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Sample records for pesticide residue analysis

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

    Kai ZHANG; Jon W WONG; Perry G WANG

    2011-01-01

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

  2. Multi-Residue Analysis of Pesticide Residues in Crude Pollens by UPLC-MS/MS

    Zhou Tong

    2016-12-01

    Full Text Available A multi-residue method for the determination of 54 pesticide residues in pollens has been developed and validated. The proposed method was applied to the analysis of 48 crude pollen samples collected from eight provinces of China. The recovery of analytes ranged from 60% to 136% with relative standard deviations (RSDs below 30%. Of the 54 targeted compounds, 19 pesticides were detected. The major detection rates of each compound were 77.1% for carbendazim, 58.3% for fenpropathrin, 56.3% for chlorpyrifos, 50.0% for fluvalinate, 31.3% for chlorbenzuron, and 29.2% for triadimefon in crude pollen samples. The maximum values of each pesticide were 4516 ng/g for carbendazim, 162.8 ng/g for fenpropathrin, 176.6 ng/g for chlorpyrifos, 316.2 ng/g for fluvalinate, 437.2 ng/g for chlorbenzuron, 79.00 ng/g for triadimefon, and so on. This study provides basis for the research on the risks to honeybee health.

  3. [Quantitative Analysis of Dimethoate Pesticide Residues in Honey by Surface-Enhanced Raman Spectroscopy].

    Sun, Xu-dong; Dong, Xiao-ling

    2015-06-01

    The feasibility of a combination method of surface-enhanced Raman spectroscopy (SERS) technology and linear regression algorithm was investigated for rapid quantitative analysis of pesticide residues in honey. The total of 30 samples was applied in the experiment with dimethoate pesticide residues range from 1 ppm to 10 ppm. The samples were divided into calibration set (20) and prediction set (10). The substrate of Klarite with an inverted pyramidal structure was adopted for improvement of the relative intensity of the majority of Raman shift peaks. The comparative analysis was carried out between SERS spectra of dimethoate pesticide residues in honey samples and conventional Raman spectra of dimethoate standard sample. And four characteristic Raman shift peaks at the wavenumbers of 867, 1 065, 1 317 and 1 453 cm(-1) were found, which were related with the vibrational information of dimethoate molecule. The relationship was developed by linear regression algorithm between the intensity of Raman shift and the concentration of dimethoate pesticide residues. The 10 new samples in the prediction set were applied to evaluate the performance of the models. By comparison, the optimal model was obtained with the characteristic Raman shift peak of 867 cm(-1). The higher correlation coefficient of prediction of 0.984 and lower root mean square error of prediction of 0.663 ppm were obtained. The detection limit of this method was 2 ppm, which was close to the maximum levels of pesticide residue detection limits. Experimental results showed that it was feasible to rapidly analyze quantitative of pesticide residues in honey with the combination method of SERS technology and linear regression algorithm. Compared with the conventional method coupled with the suitable pretreatment, the combination method of SERS technology and linear regression method could analyze the dimethoate pesticide residues in honey, and it also provided an optional method for rapid quantitative analysis

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

    U.S.Pujeri

    2010-10-01

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

  5. Research Progress on Pesticide Residue Analysis Techniques in Agro-products

    HE Ze-ying

    2016-07-01

    Full Text Available There are constant occurrences of acute pesticide poisoning among consumers and pesticide residue violations in agro-products import/export trading. Pesticide residue analysis is the important way to protect the food safety and the interest of import/export enterprises. There has been a rapid development in pesticide residue analysis techniques in recent years. In this review, the research progress in the past five years were discussed in the respects of samples preparation and instrument determination. The application, modification and development of the QuEChERS method in samples preparation and the application of tandem mass spectrometry and high resolution mass spectrometry were reviewed. And the implications for the future of the field were discussed.

  6. Modelling pesticides residues

    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. Effects of food processing on pesticide residues in fruits and vegetables: a meta-analysis approach.

    Keikotlhaile, B M; Spanoghe, P; Steurbaut, W

    2010-01-01

    Pesticides are widely used in food production to increase food security despite the fact that they can have negative health effects on consumers. Pesticide residues have been found in various fruits and vegetables; both raw and processed. One of the most common routes of pesticide exposure in consumers is via food consumption. Most foods are consumed after passing through various culinary and processing treatments. A few literature reviews have indicated the general trend of reduction or concentration of pesticide residues by certain methods of food processing for a particular active ingredient. However, no review has focused on combining the obtained results from different studies on different active ingredients with differences in experimental designs, analysts and analysis equipment. In this paper, we present a meta-analysis of response ratios as a possible method of combining and quantifying effects of food processing on pesticide residue levels. Reduction of residue levels was indicated by blanching, boiling, canning, frying, juicing, peeling and washing of fruits and vegetables with an average response ratio ranging from 0.10 to 0.82. Baking, boiling, canning and juicing indicated both reduction and increases for the 95% and 99.5% confidence intervals.

  8. Meta-analysis of food processing on pesticide residues in fruits.

    Liang, Y; Liu, Y; Ding, Y; Liu, X J

    2014-01-01

    The combining and quantifying effects of food processing on pesticide residues in fruits were analysed by a meta-analysis approach. Data were collected from many publications and used to calculate response ratios, confidence intervals and intra-assay coefficients of variation. The response ratios for washing by tap water, boiling and sun drying were 0.59, 0.71 and 0.65, respectively, indicating that they could reduce the pesticide residues effectively. Peeling and juicing, where response ratios were 0.11 and 0.14, respectively, showed they could reduce the pesticide residues to a very small extent. An increase of pesticide residues was indicated by oven drying with a response ratio of more than 1. Oven drying and sun drying indicated both a reduction and an increase at the 99.5% confidence interval. The response ratios given by a meta-analysis approach could be used as processing factors in food safety risk assessment and as a guide for consumers on how to reduce pesticides effectively in fruit.

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

    Sheheli Islam

    2009-01-01

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

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

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

    2013-01-01

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

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

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

    2005-01-01

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

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

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

    2013-01-01

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

  13. Use of Carbon Nanotubes for the Analysis of Pesticide Residues in Fruits and Vegetables.

    Abdulrauf, Lukman Bola; Tan, Guan Huat

    2016-11-01

    This review presents the application of carbon nanotubes as sorbent materials in the analysis of pesticide residues in fruits and vegetables. The advantages, limitations, and challenges of carbon nanotubes, with respect to their use in analytical chemistry, are presented. The efficiency of their application as extraction sorbent materials (in terms of LOD, LOQ, linearity, relative recovery, and RSD) in SPE, solid-phase microextraction, multi-plug filtration clean-up, matrix solid-phase dispersion, and the quick, easy, cheap, effective, rugged and safe method is reported. The synthesis, functionalization, purification, and characterization methods of carbon nanotubes are also discussed.

  14. Codex alimentarius approach to pesticide residue standards.

    Maybury, R B

    1989-01-01

    To protect consumers' health, most countries have maximum legal limits for pesticide residues in foods. Trade difficulties can arise when limits differ between countries. The Codex Alimentarius Commission was established in 1962 to implement the Joint FAO/WHO Food Standards Programme, the purpose of which is to protect consumer health and ensure fair practices in international food trade. The Codex Committee on Pesticide Residues (CCPR), an intergovernmental body which advises the Commission on matters related to pesticide residues, is responsible for establishing maximum residue limits (MRLs) for pesticides in foods and feeds that move in international trade. Codex MRLs are based on residue data obtained mainly from supervised trials that reflect approved pesticide use in accordance with "good agricultural practice." MRLs must be toxicologically acceptable in terms of estimated pesticide intake by consumers. CCPR Working Groups examine problems related to establishing and implementing MRLs, including sampling and methods of analysis. Despite time and effort expended, acceptance and application of Codex MRLs face many problems in international trade.

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

    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.

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

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

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

    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 μg/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 μg/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 μg/g) in all 40 samples of Basmati rice grains and soil. It was also observed as BDL (<0.001-0.05 μg/L) for 12 water samples (2009-2010). The residues of tricyclazole, propioconazole, chlorpyrifos, hexaconazole, pretilachlor, and λ-cyhalothrin were also found as BDL (<0.001-0.05 μg/g) in 40 samples of Basmati rice grains and soil and 12 water samples (<0.001-0.05 μg/L) (2010-2011).

  18. Evaluation of pesticide residues in fruits and vegetables from Algeria.

    Mebdoua, Samira; Lazali, Mohamed; Ounane, Sidi Mohamed; Tellah, Sihem; Nabi, Fahima; Ounane, Ghania

    2017-01-17

    A total of 160 samples of 13 types of fresh fruits and vegetables from domestic production and import were analysed to detect the presence of pesticide residues. Analysis was performed by multi-residual extraction followed by gas chromatography-mass spectrometry. In 42.5% of the tested samples, no residues were found and 12.5% of samples contained pesticide residues above maximum residue limits. Risk assessment for long-term exposure was done for all pesticides detected in this study. Except chlorpyrifos and lambda-cyhalothrin, exposure to pesticides from vegetables and fruits was below 1% of the acceptable daily intake. Short-term exposure assessment revealed that in seven pesticide/commodity combinations, including three pesticides (chlorpyrifos, deltamethrin and lambda-cyhalothrin), the acute reference dose had been exceeded.

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

    Alder, Lutz

    2011-01-01

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

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

    Mukherjee, S.

    2015-12-01

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

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

    Ana M Domínguez

    2014-04-01

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

  2. Analysis of pesticide residues in tobacco with online size exclusion chromatography with gas chromatography and tandem mass spectrometry.

    Guo, Weiyun; Bian, Zhaoyang; Tang, Gangling; Wang, Deguo; Li, Guanghui; Wang, Jianlong

    2016-07-01

    An ultrasensitive method for the simultaneous analysis of pesticides residues in tobacco was developed with online size exclusion chromatography with gas chromatography and tandem mass spectrometry. Tobacco samples were extracted with the solvent mixture of cyclohexane and acetone (7:3, v/v) and centrifuged. Then, the supernatant liquors were injected directly into the online size exclusion chromatography with gas chromatography and tandem mass spectrometry without any other purification procedures after being filtered with a 0.22 μm organic phase filter. The matrix interferences were effectively removed and recoveries of most pesticides were in the range of 72-121%. Especially, for chlorothalonil, the analysis efficiency of this method was much more favorable than that of the general method, in which dispersive solid-phase extraction was used as an additional purified procedure. In addition, the limits of quantitation of this method were from 1 to 50 μg/kg. Therefore, a rapid, cost-effective, labor-saving method was proposed in the present work, which was suitable for the analysis of 41 pesticide residues in tobacco.

  3. New Trends in Pesticide Residue Analysis in Cereals, Nutraceuticals, Baby Foods, and Related Processed Consumer Products.

    Raina-Fulton, Renata

    2015-01-01

    Pesticide residue methods have been developed for a wide variety of food products including cereal-based foods, nutraceuticals and related plant products, and baby foods. These cereal, fruit, vegetable, and plant-based products provide the basis for many processed consumer products. For cereal and nutraceuticals, which are dry sample products, a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method has been used with additional steps to allow wetting of the dry sample matrix and subsequent cleanup using dispersive or cartridge format SPE to reduce matrix effects. More processed foods may have lower pesticide concentrations but higher co-extracts that can lead to signal suppression or enhancement with MS detection. For complex matrixes, GC/MS/MS or LC/electrospray ionization (positive or negative ion)-MS/MS is more frequently used. The extraction and cleanup methods vary with different sample types particularly for cereal-based products, and these different approaches are discussed in this review. General instrument considerations are also discussed.

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

    Oellig, Claudia

    2016-05-06

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

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

    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 μg 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.

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

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

    2014-01-01

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

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

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

    2016-02-01

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

  8. Earthworm tolerance to residual agricultural pesticide contamination

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

    2014-01-01

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

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

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

    2014-01-01

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

  10. Liquid chromatography-high-resolution mass spectrometry for pesticide residue analysis in fruit and vegetables: screening and quantitative studies.

    Gómez-Ramos, M M; Ferrer, C; Malato, O; Agüera, A; Fernández-Alba, A R

    2013-04-26

    This work reviews the current state-of-the-art of liquid chromatography coupled to high-resolution mass spectrometry (LC-HRMS) techniques applied to the analysis of pesticides in fruit-based and vegetable-based matrices. Nowadays, simultaneous trace analysis of hundreds of pesticides from different classes is required, preferably in just one run. The most commonly used QqQ-MS technology presents certain limitations in its application in a cost and effective way when analyzing a large number of pesticides. Thus, this review includes HRMS technology as a reliable complementary alternative allowing the analysis of a wide range of pesticides in food. Its capabilities and limitations in identifying, confirming and quantifying pesticides are discussed. HRMS instruments can adequately address such issues; however, the main drawbacks are as a result of insufficient prior optimization of the operational parameters during non-target analysis in full-scan mode and due to software shortcomings.

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

    This study demonstrates the application of a novel lipid removal product to the residue analysis of 65 pesticides and 52 environmental contaminants in kale, pork, salmon, and avocado by fast, low pressure gas chromatography – tandem mass spectrometry (LPGC-MS/MS). Sample preparation involves QuEChE...

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

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

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

    European Food Safety Authority

    2014-05-01

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

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

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

    2015-11-01

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

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

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

    2013-10-01

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

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

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

    2016-08-01

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

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

    DRAGAN MARKOVIC

    2007-08-01

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

  18. Rapid screening and quantification of residual pesticides and illegal adulterants in red wine by direct analysis in real time mass spectrometry.

    Guo, Tianyang; Fang, Pingping; Jiang, Juanjuan; Zhang, Feng; Yong, Wei; Liu, Jiahui; Dong, Yiyang

    2016-11-04

    A rapid method to screen and quantify multi-class analytic targets in red wine has been developed by direct analysis in real time (DART) coupled with triple quadruple tandem mass spectrometry (QqQ-MS). A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure was used for increasing analytical speed and reducing matrix effect, and the multiple reaction monitoring (MRM) in DART-MS/MS ensured accurate analysis. One bottle of wine containing 50 pesticides and 12 adulterants, i.e., preservatives, antioxidant, sweeteners, and azo dyes, could be totally determined less than 12min. This method exhibited proper linearity (R(2)≥0.99) in the range of 1-1000ng/mL for pesticides and 10-5000ng/mL for adulterants. The limits of detection (LODs) were obtained in a 0.5-50ng/mL range for pesticides and 5-50ng/mL range for adulterants, and the limits of quantification (LOQs) were in a 1-100ng/mL range for pesticides and 10-250ng/mL range for adulterants. Three spiked levels for each analyte in wine were evaluated, and the recoveries were in a scope of 75-120%. The results demonstrated DART-MS/MS was a rapid and simple method, and could be applied to rapid analyze residual pesticides and illegal adulterants in a large quantities of red wine.

  19. Rocky Mountain Arsenal National Wildlife Refuge sampling and analysis plan : bison pesticide residue study

    US Fish and Wildlife Service, Department of the Interior — The purpose of this Sampling and Analysis Plan (SAP) is to demonstrate that dieldrin concentrations in bison tissues from the Rocky Mountain Arsenal National...

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

    Terence Centner

    2014-05-01

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

  1. Three years monitoring survey of pesticide residues in Sardinia wines following integrated pest management strategies.

    Angioni, Alberto; Dedola, Fabrizio

    2013-05-01

    This paper reports the results of a pesticide monitoring survey on wine grapes from the 2008-2010 vintage from vineyards grown according to integrated pest management strategies. A multi-residue gas chromatography-mass spectrometry method in electron ionization and chemical ionization mode has been used for the determination of 30 pesticides in wine samples. The analytical method showed good recoveries and allowed a good separation of the selected pesticides. Repeatability and intermediate precision showed good results with CV < 20 %. The instrumental method limits of determination (LOD) and of quantification (LOQ) were below the maximum residue levels set in wine. The analysis of the wines showed that pesticide residues were below the instrumental LOQ, and most of them were undetectable (pesticide applied has been detected in at least one cultivar. Metalaxil, myclobutanil, and penconazole were the pesticides most frequently found, while carignano and vermentino were the cultivars with the higher number of residues.

  2. Automated multi-plug filtration cleanup for liquid chromatographic-tandem mass spectrometric pesticide multi-residue analysis in representative crop commodities.

    Qin, Yuhong; Zhang, Jingru; Zhang, Yuan; Li, Fangbing; Han, Yongtao; Zou, Nan; Xu, Haowei; Qian, Meiyuan; Pan, Canping

    2016-09-01

    An automated multi-plug filtration cleanup (m-PFC) method on modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts was developed. The automatic device was aimed to reduce labor-consuming manual operation workload in the cleanup steps. It could control the volume and the speed of pulling and pushing cycles accurately. In this work, m-PFC was based on multi-walled carbon nanotubes (MWCNTs) mixed with other sorbents and anhydrous magnesium sulfate (MgSO4) in a packed tip for analysis of pesticide multi-residues in crop commodities followed by liquid chromatography with tandem mass spectrometric (LC-MS/MS) detection. It was validated by analyzing 25 pesticides in six representative matrices spiked at two concentration levels of 10 and 100μg/kg. Salts, sorbents, m-PFC procedure, automated pulling and pushing volume, automated pulling speed, and pushing speed for each matrix were optimized. After optimization, two general automated m-PFC methods were introduced to relatively simple (apple, citrus fruit, peanut) and relatively complex (spinach, leek, green tea) matrices. Spike recoveries were within 83 and 108% and 1-14% RSD for most analytes in the tested matrices. Matrix-matched calibrations were performed with the coefficients of determination >0.997 between concentration levels of 10 and 1000μg/kg. The developed method was successfully applied to the determination of pesticide residues in market samples.

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

    Gómez-Almenar, M. C.

    2015-06-01

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

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

    Husniye Imamoglu

    2016-01-01

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

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

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

    2015-01-01

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

  6. Organochlorine Pesticide Residues in the Processing of Pressed Cheese

    Dorin Ţibulcă

    2015-11-01

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

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

    Francisco Sanchez-Bayo

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

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

    Sanchez-Bayo, Francisco; Goka, Koichi

    2014-01-01

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

  9. Analysis of eight organophosphorus pesticide residues in fresh vegetables retailed in agricultural product markets of Nanjing, China.

    Wang, Ligang; Liang, Yongchao; Jiang, Xin

    2008-10-01

    A method to effectively remove pigments in fresh vegetables using activated carbon followed cleanup through solid phase extraction (SPE) cartridge to further reduce matrix interference and contamination, was established to determine eight organophosphorous pesticides (OPPs) by gas chromatography (GC) with nitrogen-phosphorus detection (NPD) in this study, and it has been successfully applied for the determination of eight OPPs in various fresh vegetables with the recoveries ranging from 61.8% to 107%. To evaluate eight OPPs residue level, some fresh vegetables retailed at three agricultural product markets (APM) of Nanjing in China were detected, the results showed that phorate in Shanghai green (0.0257 microg g(-1)) and Chinese cabbage (0.0398 microg g(-1)), dimethoate in Shanghai green (0.0466-0.0810 microg g(-1)), Chinese cabbage (0.077 microg g(-1)), and spinach (0.118-0.124 microg g(-1)), methyl-parathion in Shanghai green (0.0903 microg g(-1)), Chinese cabbage (0.157 microg g(-1)), and spinach (0.0924 microg g(-1)), malathion in Shanghai green (0.0342-0.0526 microg g(-1)), chorpyrifos in spinach (0.106-0.204 microg g(-1)), and Chinese cabbage (0.149 microg g(-1)), chlorfenvinfos in carrot (0.094-0.131 microg g(-1)), were found. However, fonofos and fenthion were not detected in all the collected vegetable samples.

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

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

    2012-08-17

    In this study, a new gas chromatography-mass spectrometry (GC-MS) method, using the very selective negative chemical ionization (NCI) mode, was developed and applied in combination with a modified acetonitrile-based extraction method (QuEChERS) for the analysis of a large number of pesticide residues (51 pesticides, including isomers and degradation products) in green coffee beans. A previously developed integrated sample homogenization and extraction method for both pesticides and mycotoxins analysis was used. An homogeneous slurry of green milled coffee beans and water (ratio 1:4, w/w) was prepared and extracted with acetonitrile/acetic acid (1%), followed by magnesium sulfate addition for phase separation. Aliquots from this extract could be used directly for LC-MS/MS analysis of mycotoxins and LC-amenable pesticides. For GC-MS analysis, a further clean-up was necessary. C18- and PSA-bonded silica were tested as dispersive solid-phase extraction (d-SPE) sorbents, separate and as a mixture, and the best results were obtained using C18-bonded silica. For the optimal sensitivity and selectivity, GC-MS detection in the NCI-selected ion monitoring (SIM) mode had to be used to allow the fast analysis of the difficult coffee bean matrix. The validation was performed by analyzing recovery samples at three different spike concentrations, 10, 20 and 50 μg kg(-1), with 6 replicates (n=6) at each concentration. Linearity (r(2)) of calibration curves, estimated instrument and method limits of detection and limits of quantification (LOD(i), LOD(m), LOQ(i) and LOQ(m), respectively), accuracy (as recovery %), precision (as RSD%) and matrix effects (%) were determined for each individual pesticide. From the 51 analytes (42 parent pesticides, 4 isomers and 5 degradation products) determined by GC-MS (NCI-SIM), approximately 76% showed average recoveries between 70-120% and 75% and RSD ≤ 20% at the lowest spike concentration of 10 μg kg(-1), the target method LOQ. For the

  11. Rapid analysis of multi-pesticide residues in lotus seeds by a modified QuEChERS-based extraction and GC-ECD.

    Miao, Qing; Kong, Weijun; Yang, Shihai; Yang, Meihua

    2013-05-01

    A modified quick, easy, cheap, efficient, rugged and safe method (QuEChERS) coupled to gas chromatography with electron capture detector (GC-ECD) was developed for rapid extraction and simultaneous determination of 36 pesticides in lotus seeds. The extraction solvent (acetone, ethyl acetate, acetonitrile, n-hexane and n-hexane in combination with ethyl acetate) and purifying agent (neutral alumina, primary secondary amine, graphite carbon block and florisil) for QuEChERS extraction were optimized. The GC-ECD method was in-house validated in terms of linearity, selectivity, reproducibility, stability and recovery. The limits of detection (LODs) of the developed GC-ECD method for all investigated pesticides ranged from 0.01 to 3.0μgL(-1) and limits of quantification (LOQs) from 0.05 to 10.0μgL(-1). The satisfactory data demonstrated the good reproducibility and stability of the method with relative standard deviations (RSDs) lower than 15%. Recoveries for spiked lotus seed samples were from 60.84% to 119.91% with RSDs lower than 13.06%. Two out of 24 batches of lotus seeds collected in China were found to be contaminated with trans-chlordane, which were below LOQ. This is the first attempt in China using QuEChERS to GC-ECD to determine 36 major pesticides with differences in physio-chemical properties in lotus seeds. The method described here was found to be practicable in the routine residue analysis of pesticides in lotus seeds.

  12. Rapid analysis of pesticide residues in drinking water samples by dispersive solid-phase extraction based on multiwalled carbon nanotubes and pulse glow discharge ion source ion mobility spectrometry.

    Zou, Nan; Gu, Kejia; Liu, Shaowen; Hou, Yanbing; Zhang, Jialei; Xu, Xiang; Li, Xuesheng; Pan, Canping

    2016-03-01

    An analytical method based on dispersive solid-phase extraction with a multiwalled carbon nanotubes sorbent coupled with positive pulse glow discharge ion mobility spectrometry was developed for analysis of 30 pesticide residues in drinking water samples. Reduced ion mobilities and the mass-mobility correlation of 30 pesticides were measured. The pesticides were divided into five groups to verify the separation capability of pulse glow discharge in mobility spectrometry. The extraction conditions such as desorption solvent, ionic strength, conditions of adsorption and desorption, the amounts of multiwalled carbon nanotubes, and solution pH were optimized. The enrichment factors of pesticides were 5.4- to 48.7-fold (theoretical enrichment factor was 50-fold). The detection limits of pesticides were 0.01∼0.77 μg/kg. The linear range was 0.005-0.2 mg/L for pesticide standard solutions, with determination coefficients from 0.9616 to 0.9999. The method was applied for the analysis of practical and spiked drinking water samples. All results were confirmed by high-performance liquid chromatography with tandem mass spectrometry. The proposed method was proven to be a commendably rapid screening qualitative and semiquantitative technique for the analysis of pesticide residues in drinking water samples on site.

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

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

    2008-12-01

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

  14. Organochlorine pesticide residues in the northern Indian Ocean

    Shailaja, M.S.; Sarkar, A.

    periodic monitoring of the levels of the major pollutants. One on-going exercise has been to evaluate, qualitatively and quantitatively, the persistent organochlorine pesticide residues in the Northern Indian Ocean. The baseline levels of some...

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

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

    2009-01-01

    -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......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...

  16. Pesticide residues screening in wine by mass spectrometry

    Machado Andrea F.

    2016-01-01

    Full Text Available Recently, a study (from PAN Europe covered 40 bottles of wine – 34 conventional and six organic ones – purchased inside the EU. According to the results, the 34 bottles of conventional wine together contained 148 pesticide residues. All 34 bottles contained from one to ten pesticides, bringing the average per bottle to more than four. Of the six bottles of organic wine tested, one sample contained a low concentration of a possibly carcinogenic pesticide. According to PAN Europe, the “contamination of wines is a direct result of over-reliance on pesticides in grape production”. This study, between others, to prove the importance of develop methods sensivity and confident for pesticide detection in wine. A multi-residue method was developed for the determination ca of 250 pesticide residues in wine using Quechers extraction, gas chromatography-tandem mass spectrometry (GC-MS-MS and liquid chromatography-tandem mass spectrometry (LC-MS-MS. The method was validated with the evaluation of follow parameters: Linearity, Precision, Accuracy, Matrix effect, Limit of detection and Limit of Quantification. The method was approved and was able to quantify pesticide residues in more than 60 samples of wine.

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

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

    2015-11-01

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

  18. A novel device based on a fluorescent cross-responsive sensor array for detecting pesticide residue

    Huang, Jing; Hou, Changjun; Lei, Jincan; Huo, Danqun; Luo, Xiaogang; Dong, Liang

    2016-11-01

    In this paper, a novel, simple, rapid, and low-cost detection device for pesticide residue was constructed. A sensor array based on a cross-responsive mechanism was designed. The data collection and processing system was used to detect fluorescent signal of the sensor arrays, and to extract unique patterns of the tested pesticide residue. Four selected pesticides, carbendazim, diazine, fenvalerate, and pentachloronitrobenzene, were detected by the proposed device. Unsupervised pattern recognition methods, hierarchical cluster analysis and principal component analysis, were used to analyze the data. The results showed that the methods could 100% discriminate the four pesticide residues. According to the standard regression linear curve of the fluorescence intensity and the concentration of pesticide, the quantitative value of the pesticide was detected, and the device obtained responses at concentrations below 8 ppb, and it has a good linear relationship in the range of 0.01-1 ppm. According to the results, the proposed detection device showed excellent selectivity and discrimination ability for the pesticide residues. However, our preliminary study demonstrated that the proposed detection device has excellent potential application for the safety inspection of food.

  19. 40 CFR 158.2172 - Experimental use permit microbial pesticides residue data requirements table.

    2010-07-01

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

  20. 40 CFR 158.2130 - Microbial pesticides residue data requirements table.

    2010-07-01

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

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

    Poulsen, Mette Erecius; Naef, A.; Gasser, S.;

    2009-01-01

    % 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......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....... 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...

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

    Cervera, M I; Portolés, T; Pitarch, E; Beltrán, J; Hernández, F

    2012-06-29

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

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

    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.

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

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

    2015-11-01

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

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

    Neff Roni A

    2012-01-01

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

  6. Analysis on monitoring results of multi-pesticide residues in vegetables in Anshan City in 2011%2011年鞍山市蔬菜中多种农药残留监测结果分析

    李晨光; 魏欧

    2013-01-01

    目的 了解鞍山市蔬菜食品中有机磷、氨基甲酸酯及拟除虫菊酯农药残留的情况.方法 按GB/T 5009-2003《食品卫生检验方法理化部分》检测有机磷、氨基甲酸酯及拟除虫菊酯农药残留量.结果 100份蔬菜中检出甲胺磷农药残留4份,乙酰甲胺磷农药残留4份,毒死蜱农药残留10份,克百威农药残留6份,灭多威农药残留20份,氯氰菊酯农药残留14份,氯氟氰菊酯农药残留2份,均无超标样品.结论 鞍山市蔬菜中农药残留水平较低.%[Objective]To know the condition of residues of organophosphorous pesticide, carbamate and pyrethroid in vegetables in Anshan City. [ Methods]The contents of residues of organophosphorous pesticide, carbamate and pyrethroid were detected according to the Methods of food hygienic analysis-Physical and chemical section ( GB/T 5009-2003). [Results] Among 100 samples of vegetables, there were 4 samples of methamidophos residue, 4 samples of acephate residue, 10 samples of chlorpyrifos residue, 6 samples of carbofuran residue, 20 samples of methomyl residue, 14 samples of cypermethrin residue and 2 samples of cyhalothrin residue, while no over standard samples were found. [ Conclusion] The level of pesticide residues in vegetables is low in Anshan City.

