extracting strong non-polar but also more polar analytes. The classical GPC was scaled down to ensure a 50% lower solvent consumption. The comprehensive investigation of conventional and modern zirconium-oxide-coated SPE materials resulted in the selection of octadecyl-modified silica (C18) combined with primary secondary amine using acetonitrile as elution solvent for GC amenable analytes and pure C18 in combination with acidified methanol for LC amenable pesticides. Compared to the currently established EN 1528 method the sample preparation proposed offered a higher sample throughput and a lower solvent consumption. Furthermore, for the first time the clean-up effectiveness of the sample preparation steps was documented as shown by means of thin-layer chromatography. The validation of chicken eggs proved the fulfillment of the quality control criteria for 164 of the 178 analytes tested, mostly at the lowest validated level of 5?g/kg for pesticides and 0.5?g/kg for the single indicator PCBs. However, the analysis of strongly polar analytes was still problematic, which could be attributed to the extraction and the GPC step. Nevertheless, the successful investigation of EU proficiency test materials (EUPT AO 07-09) confirmed the comparability of the results with the currently established sample preparation procedures and demonstrated the potential of the applicability of the presented method to other matrices as exemplified for lean poultry meat and fatty liquid cream. PMID:26051081

  10. 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)

  11. 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

  12. Proficiency test on the determination of pesticide residues in grapes with multi-residue methods.

    Science.gov (United States)

    Dehouck, Pieter; Grimalt, Susana; Dabrio, Marta; Cordeiro, Fernando; Fiamegos, Yiannis; Robouch, Piotr; Fernández-Alba, Amadeo R; de la Calle, Beatriz

    2015-05-22

    This manuscript presents the results of the International Measurement Evaluation Programme 37 (IMEP-37) study, a proficiency test (PT) which was organised to assess the world-wide performance of food control laboratories on the determination of pesticide residues in grapes. This PT supports the implementation of Regulation (EC) No 396/2005 on maximum residue levels of pesticides in or on food and feed of plant and animal origin. Eighty-one participants reported results, forty from EU Member States and forty-one from outside the EU. The test item was a grape sample spiked with 20 selected pesticides. The results of the participants were rated with z- and zeta (?-) scores in accordance with ISO 13528 and ISO 17043. The standard deviation for the proficiency assessment, ?ˆ, of this PT was set at 25% for the 20 measured pesticides based on previous experience with similar measurands. The results reported to IMEP-37 showed that the participants performed satisfactorily, ranging from 81% (carbendazim) to 97% (azoxystrobin, penconazole, pyrimethanil) of the participating laboratories. However, only 30% of the participants managed to analyze all pesticides satisfactorily. Overall, the performance of the participants in this PT was good but there is room for improvement in the development of multi-residue methods for the simultaneous analysis of a large number of pesticides with an increased accuracy. PMID:25888097

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

    Directory of Open Access Journals (Sweden)

    ZHU Pan

    2013-02-01

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

  14. 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.

  15. Research of pesticide residues on fruit by terahertz spectroscopy technology

    Science.gov (United States)

    Ma, Yehao; Wang, Qiang; Wang, Xiaowei; Wang, Huali

    2011-11-01

    Pesticide residues on the fruit skin are measured by terahertz time-domain spectroscopy (THz-TDS) in 0.2-1.3THz. Pesticide is mainly residues for fruit, which threatens health of human, so the research about the fruit residues is absolutely important. In the experiment, a kind of pesticide carbendazim, orange, and the mixture of them are measured by THz-TDS, and then calculate absorption spectrums through Fourier transform and Fresnel formula. Experiment results indicate that THz-TDS is an effective tool for the measurement of pesticide residues on the fruit skin.

  16. Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in canned and fresh peach.

    Science.gov (United States)

    Costa, Fabiane Pinho; Caldas, Sergiane Souza; Primel, Ednei Gilberto

    2014-12-15

    Original, citrate and acetate QuEChERS methods were studied in order to evaluate the extraction efficiency and the matrix effect in the extraction of pesticides from canned peach samples. Determinations were performed by gas chromatography coupled to mass spectrometry (GC-MS). The proposed method with extraction using the original QuEChERS method and determination by GC-MS was validated. LOQs ranged between 1 and 10 ?g kg(-1) and all analytical curves showed r values higher than 0.99. Recovery values varied from 69% to 125% with RSDs less than 20%. The matrix effect was evaluated and most compounds showed signal enrichment. Robustness was demonstrated using fresh peaches, which provided recovery values within acceptable limits. The applicability of the method was verified and residues of tebuconazole and dimethoate were found in the samples. PMID:25038716

  17. 40 CFR 158.2172 - Experimental use permit microbial pesticides residue data requirements table.

    Science.gov (United States)

    2010-07-01

    ...permit microbial pesticides residue. The test...EUP Microbial Pesticides Residue Data Requirements...Notes 885.2100 Chemical Identity CR ...potable water, fish, and irrigated...permit microbial pesticides residue as referenced...cause adverse human health effects or...

  18. Organochlorine pesticide residues in bovine milk.

    Science.gov (United States)

    Nag, Subir K; Raikwar, Mukesh K

    2008-01-01

    Monitoring of bovine milk of different places in Bundelkhand region of India was carried out to evaluate the status of organochlorine pesticide (OCP) residues. Out of a total of 325 samples 206 (63.38%) were contaminated with residues of different OCPs. The average concentration of total HCH was 0.162 mg/kg. Among the different HCH isomers the frequency of occurrence of alpha-isomer was maximum followed by delta-, gamma- and beta. Endosulfan (alpha, beta, sulfate) was detected in 89 samples with mean concentration of 0.0492 mg/kg while total DDT comprising of DDT, DDE and DDD was present in 114 samples having mean concentration of 0.1724 mg/kg. Dicofol was positive in 17 samples. PMID:17940716

  19. 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.

  20. 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; D. L. Silva

    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...

  1. 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.

  2. 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

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

  3. 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

    ...Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...establishment or modification of regulations for residues of pesticide chemicals in or on various...of regulations in 40 CFR part 180 for residues of pesticide chemicals in or on...

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

    Science.gov (United States)

    2010-10-22

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

  5. 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.

  6. [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

  7. 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.

  8. Monitoring of pesticide residues in human blood from Punjab, India.

    Science.gov (United States)

    Sharma, Anupama; Gill, Jatinder Paul Singh; Bedi, Jasbir Singh

    2015-05-01

    In the present study, the current levels of pesticide residues were studied in the human populace of Punjab state. A total of 111 human blood samples were analyzed by gas chromatography and pesticide residues were detected in 35 % of the blood sample(s). Residues of alpha-hexachlorocyclohexane (?-HCH), beta-hexachlorocyclohexane (?-HCH), p,p'-dichlorodiphenyldichloroethane (p,p' DDD), p,p' dichlorodiphenyldichloroethylene (p,p' DDE), p,p' dichlorodiphenyldichloroethane (p,p' DDT), ?-endosulfan, monocrotophos, profenophos and phosalone were found in human blood samples with mean levels of 1.11, 5.89, 0.51, 3.88, 0.39, 34.90, 0.79, 0.39 and 6.76 ng ml(-1), respectively, with ?-endosulfan as a leading pesticide residue. A paradigm shift in the pattern of the pesticide usage was observed with a shift from organochlorine pesticides to organophosphates. PMID:25773703

  9. 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

  10. Analysis of pesticide residues using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) pesticide multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection.

    Science.gov (United States)

    Payá, Paula; Anastassiades, Michelangelo; Mack, Dorothea; Sigalova, Irina; Tasdelen, Bünyamin; Oliva, José; Barba, Alberto

    2007-11-01

    The Quick Easy Cheap Effective Rugged and Safe multiresidue method (QuEChERS) has been validated for the extraction of 80 pesticides belonging to various chemical classes from various types of representative commodities with low lipid contents. A mixture of 38 pesticides amenable to gas chromatography (GC) were quantitatively recovered from spiked lemon, raisins, wheat flour and cucumber, and determined using gas chromatography-tandem mass spectrometry (GC-MS/MS). An additional mixture of 42 pesticides were recovered from oranges, red wine, red grapes, raisins and wheat flour, using liquid chromatography-tandem mass spectrometry (LC-MS/MS) for determination. The pesticides chosen for this study included many of the most frequently detected ones and/or those that are most often found to violate the maximum residue limit (MRL) in food samples, some compounds that have only recently been introduced, as well as a few other miscellaneous compounds. The method employed involved initial extraction in a water/acetonitrile system, an extraction/partitioning step after the addition of salt, and a cleanup step utilizing dispersive solid-phase extraction (D-SPE); this combination ensured that it was a rapid, simple and cost-effective procedure. The spiking levels for the recovery experiments were 0.005, 0.01, 0.02 and 0.2 mg kg(-1) for GC-MS/MS analyses, and 0.01 and 0.1 mg kg(-1) for LC-MS/MS analyses. Adequate pesticide quantification and identity confirmation were attained, even at the lowest concentration levels, considering the high signal-to-noise ratios, the very good accuracies and precisions, as well as the good matches between the observed ion ratios. Mean recoveries mostly ranged between 70 and 110% (98% on average), and relative standard deviations (RSD) were generally below 10% (4.3% on average). The use of analyte protectants during GC analysis was demonstrated to provide a good alternative to the use of matrix-matched standards to minimize matrix-effect-related errors. Based on these results, the methodology has been proven to be highly efficient and robust and thus suitable for monitoring the MRL compliance of a wide range of commodity/pesticide combinations. PMID:17909760

  11. Multiresidue analysis of four pesticide residues in water dropwort (Oenanthe javanica) via pressurized liquid extraction, supercritical fluid extraction, and liquid-liquid extraction and gas chromatographic determination.

    Science.gov (United States)

    Jeon, Hyang-Rang; Abd El-Aty, Abd El-Aty Mostafa; Abd El-Aty, Mostafa Abd El-Aty; Cho, Soon-Kil; Choi, Jeong-Heui; Kim, Kil-Yong; Park, Ro-Dong; Shim, Jae-Han

    2007-08-01

    The primary objective of this study was to simultaneously analyze the residues of the most commonly used pesticides, chlorpyrifos-methyl, endosulfan, EPN, and iprodione in the water dropwort, via accelerated solvent extraction (ASE), supercritical fluid extraction (SFE), and conventional solvent extraction (LLE) techniques. Residue levels were determined using GC with electron-capture detection (GC-ECD). The confirmation of pesticide identity was performed by GC-MS in a selected ion-monitoring (SIM) mode. In none of the ASE and SFE techniques were the extraction conditions optimized. Rather, the experimental variables were predicated on the author's experience. The ECD response for all pesticides was linear in the studied range of concentrations of 0.005-5.0 ppm, with correlation coefficients in excess of 0.9991. At each of the two studied fortification levels, the pesticides yielded recoveries in excess of 72% with RSDs between 1 and 19%. The LODs were achieved at a range of levels from 0.001 to 0.063 ppm, depending on the pesticide utilized. The LOQs, which ranged from 0.003 to 0.188 ppm, were lower than the maximum residue limits (MRLs) authorized by the Korean Food and Drug Administration (KFDA). All of the methods were applied successfully to the determination of pesticide residues in the real samples. It could, therefore, be concluded that any of the techniques utilized in this investigation might prove successful, given that the applied extraction conditions are wisely chosen. PMID:17638354

  12. 77 FR 3229 - Codex Alimentarius Commission: Codex Committee on Pesticide Residues (CCPR)

    Science.gov (United States)

    2012-01-23

    ...pesticide residues in food and feed; considering...to the safety of food and feed containing pesticide residues; and establishing...environmental and industrial contaminants showing chemical or other similarity to pesticides, in specific food items or...

  13. 76 FR 3601 - Codex Alimentarius Commission: Meeting of the Codex Committee on Pesticide Residues

    Science.gov (United States)

    2011-01-20

    ...pesticide residues in food and feed; considering...to the safety of food and feed containing pesticide residues; and establishing...environmental and industrial contaminants showing chemical or other similarity to pesticides, in specific food items or...

  14. 78 FR 16243 - Codex Alimentarius Commission: Codex Committee on Pesticide Residues (CCPR)

    Science.gov (United States)

    2013-03-14

    ...pesticide residues in food and feed; considering...to the safety of food and feed containing pesticide residues; and establishing...environmental and industrial contaminants showing chemical or other similarity to pesticides, in specific food items or...

  15. 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...

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

    Science.gov (United States)

    de 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 115% with relative standard deviations below 16%. The limits of detection for the pesticides in water and sediment were below 0.003 mg L?1 and 0.02 mg kg?1, respectively. PMID:21165598

  17. Considerations on the Content of Pesticides Residues in Vegetables

    OpenAIRE

    Florica Morar; Catalina-Cristina Bloj

    2011-01-01

    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 amou...

  18. 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

  19. Removal of trace pesticide residues from farm produce

    International Nuclear Information System (INIS)

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

  20. 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...

  1. A multiresidue method for the analysis of pesticide residues in polished rice (Oryza sativa L.) using accelerated solvent extraction and gas chromatography and confirmation by mass spectrometry.

    Science.gov (United States)

    Cho, Soon-Kil; Abd El-Aty, A M; Park, Young-Seok; Choi, Jeong-Heui; Khay, Sathya; Kang, Cheol-Ah; Park, Byung-Jun; Kim, Sun-Ju; Shim, Jae-Han

    2007-06-01

    An analytical procedure using accelerated solvent extraction and gas chromatography with an electron capture detector has been optimized to simultaneously determine the residue of two insecticides (diazinon and EPN) and one fungicide (isoprothiolane) in polished rice and was confirmed by GC-mass spectrometry. Several parameters, including temperature, pressure, solvent ratio, cell size and cell cycle, were thoroughly investigated to find the optimal extraction conditions. The average recoveries of the three pesticides were between 82.7 and 126.4% at spiking levels of 0.1 and 0.5 ppm. The relative standard deviations were less than 7% for all of the recovery tests. The optimum accelerated solvent extraction operating conditions were 100 degrees C, 1500 atm, acetone-n-hexane (20:80 v/v) as the extraction solvent, two cycles, and a cell size of 33 ml. The total extraction time was approximately 20 min. The optimized procedure has also been applied to the determination of diazinon, isoprothiolane and EPN in real rice samples. In conclusion, accelerated solvent extraction was used for the first time for the analysis of diazinon, isoprothiolane and EPN in polished rice and offers the possibility of a fast and simple process for obtaining a quantitative extraction of the studied pesticides. PMID:17385804

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

    Science.gov (United States)

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

  3. 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.

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

    International Nuclear Information System (INIS)

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

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

    Science.gov (United States)

    Malinowska, El?bieta; Jankowski, Kazimierz; Sosnowski, Jacek; Wi?niewska-Kad?ajan, Beata

    2015-06-01

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

  7. Threshold conditions for integrated pest management models with pesticides that have residual effects.

    Science.gov (United States)

    Tang, Sanyi; Liang, Juhua; Tan, Yuanshun; Cheke, Robert A

    2013-01-01

    Impulsive differential equations (hybrid dynamical systems) can provide a natural description of pulse-like actions such as when a pesticide kills a pest instantly. However, pesticides may have long-term residual effects, with some remaining active against pests for several weeks, months or years. Therefore, a more realistic method for modelling chemical control in such cases is to use continuous or piecewise-continuous periodic functions which affect growth rates. How to evaluate the effects of the duration of the pesticide residual effectiveness on successful pest control is key to the implementation of integrated pest management (IPM) in practice. To address these questions in detail, we have modelled IPM including residual effects of pesticides in terms of fixed pulse-type actions. The stability threshold conditions for pest eradication are given. Moreover, effects of the killing efficiency rate and the decay rate of the pesticide on the pest and on its natural enemies, the duration of residual effectiveness, the number of pesticide applications and the number of natural enemy releases on the threshold conditions are investigated with regard to the extent of depression or resurgence resulting from pulses of pesticide applications and predator releases. Latin Hypercube Sampling/Partial Rank Correlation uncertainty and sensitivity analysis techniques are employed to investigate the key control parameters which are most significantly related to threshold values. The findings combined with Volterra's principle confirm that when the pesticide has a strong effect on the natural enemies, repeated use of the same pesticide can result in target pest resurgence. The results also indicate that there exists an optimal number of pesticide applications which can suppress the pest most effectively, and this may help in the design of an optimal control strategy. PMID:22205243

  8. Pesticide residues in liquid pekmez (grape molasses).

    Science.gov (United States)

    Erdo?rul, Ozlem

    2008-09-01

    In this study 32 pesticide residues and eight polybrominated diphenlyl ether (PBDE) congeners were measured in seven liquid samples from Kahramanmara?, Turkey. A new method based on the best recovery was column extraction with n-hexane/acetone followed by gas chromatography electron-capture detection (GC-ECD), and mass spectrometry (GC-MS). Limit of Detection (LOD) was 0.02 ng/g for PCBs and PBDEs and 0.05 ng/g for the others. alpha-HCH, gamma-HCH, HCB, and Heptachlor were being measured in all LP samples. The sum of HCHs, DDTs and PCBs in samples was 1.56, 0.76 and 5.42 ng/g, respectively. p,p'-DDD, p,p'-DDT, o,p'-DDT, cis-nonachlor, beta-endosulfan, endrin, PCB 118, PCB 138, PCB 180 and PBDEs were not detected. The mean values of alpha-HCH, beta-HCH, gamma-HCH, HCB were 0.72, 2.03, 1.92, 3.58 and alpha-chlordan, trans-nonachlor, heptachlor, malathion, aldrin, bromophos methyl, bromophos ethyl, cis-HCE, trans-HCE, chlordan, alpha-endosulfan, dieldrin were 2.44, 0.27, 1.25, 1.27, 0.91, 0.10, 0.50, 0.26, 0.63, 2.44, 0.30, 0.30 ng/g respectively. The mean values of p,p'-DDE, o,p'-DDE, o,p'-DDD were 0.26, 0.48, 0.68 and PCB 28, PCB 52, PCB 101, PCB 153 were 2.35, 35.27, 0.16, 0.18 ng/g, respectively. PMID:17985204

  9. 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)

  10. 77 FR 30481 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2012-05-23

    ...code 311). Pesticide manufacturing...at the end of the pesticide petition summary...and adverse human health impacts or environmental...exposure to the pesticides discussed in this...residues of pesticide chemicals in or on various...moiety, in or on fish at 0.05...

  11. 78 FR 70906 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2013-11-27

    ...manufacturer, or pesticide manufacturer. The...code 311). Pesticide manufacturing...and adverse human health impacts or environmental...exposure to the pesticides discussed in this...residues of pesticide chemicals in or on various...proposing tolerances for fish- freshwater...

  12. 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.

  13. 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

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

    International Nuclear Information System (INIS)

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

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

    Science.gov (United States)

    Wan, Michael T

    2013-01-01

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

  16. 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)

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

    International Nuclear Information System (INIS)

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

  18. 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)

  19. 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

  20. 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.

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

    Science.gov (United States)

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

    2011-06-01

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

  2. 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.

  3. 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.

  4. "Keep a low profile": pesticide residue, additives, and freon use in Australian tobacco manufacturing

    OpenAIRE

    Chapman, S

    2003-01-01

    Objectives: To review the Australian tobacco industry's knowledge of pesticide residue on Australian tobacco and its policies and practices on resisting calls by tobacco control advocates that consumers should be informed about pesticide residue as well as additives.

  5. 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)

  6. 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

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

    OpenAIRE

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

    2011-01-01

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

  8. 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...

  9. 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...

  10. 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.

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

    International Nuclear Information System (INIS)

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

  12. 40 CFR 158.2130 - Microbial pesticides residue data requirements table.

    Science.gov (United States)

    2010-07-01

    ...requirements for microbial pesticides residue. The test...Table—Microbial Pesticides Residue Data Requirements...Notes 885.2100 Chemical Identity CR ...potable water, fish, and irrigated...requirements for microbial pesticides residue as referenced...cause adverse human health effects or...

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

    Science.gov (United States)

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

    2012-01-01

    A multiresidue method based on GC or LC and MS or MS/MS for the determination of 204 pesticides in diverse food matrixes of animal and plant origin is described. The method can include different stages of cleanup according to the chemical characteristics of each sample. Samples were extracted using accelerated solvent extraction. Those with a high fat content or that contained chlorophyll required further purification by gel permeation chromatography and/or SPE (ENVI-Carb). The methodology developed here was fully validated; the LOQs for the 204 pesticides are presented. The LOQ values lie between 0.01 to 0.02 mg/kg. However, in some cases, mainly in baby food, they were as low as 0.003 mg/kg, thereby meeting European Union requirements on maximum residue levels for pesticides, as outlined in European regulation 396/2005 and the Commission Directive 2003/13/EC. The procedure has been accredited for a wide scope of pesticides and matrixes by the Spanish Accreditation Body (ENAC) following ISO/IEC 17025:2005, as outlined in ENAC technical note NT-19. PMID:23451398

  14. 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

  15. Enzyme Biosensor for Detection of Organophosphate Pesticide Residues Base on Screen Printed Carbon Electrode (SPCE)-Bovine Serum Albumin (BSA)

    OpenAIRE

    Ani Mulyasuryani; Mochammad Dofir

    2014-01-01

    The maximum level of organophosphate pesticide residues in rice is 0.1 mg/kg and 0.5 mg/kg in vegetables. The control of pesticide residues in agricultural products required a method of analysis quickly and accurately. The research developed a biosensor for the detection of organophosphate pesticide residues in agricultural products. The research studied immobilized organophosphate hydrolase (OPH) mass and characterization of biosensor. The solution conductivity meas...

  16. 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.

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

    Science.gov (United States)

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

  18. 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

    ...at the end of the pesticide petition summary...and adverse human health impacts or environmental...exposure to the pesticides discussed in this...residues of pesticide chemicals in or on various...and evaluate the chemical forchlorfenuron...parent, in or on fish--...

  19. 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...

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

    Directory of Open Access Journals (Sweden)

    Korrapati Kotinagu

    2015-04-01

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

  1. Organochlorine pesticides residue in lakes of Khorezm, Uzbekistan

    Science.gov (United States)

    Rosen, Michael R.; Nishonov, Bakhriddin; Fayzieva, Dilorom; Saito, L.; Lamers, J.

    2009-01-01

    The Khorezm province in northwest Uzbekistan is a productive agricultural area within the Aral Sea Basin that produces cotton, rice and wheat. Various organochlorine pesticides were widely used for cotton production before Uzbekistan's independence in 1991. In Khorezm, small lakes have formed in natural depressions that receive inputs mostly from agricultural runoff. Samples from lake waters and sediments, as well as water from the Amu Darya River (which is the source of most of the lake water) have been analyzed to study variations in the concentrations of organochlorine pesticides residues during the year. Low concentrations of DDT, DDD, DDE, a-HCH and y-HCH compounds were found in water and sediment samples. The concentration of persistent organochlorine pesticides (DDT and HCH) in water and sediment is much lower than the maximum permissible concentrations that exist for water and soil. According to these preliminary results, the investigated lakes in Khorezm appear to be suitable for recreation or for aquaculture.

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

    Science.gov (United States)

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

    2015-08-01

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

  3. 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.

  4. Rapid simultaneous screening and identification of multiple pesticide residues in vegetables.

    Science.gov (United States)

    Zhang, Fang; Yu, Chongtian; Wang, Wenwen; Fan, Ruojing; Zhang, Zhixu; Guo, Yinlong

    2012-12-13

    A method for the rapid simultaneous screening and identification of multiple pesticide residues in vegetables was established using a novel database and gas chromatography in combination with hybrid quadrupole time-of-flight mass spectrometry (GC-QTOF MS). A total of 187 pesticides with different chemical species were measured by GC-QTOF MS to create the database, which collected the retention time and exact masses of ions from the first-stage mass spectrum (MS(1) spectrum) and second-stage mass spectrum (MS(2) spectrum) for each pesticide. The workflow of the created database consisted of "MS(1) screening" for possible pesticides by chemical formula match and "MS(2) identification" for structural confirmation of product ion by accurate mass measurement. To evaluate the applicability of the database, a spinach matrix was prepared by solid phase extraction, spiked with a mixture of 50 pesticides at seven concentrations between 0.1 and 10ppb, and analyzed by GC-QTOF MS. It was found that all of the 50 pesticides with concentrations as low as 5ppb were detected in the "MS(1) screening" step and accurate masses were identified with errors less than 2.5mDa in the "MS(2) identification" step, indicating high sensitivity, accuracy, selectivity and specificity. Finally, to validate the applicability, the new method was applied to four fresh celery, rape, scallion and spinach vegetables from a local market. As a result, a total of 13 pesticides were found, with 11 in celery, 9 in rape, 3 in scallion and 2 in spinach. In conclusion, GC-QTOF MS combined with an exact mass database is one of the most efficient tools for the analysis of pesticide residues in vegetables. PMID:23206394

  5. 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)

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

    Scientific Electronic Library Online (English)

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

    2015-03-01

    Full Text Available Demand for organic products is intensified in many countries each year. Following this trend, Brazil produces increasing volumes of organic grape juice. In this way, a survey of organic grape juices made from grapes produced according to this system was carried out where physicochemical composition, [...] minerals, trace elements, and pesticide residues were determined. Variables related to grape juice composition were performed by physicochemical procedures; minerals and trace elements, by inductively plasma optical emission spectrometry; pesticide residues, by liquid chromatography-mass spectrometry. Main results show that the physicochemical composition of organic grape juices was in general in accordance to the Brazilian legislation. The mean concentrations of trace elements were very low, varying from 0.002 (Cd) to 0.970 (Ba) mg L–1. Pesticide residues were not detected in any sample analyzed (MRL= 10 µg L–1). These results show that the Serra Gaúcha viticultural region present conditions to produce organic grape juices, despite the adverse climate factors that occurs in some years. Nevertheless, these products should be made with grape varieties, such as the labrusca ones, less susceptibles to the main grapevine pathogens.

  7. 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.

  8. 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

  9. 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

  10. Organochlorine pesticide residues in biological compartments of healthy mothers.

    Science.gov (United States)

    Elserougy, Safaa; Beshir, Safia; Saad-Hussein, Amal; Abouarab, Assem

    2013-06-01

    The present study was conducted to detect placental and breast milk (BM) transfer of organochlorine pesticides (OCPs) between biological compartments in healthy lactating mothers. The study explores the effect of parity, breast-feeding and urban/rural residence on body burden of OCP residues. The study included 38 healthy participants submitted to cesarean delivery. Sociodemographic data and specimens of maternal and umbilical sera, adipose tissue (Adp T) and BM were collected. Specimens were analyzed to detect OCP residues. The lindane in BM, o,p'-dichlorodiphenyldichloroethane (DDD) in maternal serum (MS) and total dichlorodiphenyltrichloroethane (DDT) and o,p'-dichlorodiphenyldichloroethylene in umbilical serum were the only detected residues in significantly higher frequencies and/or means in the primigravidae than multigravidae. There was a high risk of detecting o,p'-DDD (odds ratio = 8.3) in umbilical serum of the mothers with o,p'-DDD detected in the MS. Total DDT was detected in about 65% of specimens of BM, MS and Adp T and in about 40% of the umbilical serum specimens. There was only a significant positive correlation between total DDT residues in the BM and Adp T. Total DDT residues in umbilical serum and Adp T were significantly higher in the urban than in the rural mothers. The detection of some OCPs in maternal biological compartments suggests their potential placental and BM transfer to her child during pregnancy and lactation, respectively. Furthermore, it might reflect the persistence or recent use of these pesticides in the environment. PMID:22368179

  11. Use of Combined Uncertainty of Pesticide Residue Results for Testing Compliance with Maximum Residue Limits (MRLs).

    Science.gov (United States)

    Farkas, Zsuzsa; Slate, Andrew; Whitaker, Thomas B; Suszter, Gabriella; Ambrus, Árpád

    2015-05-13

    The uncertainty of pesticide residue levels in crops due to sampling, estimated for 106 individual crops and 24 crop groups from residue data obtained from supervised trials, was adjusted with a factor of 1.3 to accommodate the larger variability of residues under normal field conditions. Further adjustment may be necessary in the case of mixed lots. The combined uncertainty of residue data including the contribution of sampling is used for calculation of an action limit, which should not be exceeded when compliance with maximum residue limits is certified as part of premarketing self-control programs. On the contrary, for testing compliance of marketed commodities the residues measured in composite samples should be greater than or equal to the decision limit calculated only from the combined uncertainty of the laboratory phase of the residue determination. The options of minimizing the combined uncertainty of measured residues are discussed. The principles described are also applicable to other chemical contaminants. PMID:25658668

  12. Pesticide residues in groundwater in The Netherlands: state of observations and future directions of research.

    Science.gov (United States)

    Loch, J P; Verdam, B

    1989-01-01

    In the first stage of a programme of sampling and analysis for pesticide residues in groundwater in The Netherlands, the upper groundwater below four vulnerable soils was analysed for nearly 2,5 years in eight sampling rounds. Of 18 compounds analysed, including some metabolites, 1,3-dichloropropene, aldicarb, ethoprophos dinoseb, metamitron, atrazine, desethyl- and desisopropylatrazine, metolachlor and ethylenethioureum were repeatedly detected in the groundwater in concentrations above 0.1 micrograms.dm-3, the limit for pesticides in drinking water set by the EC. These observations were made below fields with potatoe-, maize- and bulb flower culture, all on low-humic to moderately humic sandy soils. No residues were found below a cracked light clay on a sandy subsoil. On the locations sampled evidence was found for complete in situ removal in the upper groundwater of 1,3-dichloropropene, high persistence of aldicarb residues and partial in situ degradation of dinoseb. PMID:2756375

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

    OpenAIRE

    Spiridon Kintzios; Alexandros Michaelides; Olga Mangana; Georgia Moschopoulou; Kelly Flampouri; Sophie Mavrikou

    2008-01-01

    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 ...

  14. Application of high-performance liquid chromatography-tandem mass spectrometry with a quadrupole/linear ion trap instrument for the analysis of pesticide residues in olive oil.

    Science.gov (United States)

    Hernando, M D; Ferrer, C; Ulaszewska, M; García-Reyes, J F; Molina-Díaz, A; Fernández-Alba, A R

    2007-11-01

    This article describes the development of an enhanced liquid chromatography-mass spectrometry (LC-MS) method for the analysis of pesticides in olive oil. One hundred pesticides belonging to different classes and that are currently used in agriculture have been included in this method. The LC-MS method was developed using a hybrid quadrupole/linear ion trap (QqQ(LIT)) analyzer. Key features of this technique are the rapid scan acquisition times, high specificity and high sensitivity it enables when the multiple reaction monitoring (MRM) mode or the linear ion-trap operational mode is employed. The application of 5 ms dwell times using a linearly accelerating (LINAC) high-pressure collision cell enabled the analysis of a high number of pesticides, with enough data points acquired for optimal peak definition in MRM operation mode and for satisfactory quantitative determinations to be made. The method quantifies over a linear dynamic range of LOQs (0.03-10 microg kg(-1)) up to 500 microg kg(-1). Matrix effects were evaluated by comparing the slopes of matrix-matched and solvent-based calibration curves. Weak suppression or enhancement of signals was observed (product ion (EPI) and MS3 were developed. PMID:17713761

  15. 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.

  16. 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.

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

    Science.gov (United States)

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

    2014-09-01

    This study investigates if acclimatization to residual pesticide contamination in agricultural soils is reflected in detoxification, antioxidant enzyme activities and energy budget of earthworms. Five fields within a joint agricultural area exhibited different chemical and farming histories from conventional cultivation to organic pasture. Soil multiresidual pesticide analysis revealed up to 9 molecules including atrazine up to 2.4 ng g(-1) dry soil. Exposure history of endogeic Aporrectodea caliginosa and Allolobophora chlorotica modified their responses to pesticides. In the field, activities of soluble glutathione-S-transferases (sGST) and catalase increased with soil pesticide contamination in A. caliginosa. Pesticide stress was reflected in depletion of energy reserves in A. chlorotica. Acute exposure of pre-adapted and naïve A. caliginosa to pesticides (fungicide Opus(®), 0.1 ?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. PMID:24874794

  18. 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

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

    Science.gov (United States)

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

    2015-08-01

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

  20. 77 FR 8755 - Receipt of a Pesticide Petition Filed for Temporary Tolerance Exemption for Residues of...