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

    Mekonen, Seblework; Ambelu, Argaw; Spanoghe, Pieter

    2015-09-30

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

  8. 76 FR 2110 - Notice of Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on...

    2011-01-12

    ...This notice announces the Agency's receipt of an initial filing of a pesticide petition proposing the establishment or modification of regulations for residues of pesticide chemicals in or on various...

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

    Fernandes, Virgínia C; Lehotay, Steven J; Geis-Asteggiante, Lucía; Kwon, Hyeyoung; Mol, Hans G J; van der Kamp, Henk; Mateus, Nuno; Domingues, Valentina F; Delerue-Matos, Cristina

    2014-01-01

    This study analysed 22 strawberry and soil samples after their collection over the course of 2 years to compare the residue profiles from organic farming with integrated pest management practices in Portugal. For sample preparation, we used the citrate-buffered version of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. We applied three different methods for analysis: (1) 27 pesticides were targeted using LC-MS/MS; (2) 143 were targeted using low pressure GC-tandem mass spectrometry (LP-GC-MS/MS); and (3) more than 600 pesticides were screened in a targeted and untargeted approach using comprehensive, two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOF-MS). Comparison was made of the analyses using the different methods for the shared samples. The results were similar, thereby providing satisfactory confirmation of both similarly positive and negative findings. No pesticides were found in the organic-farmed samples. In samples from integrated pest management practices, nine pesticides were determined and confirmed to be present, ranging from 2 µg kg(-1) for fluazifop-p-butyl to 50 µg kg(-1) for fenpropathrin. Concentrations of residues in strawberries were less than European maximum residue limits.

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

    Judy Y Wu

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

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

    Spiridon Kintzios

    2008-04-01

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

  12. Bioeconomic Analysis of Pesticide Demand

    Moffitt, L. Joe; Farnsworth, Richard L.

    1981-01-01

    The ability of insects to develop resistance to specific pesticides affects pesticide demand. However, the affect of resistance on demand cannot be observed or measured. This analysis substitutes an expression for the unobserved resistance variable in a pesticide demand model and then illustrates the model's potential by estimating demand for DDT. To arrive at the expression characterizing the unobserved resistance variable a biological resistance model is constructed then incorporated into t...

  13. Application of Dispersive Liquid-liquid Microextraction in Pesticide Residue Analysis of Samples Pretreatment%分散液相微萃取技术在农药残留分析样品前处理中的应用

    田海; 罗金辉; 谢德芳; 吕岱竹

    2013-01-01

    介绍了分散液相微萃取技术的原理和影响萃取效率的因素,重点关注了其最近几年在农药残留中的研究和应用情况,并探讨了应用前景,以期能够为该技术在农药残留分析方面的应用提供参考.%The principles of dispersive liquid-liquid microextraction(DLLME) and the factors that affect the extraction efficiency were introduced, the investigations and applications of DLLME in pesticide residue analysis in recent years were focused on, and the future of the technique was prospected. As a result, it could provide a reference about the application of DLLME in pesticide residue analysis.

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

    Nema S. Shaban

    2016-03-01

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

  15. Application of gas chromatography/tandem quadrupole mass spectrometry to the multi-residue analysis of pesticides in green leafy vegetables.

    Walorczyk, Stanisław

    2008-12-01

    A new, sensitive and specific method has been developed for the simultaneous determination of 129 pesticides in lettuce and other green leafy vegetables. The samples were extracted with acetonitrile and co-extractives such as fatty acids and pigments were removed using dispersive solid-phase extraction (dispersive-SPE) with primary secondary amine (PSA) and graphitized carbon black (GCB). All pesticides were analyzed in a single injection gas chromatography/tandem quadrupole mass spectrometry (GC/MS/MS) acquisition method. Two multiple reaction monitoring (MRM) transitions of precursor ions fragmenting into product ions were recorded for the targeted pesticides, thus fulfilling the EU identification points system criteria for the identification of contaminants (2002/657/EC). Calibration curves were determined using matrix-matched standards, and exhibited excellent linearity at two orders of magnitude from 0.005 to 0.5 mg/kg for almost all the pesticides studied (R(2) > or = 0.99). The analytical performance was demonstrated by the analysis of lettuce samples spiked at five concentration levels ranging from 0.005 to 0.5 mg/kg for each pesticide. The recovery and repeatability results satisfied SANCO/2007/3131 criteria (i.e. average recoveries were in the range 70-120% with RSDs vegetable samples such as lettuce, cabbage and leek.

  16. Bioenergy residues as novel sorbents to clean up pesticide pollution

    Mukherjee, Santanu

    2016-04-01

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

  17. Pesticide residues in passifloras crops in regions of high production in Colombia

    Dario A. Bastidas

    2013-08-01

    Full Text Available As one of the most bio-diverse countries in the world, Colombia boasts a wide diversity of highly palatable tropical fruits. Even though Colombian fruit production has primarily targeted the domestic market, several fruit species, such as passion fruit (PassifloraSpp, are steadily gaining ground in the broader international arena.  Production of these crops and respond to raising domestic and international demand, many Colombian small-scale farmers use pesticides for pest and disease control. Inadequate use of pesticides could possibly entail public health risks, environmental contamination and ultimately interfere with international trade. Surveys were carried out to passifloras producers of three spices of passiflora crops, yellow passion fruit, sweet passion fruit and purple passion fruit  from the largest producers municipalities in Colombia with the aim to know the integrate pest control and agricultural practices related with pesticides applied in the crops. Ramdomly sampling was realized and samples were analyzed by multiresidue analysis methodology validated in the laboratory and based on IAEA-QuEChERS method. With the results of survey and laboratory analysis it is showed the presence of pesticide residues that exceed maximum residue limits in some samples and the pesticides identified in the samples correspond to those used by farmers. It was found that the presence of residues is mainly due to the shortcomings in the proper use of agricultural practices related primarily to the implementation of agricultural products no registered for such crops.

  18. Organochlorine pesticide residues in cow's milk and butter in Mexico.

    Waliszewski, S M; Pardío, V T; Waliszewski, K N; Chantiri, J N; Aguirre, A A; Infanzón, R M; Rivera, J

    1997-12-03

    This monitoring study of 355 samples of cow's milk collected from the central region of Veracruz state and 448 samples of national butter brands was conducted to determine the contamination levels of organochlorine pesticides. The results obtained for mean HCH levels were 0.094 and 0.093 mg/kg on fat basis in cow's milk and butter samples, respectively. The mean DDT levels were 0.159 and 0.049 mg/kg, respectively. In relation to cow's milk, the total HCH levels in Veracruz state were higher but total DDT levels were comparable to those reported in other countries. On the other hand, organochlorine levels detected in national brand butter samples were lower than those found in other countries, where these pesticides are still used in sanitary actions. These results confirmed that dairy products in Mexico presented organochlorine pesticide residues (owing to their use in sanitary actions) indicating a human exposure through these food products.

  19. Pesticide residues in fruits and vegetables in Ghana: a review.

    Donkor, Augustine; Osei-Fosu, Paul; Dubey, Brajesh; Kingsford-Adaboh, Robert; Ziwu, Cephas; Asante, Isaac

    2016-10-01

    Pesticides are known to improve agriculture yield considerably leading to an increase in its application over the years. The use of pesticides has shown varying detrimental effects in humans as well as the environment. Presently, enough evidence is available to suggest their misuse and overuse in the last few decades in most developing nations primarily due to lack of education, endangering the lives of farmers as well as the entire population and environment. However, there is paucity of data especially over long durations in Ghana resulting in the absence of effective monitoring programs regarding pesticide application and subsequent contamination in fruits and vegetables. Therefore, this review discusses comprehensively pesticide type and use, importation, presence in fruits and vegetables, human exposure, and poisoning in Ghana. This is to alert the scientific community in Ghana of the need to further research into the potential implications of pesticide residues in food commodities in order to generate a comprehensive and reliable database which is key in drafting policies simultaneous with food regulation, suitable monitoring initiatives, assessment, and education to minimize their effects thereon.

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

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

    2015-08-01

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

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

    Korrapati Kotinagu

    2015-04-01

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

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

    Sarah Blankson-Arthur

    2011-06-01

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

  3. Screening of the presence organophosphates and organochlorines pesticide residues in vegetables and fruits using gas chromatography-mass spectrometry

    Putri, Dillani; Aryana, Nurhani; Aristiawan, Yosi; Styarini, Dyah

    2017-01-01

    Pesticides is commonly used to improve the quality of agricultural product, especially in vegetables and fruits. Due to pesticide residues in the product become a concern to consumer health, monitoring and analysis of pesticide residues in agriculture product need to be established. The certified reference material (CRM) is often benefited to obtain accurate results in analysis. It is required as the quality control to improve quality assurance of the testing results. Unfortunately in Indonesia, the development of matrix CRM for the analysis of pesticide residues in vegetables and fruits is still limited. This study is aimed to determine the type of commodity and target analyte to be employed in the development of CRM for pesticides in vegetables and fruits. As the preliminary study, the screening of 11 commodities of fresh vegetables and fruits has been conducted to review the information about the presence of organophosphates (OPs) and organochlorines (OCs) in the sample. In this analysis, QuEChERS technique was used in the extraction process and the qualitative analysis was evaluated by using GC-MS. The results showed that strawberry and celery contain residues of pesticide chlorpyrifos. Further analysis of the commodity celery from seven different places has been conducted, resulting that from 3 of all 7 samples (43%) were positive containing chlorpyrifos. Therefore, the development of CRM for chlorpyrifos in celery will be our next research project.

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

    Chung, Stephen W C; Chan, Benny T P

    2010-07-16

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

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

    Mol, H.G.J.; Rooseboom, A.; Dam, R. van; 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 μL) injecti

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

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

    2007-01-01

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

  7. Multi-residue analysis of pesticides, plant hormones, veterinary drugs and mycotoxins using HILIC chromatography - MS/MS in various food matrices.

    Danezis, G P; Anagnostopoulos, C J; Liapis, K; Koupparis, M A

    2016-10-26

    One of the recent trends in Analytical Chemistry is the development of economic, quick and easy hyphenated methods to be used in a field that includes analytes of different classes and physicochemical properties. In this work a multi-residue method was developed for the simultaneous determination of 28 xenobiotics (polar and hydrophilic) using hydrophilic interaction liquid chromatography technique (HILIC) coupled with triple quadrupole mass spectrometry (LC-MS/MS) technology. The scope of the method includes plant growth regulators (chlormequat, daminozide, diquat, maleic hydrazide, mepiquat, paraquat), pesticides (cyromazine, the metabolite of the fungicide propineb PTU (propylenethiourea), amitrole), various multiclass antibiotics (tetracyclines, sulfonamides quinolones, kasugamycin and mycotoxins (aflatoxin B1, B2, fumonisin B1 and ochratoxin A). Isolation of the analytes from the matrix was achieved with a fast and effective technique. The validation of the multi-residue method was performed at the levels: 10 μg/kg and 100 μg/kg in the following representative substrates: fruits-vegetables (apples, apricots, lettuce and onions), cereals and pulses (flour and chickpeas), animal products (milk and meat) and cereal based baby foods. The method was validated taking into consideration EU guidelines and showed acceptable linearity (r ≥ 0.99), accuracy with recoveries between 70 and 120% and precision with RSD ≤ 20% for the majority of the analytes studied. For the analytes that presented accuracy and precision values outside the acceptable limits the method still is able to serve as a semi-quantitative method. The matrix effect, the limits of detection and quantification were also estimated and compared with the current EU MRLs (Maximum Residue Levels) and FAO/WHO MLs (Maximum Levels) or CXLs (Codex Maximum Residue Limits). The combined and expanded uncertainty of the method for each analyte per substrate, was also estimated.

  8. Study of Organochlorinated Pesticide Residues and Polychlorinated Biphenyls in Soil Samples

    MSc. Vlora Gashi

    2013-12-01

    Full Text Available This paper presents and discusses the data obtained for organochlorinated pesticides and their residues in the soil samples of agricultural areas. Soil contamination is one of most important factors influencing the quality of agricultural products. Usage of heavy farm equipment, the land drainage, an exces­sive application of agrochemicals, emissions originating from mining, metallurgical, and chemical and coal power plants and transport, all generate a number of undesired substances (nitric and sulphur oxides, PAHs, heavy metals, pesticides, which after deposition in soil may influence crop quality. Thus, input of these contaminants into the environment should be carefully monitored. Levels of organochlorinated pesticides contamination were evaluated in agriculture areas that are in use. 10 soil samples were taken in agricultural areas  Plane of  Dugagjini , Kosovo. Representa­tive soil samples were collected from 0-30 cm top layer of the soil. In the analytical method we combined ultrasonic bath extraction and a Florisil column for samples clean-up. The analysis of the organochlorinated pesticides in soil samples was performed by gas chromatography technique using electron capture detector (GC/ECD. Optima-5 (low/mid polarity, 5% phenyl methyl siloxane 60 m x 0.33 mm x 0.25μm film capillary column was used for isolation and determination of organochlorinated pesticides. Low concentrations of organochlorinated pesticide and their metabolites were found in the studied samples. The presence of organochlorinated pesticides and their residues is probably resulting of their previous uses for agricultural purposes.

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

    冷静; 邓斌; 李琦华; 杨舒黎; 苟潇; 毛华明

    2011-01-01

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

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

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

    2013-04-01

    estimated. Recoveries were above 70% for all pesticides. Good linear relationships of the calibration curves (0.01-1 μg mL-1) were obtained for all the compounds by the two analytical methods with regression coefficients (r2) higher than 0.99 in the range of concentrations studied. Detection limits were 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.

  11. [Study on experiment of absorption spectroscopy detection of pesticide residues of carbendazim in orange juice].

    Ji, Ren-Dong; Chen, Meng-Lan; Zhao, Zhi-Min; Zhu, Xing-Yue; Wang, Le-Xin; Liu, Quan-Jin

    2014-03-01

    Absorption spectra were studied for the carbendazim, in the mixed solution of orange juice and carbendazim using spectrophotometer. The most intensive characteristic peak (285 nm) was found in the spectrum of carbendazim standard solution. Compared with the carbendazim drug solution, the peak position of absorption spectrum has the blue shift (285-280 nm) when carbendazim (0.28 mg x mL(-1))was added in the orange juice. So that we can conclude that interaction happened between the orange juice and carbendazim. Through the method of least squares fitting, the prediction models between the absorbance of orange juice and carbendazim content was obtained with a good linear relationship. The linear function model was: I = 2.41 + 9.26x, the correlation coefficient was 0.996, and the recovery was: 81%-102%. According to the regression model, we can obtain the amount of carbendazim pesticide residues in orange juice. It was verified that the method of using ultraviolet-visible absorption spectra was feasible to detect the carbendazim residues in orange juice. The result proved that it is possible to detect pesticide residues of carbendazim in orange juice, and it can meet the needs of rapid analysis. This study provides a new way for the detection of pesticide residues.

  12. 76 FR 69692 - Withdrawal of a Pesticide Petition for Residues of Pesticide Chemicals in or on Various Commodities

    2011-11-09

    ... 23, 2010 (75 FR 57942) (FRL-8845-4), which announced the submission of a pesticide petition (PP... exemption from the requirement of a tolerance for residues of lactoperoxidase (CAS No. 9003-99-0) in or...

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

    Wen Li

    2013-04-01

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

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

    Bajwa, Usha; Sandhu, Kulwant Singh

    2014-02-01

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

  15. Pesticide residue analysis by off-line SPE and on-line reversed-phase LC-GC using the through-oven-transfer adsorption/desorption interface.

    Perez, M; Alario, J; Vazquez, A; Villén, J

    2000-02-15

    A new method to determine pesticide residue in water is presented. The described method includes using off-line solid-phase extraction (SPE) and on-line reversed-phase liquid chromatography-gas chromatography (RPLC-GC). An interface, based on a modified programmed temperature vaporizer (PTV) injector, packed with a suitable trapping material, is used for on-line RPLC-GC. The changes made in the PTV injector affect the pneumatic system, sample introduction, and solvent elimination. The new interface is easily capable of automation. Methanol/wate (70/30) is used as the eluent in the LC preseparation step. The LC column flow during elution is different from the flow during the transfer step. The transferred volumes range from 500 to 1400 microL (volume of the fractions of interest). Solvent elimination is almost 100% before the sample reaches the GC column. The described system does not show any variation of the peak retention times. The detection limit for real samples ranges from 0.04 to 1.5 ng/L, using NP detection.

  16. Review of Cloud Point Extraction Technology and Its Application in Pesticide Residue Analysis%浊点萃取技术及其在农药残留分析中的应用

    陈建波; 王云飞; 奚道珍

    2011-01-01

    浊点萃取技术是基于表面活性剂溶液相分离现象的一种新兴的液-液萃取技术,已经成功的与多种分析仪器联用,用于农药残留样品的前处理中.介绍了浊点萃取技术的原理和影响因素,重点综述了浊点萃取作为气相色谱、液相色谱、分光光度计、荧光光度计的前处理技术在农药残留分析中的应用进展,探讨了该技术方法的发展前景.%Cloud point extraction (CPE) is a new liquid-liquid extraction technique based on the separation in aqueous surfactant solution. It has been combined with many analytical instruments and used for the pretreatment of pesticide residue. In this paper, the principle of CPE was introduced. The applications of CPE to the pretreatment technique of pesticide residue analysis by gas chromatography (GC), high performance liquid chromatography (HPLC),spectrophotometer and fluorophotometer were emphatically summarized. The development trend of the CPE was also presented.

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

    2012-01-23

    ... No. FSIS-2011-0035] Codex Alimentarius Commission: Codex Committee on Pesticide Residues (CCPR....) positions that will be discussed at the 44th Session of the Codex Committee on Pesticide Residues (CCPR) of the Codex Alimentarius Commission (Codex), which will be held in Shanghai, P.R. China April...

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

    Md. Nur Alam

    2015-01-01

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

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

    叶雪珠; 赵燕申; 王强; 蒋玉根

    2012-01-01

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

  20. Pesticide food safety standards as companions to tolerances and maximum residue limits

    Carl K Winter; Elizabeth A Jara

    2015-01-01

    Alowable levels for pesticide residues in foods, known as tolerances in the US and as maximum residue limits (MRLs) in much of the world, are widely yet inappropriately perceived as levels of safety concern. A novel approach to develop scientiifcaly defensible levels of safety concern is presented and an example to determine acute and chronic pesticide food safety standard (PFSS) levels for the fungicide captan on strawberries is provided. Using this approach, the chronic PFSS level for captan on strawberries was determined to be 2000 mg kg–1 and the acute PFSS level was determined to be 250 mg kg–1. Both levels are far above the existing tolerance and MRLs that commonly range from 3 to 20 mg kg–1, and provide evidence that captan residues detected at levels greater than the tolerance or MRLs are not of acute or chronic health concern even though they represent violative residues. The beneifts of developing the PFSS approach to serve as a companion to existing tolerances/MRLs include a greater understanding concerning the health signiifcance, if any, from exposure to violative pesticide residues. In addition, the PFSS approach can be universaly applied to al potential pesticide residues on al food commodities, can be modiifed by speciifc jurisdictions to take into account differences in food consumption practices, and can help prioritize food residue monitoring by identifying the pesticide/commodity combinations of the greatest potential food safety concern and guiding development of ifeld level analytical methods to detect pesticide residues on prioritized pesticide/commodity combinations.

  1. Residue Levels and Risk Assessment of Pesticides in Pistachio Nuts in Iran

    Azadeh Emami

    2017-02-01

    Full Text Available Background: Pistachio is one of the main nutrients, not only as a strategic crop but also as a main type of nut, in Iranians’ food cycle. The aim of this study was to measure the relative safety of Iranian pistachio based on the standard pesticide’s residue limits, which should be monitored and assessed in the cultivation of pistachio in order to confirm its public health. Methods: Fifty samples of pistachios of different brands were collected from Tehran markets in 2015. QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe sampling method was used in order to determine the pesticide’s residue in the pistachio nuts by Gas chromatography/Mass spectrometry (GC/MS.The method was validated with related parameters. Recovery took place at five concentration rates (n=3 ranging from 81.40% to 93.08% with the majority of RelativeStandard Deviation being lower than 20%. Limits of detection and quantification for all the pesticides were 2µg/kg and10µg/kg, respectively. The validated method seemed to be appropriate for the analysis of pesticide’s residue in pistachio nuts. Results: Identified pesticides included Fenitrothion, Carbaryl and Diazinon. Detectable pesticide’s residue existed in 10% (5 samples of the samples. Conclusion: All the results were compared with the Iran’s National Standards and the European Maximum Residue Limits. As compared to the acceptable daily intake, the calculated daily intake of each pesticide was much lower than the standard level, which could not cause any public health problem.

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

    Bakırcı, Gözde Türköz; Yaman Acay, Dilek Bengü; Bakırcı, Fatih; Ötleş, 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.

  3. 78 FR 33785 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2013-06-05

    ...; 119415-05-3; 121158-61-0; 121158-63-2; 125139-13-1; 125301-86-2; 125301-87-3; 126646-03-5; 129870-77-5...; 27731-62-0; 34431-25-9; 35015-74- 8; 52286-18-7; 52286-19-8; 54116-08-4; 61702-79-2; 63428-86-4; 63428...; FRL-9386-2] Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

  4. Public Health Implications of Pesticide Residues in Meat

    Jadhav V.J. and Waskar V.S.

    2011-01-01

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

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

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

    2015-07-01

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

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

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

    2012-01-01

    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...

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

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

    1996-12-31

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

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

    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...

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

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

    2015-01-01

    . 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...

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

    Andreou, Kostas; Semple, Kirk; Jones, Kevin

    2010-05-01

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

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

    Boesten, J.J.T.I.

    2016-01-01

    The environmental significance of soil bound pesticide residues (SBPR) is potentially large because approximately one third of the applied mass of the pesticides in agriculture ends up as SBPR. At EU level, there is little regulatory guidance available on the environmental risk assessment of SBPR

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

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

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

    Poulsen, M.; Wenneker, M.; Withagen, J.C.M.; Christensen, H.B.

    2012-01-01

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

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

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

    2013-05-01

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

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

    Md. Shakhaoat Hossain

    2013-02-01

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

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

    Indraningsih

    2006-06-01

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

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

    Maryam Amirahmadi

    2013-01-01

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

  18. Study and analysis on pesticide residues in strawberry product in Baoding district%保定辖区草莓制品农药残留研究分析

    高雪; 王翠芬; 刘萍; 刘晓慧; 颜红; 谢英; 冉升

    2015-01-01

    Objective Through calculating strawberry products pesticide detection situation in Baoding district, the causes of pollution of strawberry products pesticide were investigated for providing the basis for treatment. Methods Five kinds of pesticide residues in strawberry products were determined by using GB/T 5009.146-2008 “Determination of organochlorines and pyrethroid pesticide multiresidues in vegetable foods”and GB/T 19648-2006 “Method for determination of 500 pesticides and related chemicals in fruits and vegetables”. Results In 2011~2013, the detection rate of pesticide residues was 13.99% in strawberry products. The results indicated that detection rate of pesticide residue in strawberry products in Baoding district decreased year after year as the supervised and management measures were carried out by government, with the detection rate of pesticide residues fell from 16.20% in 2011 to 8.54% in 2013. Conclusion Therefore, we should continue to strengthen the supervision and management, to provide guarantee for the quality of products.%目的:通过统计保定辖区草莓制品中各类农药检出情况,了解保定辖区草莓制品中农药残留污染现状,探讨污染原因,为监督管理提供依据。方法采用GB/T 5009.146-2008《植物性食品中有机氯和拟除虫菊酯类农药多种残留量的测定》和 GB/T 19648-2006《水果和蔬菜中500种农药及相关化学品残留量的测定气相色谱-质谱法》,测定草莓制品中5种农药残留。结果2011~2013年草莓制品中农药残留检出率13.99%。随着政府各项监督管理措施的落实,检出率呈下降趋势,由2011年16.20%下降至2013年8.54%。结论应继续加强监督管理,为产品质量提供保障。

  19. International Comparative Analysis of Standards for Tea Pesticide Residue Limits%国内外茶叶农药残留限量标准的比较分析

    马惠民; 王永强; 钱和

    2012-01-01

    本文系统分析了美国、日本、欧盟等发达国家或地区以及联合国食品法典农药残留委员会(CODEX)的茶叶农药残留限量标准,并与我国最新茶叶农药残留限量标准进行了比较,在此基础上提出了较为具体的应对措施:借鉴国际经验,完善茶叶农残标准;合理选用农药,研发替代农药,推广病虫害综合防治技术;加强与国际信息交流,建立茶叶出口预警机制;源头控制,提高茶叶安全性。%The paper provided a comparative analysis of standards for maximum residue limits in tea among China, main developed countries or regions such as the USA, EU, Japan, and Codex Alimentarius Commission. Based on the analysis, some measures should be taken in such areas as revising standards with international experiences, selecting suitable pesticides, researching and development of alternative pesticides, promoting comprehensive prevention and control technology on plant diseases and insect pests, strengthening international information exchange, creating tea exports early warning mechanism, upgrading Chinese tea brands. Improving the tea security from the source.

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

    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.

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

    Herrmann, Susan Strange; Poulsen, Mette Erecius

    2015-01-01

    -MS/MS. In order to reduce the amount and the effects of matrix we tested the effect of using six different amounts of primary secondary amine (PSA) (0, 25, 50, 100, 150 and 200mg/ml extract) with and without the addition of six different amounts of C18 (0, 25, 50, 100, 150 and 200mg/ml extract) in the dispersive...... low intensity of the matrix peak. For oat the analytical responses of the target pesticides generally increased with increasing amount of PSA. C18 had no significant effect on the intensity of the major matrix peaks and even resulted in lower analytical responses for several of the target pesticides...

  2. [Investigation on the detection of pesticide residue in vegetable based on infrared spectroscopy].

    Li, Wen-xiu; Xu, Ke-xin; Wang, Yan; Lei, Zhen-lin; Zhang, Zhen-hou

    2004-10-01

    In this paper, the mid-infrared Attenuated Total Reflection (ATR) spectra of two slathered pesticides dichlorvos and trichlorfon in vegetable juice solution have been investigated. It can be concluded that within characteristic absorption region of the two pesticides in the mid-infrared range, the pigments inside the vegetable have no effect on the pesticide' s absorbance; pesticides in standard solution and vegetable juice solution share almost the same absorbance characteristics. These results indicate that: the authors can use the model built by the absorbance data of pesticides in water solution to simulate their absorbance in vegetable solution, then based upon infrared spectroscopy, the direct detection of pesticide residue on the vegetable can be achieved; it also provides a possible way of rapid detection on vegetable in the future.

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

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

    2015-01-01

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

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

    Abd Naser Haji Samoh

    2009-01-01

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

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

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

    2013-01-01

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

  6. Chemical Prevention and Control of Mulberry Fruit Sclerotiniosis and Analysis of Pesticide Residues%桑椹菌核病化学防控与农药残留分析

    吕蕊花; 肖伟; 吉洁; 王茜龄; 蒲龙; 赵爱春; 鲁成; 余茂德

    2014-01-01

    为探寻桑椹菌核病化学防控药剂并分析其桑椹中农药的残留量,以桑椹肥大性菌核病病原菌为材料,用市售农药对该菌的初始传染源---子囊孢子进行了抑菌实验,实验结果显示:甲基硫菌灵和腐霉利对子囊孢子抑制效果最好,其 EC50分别为0.0155 mg/mL 和0.0153 mg/mL .经大田防治实验,结果表明,在适时交替喷洒甲基硫菌灵和腐霉利,对桑椹菌核病的防治效果高达97.96%±0.2%,而对照区发病率高达40.93%±0.2%.对化学防控实验区成熟桑椹,分别采用 HPLC 和 GC 对其农药残留进行分析,甲基硫菌灵的残留量超过国际标准限量,而腐霉利的残留量则在国际标准限量之内.其研究结果对改进桑椹菌核病的防控具有重要参考意义.%In order to provide useful information for the improvement of mulberry fruit sclerotiniosis pre-vention and control with chemical agents in mulberry gardens ,a few pesticides were tested and the resi-dues in mulberry fruit were determined .In an inhibition test ,several commercially available pesticides were used to treat the ascospores of hypertrophy sorosis sclerotenisis - the initial source of infection of the disease ,and the results showed that thiophanate-methyl and procymidone had the best inhibitory effect on their grow th ,their EC50 value being 0.015 5 mg /mL and 0.015 3 mg/mL ,respectively .In a field control experiment ,timely alternate spay of thiophanate-methy and procymidone gave a control effect on mulberry fruit sclerotiniosis of up to 97.96% ,while a high incidence of 40.93% was recorded in the control plot . HPLC and GC were used for the analysis of the pesticide residues in the ripe mulberry fruit .Thiophanate-methyl residues exceeded the national standard limit ,and procymidone residues were within the limits of national standards .

  7. Rapid determination of pesticide residues in herbs using selective pressurized liquid extraction and fast gas chromatography coupled with mass spectrometry.

    Du, Gang; Xiao, Yao; Yang, Hua-Rong; Wang, Li; Song, Yue-Lin; Wang, Yi-Tao

    2012-08-01

    A selective pressurized liquid extraction and gas chromatography coupled with triple quadrupole mass spectrometer method was developed for simultaneous determination of 52 pesticide residues in medicine and food dual-purpose herbs. The developed extraction method integrated extraction and cleanup processes for sample preparation. The sorbents, 5 g Florisil and 100 mg graphitized carbon black, were placed inside the extraction cell to remove matrix interferences. Optimized conditions of selective pressurized liquid extraction were ethyl acetate as extraction solvent, 120°C of extraction temperature, 6 min of static extraction time, 50% of flush volume extracted for two cycles. An ultra inert capillary GC-MS HP-5 UI column (20 m × 0.18 mm id, 0.18 μm) and column backflush system were used for the analysis. Multiple-reaction monitoring was employed for the quantitative analysis with electron ionization mode. All calibration curves showed good linearity (r(2) > 0.995) within the test ranges. The average recoveries of most pesticides were from 81 to 118%. The validated method was successfully applied for the determination of pesticide residues in four herbs. The results indicate that selective pressurized liquid extraction and GC-MS/MS is a sensitive and reliable analytical method for the simultaneous determination of multiple pesticide residues in herbs.

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

    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

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

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

    2013-09-01

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

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

    Hjorth, Karen; Johansen, K.; Holen, B.;

    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 samp...

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

    Balawejder Maciej

    2014-12-01

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

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

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

    1998-01-01

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

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

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

    2016-01-01

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

  14. Chronic dietary risk for pesticide residues in food in Brazil: an update.

    Caldas, E D; Souza, L C K R

    2004-11-01

    The objective was to conduct a dietary risk assessment of pesticides registered in Brazil up to 14 January 2004. The theoretical maximum daily intake (TMDI) was calculated for 275 compounds using the Brazilian maximum residue limits (MRL) and food consumption. The chronic dietary risk assessment was conducted by comparing the TMDI with the Brazilian acceptable daily intake (ADI) or, when not available, with the ADI from other sources. The TMDI was higher than the ADI (%ADI>100) in at least one Brazilian region for eight pesticides, including five organophosphorus insecticides. For these compounds, the higher TMDI (expressed as %ADI) ranged from 140 (metam sodium) to 14,000 (methyl bromide). Rice, beans, citrus and tomato were the commodities that contributed most to ingestion. Change in pesticide use patterns and the establishment of ADIs by the Brazilian government have reduced the number of compounds for which the TMDI exceeded the ADI in the last 4 years. Risk assessment methodology based on TMDI calculation, however, is conservative as it assumes that the food supply is always treated with all the registered pesticides for that crop and that one always consumes food containing residues at the tolerance level. Furthermore, for six compounds with TMDI exceeding the ADI, a more realistic estimation of the pesticide daily intake was conducted using monitoring residue data from the Brazilian National Pesticide Residue Program. For these compounds, the higher refined intakes ranged from 2% (dimethoate) to 180% (fenitrothion) of the ADIs. The implementation of a national pesticide residue monitoring programme by the government was important to allow the refinement of the risk assessment. However, adequate daily food consumption data are still needed to assess better the public health risk to Brazilian consumers from food produced from crops treated with pesticides.

  15. Pressurised fluid extraction (PFE) as an alternative general method for the determination of pesticide residues in rape seed.

    Pihlström, Tuija; Isaac, Giorgis; Waldebäck, Monica; Osterdahl, Bengt-Göran; Markides, Karin E

    2002-04-01

    A pressurised fluid extraction (PFE) multi-method has been developed for the determination of pesticide residues in rape seed. The method was validated for 25 different pesticides and metabolites. The reliability and efficiency of PFE for extracting pesticide residues from rape seed was investigated. The traditional extraction solvent, hexane saturated with acetonitrile, was used at elevated temperature and pressure. With increased temperature, the extraction kinetics were improved but at the same time more co-extractives were obtained in the form of lipids. When 1 g of rape seed was extracted at temperatures from 60 degrees C to 150 degrees C, the lipid content extracted was found to be as high as 17-26%. An additional clean-up step was therefore required and lipid co-extractives were effectively removed by gel permeation chromatography. The interpretation of the chromatograms and the quantification of the results were satisfactorily improved by the removal of interfering lipids. The developed method was used to extract vinclozolin and iprodione from incurred samples, resulting in a concentration in accordance with the results using conventional liquid-liquid extraction (LLE) between hexane and acetonitrile and also supercritical fluid extraction (SFE) using carbon dioxide. The results of the present study suggest that PEE is a good alternative extraction technique for the determination of pesticide residues in oil seed. Despite the necessity for a lipid-removal clean-up step, the PFE technique facilitated the extraction process by faster extractions and the possibility of automated analysis.

  16. Residual Characters and Sources of Organochlorine Pesticides in Soils of Tianjin Area, China

    WANG Ying

    2016-09-01

    Full Text Available The spatial distribution characteristics and the sources of organochlorine pesticides(OCPs were studied according to the field sampling and quantitative analysis of OCPs of soils in 188 points with 6 land-use types and 2 irrigation types from Tianjin area. This article investigated the residual levels, spatial and profile distribution of the isomers of hexachloro -cyclohexane soprocide(HCHs and dichlorodiphenyl trichloroethane (DDTs firstly, and then made the comparison with the residues in the past. The results showed that the con-tents of HCHs and DDTs in the soil of Tianjin reached to class A of the national standard. The distribution characteristics of HCHs in soils from Tianjin indicated that the inner suburban district and the coastal region were the most polluted areas, downtown took the second place, and outer suburban district was the least polluted. The distribution characteristics of DDTs showed that the inner suburban district and the downtown were the most polluted area, outer suburban district took the second place, and the coastal region was the least polluted. In different land-use types, there was the highest OCPs residues in urban green area. And there was no significant differences of OCPs residues between irrigation area and sewage irrigation area. The results of profile analysis indicated that the total amount of OCPs was mainly found in the 0~30 cm of farming layer. Based on the comparison of the residues of HCHs with that of DDTs, the degradation rate of DDTs was higher than that of HCHs, and abnormal residual levels were found in some areas of Tianjin.

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

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

    2015-10-01

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

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

    1998-01-01

    In order to assess the dietary risk resulting from the use of pesticides or veterinary drugs the nature of the chemical residues on food commodities needs to be determined. Elucidation of the nature of the chemical residue is carried out using radiolabelled studies where the radiolabelled xenobiotic is applied or dosed in a manner which reflects use conditions. Food commodities are exhaustively extracted to remove the individual components of the residue. Once extracted the identity and toxic...

  19. Pesticide residues in Portuguese strawberries grown in 2009-2010 using integrated pest management and organic farming.

    Fernandes, Virgínia C; Domingues, Valentina F; Mateus, Nuno; Delerue-Matos, Cristina

    2012-11-01

    Pesticides are among the most widely used chemicals in the world. Because of the widespread use of agricultural chemicals in food production, people are exposed to low levels of pesticide residues through their diets. Scientists do not yet have a total understanding of the health effects of these pesticide residues. This work aims to determine differences in terms of pesticide residue content in Portuguese strawberries grown using different agriculture practices. The Quick, Easy, Cheap, Effective, Rugged, and Safe sample preparation method was conducted and shown to have good performance for multiclass pesticides extraction in strawberries. The screening of 25 pesticides residue was performed by gas chromatography-tandem mass spectrometry. In quantitative validation, acceptable performances were achieved with recoveries of 70-120 and integrated pest management (IPM) practices harvested in 2009-2010. The results showed the presence of fludioxonil, bifenthrin, mepanipyrim, tolylfluanid, cyprodinil, tetraconazole, and malathion when using IPM below the maximum residue levels.

  20. Organochlorine pesticides residues in bottled drinking water from Mexico City.

    Díaz, Gilberto; Ortiz, Rutilio; Schettino, Beatriz; Vega, Salvador; Gutiérrez, Rey

    2009-06-01

    This work describes concentrations of organochlorine pesticides in bottled drinking water (BDW) in Mexico City. The results of 36 samples (1.5 and 19 L presentations, 18 samples, respectively) showed the presence of seven pesticides (HCH isomers, heptachlor, aldrin, and p,p'-DDE) in bottled water compared with the drinking water standards set by NOM-127-SSA1-1994, EPA, and World Health Organization. The concentrations of the majority of organochlorine pesticides were within drinking water standards (0.01 ng/mL) except for beta-HCH of BW 3, 5, and 6 samples with values of 0.121, 0.136, and 0.192 ng/mL, respectively. It is important monitoring drinking bottled water for protecting human health.

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

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

    2014-06-15

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

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

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

    2015-06-01

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

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

    Uthuppu, Basil; Kostesha, Natalie; Jakobsen, Mogens Havsteen;

    2011-01-01

    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......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...

  4. Monitoring of organophosphorus pesticide residues in vegetables of agricultural area in Venezuela.

    Quintero, América; Caselles, María J; Ettiene, Gretty; de Colmenares, Nélida G; Ramírez, Tibisay; Medina, Deisy

    2008-10-01

    The purpose of this study was to determine the residues of seven pesticides organophosphorus (methamidophos, diazinon, chlorpyriphos, parathion-methyl, dimethoate, malathion and tetrachlorvinphos), in some vegetables like: potato, lettuce, tomato, onion, red pepper and green onion cultivated in José María Vargas County in Táchira State, Venezuela. The research permitted to detect that 48.0% of the samples were contaminated with some of the pesticides studied. Methamidophos was founded in the vegetables in the rank of 6.3%-65.5%. The results show that 16.7% of the samples tested have residues higher than the maximum limits permitted.

  5. Results from the monitoring of pesticide residues in fruit and vegetables on the Danish market 1998-99

    Andersen, Jens Hinge; Poulsen, Mette Erecius

    2001-01-01

    The objective of the Danish pesticide monitoring programme for fruit and vegetables was to check for compliance with the maximum residue levels in foods and to monitor the residue levels to assess the pesticide exposure of the Danish population. Sampling plans were designed based on previous find....... Residues were found in 54% of the samples of fruit but only in 13% of the vegetables. Residues above the MRL were found in 4% of all samples of fruit and in 1% of vegetables....

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

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

    2016-02-01

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

  7. Identification and quantification of pesticide residues in water samples of Dhamrai Upazila, Bangladesh

    Hasanuzzaman, M.; Rahman, M. A.; Salam, M. A.

    2016-10-01

    Being agricultural country, different types of pesticides are widely used in Bangladesh to prevent the crop losses due to pest attack which are ultimately drain to the water bodies. The present study was conducted to identify and quantify the organochlorine (DDT, DDE and DDD), organophosphorus (malathion, diazinon and chloropyrifos) and carbamate (carbaryl) residues in water samples of different sources from Dhamrai upazila of Bangladesh using high performance liquid chromatography (HPLC) equipped with ultra violate (UV) detector. Thirty water samples from fish pond, cultivated land and tube-well were collected in winter season to analyze the pesticide residues. Among the organophosphorus pesticides, malathion was present in seven water samples ranging from 42.58 to 922.8 μg/L, whereas diazinon was detected in water sample-8 (WS-8) and the concentration was 31.5 μg/L. None of the tested water samples was found to be contaminated with chlorpyrifos, carbaryl or DDT and its metabolites (DDE and DDD). Except for a tube-well water sample, concentrations of the detected residues are above the acceptable limit for human body as assigned by different organizations. To avoid the possible health hazards, the indiscriminate application of pesticides should be restricted and various substitute products like bio-pesticide should be introduced in a broad scale as soon as possible.

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

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

    2016-09-14

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

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

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

    2007-01-01

    , no significant effect was found for organophosphorus pesticides and pyrethroids, whereas the number of samples with residues of benzilates, phenylamids and triazoles was insufficient to demonstrate any significant effects. An intake calculation showed that the average intake from Italian grapes was 3.9 mu g day...

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

    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 q

  11. 78 FR 16243 - Codex Alimentarius Commission: Codex Committee on Pesticide Residues (CCPR)

    2013-03-14

    ...; ] DEPARTMENT OF AGRICULTURE Food Safety and Inspection Service Codex Alimentarius Commission: Codex Committee... at the 45th Session of the Codex Committee on Pesticide Residues (CCPR) of the Codex Alimentarius Commission (Codex), which take place in Beijing, People's Republic of China, May 6-13, 2013. The...

  12. 76 FR 3601 - Codex Alimentarius Commission: Meeting of the Codex Committee on Pesticide Residues

    2011-01-20

    ... Food Safety and Inspection Service Codex Alimentarius Commission: Meeting of the Codex Committee on... that will be discussed at the 43rd Session of the Codex Committee on Pesticide Residues (CCPR) of the Codex Alimentarius Commission (Codex), which will be held in Beijing, P.R. China April 4-9, 2011....

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

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

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

    Kimberly A Stoner

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

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

    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 μg per bee (range 166,000X), and even among insecticides LD50 values ranged from 0.006 to 59.8 μg/bee (10,000X); therefore we propose that in studies of honey bee exposure to pesticides that concentrations be reported as Hazard Quotients as well as in standard concentrations such as parts per billion. We used both contact and oral LD50 values to calculate Pollen Hazard Quotients (PHQ = concentration in ppb ÷ LD50 as μg/bee) when both were available. In this study, pesticide Pollen Hazard Quotients ranged from over 75,000 to 0.01. The pesticides with the greatest Pollen Hazard Quotients at the maximum concentrations found in our study were (in descending order): phosmet, Imidacloprid, indoxacarb, chlorpyrifos, fipronil, thiamethoxam, azinphos-methyl, and fenthion, all with at least one Pollen Hazard Quotient (using contact or oral LD50) over 500. At the maximum rate of pollen consumption by nurse bees, a Pollen Hazard Quotient of 500 would be approximately equivalent to consuming 0.5% of the LD50 per day. We also present an example of a Nectar Hazard Quotient and the percentage of LD50 per day at the maximum nectar consumption rate.

  16. A positive analysis of excessively rigorous proof of the standards about maximum residue limits for pesticide in agri-food%我国农药最大残留限量标准过严的实证分析

    李太平

    2012-01-01

    Under the information asymmetry and market supervision lack of agri-food quality,the excessively rigorous standard of maximum residue limits(MRLs)for pesticide in agrifood is not only unbeneficial to protect consumer health and ecological environment,but also aggregate serious pesticide residues in agrifood.Taking national standard Maximum Residue Limits for Pesticides in Food(GB2763-2005)as a case,calculated the Theory Daily Intake(TDI)related agrifoods of 439 residue indexes of 126 pesticides with the quantity relation between MRLs,acceptable daily intake(ADI)and TDI,and compared with the customer's Real Daily Intake(RDI)related agrifoods.It was found that there were 111 residue indexes related agri-foods which TDI were overly above and beyond their RDI of Chinese residents,accounted for 23.22% of 478 pesticide residue indexes in this national standards.This evidence proved that the national standard had the excessively rigorous tendency really and suggested our government would revise this standard at once in order to eliminate the food safety management trap.%在农产品质量信息不对称、市场监管不到位的情况下,农药最大残留限量标准制定过严,不但不能保护消费者健康和农业生态环境,反而会加剧农产品的农药残留问题泛滥。利用农药最大残留限量(MRLs)、日允许摄入量(ADI)与被测食品每日最大理论摄入量(TDI)三者之间的数量关系,以《食品中农药最大残留限量》GB2763-2005为例,计算了126种农药439个残留指标的TDI值,发现有111个残留指标的TDI值远远大于我国居民每日实际摄入量(RDI),占GB2763-2005国家标准478个残留限量指标的23.22%,表明我国农药最大残留限量国家标准部分指标值设定存在过严的倾向,建议政府尽快修订该标准,以消除食品安全管理隐患。

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

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

    2014-01-01

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

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

    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

  19. Present Situation and Control Countermeasures of Pesticide Residue on Crops in Yinzhou District of Ningbo City, China

    XU Pei-juan

    2014-02-01

    Full Text Available Tatal of 411 batches of rice, leaf vegetables, fruits, beans, solanums and tubers were sampled monthly, in accordance with related national regulations on 22 detected pesticides in the Yinzhou District, Ningbo City. The results showed that the pesticide detection rate was0.3%, the qualified rate of pesticide residues in agricultural products was 97.82%. Pesticide residues detection accounted for 88.89%. The samples beyond the pesticide residue standard were mainly vegetables from May to October. Leaf vegetables exceeding the standard sample rate reached 3.72%. Pesticide residue samples exceeding the standard were found in retail in plain and coastal areas, but were found in all scale farming in mountainous areas. The rate of exceeding the pesticide residues standard of farmers with primary school education level was4.50%, which was 6.16 times higher than that farmers with university education. In order to reduce the pesticide residual in Yinzhou District,we put forward control countermeasures in 5 aspects.

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

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

    2016-11-01

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

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

    B Shabankhani

    2006-01-01

    Full Text Available Introduction: Considering the importance and usefulness of fruits in 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. A rapid spectrophotometric assay of some organophosphorus pesticide residues in vegetable samples

    Mathew, Sunitha B.; Pillai, Ajai K.; Gupta, Vinay K.

    2007-08-01

    A rapid and sensitive spectrophotometric method for the determination of some organophosphorus insecticides, i.e. malathion, dimethoate and phorate is described. It is based on the oxidation of organophosphorus pesticide with slight excess of N-bromosuccinimide (NBS) and the unconsumed NBS is determined with rhodamine B (lambda max: 550 nm). Beer's law is obeyed in the concentration range 0.108-1.08, 0.056-0.56 and 0.028-0.28 μg mL -1 for malathion, phorate and dimethoate, respectively. The method has been successfully applied for the determination of organophosphorus pesticide residues in various vegetable samples.

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

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

    2016-07-01

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

  4. Detection of pesticides residues in water samples from organic and conventional paddy fields of Ledang, Johor, Malaysia

    Abdullah, Md Pauzi; Othman, Mohamed Rozali; Ishak, Anizan; Nabhan, Khitam Jaber

    2016-11-01

    Pesticides have been used extensively by the farmers in Malaysia during the last few decades. Sixteen water samples, collected from paddy fields both organic and conventional, from Ledang, Johor, were analyzed to determine the occurrence and distribution of organochlorine (OCPs) and organophosphorus (OPPs) pesticide residues. GC-ECD instrument was used to identify and determine the concentrations of these pesticide residues. Pesticide residues were detected in conventional fields in the range about 0.036-0.508 µg/L higher than detected in organic fields about 0.015-0.428 µg/L. However the level of concentration of pesticide residues in water sample from both paddy fields are in the exceed limit for human consumption, according to European Economic Commission (EEC) (Directive 98/83/EC) at 0.1 µg/L for any pesticide or 0.5 µg/L for total pesticides. The results that the organic plot is still contaminated with pesticides although pesticides were not use at all in plot possibly from historical used as well as from airborne contamination.

  5. Compound specific isotope analysis of organophosphorus pesticides.

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

    2014-09-01

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

  6. [Determination of pesticide residues from seed coating reagent in agricultural products using ultra performance liquid chromatography-tandem mass spectrometry].

    Chen, Yue; Wang, Jinhua; Lu, Xiaoyu; Wang, Wanchun; Huang, Mei; Xu, Chaoyi

    2008-11-01

    An ultra performance liquid chromatography-tandem mass spectrometric method (UPLC-MS/MS) has been developed for the simultaneous determination of eight pesticide residues from seed coating in fruits, vegetable and grain. The sample was extracted by methanol-water (1:1, v/v) and determined by ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry in positive mode (ESI+) and multiple reaction monitoring (MRM) mode. The UPLC analyses were performed on an Acquity UPLC C18 column with gradient eluation. The utility of the method was demonstrated by the analysis of crude extracts, with no sample clean up, from soybean. The linear range was 1 - 200 microg/L. The correlation coefficients (r) were under 0.997. The average recoveries of eight pesticides in samples (from 0.006 to 1.2 mg/kg) ranged from 60% to 110%, and the relative standard deviations (RSDs) were less than 10%. The results indicate that the method is easier, faster, more sensitive, and suitable for the qualitative and quantitative confirmation of pesticide residues from seed coating reagent in fruit, vegetable and grain samples.

  7. 近红外光谱技术在果蔬农药残留检测中的应用研究进展%Application of near infrared spectrum analysis technique in pesticide residues detection of fruits and vegetables

    戴莹; 冯晓元; 韩平; 王蒙; 王纪华

    2014-01-01

    Near-infrared spectroscopy (NIR) is a new analytical technique with the features of non-destructive, rapid and low cost, which can realize the qualitative and quantitative monitoring of pesticide residues in agricultural products especially in fruits and vegetables. Near-infrared spectroscopy will have broad prospects in the agricultural products security field because of the outstanding advantages of non-destructive testing characteristic. This paper summarized the basic principles and the characteristics of NIR, introduced the pretreatment technology of NIR such as the pre-concentration technologies and the quantitative calibration models and reviewed the application situations of the near infrared spectrum technology in the detection of pesticide residues in fruits and vegetables. With the continuous development and perfection of the near infrared spectrum technology and the relevant processing technology, the application of near infrared spectroscopy de-tection of pesticide residues in fruits and vegetables is being developed with a tendency of high sensitivity and accuracy, easy automation and on the spot operation.%近红外光谱技术是一种具有无损、快速、低成本等诸多特点的新型分析检测技术,可以方便地实现对农产品尤其是水果、蔬菜中农药残留的定性和定量监控。近红外光谱技术所具有的无损检测这一突出优势,使其在农产品安全领域有着广阔的应用前景。本文概述了近红外光谱技术的基本原理、应用特点、目前近红外光谱技术常用的样品前处理技术-预浓缩技术和定量校正模型,并对近红外光谱技术在果蔬农药残留检测领域的应用情况进行综述。随着近红外光谱技术的不断革新、相关前处理技术的不断发展和完善,未来近红外光谱技术在果蔬农药残留检测中会向着更加灵敏、更加准确、更加自动化、更加现场化等方向发展。

  8. Pre-concentration of pesticide residues in environmental water samples using Silica nanoparticles and identification of residues By GC-MS method

    Tentu. Nageswara Rao

    2016-08-01

    Full Text Available The silica nanoparticles prepared by stober’s mechanism by reaction of tetraethylorthosilicate (TEOS with ammonia was tested for their adsorption capacity in the pre-concentration of residues of pesticides in water. The synthesized nanoparticles were characterized by Scanning Electron Microscope (SEM, Transmission Electron Microscope (TEM and X-Ray Diffraction (XRD. The size of the silica nanoparticles were 50 to 250 nm. The solid phase extraction (SPE cartridges were prepared by filling the empty cartridges of 5.5 cm length and 0.3 cm i.d. with 200 mg of nanoparticles and protected between two polytetrafluroethylene (PTFE frits. To avoid the passage of nanoparticles, 2% solution of polystyrene in chloroform was passed through PTFE frits and dried in air for two hours at room temperature before fitted into the cartridges. This process is to reduce the pore size of the PTFE frits. These cartridges are used in pre-concentration of different types of residues of pesticides in water. The pyrethroids tested for the pre-concentration are tetramethrin, lambda-cyhalothrin, cyphenothrin. The water samples were spiked with aliquots of pesticides and were passed through the cartridges. The amounts of the pesticides adsorbed on the cartridges were tested. The influence of temperature, sample volume, flow rate, pH and ionic strength on the performance of the cartridges was checked. The results of fortified sample analysis were compared with the data obtained from the commercially available C18 cartridges for the sample volume. The separation parameters were established for the simultaneous determination of residues using GC-EI-MS. The method was validated by means of linearity, precision, and assay accuracy. The limit of detection (LOD and the limit of quantification (LOQ were established based on the signal to noise ratio 3:1 and 10:1 respectively. An analytical method for the enrichment of residues using nanoparticles based SPE cartridges were developed

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

    Anita Osei Tutu

    2011-03-01

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

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

    Faqir Muhammad

    2013-01-01

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

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

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

    2013-01-01

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

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

    VALENTINA L. CHRISTOVA-BAGDASSARIAN

    2014-07-01

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

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

    Faustin Vidogbéna

    2015-10-01

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

  14. Levels of organochlorine pesticides residues in human adipose tissue, data from Tabasco, Mexico.

    Waliszewski, Stefan M; Caba, M; Rodríguez Díaz, S S; Saldarriaga-Noreña, H; Meza, E; Zepeda, R; Infanzón, R

    2012-11-01

    The objective of this study was to determine the levels of organochlorine pesticides HCB, α-β-γ-HCH, p,p'-DDE, o,p'-DDT and p,p'-DDT in 150 adipose tissue of inhabitants of Tabasco, Mexico. The following pesticides were detected: p,p'-DDE in 100% of samples at mean 1.034 mg/kg; p,p'-DDT in 96.7% at mean 0.116 mg/kg; o,p'-DDT in 78.7% at mean 0.022 mg/kg and β-HCH in 58.0% at mean 0.049 mg/kg. The pooled sample was divided according to sex of donors (75 female and 75 male). Significantly higher levels of all organochlorine pesticides in females were found. The sample was divided into three age's ranges (15-28, 29-45 and 46-84 years). The mean and median levels of β-HCH, p,p'-DDE and Σ-DDT increase significantly (p < 0.05) from the first to the second and third group. The presence of organochlorine pesticide residues in Tabasco inhabitants is still observed, indicating sources of exposure to the pesticides.

  15. Removal of prioritary pesticides contamining r'mel ground water by using organic waste residues.

    El Bakouri, H; Morillo, J; Usero, J; Ouassini, A

    2007-01-01

    This study evaluated pesticide contamination of R'mel ground water located in northwest Morocco. The study area is densely populated and thriving, with intensive agriculture. Various techniques, including stir bar sorptive extraction (SBSE) and gas chromatography with mass spectroscopy detection (GC-MS), were used for the quantitative determination of 13 pesticides including alachlor, aldrin, atrazine, chlorpyrifos, chlorfenvinphos, dieldrin, alpha-endosulfan, endrin, hexachlorobenzene, beta-HCH, gamma-HCH (lindane), simazine and trifluralin. The survey results showed that contamination by pesticide residues is widespread in the area. With the exception of atrazine, the average concentrations were all below the regulatory limits established by the European Union. The potential of ten natural organic substances to eliminate pesticides included in the European Water Framework Directive was evaluated. The absorbents with the highest removal efficiency were date and olives stones and, to a Lesser degree, Raphanus raphanistrum and Cistus ladaniferus. The adsorption tests gave very satisfying results and pointed to the possible application of these supports as ecoLogical remediation techniques to prevent pesticide pollution of aquatic ecosystems.

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

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

    2014-01-01

    Flow injection combined with tandem mass spectrometry (MS/MS) was investigated for the rapid detection of highly polar pesticides that are not amenable to multi-residue methods because they do not partition into organic solvents and require dedicated chromatographic conditions. The pesticides includ

  17. Organochlorine pesticide residues in bovine milk from organic farms in Chiapas, Mexico.

    Gutiérrez, Rey; Ruíz, Jorge Luis; Ortiz, Rutilio; Vega, Salvador; Schettino, Beatriz; Yamazaki, Alberto; de Lourdes Ramírez, María

    2012-10-01

    Thirty six samples of bovine milk were collected from Chiapas State, Mexico between January 2011 and December 2011 with the intention of identifying and quantifying organochlorine pesticide residues in organic farms. The analyses were done using gas chromatography with an electron capture detector (Ni(63)). In general the values found in raw milk were lower than the permissible limit proposed by FAO/WHO/Codex Alimentarius 2006. Average concentrations for alpha + beta HCH were 3.62 ng/g, gamma HCH 0.34 ng/g, heptachlor + epoxide 0.67 ng/g, DDT and isomers 1.53 ng/g, aldrin + dieldrin 0.77 ng/g, and endrin 0.66 ng/g (only present in samples from farm 2). The organic milk from Chiapas has shown low concentrations of pesticide residues in recent years and satisfies international and national regulations for commercialization.

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

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

    2007-06-01

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

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

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

    2005-01-01

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

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

    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.

  1. Contamination of liquid milk and butter with pesticide residues in the Ludhiana district of Punjab state, India.

    Battu, R S; Singh, Balwinder; Kang, B K

    2004-11-01

    An analysis of 92 samples of liquid milk from Ludhiana, India, during 1999-2001 revealed the presence of DDT in 6 (7.4%) samples and of these 2 samples were found to exceed the maximum residue limit (MRL) of DDT fixed at 0.05 mg kg(-1) (on a whole milk basis). HCH residues were detected in 49 (53.3%) samples and constituted only gamma-HCH (lindane). The MRL of lindane is fixed at 0.01 mg kg(-1) (whole milk basis), and all 49 liquid milk samples exceeded this value. These results are indicative of contamination of bovine milk with pesticide residues as a result of the ban on the use of DDT and HCH in agriculture and public health programs. Similarly, analysis of 40 samples of butter showed the presence of DDT and HCH in 28 and 8 samples, respectively. However, none of the samples exceeded the MRL value of either DDT or any isomer of HCH. DDT residues comprised mainly p,p-DDE and p,p-TDE, whereas HCH residues were present as lindane in 6 samples, and 2 samples revealed the presence of beta-HCH. The estimated daily intake of lindane through the consumption of contaminated liquid milk exceeded its acceptable daily intake value for children. Interestingly, none of the liquid milk or butter samples revealed the presence of any commonly used organophosphorus or synthetic pyrethroid insecticides at their detection limit of 0.01 mg kg(-1).

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

    F. Upadhi

    2012-11-01

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

  3. Preparation and characterization of amino functionalized nano-composite material and its application for multi-residue analysis of pesticides in cabbage by gas chromatography-triple quadrupole mass spectrometry.