    Science.gov (United States)

    2012-02-15

    ...for Temporary Tolerance Exemption for Residues of Prohydrojasmon in or on Various Commodities...requesting the amendment of regulations for residues of pesticide chemicals in or on various...of a regulation in 40 CFR part 180 for residues of pesticide chemicals in or on...

  1. [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

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

    OpenAIRE

    Charles M. Benbrook; Brian P. Baker

    2014-01-01

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

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

    DEFF Research Database (Denmark)

    Petersen, Annette; Jensen, Bodil Hamborg

    2013-01-01

    The present report presents the results from the 2004-2011 period of the monitoring programmes conducted by The Danish Veterinary and Food Administration. The programmes included commodities of fruit, vegetable, cereals and animal origin using random sampling from food on the Danish market. Since the beginning of the 1960, Denmark has monitored fruit and vegetables for pesticides residues. For the periods 1993-1997 and 1998-2003, results were collated and the dietary exposure was calculated. In this report data for the analyses carried out in the period 2004-2011 are reported as well as the exposure calculations performed on the background of the residues found. All the analyses have been carried out by the laboratory of the Danish Veterinary and Food Administration in Ringsted. The samples were collected by the food control offices. The residue data have been combined with consumption data and the exposures for different consumer groups have been estimated.

  4. 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

  5. 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

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

    Science.gov (United States)

    Seiber, James N; Kleinschmidt, Loreen A

    2011-07-27

    The principles of modern pesticide residue chemistry were articulated in the 1950s. Early authors pointed out the advantages of systematizing and standardizing analytical methods for pesticides so that they could be widely practiced and the results could be reproduced from one laboratory to the next. The availability of improved methods has led to a much more complete understanding of pesticide behavior and fate in foods and the environment. Using methods based largely upon gas chromatography (GC) and high-performance liquid chromatography (HPLC) coupled increasingly with mass spectrometry (MS) and MS(n) as the detection tool, residues can be measured at parts per billion levels and below in a variety of food and environmental matrices. Development of efficient extraction and cleanup methods, techniques such as ELISA, efficient sample preparation techniques such as QuEChERS, and automated laboratory and field instrumentation has also contributed to the tools available for use in modern pesticide residue analysis. As a result, great strides have been made in improving food and worker safety and in understanding environmental behavior and fate of pesticides. There are many challenges remaining in the field of pesticide residue chemistry that will continue to stimulate analytical chemists. New chemistries are emerging, often patterned on complex natural products. Analyzing for the parent chemicals and potentially multiple breakdown products will require analytical ingenuity. The development of more sensitive bioassays and knowledge of unintended side effects will challenge residue chemistry as well, as in the case of following the fate of environmental endocrine disruptors associated with some pesticides as well as nonpesticide contaminants from packaging materials and other familiar articles. Continued funding and other resources to ensure better training, international cooperation, and accelerated research and development activities will be a constant need in pesticide residue chemistry as it is for all areas of science that aim to mitigate or eliminate contaminants that can affect human and environmental health and safety. PMID:21473621

  7. 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.

  8. 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

  9. REDUCTION OF MATRIX EFFECTS IN PESTICIDE RESIDUE ANALYSIS IN FOOD BY PROGRAMMABLE TEMPERATURE VAPORIZER / REDUCCIÓN DEL EFECTO MATRIZ EN EL ANÁLISIS DE RESIDUOS DE PLAGUICIDAS EN ALIMENTOS MEDIANTE EL USO DEL INYECTOR DE TEMPERATURA PROGRAMADA

    Scientific Electronic Library Online (English)

    D.A, AHUMADA; J.A., GUERRERO.

    2013-12-01

    Full Text Available Background: The phenomenon known as the ''matrix-induced chromatographic response enhancement'' commonly affects the sensibility, precision, and accuracy in pesticide residue analysis. The presence of matrix effects can be given by adsorption and/or thermal decomposition of pesticides on the gas chr [...] omatograph injection port. Objective: To reduce the matrix-induced chromatographic response enhancement on pesticide residues analysis in food through the use of several operational modes of programmable temperature vaporizer inlet. Methods: The analyses were carried out in potato (Solanum tuberosum) extracts by gas chromatography with mass spectrometry detector. In this study, four programmable temperature vaporizer splitless modes were investigated: hot, pulsed, cold and solvent vent. Another topic developed in this study has to do with the influence of injection volume, assessed for the matrix effects. Results: The analysis of variance (ANOVA) (? = 0.05) indicates that when the hot splitless is used most compounds are subjected to matrix-induced chromatographic response enhancement. Furthermore, with the pulsed splitless, a decrease in the number of compounds with matrix-induced chromatographic response enhancement was found, approximately 20% compared to the classic hot splitless. Finally, a remarkable decrease in matrix-induced effects was found when cold splitless mode was used, since there was up to 55% reduction in the compounds, relative to traditional hot splitless, that showed statistical differences between responses in matrix-free standards and matrix-matched standards. Conclusions: It was found that the use of conventional hot splitless and pulsed splitless modes caused matrix-induced effects in more than 70% of the studied compounds. In addition, the results indicate that for most compounds there is an inverse relationship between matrix-induced chromatographic response enhancement and the volume of injection.

  10. 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

    ...chemicals in or on various food commodities. EPA has...of pesticides in or on food commodities. Further...for residues of the antifungal agent Aspergillus flavus...this pesticide occurs naturally and would be present...commodities, Feed additives, Food additives,...

  11. 78 FR 1798 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2013-01-09

    ...chemicals in or on various food commodities. The Agency is...residues of pesticides in or on food commodities. Further information...this unit. PP 2F8056. Fine Agrochemicals Ltd. c/o SciReg, Inc...commodities, Feed additives, Food additives, Pesticides...

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

    Directory of Open Access Journals (Sweden)

    Wen Li

    2013-04-01

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

  13. 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

  14. [Laser Raman spectrum analysis of carbendazim pesticide].

    Science.gov (United States)

    Wang, Xiao-bin; Wu, Rui-mei; Liu, Mu-hua; Zhang, Lu-ling; Lin, Lei; Yan, Lin-yuan

    2014-06-01

    Raman signal of solid and liquid carbendazim pesticide was collected by laser Raman spectrometer. The acquired Raman spectrum signal of solid carbendazim was preprocessed by wavelet analysis method, and the optimal combination of wavelet denoising parameter was selected through mixed orthogonal test. The results showed that the best effect was got with signal to noise ratio (SNR) being 62.483 when db2 wavelet function was used, decomposition level was 2, the threshold option scheme was 'rigisure' and reset mode was 'sln'. According to the vibration mode of different functional groups, the de-noised Raman bands could be divided into 3 areas: 1 400-2 000, 700-1 400 and 200-700 cm(-1). And the de-noised Raman bands were assigned with and analyzed. The characteristic vibrational modes were gained in different ranges of wavenumbers. Strong Raman signals were observed in the Raman spectrum at 619, 725, 964, 1 022, 1 265, 1 274 and 1 478 cm(-1), respectively. These characteristic vibrational modes are characteristic Raman peaks of solid carbendazim pesticide. Find characteristic Raman peaks at 629, 727, 1 001, 1 219, 1 258 and 1 365 cm(-1) in Raman spectrum signal of liquid carbendazim. These characteristic peaks were basically tallies with the solid carbendazim. The results can provide basis for the rapid screening of pesticide residue in food and agricultural products based on Raman spectrum. PMID:25358165

  15. 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 pesticides 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.

  16. Organochlorine pesticide residues in dairy products in Jordan.

    Science.gov (United States)

    Salem, Nida' M; Ahmad, Rafat; Estaitieh, Hussein

    2009-10-01

    The use of aldrin, dieldrin, endrin, heptachlor and hexachlorobenzene (HCB) has been banned in Jordan officially in 1981, and of dichlorodiphenyltrichloroethane (DDT) in 1995. However, residues of such compounds can still be found in the environment and in foodstuffs. Dairy products are an important exposure route for organochlorine pesticides (OCPs) to humans. For this reason, the presence of OCP residues in 233 dairy product samples; comprising milk, butter, cheese, labaneh and yoghurt collected from Jordan was determined. All samples were analyzed for their residual contents of aldrin, DDT and metabolites (DDTs), dieldrin, endosulfan isomers, endrin, hexachlorocyclohexane isomers (HCHs), heptachlor and HCB. Levels of these compounds were determined by gas chromatography with electron capture detector (GC-ECD). The results indicated that 9% (21/233), 8.5% (20/233), 6% (14/233) and 2.1% (5/233) of the examined samples were contaminated with beta-HCH, pp'-DDE, alpha-HCH and gamma-HCH, respectively. Heptachlor and alpha-endosulfan were only present in less than 2% of the analyzed samples. None of the samples revealed the presence of aldrin, op'-DDD, pp'-DDD, op'-DDE, op'-DDT, pp'-DDT, dieldrin, beta-endosulfan, endrin and HCB at their detection limits. The order for the contamination in the analyzed dairy products was labaneh>cheese>yoghurt>butter>milk. This study has provided the preliminary information on the concentration of OCPs in dairy products for the first time in Jordan. The results will help in a scientific assessment of the implications of pesticide residues with regards to human risks in Jordan. PMID:19695668

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

    OpenAIRE

    Yao Xin; Jiang Feng; Liu Xiaoyu; Hu Haoyu; Cui Xiaocheng

    2010-01-01

    Abstract Background Organophosphorous pesticides are the most popular pesticides used in agriculture. As acetylcholinesterase inhibitors, organophosphorous pesticides are toxic organic chemicals. The control and detection of organophosphorous pesticide residue in food, water, and environment therefore plays a very important role in maintaining physical health. A sensitive, rapid, simple chemiluminescence(CL) method has been developed for the determination of quinalphos based on the reaction o...

  18. 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...

  19. 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

  20. Practical tracer investigations of pesticide residues in agricultural ecosystem

    International Nuclear Information System (INIS)

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

  1. 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.

  2. Residues of organochlorine pesticides in human fat in Belgium.

    Science.gov (United States)

    Dejonckheere, W; Steurbaut, W; Verstraeten, R; Kips, R H

    1978-03-01

    In 1975, 60 samples of human body fat taken during the course of routine examinations by pathologists were analysed for organochlorine pesticide residues. The mean detected concentrations are 1.36 ppm for HCB, 0.76 ppm for betaHCH, 0.38 ppm for heptachlor epoxide, 0.26 ppm for dieldrin, 6.50 ppm for ppDDE, 0.27 ppm for ppDDD and 1.52 ppm for ppDDT. By comparing these results with earlier studies in 1969 and 1966 a decrease in the total HCH and ppDDT content and an increase in the dieldrin and heptachlor epoxide content is observed. HCB was not determined in earlier studies. PMID:741475

  3. 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)

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

    Science.gov (United States)

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

  5. 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.

  6. 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

  7. 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...

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

    OpenAIRE

    FERDI BRAHUSHI; ENDRIT KULLAJ

    2014-01-01

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

  9. 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.

  10. 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.

    Science.gov (United States)

    Sapozhnikova, Yelena; Lehotay, Steven J

    2013-01-01

    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 1h/analyst, and LP-GC/MS-MS analysis provided fast separation of multiple analytes within 9min 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 0.1-0.5ng g(-1) for PCBs, 0.5-10ng g(-1) for PBDEs, 0.5-5ng g(-1) for select pesticides and PAHs and 1-10ng g(-1) for flame retardants. The developed method was successfully applied for analysis of catfish samples from the market. PMID:23245899

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

    OpenAIRE

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

    2013-01-01

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

  12. 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)

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

    Directory of Open Access Journals (Sweden)

    Charles M. Benbrook

    2014-05-01

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

  14. 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

  15. 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

  16. Public Health Implications of Pesticide Residues in Meat

    OpenAIRE

    Jadhav V.J. and Waskar V.S.

    2011-01-01

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

  17. Multi-Analyst, Multi-Matrix Performance of the QuEChERS Approach for Pesticide Residues in Foods and Feeds Using LC-MS/MS Analysis with Different Calibration Techniques

    Science.gov (United States)

    Three different calibration approaches were applied in liquid chromatography – triple quadrupole tandem mass spectrometry (LC-MS/MS) using electrospray ionization for the determination of 14 diverse pesticide residues at different levels in a variety of food matrices. This study was conducted as p...

  18. ORGANOPHOSPHORUS PESTICIDE RESIDUES IN GREEK VIRGIN OLIVE OIL: LEVELS, DIETARY INTAKE AND RISK ASSESSMENT

    OpenAIRE

    Tsoutsi, Charoula; Konstantinou, Ioannis; Hela, Dimitra

    2008-01-01

    Abstract In this study, the occurrence of organophosphorus pesticides (OPs) and metabolite residues was investigated in 167 samples of Greek virgin olive oil during a two-year (2004–2005) sampling campaign. A total of 30.5% of samples contained detectable residues while only one sample contained dimethoate residues higher than the maximum residue limits. Among the seven detected OPs, fenthion and fenthion sulfoxide residues were detected in 10.8% and 14.4% of the samples...

  19. Occurrence of pesticide residues and transformation products in different types of dietary supplements.

    Science.gov (United States)

    Páleníková, Agneša; Martínez-Domínguez, Gerardo; Arrebola, Francisco Javier; Romero-González, Roberto; Hrouzková, Svetlana; Garrido Frenich, Antonia

    2015-06-01

    The purpose of this study was to evaluate the presence of pesticide residues and transformation products in dietary supplement products. Thirty-two samples were analysed to determine 177 pesticides by gas chromatography-tandem mass spectrometry (GC-MS/MS) and 333 pesticides by liquid chromatography-high-resolution mass spectrometry (LC-HRMS). Pesticides were extracted from different kinds of dietary supplements by the use of a modified QuEChERS extraction method. Six samples contained pesticide residues at concentration up to 92.7 µg kg(-1), but only butralin exceeded the maximum residue limits set for raw material. In addition to target compounds, LC-HRMS enables the simultaneous detection of non-target pesticides. In this case, transformation products of pesticides were detected in the analysed samples using HRMS analyser (Exactive-Orbitrap). These compounds were not included in the original method, and they were monitored as post-target compounds, knowing their molecular formula and exact mass. Mass accuracy was always < 2 ppm, corresponding to a maximum mass error. The positive findings endorse the idea that a deeper and continuous investigation of pesticide residues and transformation products in dietary supplement products is necessary in order to guaranty consumer's safety. PMID:25856415

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

    Directory of Open Access Journals (Sweden)

    Md. Shakhaoat Hossain

    2013-02-01

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

  1. 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

  2. Comparative assessment of pesticide residues in grain, soil, and water from IPM and non-IPM trials of basmati rice.

    Science.gov (United States)

    Arora, Sumitra; Mukherjee, Irani; Kumar, Aman; Garg, D K

    2014-01-01

    The integrated pest management (IPM) modules of pesticide schedule on Basmati rice were validated at field experiments conducted in Northern India for consecutive 3 years (2005-2008). The pesticide residues were found below the detectable limit (basmati rice as safe and economical with pesticide residue-free rice grains. PMID:23996682

  3. 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

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

    OpenAIRE

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

    2013-01-01

    The present study was designed to assess the health risk of pesticide residues via dietary intake of vegetables collected from four top agro-based markets of Dhaka, Bangladesh. High performance liquid chromatography with a photo diode array detector (HPLC-PDA) was used to determine six organophosphorus (chlorpyrifos, fenitrothion, parathion, ethion, acephate, fenthion), two carbamate (carbaryl and carbofuran) and one pyrethroid (cypermethrin) pesticide residues in twelve samples of three comm...

  5. 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)

  6. 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...

  7. 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.

  8. 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.

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

    Directory of Open Access Journals (Sweden)

    Hamedani Morteza Pirali

    2013-01-01

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

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

    Science.gov (United States)

    2013-01-01

    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. PMID:23369650

  11. 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.

  12. Detection of cyclodiene pesticide residues in buffalo meat and effect of cooking on residual level of endosulfan

    OpenAIRE

    Muthukumar, M.; K. Sudhakar Reddy; Narendra Reddy, C.; K. Kondal Reddy; A. Gopala Reddy; Jagdishwar Reddy, D.; Kondaiah, N.

    2010-01-01

    Levels of cyclodiene pesticides (aldrin, ?-endosulfan, ?-endosulfan, endosulfan sulfate and heptachlor) residues in muscle, liver and kidney tissues of buffalo were estimated. The effects of common cooking methods (microwave cooking, boiling, broiling and pressure cooking) on the levels of endosulfan were determined. Aldrin and total endosulfan (?-endosulfan, ?-endosulfan, endosulfan sulfate) residues were found in 42.86 and 64.29% of buffalo tissue samples, with overall mean residual con...

  13. [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

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

    Directory of Open Access Journals (Sweden)

    YAO Xue-Peng

    2013-02-01

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

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

    Science.gov (United States)

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

    2012-12-01

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

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

    Directory of Open Access Journals (Sweden)

    Arafin Gulsan Ara

    2014-02-01

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

  17. Organochlorine pesticide (OCP) residues in cow's, buffalo's, and sheep's milk from Afyonkarahisar region, Turkey.

    Science.gov (United States)

    Bulut, Sait; Akkaya, Levent; Gök, Veli; Konuk, Muhsin

    2011-10-01

    In this study, it was aimed to determine organochlorine pesticides (OCPs) in three types of milk (cow's, buffalo's, and sheep's milk) produced in Afyonkarahisar province of Turkey. The results indicated that these milk specimens were found to be contaminated by 21 different pesticides. Sixteen OCP residues were detected in sheep's milk and it was followed with 14 pesticides in buffalo's milk and 11 pesticides in cow's milk. Dominant pesticides in all samples examined were beta-HCH in buffalo's, cow's, and sheep's milk in the concentrations of 63.36, 91.32, and 122.98 ng/ml, respectively. Total OCP levels were found to be 243.81 ng/ml in sheep's milk, 151.02 ng/ml in cow's milk, and 133.38 ng/ml in buffalo's milk. Some of the pesticides detected were found to be in the excess amount of the acceptable level regarding the EU regulations. PMID:21188503

  18. 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.

  19. 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.

  20. 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

  1. 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.

  2. Radiotracer studies of pesticide residues in food plants

    International Nuclear Information System (INIS)

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

  3. 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)

  4. 75 FR 17715 - Notice of Receipt of a Pesticide Petition Filed for Temporary Tolerance Exemption for Residues of...

    Science.gov (United States)

    2010-04-07

    ...for Temporary Tolerance Exemption for Residues of Prohydrojasmon on Red Apple Varieties...from the requirement of a tolerance for residues of pesticide chemicals in or on various...regulations in 40 CFR part 174 or part 180 for residues of the pesticide chemical...

  5. 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.

  6. 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

  7. 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.

  8. 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)

  9. 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.

  10. 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)

  11. [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

  12. 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 ...

  13. 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)

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

    Directory of Open Access Journals (Sweden)

    A. Mustapha

    2010-01-01

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

  15. 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.

  16. [Analysis on influential factors of Chinese medicinal herb growers' willingness to use green pesticides: evidence on Panax notoginseng production areas in Wenshan, Yunnan province].

    Science.gov (United States)

    Qian, Yun-Xu; Yang, Yue; Zhao, Wei; Cui, Xiu-Ming; Bi, Kai-Shun

    2013-10-01

    The purpose of the article is to apply a binary logistic model to analyze the major factors, which influence Chinese medicinal herb growers' willingness to use green pesticides by using survey data collected in Wenshan, Yunnan Province. The results indicate that, output per capita, average pesticide cost per mu, cognition of pesticide residues, expectations on Panax notoginseng prices, cognition of pesticides' effect of pests control, cognition of P. notoginseng prices of low pesticide residues have a significant influence on growers' willingness to use green pesticides. According to the analysis above, some proposals for enhancing Chinese medicinal herb growers' willingness to use green pesticides are put forward, such as, moving toward the intensive planting systems, fetching down the pieces of green pesticides, emphasizing and propagating the advantages of green pesticides, keeping the prices of Chinese medicinal herb running at steady rates. PMID:24490552

  17. 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...

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

    Directory of Open Access Journals (Sweden)

    A Allahresani

    2010-02-01

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

  19. 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...

  20. 40 CFR 158.2120 - Microbial pesticides product analysis data requirements table.

    Science.gov (United States)

    2010-07-01

    ... Microbial pesticides product analysis data requirements table. 158.2120 Section 158.2120 Protection of Environment ENVIRONMENTAL PROTECTION...AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES...

  1. Potential transport and degradation of “Aged” pesticide residues in soil

    Science.gov (United States)

    “Aging” has been shown to affect the sorption-desorption of pesticides in the soil, which in turn can control transport and degradation processes. Aging effects have been characterized by batch sequential extraction methods, in which sorption coefficients (i.e. Kd) are determined for the chemical re...

  2. 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

  3. 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.

  4. 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...

  5. Residual pesticide detection on food with particle-enhanced Raman scattering

    Science.gov (United States)

    Ranjan, Bikas; Huang, LiChuan; Masui, Kyoko; Saito, Yuika; Verma, Prabhat

    2014-08-01

    Modern farming relies highly on pesticides to protect agricultural food items from insects for high yield and better quality. Increasing use of pesticide has raised concern about its harmful effects on human health and hence it has become very important to detect even small amount of pesticide residues. Raman spectroscopy is a suitable nondestructive method for pesticide detection, however, it is not very effective for low concentration of pesticide molecules. Here, we report an approach based on plasmonic enhancement, namely, particle enhanced Raman spectroscopy (PERS), which is rapid, nondestructive and sensitive. In this technique, Raman signals are enhanced via the resonance excitation of localized plasmons in metallic nanoparticles. Gold nanostructures are promising materials that have ability to tune surface plasmon resonance frequency in visible to near-IR, which depends on shape and size of nanostructures. We synthesized gold nanorods (GNRs) with desired shape and size by seed mediated growth method, and successfully detected very tiny amount of pesticide present on food items. We also conformed that the detection of pesticide was not possible by usual Raman spectroscopy.

  6. 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

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

    International Nuclear Information System (INIS)

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

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

    Science.gov (United States)

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

    2013-05-01

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

  9. 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)

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

    OpenAIRE

    Syeda Azeem Unnisa

    2014-01-01

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

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

    OpenAIRE

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

    2007-01-01

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

  12. 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.

  13. Identification of residual pesticides in water by GC/QPMS.

    Science.gov (United States)

    Murata, T; Takahashi, S

    1991-10-01

    The extensive use of the broad range of pesticides employed to maintain golf courses has prompted serious environmental concerns in Japan since courses tend to be located in mountainous regions, often in close proximity to virgin water sources. Since older empirical methods are not appropriate for substance identification and determination of substance concentrations on the ppb order, gas chromatographyquadrupole mass spectrometry (GC/QPMS) can be employed. A simple extraction of 500 ml of drainage pond water gives a sample which allows identification of pesticides with quantitation on the ppb order using selected ion monitoring (SIM). A sample of drainage pond water from a golf course revealed fenitrothion, funitrothion, chlorothalonil and isoprothiolane in concentrations of 120.1, 20.7, 45.6 and 130.5 ppb, respectively. PMID:24233925

  14. Organochlorine pesticide residues in the northern Indian Ocean

    Digital Repository Service at National Institute of Oceanography (India)

    Shailaja, M.S.; Sarkar, A.

    1992-01-01

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

  15. A MULTI-RESIDUE METHOD FOR THE ANALYSIS OF INSECTICIDES COLLECTED ON COTTON SURFACE WIPES

    Science.gov (United States)

    A method was developed for the extraction, clean-up, and analysis of multiple pesticides from cotton wipe media used in human exposure studies to collect residues from residential hard surfaces. Measurements of pesticides are critical for estimating dermal and indirect ingestion ...

  16. 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

  17. Assessment of organochlorine pesticide residue levels in dairy milk and buffalo milk from Jaipur City, Rajasthan, India.

    Science.gov (United States)

    John, P J; Bakore, N; Bhatnagar, P

    2001-04-01

    The widespread application of pesticides in agriculture, public health, and industry and in and around the home can result in the accumulation of pesticides in the environment. Therefore, a survey has been conducted during 1993-1996 to investigate the magnitude of contamination of bovine milk with organochlorine pesticide (OCP) residues from Jaipur City, Rajasthan, India. Milk samples, i.e., dairy (toned and whole) and buffalo milk, were collected seasonally, and pesticide residues were assessed using a gas chromatograph (GC) with an electron capture detector (ECD). The results indicate that all the milk samples were contaminated with dichlorodiphenyltrichloroethane (DDT) and its metabolites (DDE and p,p'-dichlorodiphenyldichloroethane [DDD]), isomers of hexachlorocyclohexane (HCH; alpha, beta, and gamma), heptachlor and its epoxide, and aldrin. Seasonal variations of these pesticide residue levels were also observed in all the milk samples. Samples collected during winter season were found to contain higher residue levels as compared to other seasons. PMID:11341290

  18. 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.

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

    DEFF Research Database (Denmark)

    Poulsen, Mette E.; Wenneker, Marcel

    2012-01-01

    In this study, field trials on fine and coarse spray quality application of pesticides on apples were performed. The main objectives were to study the variation of pesticide residue levels in individual fruits versus composite samples, and the effect of standard fine spray quality application versus coarse spray quality application on residue levels. The applications included boscalid, bupirimate, captan, fenoxycarb, indoxacarb, pirimicarb, pyraclostrobin and thiophanate-methyl. Apples were collected from four zones in the tree and pesticide residues were detected in the individual apples. None of the results for the pesticides residues measured in individual apples exceeded the EU Maximum Residue Levels (MRLs). However, there was a large variation in the residues levels in the apples, with levels from 0.01 to 1.4 mg kg?1 for captan, the pesticide with the highest variation, and from 0.01 to 0.2 mg kg?1 for pyraclostrobin, the pesticide with the lowest variation. Residues of fenoxycarb and indoxacarb were only found in a few apples, probably due to the early application time of these two compounds. The evaluation of the effect of spray quality did not show any major difference between fine and coarse spray quality, except for carbendazim, the degradation product of thiophanate-methyl, where fine spray quality resulted in higher carbendazim residue levels than coarse spray quality. To examine the relationship between individual results and average results from ten apples, 20 composite samples were statistically constructed from sets of ten of the individual results. The variability factors for the individual samples (n = 80) at the 97.5 percentile were calculated for both standard and air induction nozzle application and were in the range of 0.9–9.4. The variability factor of seven used when EU member states calculate possible exceeding of Acute Reference Dose (ARfD) was adequate to encompass almost all the average results from the analyses of ten individual apples. However, for captan up to 9% of the results werenot covered depending on which of the mathematically constructed composite concentrations was chosen. The variability factor of three, recommend by Codex, seems to be too low, because up to 30% of the apple samples for captan were not covered if the worst case scenario was chosen. The factor of three seems was also too low for thiophanate-methyl.

  20. Evaluation of Pesticide Residues in Human Blood Samples of Agro Professionals and Non-Agro Professionals

    Directory of Open Access Journals (Sweden)

    Yawar Latif

    2012-08-01

    Full Text Available The aim of the present study was to evaluate the pesticide residues in human blood samples of volunteers related to Hyderabad and Mirpurkhas districts, Pakistan. The volunteers of both districts were divided into four groups on the basis of their exposure period to pesticides i.e. Group A-5 to 9 years, Group B-10 to 14 years, Group C-15 to19 years and Group D-above 20 years. Out of total 188 volunteers, 145 volunteers (77.1% were agro–professionals and 43 volun- teers (32.9% were non–agro professionals. Chlorpyrifos, endosulfan, 1, 1, 1-trichloro-2, 2-bis (p-chorophenyl ethane (p,p'-DDT and parathion residues were detected in many samples. The predominant pesticides found in blood samples of both district volunteers were chlorpyrifos (with highest mean concentration of 0.37 mg kg-1 in the D group of Mirpurkhas and endosulfan (with highest mean concentration of 0.30 mg kg-1 in the D group of Hyderabad. The quantity of pesticide residues detected in some blood samples of agro-professionals were found to be at the alarming level.

  1. 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

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

    Directory of Open Access Journals (Sweden)

    Botwe, B. O.

    2011-08-01

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

  3. 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.

  4. 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)

  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 (-0.73soil surface influenced the mobility of pesticides as it was observed in decomposing mulch of crop residues (Aslam et al., 2013). As a result, the type of cover crop and the changes of cover crop residues composition during decomposition in field may control differently the movement of non-ionic pesticides compared to ionic compounds such as glyphosate, largely used in conservation agriculture practices. Keywords : Cover crops ; Glyphosate ; S-metolachlor ; Epoxiconazole ; Mulch; Sorption ; Biochemical composition References Alletto L., Benoit P., Justes E., Coquet Y. 2012. Effects of tillage and fallow period management on the fate of the herbicide isoxaflutole in an irrigated continuous-maize field. Agriculture, Ecosystems Environment, 153, 40- 49. http://dx.doi:10.1016/j.agee.2012.03.002 Alletto L., Benoit P., Coufignal M., Bergheaud V., 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. 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)

  7. 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

  8. Awareness of pesticide residues in locally available food and condiments among food sellers: a case study of Osun state, Nigeria

    OpenAIRE

    Samson Ayo Deji

    2012-01-01

    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 s...

  9. 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)

  10. 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.

  11. 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.

  12. 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 [...] 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%.

  13. [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

  14. 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.

  15. 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...

  16. [Determination of 16 pesticide residues in fruits and vegetables by QuEChERS-liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Wu, Yan; Jiang, Bing; Xu, Yigang; Zhao, Wei; Meng, Xiangrui; Zhou, Yuan; Yu, Jiahui; Zu, Yuangang

    2015-03-01

    A sensitive and convenient liquid chromatography-tandem mass spectrometric method was developed for the determination of 16 pesticides such as imidacloprid, prochloraz, difenoconazole, azoxystrobin, and thiamethoxam in fruits and vegetables. After compared with methanol and acetone-cyclohexane (1:2, v/v), acetonitrile was chosen as the extraction solvent. The samples were extracted by acetonitrile in high-speed homogenization. The extraction solution was cleaned up by liquid-liquid extraction, and the supernatant was collected. In this work, QuEChERS exhibited much higher efficiency than Carbon-NH2 solid-phase extraction in purification. The pigments and organic acids were removed by purge line (150 mg primary secondary amine (PSA) sorbent and 900 mg absolute magnesium sulfate), leading to the decrease of the background interferences. The average recoveries of the 16 pesticides were almost in the range of 75%-111% at the three spiked levels, and the relative standard deviations were less than 16%. The qualitative analysis and quantitative analysis were investigated by LC-MS/MS and matrix-matched calibration curves. The results showed that the method of QuEChERS combined with LC-MS/MS is rapid, accurate and sensitive for the determination of the 16 pesticide residues in fruits and vegetables. PMID:26182463

  17. Stricter regulation boosts exports: the case of Maximum Residue Levels in pesticides

    OpenAIRE

    Foletti, Liliana; Shingal, Anirudh

    2014-01-01

    Constructing an original panel on Maximum Residue Levels (MRLs) in pesticides for 50 countries over 2006-2012, this paper studies the effect of heterogeneity in MRL regulation on bilateral trade. We find evidence of regulatory heterogeneity diminishing trade at the extensive margin when the exporter faces more stringent regulation abroad, suggesting compliance costs in entering the destination market. Significantly, however, we also find strong evidence of regulatory heterogeneity increasing ...

  18. Assessment of Pesticide Residues in Honey Samples from Portugal and Spain

    OpenAIRE

    Blasco, Cristina; Fernández, Mónica; Pena, Angelina; Lino, Celeste; Silveira, Mª Irene; Font, Guillermina; Picó, Yolanda

    2003-01-01

    Fifty samples of honey collected from local markets of Portugal and Spain during year 2002 were analyzed for 42 organochlorine, carbamate, and organophosphorus pesticide residues. An analytical procedure based on solid-phase extraction with octadecyl sorbent followed by gas chromatography?mass spectrometry (GC?MS), for organochlorines, and by liquid chromatography?atmospheric pressure chemical ionization-mass spectrometry (LC?APCI-MS), for organophosphorus and carbamates, has been dev...