    Zhao, Yong-Gang; Shen, Hao-Yu; Shi, Jia-Wei; Chen, Xiao-Hong; Jin, Mi-Cong

    2011-08-19

    In this paper, a novel and recyclable amino-functionalized nano-composite material (NCM) using tetraethylenepentamine (TEPA) as a coupling agent was synthesized. The properties of the TEPA-NCM were characterized by transmission electron microscopy (TEM), Fourier transform infrared analysis (FTIR), thermogravimetric analysis (TGA) and elemental analysis (EA). An effective dispersive solid-phase extraction (dSPE) procedure using the TEPA-NCM was developed, and comparative studies were carried out among Carbon/NH₂ SPE, primary secondary amine (PSA) dSPE and TEPA-NCM dSPE. The results showed that TEPA-NCM dSPE was faster, easier and more effective to clean and enrich than the Carbon/NH₂ cartridges, and the TEPA-NCM was much more effective to remove the pigments in vegetable samples than the PSA materials. The TEPA-NCM could be reused at least five times without much sacrifice of the cleanup efficiency. Furthermore, a gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS/MS) method was established for the simultaneous determination of 29 pesticides (such as organochlorine and organophosphorus pesticides) in vegetables by dSPE using acetonitrile as an extraction solvent and TEPA-NCM as an adsorbent instead of PSA. The recoveries were in the range of 75-114% for all analytes except for trans-chlordane. The RSDs were in the range of 2-17%. The linearities were in the range of 0.4-100.0 μg/kg with determination coefficients (r²) higher than 0.986 for all compounds. The limits of detection (LODs) for all pesticides were less than 0.29 μg/kg and the limits of quantification (LOQs) were between 0.17 and 0.95 μg/kg. The developed method was applied to fifteen real vegetable samples, and it was confirmed that the TEPA-NCM was one of a kind of highly effective dSPE materials used for the pesticides analyses.

  4. Screening of pesticide residues in honeybee wax comb by LC-ESI-MS/MS. A pilot study.

    Herrera López, Sonia; Lozano, Ana; Sosa, Alexis; Hernando, M Dolores; Fernández-Alba, Amadeo R

    2016-11-01

    A developed multi-residue method using microflow-LC-ESI-QqQ-MS provided a wide-scope analysis for medium-polar and polar pesticide residues (120 compounds including breakdown products). Honeybee wax comb samples were extracted using a generic QuEChERS based procedure. Acceptable recoveries at concentration levels of 5 and 50 μg kg(-1) were within the 70-120% range with an associated precision RSD  9 μg kg(-1); fungicides at concentrations ranging from 1 to 23 μg kg(-1.) The number of positive detections due to herbicides was lower as expected and at a lower level of concentration, from 1 to 5.9 μg kg(-1).

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

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

    2014-01-01

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

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

    Malinowska, Elżbieta; Jankowski, Kazimierz

    2015-12-01

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

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

    Das, Biplob; Khan, Y.S.A.; Das, Pranab; Shaheen, S.M

    2002-12-01

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

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

    孙俊; 董梁; 张梅霞; 刘枭; 邬婷; 高洪燕

    2014-01-01

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

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

    Bache, Michael; Taboryski, Rafael Jozef; Schmid, Silvan;

    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....

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

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

    2011-11-01

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

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

    Aamand Jens

    2011-01-01

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

  12. Organochlorine pesticide residues: an extensive monitoring of Italian fishery and aquaculture.

    Masci, Maurizio; Orban, Elena; Nevigato, Teresina

    2014-01-01

    A sampling campaign from 21 sites in Italy was carried out to investigate the presence of organochlorine pesticide residues in different fish species. Samples came from marine fishery and either from sea- or freshwater aquaculture. Fish feed used in some fish farms were also analyzed. Pesticides studied belong to Persistent Organic Pollutants widely used in the past such as DDT, chlordane, heptachlor, and others. To ensure good quality results and proper data validation the main existing guidelines in the field were applied. The instrumental technique was a Dual column-Dual detector Gas Chromatography (GC-ECD and Ion Trap GC-MS) which allowed that complementary data on the same sample were acquired. Results for fishery showed a wide range of concentrations depending from the area and species examined. DDT, the major OC pesticide detected, varied from 0.02 to 130.03 ng g(-1) edible portion. As regards the products of aquaculture we observed slightly lower average levels of pollutants in a more narrow range of concentration: this is probably due to fish feed used as shown by some measures performed in the present study. Organochlorine pesticide residues were detected in all samples examined but they were generally well below the existing tolerance or action levels. Also the estimated daily intakes are well below than those recommended by WHO. This is a good indication about OCPs in the areas investigated but some further considerations on fish safety must be taken into account. An example on how fishes may act as bioindicators is reported.

  13. 77 FR 75082 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2012-12-19

    ... environmental justice issues, the Agency seeks information on any groups or segments of the population who, as a... ingredient in pesticide formulations for a packaging film for unit dose packaging of pesticides and...

  14. Spatial distribution, source apportionment and ecological risk assessment of residual organochlorine pesticides (OCPs) in the Himalayas.

    Devi, Ningombam Linthoingambi; Yadav, Ishwar Chandra; Raha, Priyankar; Shihua, Qi; Dan, Yang

    2015-12-01

    The Indian Himalayan Region (IHR) is one of the important mountain ecosystems among the global mountain system which support wide variety of flora, fauna, human communities and cultural diversities. Surface soil samples collected from IHR were analysed for 23 organochlorine pesticides (OCPs). The concentration of ∑OCPs ranged from 0.28 to 2143.96 ng/g (mean 221.54 ng/g) and was mostly dominated by DDTs. The concentration of ∑DDTs ranged from 0.28 to 2126.94 ng/g (mean 216.65 ng/g). Other OCPs such as HCHs, endosulfan and heptachlor, Aldrin and dieldrin were detected in lower concentration in IHR. Their concentrations in soil samples ranged from ND to 2.79 ng/g for HCHs, ND to 2.83 ng/g for endosulfans, NDto 1.46 ng/g for heptachlor, ND to 2.12 ng/g for Aldrin and ND to 1.81 ng/g for dieldrin. Spatial distribution of OCPs suggested prevalence of DDTs and HCHs at Guwahati and Itanagar, respectively. The close relationship between total organic carbon (TOC) and part of OCP compounds (especially α- and γ-HCH) indicated the important role of TOC in accumulation, binding and persistence of OCP in soil. Diagnostic ratio of DDT metabolites and HCH isomers showed DDT contamination is due to recent application of technical DDT and dicofol, and HCH contamination was due to mixture of technical HCH and lindane source. This was further confirmed by principal component analysis. Ecological risk analysis of OCP residues in soil samples concluded the moderate to severe contamination of soil.

  15. 非接触热解析封闭式低温等离子体电离源质谱法快速分析3种农药残留%Rapid Analysis of Three Kinds of Pesticide Residues by Non-contact Thermal Desorbing and Closing Low Temperature Plasma Ionization Mass Spectrometry

    苏明扬; 李海洋; 侯可勇; 黄泽健; 江游; 陈文东; 陈平; 蒋吉春; 赵无垛; 裴克梅

    2014-01-01

    A new method was established for the direct, rapid and quantitative analysis of pesticide residues, dimethoate chlorothalonil and malathion by low temperature plasma ( LTP) ionization miniature ion trap mass spectrometer. The LTP ionization probe and sample inlet of ion trap mass spectrometry were enclosed in a metal cavity. With non-contact heating, the samples placed on the sample platform were desorbed into gaseous phase and ionized by LTP ionization probe. The results showed that closed ionization had an edge over the opened ionization. The quantitative analysis of 3 pesticides within the range of 0. 5-10 mg/L was realized by optimizing heating time and flow rate of air, and the relative standard deviations of signal intensity is less than 11%. LODs of pesticide, which were obtained within 5 s, were as low as several hundred pictograms. The results showed that the method could be used for the analysis of pesticide residue on green and organic fruits or vegetables.%利用低温等离子体电离源微型离子阱质谱建立了一种常压离子化质谱直接、快速、定量分析农药残留的新方法。低温等离子体电离源与质谱进样口处于封闭金属腔体内部,在负离子探测模式下,将样品放置于低温等离子体电离源前的采样平台上,利用卤素灯快速无接触热解析样品。结果表明,封闭离子源更具优势,通过对加热时间、辅助气流流量等条件的优化,实现了对3种农药在0.5~10 mg/L范围内的定量分析,相对标准偏差控制在11%左右,5 s内的样品检出限均在pg量级。该检测方法无需样品前处理,样品可直接检测,分析时间快,有望广泛应用于有机和绿色果蔬中农药残留的快速检测。

  16. Monitoring and exposure assessment of pesticide residues in cowpea (Vigna unguiculata L. Walp) from five provinces of southern China.

    Huan, Zhibo; Xu, Zhi; Luo, Jinhui; Xie, Defang

    2016-11-01

    Residues of 14 pesticides were determined in 150 cowpea samples collected in five southern Chinese provinces in 2013 and 2014.70% samples were detected one or more residues. 61.3% samples were illegal mainly because of detection of unauthorized pesticides. 14.0% samples contained more than three pesticides. Deterministic and probabilistic methods were used to assess the chronic and acute risk of pesticides in cowpea to eight subgroups of people. Deterministic assessment showed that the estimated short-term intakes (ESTIs) of carbofuran were 1199.4%-2621.9% of the acute reference doses (ARfD) while the rates were 985.9%-4114.7% using probabilistic assessment. Probabilistic assessment showed 4.2%-7.8% subjects may suffer from unacceptable acute risk from carbofuran contaminated cowpeas from the five provinces (especially children). But undue concern is not necessary, because all the estimations are based on conservative assumption.

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

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

    2004-09-15

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

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

    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 μg 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.

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

    Mobeen Akhtar

    2014-01-01

    Full Text Available 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 μg 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.

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

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

    2015-05-01

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

  1. Determination of pesticide residues in Turkey's table grapes: the effect of integrated pest management, organic farming, and conventional farming.

    Turgut, Cafer; Ornek, Hakan; Cutright, Teresa J

    2011-02-01

    Turkey is one of the world's largest producers and exporters of table grapes. Growing social concerns over excessive pesticide use have led to farming to move from conventional to organic practices. Table grapes were collected from 99 different farms in three Aegean regions. Pesticide residues were only detected in farms using conventional agriculture practices while no pesticides were detected in grapes from farms using organic or integrated pest management. A risk assessment model indicated that lambda-cyhalothrin posed the most significant risk at conventional farms.

  2. Chronic dietary risk characterization for pesticide residues: a ranking and scoring method integrating agricultural uses and food contamination data.

    Nougadère, Alexandre; Reninger, Jean-Cédric; Volatier, Jean-Luc; Leblanc, Jean-Charles

    2011-07-01

    A method has been developed to identify pesticide residues and foodstuffs for inclusion in national monitoring programs with different priority levels. It combines two chronic dietary intake indicators: ATMDI based on maximum residue levels and agricultural uses, and EDI on food contamination data. The mean and 95th percentile of exposure were calculated for 490 substances using individual and national consumption data. The results show that mean ATMDI exceeds the acceptable daily intake (ADI) for 10% of the pesticides, and the mean upper-bound EDI is above the ADI for 1.8% of substances. A seven-level risk scale is presented for substances already analyzed in food in France and substances not currently sought. Of 336 substances analyzed, 70 pesticides of concern (levels 2-5) should be particularly monitored, 22 of which are priority pesticides (levels 4 and 5). Of 154 substances not sought, 36 pesticides of concern (levels 2-4) should be included in monitoring programs, including 8 priority pesticides (level 4). In order to refine exposure assessment, analytical improvements and developments are needed to lower the analytical limits for priority pesticide/commodity combinations. Developed nationally, this method could be applied at different geographic scales.

  3. Comparative residual toxicities of pesticides to the predator Agistemus industani (Acari: Stigmaeidae) on citrus in Florida.

    Childers, C C; Villanueva, R; Aguilar, H; Chewning, R; Michaud, J P

    2001-01-01

    Residual toxicities of registered and selected experimental pesticides used on citrus against Agistemus industani Gonzalez (Acari: Stigmaeidae) were compared. Pesticides considered highly toxic to A. industani were: abamectin 0.15 EC at 731 ml/ha + FC 435-66 petroleum oil at 46.8 l/ha, pyridaben 75 WP at 469 g/ha, ethion 4 EC at 7.01 l/ha + FC 435-66 petroleum oil at 46.8 l/ha, propargite 6.55 EC at 3.51 l/ha, chlorfenapyr 2 SC at 1.46 l/ha applied alone or in combination with FC 435-66 petroleum oil at 46.8 l/ha, sulphur 80 DF at 16.81 kg/ha. dicofol 4EC at 7.01 l/ha, fenbutatin oxide 50 WP at 2.24 kg/ha, benomyl 50 WP at 2.24 kg/ha, benomyl 50 WP at 1.68 kg/ha + ferbam 76 GF at 5.60 kg/ha, ferbam 76 GF at 11.21 kg/ha, neem oil 90 EC at 46.8 l/ha, and copper hydroxide DF (40% metallic copper) at 4.48 kg metallic copper/ha + FC 435-66 petroleum oil at 46.8 l/ha. Pesticides that were moderately to slightly toxic included: copper sulphate 98% at 4.48 kg metallic copper/ha + FC 435-66 petroleum oil at 46.8 l/ha, fenbuconazole 2 F at 280 ml/ha + FC 435-66 petroleum oil at 46.8 l/ha, FC 435-66 petroleum oil applied alone at 46.8 l/ha or 23.41/ha, and diflubenzuron 25 WP at 1.40 kg/ha. Pesticides that were non-toxic included: fenbuconazole 2 F at 585 ml/ha, malathion 57 EC at 5.85 l/ha, FC 435-66 petroleum oil at 46.8 l/ha, carbaryl 80 S at 3.36 kg/ha. chlorpyrifos 4 EC at 4.68 l/ha, and formetanate 92 SP at 1.12 kg/ha. Understanding the toxic effects of field weathered pesticides against key predacious mite species is important for effective IPM. The results of this study provide a comparison of direct and indirect toxic effects of various pesticides to A. industani under field conditions.

  4. Pesticide and plasticizer residues in bergamot essential oils from Calabria (Italy).

    Di Bella, Giuseppa; Saitta, Marcello; La Pera, Lara; Alfa, Maria; Dugo, Giacomo

    2004-08-01

    Organophosphorus and organochlorine pesticides, phosphorated plasticizers, chloroparaffins and phthalate esters contamination in bergamot essential oils produced in Calabria in the crop years 1999-2000 was studied by HRGC in connection with detectors FPD, ECD, MS. Residues of dicofol and tetradifon were found in oils from both crop years. The mean dicofol concentration was 0.26 mg/l in samples from 1999 and 0.20 mg/l in those from 2000; the mean tetradifon content was 0.06 mg/l for both the crop years. Among plasticizers, residues of diisobutyl phthalate, di-n-butyl phthalate, and bis(2-ethylhexyl) phthalate were found in samples from crop years 1999 and 2000, the mean content were 1.22 and 1.23 mg/l, 1.51 and 1.65 mg/l, 1.38 and 1.42 mg/l respectively.

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

    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

  6. Organochlorine pesticide residues in cow's milk from a tropical region of Mexico.

    Pardío, V T; Waliszewski, K N; Landín, L A; Bautista, R G

    2003-03-01

    A monitoring study was conducted to assess the magnitude of DDT [(1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane)] and HCH (hexachlorocyclohexane) contamination of bovine milk from the central tropical region of Mexico as the chemicals are extensively used in livestock and public-health programmes. Among pesticide residues analysed, the milk samples collected from Tlalixcoyan showed a mean level of gamma-HCH (0.128 mg x kg(-1)), which was significantly higher than residues in milk samples from Medellin (0.049 mg x kg(-1)) and Paso San Juan (0.022 mg x kg(-1)). The mean level of pp'-DDE in Medellin samples (0.039 mg x kg(-1)) was significantly higher than in Paso San Juan (0.018 mg x kg(-1)) and Tlalixcoyan (0.024 mg x kg(-1)) milk samples. The pp'-DDT mean level from Medellin milk samples (0.089 mg x kg(-1)) was significantly higher than the levels detected in the other two areas. The highest mean Sigma-DDT level detected in Medellin samples (0.146 mg x kg(-1)) was three times the FAO/WHO tolerance level. The highest acceptable daily intakes calculated for Sigma-DDT were 0.017 microg x kg(-1) bw day(-1) for adults and 0.530 microg x kg(-1) bw day(-1) for infants; for gamma-HCH residues, they were 0.021 microg x kg(-1) bw day(-1) for adults and 0.666 microg x kg(-1) bw day(-1) for infants, indicating that infants are more exposed to pesticide residues. Results indicate that cattle exposure to HCH and DDT results in high levels in dairy milk and a potential health risk for consumers.

  7. 液相微萃取技术在农药残留分析中的应用研究进展%Review on the application of liquid phase microextraction in pesticide residue analysis

    王素利; 杨素萍; 刘丰茂; 薛佳莹; 尤祥伟

    2012-01-01

    Liquid phase microextraction (LPME) is one of novel sample pretreatment techniques which has many advantages such as quick, simple, economic, highly selective and accurate, less-solvent consuming and environmental friendly. It can be matched easily with most of analytical instruments. It includes several types such as single drop microextraction ( SDME) , hollow fiber liquid phase microextraction ( HF-LPME) , dispersive liquid-liquid microextraction ( DLLME ) , solidified floating organic drop microextraction ( SFODME) , continuous-flow microextraction ( CFME ) and directly-suspended droplet microextraction (DSDME) etc. It is a very potential sample pretreatment technique for theoretic and application studies. In this review, the historical development and overview of these miniaturized liquid phase extraction methodologies were discussed and a comprehensive collection of application of these methods for preconcentration and determination of pesticide residue in various matrices were summarized.%液相微萃取技术(LPME)是一种新型的样品前处理方法,具有快速、简单、廉价、选择性强、准确度高、溶剂消耗量少、环境污染小等优点,方便与各种分析仪器联用.其具有多种模式:单滴液相微萃取(SDME)、中空纤维液相微萃取(HF-LPME)、分散液相微萃取(DLLME)、悬浮固化液微萃取(SFODME)、连续流动微萃取(CFME)、直接悬挂液滴微萃取(DSDME)等,具有很好的研究潜力和应用前景.对液相微萃取技术在农药残留分析中的应用研究进展进行了综述.

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

    Wanpen Mesomya

    2012-11-01

    Full Text Available The comparative effects of organic rice and conventional rice on the protein efficiency ratio (PER in rats were investigated by feeding 40 male Sprague-Dawley rats for four weeks with three experimental diets containing polished conventional rice (PCR, unpolished conventional rice (UCR, unpolished organic rice (UOR and a control protein diet (casein under standardised conditions. All diets were prepared according to AOAC guidelines. The results showed no statistically significant difference (P > 0.05 among the values of PER (2.75 ± 0.14 - 2.80 ± 0.09 in rats fed with diets containing PCR, UCR or UOR. Similar growth was also observed among the three groups fed with different experimental diets. Additionally, residues of pesticides, viz. carbofuran, methyl parathion, p-nitrophenol and -cyfluthrin, in rat blood and rice samples were determined using liquid chromatography–electrospray ionisation tandem mass spectrometry. Pesticide residues were not detected in all serum samples of experimental rats and only p-nitrophenol was found (8.23 ± 0.65 - 12.84 ± 2.58 mg/kg in all samples of the cooked rice diets, indicating that organic rice produced similar effect as conventional rice on PER and growth in rats.

  9. Comparison of organochlorine pesticides and polychlorinated biphenyls residues in vegetables, grain and soil from organic and conventional farming in Poland.

    Witczak, Agata; Abdel-Gawad, Hassan

    2012-01-01

    Organic and conventional crops were studied by identifying the relationship between persistent organic pollutants in cereals, vegetables and soil. The residues of organochlorine pesticides and polychlorinated biphenyls (PCBs) were determined in grains (rye and wheat), vegetables (carrots and beets) and soil collected from the fields. PCB residues recorded in the beets from organic farming were as high as 3.71 ppb dry weight (dry wt.), while in the soil from conventional farming of beets 0.53 ppb dry wt. Among vegetables, higher concentrations of pesticides were detected in organically grown beets (190.63 ppb dry wt.). Soil samples from the organic farming contained lower levels of organochlorine pesticide residues compared to the conventional farming. Taking into account toxicity equivalent (TEQ), the conventionally grown carrots accumulated the most toxic PCBs. Non-ortho and mono-ortho PCBs were also noted in the grain of conventionally grown rye and amounted to 3.05 pg-TEQ/g wet wt.

  10. 40 CFR 158.2171 - Experimental use permit microbial pesticides product analysis data requirements table.

    2010-07-01

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

  11. 40 CFR 158.2120 - Microbial pesticides product analysis data requirements table.

    2010-07-01

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

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

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

    2012-05-09

    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, λ-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.

  13. Pesticide residues and estrogenic activity in fruit and vegetables sampled from major fresh produce markets in South Africa.

    Mutengwe, Mbulaheni Thomas; Aneck-Hahn, Natalie Hildegard; Korsten, Lise; Van Zijl, Magdalena Catherina; De Jager, Christiaan

    2016-01-01

    Food is likely to be one of the major pathways through which people are exposed to endocrine-disrupting chemicals. With the exception of residual effects, there are concerns that a number of naturally occurring and synthetic chemicals exert adverse effects upon endocrine systems in wildlife and humans. The current study reports selected pesticide concentrations and the total estrogenic activity of fruit and vegetables using the recombinant yeast oestrogen screen (YES) and T47D-KBluc reporter gene assays. A total of 53 food samples (27 fruit and 26 vegetables) from Johannesburg and Tshwane fresh produce markets (in South Africa) were analysed. Of these, 17 contained one to three different pesticide residues with concentrations ranging between 0.01 and 0.68 mg kg(-1), whereas in the rest of the samples no residues were detected. All pesticides detected except in one sample were below the maximum residue level (MRL), but others were unauthorised for use in specified fruit and vegetables. Estrogenic activity was detected in 26.4% (14 samples) of the samples tested, and the estradiol equivalents ranged from 0.007 to 2 pg g(-1). Although the estrogenic activity was low, it may contribute to adverse health effects. Continuous monitoring for pesticides in fruit and vegetables is important in view of the unauthorised pesticides detected in produce from South Africa and the endocrine-disrupting chemical activity found.

  14. Shell thickness-dependent Raman enhancement for rapid identification and detection of pesticide residues at fruit peels.

    Liu, Bianhua; Han, Guangmei; Zhang, Zhongping; Liu, Renyong; Jiang, Changlong; Wang, Suhua; Han, Ming-Yong

    2012-01-03

    Here, we report the shell thickness-dependent Raman enhancement of silver-coated gold nanoparticles (Au@Ag NPs) for the identification and detection of pesticide residues at various fruit peels. The Raman enhancement of Au@Ag NPs to a large family of sulfur-containing pesticides is ~2 orders of magnitude stronger than those of bare Au and Ag NPs, and there is a strong dependence of the Raman enhancement on the Ag shell thickness. It has been shown for the first time that the huge Raman enhancement is contributed by individual Au@Ag NPs rather than aggregated Au@Ag NPs with "hot spots" among the neighboring NPs. Therefore, the Au@Ag NPs with excellent individual-particle enhancement can be exploited as stand-alone-particle Raman amplifiers for the surface identification and detection of pesticide residues at various peels of fruits, such as apple, grape, mango, pear, and peach. By casting the particle sensors onto fruit peels, several types of pesticide residues (e.g., thiocarbamate and organophosphorous compounds) have been reliably/rapidly detected, for example, 1.5 nanograms of thiram per square centimeter at apple peel under the current unoptimized condition. The surface-lifting spectroscopic technique offers great practical potentials for the on-site assessment and identification of pesticide residues in agricultural products.

  15. Pesticides in persimmons, jujubes and soil from China: Residue levels, risk assessment and relationship between fruits and soils.

    Liu, Yihua; Li, Shiliang; Ni, Zhanglin; Qu, Minghua; Zhong, Donglian; Ye, Caifen; Tang, Fubin

    2016-01-15

    Extreme and uncontrolled usage of pesticides produces a number of problems for vegetation and human health. In this study, the existence of organophosphates (OPs), organochlorines (OCs), pyrethroids (PYs) and fungicides (FUs) were investigated in persimmons/jujubes and their planted soils, which were collected from China. One OP (dimethoate), three OCs (DDT, quintozene and aldrin), six PYs (bifenthrin, fenpropathrin, cyhalothrin, cypermethrin, fenvalerate and deltamethrin) and two FUs (triadimefon and buprofezin) were found in 36.4% of persimmons and 70.8% of jujubes, with concentrations from 1.0 μg/kg to 2945.0 μg/kg. The most frequently detected pesticides in the two fruits were fenpropathrin in persimmons and cypermethrin in jujubes, with the detection frequencies of 30.0% and 22.7%, respectively. The residues of 4.5% (persimmon) and 25.0% (jujube) of samples were higher than the maximum residue limits (MRLs) of China. Compared with the fruits, more types of pesticides and higher residues were observed in their planted soils. The most frequently detected pesticides were HCH in persimmon soil and DDT in jujube soil, with the detection frequencies of 10.9% and 12.7%, respectively. For the tested samples, 39.1% of fruit samples and 63.0% of soil samples with multiple residues (containing more than two pesticides) were noted, even up to 8 residues in fruits and 14 residues in soils. Except for cyhalothrin, the other short-term risks for the tested pesticides in the fruits were below 10%, and the highest long-term risk was 14.13% for aldrin and dieldrin. There was no significant health risk for consumers via consumption of the two fruits.

  16. Simultaneous determination of 200 pesticide residues in honey using gas chromatography-tandem mass spectrometry in conjunction with streamlined quantification approach.

    Shendy, Amr H; Al-Ghobashy, Medhat A; Mohammed, Moustapha N; Gad Alla, Sohair A; Lotfy, Hayam M

    2016-01-01

    A sensitive, accurate and reliable multi-class GC-MS/MS assay protocol for quantification and confirmation of 200 common agricultural pesticides in honey was developed and validated according to EU guidelines. A modified extraction procedure, based on QuEChERS method (quick, easy, cheap, effective, rugged and safe) was employed. Mass spectrophotometric conditions were individually optimized for each analyte to achieve maximum sensitivity and selectivity in MRM mode. The use of at least two reactions for each compound allowed simultaneous identification and quantification in a single run. The pesticides under investigation were separated in less than 31 min using the ultra-inert capillary column (DB-35MS). For all analytes, neat standard calibration curves in conjunction with correction for matrix effect were successfully employed. The detection limits of the assay ranged from 1.00 to 3.00 ng mL(-1) for the studied pesticides. The developed assay was linear over concentration range of 10.00-500.00 ng mL(-1), with correlation coefficient of more than 0.996. At the LOQ, 81% of the studied pesticides were efficiently recovered in the range of 70.00-120.00%, with CV% less than 15.00% while 99.3% compounds had mean percentage recovery of 60.00-140.00%, with CV% less than 21.00% (N=18, over three different days). The proposed assay was successfully applied for the analysis of the studied pesticide residues in one PT sample and 64 commercial honey samples collected over 1 year from different districts around Egypt. Results revealed that only one honey sample out of the 64 analyzed samples was contaminated with tau-Fluvalinate (10.00 μg kg(-1)). This wide scope assay protocol is applicable for monitoring pesticide residues in honey by national regulatory authorities and accredited labs; that should help ensure safety of such widely used product.

  17. Evaluation of ozonation technique for pesticide residue removal and its effect on ascorbic acid, cyanidin-3-glucoside, and polyphenols in apple (Malus domesticus) fruits.

    Swami, Saurabh; Muzammil, Raunaq; Saha, Supradip; Shabeer, Ahammed; Oulkar, Dasharath; Banerjee, Kaushik; Singh, Shashi Bala

    2016-05-01

    Ozonated water dip technique was evaluated for the detoxification of six pesticides, i.e., chlorpyrifos, cypermethrin, azoxystrobin, hexaconazole, methyl parathion, and chlorothalonil from apple fruits. Results revealed that ozonation was better than washing alone. Ozonation for 15 min decreased residues of the test pesticides in the range of from 26.91 to 73.58%, while ozonation for 30 min could remove the pesticide residues by 39.39-95.14 % compared to 19.05-72.80 % by washing. Cypermethrin was the least removed pesticide by washing as well as by ozonation. Chlorothalonil, chlorpyrifos, and azoxystrobin were removed up to 71.45-95.14 % in a 30-min ozonation period. In case of methyl parathion removal, no extra advantage could be obtained by ozonation. The HPLC analysis indicated that ozonation also affected adversely the ascorbic acid and cyanidin-3-glucoside content of apples. However, 11 polyphenols studied showed a mixed trend. Gallic acid, 3,4-dihydroxybenzoic acid, catechin, epicatechin, p-coumaric acid, quercetin-3-O-glucoside, quercetin, and kaempferol were found to decrease while syringic acid, rutin, and resveratrol were found to increase in 30-min ozonation.

  18. Hair as a marker for pesticides exposure.

    Smith-Baker, Charlotte; Saleh, Mahmoud A

    2011-01-01

    Rats were orally treated with mixtures of chlorinated pesticides. Hair was collected and analyzed for pesticide residues over a period of up to four weeks. Quantitative and qualitative analysis of the recovered pesticides in hair were determined using gas chromatography with electron capture detector. Results suggest that hair can be used as a biomarker for the monitoring of organochlorinated pesticide residues at low parts per billion levels. Chlorinated pesticides were also detected in human hair of environmentally exposed and occupationally exposed individuals, which indicates that hair can be used for monitoring pesticides exposure.

  19. [Study of multi-residue method for determining pesticide residues in processed foods manufactured from agricultural products by LC-MS/MS].

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

    2013-01-01

    A rapid multi-residue method for determination of pesticide residues in processed foods manufactured from agricultural products was examined. Five mL water was added to 5 g sample in a polypropylene tube, and the tube was left to stand at room temperature for 30 min. Then, 20 mL acetonitrile was added to the sample. The mixture was homogenized in a high-speed homogenizer, followed by salting out with 1 g NaCl and 4 g anhydrous MgSO4. After centrifugation, the organic layer was purified on a graphitized carbon/PSA cartridge column. After removal of the solvent, the extract was resolved in methanol-water and analyzed with LC-MS/MS. The recoveries of 93 pesticides fortified into 5 kinds of processed foods [Chinese cabbage kimchi, marmalade, raisin, umeboshi (pickled plum) and worcester sauce] were examined at the concentrations of 0.02 and 0.1 μg/g (n=5). The recoveries of 61 pesticides in all foods were 70-120% with relative standard deviation below 20% at both concentrations. Seventy-four processed foods obtained from markets in Japan were examined with this method. Pesticide residues over the maximum residue limit (0.01 μg/g) were detected in 2 processed foods.

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

    Boesten, J J T I

    2016-02-15

    The environmental significance of soil bound pesticide residues (SBPR) is potentially large because approximately one third of the applied mass of the pesticides in agriculture ends up as SBPR. At EU level, there is little regulatory guidance available on the environmental risk assessment of SBPR in spite of some 50 years of SBPR research. This lack of guidance is partially caused by the fact that the current definitions of SBPR are founded on non-extractability in soil in the laboratory whereas for the environmental risk assessment not the soil in the laboratory but the soil in the field is the system of interest. Therefore a definition of SBPR is proposed that is based on the field soil: a molecule (further called 'the mother molecule') is soil bound if a relevant part of this molecule has become part of the solid phase in the soil and if this relevant part will never be released again to the liquid phase in soil under relevant field conditions in the form of this mother molecule or in the form of another molecule that may possibly raise environmental or human toxicological concerns. This mother molecule may be the parent substance that is applied to the soil but it may also be a metabolite of this parent substance. A consequence of the definition is that the SBPR terminology becomes more precise because the mother molecule of the soil bound residue has to be specified. A further consequence is that very strong but reversible sorption of molecules such as paraquat is not considered soil-bound residue anymore (as may be demonstrated by a self-exchange extraction procedure). Furthermore, the definition requires that risk managers have to define what they consider as 'relevant field conditions' (e.g. include also changes of agricultural fields into forests?).

  1. 78 FR 6274 - Withdrawal of Pesticide Petitions for Residues of Pesticide Chemicals in or on Various Commodities

    2013-01-30

    ...), which announced the filing of a pesticide petition (PP 0E7754) by Quimica Agronomica de Mexico, S. de R... Quimica Agronomica de Mexico) notified EPA that it was withdrawing this petition. Contact: Shaunta Hill...), which announced the filing of pesticide petition (PP 0E7755) by Quimica Agronomica de Mexico, S. de...

  2. Occurrence and spatial distribution of pesticide residues in butter and ghee (clarified butter fat) in Punjab (India).

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

    2016-02-01

    The present study was undertaken to monitor organochlorine, organophosphate, and synthetic pyrethroid pesticide residues in butter (n = 55) and ghee (n = 56) samples collected from three different regions of Punjab. The estimation of pesticide residues was done by multiple residue analytical technique using gas chromatography equipped with GC-ECD and GC-FTD. The confirmation of residues was done on gas chromatography mass spectrometry in both selective ion monitoring (SIM) and scan mode. Results indicated the presence of hexacholorocyclohexane (HCH) and p,p' DDE as predominant contaminant in both butter and ghee. Residues of HCH were detected in 25 and 23% samples of butter and ghee, respectively, while residues of p,p' DDE were recorded in 29 and 25% of butter and ghee samples, respectively. None of the butter and ghee sample violated the MRL values of 200 ng g(-1) for HCH and 1250 ng g(-1) for dichorodiphenyl tricholorethane (DDT). The presence of endosulfan, cypermethrin, fenvalerate, deltamethrin, and chlorpyrifos were observed in a few butter and ghee samples at traces. The spatial variation for comparative occurrence of pesticide residues indicated higher levels in the south-western region of Punjab. Additionally, the temporal variation indicated the significant reduction of HCH and DDT levels in butter and ghee in Punjab.

  3. Pesticides

    ... FAQ Methadone FAQ Buprenorphine FAQ Dextromethorphan Ethylene Glycol Pesticides AnabolicSteroids HomeNaloxone Button Batteries Cocaine Carbon Monoxide Designer Amphetamines NSAID_FAQ Killer Bees Energy Drinks Heat Illness Nicotine Magnets Synthetic Cannabinoids ...

  4. Screening and quantification of pesticide residues in fruits and vegetables making use of gas chromatography-quadrupole time-of-flight mass spectrometry with atmospheric pressure chemical ionization.

    Cervera, M I; Portolés, T; López, F J; Beltrán, J; Hernández, F

    2014-11-01

    An atmospheric pressure chemical ionization source has been used to enhance the potential of gas chromatography coupled with quadrupole time-of-flight (QTOF) mass spectrometry (MS) for screening and quantification purposes in pesticide residue analysis. A screening method developed in our laboratory for around 130 pesticides has been applied to fruit and vegetable samples, including strawberries, oranges, apples, carrots, lettuces, courgettes, red peppers, and tomatoes. Samples were analyzed together with quality control samples (at 0.05 mg/kg) for each matrix and for matrix-matched calibration standards. The screening strategy consisted in first rapid searching and detection, and then a refined identification step using the QTOF capabilities (MS(E) and accurate mass). Identification was based on the presence of one characteristic m/z ion (Q) obtained with the low collision energy function and at least one fragment ion (q) obtained with the high collision energy function, both with mass errors of less than 5 ppm, and an ion intensity ratio (q/Q) within the tolerances permitted. Following this strategy, 15 of 130 pesticides were identified in the samples. Afterwards, the quantitation capabilities were tested by performing a quantitative validation for those pesticides detected in the samples. To this aim, five matrices were selected (orange, apple, tomato, lettuce, and carrot) and spiked at two concentrations (0.01 and 0.1 mg/kg), and quantification was done using matrix-matched calibration standards (relative responses versus triphenyl phosphate used as an internal standard). Acceptable average recoveries and relative standard deviations were obtained for many but not all pesticide-matrix combinations. These figures allowed us to perform a retrospective quantification of positives found in the screening without the need for additional analysis. Taking advantage of the accurate-mass full-spectrum data provided by QTOF MS, we searched for a higher number of compounds

  5. [Comparison of the performances of gas chromatography-quadrupole time of flight mass spectrometry and gas chromatography-tandem mass spectrometry in rapid screening and confirmation of 208 pesticide residues in fruits and vegetables].

    Cao, Xinyue; Pang, Guofang; Jin, Linghe; Kang, Jian; Hu, Xueyan; Chang, Qiaoying; Wang, Minglin; Fan, Chunlin

    2015-04-01

    The performances of gas chromatography-tandem mass spectrometry (GC-MS/MS) and gas chromatography quadrupole time of flight mass spectrometry (GC-QTOF/MS) for the determination of 208 pesticide residues in fruit and vegetable samples, including apple, orange, tomato and cucumber, were compared comprehensively. Based on the differences of the two instruments, their respective characteristics and scopes of application in the detection of the pesticide residues were presented, which provided the reference for the analysis of pesticide residues. The performance parameters of the two instruments, such as overall recoveries, precisions, limits of detection, linear ranges, identification points and matrix effects, were evaluated according to a designed experiment. At three spiked levels (5.0, 10.0 and 20.0 µg/kg), the average recoveries for the majority of pesticides (93.0%) ranged from 70% to 120% in the four matrices with relative standard deviations below 20%. The limits of detection for most of the pesticides by GC-MS/MS and GC-Q-TOF/MS were less than 5.0 µg/kg. Compared with GC-QTOF/MS, GC-MS/MS showed relatively lower limits of detection and wider linear ranges, and its performance was more satisfactory in accurate quantitative analysis due to its superior sensitivity. On the other hand, GC-QTOF/MS provided accurate mass measurement, which was proved to be an efficient analytical tool on the rapid screening and confirmation of a large number of pesticides and non-target compounds.

  6. Pesticide nonextractable residue formation in soil: insights from inverse modeling of degradation time series.

    Loos, Martin; Krauss, Martin; Fenner, Kathrin

    2012-09-18

    Formation of soil nonextractable residues (NER) is central to the fate and persistence of pesticides. To investigate pools and extent of NER formation, an established inverse modeling approach for pesticide soil degradation time series was evaluated with a Monte Carlo Markov Chain (MCMC) sampling procedure. It was found that only half of 73 pesticide degradation time series from a homogeneous soil source allowed for well-behaved identification of kinetic parameters with a four-pool model containing a parent compound, a metabolite, a volatile, and a NER pool. A subsequent simulation indeed confirmed distinct parameter combinations of low identifiability. Taking the resulting uncertainties into account, several conclusions regarding NER formation and its impact on persistence assessment could nonetheless be drawn. First, rate constants for transformation of parent compounds to metabolites were correlated to those for transformation of parent compounds to NER, leading to degradation half-lives (DegT50) typically not being larger than disappearance half-lives (DT50) by more than a factor of 2. Second, estimated rate constants were used to evaluate NER formation over time. This showed that NER formation, particularly through the metabolite pool, may be grossly underestimated when using standard incubation periods. It further showed that amounts and uncertainties in (i) total NER, (ii) NER formed from the parent pool, and (iii) NER formed from the metabolite pool vary considerably among data sets at t→∞, with no clear dominance between (ii) and (iii). However, compounds containing aromatic amine moieties were found to form significantly more total NER when extrapolating to t→∞ than the other compounds studied. Overall, our study stresses the general need for assessing uncertainties, identifiability issues, and resulting biases when using inverse modeling of degradation time series for evaluating persistence and NER formation.

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

    Yuningsih

    2006-03-01

    Full Text Available Organochlorine pesticide contamination in feed can cause residue in animal product (tissue and milk, so its become a problem in food safety. Solid phase extraction (SPE has been carried out for determination organochlorine pesticide residues in food animal production. The technique was rapid, not costly and produce limited amount of hazardous-waste. Samples were homogenized with acetonitrile trough cartridge C18, eluted in fluorocyl column with 2% ether-petroleum or acetonitrile fortissue and milk samples respectively. The recoveries of tissue sample by addition lindane standard solution: 0.50 and 1.00 μg are 85.10 and 103.10% respectively, while that of milk with the addition of 0.50, 1.00 and 1.50 μg are 83.80, 88.69 and 91.24% respectively. Three replicates were carried out for every sample. According of validation criteria of FAO/IAEA the recovery for analysis of pesticide residues was 70-110%. Therefore, the method is applicable.

  8. [Determination of five pyrethroid pesticides residues in Anoectochilus roxburghii by cloud point extraction-back extraction and GC-MS].

    Liu, Hong-Bo; Zhao, Xiao-Fang; Shi, Gui-Ying; Shao, Qing-Song; Li, Mine-Van

    2014-08-01

    A method for residual determination of 5 pyrethroid pesticides in Anoectochilus roxburghii by cloud point extraction-back extraction-GC-MS was established. PEG 6000 was used as extraction agent and isooctane was used for back-extractant. The con- tent was calculated by external standard method. The linear range was from 15 to 2 000 μg x kg(-1) with the good correlation coefficients (0.955-0.999). The recoveries at spiked concentrations of 50-500 μg x kg(-1) ranged from 85.12% to 101.6%. The limit of detection and quantification of 5 pyrethroid pesticides were in the range of 0.63-3.10 μg x kg(-1) and 2.10-10.31 μg x kg(-1), respectively. The proposed method can be applied to the determination of pyrethroid pesticides residues in A. roxburghii.

  9. Prediction of Gas Chromatography-Mass Spectrometry Retention Times of Pesticide Residues by Chemometrics Methods

    Elaheh Konoz

    2013-01-01

    Full Text Available A quantitative structure-retention relationships (QSRRs method is employed to predict the retention time of 300 pesticide residues in animal tissues separated by gas chromatography-mass spectroscopy (GC-MS. Firstly, a six-parameter QSRR model was developed by means of multiple linear regression. The six molecular descriptors that were considered to account for the effect of molecular structure on the retention time are number of nitrogen, Solvation connectivity index-chi 1, Balaban Y index, Moran autocorrelation-lag 2/weighted by atomic Sanderson electronegativity, total absolute charge, and radial distribution function-6.0/unweighted. A 6-7-1 back propagation artificial neural network (ANN was used to improve the accuracy of the constructed model. The standard error values of ANN model for training, test, and validation sets are 1.559, 1.517, and 1.249, respectively, which are less than those obtained reveals by multiple linear regressions model (2.402, 1.858, and 2.036, resp.. Results obtained the reliability and good predictability of nonlinear QSRR model to predict the retention time of pesticides.

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

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

    2015-09-25

    The presence of pesticide residues in the surface water of Bertam River in the agricultural areas of Cameron Highlands in Pahang, Malaysia was monitored from May to October 2014. The sampling sites were located at 10 sampling points along the Bertam River in the vegetable planting areas. The extraction method of the pesticide (organophosphate/pyrethroid) from the river samples used solid phase extraction followed by gas chromatography (with electron capture detector, ECD). Insecticides, cypermethrin and chlorpyrifos were found in the surface water of Bertam River. High level concentrations of those insecticides in the river were observed during the period from May to October 2014, a period which included both seasons (wet and dry seasons). The highest concentration of 2.66 µg/mL and 1.23 µg/mL of cypermethrin was observed during the wet and dry seasons respectively. This could be due to the frequent usage of the above-mentioned insecticides coupled with contamination that could have originated from the application sites. Meanwhile, the lowest concentration detected in the surface water was chlorpyrifos (0.11 µg/mL and 0.17 µg/mL) during the dry and wet seasons, respectively.

  11. Field evaluations of residual pesticide applications and misting system on militarily relevant materials against medically important mosquitoes in Thailand

    A key strategy to reduce insect-borne disease is to reduce contact between disease vectors and hosts. In the current study, residual pesticide application and misting system were applied on militarily relevant materials and evaluated against medically important mosquitoes. Field evaluations were car...

  12. [Evidence of pesticide exposure by hair analysis].

    Cirimele, V; Kintz, P; Ludes, B

    1999-01-01

    The current report summarizes the development of an analytical method for the identification and the quantification of pesticides in hair by gas chromatography/mass spectrometry and its application to 75 real samples. Hair strands [table: see text] were obtained from wine workers exposed to one or more pesticides. After decontamination, hair were cut into small pieces and incubated overnight at 45 degrees C in methanol. The solvent was evaporated to dryness, the dry extract was redissolved in methanol and injected in a gas chromatography/mass spectrometry system. The detector was operated in electronic impact and in negative chemical ionization mode of detection (reactant gas: methane). In the first series of 75 hair specimens, obtained before the period of pesticide use, none of the 15 target compounds was detected. In the second series of 75 specimens, obtained from the same subjects but after the use of pesticides, 14 tested positive for 9 different pesticides.

  13. Employing Solid Phase Microextraction as Extraction Tool for Pesticide Residues in Traditional Medicinal Plants

    Gondo, Thamani T.; Mmualefe, Lesego C.; Okatch, Harriet

    2016-01-01

    HS-SPME was optimised using blank plant sample for analysis of organochlorine pesticides (OCPs) of varying polarities in selected medicinal plants obtained from northern part of Botswana, where OCPs such as DDT and endosulfan have been historically applied to control disease carrying vectors (mosquitos and tsetse fly). The optimised SPME parameters were used to isolate analytes from root samples of five medicinal plants obtained from Maun and Kasane, Botswana. The final analytes determination was done with a gas chromatograph equipped with GC-ECD and analyte was confirmed using electron ionisation mass spectrometer (GC-MS). Dieldrin was the only pesticide detected and confirmed with MS in the Terminalia sericea sample obtained from Kasane. The method was validated and the analyte recoveries ranged from 69.58 ± 7.20 to 113 ± 15.44%, with RSDs ranging from 1.19 to 17.97%. The method indicated good linearity (R2 > 0.9900) in the range of 2 to 100 ng g−1. The method also proved to be sensitive with low limits of detection (LODs) ranging from 0.48 ± 0.16 to 1.50 ± 0.50 ng g−1. It can be concluded that SPME was successfully utilized as a sampling and extraction tool for pesticides of diverse polarities in root samples of medicinal plants. PMID:27725893

  14. Detection of residual organochlorine and organophosphorus pesticides in agricultural soil in Rio Verde region of San Luis Potosi, Mexico.

    Velasco, Antonio; Hernández, Sergio; Ramírez, Martha; Ortíz, Irmene

    2014-01-01

    Organochlorine pesticides were intensively used in Mexico from 1950 until their ban and restriction in 1991. However, the presence of these compounds is commonly reported in many regions of the country. The aim of the present study was to identify and quantify residual organochlorine and organophosphorus pesticides in agricultural soil in Rio Verde region, San Luis Potosi state, which has been identified as possibly polluted by pesticides. Composed samples from 24 zones covering an area of approximately 5,440 ha were analyzed. The most frequently found pesticides were p,p'-DDT followed by ,p,p'-DDE, heptachlor, endosulfan and γ-HCH whose frequency rates were 100, 91, 83 and 54%, respectively. The concentration of p,p'-DDT in the crops grown in these soils was in the following order: chili > maize > tomato > alfalfa. The results obtained in this study show that p,p'-DDT values are lower or similar to those found in other agricultural regions of Mexico. Methyl and ethyl parathion were the most frequent organophosphate pesticide detected in 100% and 62.5% of the samples with average concentrations of 25.20 and 47.48 μg kg(-1), respectively. More research is needed to establish the background levels of pesticides in agricultural soils and their potential ecological and human health effects in this region.

  15. Multiresidue analysis of pesticides in vegetables and fruits using a high capacity absorbent polymer for water.

    Obana, H; Akutsu, K; Okihashi, M; Kakimoto, S; Hori, S

    1999-08-01

    A single extraction and a single clean-up procedure was developed for multi-residue analysis of pesticides in non-fatty vegetables and fruits. The method involves the use of a high capacity absorbent polymer for water as a drying agent in extraction from wet food samples and of a graphitized carbon column for clean-up. A homogeneously chopped food sample (20 g) and polymer (3 g) were mixed to absorb water from the sample and then 10 min later the mixture was vigorously extracted with ethyl acetate (100 ml). The extract (50 ml), separated by filtration, was loaded on a graphitized carbon column without concentration. Additional ethyl acetate (50 ml) was also eluted and both eluates were concentrated to 5 ml for analysis. The procedure for sample preparation was completed within 2 h. In a recovery test, 107 pesticides were spiked and average recoveries were more than 80% from asparagus, orange, potato and strawberry. Most pesticides were recovered in the range 70-120% with usually less than a 10% RSD for six experiments. The results indicated that a single extraction with ethyl acetate in the presence of polymer can be applied to the monitoring of pesticide residues in foods.

  16. Spectrum of Organochlorine Pesticide Residues in Fish Samples from the Densu Basin

    Samuel Afful

    2010-07-01

    Full Text Available In this study, the levels of organochlorine pesticide residues in the Densu basin have been investigated using fish sam ples as a case study. Six fish species namely Heterotis niloticus, Channa obscura, Hepsetus odoe, Tilapia zilli, Clarias gariepinus and Chrysichthys nigrodigitatus were collected from the sampling towns, Weija and Nsawam along the Densu river basin in the Greater Accra Region of Ghana. Composite samples w ere homogenized, freeze dried and ground to obtain powdered samples. The powdered samples were extracted by soxhlet extraction procedure using (3:1 hexane: acetone mixture. The extracts were cleaned-up using florisil adsorbent and characterized for organochlorine content using Gas Chromatography (GC equipped with Electron Capture Detector (ECD. The GC recoveries of spiked samples were between 80 to 96%. Fourteen organochlorines (OCs namely gamma-HCH, delta-HCH, heptachlor, aldrin, gammachlordane, p,p’-DDE, alpha-endosulfan, dieldrin, endrin, endrin-aldehyde, endosulfan-sufate, p,p’-DDT, endrinketone and methoxychlor were identified and quantified. A 100% incidence was recorded for gamma-HCH, delta-HCH, heptachlor, aldrin, gamma-chlordane, alpha-endosulfan, dieldrin and p,p’-DDT, while 75% incidence was recorded for the metabolites, p,p’-DDE and endosulfan-sulfate. The concentrations of OCs ranged from 0.3 to 71.3 :g/kg and were however, below the Australian Maximum Residue Limits (MRL of 50 to 1000 :g/kg for fresh w ater fish.

  17. Pesticide residues in tomatoes from greenhouses in Souss Massa Valley, Morocco.

    Salghi, R; Luis, G; Rubio, C; Hormatallah, A; Bazzi, L; Gutiérrez, A J; Hardisson, A

    2012-03-01

    Eight pesticide residues in tomato samples collected in the area of Souss Massa Valley (Southern Morocco) were analyzed. The detected residue levels ranged from 0.001 to 0.400 mg kg(-1) for dicofol, from 0.003 to 0.170 mg kg(-1) for procymidone, from 0.001 to 0.250 mg kg(-1) for chlorothalonil, from 0.050 to 0.500 mg kg(-1) for bifenthrin, from 0.001 to 0.010 mg kg(-1) for λ-cyhalothrin, from 0.001 to 0.300 mg kg(-1) for cypermethrin, from 0.010 to 1 mg kg(-1) for deltamethrin and from 0.003 to 1.123 mg kg(-1) for endosulfan. European MRL for endosulfan in tomatoes set in 0.500 mg kg(-1), was exceeded in 8 samples, and MRL for deltamethrin set in 0.300 mg kg(-1) for tomatoes was exceeded in 2 samples.

  18. Organochlorine pesticide residues in sediments from the Uganda side of Lake Victoria.

    Wasswa, John; Kiremire, Bernard T; Nkedi-Kizza, Peter; Mbabazi, Jolocam; Ssebugere, Patrick

    2011-01-01

    Organochlorine (OC) residues were analysed in 117 sediment samples collected from four bays of the Uganda side of Lake Victoria. The sediments were collected with a corer at a depth of 0-20 cm, and extracted for OC residues using a solid dispersion method. The extracts were cleaned using gel permeation chromatography and analysed for pesticide residues using a gas chromatograph (GC) equipped with an electron capture detector. The results were confirmed using a GC equipped with a mass spectrometer (MS). A total of 16 OC residues, most of them persistent organic pollutants (POPs) were identified and quantified. The OC residue levels were expressed on an oven dry weight (d.w.) basis. Endosulphan sulphate, in the range of 0.82-5.62 μg kg⁻¹ d.w., was the most frequently detected residue. Aldrin and dieldrin were in the ranges of 0.22-15.96 and 0.94-7.18 μg kg⁻¹ d.w., respectively. DDT and its metabolites lay between 0.11-3.59 for p,p'-DDE, 0.38-4.02 for p,p'-DDD, 0.04-1.46 for p,p'-DDT, 0.07-2.72 for o,p'-DDE and 0.01-1.63 μg kg⁻¹ d.w. for o,p'-DDT. The levels of γ-HCH varied from 0.05 to 5.48 μg kg⁻¹ d.w. Heptachlor was detected only once at a level of 0.81 μg kg⁻¹ d.w., while its photo-oxidation product, heptachlor epoxide, ranged between non-detectable (ND) to 3.19 μg kg⁻¹ d.w. Chlordane ranged from ND to 0.76 μg kg⁻¹ d.w. Based on the threshold effect concentration (TEC) for fresh water ecosystems, aldrin and dieldrin were the only OCs that seemed to be a threat to the lake environment.

  19. [Validation Study on a Multi-Residue Method for Determination of Pesticide Residues in Vegetables and Fruits by using General Matrix Standard Solutions].

    Fukui, Naoki; Takatori, Satoshi; Yamaguchi, Satoko; Kitagawa, Yoko; Yoshimitsu, Masato; Osakada, Masakazu; Kajimura, Keiji; Obana, Hirotaka

    2015-01-01

    Quantitative methods using the matrix-matched standard solutions approach are widely used for multi-residue pesticide determination by GC-MS/MS to deal with the issue of matrix effects. However, preparing matrix-matched standard solutions in analyses of many kinds of samples is very time-consuming. In order to solve this problem, a method that employs general matrix standard solutions has been developed using polyethylene glycol (PEG), extract of vegetables-fruit juice (VFJm) and triphenyl phosphate (named the PEG-VFJm method). Here, a validation study for 168 pesticides was performed on three kinds of samples [potato, spinach and apple] at concentrations of 0.010 and 0.050 μg/g. In these three commodities, 144 to 158 pesticides satisfied the required criteria using the matrix-matched method and 129 to 149 pesticides satisfied the same criteria using the PEG-VFJm method. Our results suggest that application of general matrix standard solutions would enable rapid and effective analyses of pesticides.

  20. Human health risks associated with residual pesticide levels in edible tissues of slaughtered cattle in Benin City, Southern Nigeria

    Isioma Tongo

    2015-01-01

    Full Text Available Pesticide residues in meat is of growing concern due to possible adverse effects on humans. Pesticide levels were assessed in five edible cattle parts: muscle, liver, kidney and tongue tissues to determine human health risk associated with consumption of these tissues. Health risk estimates were analysed using estimated daily intake (EDI, hazard quotient (HQ and hazard index (HI for two (2 age/weight categories: 1–11years/30 kg for children while 70 kg was used for adult. Risks were categorized for non-carcinogenic and carcinogenic health effects and measured at the average, maximum, 50th and 95th percentiles of the measured exposure concentrations (MEC. Total pesticide residues ranged from 2.38 to 3.86 μg/kg (muscle, 3.58 to 6.3 μg/kg (liver, 1.87 to 4.59 μg/kg (kidney and 2.54 to 4.35 μg/kg (tongue. Residual pesticide concentrations in the tissues were in the order: Liver > Tongue > Muscle > Kidney. The concentrations of all the assessed pesticides observed in the tissues were however lower than the recommended maximum residual limits (MRLs. Human health risk estimations for the children showed EDI values for heptachlor epoxide, aldrin and dieldrin exceeding threshold values. Non-cancer risk posed to children on consumption of contaminated cattle parts showed HQ values for heptachlor epoxide, aldrin, dieldrin and HI values for organochlorines exceeding 1, indicating the possibility of non-carcinogenic health risks to consumers especially children from consumption of cattle meat from the selected abattoirs.

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

    M. H. EL-Saeid

    2013-01-01

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

  2. Automated Multiplug Filtration Cleanup for Pesticide Residue Analyses in Kiwi Fruit (Actinidia chinensis) and Kiwi Juice by Gas Chromatography-Mass Spectrometry.

    Qin, Yuhong; Zhang, Jingru; He, Yining; Han, Yongtao; Zou, Nan; Li, Yanjie; Chen, Ronghua; Li, Xuesheng; Pan, Canping

    2016-08-10

    To reduce labor-consuming manual operation workload in the cleanup steps, an automated multiplug filtration cleanup (m-PFC) method for QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts was developed. It could control the volume and speed of pulling and pushing cycles accurately. In this study, m-PFC was based on multiwalled carbon nanotubes (MWCNTs) mixed with primary-secondary amines (PSA) and anhydrous magnesium sulfate (MgSO4) in a packed column for analysis of pesticide residues followed by gas chromatography-mass spectrometry (GC-MS) detection. It was validated by analyzing 33 pesticides in kiwi fruit and kiwi juice matrices spiked at two concentration levels of 10 and 100 μg/kg. Salts, sorbents, m-PFC procedure, 4 mL of automated pulling and pushing volume, 6 mL/min automated pulling speed, and 8 mL/min pushing speed were optimized for each matrix. After optimization, spike recoveries were within 71-120% and kiwi fruit and kiwi juice. Matrix-matched calibrations were performed with the coefficients of determination >0.99 between concentration levels of 10 and 1000 μg/kg. The developed method was successfully applied to the determination of pesticide residues in market samples.

  3. European Pesticide Tax Schemes in Comparison: An Analysis of Experiences and Developments

    Thomas Böcker

    2016-04-01

    Full Text Available Policy measures are needed to reduce the risks associated with pesticides’ application in agriculture, resulting in more sustainable agricultural systems. Pesticide taxes can be an important tool in the toolkit of policy-makers and are of increasing importance in European agriculture. However, little is known about the effects of such tax solutions and their impacts on the environment, farmers, and human health. We aim to fill this gap and synthesize experiences made in the European countries that have introduced pesticide taxes, i.e., France, Denmark, Norway, and Sweden. The major findings of our analysis are: (1 overall, the effectiveness of pesticide taxes is limited, but if a tax on a specific pesticide is high enough, the application and the associated risks will be reduced significantly; (2 in all countries, hoarding activities have been observed before a tax introduction or increase. Therefore, short-term effects of taxes are substantially smaller than long-term effects; (3 differentiated taxes are superior to undifferentiated taxes because fewer accompanying measures are required to reach policy goals; (4 tax scheme designs are not always in line with the National Action Plan targets. Low tax levels do not necessarily lead to a reduction of pesticide input and differentiated taxes do not necessarily lead to fewer violations of water residue limits.