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

    International Nuclear Information System (INIS)

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

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

    Science.gov (United States)

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

    2007-06-01

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

  1. Organochlorine pesticide residues in human milk of mothers living in northern Tunisia.

    Science.gov (United States)

    Ennaceur, S; Gandoura, N; Driss, M R

    2007-05-01

    The levels of 13 organochlorine pesticides (OCPs) were measured in breast milk from 87 Tunisian mothers throughout their lactation periods. Breast milk levels of OCP residues were determined using a validated methodology that included capillary column gas chromatography with electron-capture detection. All samples contained detectable residues of p,p'-DDE (2.421 mg/kg milk fat) and HCB (0.260 mg/kg milk fat). The other OCP residues were detected in the following order of frequency: Dieldrin 38%, beta-HCH 22.9% and gamma-HCH 6.8%. It was made an attempt to point out the relationship between some factors and the transfer of OCP residues into breast milk. In this study we found that concentrations of OCPs increased with mothers' age, these levels decreased with the number of children. PMID:17619799

  2. Residues of organochlorine pesticides and polycyclic aromatic hydrocarbons in drinking water of Ahmedabad City, India

    Energy Technology Data Exchange (ETDEWEB)

    Jani, J.P.; Mistry, J.S. (Univ. of Pittsburgh, PA (United States)); Raiyani, C.V.; Patel, J.S.; Desai, N.M.; Kashyap, S.K. (National Inst. of Occupational Health, Ahmedabad (India))

    1991-09-01

    The ubiquitous environmental pollutants organochlorine pesticides (OCP) and polycyclic aromatic hydrocarbons (PAH) have been extensively studied for their toxicity. Monitoring of OCP and PAH residues has always been considered important for controlling human exposure. As compared to several other countries, the higher body burden of OCP in Indian general population is indicative of higher exposure to these chemicals. Recent studies have shown higher residues of OCP in food commodities including human mother's milk. The levels of OCP in drinking water is still a matter of concern and practically nothing is known about the residues of PAH in drinking water in India. This is the first report of its kind regarding the residues of OCP and PAH in drinking water of Ahmedabad City, the sixth largest city of India with a population of more than 2.5 million.

  3. Rapid determination of pesticide residues in Chinese materia medica using QuEChERS sample preparation followed by gas chromatography–mass spectrometry

    Directory of Open Access Journals (Sweden)

    Yichen Hu

    2012-06-01

    Full Text Available Pesticide residue analysis plays an important role in the quality control of Chinese materia medica. This paper reports the development and validation of an analytical method for the quantitative determination of the residues of 39 pesticides in 12 different matrices of Chinese materia medica. Sample preparation utilized the QuEChERS method with acetonitrile:1% aqueous acetic acid (9:1, v/v as extraction solvent followed by sample clean-up by dispersive solid phase extraction using primary secondary amine sorbent and graphitized carbon black. Extracts were then analysed by gas chromatography coupled with electron impact mass spectrometry in the selected ion monitoring mode. Limit of detection (LOD and limit of quantitation (LOQ values were in the ranges 0.5–50 ng/g and 1–100 ng/g, respectively. The recoveries of the 39 pesticides were in the range 75–112% with precision (as relative standard deviation, RSD <15%. The results show that the modified QuEChERS method allows rapid and sensitive analysis of multiple pesticide residues in Chinese materia medica.

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

    Science.gov (United States)

    Amaraneni, S R; Pillala, R R

    2001-01-01

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

  5. Preparation of activated carbons from agricultural residues for pesticide adsorption.

    Science.gov (United States)

    Ioannidou, Ourania A; Zabaniotou, Anastasia A; Stavropoulos, George G; Islam, Md Azharul; Albanis, Triantafyllos A

    2010-09-01

    Activated carbons (ACs) can be used not only for liquid but also for vapour phase applications, such as water treatment, deodorisation, gas purification and air treatment. In the present study, activated carbons produced from agricultural residues (olive kernel, corn cobs, rapeseed stalks and soya stalks) via physical steam activation were tested for the removal of Bromopropylate (BP) from water. For the characterization of the activated carbons ICP, SEM, FTIR and XRD analyses were performed. Adsorption kinetics and equilibrium isotherms were investigated for all biomass activated carbons in aqueous solutions. Experimental data of BP adsorption have fitted best to the pseudo 2nd-order kinetic model and Langmuir isotherm. The study resulted that corn cobs showed better adsorption capacity than the other biomass ACs. Comparison among ACs from biomass and commercial ones (F400 and Norit GL50) revealed that the first can be equally effective for the removal of BP from water with the latter. PMID:20598734

  6. 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.

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

    International Nuclear Information System (INIS)

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

  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

    Scientific Electronic Library Online (English)

    Isabel Cristina Sales Fontes, Jardim; Juliano de Almeida, Andrade; Sonia Claudia do Nascimento de, Queiroz.

    Full Text Available [...] Abstract in english 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 toxic [...] ity 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. De-contamination of pesticide residues in food by ionizing radiation

    Science.gov (United States)

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

    2012-04-01

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

  11. 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.

  12. 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

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

    DEFF Research Database (Denmark)

    Bache, Michael; Taboryski, Rafael Jozef

    2011-01-01

    The attachment of an antibody to an antigen-coated cantilever has been investigated by repeated experiments, using a cantilever-based detection system by Cantion A/S. The stress induced by the binding of a pesticide residue BAM (2,6 dichlorobenzamide) immobilized on a cantilever surface to anti-BAM antibody is measured using the CantiLab4© system from Cantion A/S with four gold-coated cantilevers and piezo resistive readout. The detection mechanism is in principle label-free, but fluorescent-marked antibodies have been used to subsequently verify the binding on the cantilever surface. The bending and increase in mass of each cantilever has also been investigated using a light interferometer and a Doppler Vibrometer. The system has been analyzed during repeated measurements to investigate whether the CantiLab4© system is a suited platform for a pesticide assay system. © 2011 Bache et al.

  14. On-column partition cleanup of fatty extracts for organophosphate pesticide residue determination.

    Science.gov (United States)

    Di Muccio, A; Cicero, A M; Camoni, I; Pontecorvo, D; Dommarco, R

    1987-01-01

    A fast, single-step, and efficient partition between n-hexane and acetonitrile on ready-to-use, disposable mini-columns of Kieselghur-type material has been developed for the cleanup of fatty extracts for organophosphate (OP) pesticide residue determination by gas chromatography with flame photometric detection. Nine OP pesticides (diazinon, etrimfos, chlorpyrifos-methyl, pyrimiphos-methyl, chlorpyrifos, bromophos, bromophos-ethyl, malathion, fenitrothion) most commonly used for protection of stored cereals, oil seeds, and legumes were separated from up to 2.0 g lipidic material with recoveries between 80 and 107% at spiking levels ranging for the different compounds from 0.1 to 5.0 ppm. PMID:3558258

  15. 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...

  16. 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.

  17. 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

  18. 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...

  19. 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

  20. 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)

  1. 40 CFR 158.2171 - Experimental use permit microbial pesticides product analysis data requirements table.

    Science.gov (United States)

    2010-07-01

    40 Protection of Environment 23 2010-07-01...Experimental use permit microbial pesticides product analysis data...2171 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA...

  2. 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

  3. 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 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.

  4. 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.

  5. 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

  6. UNE-EN ISO/IEC 17025:2005-accredited method for the determination of pesticide residues in fruit and vegetable samples by LC-MS/MS.

    Science.gov (United States)

    Camino-Sánchez, F J; Zafra-Gómez, A; Oliver-Rodríguez, B; Ballesteros, O; Navalón, A; Crovetto, G; Vílchez, J L

    2010-11-01

    A rapid, simple and sensitive multi-residue method was developed and validated for the simultaneous quantification and confirmation of 69 pesticides in fruit and vegetables using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted following the quick, easy, cheap, effective, rugged and safe method known as QuEChERS. Mass spectrometric conditions were individually optimised for each analyte in order to achieve maximum sensitivity in multiple reaction monitoring (MRM) mode. Using the developed chromatographic conditions, 69 pesticides can be separated in less than 17 min. Two selected reaction monitoring (SRM) assays were used for each pesticide to obtain simultaneous quantification and identification in one run. With this method in SRM mode, more than 150 pesticides can be analysed and quantified, but their confirmation is not possible in all cases according to the European regulations on pesticide residues. Nine common representative matrices (zucchini, melon, cucumber, watermelon, tomato, garlic, eggplant, lettuce and pepper) were selected to investigate the effect of different matrices on recovery and precision. Mean recoveries ranged from 70% to 120%, with relative standard deviations (RSDs) lower than 20% for all the pesticides. The proposed method was applied to the analysis of more than 2000 vegetable samples from the extensive greenhouse cultivation in the province of Almeria, Spain, during one year. The methodology combines the advantages of both QuEChERS and LC-MS/MS producing a very rapid, sensitive, accurate and reliable procedure that can be applied in routine analytical laboratories. The method was validated and accredited according to UNE-EN-ISO/IEC 17025:2005 international standard (accreditation number 278/LE1027). PMID:20730643

  7. 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

  8. Occurrence and distribution study of residues from pesticides applied under controlled conditions in the field during rice processing.

    Science.gov (United States)

    Pareja, Lucía; Colazzo, Marcos; Pérez-Parada, Andrés; Besil, Natalia; Heinzen, Horacio; Böcking, Bernardo; Cesio, Verónica; Fernández-Alba, Amadeo R

    2012-05-01

    The results of an experiment to study the occurrence and distribution of pesticide residues during rice cropping and processing are reported. Four herbicides, nine fungicides, and two insecticides (azoxystrobin, byspiribac-sodium, carbendazim, clomazone, difenoconazole, epoxiconazole, isoprothiolane, kresoxim-methyl, propanil, quinclorac, tebuconazole, thiamethoxam, tricyclazole, trifloxystrobin, ?-cyhalotrin) were applied to an isolated rice-crop plot under controlled conditions, during the 2009-2010 cropping season in Uruguay. Paddy rice was harvested and industrially processed to brown rice, white rice, and rice bran, which were analyzed for pesticide residues using the original QuEChERS methodology and its citrate variation by LC-MS/MS and GC-MS. The distribution of pesticide residues was uneven among the different matrices. Ten different pesticide residues were found in paddy rice, seven in brown rice, and eight in rice bran. The highest concentrations were detected in paddy rice. These results provide information regarding the fate of pesticides in the rice food chain and its safety for consumers. PMID:22497619

  9. Screening of pesticide residues in soil and water samples from agricultural settings

    Directory of Open Access Journals (Sweden)

    Djouaka Rousseau F

    2006-03-01

    Full Text Available Abstract Background The role of agricultural practices in the selection of insecticide resistance in malaria vectors has so far been hypothesized without clear evidence. Many mosquito species, Anopheles gambiae in particular, lay their eggs in breeding sites located around agricultural settings. There is a probability that, as a result of farming activities, insecticide residues may be found in soil and water, where they exercise a selection pressure on the larval stage of various populations of mosquitoes. To confirm this hypothesis, a study was conducted in the Republic of Benin to assess the environmental hazards which can be generated from massive use of pesticides in agricultural settings. Methods Lacking an HPLC machine for direct quantification of insecticide residues in samples, this investigation was performed using indirect bioassays focussed on the study of factors inhibiting the normal growth of mosquito larvae in breeding sites. The speed of development was monitored as well as the yield of rearing An. gambiae larvae in breeding sites reconstituted with water and soil samples collected in agricultural areas known to be under pesticide pressure. Two strains of An. gambiae were used in this indirect bioassay: the pyrethroid-susceptible Kisumu strain and the resistant Ladji strain. The key approach in this methodology is based on comparison of the growth of larvae in test and in control breeding sites, the test samples having been collected from two vegetable farms. Results Results obtained clearly show the presence of inhibiting factors on test samples. A normal growth of larvae was observed in control samples. In breeding sites simulated by using a few grams of soil samples from the two vegetable farms under constant insecticide treatments (test samples, a poor hatching rate of Anopheles eggs coupled with a retarded growth of larvae and a low yield of adult mosquitoes from hatched eggs, was noticed. Conclusion Toxic factors inhibiting the hatching of anopheles eggs and the growth of larvae are probably pesticide residues from agricultural practices. Samples used during this indirect assay have been stored in the laboratory and will be analysed with HPLC techniques to confirm hypothesis of this study and to identify the various end products found in soil and water samples from agricultural settings under pesticide pressure.

  10. Organochlorine pesticide residues in human milk of a Hmong hill tribe living in Northern Thailand.

    Science.gov (United States)

    Stuetz, W; Prapamontol, T; Erhardt, J G; Classen, H G

    2001-06-12

    In December 1998 whole breast milk samples from 25 Hmong mothers living in the village of Mae Sa Mai, 40 km north of Chiang Mai City, Northern Thailand, were collected and analysed for DDT, heptachlor, HCB and HCH residues (fat normalized data). Short questionnaires and anthropometric measurements were used to obtain information on personal characteristics, lifestyle, contact with pesticides, dietary habits and former residences. DDT was detected in all samples with a median and maximum level of 209 and 2012 ng of total DDT isomers per millilitre of milk, respectively. The median and highest percentages of p,p'-DDT were 23.2 and 44.7%. In 15 samples heptachlor was detected in the metabolized form of heptachlor-epoxide with a median value of 4.4 ng/ml. The estimated daily intakes of DDT, heptachlor and heptachlor-epoxide by the infants exceeded up to 20 times the acceptable daily intakes as recommended by the FAO and WHO. In nine samples HCB was detected with a median value of 5.4 ng/ml from which seven of the nine also had the highest values of DDT residues. The gamma-isomer of HCH was only found in one sample with 3.6 ng/ml. The mean sum-DDT residues with 14.96 mg/kg milk fat, as well as the estimated daily intakes by the infants are one of the highest reported in the 1990s. The fact that the mother breast-feeds her first child and that she originally comes from a region where DDT is still in use as a vector control agent, as well as the former use of organochlorine pesticides (OCPs) in agriculture, seem to be the main factors for high DDT and other OCP residues in the mothers' milk. PMID:11419602

  11. 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.

  12. 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

  13. Determination of pesticide residues in soil by modified matrix solid-phase dispersion and gas chromatography.

    Science.gov (United States)

    Shen, Xia; Su, Qingde; Zhu, Xiaolan; Gao, Yun

    2007-08-01

    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). PMID:17899878

  14. EXTENSION OF MULTI-RESIDUE METHODOLOGY. I. DETERMINING MULTICLASS PESTICIDE RESIDUES IN SOIL BY GAS CHROMATOGRAPHY. II. DYNAMIC FLUOROGENIC LABELLING DETECTOR FOR CARBAMATES

    Science.gov (United States)

    A multi-residue procedure was devised for the extraction, cleanup and determination of forty seven pesticides in fortified soil samples. Most of the compounds were determined by gas chromatography interfaced with either the electron capture or the flame photometric detector. Seve...

  15. A multi-residue method for the determination of 90 pesticides in matrices with a high water content by LC-MS/MS without clean-up.

    Science.gov (United States)

    Madureira, Fernando Diniz; da Silva Oliveira, Fabiano Aurélio; de Souza, Wesley Robert; Pontelo, Ana Paula; de Oliveira, Mauro Lúcio Gonçalves; Silva, Gilsara

    2012-01-01

    A method using QuEChERS extraction and LC-MS/MS in electrospray positive ionisation mode was developed and validated for the analysis of 90 pesticides in a high water content matrix (tomato) in a single chromatographic run. To assess the intra-laboratory reproducibility of the method, validation was conducted on four different days by two different analysts. The validation data was treated using a spreadsheet developed in-house, which sets the most appropriate model for linear fit by determining whether the residuals of the calibration curves are homocedastic or heterocedastic. A statistical test for the significance of regression was also carried out. Calibration was always matrix-matched and the curves were obtained over the range 0.0075-0.10 or 0.020-0.125 mg kg(-1). Identification of analytes was based on retention times and MRM ratios. Recoveries were assessed at four different levels for each analyte and were between 73 and 106%, with relative standard deviations under reproducibility conditions of pesticide analysed were below 50%. Previous validation of the same method, applied to papaya samples and satisfactory results obtained in various proficiency tests with different high water content matrices, demonstrated the applicability of the method to these classes of commodities, without clean-up. The validated method will be applied routinely in the pesticide residues monitoring programme that constitutes the National Residue and Contaminant Control Plan of Brazil. PMID:22059454

  16. 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 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

  17. 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...

  18. Multiresidue analysis of pesticides in olive oil by gel permeation chromatography followed by gas chromatography-tandem mass-spectrometric determination

    International Nuclear Information System (INIS)

    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 ?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

  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

    ...Spinetoram; Human-Health Assessment Scoping...Spinetoram; Human-Health Assessment Scoping...to their initial pesticide petition 2F8139...proposing tolerances for fish-freshwater finfish...more than 15% of a pesticide formulation, as...on the physical chemical...

  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

    ...a pesticide petition (PP 0E7754) by Quimica Agronomica de Mexico, S. de R.L...Gowan Company (U.S. agent on behalf of Quimica Agronomica de Mexico) notified EPA that...of pesticide petition (PP 0E7755) by Quimica Agronomica de Mexico, S. de...

  1. 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.

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

    Science.gov (United States)

    Mol, Hans G J; van Dam, Ruud C J

    2014-11-01

    Flow injection combined with tandem mass spectrometry (MS/MS) was investigated for the rapid detection of highly polar pesticides that are not amenable to multi-residue methods because they do not partition into organic solvents and require dedicated chromatographic conditions. The pesticides included in this study were amitrole, chlormequat, cyromazine, daminozide, diquat, ethephon, fosetyl-Al, glufosinate, glyphosate and its metabolite aminomethylphosphonic acid, maleic hydrazide, mepiquat and paraquat. The composition of the flow-injection solvent was optimized to achieve maximum MS/MS sensitivity. Instrumental limits of detection varied between <0.05 and 1 pg. Fruit, vegetable, cereal, milk and kidney samples were extracted with water (1% formic acid in case of paraquat/diquat) and ten times diluted in either methanol/0.1% formic acid, methanol/0.1% ammonia or acetonitrile/0.1% ammonia, depending on the pesticide. The ion suppression observed depended strongly on both the matrix and the pesticide. This could be largely compensated for by matrix-matched calibration, but more accurate quantification was obtained by using isotopically labelled standards (commercially available for most of the pesticides studied). The method detection limits ranged from 0.02 mg/kg for chlormequat and mepiquat to 2 mg/kg for maleic hydrazide and were 0.05-0.2 mg/kg for most other pesticide/matrix combinations. This was sufficiently low to test compliance with EU maximum residue limits for many relevant pesticide/commodity combinations. The method substantially reduces the liquid chromatography-MS/MS capacity demand which for many laboratories is prohibitive for inclusion of these pesticides in their monitoring and surveillance programmes. PMID:24518902

  3. Determination of 23 pesticide residues in leafy vegetables using gas chromatography-ion trap mass spectrometry and analyte protectants.

    Science.gov (United States)

    González-Rodríguez, Rosa Ma; Rial-Otero, Raquel; Cancho-Grande, Beatriz; Simal-Gándara, Jesús

    2008-07-01

    A gas chromatographic method was developed for simultaneously determining residues of 12 insecticides (acrinathrin, bifenthrin, carbofuran, cyfluthrin, lambda-cyhalothrin, cypermethrin, chlorfenvinphos, deltamethrin, esfenvalerate, fenamiphos, methiocarb and tau-fluvalinate) and 11 fungicides (cyprodinil, fludioxonil, iprodione, metalaxyl, penconazole, pyrimethanil, procymidone tebuconazole, triadimefon, triadimenol and vinclozolin) in leafy vegetables. Samples were extracted with acetonitrile and cleaned-up with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. The eluate was finally evaporated and redissolved with 0.5 mL of acetone containing the internal standards (pentachlorobenzene and fenpropathrin) and three analyte protectants (3-ethoxy-1,2-propanediol, d-sorbitol and l-gulonic acid gamma-lactone). The addition of analyte protectants allows to avoid the matrix-induced response enhancement effect on quantitation process with absolute recoveries ca. 100%. Precision (expressed as relative standard deviation) was lower than 10% for all pesticides and finally, limits of detection were also 10-20 times lower than maxima residue levels (MRLs) established by European Regulation. The proposed method was applied to determine pesticide residues in commercial leafy vegetables (lettuce, Swiss chard and spinach) purchased from markets in Orense (NW Spain). Pesticide residues were detected in 84% of the total samples (63 from 75 samples) and pesticide concentrations were higher than MRL in 18 samples. PMID:18343389

  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. Multi-residue analysis of 30 currently used pesticides in fine airborne particulate matter (PM 2.5) by microwave-assisted extraction and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Coscollà, Clara; Yusà, Vicent; Beser, Ma Isabel; Pastor, Agustin

    2009-12-18

    A confirmatory and rapid procedure has been developed for the determination of 30 currently used pesticides (CUP) in fine airborne particulate matter (PM 2.5) at trace level. The proposed method includes extraction of PM 2.5-bound pesticides by microwave-assisted extraction (MAE) followed by a direct injection into LC-MS/MS. The main parameters affecting the MAE extraction (time, temperature and volume of solvent) were optimised using statistical design of experiments (DoE). The matrix effect was also evaluated. Recoveries ranged from 72 to 109% and the limit of quantification (LoQ) was 32.5 pg m(-3) for chlorpyrifos, 13.5 pg m(-3) for fenhexamid, imazalil and prochloraz, and 6.5 pg m(-3) for the rest of pesticides, when air volumes of 760 m(3) were collected. The method was applied to 54 samples collected from three stations of the atmospheric monitoring network of the Regional Valencia Government (Spain) during April-July 2009. Nineteen out of 30 pesticides investigated were found in at least one sample: omethoate, carbendazim, acetamiprid, thiabendazole, malathion, flusilazole, metalaxyl, azoxystrobin, iprovalicarb, myclobutanil, tebuconazole, triflumizole, cyprodinil, tebufenpyrad, buprofezin, pyriproxyfen, hexythiazox, flufenoxuron and fenazaquin. The measured concentrations ranged from 6.5 to 1208 pg m(-3). To our knowledge, 11 of the pesticides detected have been reported for the first time in ambient air. PMID:19913234

  6. Selective, on-column extraction of organochlorine pesticide residues from milk.

    Science.gov (United States)

    Di Muccio, A; Rizzica, M; Ausili, A; Camoni, I; Dommarco, R; Vergori, F

    1988-12-01

    A rapid procedure has been developed that allows a single-step, selective extraction of organochlorine pesticide (OCP) residues from milk on solid-matrix disposable columns by means of acetonitrile-saturated light petroleum. Recovery experiments were carried out on homogenized milk (3.6% fat content) spiked with an ethanolic solution of nine OCPs, viz., HCB, alpha-HCH, beta-HCH, gamma-HCH, heptachlor epoxide, dieldrin, endrin, p,p'-DDE and p,p'-DDT, at levels ranging from 0.002 mg/kg for alpha-HCH to 0.008 mg/kg for p,p'-DDT. Average recoveries of four replicates were 77% for HCB and almost quantitative (94-113%) for the other pesticides, with relative standard deviations from 2.9 to 7.3%. Coextracted fatty material amounted to about 5 mg/ml of milk before the clean-up. The described procedure also showed a satisfactory performance with milk powder. The extraction procedure requires about 60 min. The main advantages are that 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:3243863

  7. Magnetic "one-step" quick, easy, cheap, effective, rugged and safe method for the fast determination of pesticide residues in freshly squeezed juice.

    Science.gov (United States)

    Zheng, Hao-Bo; Ding, Jun; Zheng, Shu-Jian; Yu, Qiong-Wei; Yuan, Bi-Feng; Feng, Yu-Qi

    2015-06-12

    A "one-step" quick, easy, cheap, effective, rugged and safe (QuEChERS) method was proposed for pesticide residue analysis in freshly squeezed juice of fruits and vegetables. In this method, a new magnetic adsorbent prepared by simple physical blending was adopt, which could endow the sample mixture with magnetic separability. To achieve the best performance of the modified QuEChERS towards target analytes, the amounts of adsorbents were investigated. Under the optimized conditions, a simple, rapid and sensitive method for the determination of 11 pesticide residues in freshly squeezed juice was established by coupling modified QuEChERS to gas chromatography/mass spectrometry analysis. The limits of quantification of the proposed method for 11 pesticides ranged from 2.0 to 49.6ng/g. Good linearities (R value ?0.9993) were achieved at different concentration ranges, and acceptable method reproducibility was obtained by evaluating intra- and inter-day precisions with the relative standard deviations being less than 8.5% and 13.5%, respectively. The recoveries were in the range of 70.3-114.1% at different concentrations for real samples. Compared with the traditional QuEChERS methods, extraction/partitioning and purification were integrated into one step in the proposed method, which thus was time-saving (within 3.5min) with keeping good clean-up performance. PMID:25935797

  8. 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

  9. 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.

  10. 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

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

    OpenAIRE

    Terence Centner; Nicholas Eberhart

    2014-01-01

    Agricultural producers and public health authorities apply pesticides to control pests that damage crops and carry diseases. Due to the toxic nature of most pesticides, they are regulated by governments. Regulatory provisions require pesticides to be registered and restrictions operate to safeguard human health and the environment. Yet pesticides used near surface waters pose dangers to non-target species and drinking water supplies leading some governments to regulate discharges of pesticid...

  12. 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.

  13. 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.

  14. Design of a compressed air modulator to be used in comprehensive multidimensional gas chromatography and its application in the determination of pesticide residues in grapes.

    Science.gov (United States)

    Pizzutti, Ionara R; Vreuls, René J J; de Kok, André; Roehrs, Rafael; Martel, Samile; Friggi, Caroline A; Zanella, Renato

    2009-04-10

    In this study, a new modulator that is simple, robust and presents low operation costs, was developed. This modulator uses compressed air to cool two small portions in the first centimeters of the second chromatographic column of a comprehensive multidimensional gas chromatography (GCxGC) system. The results show a variation in the peak area less than 3 and 5% to alkanes and pesticides, respectively. The standard deviations for the retention times in the first and second dimension are around 0.05 min and 0.05s for all the compounds. The system was optimized with n-alkanes. The GCxGC system proposed was applied in the determination of pyrethroid pesticides (bifenthrin, cypermethrin, deltamethrin, fenvalerate, esfenvalerate, cis- and trans-permethrin) in grape samples. Samples were extracted by the mini-Luke modified method and pesticides were quantified by comprehensive multidimensional gas chromatography with micro electron-capture detection (microECD). The values of method limit of quantification (LOQ) were 0.01-0.02 mg kg(-1) for all studied pyrethroid and the values of recovery were between 94.3 and 115.2%, with good precision (RSDair has the potential for application in the analysis of a wider range of pesticide residues in other commodities since it provides low values of LOQ with acceptable accuracy and precision. PMID:19233371

  15. 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.

    2011-10-01

    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.

  16. 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...

  17. Enhanced pesticide sensitivity of novel housefly acetylcholinesterases: a new tool for the detection of residual pesticide contamination.

    Science.gov (United States)

    Tan, Furong; Wang, Ligang; Wang, Jinbin; Wu, Xiao; Zhu, Hong; Jiang, Lingxi; Tao, Shiru; Zhao, Kai; Yang, Yan; Tang, Xueming

    2011-03-01

    The full-length cDNA encoding an acetylcholinesterase (AChE) was cloned and sequenced from the housefly, Musca domestica, by reverse transcriptase-polymerase chain reaction (RT-PCR). Sequence analysis revealed that this 2,076 bp sequence encodes a mature protein of 612 amino acids (67 kDa) and a 79 residue signal peptide. The amino acid sequence shared 52.8-81.4% identity with the AChE proteins of other insects. The cDNA sequence, which lacked the signal peptide was inserted into the vector pPIC9K and then introduced into strain GS115 of the yeast Pichia pastoris. The recombinant AChE protein was then expressed in P. pastoris strain GS115 by methanol induction. Site-directed mutagenesis of the A262G, Y327F, Y327D and I374D residues, either singly or in combination, was performed by reverse PCR. These mutants improved the catalytic activity and sensitivity to the organophosphate and carbamate insecticides. Although the sensitivity of other mutants was slightly increased, the results still showed that the sensitivity of triple mutant, GDD (A262G/Y327D/I374D), enhanced remarkably as much as 16 times for methomyl, 14 times for both carbofuran and chlorpyrifos, and ten times for parathion-methyl, compared to that of the wild-type. The results strongly suggested that these residues are the key structural elements controlling AChE enzyme catalytic activity and sensitivity to inhibition by insecticides. The AChE enzyme obtained by this method could be used to detect the organophosphate and carbamate insecticide residues in fruits and vegetables, a characteristic of great potential research and industrial application. PMID:20963445

  18. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce.

    Science.gov (United States)

    Anastassiades, Michelangelo; Lehotay, Steven J; Stajnbaher, Darinka; Schenck, Frank J

    2003-01-01

    A simple, fast, and inexpensive method for the determination of pesticide residues in fruits and vegetables is introduced. The procedure involves initial single-phase extraction of 10 g sample with 10 mL acetonitrile, followed by liquid-liquid partitioning formed by addition of 4 g anhydrous MgSO4 plus 1 g NaCl. Removal of residual water and cleanup are performed simultaneously by using a rapid procedure called dispersive solid-phase extraction (dispersive-SPE), in which 150 mg anhydrous MgSO4 and 25 mg primary secondary amine (PSA) sorbent are simply mixed with 1 mL acetonitrile extract. The dispersive-SPE with PSA effectively removes many polar matrix components, such as organic acids, certain polar pigments, and sugars, to some extent from the food extracts. Gas chromatography/mass spectrometry (GC/MS) is then used for quantitative and confirmatory analysis of GC-amenable pesticides. Recoveries between 85 and 101% (mostly > 95%) and repeatabilities typically pesticides, including very polar and basic compounds such as methamidophos, acephate, omethoate, imazalil, and thiabendazole. Using this method, a single chemist can prepare a batch of 6 previously chopped samples in < 30 min with approximately 1 dollar (U.S.) of materials per sample. PMID:12723926

  19. 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.

  20. 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)

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

    Science.gov (United States)

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

    2014-06-01

    The development and application of an analytical methodology for the pretreatment and determination of 253 multiclass pesticides, in lake sediment samples, using liquid chromatography coupled with mass spectrometry (LC-MS/MS) are described in this work. Sediments of lakes Volvi, Doirani, and Kerkini, located in northern Greece, were collected in two-time periods (fall/winter 2010 and spring/summer 2011) and analyzed, applying the developed analytical methodology. Microwave-assisted extraction (MAE) was applied to extract the pesticide residues from lake sediment samples. Analytical results were stored, categorized, and visualized using geographical information systems, in order to assess and observe spatial and temporal variations of the pollution. Main pesticides that were detected included the following: amitrole, tebuconazole, phoxim, diniconazole, sethoxydim, temephos, tetrachlorvinphos, pendimethalin, boscalid, disulfoton sulfone, lenacil, propiconazole, cycloxydim, pyridaben, and terbuthylazine. Amitrole, diniconazole, and tebuconazole were found to be common in all three lakes. Lakes Kerkini and Doirani exhibited increased concentrations during the first sampling period (winter 2010) with predominant pesticide classes, triazines/triazoles and organophosphates. Pollution is mainly located near the populated villages of the lakes and the nearby cultivations. During the second sampling period, pesticide concentrations appear lower and located in sediments near the center of the lake. Lake Volvi exhibits increased pesticide concentrations during the second sampling period, temporal and spatial variations and different pesticide profile pattern. Increased pollution occurs near the center of the lake during the first sampling period, mainly comprised by triazines/triazoles and organophosphates. During the second sampling period, the majority of the sediment samples demonstrated a different pesticide profile dominated by unclassified pesticides and triazines/triazoles. Mineralogical analysis of the samples demonstrates that sediments are mainly composed of clay, mud, and sand particles, and they present spatial variations. Near the center of the lakes, sediments appear to be more fine-grained with higher clay content and are more likely to adsorb pesticides. PMID:24691934

  2. 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)

  3. 40 CFR 158.2040 - Biochemical pesticides residue data requirements table.