  4. Study of Organochlorinated Pesticide Residues and PCBs in Vegetable and Fruit Samples from market in Peja –Kosovo

    MSc. Defrime Berisha

    2013-12-01

    In this study, were analyzed samples of fruit and vegetables from the market of Peja, Kosovo in September 2011. Ultrasonic extraction was used for extracting pesticide residues from samples. Clean-up procedure was performed using firstly sulfuric acid followed a second clean-up procedure in an “open” florisil column. The organochlorine pesticides detected were HCHs (a-, b-, γ- and d-isomers and the DDT-related chemicals (o,p-DDE, p,p-DDE, p,p-DDD, p,p-DDT, hexachlorobenzene (HCB, heptachlor, heptachlor epoxide, methoxychlor and Aldrine’s. Analyses were done with capillary column Rtx-5, 60m long, 0.32mm internal diameter, 0.25 μm film thicknesses on a gas chromatograph Dani 1000, with μECD detector. The found concentrations of the chlorinated pesticides were lower than accepted levels for studied samples

  5. 75 FR 13277 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-03-19

    ... manufacturing (NAICS code 311). Pesticide manufacturing (NAICS code 32532). This listing is not intended to be...-chloro-3,3,3,-trifluoro-1-propenyl)-2,2- dimethylcyclopropanecarboxylate), in or on tea (import tolerance... onion, bulb, subgroup 3-07A at 0.2 ppm; onion, green, subgroup 3-07B at 9.0 ppm; caneberry subgroup...

  6. Reduction in pesticide residue levels in olives by ozonated and tap water treatments and their transfer into olive oil.

    Kırış, Sevilay; Velioglu, Yakup Sedat

    2016-01-01

    The effects of different wash times (2 and 5 min) with tap and ozonated water on the removal of nine pesticides from olives and the transfer ratios of these pesticides during olive oil production were determined. The reliability of the analytical methods was also tested. The applied methods of analysis were found to be suitable based on linearity, trueness, repeatability, selectivity and limit of quantification all the pesticides tested. All tap and ozonated water wash cycles removed a significant quantity of the pesticides from the olives, with a few exceptions. Generally, extending the wash time increased the pesticide reduction with ozonated water, but did not make significant differences with tap water. During olive oil processing, depending on the processing technique and physicochemical properties of the pesticides, eight of nine pesticides were concentrated into olive oil (processing factor > 1) with almost no significant difference between treatments. Imidacloprid did not pass into olive oil. Ozonated water wash for 5 min reduced chlorpyrifos, β-cyfluthrin, α-cypermethrin and imidacloprid contents by 38%, 50%, 55% and 61% respectively in olives.

  7. Residual analysis for spatial point processes

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

    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...

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

    Samson Ayo Deji

    2012-10-01

    Full Text Available The specific objectives are: i to determine the level of awareness of pesticide residue in locally available food among food sellers in Ile Ife area of Osun state, Nigeria; ii to identify the demographic and socio-economic characteristics of food sellers who use pesticides, natural means in preserving their foodstuff from getting spoilt; iii to determine the level of understanding of food sellers who use pesticides about the likely health implications that could result. The design of the study is cross sectional. Structured open-ended questionnaires were administered to 98 randomly selected food sellers in Ile Ife area Osun state, Nigeria. This includes males and female. The inference from the study shows that majority of the food sellers were between ages 21 and 30 years, suggesting that more of the young people are involved in the selling of foodstuff in the area of study. Most of the food sellers used phostozin, an organophosphate compound as preservatives for cereals. The majority of those that were aware of the health hazards associated with the usage of pesticides as preservative were literate school leavers. Among respondents to the questionnaire, it was expected that many of those food sellers likely to demonstrate caution in the usage of pesticide would be the literate school leavers. This is because they are more aware of the possible associated health hazards than their fellow food sellers who are not literate. The level of awareness of health implications associated with use of pesticides on consumable food items is higher among school certificate holders who are food sellers. Phostozin, an organophosphate, is a common preservative pesticide used on cereals foodstuff (e.g., bean, rice, maize in the area of study, especially among the age group between 21 and 30 years.

  9. [Determination of 99 pesticide residues in Paeoniae Radix Alba by gas chromatography-triple quadrupole tandem mass spectrometry].

    Liu, Xiaoqin; Tong, Ling; Meng, Wenting; Sun, Guoxiang

    2015-08-01

    A method was established for the simultaneous determination of 99 pesticide residues with combination of solid-phase extraction technique ( SPE) and gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS). The sample was extracted with ethyl acetate, and cleaned-up by an amino SPE column. The extract was determined by GC-MS/MS in multi-reaction monitoring (MRM) mode, and matrix-matched internal standard method was applied to quantify the pesticides. The results of all the 99 pesticides showed good linearity in the range of 0.001-0.25 mg/L, with correlation coefficients (r2) > 0.99. The limits of quantification (LOQs) were between 0.001-0.050 mg/kg. The recoveries were between 66.7% and 128.0% with RSD values typically lower than 18.3% at three spiked levels of 0.05, 0.10 and 0.20 mg/kg. This method has been applied to determine thirteen batches of commercially available samples, chlorpyriphos-ethyl and p,p'-DDE were detected in four batches of Paeoniae Radix Alba. The method is highly accurate, reliable and sensitive for monitoring the 99 pesticide residues in Paeoniae Radix Alba.

  10. [Contamination of Organophosphorus Pesticides Residue in Fresh Vegetables and Related Health Risk Assessment in Changchun, China].

    Yu, Rui; Liu, Jing-shuang; Wang, Qi-cun; Liu, Qiang; Wang, Yang

    2015-09-01

    This study aims to investigate the concentrations of organophosphorus pesticides (OPs) in fresh vegetables. A total of Z14 samples from seven types of vegetables were collected from the suburb in Changchun City. The OPs were analyzed by gas chromatography coupled with flame photometric detector (GC-FPD). Target hazard quotients (THQ) were applied to estimate the potential health risk to inhabitants. Results showed that OPs concentrations exceeded the Maximum Residue Limit (MRL) in more than 23. 4% samples, and were not detected in only 7. 9% samples. Detection rates of OPs was as follow in the decreased order: diazinon (82. 2%) > phorate (45. 8%) > dimethoate (29. 4%) > parathion-methyl (27. 6%) > omethoate (23. 8%) > dichlorvos (22. 9%) > fenitrothion (21%) > fenthion (18. 7%) > parathion (18. 2%) > methamidophos (17. 3%) > malathion (12. 1%). The percentages above MRL for leaves were higher than for non-leafy vegetables. The order of percentages of OPs above MRL was as follows: green onion (82. 5%) > radish (37. 5%) > red pepper (17. 2%) > Chinese vegetable (14. 3%) > cucumber (3. 2%) > eggplant (2. 9%) > tomato (0%). 49. 5% vegetables samples showed more than one OP. The average target hazard quotients (ave THQ) were all less than one and the average Hazard Index (ave HI) was 0. 462, so that inhabitants who expose average OP levels may not experience adverse health effects.

  11. Residues and Characteristics of Organochlorine Pesticides in the Surface Water in the Suburb of Beijing

    CHEN, Jiawei; LIU, Chen; YANG, Zhongfang; WANG, Jiyuan

    Organochlorine Pesticides (OCPs), such as DDT and HCH, have stable chemical properties and less biodegradability. As a kind of persistent organic pollutants, they have high risk to the environment and human health. Although DDT and HCH have been prohibited in China since 1983, they are still found in some soil and water nowadays. Water resource is very important in natural environment and essential for agriculture. The existence of OCPs in some surface water in Beijing has been detected with different levels according to previous investigations. In recent years, many measures have been taken to control the pollution and to monitor the environment, and more attention has been paid to the status of surface water today. In this study, the water samples were collected from the Wenyu, Beiyun, Yanqing, Fangshan, Changping, and Shunyi Rivers in the suburb of Beijing, and the residues and characteristics of DDT and HCH were studied. The results showed that the contents of DDTs and HCHs were ND-13.98 ng/L and 3.87-146.42 ng/L, respectively. According to the indicators of the ratio values of (DDD+DDE)/DDT and α-HCH/γ-HCH, the source of pollution and its potential risk are also discussed in this article.

  12. Organophosphorus pesticide residues in vegetables from farms, markets, and a supermarket around Kwan Phayao Lake of Northern Thailand.

    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.

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

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

    2015-07-15

    Various drug residues, pesticides and phthalates are ubiquitous in the environment. Their presence in the environment has attracted considerable attention due to their potential impacts on ecosystem functioning and on public health. In this work, 14 drug residues, 24 pesticides and 6 phthalates have been quantified in three matrices (in the dissolved phase, associated to suspended solid matter (SSM), and in sediment) collected from fifteen watercourses and rivers located in a highly industrialized zone at the cross-border area of Northern France and Belgium. The extractions have been carried out using accelerated solvent extraction (ASE) for solid matrices (SSM and sediment) and using solid phase extraction (SPE) for liquid matrix. The final extract was analyzed using GC-MS technique. Among the three classes of compounds, phthalates have been found at highest level compared to pesticides and drug residues. The Σ6PAE concentrations were ranging from 17.2±2.58 to 179.1±26.9μgL(-1) in dissolved phase, from 2.9±0.4 to 21.1±3.2μgL(-1) in SSM and from 1.1±0.2 to 11.9±1.8μgg(-1)dw in sediment. The Σ14drug residue concentrations were lower than 1.3μgL(-1) in the dissolved phases, lower than 30ngL(-1) associated to SSM and from nondetectable levels to 60.7±9.1ngg(-1)dw in sediment. For pesticides, all compounds were below the LOQ values in dissolved phase and in sediment, and only EPTC could be quantified in SSM.

  14. [Analysis of pesticide multiresidues in rice by gas chromatography-mass spectrometry coupled with solid phase extraction].

    Liu, Pengyan; Liu, Qingxue; Ma, Yusong; Liu, Jinwei; Jia, Xuan

    2006-05-01

    A new analytical method was developed to simultaneously determine multiple pesticide residues in rice including organophosphorus, organochlorine, carbamate and pyrethroid. First, the solvents for pesticide extraction were selected for optimization. Eight solvents were screened to find that the extraction efficiency with dichloromethane was the best. Second, clean-up was performed by solid phase extraction using a Florisil cartridge. Various mixtures of hexane and acetone were tested to show that the mixture of hexane-acetone (4:1, v/v) had the best performance. The clean-up helped the sample purification significantly. The prepared sample was analyzed using gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. The pesticides were identified with retention time and selected ions and their relative abundances, and they were quantified based on extract of spiking standards in a blank sample. The limits of detection (LODs) were evaluated on the values of the lower concentration fortified sample under the signal-to-noise ratio of 3:1. The recoveries and relative standard deviations (RSDs) were checked by adding pesticide standard solution at two levels to untreated samples, and the triplicate analysis of the samples were carried out for each spiked level. The LODs were at microg/kg level. The average recoveries of most pesticides were from 75% to 120 %. The RSDs were less than 10.4% (n = 3). These results indicated that this method is simple, rapid, sensitive for the simultaneous determination requirements of multiple pesticide residues in rice.

  15. Multi-residue method for the determination of pesticides and pesticide metabolites in honeybees by liquid and gas chromatography coupled with tandem mass spectrometry--Honeybee poisoning incidents.

    Kiljanek, Tomasz; Niewiadowska, Alicja; Semeniuk, Stanisław; Gaweł, Marta; Borzęcka, Milena; Posyniak, Andrzej

    2016-02-26

    A method for the determination of 200 pesticides and pesticide metabolites in honeybee samples has been developed and validated. Almost 98% of compounds included in this method are approved to use within European Union, as active substances of plant protection products or veterinary medicinal products used by beekeepers to control mites Varroa destructor in hives. Many significant metabolites, like metabolites of imidacloprid, thiacloprid, fipronil, methiocarb and amitraz, are also possible to detect. The sample preparation was based on the buffered QuEChERS method. Samples of bees were extracted with acetonitrile containing 1% acetic acid and then subjected to clean-up by dispersive solid phase extraction (dSPE) using a new Z-Sep+ sorbent and PSA. The majority of pesticides, including neonicotionoids and their metabolites, were analyzed by liquid chromatography tandem mass spectrometry (LC-MS/MS) but some of pesticides, especially pyrethroid insecticides, were analyzed by gas chromatography tandem mass spectrometry (GC-MS/MS). The procedure was validated according to the Guidance document SANCO/12571/2013 at four concentration levels: 1, 5, 10 and 100 ng/g bees and verified in the international proficiency test. The analysis of bee samples spiked at the limit of quantification (LOQ) showed about 98% mean recovery value (trueness) and 97% of analytes showed recovery in the required range of 70-120% and RSDr (precision) below 20%. Linearity and matrix effects were also established. The LOQs of pesticides were in the range of 1-100 ng/g. The developed method allows determination of insecticides at concentrations of 10 ng/g or less, except abamectin and tebufenozide. LOQ values are lower than the median lethal doses LD50 for bees. The method was used to investigate more than 70 honeybee poisoning incidents. Data about detected pesticides and their metabolites are included.

  16. Guidelines for application of the good laboratory practices and quality assurance and control in pesticide residues analysis; Linee guida per l`applicazione delle buone pratiche di laboratorio e l`assicurazione e il controllo della qualita` nell`analisi di residui di prodotti fitosanitari

    Attard Barbini, Danilo [Istituo Superiore di Sanita`, Rome (Italy); Biancardi, Gino [Agenzia Regionale per la Protezione dell`Ambiente, Massa Carrara (Italy); Bove, Bruno [Presiduo Multizonale di Prevenzione, Potenza (Italy)] [and others

    1997-09-01

    The guidelines, particularly aimed at laboratories which carry out studies in the field of pesticide residues in food and environment, are intended to give practical, organizational and operational hints along the lines set up by the Italian Legislative Decree n. 120 of January 27, 1992 and the European standard UNI CEI EN 45001, to which the laboratories dealing with official control and monitoring should conform. The main items discussed include: organization of the laboratory, personnel and equipment, working procedures related to analytical methodology, confirmation criteria for violation of maximum residue limits and quality control.

  17. Multiresidue analysis of pesticides in vegetables and fruits using two-layered column with graphitized carbon and water absorbent polymer.

    Obana, H; Akutsu, K; Okihashi, M; Hori, S

    2001-09-01

    A high-throughput multiresidue analysis of pesticides in non-fatty vegetables and fruits was developed. The method consisted of a single extraction and a single clean-up procedure. Food samples were extracted with ethyl acetate and the mixture of extract and food dregs were poured directly into the clean-up column. The clean-up column consisted of two layers of water-absorbent polymer (upper) and graphitized carbon (lower), which were packed in a reservoir (75 ml ) of a cartridge column. The polymer removed water in the extract while the carbon performed clean-up. In a recovery test, 110 pesticides were spiked and average recoveries were more than 95% from spinach and orange. Most pesticides were recovered in the range 70-115% with RSD usually < 10% for five experiments. The residue analyses were performed by the extraction of 12 pesticides from 13 samples. The two methods resulted in similar residue levels except chlorothalonil in celery, for which the result was lower with the proposed method. The results confirmed that the proposed method could be applied to monitoring of pesticide residue in foods.

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

    陈述

    2014-01-01

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

  19. 76 FR 3885 - Notice of Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on...

    2011-01-21

    ... this unit could also be affected. The North American Industrial Classification System (NAICS) codes... the requirement of a tolerance for residues of Bacillus thuringiensis eCry3.1Ab protein under 40 CFR... exemption from the requirement of a tolerance for residues of the plant-incorporated protectant...

  20. Determination of Pesticide Residues in Banana by Using High Performance Liquid Chromatography and Gas Chromatography-Mass Spectrometry

    R. Paranthaman

    2012-01-01

    Full Text Available Problem statement: The occurrence of endosulfan, carbendazim, chloropyripos in 10 banana samples in southern area of Tamilnadu, India (hill banana, karpuravalli, monthan, nendran, ney poovan, pachanadan, poovan, rasthali, red banana, robusta was investigated. Approach: In 7 samples, Carbendazim was found at concentrations ranging from 0.002-0.11 mg kg-1. In three samples, carbendazim was not found, whereas endosulfan, chloropyripos was not detected in any sample. Results: Analysis was carried out using HPLC-UV and samples were confirmed by GC-MS. The seven samples contained carbendazim that not exceeded the FAO/WHO codex alimentarius standards for MRLs (Maximum Residue Limit values of carbendazim pesticide on banana (whole is 1.0 mg kg-1. Conclusion/Recommendations: Based on the HPLC results carbendazim is finding in Hill banana (0.007 mg kg-1, Monthan (0.019 mg kg-1, Nendran (0.002 mg kg-1, Pachanadan (0.007 mg kg-1, Poovan (0.016 mg kg-1, Rasthali (0.017 mg kg-1 and Robusta (0.11 mg kg-1 and carbendazim is not finding Karpuravalli, Ney poovan and Red banana. Endosulfan, Chloropyrifos and Carbendazim in Robusta Banana sample are identified by matching their retention times and characteristic ion. TIC chromatogram for a positive Robusta Banana sample.

  1. 分散液液微萃取技术及其在食品和环境农药残留检测中的应用%Application of Dispersive Liquid-liquid Microextraction for Analysis of Pesticide Residues in Food and Environment

    张雪莲; 焦必宁

    2012-01-01

    Dispersive liquid-liquid microextraction(DLLME) is a novel sample preparation technique.It integrates extraction and condensation,and has the advantages of simple operation,short time consumption,low cost,high recovery rate,high enrichment factor and low environmental pollution.In this paper,the principle,procedures and influencing factors of DLLME are introduced.The recent applications of this novel technique in the analysis of pesticide residues in food and environment are also emphatically discussed.Moreover,its application prospect is proposed.%分散液液微萃取是一种新型的样品前处理技术,该技术集萃取和浓缩于一体,具有操作简单、快速、成本低、富集效率高且对环境友好等优点。本文就分散液液微萃取原理、操作过程、影响因素进行介绍,重点综述该项新技术在食品和环境农药残留检测中的应用,并对其应用前景进行展望。

  2. 75 FR 14154 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-03-24

    ... establish tolerances in 40 CFR part 180 for residues of the insecticide thiamethoxam, 3- tetrahydro-5-methyl...., has submitted practical analytical methodology for detecting and measuring levels of thiamethoxam...

  3. 76 FR 53372 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2011-08-26

    ... for residues of the insecticide thiamethoxam [3-[(2-chloro-5- thiazolyl)methyl]tetrahydro-5-methyl-N... of thiamethoxam in or on raw agricultural commodities. This method is based on crop specific...

  4. 76 FR 36479 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    2011-06-22

    ... 40 CFR part 180 for residues of the insecticide thiamethoxam, (3-[(2-chloro-5- thiazolyl) methyl... for detecting and measuring levels of thiamethoxam in or on raw agricultural commodities. This...

  5. 75 FR 48667 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-08-11

    ... for residues of the insecticide thiamethoxam, (3- tetrahydro-5-methyl-N- nitro-4H-1,3,5-oxadiazin-4... practical analytical methodology for detecting and measuring levels of thiamethoxam in or on...

  6. Food safety in Thailand 4: comparison of pesticide residues found in three commonly consumed vegetables purchased from local markets and supermarkets in Thailand

    Sompon Wanwimolruk

    2016-09-01

    Full Text Available Background The wide use of pesticides raises concerns on the health risks associated with pesticide exposure. For developing countries, like Thailand, pesticide monitoring program (in vegetables and fruits and also the maximum residue limits (MRL regulation have not been entirely implemented. The MRL is a product limit, not a safety limit. The MRL is the maximum concentration of a pesticide residue (expressed as mg/kg recommended by the Codex Alimentarius Commission to be legally permitted in or on food commodities and animal feeds (Codex Alimentarius Commission, 2015; European Commission, 2015. MRLs are based on supervised residue trial data where the pesticide has been applied in accordance with GAP (Good Agricultural Practice. This study aims at providing comparison data on pesticide residues found in three commonly consumed vegetables (Chinese kale, pakchoi and morning glory purchased from some local markets and supermarkets in Thailand. Methods These vegetables were randomly bought from local markets and supermarkets. Then they were analyzed for the content of 28 pesticides by using GC-MS/MS. Results Types of pesticides detected in the samples either from local markets or supermarkets were similar. The incidence of detected pesticides was 100% (local markets and 99% (supermarkets for the Chinese kale; 98% (local markets and 100% (supermarkets for the pakchoi; and 99% (local markets and 97% (supermarkets for the morning glory samples. The pesticides were detected exceeding their MRL at a rate of 48% (local markets and 35% (supermarkets for the Chinese kale; 71% (local markets and 55% (supermarkets for the pakchoi, and 42% (local markets and 49% (supermarkets for the morning glory. Discussion These rates are much higher than those seen in developed countries. It should be noted that these findings were assessed on basis of using criteria (such as MRL obtained from developed countries. Our findings were also confined to these vegetables sold

  7. Food safety in Thailand 4: comparison of pesticide residues found in three commonly consumed vegetables purchased from local markets and supermarkets in Thailand

    Phopin, Kamonrat; Boonpangrak, Somchai; Prachayasittikul, Virapong

    2016-01-01

    Background The wide use of pesticides raises concerns on the health risks associated with pesticide exposure. For developing countries, like Thailand, pesticide monitoring program (in vegetables and fruits) and also the maximum residue limits (MRL) regulation have not been entirely implemented. The MRL is a product limit, not a safety limit. The MRL is the maximum concentration of a pesticide residue (expressed as mg/kg) recommended by the Codex Alimentarius Commission to be legally permitted in or on food commodities and animal feeds (Codex Alimentarius Commission, 2015; European Commission, 2015). MRLs are based on supervised residue trial data where the pesticide has been applied in accordance with GAP (Good Agricultural Practice). This study aims at providing comparison data on pesticide residues found in three commonly consumed vegetables (Chinese kale, pakchoi and morning glory) purchased from some local markets and supermarkets in Thailand. Methods These vegetables were randomly bought from local markets and supermarkets. Then they were analyzed for the content of 28 pesticides by using GC-MS/MS. Results Types of pesticides detected in the samples either from local markets or supermarkets were similar. The incidence of detected pesticides was 100% (local markets) and 99% (supermarkets) for the Chinese kale; 98% (local markets) and 100% (supermarkets) for the pakchoi; and 99% (local markets) and 97% (supermarkets) for the morning glory samples. The pesticides were detected exceeding their MRL at a rate of 48% (local markets) and 35% (supermarkets) for the Chinese kale; 71% (local markets) and 55% (supermarkets) for the pakchoi, and 42% (local markets) and 49% (supermarkets) for the morning glory. Discussion These rates are much higher than those seen in developed countries. It should be noted that these findings were assessed on basis of using criteria (such as MRL) obtained from developed countries. Our findings were also confined to these vegetables sold in

  8. Tank 12H residuals sample analysis report

    Oji, L. N. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Shine, E. P. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Diprete, D. P. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Coleman, C. J. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Hay, M. S. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2015-06-11

    The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) to provide sample preparation and analysis of the Tank 12H final characterization samples to determine the residual tank inventory prior to grouting. Eleven Tank 12H floor and mound residual material samples and three cooling coil scrape samples were collected and delivered to SRNL between May and August of 2014.

  9. Levels of organochlorine pesticide residues in butter samples collected from the Black Sea Region of Turkey.

    Aksoy, Abdurrahman; Dervisoglu, Muhammed; Guvenc, Dilek; Gul, Osman; Yazici, Fehmi; Atmaca, Enes

    2013-01-01

    The aim of the present study was to evaluate the levels of 9 organochlorine compounds (aldrin, hexachlorobenzene, 2,4-DDE, 4,4-DDE, 2,4-DDT, 4,4-DDT, and α-, β-, and γ-HCH) in butter samples collected in the Eastern, Middle and Western Black Sea Regions of Turkey between October 2009 and June 2010. The liquid-liquid extraction method was used to extract the organochlorine compounds from the samples and the measurements were performed by using a gas chromatograph-electron capture detector system. DDT metabolites, aldrin, hexachlorobenzene (HCB), and α-, and γ-HCH were not detected in the samples but β-HCH was detected in 3 of a total of 88 samples. In the first period, only one sample from the West Black Sea Region was β-HCH positive (0.014 mg kg(-1)). The other β-HCH positive samples collected in Middle and West Black Sea Regions in the second period had a concentration of 0.066 and 0.019 mg kg(-1), respectively. All concentrations of the detected compounds exceeded the legal limits of 0.003 mg kg(-1) for β-HCH, as prescribed by the Turkish Food Codex, and therefore pose a potential health risk for consumers. The contamination detected is most likely due to the past usage of β-HCH in agriculture and its long term persistence in the environment. These results strongly suggest that further research should be focused on the detection of pesticide residues in agricultural areas across the nation.

  10. Honey bees (Apis mellifera) reared in brood combs containing high levels of pesticide residues exhibit increased susceptibility to Nosema (Microsporidia) infection.

    Wu, Judy Y; Smart, Matthew D; Anelli, Carol M; Sheppard, Walter S

    2012-03-01

    Nosema ceranae and pesticide exposure can contribute to honey bee health decline. Bees reared from brood comb containing high or low levels of pesticide residues were placed in two common colony environments. One colony was inoculated weekly with N. ceranae spores in sugar syrup and the other colony received sugar syrup only. Worker honey bees were sampled weekly from the treatment and control colonies and analyzed for Nosema spore levels. Regardless of the colony environment (spores+syrup added or syrup only added), a higher proportion of bees reared from the high pesticide residue brood comb became infected with N. ceranae, and at a younger age, compared to those reared in low residue brood combs. These data suggest that developmental exposure to pesticides in brood comb increases the susceptibility of bees to N. ceranae infection.

  11. Pesticide residue concentration in soil following conventional and Low-Input Crop Management in a Mediterranean agro-ecosystem, in Central Greece

    Karasali, Helen, E-mail: e.karassali@bpi.gr [Laboratory of Chemical Control of Pesticides, Department of Pesticides Control and Phytopharmacy, Benaki Phytopathological Institute, 8 St. Delta Street, Kifissia, 14561 Athens (Greece); Marousopoulou, Anna [Laboratory of Chemical Control of Pesticides, Department of Pesticides Control and Phytopharmacy, Benaki Phytopathological Institute, 8 St. Delta Street, Kifissia, 14561 Athens (Greece); Machera, Kyriaki, E-mail: k.machera@bpi.gr [Laboratory of Pesticides Toxicology, Department of Pesticides Control and Phytopharmacy, Benaki Phytopathological Institute, 8 St. Delta Street, Kifissia, 14561 Athens (Greece)

    2016-01-15

    The present study was focused on the comparative evaluation of pesticide residues, determined in soil samples from Kopaida region, Greece before and after the implementation of Low-Input Crop Management (LCM) protocols. LCM has been suggested as an environmental friendly plant protection approach to be applied on crops growing in vulnerable to pollution ecosystems, with special focus on the site specific problems. In the case of the specific pilot area, the vulnerability was mainly related to the pollution of water bodies from agrochemicals attributed to diffuse pollution primarily from herbicides and secondarily from insecticides. A total of sixty-six soil samples, were collected and analyzed during a three-year monitoring study and the results of the determined pesticide residues were considered for the impact evaluation of applied plant protection methodology. The LCM was developed and applied in the main crops growing in the pilot area i.e. cotton, maize and industrial tomato. Herbicides active ingredients such as ethalfluralin, trifluralin, pendimethalin, S-metolachlor and fluometuron were detected in most samples at various concentrations. Ethalfluralin, which was the active ingredient present in the majority of the samples ranged from 0.01 μg g{sup −1} to 0.26 μg g{sup −1} soil dry weight. However, the amount of herbicides measured after the implementation of LCM for two cropping periods, was reduced by more than 75% in all cases. The method of analysis was based on the simultaneous extraction of the target compounds by mechanical shaking, followed by liquid chromatography mass spectrometric and gas chromatography electron capture (LC–MS/MS and GC–ECD) analysis. - Highlights: • Effect of Low Input Crop Management (LCM) in a vulnerable to pollution ecosystem. • LCM resulted in herbicide residues reduction in the range of 75 and 100% in all cases. • Conventional practices resulted in increased herbicide residues up to 18%. • Anthropogenic

  12. Effects of Two Composted Plant Pesticide Residues,Incorporated with Trichoderma viride,on Root-Knot Nematode in Balloonflower

    ZHANG Shuang-xi; ZHANG Xing

    2009-01-01

    Plant pesticide residues,such as chinaberry(Melia toosendan)residue and sand cypress(Sabina vulgaris)residue,are pesticidal plant materials discarded after the bioactive ingredient has been extracted with organic solvents.The only option for botanical pesticide residue utilization has been as landfill.Chinaberry residue(CBR)and sand cypress residue(SCR)were collected and composted in Yangling,Shaanxi Province,China.We studied the effects of chinaberry residue compost(CBRC),CBRC incorporated with Trichoderma viride(CBRCT),sand cypress residue compost(SCRC),and SCRC incorporated with T.viride(SCRCT)on the root-knot nematode,Meloidogyne incognita,infesting the balloonflower(Platycodon grandiflorum).Bioassay results indicated that stock solutions of the CBRCT and SCRCT extracts significantly inhibited egg hatching and caused high larval mortality,followed in degree by the CBRC and SCRC extracts.The CBR and SCR extracts caused very low inhibition of eggs and larvae.Supplementing potting mixtures with these four composts reduced the severity of root galling and increased the proportion of marketable roots.The severity of root galling decreased and the average weight of the marketable roots increased with an increase in all the composts when supplemented at rates from 5 to 30%.CBR- and SCR-supplemented pot soils also inhibited the nematodes,but CBR and SCR applied to the soil had a phytotoxic effect and inhibited balloonflower growth.Supplementing field soil with the composts reduced the severity of root galling and the populations of southern root-knot nematodes in the soil.CBRCT and SCRCT clearly enhanced the average weight of the marketable roots by 30.45 and 26.64%,respectively.Continuous supplementation with CBRCT or SCRCT in the same field significantly enhanced the control of the root-knot nematode,and the populations of nematodes continued to decrease with second inoculations.The populations of total Trichoderma spp.were distinctly enhanced and were maintained at

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

    赵小中; 魏小春; 朱香玲; 董森森

    2013-01-01

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

  14. Residual analysis for spatial point processes

    Waagepetersen, Rasmus Plenge

    2005-01-01

    Discussion of the paper "Residual analysis for spatial point processes" by A. Baddeley, M. Hazelton, J. Møller and R. Turner. Journal of the Royal Statistical Society, Series B, vol. 67, pages 617-666, 2005.......Discussion of the paper "Residual analysis for spatial point processes" by A. Baddeley, M. Hazelton, J. Møller and R. Turner. Journal of the Royal Statistical Society, Series B, vol. 67, pages 617-666, 2005....

  15. Comparison of accelerator mass spectrometry with gas chromatography for the determination of pesticide residues in individual items in the diets of wild birds and mammals.

    Brown, Peter; Garner, Colin; Glass, Richard; Ridgway, Chris; Hart, Andy

    2004-06-16

    Methods to refine the assessment of exposure of wild birds and mammals to pesticides required measurement of pesticide residues in very small samples of their diets. Sample sizes were in the 1-100 mg range, and the target residue for measurement was 0.01 mg/kg. Gas chromatography-mass spectrometry (GC-MS) with large volume injection was compared with the use of an accelerator mass spectrometer (AMS) to measure residues of pesticide labeled at near-background levels with carbon-14. The GC-MS method was able to detect residues down to 0.1 ng per item of diet, and the AMS detected the radiolabel down to 1 mBq (0.06 disintegration per minute, 1 ng of pesticide at the specific activity used) per sample. The target residue level was achieved by the GC-MS method for samples down to 10 mg. The GC method appeared to be best suited to monitoring residues in field studies, and the AMS shows great potential for use in laboratory experiments concerning pesticide degradation.

  16. QuEChERS sample preparation for the determination of pesticides and other organic residues in environmental matrices: a critical review.

    Bruzzoniti, Maria Concetta; Checchini, Leonardo; De Carlo, Rosa Maria; Orlandini, Serena; Rivoira, Luca; Del Bubba, Massimo

    2014-07-01

    Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) is an extraction and clean-up technique originally developed for recovering pesticide residues from fruits and vegetables. Since its introduction, and until December 2013, about 700 papers have been published using the QuEChERS technique, according to a literature overview carried out using SciFinder, Elsevier SciVerse, and Google search engines. Most of these papers were dedicated to pesticide multiresidue analysis in food matrices, and this topic has been thoroughly reviewed over recent years. The QuEChERS approach is now rapidly developing beyond its original field of application to analytes other than pesticides, and matrices other than food, such as biological fluids and non-edible plants, including Chinese medicinal plants. Recently, the QuEChERS concept has spread to environmental applications by analyzing not only pesticides but also other compounds of environmental concern in soil, sediments, and water. To the best of our knowledge, QuEChERS environmental applications have not been reviewed so far; therefore, in this contribution, after a general discussion on the evolution and changes of the original QuEChERS method, a critical survey of the literature regarding environmental applications of conventional and modified QuEChERS methodology is provided. The overall recoveries obtained with QuEChERS and other extraction approaches (e.g., accelerated solvent extraction, ultrasonic solvent extraction, liquid/solid extraction, and soxhlet extraction) were compared, providing evidence for QuEChERS higher recoveries for various classes of compounds, such as biopesticides, chloroalkanes, phenols, and perfluoroalkyl substances. The role of physicochemical properties of soil (i.e., clay and organic carbon content, as well as cation exchange capacity) and target analytes (i.e., log KOW, water solubility, and vapor pressure) were also evaluated in order to interpret recovery and matrix effect data.

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

    Nurul Karim

    2012-09-01

    Full Text Available Several types of organophosphorous and carbamate pesticides have been used extensively by the farmers in Bangladesh during the last few decades. Twenty seven water samples collected from both paddy and vegetable fields in the Savar and Dhamrai Upazilas in Bangladesh were analyzed to determine the occurrence and distribution of organo-phosphorus (chlorpyrifos, malathion and diazinon and carbamate (carbaryl and carbofuran pesticide residues. A high performance liquid chromatograph instrument equipped with a photodiode array detector was used to determine the concentrations of these pesticide residues. Diazinon and carbofuran were detected in water samples collected from Savar Upazila at 0.9 μg/L and 198.7 μg/L, respectively. Malathion was also detected in a single water sample at 105.2 μg/L from Dhamrai Upazila. Carbaryl was the most common pesticide detected in Dhamrai Upazila at 14.1 and 18.1 μg/L, while another water sample from Dhamrai Upazila was contaminated with carbofuran at 105.2 μg/L. Chlorpyrifos was not detected in any sample. Overall, the pesticide residues detected were well above the maximum acceptable levels of total and individual pesticide contamination, at 0.5 and 0.1 μg/L, respectively, in water samples recommended by the European Economic Community (Directive 98/83/EC. The presence of these pesticide residues may be attributed by their intense use by the farmers living in these areas. Proper handling of these pesticides should be ensured to avoid direct or indirect exposure to these pesticides.

  18. 75 FR 9596 - Notice of Filing of a Pesticide Petition for Residues of a Aspergillus flavus AF36 on Corn Food...

    2010-03-03

    ... From the Federal Register Online via the Government Publishing Office ENVIRONMENTAL PROTECTION AGENCY Notice of Filing of a Pesticide Petition for Residues of a Aspergillus flavus AF36 on Corn Food... residues of the antifungal ] agent, Aspergillus flavus AF36, in or on corn food and feed commodities....

  19. 76 FR 6465 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2011-02-04

    ... 180 for residues of the herbicide glyphosate, N-(phosphonomethyl) glycine, in or on corn, field, forage at 13 ppm to support the use of glyphosate in RHS seed corn production. Adequate enforcement... limited to: Crop production (NAICS code 111). Animal production (NAICS code 112). Food...

  20. 77 FR 59578 - Notice of Filing of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2012-09-28

    ... from the requirement of a tolerance for residues of cationic hydroxypropyl guar (CAS No. 71329-50-5... relies upon available data for cationic hydroxypropyl guar and the structurally similar substance, guar gum. The cationic hydroxypropyl guar data presented in this tolerance exemption petition are on...

  1. 78 FR 63938 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2013-10-25

    ... be exhaustive, but rather provides a guide to help readers determine whether this document applies to...., Princeton, NJ 08540, requests to establish tolerances in 40 CFR part 180 for residues of the fungicide..., field, hay at 15 ppm; pea, field, vines at 4.0 ppm; chickpea, seed at 0.06 ppm; and lentil, seed at...

  2. 75 FR 78240 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-12-15

    ...- triazole-1-ethanol], including its metabolites and degradates, in or on sweet corn, field corn and cotton.... Residues of flutriafol in sweet corn, field corn and cotton raw agricultural commodity products can be...-triazole-1-ethanol], including its metabolites and degradates, in or on corn, field, forage at 4.0...

  3. 78 FR 79359 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2013-12-30

    ... enforcement of tolerances in plant commodities. (RD) 2. PP 3E8202. (EPA-HQ-OPP-2013-0712). Interregional... enforcement purposes for spinetoram in plant and animal matrices. For more details on the analytical methods... tolerances in 40 CFR part 180 for residues of the insecticide spinosad, a fermentation product...

  4. 75 FR 5790 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2010-02-04

    ..., but are not limited to: Crop production (NAICS code 111). Animal production (NAICS code 112). Food... CFR part 180 for residues of the herbicide S-ethyl dipropylthiocarbamate (EPTC), in or on grasses...-36-0); Poly(oxy-1,2-ethanediyl), -hydro- -hydroxy-, mono-C 12 - 15 -alkyl ethers, phosphates...

  5. 78 FR 43115 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2013-07-19

    ... include: Crop production (NAICS code 111). Animal production (NAICS code 112). Food manufacturing (NAICS... to establish an exemption from the requirement of a tolerance for residues of the insecticide ethyl... octadec 9 enol or polyethyleneglycol ethers of octanol, decanol, dodecanol, tetradecanol,...

  6. Hair decontamination procedure prior to multi-class pesticide analysis.

    Duca, Radu-Corneliu; Hardy, Emilie; Salquèbre, Guillaume; Appenzeller, Brice M R

    2014-06-01

    Although increasing interest is being observed in hair analysis for the biomonitoring of human exposure to pesticides, some limitations still have to be addressed for optimum use of this matrix in that specific context. One main possible issue concerns the need to differentiate chemicals biologically incorporated into hair from those externally deposited on hair surface from contaminated air or dust. The present study focuses on the development of a washing procedure for the decontamination of hair before analysis of pesticides from different chemical classes. For this purpose, three different procedures of artificial contamination (with silica, cellulose, and aqueous solution) were used to simulate pesticides deposition on hair surface. Several washing solvents (four organic: acetone, dichloromethane, methanol, acetonitrile; and four aqueous: water, phosphate buffer, shampoo, sodium dodecylsulfate) were evaluated for their capacity to remove artificially deposited pesticides from hair surface. The most effective washing solvents were sodium dodecylsulfate and methanol for aqueous and organic solvents, respectively. Moreover, after a first washing with sodium dodecylsulfate or methanol, the majority of externally deposited pesticides was removed and a steady-state was reached since significantly lower amounts were removed by additional second and third washings. Finally, the effectiveness of a decontamination procedure comprising washing with sodium dodecylsulfate and methanol was successively demonstrated. In parallel, it was determined that the final procedure did not affect the chemicals biologically incorporated, as hair strands naturally containing pesticides were used. Such a procedure appears to remove in one-shot the fraction of chemicals located on hair surface and does not require repeated washing steps.

  7. Organochlorine pesticide residues in human breast milk and placenta in Tohoku, Japan

    Nakai, K.; Suzuki, K.; Oka, T.; Sugawara, N.; Ohba, T.; Kameo, S.; Satoh, H. [Environmental Heath Sciences, Tohoku Univ. Graduate School of Medicine, Sendai (Japan); Nakamura, T.; Saitoh, Y. [Miyagi Prefectural Inst. of Piblic Health and Environment (Japan); Okamura, K. [Dept. of Obstetrics, Tohoku Univ. Graduate School of Medicine, Sendai (Japan)

    2004-09-15

    Recently, we have started a birth cohort study to examine the effects of exposure to persistent organochemical pollutants and heavy metals on neurodevelopment in Japanese children, The Tohoku Study of Child Development. In this cohort study, biological samples, including maternal peripheral blood, cord blood, placenta, cord tissue, and breast milk have been collected from more than six hundred mother-infant pairs for chemical determinations. The growth of infants has been monitored using neurodevelopmental tests, including the Brazelton Neonatal Behavioral Assessment Scale, the Bayley Scale of Infant Development, the Kyoto Scale of Psychological Development, and others. Exposures to dioxin and related compounds, polychlorinated biphenyls, methylmercury, and several heavy metals were assessed. Additionally, since perinatal exposure to organochlorine pesticides may affect the neurodevelopment of children, we examined the effects of those pesticides in the cohort study. In the present study, several organochlorine pesticides were analyzed in human breast milk and placenta from 20 mothers to identify the major pesticide compounds found in the cohort subjects. The relationship between pesticides in breast milk and the placenta was analyzed to examine the utilization of the placenta as the material for exposure assessment. Some information regarding the factors affecting the contamination of breast milk and the placenta with organochlorine pesticides are also discussed.

  8. Pesticide residues in heterogeneous plant populations, a model-based approach applied to nematicides in banana (Musa spp.).

    Tixier, Philippe; Chabrier, Christian; Malézieux, Eric

    2007-03-21

    Nematicides are widely used to control plant-parasitic nematodes in intensive export banana (Musa spp.) cropping systems. Data show that the concentration of fosthiazate in banana fruits varies from zero to 0.035 g kg-1, under the maximal residue limit (MRL=0.05 mg kg-1). The fosthiazate concentration in fruit is described by a Gaussian envelope curve function of the interval between pesticide application and fruit harvest (preharvest interval). The heterogeneity of phenological stages in a banana population increases over time, and thus the preharvest interval of fruits harvested after a pesticide application varies over time. A phenological model was used to simulate the long-term harvest dynamics of banana at field scale. Simulations show that the mean fosthiazate concentration in fruits varies according to nematicide application program, climate (temperature), and planting date of the banana field. This method is used to assess the percentage of harvested bunches that exceed a residue threshold and to help farmers minimize fosthiazate residues in bananas.

  9. A novel paper rag as 'D-SERS' substrate for detection of pesticide residues at various peels.

    Zhu, Yiqun; Li, Minqiang; Yu, Daoyang; Yang, Liangbao

    2014-10-01

    Many important considerations in the design of practical Surface enhanced Raman spectroscopy (SERS) substrates are necessary, such as the low cost, simple preparation, mass production and high efficiency of sample collection, which the conventional rigid substrates are lack of. In this work, practical SERS substrates based on deposition of silver nanoparticles (Ag NPs) on commercially available low-cost filter paper were prepared by simple silver mirror reaction in a large scale, and utilized for rapid, portable and accurate identification and detection of pesticide residues at various peels. Compared with conventional substrates, this novel SERS substrate dramatically enhanced the sample collection efficiency by simply swabbing paper-based device across different surfaces without destroying the sample, meanwhile avoiding the substrate signal of real-world samples. Considering their low cost, portability, simplicity and high sample collection efficiency, Ag NP-decorated filter paper, as practical SERS substrate, are used in solving critical problems for detection of pesticide residues at various peels. SERS experiments were carried out on Ag NP-decorated filter paper combined with 'dynamic SERS' (D-SERS) due to its high detection sensitivity. The excellent detection performance of the Ag NP-based filter paper was demonstrated by detection thiram and paraoxon residues at various peels. Besides, the stability and reproducibility of the practical substrates were also involved.

  10. Pesticide residues in Nile tilapia (Oreochromis niloticus) and Nile perch (Lates niloticus) from Southern Lake Victoria, Tanzania

    Henry, L. [Chemistry Department, University of Dar es Salaam. PO Box 35061, Dar es Salaam (Tanzania); Kishimba, M.A. [Chemistry Department, University of Dar es Salaam. PO Box 35061, Dar es Salaam (Tanzania)]. E-mail: kishimba@chem.udsm.ac.tz

    2006-03-15

    Nile tilapia (Oreochromis niloticus) and Nile perch (Lates niloticus) samples were collected from fish landing stations in nine riparian districts on the Tanzanian side of Lake Victoria and screened for residues of 64 organochlorine, organophosphorus, carbamate, and pyrethroid pesticides. The residue levels in the fish fillet were up to 0.003, 0.03 and 0.2 mg/kg fresh weight (0.7, 3.8 and 42 mg/kg lipid weight) of fenitrothion, DDT and endosulfan, respectively. Mean levels within sites were up to 0.002, 0.02 and 0.1 mg/kg fresh weight (0.5, 0.5 and 16 mg/kg lipid weight), respectively. The detection of higher levels of p,p'-DDT than the degradation products (p,p'-DDD and p,p'-DDE), and higher levels of endosulfan isomers ({alpha} and {beta}) than the sulphate, in fish samples, implied recent exposure of fish to DDT and endosulfan, respectively. Generally, most of the fish samples had residue levels above the average method detection limits (MDLs), but were within the calculated ADI. - Fish from Lake Victoria had relatively low pesticide levels.

  11. 我国主产地柑橘的农药残留现状研究%Current Situation of Pesticide Residues in Citrus from China

    张耀海; 焦必宁; 赵其阳; 王成秋; 周志钦

    2011-01-01

    我国柑橘生产使用农药种类多、剂量大,对产品质量安全有一定影响.文中采用气相色谱和高效液相色谱检测技术,对我国6省(市)柑橘产地抽取的198个鲜果样品进行了26种农药残留的检测与评价.10种农药残留检出,包括禁限用农药,其中1个样品有1种农残超标,超标率为0.47%,各省(市)柑橘鲜果样品的农药残留检出率均在48.9%以上,我国柑橘质量安全存在潜在风险.%The wide varieties and massive doses of pesticide residues applied in citrus production has influence on citrus safety quality in China.The current situation of citrus safety was investigated to provide basic reference in the evaluation of potential risks.All samples from six provinces or cities were determined by gas chromatography (GC) and high performance liquid chromatography (HPLC) to monitor twenty-six pesticides.Ten of twenty six pesticides residues were detected and one exceeded the MRLs.Of all the samples, 0.47% exceeded the MRLs.The detectable rates of samples from six main producing areas were above 48.9%.There is a potential risk in Citrus products in China.In order to ensure the citrus safety in China, we need to strengthen pesticide residue examination, enhance disease-carrying insect monitor and preventing technical guidance, promote non-environmental damage and green citrus production technology.We also need to improve our detecting technology and catch up with international advanced analysis method.

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

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

    2015-01-01

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

  13. 76 FR 43231 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2011-07-20

    ...; onion, green, subgroup 3-07B at 7.5 ppm; caneberry subgroup 13-07A at 5.0 ppm; bushberry subgroup 13-07B... of food with residues at or above the levels set in these tolerances. The Analytical Chemistry...; onion, green subgroup 3-07B at 7.0 ppm; caneberry subgroup 13-07A at 5.0 ppm; bushberry subgroup...

  14. Integrated Pest Management Practices Reduce Insecticide Applications, Preserve Beneficial Insects, and Decrease Pesticide Residues in Flue-Cured Tobacco Production.

    Slone, Jeremy D; Burrack, Hannah J

    2016-09-22

    Integrated pest management (IPM) recommendations, including scouting and economic thresholds (ETs), are available for North Carolina flue-cured tobacco growers, although ETs for key pests have not been updated in several decades. Moreover, reported IPM adoption rates by flue-cured tobacco growers remain low, at pests reached ET (IPM), while the other field was managed per grower discretion (Grower Standard). IPM fields received an average of two fewer insecticide applications without compromising yield. More insecticide applications resulted in higher pesticide residues in cured leaf samples from Grower Standard fields than those from IPM fields. Reductions in insecticides and management intensity also resulted in larger beneficial insect populations in IPM fields.

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

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

    1988-01-01

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

  16. Multiresidue analytical procedures for pesticides residues in vegetable products; Metodi mutiresiduo per l`analisi di residui di antiparassitari in prodotti vegetali

    Gruppo di lavoro per i residui di antiparassitari della Commissione permanente di coordinamento interregionale per i problemi relativi al controllo ufficiale dei prodotti alimentari

    1997-09-01

    Multiresidue methods for pesticide residues in vegetable products, most frequently used by laboratories of the Italian national health service, by the regional and provincial agencies for environmental protection and by the National health institute. The analytical behaviour is presented for 249 pesticides through the different steps of extraction and cleanup, along with data for the gas chromatography (GC), gas chromatography coupled to mass spectrometry (GC/MS) and high performance liquid chromatography coupled to spectrophotometric detector (HPL/UV).

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

    European Food Safety Authority

    2013-07-01

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

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

    European Food Safety Authority

    2014-07-01

    Full Text Available In accordance with Article 43 of Regulation (EC No 396/2005, EFSA received a request from the European Commission to provide support for the preparation of the EU position for 46th session of the Codex Committee on Pesticide Residues (CCPR. In 2013, JMPR evaluated 10 active substances regarding the setting of toxicological reference values to be used in consumer risk assessment (diquat, chlorfenapyr, picoxystrobin, benzovindiflupyr, bixafen, fenamidone, fluesulfone, isoxaflutole, tolfenpyrad, and trinexapac and 31 active substances regarding the setting of Maximum Residue Limits (MRLs (diquat, malathion, chlorpyrifos methyl, triazophos, glyphosate, propiconazole, bentazone, dithianon, fenpyroximate, fenbuconazole, flutriafol, cyprodinil, fludioxonil, indoxocarb, difenoconazole, pyrimethanil, azoxystrobin, chlorantraniliprole, mandipropamid, spirotetramate, cyproconazole, dicamba, sulfoxaflor, penthiopyrad, cyantraniliprole, imazapic, imazapyr, isoxaflutole, tolfenpyrad and trinexapac.

  19. Monitoring of organochlorine pesticide residue levels in adipose tissue of Veracruz, Mexico inhabitants.

    Waliszewski, Stefan M; Caba, M; Herrero-Mercado, M; Saldariaga-Noreña, H; Meza, E; Zepeda, R; Martínez-Valenzuela, C; Infanzon, R; Hernández-Chalate, F

    2011-11-01

    The objective of the present study was to monitor the levels of organochlorine pesticides HCB, α-β-γ-HCH, pp'DDE, op'DDT and pp'DDT in 150 adipose tissue samples of Veracruz, Mexico inhabitants. In analyzed samples, the following pesticides were detected: p,p'-DDE in 100% of the samples at mean 1.643 mg/kg; p,p'-DDT in 99.3.% of the samples at mean 0.227 mg/kg; β-HCH in 97.3% of the samples at mean 0.063 mg/kg; and op'DDT in 93.3% of the samples at mean 0.022 mg/kg. Comparing mean, median and geometric mean concentrations of organochlorine pesticides shows a decrease in values from mean to median and to geometric mean which points out a prevalence of lower concentrations among the total samples and the existence of occasional cases of extreme exposure expressed in range values. The pooled samples divided according to sex, showed only significant differences of pp'DDE median concentrations between sexes. The other organochlorine pesticides indicated no statistical differences between sexes, including the pp'DDE/pp'DDT ratio. The samples grouped according to age, showed that the third tertile was more contaminated for both sexes, indicating age as a positively associated factor with organochlorine pesticide levels in adipose tissue of Veracruz inhabitants. Comparing organochlorine pesticide levels between 2008 and 2010 years, a decreased tendency for β-HCH, pp'DDE, Σ-DDT and pp'DDE/pp'DDT ratio levels was observed.

  20. Combination of QuEChERS and DLLME for GC-MS determination of pesticide residues in orange samples.

    Andraščíková, Mária; Hrouzková, Svetlana; Cunha, Sara C

    2013-01-01

    A new method combining QuEChERS (quick, easy, cheap, effective, rugged and safe) and DLLME (dispersive liquid-liquid microextraction) followed by gas chromatography-mass spectrometry with selected ion monitoring (SIM) was developed for the simultaneous determination of 19 pesticides from nine chemical groups exhibiting or suspected to exhibit endocrine-disrupting properties in orange samples. Acetonitrile extract obtained from QuEChERS extraction was used for DLLME as dispersive solvent and carbon tetrachloride as extractive solvent to increase the enrichment factor of the extraction procedure. The effect of several extraction parameters, such as volume extract achieved by the QuEChERS method and subsequently used for DLLME, selection of extractive solvent and its volume, was tested. Under optimum conditions, good linearity, satisfactory recoveries and repeatability were obtained. Limits of quantification (LOQs) achieved (ranging from 0.02 to 47 ng/g) were below the maximum residue limits established by the European Union. The proposed method was applied to the monitoring of pesticide residue levels in oranges commercialised in Portugal.

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

    *M. A. N. Gbaguidi

    2014-06-01

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

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

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

    2011-12-15

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

  3. FUNGUS INDEX AND RESIDUAL EFFECTS OF PESTICIDES IN ACID AND ALKALINE SOILS

    Soil applied pesticides have profound effects on the population density and diversity of fungi, however, such information is lacking in tropical soils of the Amazon region. Field experiments were implemented at two experimental farms ("El Choclito", "Bello Horizonte”) of Tropical Crop Institute (ICT...

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

    宋欢; 车兰兰; 林勤保; 王蓉珍

    2012-01-01

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

  5. 77 FR 15012 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    2012-03-14

    ... analytical methods for analysis of cottonseed, pome fruit, nutmeats, almond hulls, and fruiting vegetables.... Contact: John Redden, Registration Division (7505P), (703) 305-1969, email address:...

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

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

    2011-12-01

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

  7. 77 FR 50661 - Notice of Filing of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    2012-08-22

    ..., cane at 0.2 ppm. No tolerances are proposed for the processed commodities, refined sugar and molasses... method of analysis is aqueous organic solvent extraction, column cleanup and quantitation by LC/MS/MS. In animals, the method of analysis involves base hydrolysis, organic extraction, column cleanup...

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

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

    2016-06-15

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

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

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

    2016-12-01

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

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

    刘慧玲

    2014-01-01

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

  11. 国内外农药使用与残留控制体系%Pesticide Application and Control System of Residues at Home and Abroad

    王茂华; 唐茂芝

    2012-01-01

    分析了联合国、美国、欧盟、日本等国际组织及国外对农药使用与残留控制的机制,阐述了国际组织和发达国家对农药使用及残留控制体系的发展趋势.介绍了我国对农药使用和残留控制的现状,提出了加强我国对农药使用和残留控制在制度、措施、标准等方面的建议.%The pesticide application and control system of residues in the United Nations, the United States, the European Union, Japan and other international organizations were reviewed in this paper. The situation of the pesticides application and residue control system of the international organizations and the developed countries were summarized. The development trend of residual control system was analyzed. The pesticides application and residue control situation in China was also introduced. Some suggestions on system, measures, and standard to strengthen our country' s control on pesticides use and residues control was proposed.

  12. Pesticide residue concentration in soil following conventional and Low-Input Crop Management in a Mediterranean agro-ecosystem, in Central Greece.

    Karasali, Helen; Marousopoulou, Anna; Machera, Kyriaki

    2016-01-15

    The present study was focused on the comparative evaluation of pesticide residues, determined in soil samples from Kopaida region, Greece before and after the implementation of Low-Input Crop Management (LCM) protocols. LCM has been suggested as an environmental friendly plant protection approach to be applied on crops growing in vulnerable to pollution ecosystems, with special focus on the site specific problems. In the case of the specific pilot area, the vulnerability was mainly related to the pollution of water bodies from agrochemicals attributed to diffuse pollution primarily from herbicides and secondarily from insecticides. A total of sixty-six soil samples, were collected and analyzed during a three-year monitoring study and the results of the determined pesticide residues were considered for the impact evaluation of applied plant protection methodology. The LCM was developed and applied in the main crops growing in the pilot area i.e. cotton, maize and industrial tomato. Herbicides active ingredients such as ethalfluralin, trifluralin, pendimethalin, S-metolachlor and fluometuron were detected in most samples at various concentrations. Ethalfluralin, which was the active ingredient present in the majority of the samples ranged from 0.01 μg g(-1) to 0.26 μg g(-1) soil dry weight. However, the amount of herbicides measured after the implementation of LCM for two cropping periods, was reduced by more than 75% in all cases. The method of analysis was based on the simultaneous extraction of the target compounds by mechanical shaking, followed by liquid chromatography mass spectrometric and gas chromatography electron capture (LC-MS/MS and GC-ECD) analysis.

  13. High-throughput screening of pesticide and veterinary drug residues in baby food by liquid chromatography coupled to quadrupole Orbitrap mass spectrometry.

    Jia, Wei; Chu, Xiaogang; Ling, Yun; Huang, Junrong; Chang, James

    2014-06-20

    A new analytical method was developed and validated for simultaneous analysis of 333 pesticide and veterinary drug residues in baby food. Response surface methodology was employed to optimize a generic extraction method. Ultrahigh-performance liquid chromatography and electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry (UHPLC-ESI Q-Orbitrap) was used for the separation and detection of all the analytes. The method was validated by taking into consideration the guidelines specified in Commission Decision 2002/657/EC and SANCO/12571/2013. The extraction recoveries were in a range of 79.8-110.7%, with coefficient of variation 0.99. The limits of detection for the analytes are in the range 0.01-5.35μgkg(-1). The limits of quantification for the analytes are in the range 0.01-9.27μgkg(-1). This method has been successfully applied on screening of pesticide and veterinary drugs in ninety-three commercial baby food samples, and tilmicosin, fenbendazole, tylosin tartrate and thiabendazole were detected in some samples tested in this study. The present study is very useful for fast screening of different food contaminants.