    Science.gov (United States)

    2010-07-01

    ... 860.1400 Fish NR CR NR...for biochemical pesticides product chemistry...to biochemical pesticide products...biochemical human health assessment data... 2. The same chemical identity data...uses where the pesticide is applied... 13. Data on fish are...

  4. 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

  5. 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.

  6. [Determination of 18 pesticide residues in red wine by ultra high performance liquid chromatography-high resolution mass spectrometry with isotope dilution technique].

    Science.gov (United States)

    Chen, Dawei; Lü, Bing; Ding, Hao; Zou, Jianhong; Yang, Xin; Zhao, Yunfeng; Miao, Hong

    2014-05-01

    A method for the simultaneous determination of 18 pesticide residues in red wine was developed using ultra high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS) with isotope dilution technique. The red wine samples were extracted with acetonitrile, and the extracts were cleaned up with dispersive solid phase extraction (dSPE) using the mixture of N-propyl ethylene diamine (PSA) and C18 powder as sorbent. The extracted components were separated on a BEH C18 column by gradient elution. The qualitative and quantitative analyses were operated under full scan/data dependent MS/MS (ddms2) and targeted selective ion monitoring (tSIM) by high resolution mass spectrometry, respectively. Carbendazim-D4, chlorpyrifos-D10, imidacloprid-D4, methoxyfenozide-D9, pyrimethanil-D5 and tebuconazole-D6 were used as the internal standards to reduce the matrix effects. The response of each pesticide showed a good linearity in the range of 0.5-50 microg/kg with the correlation coefficient more than 0.999. The limits of detection and quantification for the 18 pesticides in the spiked blank red wine were 0.5 microg/kg and 1.0 microg/kg, respectively. The recovery results with spiked blank red wine samples at the levels of 1 to 40 microg/kg were satisfactory with average recoveries of 85.4% - 117.9% and the RSDs of 0.5%-6.1%. The method was applied for the determination of the red wine real samples from the market. Carbendazim, imidacloprid, pyrimethanil, tebuconazole and triadimenol were detected in the samples. The results show that the method is suitable for the rapid screening and quantitative analysis of pesticide residues in red wine. PMID:25185308

  7. 76 FR 69690 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2011-11-09

    ...Additional data may be needed before EPA can make a final determination on these pesticide petitions. Pursuant to 40 CFR 180...extracted from blueberries, tomato and tomato paste with acetone. The final samples were analyzed by LC/ MS/MS for...

  8. 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

    ...180 for residues of the insecticide clothianidin, (E)-1-(2-chloro-1,3-thiazol-5-ylmethyl...products, the residue of concern, parent clothianidin, can be determined using HPLC with...demonstrated the ability to extract aged clothianidin residue. Although the plant...

  9. LC/MS/MS MULTIRESIDUE ANALYSIS OF POLAR PESTICIDES IN SOIL AND WATER

    Science.gov (United States)

    Traditionally, pesticide analysis has been by gas chromatography (GC) coupled to various detectors. However, many of the newer classes of pesticides are polar, nonvolatile chemicals, which are not amenable to analysis by GC. These pesticides have primarily been derivatized prior to analysis by GC or...

  10. A review of methods for the analysis of orphan and difficult pesticides: glyphosate, glufosinate, quaternary ammonium and phenoxy acid herbicides, and dithiocarbamate and phthalimide fungicides.

    Science.gov (United States)

    Raina-Fulton, Renata

    2014-01-01

    This article reviews the chromatography/MS methodologies for analysis of pesticide residues of orphan and difficult chemical classes in a variety of sample matrixes including water, urine, blood, and food. The review focuses on pesticide classes that are not commonly included in multiresidue analysis methods such as highly polar or ionic herbicides including glyphosate, glufosinate, quaternary ammonium, and phenoxy acid herbicides, and some of their major degradation or metabolite products. In addition, dithiocarbamate and phthalimide fungicides, which are thermally unstable and have stability issues in some solvents or sample matrixes, are also examined due to their special needs in residue analysis. PMID:25145125

  11. Distribution of phthalates, pesticides and drug residues in the dissolved, particulate and sedimentary phases from transboundary rivers (France-Belgium).

    Science.gov (United States)

    Net, Sopheak; Rabodonirina, Suzanah; Sghaier, Rafika Ben; Dumoulin, David; Chbib, Chaza; Tlili, Ines; Ouddane, Baghdad

    2015-07-15

    Various drug residues, pesticides and phthalates are ubiquitous in the environment. Their presence in the environment has attracted considerable attention due to their potential impacts on ecosystem functioning and on public health. In this work, 14 drug residues, 24 pesticides and 6 phthalates have been quantified in three matrices (in the dissolved phase, associated to suspended solid matter (SSM), and in sediment) collected from fifteen watercourses and rivers located in a highly industrialized zone at the cross-border area of Northern France and Belgium. The extractions have been carried out using accelerated solvent extraction (ASE) for solid matrices (SSM and sediment) and using solid phase extraction (SPE) for liquid matrix. The final extract was analyzed using GC-MS technique. Among the three classes of compounds, phthalates have been found at highest level compared to pesticides and drug residues. The ?6PAE concentrations were ranging from 17.2±2.58 to 179.1±26.9?gL(-1) in dissolved phase, from 2.9±0.4 to 21.1±3.2?gL(-1) in SSM and from 1.1±0.2 to 11.9±1.8?gg(-1)dw in sediment. The ?14drug residue concentrations were lower than 1.3?gL(-1) in the dissolved phases, lower than 30ngL(-1) associated to SSM and from nondetectable levels to 60.7±9.1ngg(-1)dw in sediment. For pesticides, all compounds were below the LOQ values in dissolved phase and in sediment, and only EPTC could be quantified in SSM. PMID:25829293

  12. 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

  13. Application of QuEChERS Method for Simultaneous Determination of Pesticide Residues and PAHs in Fresh Herbs

    OpenAIRE

    Sadowska-rociek, Anna; Surma, Magdalena; Cies?lik, Ewa

    2013-01-01

    The aim of this study was to evaluate the application of quick, easy, cheap, effective, rugged and safe method for simultaneous determination of polycyclic aromatic hydrocarbons and pesticide residues in fresh herbs. In the experiment two extraction solvents and standard types of sorbents were used. The extracts were analyzed using GC–SIM–MS. The results suggest that acetonitrile is more suitable extraction solvent giving more purified samples and better recovery values (71.6 %–116.9 ...

  14. Mobilization of soil bound residue of organochlorine pesticides and polycyclic aromatic hydrocarbons in an in-vitro gastrointestinal model

    OpenAIRE

    Tao, Shu; Li, Li; Ding, Junnan; Zhong, Junjun; Zhang, Diyu; Lu, Yan; Yang, Yifeng; Wang, Xilong; Li, Xiqing; Cao, Jun; Lu, Xiaoxia; Liu, Wenxin

    2010-01-01

    A previous study on mobilization of organochlorine pesticides (OCPs) in contaminated soils from the field revealed that the total amount of OCPs measured in digestive fluid and chyme of an in-vitro gastrointestinal model was higher than the quantity directly extracted using a solvent extraction without digestion, providing a clue that the bound residue of OCPs might be mobilized. This hypothesis was tested in this study for both OCPs and polycyclic aromatic hydrocarbons (PAHs). Three contamin...

  15. Behavior of Multiclass Pesticide Residue Concentrations during the Transformation from Rose Petals to Rose Absolute.

    Science.gov (United States)

    Tascone, Oriane; Fillâtre, Yoann; Roy, Céline; Meierhenrich, Uwe J

    2015-05-27

    This study investigates the concentrations of 54 multiclass pesticides during the transformation processes from rose petal to concrete and absolute using roses spiked with pesticides as a model. The concentrations of the pesticides were followed during the process of transforming the spiked rose flowers from an organic field into concrete and then into absolute. The rose flowers, the concrete, and the absolute, as well as their transformation intermediates, were analyzed for pesticide content using gas chromatography/tandem mass spectrometry. We observed that all the pesticides were extracted and concentrated in the absolute, with the exception of three molecules: fenthion, fenamiphos, and phorate. Typical pesticides were found to be concentrated by a factor of 100-300 from the rose flowers to the rose absolute. The observed effect of pesticide enrichment was also studied in roses and their extracts from four classically phytosanitary treated fields. Seventeen pesticides were detected in at least one of the extracts. Like the case for the spiked samples in our model, the pesticides present in the rose flowers from Turkey were concentrated in the absolute. Two pesticides, methidathion and chlorpyrifos, were quantified in the rose flowers at approximately 0.01 and 0.01-0.05 mg kg(-1), respectively, depending on the treated field. The concentrations determined for the corresponding rose absolutes were 4.7 mg kg(-1) for methidathion and 0.65-27.25 mg kg(-1) for chlorpyrifos. PMID:25942486

  16. 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

  17. Pesticide residues in cashew apple, guava, kaki and peach: GC-?ECD, GC-FPD and LC-MS/MS multiresidue method validation, analysis and cumulative acute risk assessment.

    Science.gov (United States)

    Jardim, Andréia Nunes Oliveira; Mello, Denise Carvalho; Goes, Fernanda Caroline Silva; Frota Junior, Elcio Ferreira; Caldas, Eloisa Dutra

    2014-12-01

    A multiresidue method for the determination of 46 pesticides in fruits was validated. Samples were extracted with acidified ethyl acetate, MgSO4 and CH3COONa and cleaned up by dispersive SPE with PSA. The compounds were analysed by GC-FPD, GC-?ECD or LC-MS/MS, with LOQs from 1 to 8 ?g/kg. The method was used to analyse 238 kaki, cashew apple, guava, and peach fruit and pulp samples, which were also analysed for dithiocarbamates (DTCs) using a spectrophotometric method. Over 70% of the samples were positive, with DTC present in 46.5%, ?-cyhalothrin in 37.1%, and omethoate in 21.8% of the positive samples. GC-MS/MS confirmed the identities of the compounds detected by GC. None of the pesticides found in kaki, cashew apple and guava was authorised for these crops in Brazil. The risk assessment has shown that the cumulative acute intake of organophosphorus or pyrethroid compounds from the consumption of these fruits is unlikely to pose a health risk to consumers. PMID:24996324

  18. Residues in Food and Feed Topic Area at the 13th IUPAC International Congress of Pesticide Chemistry.

    Science.gov (United States)

    Lehotay, Steven J; Riter, Leah S; Saha, Manasi

    2015-05-13

    The organizers of two symposia in the "Residues in Food and Feed" topic area held at the 13th IUPAC International Congress of Pesticide Chemistry introduce the papers that were contributed to this special section in the Journal. The symposia were titled "Taking Advantage of Advanced Analytical Tools" and "Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods". The oral and poster sessions generated much interest and discussion among the attendees, and some highlights are described in this introductory paper. PMID:25660997

  19. 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.

  20. Organophosphorus pesticides residues in fish samples from the River Nile tributaries in Egypt.

    Science.gov (United States)

    Malhat, Farag; Nasr, Islam

    2011-12-01

    The concentration of organophosphorus pesticides in fish samples from different tributaries of the Nile River in Egypt was monitored. Fish samples were collected from El Menofiya, canal water supplies (El-Sarsawia, El-Bagoria and Bahr Shebin), in addition to El-Embaby, El-Menofi and Miet Rabiha drainage canals each 2 month during periods of 16 month, June 2007-Septemper 2008. Chloropyrifos, cadusafos, diazinon, prothiphos and malathion were detected in fish tissues samples at level below the maximum residue limit. The highest average amount of chlorpyrifos (9.38 ng g(-1)) and malathion (8.31 ng g(-1)) were detected in El-Embaby drain. Prothiphos were found in tissues collected from El-Sarsawia canal and Miet-Rabiha drain at mean concentration of 4.91 and 6.55 ng g(-1), respectively. Diazinon was only found in one fish sample that collected from El-Menofi drain at the level of 9.23 ng g(-1). PMID:21953307

  1. 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.

  2. Organochlorine pesticide residues in mother's milk: a source of toxic chemicals in suckling infants.

    Science.gov (United States)

    Ramakrishnan, N; Kaphalia, B S; Seth, T D; Roy, N K

    1985-01-01

    A total of 24 samples of mother's milk collected during the first week of lactation from four major cities in India (Karnal, Bangalore, Calcutta and Bombay) were analysed for the estimation of organochlorine pesticides (OCPs). alpha-HCH, p,p'-DDE, and p,p'-DDT were generally the main contaminants. The average total 1,1,1-trichloro-2,2-bis (p-chlorophenyl) ethane (DDT) levels stand at 0.05, 0.11, 0.19 and 0.22 p.p.m. (whole-milk basis) in the samples from Bangalore, Calcutta, Karnal and Bombay respectively. In the same order total hexachlorocyclohexane (HCH) levels were around 0.01, 0.03, 0.03 and 0.05 p.p.m. Wide variations among OCP levels observed in the present study have no relation with the fat content of the various samples. The samples from Calcutta and Bombay showed significantly high levels of OCPs. The daily intake of total HCH and DDT residues calculated for the suckling infant was significantly higher in the present study when compared with the WHO recommended value. PMID:3988308

  3. [Validation study of a method for multiresidue analysis of pesticides in cereals and pulses using supercritical fluid extraction].

    Science.gov (United States)

    Uranishi, Katsushige; Yamashita, Hirokazu; Okayama, Akiko; Yamamoto, Keigo

    2012-01-01

    Supercritical fluid extraction (SFE) was applied to extraction of pesticides from cereals and pulses. Residues were extracted from homogenized samples mixed with water-absorbent polymer and supercritical carbon dioxide in a stainless steel tube, followed by elution with acetonitrile. Co-extractives were removed by means of mini-column clean-up. Measurement was performed by GC-MS/MS. Calibration was achieved by preparing matrix-matched calibration standards to counteract matrix effects. With the Japanese method validation guideline for pesticide residues as a reference, the method was assessed in 5 agricultural products spiked with 334 pesticides at 0.01 and 0.1 µg/g. Compounds at each level were extracted from 2 samples on 5 separate days. The trueness of the method for 137 pesticides in all samples was 70-120%, and the repeatability and within-run reproducibility were also consistent with the guideline. The trueness of the method for the other 101 pesticides was in the range of 50-70%, though the repeatability and within-run reproducibility were satisfactory. This method is available as a multiresidue analysis method for cereals and pulses. PMID:23470855

  4. 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

  5. 76 FR 43231 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2011-07-20

    ...AG-454A were developed for the determination of residues of propiconazole...apples by homogenization with acetone. An aliquot of the extract...water with subsequent residue determination by HPLC/MS/MS. The...specific cleanup procedures and determination by gas chromatography...

  6. 75 FR 864 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2010-01-06

    ...part 180 for residues of the fungicide fluopyram (N-[2-[3-chloro-5-(trifluoromethyl...part 180 for residues of the fungicide fluopyram (N-[2-[3- chloro-5-(trifluoromethyl...liver at 1.2 ppm for (P 8F7463). Fluopyram was determined to be the only...

  7. 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.

  8. Current status of persistent organic pesticides residues in air, water, and soil, and their possible effect on neighboring countries: a comprehensive review of India.

    Science.gov (United States)

    Yadav, Ishwar Chandra; Devi, Ningombam Linthoingambi; Syed, Jabir Hussain; Cheng, Zhineng; Li, Jun; Zhang, Gan; Jones, Kevin C

    2015-04-01

    Though the use of pesticides has offered significant economic benefits by enhancing the production and yield of food and fibers and the prevention of vector-borne diseases, evidence suggests that their use has adversely affected the health of human populations and the environment. Pesticides have been widely distributed and their traces can be detected in all areas of the environment (air, water and soil). Despite the ban of DDT and HCH in India, they are still in use, both in domestic and agricultural settings. In this comprehensive review, we discuss the production and consumption of persistent organic pesticides, their maximum residual limit (MRL) and the presence of persistent organic pesticides in multicomponent environmental samples (air, water and soil) from India. In order to highlight the global distribution of persistent organic pesticides and their impact on neighboring countries and regions, the role of persistent organic pesticides in Indian region is reviewed. Based on a review of research papers and modeling simulations, it can be concluded that India is one of the major contributors of global persistent organic pesticide distribution. This review also considers the health impacts of persistent organic pesticides, the regulatory measures for persistent organic pesticides, and the status of India's commitment towards the elimination of persistent organic pesticides. PMID:25540847

  9. 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

  10. Two-dimensional coordination polymer matrix for solid-phase extraction of pesticide residues from plant Cordia salicifolia.

    Science.gov (United States)

    de Carvalho, Pedro Henrique Viana; Barreto, Alysson Santos; Rodrigues, Marcelo O; Prata, Vanessa de Menezes; Alves, Péricles Barreto; de Mesquita, Maria Eliane; Alves, Severino; Navickiene, Sandro

    2009-06-01

    The 2D coordination polymer (infinity[Gd(DPA)(HDPA)]) was tested for extraction of acephate, chlorpropham, pirimicarb, bifenthrin, tetradifon, and phosalone from the medicinal plant Cordia salicifolia, whose extracts are commercialized in Brazil as diuretic, appetite suppressant, and weight loss products, using GC/MS, SIM. Considering that there are no Brazilian regulations concerning maximum permissible pesticide residue concentrations in medicinal herbs, recovery experiments were carried out (seven replicates), at two arbitrary fortification levels (0.5 and 1.0 mg/kg), resulting in recoveries in range of 20 to 107.7% and SDRSDs were between 5.6 and 29.1% for infinity[Gd(DPA)(HDPA)] sorbent. Detection and quantification limits for herb ranged from 0.10 to 0.15 mg/kg and from 0.15 to 0.25 mg/kg, respectively, for the different pesticides studied. The developed method is linear over the range assayed, 0.5-10.0 microg/mL, with correlation coefficients ranging from 0.9975 to 0.9986 for all pesticides. Comparison between infinity[Gd(DPA)(HDPA)] sorbent and conventional sorbent (neutral alumina) showed similar performance of infinity[Gd(DPA)(HDPA)] polymeric sorbent for three (bifenthrin, tetradifon, and phosalone) out of six pesticides tested. PMID:19479754

  11. 40 CFR 158.2082 - Experimental use permit biochemical pesticides residue data requirements table.

    Science.gov (United States)

    2010-07-01

    ... 860.1100 Chemical identity CR... 860.1400 Fish NR CR NR...for biochemical pesticides product chemistry...biochemical human health assessment data... 2. The same chemical identity data...uses where the pesticide is applied... 12. Data on fish are...

  12. 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.

  13. 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

    ...submitted by ISK Biosciences Corporation, 7470 Auburn Road, Suite A, Concord, OH 44057. An analytical method using LC/MS/MS for the determination of fluazinam and AMGT residues on cantaloupe and pepper has been developed and validated....

  14. 77 FR 50661 - Notice of Filing of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2012-08-22

    ...BF 500-3); expressed as parent compound, in or on sugarcane, cane at 0.2 ppm. No tolerances are proposed for the processed commodities, refined sugar and molasses, as no concentration of pyraclostrobin residues are expected...

  15. 76 FR 76674 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2011-12-08

    ...Suite 201 W, Princeton, NJ 08450, requests to establish tolerances in 40 CFR part 180 for residues of the insecticide clothianidin, (E)-1-(2-chloro-1,3- thiazol-5-ylmethyl)-3-methyl-2-nitroguanidine, in or on strawberry...

  16. 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

  17. 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)

  18. 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.

  19. Levels of organochlorine pesticides residues in milk of urban mothers in Kenya.

    Science.gov (United States)

    Kinyamu, J K; Kanja, L W; Skaare, J U; Maitho, T E

    1998-05-01

    Organochlorine compounds (OCPs) are toxic products capable of producing serious adverse health consequences. When used to control pests, certain OCPs persist in the environment and accumulate in the fatty tissues of living organisms, reaching higher levels in animals higher in the food chain. Many countries have therefore either restricted or banned the use of OCPs. DDT used to be widely used in Kenya to control pests, but is now used only to control mosquito populations. The contamination of human milk by organochlorine and other related compounds is a major concern in many parts of the world. Findings are reported from a study conducted to assess the levels of OCPs in an urban area of Kenya and to compare OCP levels in human milk from a previous study in rural areas of the country. 216 milk samples were collected from mothers aged 18-30 years in hospital maternity wards or attending postnatal clinics in selected areas in Nairobi in 1991. All mothers involved in the study were nursing either their first or second child, and had lived in Nairobi for at least 5 years before the date of sampling. Samples were collected from mothers who were up to 4 weeks postpartum and analyzed for the presence of OCP residues. 9 OCPs were detected, with p,p'DDT and p,p'DDE being the most frequently encountered contaminants in all samples analyzed. p,p'DDE was detected in 99.5% and p,p'DDT in 78.2% of all samples. Other residues detected were dieldrin (27%), beta-HCH (18.5%), lindane (12%), and alpha-HCH (8.8%). Levels of sum DDT ranged from 0.004 to 6.321 mg/kg fat. Mothers living in Nairobi have low levels of OCPs in their breast milk compared to mothers in rural areas. The relatively lower urban levels could be attributed to the restricted use of OCPs. People need to be taught how to safely use pesticides. PMID:9595188

  20. Determination of pesticide residue in soil, water and grain from IPM and non-IPM field trials of rice.

    Science.gov (United States)

    Arora, Sumitra; Mukherjee, Irani; Trivedi, T P

    2008-10-01

    Soil, water and rice grain samples from field trials conducted under the IPM and non-IPM modules in Kaithal (Haryana) region were analyzed for pendimethalin, atrazine, lindane and chlorpyriphos, and in Dehradun (Uttarakhand) region, samples were analyzed for carbendazim only. The pesticide residues were found below the detectable limit in the soil and water samples of the Kaithal region. From Dehradun region the residues of carbendazim in rice grains were detected at 0.001 mg/kg level, and in soil they were in the range of 0.03-0.001 mg/kg. The insecticides applied in IPM as well as non-IPM trials in both regions were observed to be below the prescribed maximum residue level. PMID:18679559

  1. Non-parametric production analysis of pesticides use in the Netherlands

    OpenAIRE

    A.G.J.M. Oude Lansink; Silva, E.

    2004-01-01

    Many previous empirical studies on the productivity of pesticides suggest that pesticides are under-utilized in agriculture despite the general held believe that these inputs are substantially over-utilized. This paper uses data envelopment analysis (DEA) to calculate non-parametric measures of the value of the marginal product of pesticides. Furthermore, the effect of pesticides on the value of the marginal product of productive inputs is investigated in order to analyze technical interdepen...

  2. 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

  3. 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

  4. 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

    ...Chemical Co., Ltd), proposes to establish a time-limited tolerance in 40 CFR part 180 for residues of the insecticide clothianidin, (E)-1-(2-chloro- 1,3-thiazol-5-ylmethyl)-3-methyl-2-nitroguanidine, in or on rice, grain...

  5. 77 FR 75082 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Science.gov (United States)

    2012-12-19

    ...560 for the combined residues of cloquintocet- mexyl (acetic acid, [(5-chloro-8-quniolinyl...are already established for use of cloquintocet-mexyl in conjunction with other herbicides...138.01 is for the determination of cloquintocet-mexyl (parent) and the...

  6. Development of an Automated Column Solid-Phase Extraction Cleanup of QuEChERS Extracts, Using a Zirconia-Based Sorbent, for Pesticide Residue Analyses by LC-MS/MS.

    Science.gov (United States)

    Morris, Bruce D; Schriner, Richard B

    2015-06-01

    A new, automated, high-throughput, mini-column solid-phase extraction (c-SPE) cleanup method for QuEChERS extracts was developed, using a robotic X-Y-Z instrument autosampler, for analysis of pesticide residues in fruits and vegetables by LC-MS/MS. Removal of avocado matrix and recoveries of 263 pesticides and metabolites were studied, using various stationary phase mixtures, including zirconia-based sorbents, and elution with acetonitrile. These experiments allowed selection of a sorbent mixture consisting of zirconia, C18, and carbon-coated silica, that effectively retained avocado matrix but also retained 53 pesticides with 70% recoveries of all 263 pesticides. Analysis of avocado extracts by LC-Q-Orbitrap-MS showed that the method developed was removing >90% of di- and triacylglycerols. The method was validated for 269 pesticides (including homologues and metabolites) in avocado and citrus. Spike recoveries were within 70-120% and 20% RSD for 243 of these analytes in avocado and 254 in citrus, when calibrated against solvent-only standards, indicating effective matrix removal and minimal electrospray ionization suppression. PMID:25702899

  7. The interaction between natural organic matter in raw waters and pesticide residues: a three dimensional excitation-emission matrix (3DEEM) fluorescence investigation.

    Science.gov (United States)

    Beale, David J; Porter, Nichola A; Roddick, Felicity A

    2013-01-01

    This paper examines the interaction between dissolved natural organic matter and pesticide residues, both of which are found in raw water sources, using three dimensional excitation-emission matrix (3DEEM) fluorescence spectroscopy. It was observed that pesticide residue at 0.1 mg L(-1) formed a complex with humic-like fluorophores that are commonly found in raw water samples. Applying 3DEEM fluorescence to investigate the humic fractions, it was found that identification of changes in water sources was possible, and, importantly, the presence of a number of pesticides was able to be determined. In addition, the formation of this complex, and the influence of soluble cations and anions upon it, was shown to impact the efficiency of analytical extraction procedures for pesticides; however, 3DEEM fluorescence could be an approach to account for such losses. PMID:23752373

  8. 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...

  9. 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.

  10. Analysis of Endocrine Disrupting Pesticides by Capillary GC with Mass Spectrometric Detection

    Directory of Open Access Journals (Sweden)

    Svetlana Hrouzková

    2012-09-01

    Full Text Available Endocrine disrupting chemicals, among them many pesticides, alter the normal functioning of the endocrine system of both wildlife and humans at very low concentration levels. Therefore, the importance of method development for their analysis in food and the environment is increasing. This also covers contributions in the field of ultra-trace analysis of multicomponent mixtures of organic pollutants in complex matrices. With this fact conventional capillary gas chromatography (CGC and fast CGC with mass spectrometric detection (MS has acquired a real importance in the analysis of endocrine disrupting pesticide (EDP residues. This paper provides an overview of GC methods, including sample preparation steps, for analysis of EDPs in a variety of matrices at ultra-trace concentration levels. Emphasis is put on separation method, mode of MS detection and ionization and obtained limits of detection and quantification. Analysis time is one of the most important aspects that should be considered in the choice of analytical methods for routine analysis. Therefore, the benefits of developed fast GC methods are important.

  11. 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.

  12. 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).

  13. Organophosphorus and Carbamate Pesticide Residues Detected in Water Samples Collected from Paddy and Vegetable Fields of the Savar and Dhamrai Upazilas in Bangladesh

    OpenAIRE

    Nurul Karim; Siew Hua Gan; Borhan Uddin; Mohammed Moniruzzaman; Sanjoy Banik; Md. Alamgir Zaman Chowdhury

    2012-01-01

    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 ...

  14. Non-destructive detection of pesticide residues in cucumber using visible/near-infrared spectroscopy.

    Science.gov (United States)

    Jamshidi, Bahareh; Mohajerani, Ezeddin; Jamshidi, Jamshid; Minaei, Saeid; Sharifi, Ahmad

    2015-06-01

    The feasibility of using visible/near-infrared (Vis/NIR) spectroscopy was assessed for non-destructive detection of diazinon residues in intact cucumbers. Vis/NIR spectra of diazinon solution and cucumber samples without and with different concentrations of diazinon residue were analysed at the range of 450-1000 nm. Partial least squares-discriminant analysis (PLS-DA) models were developed based on different spectral pre-processing techniques to classify cucumbers with contents of diazinon below and above the MRL as safe and unsafe samples, respectively. The best model was obtained using a first-derivative method with the lowest standard error of cross-validation (SECV = 0.366). Moreover, total percentages of correctly classified samples in calibration and prediction sets were 97.5% and 92.31%, respectively. It was concluded that Vis/NIR spectroscopy could be an appropriate, fast and non-destructive technology for safety control of intact cucumbers by the absence/presence of diazinon residues. PMID:25789964

  15. Analysis of organophosphorus pesticides in honeybee by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry.

    Science.gov (United States)

    Fernández, M; Picó, Y; Girotti, S; Mañes, J

    2001-08-01

    Pesticides applied in extended agricultural fields may be controlled by means of bioindicators, such as honeybees, in which are the pesticides bioaccumulate. Liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) experiments with positive (PI) and negative (NI) ion modes were optimized for the analysis of 22 organophosphorus pesticides in honeybee samples. The extraction required 3 g of sample, which was extracted with acetone. The extract was purified with coagulating solution and reextracted with Cl(2)CH(2). Pesticides studied could be detected by both ionization modes except for parathion, parathion-methyl, and bromophos, which did not give signals in PI mode, and triazophos, which was not detected in NI mode. Fragmentation voltage and vaporizer temperature were optimized to achieve the highest sensitivity. The spectra profile of each pesticide in PI mode showed the [M + H](+) ion as the main signal, whereas in NI mode only fragment ions were shown. The detection limit obtained in selected ion monitoring mode ranged from 1 to 15 microg kg(-1). The average recoveries from spiked honeybees at various concentration levels (0.5-5 mg kg(-1)) exceeded 65% with relative standard deviations of 4-15%. The method was applied to real samples, in which residues of coumaphos and dimethoate were detected. PMID:11513625

  16. 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)

  17. Pesticide formulation analysis by gas chromatography flame ionization detector

    International Nuclear Information System (INIS)

    Gas liquid chromatography system equipped with flame ionization detector was used in the analysis of pesticides formulation. A series of organophosphorus pesticides formulation (Cypermethrin and Dursban) were investigated under different conditions. The samples under study were consisting of 20 blank formulated sample (without active ingredient) and 5 formulated samples with active ingredients. Three capillary columns were used; 10 meter fused silica thick film containing a non-polar methyl silicone, 20- meter thin film methyl silicone and 50-m (0.25 ?m x 0.32 mm. i. d.) methyl silicone, thin film. The three types of columns were used to assess and achieve a simple and practical way for quantitative measurement with RSD within 1% for a series of organophosphours pesticide formulations. 10 meter fused silica thick film also used to separate and determine the four stereo isomers of Cypermethrin present in such formulations. Mixtures with relatively short retention times, as well as Dursban. The 10-meter column, although of high quality, only partially resolved the Cypermethrin isomers into three overlapping peaks instead of the expected four. As a consequence, the 10-meter capillary column produced the largest errors in the quantitative analysis and was unsatisfactory, especially with regard to the Cypermethrin content. The performance of the 10-meter column could not be improved even when conditions were varified however, both columns (20 m, 50 m) showed good performacolumns (20 m, 50 m) showed good performance and solved the Cypermethrin isomers completely. (author)

  18. Effect of land use change from paddy to vegetable field on the residues of organochlorine pesticides in soils

    International Nuclear Information System (INIS)

    The effect of land use change from paddy to vegetable field on the residues of organochlorine pesticides (OCPs) was investigated. Soil residues of OCPs were analyzed in vegetable fields which had been converted from paddy fields for 0, 5, 10, 15, 20, 30, 50 year in Yixing, China in 2003. The mean concentrations of OCPs followed a sequence of: ?DDTs (13.7 ?g kg-1) > ?HCHs (8.6 ?g kg-1) > > HCB (2.09 ?g kg-1) > ?-endosulfan (1.30 ?g kg-1) > endrin (1.08 ?g kg-1) > PCNB (0.76 ?g kg-1) > dieldrin (0.58 ?g kg-1). The mean residues of OCPs especially DDTs increased significantly with vegetable planting time after land use change in the first 15 years, then decreased from 20 to 30 years and increased a little afterward. The time under anaerobic and aerobic conditions was suggested to control mainly the change of the residues of OCPs. - The OCPs residues especially DDTs changed significantly with tillage time after the conversion from paddy to vegetable field

  19. Search of Organochlorine Pesticide Residues (Pocs in Bodies of Water in Cotton-Growing Area of Benin by GC-ECD

    Directory of Open Access Journals (Sweden)

    M. A. N. Gbaguidi

    2014-06-01

    Full Text Available Despite their incontestable services in agriculture, the use of pesticides is not without consequences on the environment. So, in an attempt to access the impacts of pesticides usage in agriculture in Benin, research of some residual organochloride pesticides have been conducted both in rainy and dry seasons in two cotton growing areas: the northern and central part of Benin. The analytical technique used is GC-ECD. During the dry season we notice that the DDT and its metabolites (DDE and DDD represent 36% of all organochlorine pesticides (POCs against 64 % of cyclodiens. Endosulfan comes first representing 57% of all organochlorine pesticides (POCs, then follows DDT with 17 %. During the rainy season these two types of organochlorine pesticides (POCs represent 73% for cyclodiens and 23% for DDT and its by-products. Endosulfan comes first by representing 47% of all organochlorine pesticides (POCs followed by DDT representing 12%. In the sediments and regardless of the season, the cyclodiens come first by representing 70% of all organochlorine pesticides (POCs and then follows the DDT and its by-products which represent 30%. Since in the water column, the sediments are more contaminated in rainy season than in dry season (25273 ppb of all organochlorine pesticide (POCs in rainy season against 2.256 ppb in dry season, it is derived from this study that northern areas are more contaminated than the central areas. Also a strong correlation has been established between the content of different moleculars of organochlorine pesticide (POCs. This means that the famers still use prohibited pesticides in the two areas despite existing laws like “Stockholm convention” which strictly ban the usage of those moleculars.

  20. Residual stress analysis with neutrons

    International Nuclear Information System (INIS)

    The use of neutrons for the measurement of stress is complementary to and extends traditional x-ray diffraction methods to new types of problems. This is due to the lower absorption of neutrons compared to x-ray by most engineering materials, which increases the sampling depth from microns to millimeters. It is particularly suitable for triaxial macrostress gradients through the depth of engineering components and volumetric microstresses in composites. In addition, applied stress studies may also be performed. This paper describes the nature of residual stresses, the use of diffraction of stress measurements, experimental aspects of the use of neutrons, and illustrative applications

  1. Scientific support for preparing an EU position for the 45th Session of the Codex Committee on Pesticide Residues (CCPR

    Directory of Open Access Journals (Sweden)

    European Food Safety Authority

    2013-07-01

    Full Text Available In accordance with Article 43 of Regulation (EC No 396/2005, EFSA received a request from the European Commission to provide support for the preparation of the EU position for the 45th session of the Codex Committee on Pesticide Residues (CCPR. In 2012, JMPR evaluated 12 active substances regarding the setting of toxicological reference values to be used in consumer risk assessment, 7 new compounds (ametoctradin, chlorfenapyr, dinotefuran, fluxapyroxad, MCPA, picoxystrobin, sedaxane and 4 part of periodic reevaluation (benzoate, fenpropathrin, fenvalerate, glufosinate-ammonium. Regarding the setting of Maximum Residue Limits (CXLs, JMPR assessed 26 substances (ametoctradin, azoxystrobin, buprofezin, carbofuran, chlorfenapyr, chlorothalonil, cycloxydim, cyfluthrin, cyromazine, dichlorvos, dicofol, dinotefuran, fenvalerate, fludioxonil, fluopyram, fluxapyroxad, glufosinate-ammonium, imidacloprid, MCPA, methoxyfenozide, penthiopyrad, phorate, picoxystrobin, sedaxane, spinetoram and trifloxystrobin. EFSA derived comments on the JMPR evaluations regarding the acceptability of the proposed draft Codex MRLs and the toxicological reference values.

  2. 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.

  3. A lysimeter experiment to investigate temporal changes in the availability of pesticide residues for leaching

    International Nuclear Information System (INIS)

    Leaching of three pesticides (isoproturon, chlorotoluron and triasulfuron) and a tracer (bromide) were determined in four contrasting soils ranging in texture from sandy loam to clay. The compounds were applied to undisturbed columns of soil and four columns for each soil were randomly selected and leached with 24-mm equivalent of water at prescribed time intervals (3, 9, 24, 37 and 57 d after application). A rapid decline in leached loads of isoproturon and chlorotoluron as time from application to irrigation increased was observed in all soils. In contrast, triasulfuron and bromide loads only decreased rapidly in the clay soil. Bromide losses decreased with decreasing clay contents of the soil and therefore with a decrease in structural development. Magnitudes of pesticide losses varied from soil to soil, depending on structural development and the organic carbon content. Pesticide degradation experiments on disturbed and undisturbed soil samples showed that the rapid decline of leached loads with time was faster than could be explained by degradation alone. Five physico-chemical processes are put forward to explain the different patterns of pesticide leached loads observed in the soils: (1) relative extent of preferential flow, (2) sorption capacity of the compounds to the different soils, (3) extent of degradation of the compounds in the soil, (4) variation in sorption kinetics between compounds associated with pesticide diffusion into soil aggregates, and (5) proiffusion into soil aggregates, and (5) protection of the compounds by a combination of intra-aggregate diffusion and the presence of preferential flow pathways

  4. 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.

  5. Organochlorine pesticide residues in different Indian cereals, pulses, spices, vegetables, fruits, milk, butter, Deshi ghee, and edible oils.

    Science.gov (United States)

    Kaphalia, B S; Takroo, R; Mehrotra, S; Nigam, U; Seth, T D

    1990-01-01

    A total of 244 samples of cereals (wheat flour, rice, and maize), pulses (arhar, moong, gram, lentil, and black gram), spices (turmeric, chili, coriander, and black pepper), vegetables (potato, onion, spinach, cabbage, brinjal, and tomato), fruits (mango, guava, apple, and grape), milk, butter, Deshi ghee, and edible oils (vegetable, mustard, groundnut, and sesame) collected from different cities of Northern Province (Utter Pradesh) were analyzed by gas liquid chromatography for the presence of organochlorine pesticide residues. Residues of hexachlorocyclohexane (HCH) and 2,2-bis(p-chlorophenyl)-1,1,1-trichloroethane (DDT) were detected in about 85% of the total samples of cereals, spices, milk, butter, Deshi ghee, and edible oils analyzed in the present study. However, the residue levels were either very small (less than 0.06 ppm) or not detected at all in pulses, vegetables, and fruits as compared with very high concentrations in wheat flour (4.42 and 0.12 ppm), butter (1.19 and 4.85 ppm), mustard oil (1.26 and 2.42 ppm), Deshi ghee (1.10 and 3.84 ppm), vegetable oil (1.02 and 0.59 ppm), groundnut oil (0.51 and 1.49 ppm), and chili (0.48 and 1.92 ppm). The levels of HCH and DDT residues detected in rice, maize, turmeric, corlander, black pepper, and all the vegetables and fruits were also lower than those found in wheat flour, oil, and fat samples analyzed in the present study. These findings suggest that a restricted and controlled use of such persistent pesticides may be useful for decreasing their contamination levels in different food items. PMID:1698760

  6. Multi-residue pesticide analysis (gas chromatography-tandem mass spectrometry detection)-Improvement of the quick, easy, cheap, effective, rugged, and safe method for dried fruits and fat-rich cereals-Benefit and limit of a standardized apple purée calibration (screening).

    Science.gov (United States)

    Rasche, Claudia; Fournes, Britta; Dirks, Uwe; Speer, Karl

    2015-07-17

    Some steps of the QuEChERS method for the analysis of pesticides with GC-MS/MS in cereals and dried fruits were improved or simplified. For the latter, a mixing vessel with stator-rotor-system proved to be advantageous. The extraction procedure of dried fruits is much easier and safer than the Ultra Turrax and results in excellent validation data at a concentration level of 0.01mg/kg (116 of 118 analytes with recoveries in the range of 70-120%, 117 of 118 analytes with RSD 7%), predominantly organochlorines showed recoveries of <70% in quantification when the standard QuEChERS method with water was used. A second extraction was carried out analogous to the QuEChERS method, however, without the addition of water. With this simple modification, the problematic lipophilic pesticides, which had been strongly affected by the fat content of the commodities, could be determined with recoveries above 70% even at a concentration level of 0.01mg/kg. Moreover, a GC-MS/MS screening method for 120 pesticides at a concentration level of 0.01mg/kg was established by employing analyte protectants (ethylglycerol, gulonolactone, and sorbitol). The use of only one standardized calibration, made of an apple purée extract in combination with analyte protectants, allowed for a qualitative and quantitative analysis of 120 pesticides in different matrix extracts (tomato, red pepper, sour cherries, dried apples, black currant powder, raisins, wheat flour, rolled oats, wheat germ). The analyte protectants leveled the differences in the matrix-induced protection effect of the analyzed extracts over a wide range. The majority of the pesticides were analyzed with good analytical results (recoveries in the range of 70-120% and RSD <20%). PMID:26044382

  7. Seasonal and spatial studies on pesticide residues in surface waters of the Shinano river in Japan.

    Science.gov (United States)

    Tanabe, A; Mitobe, H; Kawata, K; Yasuhara, A; Shibamoto, T

    2001-08-01

    Water samples collected once a week from early April 1996 to the end of August 1996 from four sites on the Shinano River in Japan were analyzed for pesticides and their metabolites using a gas chromatograph-mass spectrometer. Among the total of 53 chemicals found, 22 were herbicides, 15 were insecticides, 11 were fungicides, and 5 were metabolites. The concentrations of chemicals found ranged from 3 ng/L (bromobutide) to 8200 ng/L (isoprothiolane). Herbicides were found primarily during May and June at all four sites. Insecticides and fungicides were found primarily during July and August at all four sites. The presence of pesticides in the river water correlated with the time of pesticide application to the rice fields near the river. PMID:11513677

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

    OpenAIRE

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

    2006-01-01

    Although several cytogenetic biomonitoring studies on workers exposed to pesticides have been reported, there is only limited information on this topic from developing countries where pesticides have been widely used over the years. People in developing countries are at higher risk from exposure, due to poor working conditions and a lack of awareness of the potential hazards during manufacturing and application of the pesticides. The present study has assessed the genotoxic effects of pestici...

  9. 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 Ada even though it was detected in the milk samples from Accra. p,p'-DDE was recorded in all the individual milk samples from Accra. p,p'-DDE was detected in 90.5% of the milk samples from Ada. Gamma -HCH was detected in 95.2% of the milk samples from Ada. With the exception of the mean concentrations of endosulfan sulfate from Accra and Ada which are 99.052 µg/kg fat and 63.803 µg/kg fat respectively. The mean concentrations of all the other organochlorine pesticides detected were below the internationally recognized maximum residue limit. (author)

  10. 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.

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

    OpenAIRE

    Claudia R. Binder; Camilo Lesmes-Fabian

    2013-01-01

    Human exposure assessment tools represent a means for understanding human exposure to pesticides in agricultural activities and managing possible health risks. This paper presents a pesticide flow analysis modeling approach developed to assess human exposure to pesticide use in greenhouse flower crops in Colombia, focusing on dermal and inhalation exposure. This approach is based on the material flow analysis methodology. The transfer coefficients were obtained using the whole body dosimetry ...

  12. Evaluation of the performance of 57 Japanese participating laboratories by two types of z-scores in proficiency test for the quantification of pesticide residues in brown rice.

    Science.gov (United States)

    Otake, Takamitsu; Yarita, Takashi; Aoyagi, Yoshie; Numata, Masahiko; Takatsu, Akiko

    2014-11-01

    A proficiency test for the analysis of pesticide residues in brown rice was carried out to support upgrading in analytical skills of participant laboratories. Brown rice containing three target pesticides (etofenprox, fenitrothion, and isoprothiolane) was used as the test samples. The test samples were distributed to the 57 participants and analyzed by appropriate analytical methods chosen by each participant. It was shown that there was no significant difference among the reported values obtained by different types of analytical method. The analytical results obtained by National Metrology Institute of Japan (NMIJ) were 3 % to 10 % greater than those obtained by participants. The results reported by the participant were evaluated by using two types of z-scores, that is, one was the score based on the consensus values calculated from the analytical results of participants, and the other one was the score based on the reference values obtained by NMIJ with high reliability. Acceptable z-scores based on the consensus values and NMIJ reference values were achieved by 87 % to 89 % and 79 % to 94 % of the participants, respectively. PMID:25258285

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

    International Nuclear Information System (INIS)

    A superficial water quality survey in a watershed of the Paraiba do Sul River, the main water supply for the most populated cities of southeastern Brazil, was held in order to assess the impact of the expansion of agricultural activity in the near border of the Atlantic Rain Forest. The aim of this study was to investigate the presence of priority organochlorine pollutants in soils and superficial waters of Atlantic rainforest fragments in Teresopolis, Rio de Janeiro State. Soil sample preparations were compared by using ultrasound, microwave assisted extraction and Soxhlet extraction. Recoveries of matrix spiked samples ranged from 70 to 130%. Analysis of a certified soil material showed recoveries ranging from 71 to 234%. Although low concentrations of organochlorine residues were found in water and soil samples, this area is of environmental importance and concern, thus demanding a monitoring program of its compartments. - Highlights: ? The organochlorine pollutants occurrence in the Atlantic Rain Forest was investigated. ? PARNASO was considered a control area of environmental quality. ? Extractions methods were compared for typical C-rich soils samples from Brazil. ? Low concentrations of organochlorine residues were found in water and soil samples. ? A monitoring program is demanded due to the environmental importance of the area. - The occurrence of organochlorine pollutants in soils of the Atlantic rainforest fragments in Rio de Janeiro, Brazil deman in Rio de Janeiro, Brazil demands a monitoring program of its compartments.

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

    Energy Technology Data Exchange (ETDEWEB)

    Soares Quinete, Natalia, E-mail: nataliaquinete@yahoo.com.br [Instituto Nacional de Tecnologia, Departamento de Quimica Analitica, Laboratorio de Quimica Analitica e Metrologia em Quimica, Av. Venezuela, 82 - Rio de Janeiro, RJ 20081-312 (Brazil); Santos de Oliveira, Elba dos [Instituto Nacional de Tecnologia, Departamento de Energia, Av. Venezuela, 82 - Rio de Janeiro, RJ 20081-312 (Brazil); Fernandes, Daniella R. [Universidade Federal do Rio de Janeiro, Instituto de Quimica, Departamento de Quimica Analitica, CT - Bloco A, Cidade Universitaria, 21941-909 - Rio de Janeiro (Brazil); Souza Avelar, Andre de [Universidade Federal do Rio de Janeiro, Departamento de Geografia, Instituto de Geociencias, CCMN, Bloco F, Cidade Universitaria, 21941-919 - Rio de Janeiro (Brazil); Erthal Santelli, Ricardo [Universidade Federal do Rio de Janeiro, Instituto de Quimica, Departamento de Quimica Analitica, CT - Bloco A, Cidade Universitaria, 21941-909 - Rio de Janeiro (Brazil)

    2011-12-15

    A superficial water quality survey in a watershed of the Paraiba do Sul River, the main water supply for the most populated cities of southeastern Brazil, was held in order to assess the impact of the expansion of agricultural activity in the near border of the Atlantic Rain Forest. The aim of this study was to investigate the presence of priority organochlorine pollutants in soils and superficial waters of Atlantic rainforest fragments in Teresopolis, Rio de Janeiro State. Soil sample preparations were compared by using ultrasound, microwave assisted extraction and Soxhlet extraction. Recoveries of matrix spiked samples ranged from 70 to 130%. Analysis of a certified soil material showed recoveries ranging from 71 to 234%. Although low concentrations of organochlorine residues were found in water and soil samples, this area is of environmental importance and concern, thus demanding a monitoring program of its compartments. - Highlights: > The organochlorine pollutants occurrence in the Atlantic Rain Forest was investigated. > PARNASO was considered a control area of environmental quality. > Extractions methods were compared for typical C-rich soils samples from Brazil. > Low concentrations of organochlorine residues were found in water and soil samples. > A monitoring program is demanded due to the environmental importance of the area. - The occurrence of organochlorine pollutants in soils of the Atlantic rainforest fragments in Rio de Janeiro, Brazil demands a monitoring program of its compartments.

  15. Organochlorine pesticide residues in sardinella aurita from the coastal waters of Accra-Tema, Ghana and their potential health risks

    International Nuclear Information System (INIS)

    Sardinella aurita and seawater samples from the Accra-Tema coast of Ghana were analysed for organochlorine (OC) pesticides using gas chromatography (GC) with electron capture detection (ECD). Residues of DDTs (p,p'-DDT, p'p'-DDE,p,p'-DDD), hexachlorocyclohexane (HCHs - ?-HCH, ?-HCH and ?-HCH), endosulfan (?-endosulfan, ?-endosulfan, endosulfan sulphate) and heptachlor were detected in fish at average concentrations ranging from 3.0 to 1235.0 ?g/kg wet wt. These residues were, however, below the detection limit in seawater samples. Significant differences (p < 0.05) in residue levels were also observed across sites, decreasing from Chorkor to Kpone for seven (7) of the residues that were detected in S. aurita. Evaluation of hazard ratios (HRs) and the health risk associated with OC exposure from consumption of sardinellas revealed a probability of adverse health effect due to p,p'-DDT, ?-HCH and heptachlor. Hence, p,p'-DDT, ?-HCH and heptachlor may be of particular health concern. (au)

  16. Detecting Pesticide Residue by Using Modulating Temperature Over a Single SnO2-Based Gas Sensor

    Directory of Open Access Journals (Sweden)

    Zengliang Yu

    2003-09-01

    Full Text Available A new rapid detecting method (called dynamic measurements was reported to detect and distinguish the presence of two pesticide gases in the ambient atmosphere. The method employed only a single SnO2-based gas sensor in a rectangular temperature mode to perform the qualitative analysis of a binary gas mixture (acephate and trichlorphon in air. Polar plots was used for quantitative analysis which the feature extraction was performed by FFT. Experimental results showed that high selectivity of the sensor achieved in the range of 250~3000C and modulating frequency 20mHz, one can easily observe the qualitative difference among the response to pure acephate and trichlorphon gases of the same concentration and to the mixture, and the concentration of pesticide gases can be obtained based on the changes of polar plots.

  17. ANALYTICAL METHODS FOR A NATIONAL STUDY OF CHEMICAL RESIDUES IN FISH - II. PESTICIDES AND POLYCHLORINATED BIPHENYLS

    Science.gov (United States)

    Analytical methods and a quality assurance plan have been developed to determine the concentration of a select group of bioaccumulatable chemicals in fish tissue. he analytes include PCBs and 21 pesticides and industrial chemicals. he methodology has been used to conduct a survey...

  18. Adaptation of TLC detection method for the determination of pesticide residues in grains

    International Nuclear Information System (INIS)

    In this study the retention factor (Rf), relative retention factor (RRf) and minimum detectable quantities (MDQ) of some pesticide active ingredients were determined with various TLC detection methods. The MDQs of the compounds were verified with grain extracts after subjecting them to cleanup procedure with the KL-SX-3 GPC gel chromatograph. The limits of detection (LOD) of compounds were calculated. (author)

  19. QuEChERS-based method for the multiresidue analysis of pesticides in beeswax by LC-MS/MS and GC×GC-TOF.

    Science.gov (United States)

    Niell, Silvina; Cesio, Verónica; Hepperle, Julia; Doerk, Daniela; Kirsch, Larissa; Kolberg, Diana; Scherbaum, Ellen; Anastassiades, Michelangelo; Heinzen, Horacio

    2014-04-30

    The validation of an analytical procedure for the determination of pesticide residues in beeswax, an interesting matrix for environmental pollution monitoring, is presented. Using the QuEChERS template, the impacts of wax particle size, sample amount, and cleanup procedure (water addition, dispersive solid phase extraction, freeze-out, and combinations thereof) on extraction yield and coextractive load were studied. Sample preparation through liquid-liquid partitioning between acetonitrile and melted wax (?80 °C), followed by freeze-out and primary-secondary amine dispersive cleanup, was performed on incurred and pesticide-free samples for 51 residues. Determinations were made through LC-MS/MS and GC×GC-TOF, and the whole procedure was validated. Matrix effects were evaluated, with recoveries between 70 and 120% and RSDs below 20% in almost all cases. LC-MS/MS LOQs ranged from 0.01 to 0.1 mg/kg for most pesticides, but for GC-amenable pesticides, GC×GC-TOF sensitivity was lower (0.1-0.2 mg/kg). This methodology can be applied for routine analysis of pesticide residues in beeswax. PMID:24712416

  20. Organophosphate Pesticide Residues in Drinking Water from Artesian Wells and Health Risk Assessment of Agricultural Communities, Thailand

    OpenAIRE

    Jaipieam, S.; Visuthismajarn, P.; Sutheravut, P.; W Siriwong; Thoumsang, S.; Borjan, M.; Robson, M.

    2009-01-01

    Organophosphate pesticide (OPPs) concentrations in artesian wells located in Thai agricultural and non-agricultural communities were studied during both wet and dry seasons. A total of 100 water samples were collected and subjects were asked to complete a survey. Gas chromatography flame photometric detector was used for OPP analysis. The average OPP concentration in the agricultural communities (0.085 and 0.418 µg/l in dry and wet season) was higher than in the non-agricultural communities (...

  1. 76 FR 61647 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2011-10-05

    ...tandem mass spectrometric detection (LC/MS/MS). The analytical method for sulfentrazone...of the sample prior to analysis by LC/MS/MS GC/electron capture detector...phase extraction prior to analysis by LC/MS/MS. Contact: Laura Nollen,...

  2. Pesticide residues in organic and conventional pasteurized milksResíduos de agrotóxicos em leites pasteurizados orgânicos e convencionais

    Directory of Open Access Journals (Sweden)

    José Laerte Nörnberg

    2013-09-01

    Full Text Available The production of organic milk has been gaining attention due to global market demand for ecological products. However, data about this product are still very limited in Brazil. The aim of this study was to investigate the chemical residue contamination of organic and conventional pasteurized milk sold in three brazilian states. Five certified brands of pasteurized organic milk and five conventional milk brands were analyzed. The samples were subjected to the determination of 88 compounds (79 pesticides and 9 veterinary drugs. For the extraction of the analytes we applied the modified QuEChERS method and for the identification and quantification of the residue we used Liquid Chromatography Coupled to Mass Spectrometry in Series (LC-MS/MS. Results showed that both organic and conventional milk presented only pesticides contamination. Of the 56 samples, five (8.9% contained pesticides residues. Three of them being samples of organic milk; two of which, were positive for clomazone and one for chlorpyrifos. In the conventional milk positive samples, one showed monocrotophos the other presented chlorpyrifos. Although there was a low frequency of positive samples and three of the pesticides detected were below the limit of quantification, there is concern regarding these results since the use of monocrotophos has been prohibited in Brazil, and chlorpyrifos showed concentrations above the maximum limit residue, indicating irregularities. Our results reaffirm the importance of monitoring pesticide programs and chemical contaminants in milk, since milk is one of the most consumed animal food in the country. Moreover, our findings showed that the organic milk production is not in compliance with current legislation. A produção de leite orgânico vem ganhando destaque como resposta à demanda global do mercado por produtos ecológicos. São escassos os dados sobre este produto no Brasil. O objetivo do estudo foi verificar a contaminação por resíduos químicos de leites pasteurizados orgânicos e convencionais comercializados em três Estados brasileiros. Foram analisadas cinco marcas de leite pasteurizado orgânico certificadas e cinco marcas de leite pasteurizado convencional. As amostras foram submetidas à determinação de 88 compostos (79 agrotóxicos e 9 medicamentos veterinários. Para a extração dos analitos aplicou-se o método QuEChERS modificado. Para identificação e quantificação dos resíduos utilizou-se Cromatografia Líquida Acoplada à Espectrometria de Massas em Série (LC-MS/ MS. Os resultados mostraram que tanto o leite orgânico quanto o convencional apresentaram apenas contaminação por agrotóxicos. Das 56 amostras obtidas, cinco (8,9% continham resíduos de agrotóxicos, sendo que destas, três eram amostras de leite orgânico (duas foram positivas para clomazone e uma para clorpirifós. Nas duas amostras positivas do leite convencional, em uma detectou-se monocrotofós e em outra clorpirifós. Embora tenha havido baixa frequência de amostras positivas e três dos agrotóxicos detectados estavam abaixo dos limites de quantificação, os dados encontrados preocupam, pois o monocrotofós teve seu uso proibido no Brasil e o clorpirifós apresentou concentrações acima do limite estabelecido pela legislação vigente, indicando irregularidades. Esses resultados reafirmam a importância dos programas de monitoramento de agrotóxicos e contaminantes químicos no leite, visto que o leite é um dos alimentos de origem animal mais consumidos no país. Também demonstram que a produção orgânica de leite não está em conformidade com a legislação vigente.

  3. Disposal and Treatment Methods for Pesticide Containing Wastewaters: Critical Review and Comparative Analysis

    OpenAIRE

    Al Hattab, Mariam T.; Ghaly, Abdel E.

    2012-01-01

    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 forma...

  4. Efeito do processamento industrial e doméstico de alimentos nos níveis de resíduos de agrotóxicos / Effect of industrial and household food processing on pesticide residues levels

    Directory of Open Access Journals (Sweden)

    Liziara da Costa Cabrera

    2014-11-01

    Full Text Available Resíduos de agrotóxicos em alimentos representam um grande risco para a saúde pública, devido aos efeitos nocivos que podem causar. Devido à utilização de agrotóxicos na produção de alimentos, bem como por meio de contaminação ambiental, os resíduos podem ser encontrados em alimentos frescos, cozidos e processados. A maioria dos alimentos é consumida após o processamento industrial ou doméstico, como a lavagem, remoção da casca, tratamentos térmicos ou esterilização. Vários estudos têm mostrado que estes processos podem, em alguns casos, reduzir os níveis de resíduos. A eficiência de remoção de resíduos depende do processamento envolvido e das propriedades físico-químicas dos agrotóxicos, tais como estabilidade e interação com o alimento. Esta revisão tem como objetivo destacar os resultados de estudos dos efeitos de diversos processos sobre os níveis de resíduos de agrotóxicos em diferentes alimentos, especialmente a eficiência de remoção dos compostos. Esta informação é útil para avaliar a possibilidade de minimizar o risco de exposição do consumidor aos resíduos de agrotóxicos nos alimentos, tornando-se uma importante ferramenta para a segurança alimentar. ---------------------------------------------------------------------------------------------- Pesticide residues in food pose a great risk to public health due to the harmful effects they can cause. Due to the use of pesticides in food production, as well as through environmental contamination, residues can be found in fresh, cooked and processed foodstuffs. Most food is consumed after industrial or household processing, such as washing, peeling, thermal treatments and sterilization. Several studies have shown that these procedures may, in some cases, reduce residue levels. The efficiency of residues removal depends on the processing involved and the physicochemical properties of pesticides, such as stability and interaction with food. This review aims to highlight the results of studies on the effects of various processes on the levels of pesticide residues in different food, especially the removal efficiency of the compounds. This information is useful to assess the possibility of minimizing the risk of consumer exposure to pesticide residues in foods, becoming an important tool for food safety.

  5. 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

    ...Chromotagraphy with tandem Mass Spectrometry (LC/ MS/MS) method. Contact: Andrew Ertman...Adequate enforcement methodology (LC/MS/MS) methods D0603/02 (plants...filtration and finally analysis by a LC/MS/MS method. Contact: Andrew...

  6. Investigation of pesticide residues in apple fruits from conventional and integrated pest management

    OpenAIRE

    Mladenova, Rositsa; Shtereva, Deyana

    2009-01-01

    Abstract This study describes method validation for determination of more than 40 pesticides in apples using GC technique. Target compounds belong to the groups of organochlorine, organophosphorus, carbamates, pyrethroids, triazoles, dicarboximides, strobilurins etc. The sample preparation consists of acetone extraction and subsequent cleanup/concentration by SPE with polymer-based sorbent. Single quadrupole GC-MS operating in SIM mode and electron impact ionization was used for id...

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

    OpenAIRE

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

    2014-01-01

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

  8. Multifamily determination of pesticide residues in soya-based nutraceutical products by GC/MS-MS.

    Science.gov (United States)

    Páleníková, Agneša; Martínez-Domínguez, Gerardo; Arrebola, Francisco Javier; Romero-González, Roberto; Hrouzková, Svetlana; Frenich, Antonia Garrido

    2015-04-15

    An analytical method based on a modified QuEChERS extraction coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) was evaluated for the determination of 177 pesticides in soya-based nutraceutical products. The QuEChERS method was optimised and different extraction solvents and clean-up approaches were tested, obtaining the most efficient conditions with a mixture of sorbents (PSA, C18, GBC and Zr-Sep(+)). Recoveries were evaluated at 10, 50 and 100 ?g/kg and ranged between 70% and 120%. Precision was expressed as relative standard deviation (RSD), and it was evaluated for more than 160 pesticides as intra and inter-day precision, with values always below 20% and 25%, respectively. Limits of detection (LODs) ranged from 0.1 to 10 ?g/kg, whereas limits of quantification (LOQs) from 0.5 to 20 ?g/kg. The applicability of the method was proved by analysing soya-based nutraceuticals. Two pesticides were found in these samples, malathion and pyriproxyfen, at 11.1 and 1.5 ?g/kg respectively. PMID:25466092

  9. Evidence of organochlorine pesticide and polychlorinated biphenyl residues in Slovenian poultry tissues from 1997 to 1999.

    Science.gov (United States)

    Jevsnik, Mojca; Flajs, Vesna Cerkvenik; Doganoc, Darinka Zdenka

    2004-10-01

    The contamination of poultry tissues by total organochlorine (OC) pesticides and polychlorinated biphenyls (PCBs) in Slovenia was examined from a public health perspective. As part of systematic veterinary and sanitary monitoring of foods of animal origin from 1997 to 1999, 87 samples of fat tissue were examined for the presence of alpha-HCH, lindane, heptachlor, and total DDT (plus DDE and DDD) and 88 samples of fat tissue were examined for the presence of total PCBs (sum of PCB congeners). The levels of poultry tissue contamination in six regions of Slovenia were determined. Levels of OC pesticides were below detection limits in 86.2% of analyses performed. Total PCB levels for most samples (59.1%) of poultry fat tissue were in the 0.002- to 0.02-mg/kg range. The level of contamination with OC pesticides and total PCBs in poultry fat tissue was not influenced by the type of poultry and was the highest in samples from industrial areas, which have been ecologically disturbed. All samples met Slovenian and European Union tolerances. PMID:15508653

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

    International Nuclear Information System (INIS)

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

  11. High-throughput simultaneous analysis of pesticides by supercritical fluid chromatography coupled with high-resolution mass spectrometry.

    Science.gov (United States)

    Ishibashi, Megumi; Izumi, Yoshihiro; Sakai, Miho; Ando, Takashi; Fukusaki, Eiichiro; Bamba, Takeshi

    2015-05-13

    Recently, a generally applicable screening method for multiresidue pesticide analysis, which is simple, quick, and accurate and has a reliable performance, is becoming increasingly important for food safety and international trade. This paper proposes a high-throughput screening methodology that enables the detection of multiresidue pesticides using supercritical fluid chromatography coupled to a high-performance benchtop quadrupole Orbitrap mass spectrometry (SFC/Q Exactive) and an automated library-based detection. A total of 444 chemicals covering a wide polarity range (logPow from -4.2 to 7.7) and a wide molecular weight range (from 99.0 to 872.5) were analyzed simultaneously through a combination of high mass resolution (a value of m/?m = 70000), high mass accuracy (<5 ppm) with positive/negative polarity switching, and highly efficient separation by SFC. A total of 373 pesticides were detected in QuEChERS spinach extracts without dispersive solid phase extraction at the 10 ?g kg(-1) level (provisional maximum residue limits in Japan). In conclusion, the developed analytical system is a potentially useful tool for practical multiresidue pesticide screening with high throughput (time for data acquisition, 72 samples per day; and time for data processing of 72 samples, approximately 45 min). PMID:25547162

  12. [Validation study on a method for multiresidue analysis of pesticides in vegetables and fruits with supercritical fluid extraction].

    Science.gov (United States)

    Uranishi, Katsushige; Yamashita, Hirokazu; Yamamoto, Keigo

    2012-01-01

    Supercritical fluid extraction (SFE) was applied to extraction of pesticides from vegetables and fruits. Residues were extracted from homogenized samples mixed with water-absorbent polymer with supercritical carbon dioxide in a stainless steel tube, followed by elution with acetone. Co-extractives were removed by means of mini-column clean-up. Measurement was performed by GC-MS/MS. Calibration was achieved by preparing matrix-matched calibration standards to counteract matrix effects. With the Japanese method validation guideline as a reference, the method was assessed in 5 agricultural products spiked with 334 pesticides at 0.01 and 0.1 µg/g. Compounds at each level were extracted from 2 samples on 5 separate days. The trueness of the method for 189 pesticides in all samples was 70-120%, and the repeatability and within-run reproducibility were also consistent with the guideline. The trueness of the method for the other 71 pesticides was in the range of 50-70%, though the repeatability and within-run reproducibility were satisfactory. This method is available as a multiresidue analysis method for vegetables and fruits. PMID:22450672

  13. Comparison between GC-MS-SIM and GC-ECD for the determination of residues of organochlorine and organophosphorus pesticides in Brazilian citrus essential oils

    Scientific Electronic Library Online (English)

    Andréa A. R., Alves; Michelle J. C., Rezende; Ana M. C., Hovell; Humberto R., Bizzo; Ana Carolina L., Oliveira; Silvana V., Rodrigues; Claudia M., Rezende.

    2012-02-01

    Full Text Available Óleos essenciais cítricos brasileiros (mandarina, laranja, limão, bergamota e tangerina) foram analisados a fim de determinar resíduos de pesticidas organoclorados (aldrin, clordano, dieldrin e dicofol) e organofosforados (clorpirifós metílico, dimetoato, metidationa e paration metílico). Um estudo [...] comparativo entre cromatografia gasosa acoplada a espectrometria de massas em modo de monitoramento seletivo de íons (CG-EM-MSI) e cromatografia gasosa com detector por captura de elétrons (CG-DCE) foi realizado usando extração em fase sólida (EFS) com fase Florisil® para pré-concentração dos pesticidas. A recuperação média dos pesticidas foi de 71 a 83% por CG-EM-MSI e de 99 a 104% por CG-DCE. O limite de quantificação foi de 0,93 a 3,93 mg L-1 por CG-EM-MSI e de 0,09 a 0,12 mg L-1 por CG-DCE. Quinze amostras comerciais de óleos essenciais cítricos brasileiros foram analisadas e seis amostras apresentaram contaminação com valores acima do limite máximo de resíduos (LMR) permitido pelo Codex Alimentarius. Abstract in english Brazilian citrus essential oils (mandarin, orange, lemon, bergamot and tangerine) were analyzed for the determination of pesticides residues of organochlorine (aldrin, chlordane, dieldrin and dicofol) and organophosphorus (methyl chlorpyrifos, dimethoate, methidathion and methyl parathion) . A compa [...] rative study between gas chromatography-mass spectrometry in selective ion monitoring mode (GC-MS-SIM) and gas chromatography-electron capture detector (GC-ECD) was performed using solid phase extraction (SPE) with Florisil® cartridge for the pre-concentration of pesticides. The average recovery of pesticides was from 71 to 83% as determined by GC-MS-SIM analysis and 99 to 104% by GC-ECD. The limit of quantification was from 0.93 to 3.93 mg L-1 in GC-MS-SIM and 0.09 to 0.12 mg L-1 in GC-ECD. Fifteen samples of commercial Brazilian citrus essential oils were analyzed and six samples showed contamination with values above the maximum residue limit (MRL) allowed by the Codex Alimentarius.

  14. Assessment of health risk from organochlorine pesticides residues in high-fat spreadable foods produced in Poland.

    Science.gov (United States)

    Witczak, Agata; Abdel-Gawad, Hassan

    2014-01-01

    Currently, butter and margarine are food products attracting wide customer interest. Every day, consumers around the world buy these products for human consumption. Butter is obtained from milk fat, while margarine is derived from vegetable oils. The content of organochlorine pesticide (OCP) residues was examined in both types of these high fatty products. A gas chromatograph with MSD (HP 5973) detector was used for the determination of pesticides such as ?-HCH, ?-HCH, ?-HCH, DDT, DDD, DDE, aldrin, dieldrin, endrin, heptachlor and heptachlor epoxide. The examined products had diverse concentrations of the analyzed compounds. Visible was the division based on the origin of the product, which might be composed of animal or vegetable fats. The research has revealed the presence of OCP residues in all examined spreads. Quantities of organochlorine compounds did not pose an immediate danger to the consumers' health. Human and environmental health risk assessment was carried out by the estimation of lifetime average daily dose (LADD) and non-carcinogenic health hazard quotient (HQ). Total estimated LADD ranged between 1.3 × 10(-5) and 3.1 × 10(-5) mg kg(-1) d(-1) for butter, and 1.9 × 10(-6) and 4.6 × 10(-6) mg kg(-1) d(-1) for margarine and mix spread. The HQ ranged between 1.1 × 10(-4) and 3.7 × 10(-4) for butter, and 1.4 × 10(-5) and 9.0 × 10(-6) for margarine and mix spread for adults. These estimated HQs were within the safe acceptable limits, indicating a negligible risk to the residents of the study area. PMID:25310807

  15. Report on repetition analyses for pesticide residues: 1988-1995; Rapporto sulle revisioni di analisi per residui di antiparassitari-1995

    Energy Technology Data Exchange (ETDEWEB)

    Di Muccio, A.; Attard Barbini, D.; De Merulis, G.; Vergori, L.; Girolimetti, S.; Sernicola, L.; Dommarco, R. [Ist. Superiore di Sanita`, Rome (Italy). Lab. di Tossicologia Applicata

    1995-12-01

    From 1988 to 1995, 1,254 analyses were carried out on samples of fruits (61%), vegetables (29%), cereals and derived products (3%). The analyses were for 80 different pesticides, of which 51% were fungicides, 31% insecticides, 8% diphenylamine and ethoxiquin (post-harvest antioxidans agents for protection of fruits), and 5% antigermogliants and herbicides. Regions that mostly contributed with samples were: Emilia-Romagna (35%), Piedmont (15%), Liguria (11%), Tuscany (10%). Global rate of confirmation between first analysis and repetition analysis was 64% for all the samples analysed.

  16. Genotoxicity of chlororganic pesticides

    International Nuclear Information System (INIS)

    In Kazakhstan there are the warehouses of the obsolete pesticides and their container which should be buried in special burial grounds or neutralized to minimize dangerous genetic and ecological risks. The results of two yr of research were identification of substances stored in 64 former warehouses of pesticides. 64 former warehouses (in the 10 areas of Almaty oblast) are on distance of 250 km from a large city of Almaty (the former capital of Kazakhstan). A total of 352,6 ton of obsolete pesticides and 250 ton of their container were disposed. We determined the residues of DDT metabolites (dichlorodiphenyltrichloroethane) and HCH isomers (hexachlorocyclohexane) in soil around pesticides warehouses where their concentrations exceed MAC (maximum concentration limit) in tens - hundreds times. To analyze a genotoxicity of chlororganic pesticides we used their concentrations that were found in soil from former warehouses. The analysis of structural mutations of chromosomes was carried out by metaphase method in I mitoses meristem cells of barley seeds (Hordeum vulgare L.). It was ascertained that HCH isomers and DDT metabolites have genotoxic effect exceeding spontaneous mutation in 5-7 times. High contaminations by pesticides on soil around of warehouses and their ability to induce chromosome aberrations in plant cells indicate that warehouses are a new centre of contamination by POP's (proof organic pollutants). (author)

  17. Concentration and loading of pesticide residues in Lake Biwa basin (Japan).

    Science.gov (United States)

    Sudo, Miki; Kunimatsu, Takao; Okubo, Takuya

    2002-01-01

    The concentrations and loading rates of pesticides used in paddy fields were investigated over a period of 5 years in the Seta River, which is the only natural outlet of Lake Biwa. The lake's water catchment area is 3,174 km2, 20% of which contains paddy fields. Water samples were also collected in six rivers flowing into the lake in order to compare the contamination level and concentration profile. The pesticides analyzed were four herbicides (molinate, simetryn, oxadiazon, and thiobencarb), one fungicide (isoprothiolane), and two insecticides (diazinon and fenitrothion). Molinate, simetryn, oxadiazon and isoprothiolane were found at the higher frequencies with maximum concentrations of 1.1, 0.4, 0.1 and 0.5 microg,/l in the effluent river, one or two order of magnitude higher than that of effluent in influent rivers. These peak concentrations were observed during the application period in influent rivers and two or three weeks after that in effluent river. The frequency of occurrence of thiobencarb, diazinon, and fenitrothion was relatively low and their maximum concentrations in the effluent remained below 0.1 microg/l. The decrease of molinate, simetryn and oxadiazon concentrations in the effluent river were approximated by two straight lines plotted on semilogarithmic scale. Increased loading was induced by intense rainfall, which took place during the application period. Simetryn and isoprothiolane persisted in relatively high concentrations through the year were also influenced on its loading by the heavy rainfall in the following months. The percentages of the total amount of pesticides released through Lake Biwa to the basin in downstream were estimated to be 1.3-2.9% for molinate, 5.4-10.0% for simetryn, 0.6-1.3% for oxadiazon, 0.2-0.9% for thiobencarb, 1.8-6.6% for isoprothiolane, 0.3-2.1% for diazinon. and 0% for fenitrothion. PMID:11766809

  18. QuEChERS GC-MS validation and monitoring of pesticide residues in different foods in the tomato classification group.

    Science.gov (United States)

    Ramírez Restrepo, Andrés; Gallo Ortiz, Andrés Fernando; Hoyos Ossa, Duvan Esteban; Peñuela Mesa, Gustavo Antonio

    2014-09-01

    The objective of this study was to validate (SANCO/12495/2011 and NTC-ISO/IEC 17025) multi-residue multi-class methods using QuEChERS sample preparation and GC-MS for the analysis of regulated pesticides in tomatoes (Solanum lycopersicum), tamarillos (Solanum betaceum) and goldenberries (Physalis peruviana). These Latin American products are representative and widely produced in Antioquia (Colombia). Sample preparation followed the UNE-EN 15662 method (150 mg MgSO4, 25mg primary secondary amines and 25mg of octadecylsiloxane for cleanup; graphitized carbon black was added for tomatoes). Extracts were injected using a programmed temperature-vaporizing injector. The residues were validated over a range from 0.02 mg/kg to 0.20 mg/kg, with 24 analytes validated in tomatoes, 33 in tamarillos and 28 in goldenberries. An initial risk assessment was enabled by monitoring 24 samples in the municipalities of El Peñol, Marinilla and San Vicente Ferrer. Risks were found for tomatoes, but no significant risks were found for tamarillos or goldenberries. PMID:24731326

  19. Persistence of pesticide residues in Brazilian soil samples related to organic matter and microbiological activity

    International Nuclear Information System (INIS)

    Studies on the fate of the pesticides lindane, parathion, malathion and carbaryl in two Brazilian soils, one rich (Soil 1), the other poor (Soil 2) in organic matter were made in the laboratory by using gas chromatography and radiometric techniques. In order of decreasing persistence were lindane, parathion and malathion. Lindane was lost faster from Soil 2 than from Soil 1, but malathion was lost more slowly from Soil 2 than Soil 1. Parathion degraded faster to 14CO2 in the soil richer in organic matter. Carbaryl was more completely extracted from autoclaved soils than from non-autoclaved soils. (author)

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

    DEFF Research Database (Denmark)

    Petersen, Annette

    In order to cover more commodity/country-combinations, the Nordic countries (Finland, Sweden, Norway and Denmark) are co-operating in monitoring. In 2008 the countries agreed to monitor samples from Africa. Together the Nordic countries analyzed a total of 623 samples from 18 different countries. Most of the samples came from South Africa (249), followed by Egypt (129), Morocco (92) and Kenya (88). In total 45 different commodities were analyzed, oranges (162) being the largest group, followed by beans with pods (80) and table grapes (71). In the analytical scope 220 to 345 pesticides and metabolites were covered.

  1. Residue analysis of fipronil and difenoconazole in okra by liquid chromatography tandem mass spectrometry and their food safety evaluation.

    Science.gov (United States)

    Hingmire, Sandip; Oulkar, Dasharath P; Utture, Sagar C; Ahammed Shabeer, T P; Banerjee, Kaushik

    2015-06-01

    A liquid chromatography tandem mass spectrometry (LC-MS/MS) based method is reported for simultaneous analysis of fipronil (plus its metabolites) and difenoconazole residues in okra. The sample preparation method involving extraction with ethyl acetate provided 80-107% recoveries for both the pesticides with precision RSD within 4-17% estimated at the limits of quantification (LOQ, fipronil=1ngg(-1), difenoconazole=5ngg(-1)) and higher fortification levels. In field, both the pesticides dissipated with half-life of 2.5days. The estimated pre-harvest intervals (PHI) for fipronil and difenoconazole were 15 and 19.5days, and 4 and 6.5days at single and double dose of field applications, respectively. Decontamination of incurred residues by washing and different cooking treatments was quite efficient in minimizing the residue load of both the chemicals. Okra samples harvested after the estimated PHIs were found safe for human consumption. PMID:25624217

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

    Science.gov (United States)

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

    2010-01-01

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

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

    OpenAIRE

    Balinova, Anna; Mladenova, Rosica; Shtereva, Deyana

    2006-01-01

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

  4. Residuos de plaguicidas organofosforados en cabezuela de brócoli (Brassica oleracea) determinados por cromatografía de gases / Organophosphate pesticide residues in broccoli (Brassica oleracea) heads determined by gas chromatography

    Scientific Electronic Library Online (English)

    Ma. Antonia, PÉREZ; Antonio, SEGURA; Rosario, GARCÍA; Teresa, COLINAS; Mario, PÉREZ; Antonio, VÁZQUEZ; Hermilio, NAVARRO.

    2009-05-01

    Full Text Available Este trabajo documenta el historial de manejo de plagas del cultivo de brócoli y determinación de los residuos de plaguicidas organofosforados mediante cromatografía de gases en cabezuelas listas para su comercialización en 23 sitios de producción. Los resultados indican que las plagas de mayor inci [...] dencia en el brócoli son Brevicoryne brassicae, Trichoplusia ni, Copitarsia consueta, Artogeia rapae, Trialeurodes sp y Bermisia tabaci, reportadas con una frecuencia de 82.5, 80, 80, 70 y 37.7 % por los productores, respectivamente. El control de estas plagas es químico, mediante el uso de productos organofosforados, piretroides y carbamatos, realizando de 1 a 4 aplicaciones durante el ciclo de cultivo. Los residuos de plaguicidas encontrados con mayor frecuencia en el análisis cualitativo son el malatión, el diazinón y el clorfenvinfos, encontrados en 70, 65 y 43 % de las muestras, respectivamente. En cuanto a las concentraciones se encontró: clorfenvinfos, malatión y diazinón con 5.78, 2.67 y 1.16 mg kg-1, seguidos por fentión y etión con concentraciones medias de 0.041 y 0.024 mg kg-1. 87 % de las muestras de brócoli analizadas contienen residuos de al menos un plaguicida organofosforado; sin embargo, las concentraciones encontradas están por debajo de los límites recomendados. Es importante considerar el riesgo sobre la salud humana mediante un análisis del efecto aditivo de los residuos encontrados. Asimismo se recomienda tomar las medidas necesarias para que dichas concentraciones no se vean incrementadas, lo cual puede garantizarse mediante un monitoreo continuo. Abstract in english Handling of pests in broccoli culture was documented; also, the residues of organophosphate pesticides were determined in broccoli heads by means of gas chromatography and capillary column. The results indicate that the pests of most incidence in broccoli are Brevicoryne brassicae, Trichoplusia ni, [...] Copitarsia consueta, Artogeia rapae, Trialeurodes sp and Bermisia tabaci, as reported by producers, with a frequency of 82.5, 80, 80, 70 and 37.7 % respectively. The pest control is chemical in its totality, using organophosphate, pyrethroid and carbamate products, ranging from 1 to 4 applications. The pesticide residues found most frequently in the qualitative analysis are: malathion, diazinon and chlorfenvinphos, in 70, 65 and 43 % of the samples respectively. Regarding concentrations, there were found: chlorfenvinphos, malathion and diazinon with 5.78, 2.67 and 1.16 mg kg-1, followed by fenthion and ethion, with average concentrations of 0.041 and 0.024 mg kg-1. It should be noted that 87 % of the analyzed samples contained organophosphate pesticide residues; even though the concentrations are below the recommended standards, it is still important to assess the risk on human health by means of an analysis of the additive effect of the found residues. Also, it is recommended to take the necessary measures so these concentrations will not increase, which is possible to be guaranteed through continuous monitoring.

  5. Pesticide flow analysis to assess human exposure in greenhouse flower production in Colombia.

    Science.gov (United States)

    Lesmes-Fabian, Camilo; Binder, Claudia R

    2013-04-01

    Human exposure assessment tools represent a means for understanding human exposure to pesticides in agricultural activities and managing possible health risks. This paper presents a pesticide flow analysis modeling approach developed to assess human exposure to pesticide use in greenhouse flower crops in Colombia, focusing on dermal and inhalation exposure. This approach is based on the material flow analysis methodology. The transfer coefficients were obtained using the whole body dosimetry method for dermal exposure and the button personal inhalable aerosol sampler for inhalation exposure, using the tracer uranine as a pesticide surrogate. The case study was a greenhouse rose farm in the Bogota Plateau in Colombia. The approach was applied to estimate the exposure to pesticides such as mancozeb, carbendazim, propamocarb hydrochloride, fosetyl, carboxin, thiram, dimethomorph and mandipropamide. We found dermal absorption estimations close to the AOEL reference values for the pesticides carbendazim, mancozeb, thiram and mandipropamide during the study period. In addition, high values of dermal exposure were found on the forearms, hands, chest and legs of study participants, indicating weaknesses in the overlapping areas of the personal protective equipment parts. These results show how the material flow analysis methodology can be applied in the field of human exposure for early recognition of the dispersion of pesticides and support the development of measures to improve operational safety during pesticide management. Furthermore, the model makes it possible to identify the status quo of the health risk faced by workers in the study area. PMID:23528812

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

    Directory of Open Access Journals (Sweden)

    Claudia R. Binder

    2013-03-01

    Full Text Available Human exposure assessment tools represent a means for understanding human exposure to pesticides in agricultural activities and managing possible health risks. This paper presents a pesticide flow analysis modeling approach developed to assess human exposure to pesticide use in greenhouse flower crops in Colombia, focusing on dermal and inhalation exposure. This approach is based on the material flow analysis methodology. The transfer coefficients were obtained using the whole body dosimetry method for dermal exposure and the button personal inhalable aerosol sampler for inhalation exposure, using the tracer uranine as a pesticide surrogate. The case study was a greenhouse rose farm in the Bogota Plateau in Colombia. The approach was applied to estimate the exposure to pesticides such as mancozeb, carbendazim, propamocarb hydrochloride, fosetyl, carboxin, thiram, dimethomorph and mandipropamide. We found dermal absorption estimations close to the AOEL reference values for the pesticides carbendazim, mancozeb, thiram and mandipropamide during the study period. In addition, high values of dermal exposure were found on the forearms, hands, chest and legs of study participants, indicating weaknesses in the overlapping areas of the personal protective equipment parts. These results show how the material flow analysis methodology can be applied in the field of human exposure for early recognition of the dispersion of pesticides and support the development of measures to improve operational safety during pesticide management. Furthermore, the model makes it possible to identify the status quo of the health risk faced by workers in the study area.

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

    Directory of Open Access Journals (Sweden)

    Rosângela Gorni

    2004-06-01

    Full Text Available Thirty seven benthic samples of the inner shelf area of São Sebastião, Brazil, were collected between April 1994 and August 1998 and analysed for seventeen chlorinated pesticide residues and PCBs congeners. Pesticide residues and PCBs congeners levels were low (ng/g and predominantly found in the crustacean samples. DDE was the most frequently residue with a maximum of 9,7 ng/g followed by HCHs with maximum of 17,1ng/g. As for the PCBs, the heavier congeners predominate: CB 138,153,170, 180 and 183. Maximum total PCBs was 17,4 ug/g in a crab sample. Higher levels of PCBs are related to feeding habits and local inputs of raw sewage or land runoff. Although EPA and FDA (U.S.A below the guidelines for human consumption propose these levels, they do show that even in marine areas without intense agricultural or industrial activities these compounds are present at detectable levels.Trinta e sete amostras de bentos da área interna do Canal de São Sebastião, Brasil, foram coletadas entre Abril de 1994 e Agosto de 1998 e analisadas quanto aos níveis de resíduos de 17 pesticidas organoclorados os congêneres dos PCBs. Os níveis de resíduos de organoclorados e PCBs foram baixos( ng/g e encontrados com maior freqüência nas amostras de crustáceos. DDE foi o resíduo de pesticida encontrado com mais freqüência apresentado um máximo de 9,7 ng/g seguido dos isômeros de HCHs com um máximo de 17,1 ng/g. No caso dos PCBs os congêneres mais pesados foram os predominantes: CB 138, 153, 170, 180 e 183. O valor máximo de PCBs totais foi de 17,4 ug/g numa amostra de crustáceo. Níveis maiores de PCBs estão associados aos hábitos alimentares e introduções pontuais de esgotos e água de drenagem urbana. Apesar dos níveis observados estarem abaixo dos recomendados para consumo humano pela EPA e da FDA( U.S.A ,eles demonstram que mesmo em área marinhas costeiras sem agricultura intensiva ou atividades industriais de porte , estes compostos orgânicos persistentes sintéticos ( POPS estão presentes em níveis mensuráveis.

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

    Scientific Electronic Library Online (English)

    Rosângela, Gorni; Rolf Roland, Weber.

    2004-06-01

    Full Text Available Trinta e sete amostras de bentos da área interna do Canal de São Sebastião, Brasil, foram coletadas entre Abril de 1994 e Agosto de 1998 e analisadas quanto aos níveis de resíduos de 17 pesticidas organoclorados os congêneres dos PCBs. Os níveis de resíduos de organoclorados e PCBs foram baixos( ng/ [...] g) e encontrados com maior freqüência nas amostras de crustáceos. DDE foi o resíduo de pesticida encontrado com mais freqüência apresentado um máximo de 9,7 ng/g seguido dos isômeros de HCHs com um máximo de 17,1 ng/g. No caso dos PCBs os congêneres mais pesados foram os predominantes: CB 138, 153, 170, 180 e 183. O valor máximo de PCBs totais foi de 17,4 ug/g numa amostra de crustáceo. Níveis maiores de PCBs estão associados aos hábitos alimentares e introduções pontuais de esgotos e água de drenagem urbana. Apesar dos níveis observados estarem abaixo dos recomendados para consumo humano pela EPA e da FDA( U.S.A) ,eles demonstram que mesmo em área marinhas costeiras sem agricultura intensiva ou atividades industriais de porte , estes compostos orgânicos persistentes sintéticos ( POPS) estão presentes em níveis mensuráveis. Abstract in english 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 c [...] rustacean samples. DDE was the most frequently residue with a maximum of 9,7 ng/g followed by HCHs with maximum of 17,1ng/g. As for the PCBs, the heavier congeners predominate: CB 138,153,170, 180 and 183. Maximum total PCBs was 17,4 ug/g in a crab sample. Higher levels of PCBs are related to feeding habits and local inputs of raw sewage or land runoff. Although EPA and FDA (U.S.A) below the guidelines for human consumption propose these levels, they do show that even in marine areas without intense agricultural or industrial activities these compounds are present at detectable levels.

  9. Residual gas analysis in ISX-A

    Energy Technology Data Exchange (ETDEWEB)

    Simpkins, J. E.; Colchin, R. J.; Overbey, D. R.

    1978-01-01

    A computer-controlled mass analyzer was utilized to observe the residual gases in the ISX-A tokamak. This residual gas analysis (RGA) system enabled time resolved measurements of preselected m/e peak heights to be made during and after tokamak discharges. Routine mass scans were also made and displayed in the form of semilogarithmic plots of partial pressure (torr) versus m/e. Wall conditioning of the stainless steel torus consisted of hydrogen discharge cleaning and titanium gettering, which ultimately produced gage pressures on the order of 10/sup -8/ and 10/sup -9/ torr, respectively. The dominant plasma impurities, carbon and oxygen, were observed by the RGA as light hydrocarbons and water vapor. Entrapment of deuterium by the walls was investigated by monitoring the residual D/sub 2/ content after the working gas was changed to H/sub 2/. The effective nuclear charge (Z/sub eff/) was found to be proportional to the residual contaminants measured by the RGA immediately following a discharge.

  10. Determination of pesticide residues in sugarcane honey by QuEChERS, and liquid chromatography

    Scientific Electronic Library Online (English)

    Maicon R. F., Sampaio; Débora, Tomasini; Liziane V., Cardoso; Sergiane S., Caldas; Ednei G., Primel.

    2012-02-01

    Full Text Available Neste trabalho, é descrito um método para determinação dos agrotóxicos 2,4-D, diurom e fipronil em mel de cana-de-açúcar. O método QuEChERS foi empregado para extração e a quantificação foi realizada por cromatografia líquida de alta eficiência acoplada ao detector por arranjo de diodos (HPLC-DAD) e [...] cromatografia líquida acoplada à espectrometria de massas sequencial com fonte de ionização por eletronebulização(LC-ESI-MS/MS). Após a otimização dos parâmetros de extração e determinação dos agrotóxicos, o método foi validado avaliando-se a curva analítica, linearidade, limites de detecção e quantificação, precisão (repetibilidade) e exatidão (recuperação). Devido à ocorrência do efeito de matriz, a quantificação foi realizada com os padrões analíticos preparados no extrato branco da matriz. O método apresentou limites de detecção na faixa de 0,016-0,1 mg kg-1 por HPLC-DAD e de 0,00016-0,0008 mg kg-1 por LC-ESI-MS/MS. O método foi empregado na determinação de agrotóxicos em mel de cana-de-açúcar. Abstract in english This paper aims at describing a method to determine the pesticides 2,4-D, diuron and fipronil in sugarcane honey. The QuEChERS method was employed for extraction and the quantification was carried out by high performance liquid chromatography coupled with diode array detector (HPLC-DAD) and liquid c [...] hromatography-tandem mass spectrometry with electrospray ionization source (LC-ESI-MS/MS). After the optimization of the extraction parameters and the determination of the pesticides, the method was validated by evaluating the analytical curve, linearity, limits of detection and quantification, precision (repeatability) and accuracy (recovery). Due to the occurrence of matrix effect, the quantification was performed using the analytical standards prepared in the blank matrix extract. The method provided limits of detection in the range of 0.016-0.1 mg kg-1 by HPLC-DAD and 0.00016-0.0008 mg kg-1 by LC-ESI-MS/MS. The method was applied to the determination of pesticides in sugarcane honey.

  11. New approaches to uncertainty analysis for use in aggregate and cumulative risk assessment of pesticides.

    Science.gov (United States)

    Kennedy, Marc C; van der Voet, Hilko; Roelofs, Victoria J; Roelofs, Willem; Glass, C Richard; de Boer, Waldo J; Kruisselbrink, Johannes W; Hart, Andy D M

    2015-05-01

    Risk assessments for human exposures to plant protection products (PPPs) have traditionally focussed on single routes of exposure and single compounds. Extensions to estimate aggregate (multi-source) and cumulative (multi-compound) exposure from PPPs present many new challenges and additional uncertainties that should be addressed as part of risk analysis and decision-making. A general approach is outlined for identifying and classifying the relevant uncertainties and variabilities. The implementation of uncertainty analysis within the MCRA software, developed as part of the EU-funded ACROPOLIS project to address some of these uncertainties, is demonstrated. An example is presented for dietary and non-dietary exposures to the triazole class of compounds. This demonstrates the chaining of models, linking variability and uncertainty generated from an external model for bystander exposure with variability and uncertainty in MCRA dietary exposure assessments. A new method is also presented for combining pesticide usage survey information with limited residue monitoring data, to address non-detect uncertainty. The results show that incorporating usage information reduces uncertainty in parameters of the residue distribution but that in this case quantifying uncertainty is not a priority, at least for UK grown crops. A general discussion of alternative approaches to treat uncertainty, either quantitatively or qualitatively, is included. PMID:25688423

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

    Science.gov (United States)

    Sun, Xia; Wang, Xiangyou; Jia, Chuandong

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

  13. Persistence of organophosphorus pesticides in aquatic environments. Coordinated programme on isotope-tracer-aided research and monitoring on agricultural residue - biological interactions in aquatic environment

    International Nuclear Information System (INIS)

    A radiometric enzymic assay method was developed for quick measuring of organophosphorous insecticides in water samples. All steps of the assay procedure were carried out in scintillation vials. 50 ?l enzyme solution (acetylcholinesterase of electric eel) and 50 ?l buffer pH 7 were pipetted into the vial followed by 100 ?l of water sample or aqueous solution of the insecticide and the mixture was incubated for 60 minutes. 50 ?l 3H-acetylcholine were added to the vial and the enzymic reaction stopped after 10 minutes by adding 200 ?l buffer solution pH 2.5. 10 ml scintillation cocktail were then added and after shaking and 30 minutes standing the radioactivity was determined in a liquid scintillation spectrometer. Acetylcholine remained in the water phase while 3H-acetic acid released in enzymic hydrolysis may be extracted by an organic solvent. By this method, not only the parent compound but also some of its degradation products, which possess some anticholinesteratic activity can be measured. The method is suitable for combination with thin-layer chromatography for identification purposes. Using this method, we studied the degradation of the organophosphorous insecticides malathion, parathion, DDVP and imidan. The degradation in distilled water and natural water was compared. For example, the half-time of malathion in distilled water at room temperature was 6 days while in natural water (Danube river) it was 4 hours. The degradation processes were also studied in model systems containing sediment and water. Degradation was faster in models containing solid particles than in filtered water. The radiometric enzymic method was tested as analytical procedure for residue monitoring. Since 1978 a residue monitoring programme was in progress in the Danube river near Budapest. Occasionally high residue levels were detected in spring and early summer. The radiometric enzymic method has proved to be a useful analytical method for anticholinesterase pesticides in water samples. The method allows analysis directly from water samples without extraction or concentration

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

    International Nuclear Information System (INIS)

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

  15. Large volume injection of water in gas chromatography–mass spectrometry using the Through Oven Transfer Adsorption Desorption interface: Application to multiresidue analysis of pesticides.

    Science.gov (United States)

    Toledano, Rosa M; Cortés, Jose M; Andini, Juan C; Villén, Jesús; Vázquez, Ana

    2010-07-01

    In the present work, the potential of the Through Oven Transfer Adsorption Desorption (TOTAD) interface for the large volume injection (LVI) of aqueous samples in gas chromatography (GC) using a mass spectrometry (MS) detector is demonstrated. To this end, a new method for the determination of pesticides in water is presented, being the first developed method in which injection of large amounts of polar solvents using the TOTAD interface and an MS detector are combined, is applied to the determination of pesticides in water. Water samples, as large as 5 ml, were directly injected into a capillary GC. No sample pre-treatment step other than simple filtration was needed. The TOTAD interface allows the introduction of several millilitres of water, while maintaining good chromatographic characteristics. The water is almost entirely eliminated, so that LVI of aqueous samples and an MS detector can be used without problems. Organophosphorus, organochlorine, and triazine pesticides were determined in one run. Calibration curves were linear in the range tested and the sensitivity achieved injecting 5 ml of water sample was sufficient for most of the target pesticides but not for all of them. Sensitivity of the analysis can be improved by increasing the sample volume. No variability was observed in the retention times and relative standard deviations from absolute peak areas were good, considering that they corresponded to the overall analysis. The method was applied to the analysis of pesticide residues in real water samples. PMID:20605155

  16. Pesticides for Apicultural and/or Agricultural Application Found in Belgian Honey Bee Wax Combs.

    Science.gov (United States)

    Ravoet, Jorgen; Reybroeck, Wim; de Graaf, Dirk C

    2015-05-01

    In a Belgian pilot study honey bee wax combs from ten hives were analyzed on the presence of almost 300 organochlorine and organophosphorous compounds by LC-MS/MS and GC-MS/MS. Traces of 18 pesticides were found and not a single sample was free of residues. The number of residues found per sample ranged from 3 to 13, and the pesticides found could be categorized as (1) pesticides for solely apicultural (veterinary) application, (2) pesticides for solely agricultural (crop protection) application, (3) pesticides for mixed agricultural and apicultural (veterinary) application. The frequencies and quantities of some environmental pollutants bear us high concerns. Most alarming was the detection of lindane (gamma-HCH) and dichlorodiphenyltrichloroethane (including its breakdown product dichlorodiphenyldichloroethylene), two insecticides that are banned in Europe. The present comprehensive residue analysis, however, also reveals residues of pesticides never found in beeswax before, i.e. DEET, propargite and bromophos. PMID:25749505

  17. Pesticide residue determination in groundwater using solid-phase extraction and high-performance liquid chromatography with diode array detector and liquid chromatography-tandem mass spectrometry

    Scientific Electronic Library Online (English)

    Sergiane S., Caldas; Adriana, Demoliner; Fabiane P., Costa; Marcelo G. M., D' Oca; Ednei G., Primel.

    Full Text Available Resíduos de quatro agrotóxicos foram determinados durante um ano em águas de poços de uma área agrícola no Sul do Brasil. Os métodos para a separação, identificação e quantificação dos compostos incluíram cromatografia líquida de alta eficiência com detecção por arranjo de diodos (HPLC-DAD) e cromat [...] ografia líquida acoplada à espectrometria de massas (LC-ESI-MS/MS). Uma etapa de pré-concentração baseada na extração em fase sólida com cartuchos de 200 mg de C18 foi realizada. Todos os parâmetros analíticos ficaram de acordo com os limites sugeridos para a validação de métodos cromatográficos. Os limites de quantificação para o método, considerando um fator de pré-concentração de 250 vezes, foram 0,2 ?g L-1 para todos os analitos por HPLC-DAD, 4,0 ng L-1 para o clomazona, carbofurano e tebuconazol e 40,0 ng L-1 para o 2,4-D por LC-ESI-MS/MS. Nas amostras de águas subterrâneas, o 2,4-D não foi detectado e o carbofurano, clomazona e tebuconazol apresentaram concentrações que variaram entre 0,25 e 10,40 ?g L-1, 0,20 e 0,82 ?g L-1, e 0,20 e 4,16 ?g L-1, respectivamente. Os métodos mostraram-se adequados para a determinação de agrotóxicos em águas subterrâneas. Abstract in english Residues of four pesticides in groundwaters were surveyed during one year in an agricultural area in southern Brazil. The methods for separation, identification and quantification of the compounds included high-performance liquid chromatography with diode array detection (HPLC-DAD) and liquid chroma [...] tography with electrospray interface tandem mass spectrometry (LC-ESI-MS/MS). A pre-concentration step based on solid-phase extraction with 200 mg C18 cartridges was applied. All the analytical parameters were within the limits suggested for the validation of chromatographic methods. The LOQs for the methods, considering the 250-fold pre-concentration step, were 0.2 ?g L-1 for all pesticides by HPLC-DAD, 4.0 ng L-1 for clomazone, carbofuran and tebuconazole and 40.0 ng L-1 for 2,4-D by LC-ESI-MS/MS. In groundwater samples, 2,4-D was not detected, and carbofuran, clomazone and tebuconazole were detected in concentrations ranging from 0.25 to 10.40 ?g L-1, from 0.20 to 0.82 ?g L-1 and from 0.20 to 4.16 ?g L-1, respectively. The methods proved to be adequate for the analysis of pesticides in groundwaters.

  18. Liquid chromatography-electrospray ionization tandem mass spectrometry and dynamic multiple reaction monitoring method for determining multiple pesticide residues in tomato.

    Science.gov (United States)

    Andrade, G C R M; Monteiro, S H; Francisco, J G; Figueiredo, L A; Botelho, R G; Tornisielo, V L

    2015-05-15

    A quick and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method, using dynamic multiple reaction monitoring and a 1.8-?m particle size analytical column, was developed to determine 57 pesticides in tomato in a 13-min run. QuEChERS (quick, easy, cheap, effective, rugged, and safe) method for samples preparations and validations was carried out in compliance with EU SANCO guidelines. The method was applied to 58 tomato samples. More than 84% of the compounds investigated showed limits of detection equal to or lower than 5 mg kg(-1). A mild (50%) matrix effect was observed for 72%, 25%, and 3% of the pesticides studied, respectively. Eighty-one percent of the pesticides showed recoveries ranging between 70% and 120%. Twelve pesticides were detected in 35 samples, all below the maximum residue levels permitted in the Brazilian legislation; 15 samples exceeded the maximum residue levels established by the EU legislation for methamidophos; and 10 exceeded limits for acephate and four for bromuconazole. PMID:25577051

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

    Science.gov (United States)

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

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

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

    Directory of Open Access Journals (Sweden)

    Awang Bono

    2007-01-01

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

  1. Analysis of organophosphorus pesticides using FT-NMR

    International Nuclear Information System (INIS)

    A rapid and highly selective method of the identification of 23 kinds of organophosphorus pesticides was develop by using 31P FT-NMR with 1H complete decoupling method. Chemical shifts referenced by 85 % H3PO4 were within -4 to 100 ppm, and there was no overlapping among the organophosphorus pesticides used in this experiment. (author)

  2. Carcinogenic and non-carcinogenic risk of organochlorine pesticide residues in processed cereal-based complementary foods for infants and young children in Ghana.

    Science.gov (United States)

    Akoto, Osei; Oppong-Otoo, John; Osei-Fosu, Paul

    2015-08-01

    Fourteen organochlorine pesticides (OCPs) residues were analyzed in 10 brands of processed cereal-based complementary foods with the aim of assessing the health risk to infants and young children. The QuEChERS method was used for extraction and clean-up of pesticide residues. Subsequent detection and quantification were done using GC with ECD and PFPD. Levels of p,p'-DDE, dieldrin, ?-endosulfan, ?-HCH, and ?-HCH detected in the processed cereal-based complementary food were higher than their respective MRL. The mean estimated daily intakes of OCPs in infants were significantly higher than that of young children. Exposure levels of heptachlor and dieldrin were higher than their respective ADI's. Their HIs recorded were greater than 1 indicating the possibility of adverse health effect on consumers. Hazard ratio for carcinogenic risk posed by ?-HCH, dieldrin, heptachlor, ?-HCH and ?-chlordane were greater than 1. This result raises concerns of possible carcinogenicity for infants and young children. PMID:25889270

  3. Simultaneous determination of eight pesticide residues in coconut using MSPD and GC/MS.

    Science.gov (United States)

    Silva, Maria Geovânia Dantas; Aquino, Adriano; Dórea, Haroldo Silveira; Navickiene, Sandro

    2008-07-30

    A simple and effective extraction method based on matrix solid-phase dispersion (MSPD) was developed to determine dimethoate, malathion, lufenuron, carbofuran, 3-hydroxycarbofuran, thiabendazole, difenoconazole and trichlorfon in coconut pulp using gas chromatography-mass spectrometry with selected ion monitoring (GC/MS, SIM). Different parameters of the method were evaluated, such as type of solid-phase (C(18), alumina, silica-gel and Florisil), the amount of solid-phase and eluent (dichloromethane, acetone, ethyl acetate, acetonitrile, n-hexane and n-hexane:ethyl acetate (1:1, v/v)). The best results were obtained using 0.5 g of coconut pulp, 1.0 g of C(18) as dispersant sorbent, 1.0 g of Florisil as clean-up sorbent and acetonitrile saturated with n-hexane as eluting solvent. The method was validated using coconut pulp samples fortified with pesticides at different concentration levels (0.25-1.0 mg kg(-1)). Average recoveries (four replicates) ranged from 70.1% to 98.7%, with relative standard deviations between 2.7% and 14.7%, except for lufenuron and difenoconazole, for which recoveries were 47.2% and 48.2%, respectively. Detection and quantification limits for coconut pulp ranged from 0.02 to 0.17 mg kg(-1) and from 0.15 to 0.25 mg kg(-1), respectively. PMID:18585339

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

    Directory of Open Access Journals (Sweden)

    THOMMANDRU RAVEENDRANATH BAB

    2014-02-01

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

  5. Screening of pesticide residues in soil and water samples from agricultural settings

    OpenAIRE

    Djouaka Rousseau F; Akogbéto Martin C; Kindé-Gazard Dorothée A

    2006-01-01

    Abstract Background The role of agricultural practices in the selection of insecticide resistance in malaria vectors has so far been hypothesized without clear evidence. Many mosquito species, Anopheles gambiae in particular, lay their eggs in breeding sites located around agricultural settings. There is a probability that, as a result of farming activities, insecticide residues may be found in soil and water, where they exercise a selection pressure on the larval stage of various populations...

  6. A simple multi-residue method for the determination of pesticides in fruits and vegetables using a methanolic extraction and ultra-high-performance liquid chromatography-tandem mass spectrometry: optimization and extension of scope.

    Science.gov (United States)

    Hanot, V; Goscinny, S; Deridder, M

    2015-03-01

    In 2004, a new multi-residue pesticides method had been published using methanol as extraction solvent. Our goal for this study was to optimize the analytical scheme while extending the compound scope from 19 to 200 pesticides. The main changes from the original method take place at the sample extraction and processing with a special attention to make the overall method fit for routine analysis with minimal cost. Hence, after a quick Ultra-Turrax homogenization with a methanolic solution, the sample is simply diluted before the separation and detection by ultra-high-performance liquid chromatography and MS/MS detection for quantitative and confirmatory purposes. The performance of the method including limits of quantification (LOQs), linearity, matrix effect, precision was evaluated during validation in accordance with the European Union SANCO/12571/2013 regulatory guidelines. Two representative matrices, lettuce and orange, were selected and fortified at two concentration levels for these experiments. At the LOQ and ten times the LOQ, recoveries of the analytes were mostly within 70-120%, with coefficients of variation lower than 25% in intra-day repeatability conditions. In addition to being simple and fast, these results demonstrate the suitability of the optimized method for the analysis of large scope pesticides in routine laboratories. PMID:25660522

  7. Scientific support for preparing an EU position in the 46th Session of the Codex Committee on Pesticide Residues (CCPR)

    OpenAIRE

    European Food Safety Authority

    2014-01-01

    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, tolfenpyra...

  8. Scientific support for preparing an EU position for the 45th Session of the Codex Committee on Pesticide Residues (CCPR)

    OpenAIRE

    European Food Safety Authority

    2013-01-01

    In accordance with Article 43 of Regulation (EC) No 396/2005, EFSA received a request from the European Commission to provide support for the preparation of the EU position for the 45th session of the Codex Committee on Pesticide Residues (CCPR). In 2012, JMPR evaluated 12 active substances regarding the setting of toxicological reference values to be used in consumer risk assessment, 7 new compounds (ametoctradin, chlorfenapyr, dinotefuran, fluxapyroxad, MCPA, picoxystrobin, sedaxane) and 4 ...

  9. A novel optimised and validated method for analysis of multi-residues of pesticides in fruits and vegetables by microwave-assisted extraction (MAE)-dispersive solid-phase extraction (d-SPE)-retention time locked (RTL)-gas chromatography-mass spectrometry with Deconvolution reporting software (DRS).

    Science.gov (United States)

    Satpathy, Gouri; Tyagi, Yogesh Kumar; Gupta, Rajinder Kumar

    2011-08-01

    A rapid, effective and ecofriendly method for sensitive screening and quantification of 72 pesticides residue in fruits and vegetables, by microwave-assisted extraction (MAE) followed by dispersive solid-phase extraction (d-SPE), retention time locked (RTL) capillary gas-chromatographic separation in trace ion mode mass spectrometric determination has been validated as per ISO/IEC: 17025:2005. Identification and reporting with total and extracted ion chromatograms were facilitated to a great extent by Deconvolution reporting software (DRS). For all compounds LOD were 0.002-0.02mg/kg and LOQ were 0.025-0.100mg/kg. Correlation coefficients of the calibration curves in the range of 0.025-0.50mg/kg were >0.993. To validate matrix effects repeatability, reproducibility, recovery and overall uncertainty were calculated for the 35 matrices at 0.025, 0.050 and 0.100mg/kg. Recovery ranged between 72% and 114% with RSD of <20% for repeatability and intermediate precision. The reproducibility of the method was evaluated by an inter laboratory participation and Z score obtained within ±2. PMID:25214130

  10. 75 FR 69005 - Flumioxazin; Pesticide Tolerances

    Science.gov (United States)

    2010-11-10

    ...Mail: Office of Pesticide Programs (OPP...the filing of a pesticide petition (PP...or on commodity fish, freshwater at...legal limit for a pesticide chemical residue in or on...Flumioxazin. Human Health Risk...

  11. 2011 EPA Pesticide General Permit (PGP)

    U.S. Environmental Protection Agency — The 2011 EPA Pesticide General Permit (PGP) covers discharges of biological pesticides, and chemical pesticides that leave a residue, in areas where EPA is the...

  12. Pesticide exposure - Indian scene

    International Nuclear Information System (INIS)

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

  13. Assessment of pesticide residues and gene expression in common carp exposed to atrazine and chlorpyrifos: Health risk assessments.

    Science.gov (United States)

    Xing, Houjuan; Wang, Zhilei; Wu, Hongda; Zhao, Xia; Liu, Tao; Li, Shu; Xu, Shiwen

    2015-03-01

    This study assessed the impacts of atrazine (ATR), chlorpyrifos (CPF) and combined ATR/CPF exposure on the kidney of common carp (Cyprinus carpio L.). The carp were sampled after a 40-d exposure to CPF and ATR, individually or in combination, followed by a 40-d recovery to measure the expression levels of heat shock proteins genes (HSP60, HSP70 and HSP90) and pesticide residues in the kidney tissue. The results revealed that the mRNA and protein levels of HSP60, HSP70 and HSP90 were induced in the kidney of common carp by ATR, CPF, and ATR/CPF mixture. The accumulated amounts of ATR, CPF, and their metabolites in the kidney tissues exhibited dose-dependency. These results exhibited that increasing concentration of ATR and CPF in the environment causes considerable stress for common carp, suggesting that the expression levels of HSP60, HSP70 and HSP90 may act as potential biomarkers for assessing the environmental ATR and CPF risk for carp. PMID:25568939

  14. 76 FR 5711 - Bispyribac-sodium; Pesticide Tolerances

    Science.gov (United States)

    2011-02-02

    ...the pesticide chemical residue in...exposure to the pesticide chemical residue...to any other chemical that causes...Bispyribac-sodium; Human-Health Risk Assessment...Freshwater Fish'' at page...Concern Once a pesticide's...

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

    Science.gov (United States)

    Golge, Ozgur; Kabak, Bulent

    2015-06-01

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

  16. Principais técnicas de preparo de amostra para a determinação de resíduos de agrotóxicos em água por cromatografia líquida com detecção por arranjo de diodos e por espectrometria de massas / Modern techniques of sample preparation for pesticide residues determination in water by liquid chromatography with detection by diode array and mass spectrometry

    Scientific Electronic Library Online (English)

    Sergiane Souza, Caldas; Fábio Ferreira, Gonçalves; Ednei Gilberto, Primel; Osmar Damian, Prestes; Manoel Leonardo, Martins; Renato, Zanella.

    1604-16-01

    Full Text Available [...] Abstract in english The determination of pesticide residues in water samples by Liquid Chromatography require sample preparation for extraction and enrichment of the analytes with the minimization of interferences to achieve adequate detection limits. The Solid Phase Extraction (SPE), Solid Phase Microextraction (SPME) [...] , Stir Bar Sorptive Extraction (SBSE) and Dispersive Liquid-Liquid Microextraction (DLLME) techniques have been widely used for extraction of pesticides in water. In this review, the principles of these sample preparation techniques associated with the analysis by Liquid Chromatography with Diode Array Detection (LC-DAD) or Mass Spectrometry (LC-MS) are described and an overview of several applications were presented and discussed.

  17. Principais técnicas de preparo de amostra para a determinação de resíduos de agrotóxicos em água por cromatografia líquida com detecção por arranjo de diodos e por espectrometria de massas Modern techniques of sample preparation for pesticide residues determination in water by liquid chromatography with detection by diode array and mass spectrometry

    Directory of Open Access Journals (Sweden)

    Sergiane Souza Caldas

    2011-09-01

    Full Text Available The determination of pesticide residues in water samples by Liquid Chromatography require sample preparation for extraction and enrichment of the analytes with the minimization of interferences to achieve adequate detection limits. The Solid Phase Extraction (SPE, Solid Phase Microextraction (SPME, Stir Bar Sorptive Extraction (SBSE and Dispersive Liquid-Liquid Microextraction (DLLME techniques have been widely used for extraction of pesticides in water. In this review, the principles of these sample preparation techniques associated with the analysis by Liquid Chromatography with Diode Array Detection (LC-DAD or Mass Spectrometry (LC-MS are described and an overview of several applications were presented and discussed.

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

    International Nuclear Information System (INIS)

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

  19. Using Spatial Structure Analysis of Hyperspectral Imaging Data and Fourier Transformed Infrared Analysis to Determine Bioactivity of Surface Pesticide Treatment

    OpenAIRE

    Christian Nansen; Noureddine Abidi; Amelia Jorge Sidumo; Ali Hosseini Gharalari

    2010-01-01

    Many food products are subjected to quality control analyses for detection of surface residue/contaminants, and there is a trend of requiring more and more documentation and reporting by farmers regarding their use of pesticides. Recent outbreaks of food borne illnesses have been a major contributor to this trend. With a growing need for food safety measures and “smart applications” of insecticides, it is important to develop methods for rapid and accurate assessments of surface residues on f...

  20. [Determination of 61 organophosphorous pesticide residues in fruits, vegetables, milk, vegetable oils and animal muscles by dispersive solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Ye, Ruihong; Su, Jianfeng

    2011-07-01

    A dispersive solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of 61 organophosphorous pesticide residues in fruits, vegetables, milk, vegetable oils and animal muscles. The fruit, vegetable and milk samples were extracted with acetonitrile and separated with salting out method; vegetable oil samples were dissolved by n-hexane, and extracted with acetonitrile; animal muscle samples were extracted with acetonitrile-water assisted by n-hexane and separated with salting out method. And then the supernatants were purified using dispersive solid-phase extraction (C18 and primary secondary amine powder) prior to the UPLC-MS/MS analysis. The analytes were indentified in positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode. The matrix-matched external standard calibration curves were used for quantitative analysis. Under the optimal conditions, the detection limits (S/N > or = 10) of the method were 0.01 mg/kg. The recoveries were 62.8%-107%, and the relative standard deviations (RSDs) were in the range of 4.2%-19%. The method has the advantages of easy, fast, and more sensitive, and can meet the requirement of the determination of organophosphorous pesticide residues in the foods. PMID:22097787

  1. Reversed phase liquid chromatography trace analysis of pesticides in soil by on-column sample pumping large volume injection and UV detection.

    Science.gov (United States)

    Hutta, Milan; Chalányová, Mária; Halko, Radoslav; Góra, Róbert; Dokupilová, Svetlana; Rybár, Ivan

    2009-06-01

    The idea of utilization of one hydraulic line of a common commercial HPLC pump for direct on-column sample pumping injection of large sample volumes, 20 mL, was further investigated with the aim to develop multicomponent pesticides trace residues HPLC method in gram soil samples. Target pesticides group involve asulam, atrazine, 2,4-D, PCA, propazine, simazine, 4-chloro-2-methylphenoxyacetic acid, 2-(4-chloro-2-tolyloxy) propionic acid, chlortoluron, metoxuron, epoxiconazole. The results proved the applicability of this approach in experiments with mixtures of analytes at low ng/mL levels. Analysis of 20 mL of soil leachates and extracts of fortified soil samples containing these pesticides at the 10-50 ng/g level (in dry soil) revealed good figures of merit, also in the presence of large excess of humics. LODs achieved by detection at 220 nm evaluated from calibration runs of spiked soil extracts by Hubaux et al. method ranged from 5-12 ng per injected volume. For 20 mL large volume injection it represents 0.25-0.6 ng/mL of diluted soil extract, or 2.5-6 ng/mL of crude extract, or 6-5 ng/g dry soil. Recoveries of pesticides at concentration levels approaching half of maximum allowable concentration of pesticides in soil (100 ng/g) ranged from 85 to 98% with acceptable reproducibility, except asulam and metoxuron. PMID:19548212

  2. Use of ammonium formate in QuEChERS for high-throughput analysis of pesticides in food by fast, low-pressure gas chromatography and liquid chromatography tandem mass spectrometry

    Science.gov (United States)

    The “quick, easy, cheap, effective, rugged, and safe” (QuEChERS) approach to sample preparation is widely applied in pesticide residue analysis, but the use of magnesium sulfate for salting out in the method is not ideal for mass spectrometry. In this study we developed and evaluated three new diffe...

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

    OpenAIRE

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

    2013-01-01

    The detection and quantification of different pesticides in the goat milk samples collected from different localities of Faisalabad, Pakistan was performed by HPLC using solid phase microextraction. The analysis showed that about 50% milk samples were contaminated with pesticides. The mean+/-SEM levels (ppm) of cyhalothrin, endosulfan, chlorpyrifos and cypermethrin were 0.34+/-0.007, 0.063+/-0.002, 0.034+/-0.002 and 0.092+/-0.002, respectively; whereas, methyl parathion was not detected in an...

  4. [Determination of seven pesticide residues in bamboo shoots by high performance liquid chromatography-tandem mass spectrometry coupled with solid-phase extraction].

    Science.gov (United States)

    Ding, Ming; Zhong, Donglian; Tang, Fubin; Fang, Wei

    2013-02-01

    A simple and efficient method based on solid-phase extraction (SPE) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for the determination of butylene fipronil, chlorpyrifos, chlorantraniliprole, fipronil, imidacloprid, indoxacarb and phoxim residues in bamboo shoots. The sample was extracted with acetonitrile and purified by a primary secondary amine (PSA) solid-phase extraction cartridge. The detection of targets was performed by HPLC-MS/MS with multiple reaction monitoring (MRM) mode. All the seven pesticides were completely separated in 15 min with an excellent linear relationship. The limits of detection and the limits of quantification for the seven pesticides were 0.02-0.5 microg/kg and 0.08-1.5 microg/kg, respectively. The recoveries of the seven pesticides spiked in a bamboo shoot sample at the levels of 4, 8, 32 microg/kg were in the range from 76.0% to 102.6% (the RSD < or = 11.0%, n = 3). The method was successfully applied to the real bamboo shoot samples. The method has high accuracy and sensitivity, and is simple and quick. It can meet the requirement of the simultaneous determination of the seven pesticides in bamboo shoots. PMID:23697174

  5. Health risks associated with pesticide residues in water, sediments and the muscle tissues of Catla catla at Head Balloki on the River Ravi.

    Science.gov (United States)

    Mahboob, Shahid; Niazi, Fakhra; AlGhanim, K; Sultana, Salma; Al-Misned, F; Ahmed, Z

    2015-03-01

    A study of the levels of six pesticide residues (endosulfan, carbofuran, cypermethrin, profenofos, triazophos, and deltamethrin) was conducted to determine possible environmental and health risks in surface waters, sediment, and fish Catla catla. Samples were analyzed by gas chromatography with an electron capture detector. The total concentration of pesticides in water, sediment, and fish ranged from 0.005 to 3.17 ?g/l, 0.61 to 23.06 ng/g dry weight, and 0.35 to 19.15 ?g/g lipid-normalized units, respectively. According to the concentrations and detection frequencies, endosulfan and profenofos were the most dominant pesticides recorded in fish tissue and sediment samples. Profenofos and cypermethrin, meanwhile, were the most abundant pesticides recorded in water samples at these sites. Cypermethrin and triazophos were not detected in the sediment samples. The concentration of endosulfan, carbofuran, and deltamethrin were higher than the permissible limits for fish set by international agencies and pose a potential ecological risk to the aquatic ecosystem and a consequent hazard to human health. PMID:25655128

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

    International Nuclear Information System (INIS)

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

  7. Quantitative analysis of six pesticides in fruits by capillary electrophoresis-electrospray-mass spectrometry.

    Science.gov (United States)

    Juan-García, Ana; Font, Guillermina; Picó, Yolanda

    2005-04-01

    A method to identify and quantify six pesticide residues - dinoseb, pirimicarb, procymidone, pyrifenox, pyrimethanil, and thiabendazole - in peaches and nectarines using capillary electrophoresis-electrospray ionization-quadrupole ion trap-tandem mass spectrometry (CE-ESI-MS/MS) is described. Separation was carried out using a buffer of 0.3 M ammonium acetate at pH 4 with 10% methanol. Pesticide residues present in peach and nectarine samples were preconcentrated by solid-phase extraction using C(18), eluted with CH(2)Cl(2), concentrated to dryness, and redissolved in buffer to obtain lower detection limits. The recoveries of the analytes ranged from 58 to 99% and the relative standard deviations were 9 to 19%. Under optimized CE-MS/MS conditions the minimum detectable levels for the six pesticides in spiked peach samples were between 0.01 mg/kg for pirimicarb and 0.05 mg/kg for procymidone with pressure injection of 50 mbar for 5 s (5 nL) at a signal-to-noise ratio of 3, which constitutes a severalfold increase in sensitivity compared to CE-MS, using a single quadrupole, and to conventional CE-UV. The potential of the method was demonstrated by analyzing different samples taken from regional agricultural cooperatives. The pesticides most often detected were thiabendazole and procymidone. PMID:15759305

  8. Effects of temperature and purity of magnesium sulfate during extraction of pesticides residues using the QuEChERS method

    Science.gov (United States)

    Despite its many documented advantages, the QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation approach has problems with a few unstable pesticides, partly due to the exothermic reaction generated by the use of anhydrous magnesium sulfate during extraction. These pesticide...

  9. Deuterium Gas Analysis by Residual Gas Analyzer

    International Nuclear Information System (INIS)

    Hydrogen gas is generated by electrolysis method in a compact hydrogen generator. A simple procedure reduces handling and storage of hydrogen cylinders for laboratory applications. In such a system, we are producing deuterium gas from heavy water by electrolysis method. After production of the deuterium gas, we have checked the purity level of the outgoing deuterium from the electrolyser. The test was carried out in a high vacuum system in which one residual gas analyser (RGA) was mounted. The deuterium gas was inserted by one manual gas leak valve in to the vacuum system. In this study, the effect of the emission current of the RGA on the detection of the deuterium was performed. In this paper, we will discuss the detail analysis of the deuterium gas and the effect of the emission current on the partial pressure measurement.

  10. Multiresidue determination of pesticide residues in honey by modified QuEChERS method and gas chromatography with electron capture detection

    Scientific Electronic Library Online (English)

    Débora, Orso; Manoel L., Martins; Filipe F., Donato; Tiele M., Rizzetti; Magali, Kemmerich; Martha B., Adaime; Renato, Zanella.

    1355-13-01

    Full Text Available O mel pode apresentar resíduos de pesticidas devido à contaminação das abelhas durante a coleta de pólen e néctar ou por tratamento das colmeias. Assim, a determinação de resíduos de pesticidas em mel é de grande importância, apesar da dificuldade devido à complexidade da matriz. Neste estudo, um no [...] vo método para a determinação de pesticidas de diferentes grupos químicos em mel foi desenvolvido e validado. Amostras de mel foram extraídas pelo método QuEChERS modificado e analisados por cromatografia gasosa com detecção por captura de elétrons (GC-ECD). Os resultados de recuperação, avaliados em três níveis de fortificação, foram entre 71 e 119% para a maioria dos compostos, com valores de desvio padrão relativo (RSD) Abstract in english Honey can present pesticide residues due to the contamination of bees during the collection of pollen and nectar or by treatment of hives. Thus, the determination of pesticide residues in honey is of great importance, despite the difficulty due to the complexity of the matrix. In this study a new me [...] thod for the determination of pesticides from different chemical groups in honey was developed and validated. Honey samples were extracted by modified QuEChERS method and analyzed by gas chromatography with electron capture detection (GC-ECD). Recovery results, evaluated at three spike levels, were between 71 and 119% for most of the compounds, with relative standard deviation (RSD)

  11. Fast and simple extraction of pesticide residues in selected fruits and vegetables using tetrafluoroethane and toluene followed by ultrahigh-performance liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Bak?rc?, Gözde Türköz; H???l, Ya?ar

    2012-12-01

    An extraction and analytical method for the determination of pesticide residues in fruits and vegetables has been developed. The method includes extraction with a pressurised liquid solvent containing a mixture of 1,1,1,2-tetrafluoroethane and toluene, and identification/quantification of pesticides using ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry (UPLC/MS/MS). Validation studies were carried out to evaluate the performance of the method for the determination of 71 different pesticides and metabolites in tomato, cucumber, pepper, spinach, zucchini, grape, cherry, peach and apricot. Matrix-matched calibration curves were applied and correlation coefficients (r(2)) came out to be greater than 0.99. Limit of quantification (LOQ) values of the active substances were found to be lower than the maximum residue limits (MRL) according to regulations in Turkey. The recovery values were found to be between 70% and 120% with relative standard deviations less than 20%. Based on these results, the proposed method is fast, cheaper, rugged and gives quantitative results with no additional clean-up steps. PMID:22953939

  12. Analysis of House Dust and Children’s Hair for Pesticides: A Comparison of Markers of Ongoing Pesticide Exposure in Children

    Science.gov (United States)

    Ostrea, Enrique M.; Villanueva-Uy, Esterlita; Bielawski, Dawn; Birn, Sarah; Janisse, James J.

    2012-01-01

    Background/Aim The long term study of the adverse effects of pesticides on child neuro development requires monitoring not only of initial, but ongoing pesticide exposure. Our aim was to compare house dust and children’s hair as environmental and biological markers of ongoing pesticide exposure in children. Design/Methods In a continuing NIH study on the adverse effects of prenatal pesticide exposure on child neurodevelopment, ongoing pesticide exposure after birth was measured in swept house dust and hair in the children at 4 years of age for propoxur and pyrethroids (transfluthrin, bioallethrin, cyfluthrin and cypermethrin) by gas chromatography/mass spectrometry. The prevalence and concentration of pesticides in the two matrices were compared. Results Prevalence of propoxur was higher in hair compared to house dust (p<0.001) whereas prevalence of the pyrethroids was higher (p<0.001) in house dust. The overall concentrations of the pyrethroids were also higher (p<0.007) in house dust compared to hair. There was a significant (p<0.001) correlation between dust and hair for bioallethrin and cypermethrin. Conclusions Ongoing exposure of children to environmental pesticides is sensitively detected by analysis of children’s hair and house dust. However, prevalence of propoxur was higher in hair compared to swept house dust, but the opposite was found for the pyrethroids. Thus, both matrices should be analyzed. There was a significant (p<0.001) correlation between house dust and hair for bioallethrin and cypermethrin. PMID:24288586

  13. Development of MSPD method for the determination of pesticide residues in tomato by GC-MS

    Scientific Electronic Library Online (English)

    Adalberto, Menezes Filho; Sandro, Navickiene; Haroldo S., Dórea.

    2006-10-01

    Full Text Available Um método simples e eficiente baseado na técnica de dispersão da matriz em fase sólida foi desenvolvido para determinar resíduos de dimetoato, parationa-metílica, malationa, tebuconazol, e cipermetrina em tomate, por cromatografia gasosa acoplada a espectrometria de massas no modo de monitoramento d [...] e íons selecionados. Diferentes parâmetros foram avaliados, tais como: tipo (C18, alumina, sílica-gel e Florisil) e quantidade de sorbente e solvente de eluição (diclorometano, acetato de etila, n-hexano e n-hexano:acetato de etila (1:1 e 1:3, v/v)), sendo que o mais adequado foi alumina na proporção matriz:sorbente de 4:1 (m/m), Florisil como sorbente de purificação e diclorometano como solvente de eluição. Recuperações médias (n=7) de tomates fortificados (0,05-4,0 mg kg-1) variaram de 77 a 100%, com coeficiente de variação entre 3,7% e 12,9%. Os limites de detecção variaram entre 0,01 e 0,02 mg kg-1, enquanto que os limites de quantificação variaram entre 0,03 e 0,06 mg kg-1. O método foi aplicado em amostras de tomates coletadas na cidade de Aracaju, SE, sendo que resíduos de parationa-metílica, malationa e dimetoato foram detectados, porém abaixo dos limites máximos de resíduos (LMRs) estabelecidos pela legislação brasileira e pelo Codex Alimentarius. Abstract in english A simple and effective extraction method based on matrix solid-phase dispersion was developed to determine dimethoate, methyl-parathion, malathion, tebuconazole and cypermethrin in tomato using gas chromatography-mass spectrometry and selected ion monitoring (GC-MS, SIM). Different parameters of the [...] method were evaluated, such as type of solid phase (C18, alumina, sílica-gel and Florisil), the amount of solid phase and eluent [dichloromethane, ethyl acetate, n-hexane and n-hexane:ethyl acetate (1:1 and 1:3, v/v)]. The best results were obtained using 2.0 g of tomato, 0.5 g of alumina as dispersant sorbent, 0.5 g of Florisil as clean-up sorbent and dichloromethane as eluting solvent. The method was validated by fortified tomato samples at different concentration levels (0.05 to 4.0 mg kg-1). Average recoveries (7 replicates) ranged from 77% to 100% with relative standard deviation between 3.7% and 12.9%. Detection and quantification limits ranged from 0.01 to 0.02 mg kg-1 and 0.03 to 0.06 mg kg-1 for the whole fruit of tomato, respectively. The proposed method was applied to analyze of these compounds in commercial tomato samples and residues of methyl-parathion, dimethoate and malathion were detected on the tomato samples at concentrations below the maximum residue levels (MRLs) established by Brazilian legislation and Codex Alimentarius.

  14. Toxicidade residual de alguns agrotóxicos recomendado na agricultura sobre Neoseiulus californicus (McGregor (Acari: Phytoseiidae Residual toxicity of some pesticides recommended for citrus orchards on the predaceous mite Neoseiulus californicus (McGregor (Acari: phytoseiidae

    Directory of Open Access Journals (Sweden)

    Marcos Zatti da Silva

    2007-04-01

    Full Text Available O objetivo do trabalho foi avaliar a toxicidade residual de alguns agrotóxicos utilizados em citros sobre Neoseiulus californicus (McGregor em condições de laboratório. O método de bioensaio adotado foi o de contato residual. Folhas de citros da variedade Pêra, acondicionadas em arenas, foram pulverizadas em torre de Potter. A toxicidade residual dos produtos foi avaliada duas horas e 1; 3; 5; 7; 10; 14 e 21 dias após a aplicação. Em cada arena, foram transferidas dez fêmeas adultas de N. californicus, juntamente com uma quantidade suficiente de Tetranychus urticae, como fonte de alimento. As avaliações de mortalidade foram realizadas 72 horas após a transferência dos ácaros para as arenas. Os agrotóxicos acrinathrin, deltamethrin, dinocap, enxofre, fenpropathrin, óxido de fenbutatin e propargite não causaram mortalidades significativas em adultos de N. californicus. Foram registradas mortalidades de 29,8; 24,0 e 34,1% para ácaros N. californicus expostos a resíduos de duas horas de idade de abamectim, azocyclotin e cyhexatin, respectivamente. Dicofol, pyridaben e chlorfenapyr causaram 100% de mortalidade aos ácaros predadores expostos aos resíduos tóxicos dos acaricidas, com duas horas de idade. Abamectin provocou mortalidade significativa por um período inferior a um dia. Resíduos dos acaricidas azocyclotin, cyhexatin, dicofol, pyridaben e chlorfenapyr provocaram mortalidades significativas por períodos de 1; 1; 10; 10 e 21dias, respectivamente. Os resultados obtidos no presente experimento servem de subsídio para a escolha adequada dos agrotóxicos a serem utilizados em pomares de citros nos quais N. californicus esteja presente ou naqueles em que o predador venha a ser liberado. Esses resultados também servem para a escolha do momento mais favorável para a liberação dos ácaros predadores dessa espécie no campo, após a aplicação de agrotóxicos nos pomares. Estudos conduzidos em condições de campo ainda são necessários para se compreender melhor o efeito desses agrotóxicos sobre o ácaro predador.This study was carried out to evaluate the residual toxicity of some pesticides used in citrus orchards, on Neoseiulus californicus (McGregor under laboratory conditions. The residual contact bioassay method was adopted. Citrus leaves of the variety "Pêra" were sprayed in a Potter tower. The products' residual toxicity was evaluated at two hours and 1, 3, 5, 7, 10, 14 and 21 days after treatment. Ten adult females of N. californicus were transferred to each arena together with an enough amount of Tetranychus urticae to feed the predator. Mortality evaluations were performed at 72 hours after transferring the predaceous mites to the arenas. The pesticides acrinathrin, deltamethrin, dinocap, sulphur, fenpropathrin, fenbutatin oxide and propargite did not cause significant mortalities to the adults of N. californicus. Abamectim, azocyclotin and cyhexatin caused mortalities of 29.8, 24.0 and 34.1%, respectively, for N. californicus adults exposed to two-hour pesticide residues. Dicofol, pyridaben and chlorfenapyr caused 100% of mortality to the predators exposed to the two-hour acaricide residues. Abamectin provoked significant mortalities for a period shorter than one day. Residues of azocyclotin, cyhexatin, dicofol, pyridaben and chlorfenapyr caused significant mortalities for periods of 1, 1, 10, 10 and 21 days, respectively. The results of this study provided basic information for choosing the adequate pesticides to be used in citrus orchards in which N. californicus is present, or in those the predator will be released. The results are also useful for the decision of the best releasing time for N. californicus in the field, after pesticide applications. Studies carried out in the field are still necessary to understand better the effect of these pesticides under the predaceous mite.

  15. Toxicidade residual de alguns agrotóxicos recomendado na agricultura sobre Neoseiulus californicus (McGregor) (Acari: Phytoseiidae) / Residual toxicity of some pesticides recommended for citrus orchards on the predaceous mite Neoseiulus californicus (McGregor) (Acari: phytoseiidae)

    Scientific Electronic Library Online (English)

    Marcos Zatti da, Silva; Caralos Amadeu Leite de, Oliveira.

    2007-04-01

    Full Text Available O objetivo do trabalho foi avaliar a toxicidade residual de alguns agrotóxicos utilizados em citros sobre Neoseiulus californicus (McGregor) em condições de laboratório. O método de bioensaio adotado foi o de contato residual. Folhas de citros da variedade Pêra, acondicionadas em arenas, foram pulve [...] rizadas em torre de Potter. A toxicidade residual dos produtos foi avaliada duas horas e 1; 3; 5; 7; 10; 14 e 21 dias após a aplicação. Em cada arena, foram transferidas dez fêmeas adultas de N. californicus, juntamente com uma quantidade suficiente de Tetranychus urticae, como fonte de alimento. As avaliações de mortalidade foram realizadas 72 horas após a transferência dos ácaros para as arenas. Os agrotóxicos acrinathrin, deltamethrin, dinocap, enxofre, fenpropathrin, óxido de fenbutatin e propargite não causaram mortalidades significativas em adultos de N. californicus. Foram registradas mortalidades de 29,8; 24,0 e 34,1% para ácaros N. californicus expostos a resíduos de duas horas de idade de abamectim, azocyclotin e cyhexatin, respectivamente. Dicofol, pyridaben e chlorfenapyr causaram 100% de mortalidade aos ácaros predadores expostos aos resíduos tóxicos dos acaricidas, com duas horas de idade. Abamectin provocou mortalidade significativa por um período inferior a um dia. Resíduos dos acaricidas azocyclotin, cyhexatin, dicofol, pyridaben e chlorfenapyr provocaram mortalidades significativas por períodos de 1; 1; 10; 10 e 21dias, respectivamente. Os resultados obtidos no presente experimento servem de subsídio para a escolha adequada dos agrotóxicos a serem utilizados em pomares de citros nos quais N. californicus esteja presente ou naqueles em que o predador venha a ser liberado. Esses resultados também servem para a escolha do momento mais favorável para a liberação dos ácaros predadores dessa espécie no campo, após a aplicação de agrotóxicos nos pomares. Estudos conduzidos em condições de campo ainda são necessários para se compreender melhor o efeito desses agrotóxicos sobre o ácaro predador. Abstract in english This study was carried out to evaluate the residual toxicity of some pesticides used in citrus orchards, on Neoseiulus californicus (McGregor) under laboratory conditions. The residual contact bioassay method was adopted. Citrus leaves of the variety "Pêra" were sprayed in a Potter tower. The produc [...] ts' residual toxicity was evaluated at two hours and 1, 3, 5, 7, 10, 14 and 21 days after treatment. Ten adult females of N. californicus were transferred to each arena together with an enough amount of Tetranychus urticae to feed the predator. Mortality evaluations were performed at 72 hours after transferring the predaceous mites to the arenas. The pesticides acrinathrin, deltamethrin, dinocap, sulphur, fenpropathrin, fenbutatin oxide and propargite did not cause significant mortalities to the adults of N. californicus. Abamectim, azocyclotin and cyhexatin caused mortalities of 29.8, 24.0 and 34.1%, respectively, for N. californicus adults exposed to two-hour pesticide residues. Dicofol, pyridaben and chlorfenapyr caused 100% of mortality to the predators exposed to the two-hour acaricide residues. Abamectin provoked significant mortalities for a period shorter than one day. Residues of azocyclotin, cyhexatin, dicofol, pyridaben and chlorfenapyr caused significant mortalities for periods of 1, 1, 10, 10 and 21 days, respectively. The results of this study provided basic information for choosing the adequate pesticides to be used in citrus orchards in which N. californicus is present, or in those the predator will be released. The results are also useful for the decision of the best releasing time for N. californicus in the field, after pesticide applications. Studies carried out in the field are still necessary to understand better the effect of these pesticides under the predaceous mite.

  16. 76 FR 59908 - Chlorantraniliprole; Pesticide Tolerances; Correction

    Science.gov (United States)

    2011-09-28

    ...EPA-HQ-OPP-2010-0888; FRL-8888-3] Chlorantraniliprole; Pesticide Tolerances; Correction...pesticide tolerances for residues of chlorantraniliprole in or on multiple commodities...follows: Sec. [emsp14]180.628 Chlorantraniliprole; tolerances for residues....

  17. 78 FR 66651 - Imazapyr; Pesticide Tolerances

    Science.gov (United States)

    2013-11-06

    ...and children to the pesticide chemical residue in establishing...aggregate exposure to the pesticide chemical residue...forage; grass, hay; fish; shellfish; fats...Organization/World Health Organization food...

  18. Analysis of pesticides by gas chromatography/multiphoton ionization/mass spectrometry using a femtosecond laser

    Energy Technology Data Exchange (ETDEWEB)

    Li, Adan [Department of Applied Chemistry, Graduate School of Engineering, Kyushu University, 744 Motooka, Nishi-ku, Fukuoka 819-0395 (Japan); College of Chemistry and Environmental Engineering, Yanshan University, Qinhuangdao 066004 (China); Imasaka, Tomoko [Laboratory of Chemistry, Graduate School of Design, Kyushu University, 4-9-1 Shiobaru, Minami-ku, Fukuoka 815-8540 (Japan); Uchimura, Tomohiro [Department of Applied Chemistry, Graduate School of Engineering, Kyushu University, 744 Motooka, Nishi-ku, Fukuoka 819-0395 (Japan); Division of Translational Research, Center for Future Chemistry, Kyushu University, 744 Motooka, Nishi-ku, Fukuoka 819-0395 (Japan); Imasaka, Totaro, E-mail: imasaka@cstf.kyushu-u.ac.jp [Department of Applied Chemistry, Graduate School of Engineering, Kyushu University, 744 Motooka, Nishi-ku, Fukuoka 819-0395 (Japan); Division of Translational Research, Center for Future Chemistry, Kyushu University, 744 Motooka, Nishi-ku, Fukuoka 819-0395 (Japan)

    2011-09-02

    Highlights: {yields} Gas chromatography/multiphoton ionization/time-of-flight mass spectrometry was utilized for analysis. {yields} A standard mixture sample containing 49 pesticides and 4 real samples were measured. {yields} Third-harmonic emission of a Ti:sapphire laser (100 fs) was employed as an ionization source. {yields} Most of the pesticides were softly ionized by the femtosecond laser. {yields} Three pesticides were found, although some of them were not detected by GC/EI/MS-MS. - Abstract: Gas chromatography/multiphoton ionization/time-of-flight mass spectrometry (GC/MPI/TOFMS) was utilized for analysis of a standard mixture sample containing 49 pesticides and 4 real samples using the third-harmonic emission (267 nm) of a femtosecond Ti:sapphire laser (100 fs) as the ionization source. A sample of a standard mixture of n-alkane was also measured for calibration of the retention time indices of the pesticides. Two photons are required for the excitation of n-alkane due to an absorption band located in the far ultraviolet region (140 nm). The n-alkane molecule in the excited state was subsequently ionized either directly or by absorbing another photon because of a high ionization potential. Due to a large excess of energy, the molecular ion was decomposed and formed many fragment ions. Compared to n-alkanes, most of the pesticides were softly ionized by the femtosecond laser; one photon was used for excitation and another was used for the subsequent ionization. The pesticides with no conjugated double bond had a lower ionization efficiency. The present analytical instrument was applied to several samples prepared from a variety of vegetables and a single fruit after pretreatment with solid-phase extraction. Three pesticides were found in these samples, although some of them were not detected by conventional GC/EI/MS-MS due to insufficient sensitivity and selectivity.

  19. Multivariate optimization of the QuEChERS-GC-ECD method and pesticide investigation residues in apples, strawberries, and tomatoes produced in Brazilian south

    Scientific Electronic Library Online (English)

    Juliana G., Lorenz; Léa L. F., Costa; Eliane A., Suchara; Ernani S., Sant' Anna.

    1583-15-01

    Full Text Available Culturas como maçã, morango e tomate estão entre os alimentos de maior contaminação por uso de pesticidas no Brasil. Pensando nisso, a otimização multivariada do método QuEChERS, acoplado ao CG-ECD, foi proposta a fim de investigar os níveis de resíduos dos pesticidas clorpirifós, dimetoato, malatio [...] na, mevinfós, pedimentalina, simazina e trifluralina em maçãs, morangos e tomates produzidos no Estado de Santa Catarina, sul do Brasil. O processo envolveu os planejamentos fatorial completo 2(4) e Doehlert seguido de validação do método modificado e aplicação em 91 amostras reais coletadas durante os anos de 2010 e 2011. As modificações realizadas no método proporcionaram aumento de detectabilidade e valores satisfatórios de linearidade, precisão e exatidão. Nas amostras reais, resíduos de pelo menos um pesticida (> LOQ) foram encontrados em 8 (27,6%) amostras de maçãs, 12 (40,0%) morangos e 17 (53,1%) tomates. Os resultados indicaram a necessidade de monitoramento contínuo para o uso destes pesticidas em frutas e vegetais. Abstract in english Apple, strawberry and tomato are among the foods with higher contamination for pesticide use in Brazil. Thereby, a multivariate optimization of the QuEChERS method coupled to GC-ECD was proposed to investigate the level of pesticides residues clorpyrifos, dimethoate, malathion, mevinphos, pedimental [...] ina, simazine and trifluralin in apple, strawberries and tomatoes produced in Santa Catarina state, South of Brazil. The process involved a two-level full factorial and Doehlert designs followed by validation of the modified method and its application in 91 real samples collected during the years 2010 and 2011. Modifications in the method provided increased detectability and satisfactory values of linearity, accuracy and precision. In real samples, residues of at least one pesticide (> LOQ) were found in 8 (27.6%) apple, 12 (40.0%) strawberry and 17 (53.1%) tomato samples. The results indicated the necessity of continuous monitoring for pesticide use in fruits and vegetables.

  20. Multiresidue analysis of 16 pesticides in jujube using gas chromatography and mass spectrometry with multiwalled carbon nanotubes as a sorbent.

    Science.gov (United States)

    Zhao, Liuwei; Zhang, Ling; Liu, Fengmao; Xue, Xiaofeng; Pan, Canping

    2014-11-01

    Although jujube is a minor crop and very few pesticides are registered on it, the application of pesticides during the growth stage of jujube is inevitable to control the pests or diseases. This situation has led to pesticide misuse. A modified quick, easy, cheap, effective, rugged, and safe method using a novel sorbent, multiwalled carbon nanotubes, as a dispersive solid-phase extraction sorbent combined with gas chromatography with mass spectrometry, was developed for the determination of 16 pesticides in jujube. Under the optimized conditions, recoveries of 76.7-112.4% were obtained for the target analytes at three spiked concentration levels. The relative standard deviations ranged from 1.2 to 12.3%. Limits of detection and limits of quantification for 16 pesticides ranged from 1 to 10 and 3 to 30 ?g/kg, respectively. The residues of chlorpyrifos, hexaconazole, tebuconazole, and cyhalothrin were detected from samples obtained from the market. PMID:25155928

  1. Avaliação de risco crônico da ingestão de resíduos de pesticidas na dieta brasileira / Chronic dietary risk assessment for pesticide residues in Brazilian food

    Scientific Electronic Library Online (English)

    Eloisa Dutra, Caldas; Luiz César Kenupp R de, Souza.

    2000-10-01

    Full Text Available OBJETIVO: Avaliar o risco crônico da ingestão de pesticidas pela dieta, em compostos registrados no Brasil para uso agrícola até 1999. MÉTODOS: Foi calculada a Ingestão Diária Máxima Teórica (IDMT) para cada pesticida, utilizando limites máximos de resíduos estabelecidos pela legislação brasileira e [...] dados de consumo alimentar. A caracterização do risco foi feita comparando-se a IDMT com as doses diárias aceitáveis (IDA) de vários países e do Codex Alimentarius. RESULTADOS: A IDTM ultrapassou a IDA (%IDA>100) em pelo menos uma região metropolitana brasileira para 23 pesticidas. Dezesseis compostos com maior %IDA são inseticidas organofosforados, sendo o paration metílico o composto cuja ingestão mais excedeu o parâmetro toxicológico (%IDA N=9.300). O arroz, o feijão, as frutas cítricas e o tomate foram os alimentos que mais contribuíram para a ingestão. Dos compostos que apresentaram maior risco, apenas 6 foram registrados de acordo com o Decreto 98.816/90, que dispõe sobre o uso de pesticidas no País. CONCLUSÕES: Os compostos identificados como sendo de potencial risco de exposição crônica para a população brasileira, e os alimentos que mais contribuíram para a sua ingestão, devem ser priorizados pelos órgãos de saúde em programas de monitoramento de resíduos de pesticidas. Adicionalmente, dados sobre resíduos em alimentos prontos para o consumo, fatores de processamento e dados sobre consumo alimentar devem ser gerados para possibilitar o refinamento do estudo. Abstract in english OBJECTIVE: To conduct a chronic dietary risk assessment of the pesticides registered in Brazil up until 1999. METHODS: The Theoretical Maximum Daily Intake (TMDI) for each pesticide was calculated using the Brazilian maximum residue limits and food consumption data from IBGE, the Brazilian Statistic [...] al Institute. The risk characterization was done comparing the TMDI with the acceptable daily intakes (ADI) from other countries and from the Codex Alimentarius. RESULTS: The TMDI was higher than the ADI (%ADI>100) at least in one Brazilian metropolitan region for 23 pesticides. Sixteen compounds are organophosphate insecticides, with methyl parathion having the TMDI exceeding the most toxicological parameter (%ADI N=9,300). Rice, beans, citrus and tomato were the commodities which most contributed to the ingestion. From the compounds under higher risk, only 6 were registered according to the Law 98.816/90, which concerns the use of pesticides in the country. CONCLUSIONS: The compounds identified in the study as presenting a potential health concern to the Brazilian consumers, and the commodities which most contributed to the ingestion, should be prioritized by the government in pesticide residue monitoring programs and in the re-registration process. In addition, residue data in food as consumed, processing factors and appropriate consumption data should be generated to allow further studies.

  2. Avaliação de risco crônico da ingestão de resíduos de pesticidas na dieta brasileira Chronic dietary risk assessment for pesticide residues in Brazilian food

    Directory of Open Access Journals (Sweden)

    Eloisa Dutra Caldas

    2000-10-01

    Full Text Available OBJETIVO: Avaliar o risco crônico da ingestão de pesticidas pela dieta, em compostos registrados no Brasil para uso agrícola até 1999. MÉTODOS: Foi calculada a Ingestão Diária Máxima Teórica (IDMT para cada pesticida, utilizando limites máximos de resíduos estabelecidos pela legislação brasileira e dados de consumo alimentar. A caracterização do risco foi feita comparando-se a IDMT com as doses diárias aceitáveis (IDA de vários países e do Codex Alimentarius. RESULTADOS: A IDTM ultrapassou a IDA (%IDA>100 em pelo menos uma região metropolitana brasileira para 23 pesticidas. Dezesseis compostos com maior %IDA são inseticidas organofosforados, sendo o paration metílico o composto cuja ingestão mais excedeu o parâmetro toxicológico (%IDA N=9.300. O arroz, o feijão, as frutas cítricas e o tomate foram os alimentos que mais contribuíram para a ingestão. Dos compostos que apresentaram maior risco, apenas 6 foram registrados de acordo com o Decreto 98.816/90, que dispõe sobre o uso de pesticidas no País. CONCLUSÕES: Os compostos identificados como sendo de potencial risco de exposição crônica para a população brasileira, e os alimentos que mais contribuíram para a sua ingestão, devem ser priorizados pelos órgãos de saúde em programas de monitoramento de resíduos de pesticidas. Adicionalmente, dados sobre resíduos em alimentos prontos para o consumo, fatores de processamento e dados sobre consumo alimentar devem ser gerados para possibilitar o refinamento do estudo.OBJECTIVE: To conduct a chronic dietary risk assessment of the pesticides registered in Brazil up until 1999. METHODS: The Theoretical Maximum Daily Intake (TMDI for each pesticide was calculated using the Brazilian maximum residue limits and food consumption data from IBGE, the Brazilian Statistical Institute. The risk characterization was done comparing the TMDI with the acceptable daily intakes (ADI from other countries and from the Codex Alimentarius. RESULTS: The TMDI was higher than the ADI (%ADI>100 at least in one Brazilian metropolitan region for 23 pesticides. Sixteen compounds are organophosphate insecticides, with methyl parathion having the TMDI exceeding the most toxicological parameter (%ADI N=9,300. Rice, beans, citrus and tomato were the commodities which most contributed to the ingestion. From the compounds under higher risk, only 6 were registered according to the Law 98.816/90, which concerns the use of pesticides in the country. CONCLUSIONS: The compounds identified in the study as presenting a potential health concern to the Brazilian consumers, and the commodities which most contributed to the ingestion, should be prioritized by the government in pesticide residue monitoring programs and in the re-registration process. In addition, residue data in food as consumed, processing factors and appropriate consumption data should be generated to allow further studies.

  3. Multiresidue Analysis of Pesticides in Soil by Liquid-Solid Extraction Procedure

    Directory of Open Access Journals (Sweden)

    Rada ?urovi?

    2012-01-01

    Full Text Available A multiresidue method for simultaneous determination of four pesticides (diazinon,acetochlor, aldrine and carbofuran belonging to different pesticide groups, extractedfrom soil samples, is described. The method presented is based on liquid-solid extraction(LSE and determination of pesticides, i.e. the pesticides were extracted by methanol-acetone mixture, purified on florisil column and eluted by ethyl acetate-acetone mixture.Optimization of the main parameters affecting the LSE procedure, such as the choiceof purification sorbent, as well as the elution solvent and its volume, were investigated indetails and optimized. Also, validation of the proposed method was done.Gas chromatography-mass spectrometry (GC-MS was used for detection and quantificationof the pesticides studied. Relative standard deviation (RSD and recovery values formultiple analysis of soil samples fortified with 30 ?g/kg of each pesticide were below 8%and higher than 89%, respectively. Limits of detection (LOD for all the compounds studiedwere less than 4 ?g/kg.

  4. Time-dependent integrity during storage of natural surface water samples for the trace analysis of pharmaceutical products, feminizing hormones and pesticides

    Directory of Open Access Journals (Sweden)

    Prévost Michèle

    2010-04-01

    Full Text Available Abstract Monitoring and analysis of trace contaminants such as pharmaceuticals and pesticides require the preservation of the samples before they can be quantified using the appropriate analytical methods. Our objective is to determine the sample shelf life to insure proper quantification of ultratrace contaminants. To this end, we tested the stability of a variety of pharmaceutical products including caffeine, natural steroids, and selected pesticides under refrigerated storage conditions. The analysis was performed using multi-residue methods using an on-line solid-phase extraction combined with liquid chromatography tandem mass spectrometry (SPE-LC-MS/MS in the selected reaction monitoring mode. After 21 days of storage, no significant difference in the recoveries was observed compared to day 0 for pharmaceutical products, while for pesticides, significant losses occurred for DIA and simazine after 10 days (14% and 17% reduction respectively and a statistically significant decrease in the recovery was noted for cyanazine (78% disappearance. However, the estrogen and progestogen steroids were unstable during storage. The disappearance rates obtained after 21 days of storage vary from 63 to 72% for the feminizing hormones. Overall, pharmaceuticals and pesticides seem to be stable for refrigerated storage for up to about 10 days (except cyanazine and steroidal hormones can be quite sensitive to degradation and should not be stored for more than a few days.

  5. 76 FR 23882 - Metiram; Pesticide Tolerances

    Science.gov (United States)

    2011-04-29

    ...aggregate exposure to the pesticide chemical residue, including...and children to the pesticide chemical residue in...aggregate exposure to the pesticide chemical residue...combined risks from food, water, and non-occupational...the risks of ETU, a contaminant, metabolite, and...

  6. 76 FR 18906 - Mancozeb; Pesticide Tolerances

    Science.gov (United States)

    2011-04-06

    ...aggregate exposure to the pesticide chemical residue, including...and children to the pesticide chemical residue in...aggregate exposure to the pesticide chemical residue...combined risks from food, water and non-occupational...the risks of ETU, a contaminant, metabolite...

  7. / Investigation of the occurrence of pesticide residues in rural wells and surface water following application to tobacco

    Scientific Electronic Library Online (English)

    Edson C., Bortoluzzi; Danilo S., Rheinheimer; Celso S., Gonçalves; João B. R., Pellegrini; Aline M., Maroneze; Márcia H. S., Kurz; Nádia M., Bacar; Renato, Zanella.

    1872-18-01

    Full Text Available [...] Abstract in english In this work the exposure of wells and surface water to pesticides, commonly used for tobacco cropping, was assessed. Water consumption wells and surface water flows were sampled at different times. After a preconcentration step with solid phase extraction (SPE), the selected pesticides were determi [...] ned by gas chromatography with electron capture detection (GC-ECD) or high performance liquid chromatography with diode array detection (HPLC-DAD). No pesticides were detected in the well water samples and surface water flow in the winter season. However, in the spring and summer higher concentrations of chlorpyrifos and imidacloprid were found in the water source samples. Atrazine, simazine and clomazone were also found. The occurrence of pesticides in collected water samples was related with the application to tobacco.

  8. Investigation of the occurrence of pesticide residues in rural wells and surface water following application to tobacco

    Directory of Open Access Journals (Sweden)

    Edson C. Bortoluzzi

    2007-01-01

    Full Text Available In this work the exposure of wells and surface water to pesticides, commonly used for tobacco cropping, was assessed. Water consumption wells and surface water flows were sampled at different times. After a preconcentration step with solid phase extraction (SPE, the selected pesticides were determined by gas chromatography with electron capture detection (GC-ECD or high performance liquid chromatography with diode array detection (HPLC-DAD. No pesticides were detected in the well water samples and surface water flow in the winter season. However, in the spring and summer higher concentrations of chlorpyrifos and imidacloprid were found in the water source samples. Atrazine, simazine and clomazone were also found. The occurrence of pesticides in collected water samples was related with the application to tobacco.

  9. Studies to improve the extraction yields of incurred pesticide residues from crops using the QuEChERS method.

    Science.gov (United States)

    Hepperle, Julia; Dörk, Daniela; Barth, Anja; Ta?delen, Bünjamin; Anastassiades, Michelangelo

    2015-01-01

    The influence of various factors on the extraction yields of incurred pesticides from crops using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method was thoroughly studied. These factors included extraction time, extraction temperature, agitation approach, and in the case of dry commodities, sample comminution grade. Extraction yields increased with increasing extraction time, eventually reaching a plateau. Extraction temperature also played an important role in speeding up extraction, whereas the agitation approach had little influence. Based on our results we propose an extension of the first QuEChERS extraction step to 15 min when using deep frozen samples and to 2 min when using samples at ambient temperature. The extension of the second QuEChERS extraction step was shown to be less effective. Mechanical shakers can be used to facilitate extraction. This minor modification of the QuEChERS method does not alter its simple structure nor increase the manual labor and costs involved. It was further shown that the extraction yields of incurred pesticides strongly depend on their physiochemical properties, with lipophilic pesticides typically showing stronger retardation and higher yields when extraction time and/or temperature are increased. The impact of prolonging the first QuEChERS extraction step from 1 to 15 min on the extraction yields of incurred pesticides from frozen samples was studied on 132 real samples containing 85 different pesticides throughout the polarity range and representing 55 different commodity types. Out of the 408 pesticide/commodity combinations studied, 34% showed >25% yield increases when the extraction time was extended to 15 min. Also, more than half of the 132 studied samples contained at least one incurred pesticide for which the extraction yield increased by more than 25%. Similar extraction retardation effects were also observed for spiked pesticides but only if these were spiked on commodities with intact surface, not to homogenates thereof. PMID:25905753

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

    OpenAIRE

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

    2012-01-01

    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 ...

  11. Determination of 17 Organophosphate Pesticide Residues in Mango by Modified QuEChERS Extraction Method Using GC-NPD/GC-MS and Hazard Index Estimation in Lucknow, India

    OpenAIRE

    Srivastava, Ashutosh K.; Rai, Satyajeet; Srivastava, M. K.; Lohani, M.; Mudiam, M. K. R.; Srivastava, L. P.

    2014-01-01

    A total of 162 samples of different varieties of mango: Deshehari, Langra, Safeda in three growing stages (Pre-mature, Unripe and Ripe) were collected from Lucknow, India, and analyzed for the presence of seventeen organophosphate pesticide residues. The QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method of extraction coupled with gas chromatography was validated for pesticides and qualitatively confirmed by gas chromatography- mass spectrometry. The method was validated with di...

  12. Development and validation of a multi-residue analytical methodology to determine the presence of selected pesticides in water through liquid chromatography

    Scientific Electronic Library Online (English)

    Silvia H. G., Brondi; Fernando M., Lanças.

    2005-06-01

    Full Text Available No presente trabalho uma metodologia analítica é descrita para determinar a presença de multi-residuos de pesticidas utilizados na cultura da cana de açúcar (tebuthiuron, hexazinona, diuron, 2,4-D e ametrina), em fontes de água de abastecimento. Os analitos foram isolados da matriz água, através das [...] seguintes técnicas: extração liquido-liquido (LLE), utilizando diclorometano como solvente; extração em fase sólida (SPE), utilizando C18 como suporte sólido e acetonitrila como solvente para condicionamento da fase e eluição dos analitos; e extração com fluido supercrítico (SFE), utilizando C18 como suporte sólido e CO2 no estado supercrítico como solvente de extração. Análise cromatográfica foi feita por cromatografia liquida de alta eficiência (HPLC) com detector ultravioleta, utilizando acetonitrila/água como fase móvel. Dentre as três técnicas de extração avaliadas, os melhores resultados foram obtidos com extração liquido-liquido e extração em fase sólida. Abstract in english In the present work an analytical methodology is described to determine the presence of multi-residues of selected pesticides used in sugar-cane cultures (tebuthiuron, hexazinone, diuron, 2,4-D and ametrine), in source of drinking water. The analytes were isolated from the water matrix through the f [...] ollowing techniques: liquid-liquid extraction (LLE) using dichloromethane as solvent; solid phase extraction (SPE) using C18 as solid support and acetonitrile as solvent to condition the solid phase and elution of the analytes; and supercritical fluid extraction (SFE) using C18 as solid support and CO2 in supercritical state as extractant solvent. The chromatographic analysis was done by high performance liquid chromatography (HPLC) with an ultraviolet detector and using acetonitrile/water as mobile phase. Among the three evaluated extraction techniques, the best results were obtained with both liquid-liquid extraction and solid phase extraction.

  13. Radi