  14. Analysis of endocrine disrupting pesticides by capillary GC with mass spectrometric detection.

    Matisová, Eva; Hrouzková, Svetlana

    2012-09-01

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

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

    Svetlana Hrouzková

    2012-09-01

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

  16. Design and Implementation of Pesticide Residues Detector%农药残留检测仪的设计与实现

    钟金; 王红蕾

    2016-01-01

    In recent years ,large scale use of pesticides in vegetables has inevitably resulted in pesti‐cide residues ,which could endanger people’s health and life .The core task of the design is to detect pesti‐cide residues in vegetables .Based on the role of pesticides in inhibiting the enzyme ,the changes in absor‐bance before and after the inhibitory effect of pesticides on enzyme are measured .Then the rate of inhibi‐tion of pesticides on enzyme is measured .Different inhibition rates represent different concentrations of pesticides the vegetables contain .This method can detect whether a pesticide is beyond the set standard .%针对农药在蔬菜中的大量使用,造成蔬菜在食用时难免会有农药的残留,危及人们的健康及生命安全的情况。设计了农药残留检测仪。通过农药对酶的抑制,测出农药对酶抑制前后吸光度的变化,从而测出农药对酶的抑制率,不同的抑制率代表蔬菜所含农药浓度不同,从而便可检测出农药是否超出设定标准。

  17. Organochlorine pesticide residue levels in blood serum of inhabitants from Veracruz, Mexico.

    Waliszewski, Stefan M; Caba, M; Herrero-Mercado, M; Saldariaga-Noreña, H; Meza, E; Zepeda, R; Martínez-Valenzuela, C; Gómez Arroyo, S; Villalobos Pietrini, R

    2012-09-01

    The objective of the present study was to monitor the levels of organochlorine pesticides HCB; α-, β-, γ-HCH; pp'DDE; op'DDT; and pp'DDT in blood serum of Veracruz, Mexico inhabitants. Organochlorine pesticides were analyzed in 150 blood serum samples that constituted that which remained after clinical analyses, using gas chromatography-electron-capture detection (GC-ECD). The results were expressed as milligrams per kilogram on fat basis and micrograms per liter on wet weight. Only the following pesticides were detected: p,p'-DDE was the major organochlorine component, detected in 100% of samples at mean 15.8 mg/kg and 8.4 μg/L; p,p'-DDT was presented in 41.3.% of monitored samples at mean 3.1 mg/kg and 1.4 μg/L; β-HCH was found in 48.6% of the samples at mean 4.9 mg/kg and 2.7 μg/L; op'DDT was determined to be in only 3.3% of monitored samples at mean 2.7 mg/kg and 1.4 μg/L. The pooled samples divided according to sex showed significant differences of β-HCH and pp'DDE concentrations in females. The samples grouped according to age presented the third tertile as more contaminated in both sexes, indicating age as a positively associated factor with serum organochlorine pesticide levels in Veracruz inhabitants.

  18. Comparative estrogenic activity of wine extracts and organochlorine pesticide residues in food.

    Gaido, K.; Dohme, L; Wang, F.; Chen, I; Blankvoort, B; Ramamoorthy, K; Safe, S.

    1998-01-01

    The human diet contains industrial-derived, endocrine-active chemicals and higher levels of naturally occurring compounds that modulate multiple endocrine pathways. Hazard and risk assessment of these mixtures is complicated by noadditive interactions between different endocrine-mediated responses. This study focused on estrogenic chemicals in the diet and compared the relative potencies or estrogen equivalents (EQs) of the daily consumption of xenoestrogenic organochlorine pesticides in food...

  19. Analysis of organochlorine pesticides in human milk: preliminary results.

    Campoy, C; Jiménez, M; Olea-Serrano, M F; Moreno-Frías, M; Cañabate, F; Olea, N; Bayés, R; Molina-Font, J A

    2001-11-01

    In the face of evidence of human milk contamination by organochlorine pesticides, an analysis was performed on samples of milk obtained from healthy lactating women in the provinces of Granada and Almeria in Southern Spain. The samples were obtained by the Neonate Section of the Department of Pediatrics of Granada University Hospital (Neonatology Division) and by the Neonatal Service of Poniente Hospital in El Ejido, Almería. A liquid-liquid extraction procedure was performed. The cleaning of the sample before gas chromatography-mass spectrometry (GC-MS) used silica Sep-Pak. Among other pesticides, aldrin, dieldrin, DDT and its metabolites, lindane, methoxychlor and endosulfan were identified. The presence of these products was confirmed by mass spectrometry. The identification and quantification of these organochlorine molecules is important because they have estrogenic effects.

  20. Assisted distillation cleanup of pesticide residues in animal fats: new beadless distillation tube.

    Heath, A B; Black, R R

    1987-01-01

    A new assisted distillation tube has been developed which contains no glass beads or glass wool. The sample is injected into the top of the tube, and a septum is not required. Large ground-glass joints (10/19) are used at the gas inlet and at the Florisil trap connection for maximum strength. Existing assisted distillation apparatus was easily modified to accept the new tubes. Recoveries of 9 organochlorine pesticides from butter and cattle fat ranged from 87 to 104% at a tube temperature of 230 degrees C and a nitrogen flow rate of 250 mL/min. No significant change occurred in recoveries of 8 of the 9 pesticides after 85 uses of the beadless tube. Only the recovery of HCB from butter decreased, from 95 to 80%, after 51 runs. The new tube was compared with the Unitrex glass bead-packed concentric tube at flow rates of 230, 400, and 600 mL nitrogen/min. Recoveries from the Unitrex tube were similar to those of the beadless tube for all pesticides except DDT which was significantly lower, indicating incomplete distillation at 250 mL/min and possible partial breakdown at 400 and 600 mL/min. A procedure is introduced for pressurized solvent washing of distillation tubes. This procedure is more efficient than vacuum washing.

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

    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 μg/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 μg/kg, whereas limits of quantification (LOQs) from 0.5 to 20 μg/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 μg/kg respectively.

  2. Residual Stress Analysis in Thick Uranium Films

    Hodge, A M; Foreman, R J; Gallegos, G F

    2004-12-06

    Residual stress analysis was performed on thick, 1.0 to 25 {micro}m, depleted Uranium (DU) films deposited on an Al substrate by magnetron sputtering. Two distinct characterization techniques were used to measure substrate curvature before and after deposition. Stress evaluation was performed using the Benabdi/Roche equation, which is based on beam theory of a bi-layer material. The residual stress evolution was studied as a function of coating thickness and applied negative bias voltage (0-300V). The stresses developed were always compressive; however, increasing the coating thickness and applying a bias voltage presented a trend towards more tensile stresses and thus an overall reduction of residual stresses.

  3. SVD analysis of Aura TES spectral residuals

    Beer, Reinhard; Kulawik, Susan S.; Rodgers, Clive D.; Bowman, Kevin W.

    2005-01-01

    Singular Value Decomposition (SVD) analysis is both a powerful diagnostic tool and an effective method of noise filtering. We present the results of an SVD analysis of an ensemble of spectral residuals acquired in September 2004 from a 16-orbit Aura Tropospheric Emission Spectrometer (TES) Global Survey and compare them to alternative methods such as zonal averages. In particular, the technique highlights issues such as the orbital variation of instrument response and incompletely modeled effects of surface emissivity and atmospheric composition.

  4. Spectroscopic Analysis of Organophosphorus Pesticides Using Colorimetric Reactions

    Amit Kumar Sharma

    2016-01-01

    The UV-Vis and infrared (IR)absorption spectra of organophosphorus (OP)pesticides have been studied.A correlation in spectra was developed to optimize the OP pesticides in the environments.The spec-troscopic (UV-Vis and IR)spectrum of OP pesticides like methyl parathion,malathion and parathion has been interpreted in detail.A complete calculation of the normal frequencies and absolute intensities of UV-Vis and IR absorption bands are interpreted with the help of corresponding experimental data.In the colorimetric reac-tions,the bands appear at 2 077,1 637,1 455,1 015,655 cm-1 for malathion;2 081,1 639,1 316,1 015, 794,683 cm-1 for parathion;2 078,1 632,1 032,794 cm-1 for methyl parathion were used for quantitative or qualitative analysis.All these IR spectra were acquired by averaging 100 scans at a resolution of 4 cm-1 .It is determined experimentally in the region 200~450 nm for UV-Vis absorption bands and in the region 400~4 000 cm-1 for IR absorption bands.It is concluded that the mainly optically active groups (P—OH, C—O, P—O, C—O—C,P—O—C, P—S, —OH)present in pesticides which are responsible in change in sig-nificant data for quantitative and qualitative analysis.The various optical properties like wavelength,band en-ergy,wave number,and frequency,also are calculated.

  5. [A Simultaneous Determination Method with Acetonitrile-n-Hexane Partitioning and Solid-Phase Extraction for Pesticide Residues in Livestock and Marine Products by GC-MS].

    Yoshizaki, Mayuko; Kobayashi, Yukari; Shimizu, Masanori; Maruyama, Kouichi

    2015-01-01

    A simultaneous determination method was examined for 312 pesticides (including isomers) in muscle of livestock and marine products by GC-MS. The pesticide residues extracted from samples with acetone and n-hexane were purified by acetonitrile-n-hexane partitioning, and C18 and SAX/PSA solid-phase extraction without using GPC. Matrix components such as cholesterol were effectively removed. In recovery tests performed by this method using pork, beef, chicken and shrimp, 237-257 pesticides showed recoveries within the range of 70-120% in each sample. Validity was confirmed for 214 of the target pesticides by means of a validation test using pork. In comparison with the Japanese official method using GPC, the treatment time of samples and the quantity of solvent were reduced substantially.

  6. 农产品/食品中农药残留快速检测方法研究进展%Review on rapid detection of pesticide residues in agricultural and food products

    蒋雪松; 王维琴; 许林云; 卢利群; 周宏平; 陈卉卉

    2016-01-01

    Pesticides were widely applied to eliminate or control a variety of agricultural pests and diseases. However, they exhibited acute or chronic toxicity on human health through their residues in agricultural product and food. Thus, monitoring pesticide residues was extremely crucial to ensure that pesticides in agricultural products were in permitted levels. The identification and quantification of pesticides were generally based on mass spectrometry combined with gas and/or liquid chromatography, or capillary electrophoresis. However, these methods involved large and expensive instruments, time-consuming sample preparation and trained personnel. Therefore, it was important to set up onsite assays and techniques, especially highly sensitive and selective, simple, efficient, and cost effective ones for rapid detection of pesticide residues. This review summarized the application of fast analytical methodologies such as enzyme inhibition assays (EIA), immunoassays, optical spectroscopy assays and various biosensors in the analysis of pesticide residues in agro product and food in the past few years. EIA was widely used for rapid colorimetric or spectrophotometric screening of pesticides in China, which was based on the inhibition of cholinesterase (ChE) activity by organophosphate and carbamate. Immunoassays, such as enzyme-linked immunosorbent assay (ELISA), were quantitative or qualitative methods of analysis for a substance, which took antibodies as the analytical reagents. Immunoassays depended on the use of an analytical reagent that was associated with a detectable marker, such as enzyme, fluorescence, chemoluminescence radioactive element, and so on. Colloidal gold-based immunoassay was proven to be fast, sensitive and cost-effective for pesticide detection. Biosensors were analytical devices, used for the detection of analytes, which combined a biological component with a physicochemical detector. The development of biosensors for pesticides was also an active

  7. Evaluation of a new carbon/zirconia-based sorbent for cleanup of food extracts in multiclass analysis of pesticides and environmental contaminants

    A novel carbon/zirconia based material, SupelTM QuE Verde (Verde), was evaluated in a filter-vial dispersive solid phase extraction (d-SPE) cleanup of QuEChERS extracts of pork, salmon, kale, and avocado for residual analysis of pesticides and environmental contaminants. Low pressure (LP) GC-MS/MS w...

  8. Pesticide residue evaluation in major staple food items of Ethiopia using the QuEChERS method: a case study from the Jimma Zone.

    Mekonen, Seblework; Ambelu, Argaw; Spanoghe, Pieter

    2014-06-01

    Samples of maize, teff, red pepper, and coffee (green bean and coffee bean with pulp) were collected from a local market in the Jimma Zone, Ethiopia. Samples were analyzed for the occurrence of cypermethrin, permethrin, deltamethrin, chlorpyrifos ethyl, DTT and its metabolites, and endosulfan (α, β). In the analytical procedure, the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction methodology with dispersive solid phase extraction clean up (d-SPE) technique was applied. Validation of the QuEChERS method was satisfactory. Recovery percentages of most pesticides were in the range of 70% to 120%, with good repeatability (%relative standard deviation coffee bean. Residues of DDT in coffee pulp significantly differed (p < 0.01) from other food items except for red pepper. The concentration of pesticides in the food items varied from 0.011 mg/kg to 1.115 mg/kg. All food items contained 1 or more pesticides. Two-thirds of the samples had residues below corresponding maximum residue limits, and the remaining one-third of samples were above the maximum residue limits. These results indicate the need for a good pesticide monitoring program to evaluate consumer risk for the Ethiopian people.

  9. Probabilistic risk assessment of dietary exposure to single and multiple pesticide residues or contaminants: Summary of the work performed within the SAFE FOODS project

    Klaveren, van J.D.; Boon, P.E.

    2009-01-01

    This introduction to the journal's supplement on probabilistic risk assessment of single and multiple exposure to pesticide residues or contaminants summarizes the objectives and results of the work performed in work package 3 of the EU-funded project SAFE FOODS. Within this work package, we develop

  10. Organochlorine pesticide residues in human milk and estimated daily intake (EDI) for the infants from eastern region of Saudi Arabia.

    Hajjar, M Jamal; Al-Salam, Ahmad

    2016-12-01

    This study presents the level of organochlorine pesticide (OC) residues in human milk samples collected from donor mothers aged from 18 to 30 years old, from four cities in Eastern district of Saudi Arabia (Al-Hassa, Al- Khobar, Al-Jubail, and Al-Dammam). Pesticides residues were extracted from the samples and analyzed using GC-MS. The results showed that, only pp'DDE and p,pDDD, were found in 82.5% and 70% of analyzed samples respectively, the total DDT were at level of 0.37, 0.32, 0.30 and 0.46 μg/L in the four cities respectively and were far below the MRL of 50 μg/L (FAO/WHO). The estimated daily intake (EDI) of DDT ingested by infant weight 3.5 kg ranged between 0.06 and 0.10 μg/kg, which is less than the ADI issued by (EFSA, 2014). Lindane (γ-HCH) found in 91.25% of the analyzed samples at level of 0.37, 0.35, 0.35 and 0.29 μg/L. The EDIs of Lindane by infant were far below the ADI of 5 μg/kg bw/day. Dieldrin and Enderin were found in 27.5% and 58.8% of samples respectively and were lower than MRL issued by FAO/WHO, but the (EDI) was higher than the ADI issued by EFSA. The isomer A-heptachlor was detected in 51% of the samples, at levels were 15 times lower than the MRL issued by FAO/WHO, but EDIs by infants were 2-4 times higher than the ADI issued by EFSA. However, the results of the four studied areas in Saudi Arabia showed no statistically different among locations (p > 0.05).

  11. Comparative estrogenic activity of wine extracts and organochlorine pesticide residues in food.

    Gaido, K; Dohme, L; Wang, F; Chen, I; Blankvoort, B; Ramamoorthy, K; Safe, S

    1998-12-01

    The human diet contains industrial-derived, endocrine-active chemicals and higher levels of naturally occurring compounds that modulate multiple endocrine pathways. Hazard and risk assessment of these mixtures is complicated by noadditive interactions between different endocrine-mediated responses. This study focused on estrogenic chemicals in the diet and compared the relative potencies or estrogen equivalents (EQs) of the daily consumption of xenoestrogenic organochlorine pesticides in food (2.44 micrograms/day) with the EQs in a single 200-ml glass of red cabernet wine. The reconstituted organochlorine mixture contained 1,1,1-trichloro-2-(p-chlorophenyl)-2-(o-chlorophenyl)ethane, 1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane, 1,1-dichloro-2,2-bis(p-chlorophenyl)ethylene, endosulfan-1, endosulfan-2, p,p'-methoxychlor, and toxaphene; the relative proportion of each chemical in the mixture resembled the composition reported in a recent U.S. Food and Drug Administration market basket survey. The following battery of in vitro 17 beta-estradiol (E2)-responsive bioassays were utilized in this study: competitive binding to mouse uterine estrogen receptor (ER); proliferation in T47D human breast cancer cells; luciferase (Luc) induction in human HepG2 cells transiently cotransfected with C3-Luc and the human ER, rat ER-alpha, or rat ER-beta; induction of chloramphenicol acetyltransferase (CAT) activity in MCF-7 human breast cancer cells transfected with E2-responsive cathepsin D-CAT or creatine kinase B-CAT plasmids. For these seven in vitro assays, the calculated EQs in extracts from 200 ml of red cabernet wine varied from 0.15 to 3.68 micrograms/day. In contrast, EQs for consumption of organochlorine pesticides (2.44 micrograms/day) varied from nondetectable to 1.24 ng/day. Based on results of the in vitro bioassays, organochlorine pesticides in food contribute minimally to dietary EQ intake.

  12. [Occurrence of residues of organochlorine pesticides, nitromusk compounds and polychlorobiphenyls in Turkish canned fish products].

    Ozden, O; Kruse, R; Erkan, N

    2001-04-01

    In our study we elaborated an overview on the contamination grade of fish from Turkish waters by selected organochlorine pesticides, nitromusks and chlorobiphenyl congenres. We could demonstrate, that the tested fish species, being prior processed to canned products and brought to the market, contained particularly unmistakable amounts of the above mentioned analytes. Sardines, sardelles and trout gave results generally far below the German regulatory limits. However total DDT in pelamides reached an order of magnitude near the German limit of 0.5 mg/kg (based on wet weight). The necessity of enhanced systematic measurements for monitoring pollutants in fish from Turkish waters thus becomes evident.

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

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

    1995-12-01

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

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

    WANG Xiaofei; WANG Dianzhong; QIN Xiaofei; XU Xiaobai

    2008-01-01

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

  15. [Isolation and identification of degradation bacteria Enterobacter aerogenes for pyrethriods pesticide residues and its degradation characteristics].

    Liao, Min; Zhang, Hai-jun; Xie, Xiao-mei

    2009-08-15

    By incubation experiment, the bacterial strain labeled as M6R9 was isolated from the tame sludge in water course of Pesticide Factory of Hangzhou, and was identified as Enterobacter aerogenes, which had highly efficient degradation for Bifenthrin, Fenpropathrin and Cypermethrin. By investigating the physiological characteristics of the strain, the results show that the bacterium is a gram-negative aerobe bacilli, size is (0.8-1.9) microm x (0.5-1.0) microm, and is capable of utilizing Bifenthrin, Fenpropathrin and Cypermethrin as sole carbon source. Under the condition of ventilation, (25-30) degrees C, inoculated amount at D(415 nm) 0.2, pH 7.0, pesticide concentration 100 mg x L(-1) and vibrational speed 180 r x min(-1), the degradation efficiencies to Bifenthrin, Fenpropathrin and Cypermethrin are the highest by strain M6R9. Under such condition, in the mixture culture medium with 100 mg x L(-1) Bifenthrin, Fenpropathrin and Cypermethrin, the degradation ratios are 55.74%, 55.11% and 55.96% after culturing 3 d, respectively, the degradation processes are fitted for first-order kinetic equation and the half lives (t(1/2)) are 65.4,70.7 and 68.6 h respectively. The degradation ability of Enterobacter aerogenes M6R9 on Bifenthrin, Fenpropathrin and Cypermethrin is positively correlated to inoculated amount,vibrational speed and ventilation.

  16. Pesticide residues in beeswax samples collected from honey bee colonies (Apis mellifera L.) in France.

    Chauzat, Marie-Pierre; Faucon, Jean-Paul

    2007-11-01

    In 2002 a field survey was initiated in French apiaries in order to monitor the health of honey bee colonies (Apis mellifera L.). Studied apiaries were evenly distributed across five sites located in continental France. Beeswax samples were collected once a year over 2 years from a total of 125 honey bee colonies. Multiresidue analyses were performed on these samples in order to identify residues of 16 insecticides and acaricides and two fungicides. Residues of 14 of the searched-for compounds were found in samples. Tau-fluvalinate, coumaphos and endosulfan residues were the most frequently occurring residues (61.9, 52.2 and 23.4% of samples respectively). Coumaphos was found in the highest average quantities (792.6 microg kg(-1)). Residues of cypermethrin, lindane and deltamethrin were found in 21.9, 4.3 and 2.4% of samples respectively. Statistical tests showed no difference between years of sampling, with the exception of the frequency of pyrethroid residues. Beeswax contamination was the result of both in-hive acaricide treatments and, to a much lesser extent, environmental pollution.

  17. Residue behaviour of six pesticides in button crimini during home canning.

    Du, Pengqiang; Liu, Xingang; Gu, Xiaojun; Dong, Fengshou; Xu, Jun; Kong, Zhiqiang; Li, Yuanbo; Zheng, Yongquan

    2014-01-01

    The effect of home canning (including washing, boiling, cooling, adding solution and sterilisation) on residue levels of imidacloprid, diflubenzuron, abamectin, pyriproxyfen and β-cypermethrin and chlorothalonilin on button crimini was assessed. Residues of imidacloprid, diflubenzuron, abamectin and pyriproxyfen were measured by UPLC-MS/MS; the residues of β-cypermethrin and chlorothalonil were measured by GC. Results showed that washing resulted in a 3.8% reduction of the initial residue level of imidacloprid (p ≤ 0.05). From washing to sterilisation the processing effect was significant compared with raw crimini (p ≤ 0.05), but processing through cooling and adding solution had no effect. For diflubenzuron, from raw crimini to sterilisation the processing effect was significant by comparison with the initial level (p ≤ 0.05); the processing effect was not obvious between two sequential steps, and the sequential steps have list: washing and boiling, boiling and cooling, boiling and adding of solution, cooling and adding solution. The changes in abamectin levels were also significant from raw crimini to sterilisation compared with raw crimini (p ≤ 0.05), but the changes were not obvious from boiling to adding solution and amongst them. For pyriproxyfen, washing resulted in a 39% reduction, but changes were not obvious from washing to sterilisation, p ≤ 0.05 between two consecutive steps. The whole procedure could significantly decrease residues of β-cypermethrin (p ≤ 0.05); washing could significantly reduce residues of β-cypermethrin; the effects of last procedures were complicated, and p ≤ 0.05 between two consecutive steps. Washing resulted in an 80% reduction of chlorothalonil; after washing there were no detectable residues. After the whole process, the processing factors for imidacloprid, diflubenzuron, abamectin, pyriproxyfen, β-cypermethrin and chlorothalonil were 0.40, 0.22, 0.04, 0.85, 0.28 and 0, respectively.

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

    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.

  19. Rapid analytical method for the determination of pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction prior to gas chromatography-tandem mass spectrometry.

    Prados-Rosales, R C; Luque García, J L; Luque de Castro, M D

    2003-04-18

    A rapid analytical method for determination of organochlorine pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction has been developed. The main factors affecting the extraction efficiency--namely microwave power, irradiation time, volume of extractant and number of cycles--were optimized by a two-level factorial fractional design. After extraction, a liquid-liquid extraction and a clean-up step including the use of Florisil macrocolumns were required prior to injection of the extracts into the chromatograph in order to isolate the pesticide residues from the lipid fraction of the original extract. The MS-MS ion preparation mode was selected due to the high sensitivity and selectivity it provides. Seed samples were used collected near a crop subjected to aerial pesticide application. Residues of hexachlorocyclohexane isomers and endosulfan were found in the seeds although they were not subjected to pesticide application, thus showing the spray-drift contamination. The validation of the proposed approach was carried out by comparison with the ISO 659-1988 reference extraction method obtaining similar, or even better efficiencies by the proposed approach.

  20. Resíduos de agrotóxicos em frutos de tomate Pesticide residues in tomato fruits

    Leslie Maria Segura Zavatti

    1999-03-01

    Full Text Available O uso intensivo de agrotóxicos em culturas de tomates tem causado preocupações quanto à provável contaminação do produto final. Este trabalho teve como objetivo monitorar, por dois anos consecutivos, em quatro propriedades de uma área altamente tecnificada, o uso de agrotóxicos em tomate irrigado durante seu desenvolvimento, quantificar os resíduos dos principais princípios ativos utilizados, e avaliar o grau de contaminação dos frutos colhidos. Foram analisados metamidofós, clorpirifós, captan, clorotalonil, endosulfan, lambda-cialotrina, e cobre. Para avaliar o grau de contaminação dos frutos foi validado um método de análise de resíduos múltiplos capaz de quantificar esses compostos. Os resíduos encontrados foram de fungicidas e inseticidas aplicados nas fases de frutificação e maturação: captan, 0,35 mg/kg, na Fazenda 2; clorotalonil, 0,16 mg/kg e 0,95 mg/kg, nas Fazendas 1 e 2, respectivamente; lambda-cialotrina, 0,03 mg/kg, na Fazenda 2; cobre, 2,03 mg/kg, 3,75 mg/kg e 1,44mg/kg, nas Fazendas 1, 2 e 3, respectivamente, e 0,95 mg/kg, 1,70 mg/kg e 2,31 mg/kg, na Fazenda 4. Não ocorreram resíduos dos inseticidas organofosforados, aplicados principalmente durante o desenvolvimento vegetativo da cultura. Não houve contaminação dos tomates pelos agrotóxicos analisados. Os resíduos que devem ser monitorados são os dos agrotóxicos aplicados na fase de maturação da cultura.The intensive use of pesticide in tomato crops have been causing concern about a possible contamination of the final product. This work aimed at monitoring, for two years, in four farms located in a high technology area, the use of pesticides in irrigated tomato crops, quantifying the main active ingredient residues and evaluating the contamination level of the fruits. The components analised were: methamidophos, chlorpyrifos, captan, chlorothalonil, endosulfan, lambda-cyhalothrin and copper oxychloride. In order to evaluate the contamination

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

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

    2016-01-01

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

  2. PDMS固相萃取-气相色谱法检测甘蔗中有机磷农药残留%The Method of PDMS Solid Phase Membrane Extraction-Gas Chromatographic Analysis for Organ Phosphorus Pesticide Residue of Sugarcane

    赵汉民; 彭金云; 谭义秋; 农克良

    2011-01-01

    [目的]建立一套快速、简单、准确的有机磷残留量检测方法.[方法]用聚二甲基硅氧烷(PDMS)固相萃取膜吸附萃取甘蔗汁中甲拌磷和特丁硫磷,经二氯甲烷脱附后,FTD/GC直接检测.[结果]用PDMS固相萃取-气相色谱法检测了甘蔗汁中添加甲拌磷和特丁硫磷的标准品混合液,甲拌磷和特丁硫磷得到有效的分离和确认.[结论]PDMS固相萃取-气相色谱法操作简单,能快速、准确地检测有机磷农药残留.%[ Objective ] To establish a fast, simple and accurate detection method for organophosphate residues. [ Method ] Phorate and terbufos in sugarcane juice were absorbed by the membrane extraction of PDMS solid phase extraction, then disported by dichloromethane and detected directly by FID/GC. [ Result] Mixed liquid of sugar cane juice and phorate, terbufos standard substances were detected,and phorate and terbufos were effectively separated and recognized by PDMS-SPE-GC method. [Conclusion] PDMS-SPEM-GC is a simple,fast and accurate method to be detected of organ phosphorus pesticide residues.

  3. Determination of Levels of Organochlorine, Organophosphorus, and Pyrethroid Pesticide Residues in Vegetables from Markets in Dar es Salaam by GC-MS

    John A. M. Mahugija

    2017-01-01

    Full Text Available This study investigated the levels of pesticides and metabolites in vegetables from major markets in Dar es Salaam city, Tanzania. Samples of fresh cabbage, spinach, and onions from the markets were analysed for pesticide residues. Extraction was performed using acetone followed by dichloromethane : cyclohexane mixture and the extracts were cleaned up using Florisil. The compounds were determined by gas chromatography-mass spectrometry (GC-MS. Pesticides and metabolites were detected in 72.2% of the samples. The detected pesticide residues and their highest mean concentrations were p,p′-DDT 4.00 × 10−3 mg/kg, p,p′-DDD 6.40 × 10−1 mg/kg, o,p′-DDD 1.00 × 10−2 mg/kg, α-endosulfan 6.00 × 10−1 mg/kg, β-endosulfan 2.10 × 10−1 mg/kg, chlorpyrifos 3.00 mg/kg, and cypermethrin 4.00 × 10−2 mg/kg. The most frequently detected compounds were p,p′-DDD and chlorpyrifos. The order of contamination was spinach > cabbage > onions. Generally, there were no significant variations in concentrations of pesticide residues among samples and sampling sites, which indicated similarities in contamination patterns. The concentrations of contaminants were above the maximum residue limits (MRLs in 33.3–50% of the samples. The findings indicated risks and concerns for public health.

  4. Progress of Research on the Detection Techniques of Pesticides Residue in Plant-based Food%植物性食品中农药残留检测技术研究进展

    李畅

    2013-01-01

    The paper describes the detection techniques including gas chromatography,liquid chromatography,GC-MS/MS,HPLC-MS/MS,ampere assay and the immune analysis technology of pesticides in plant-based foods in re⁃cent years and put forward the development trend in the detection techniques of pesticide residues determination in future.%  综述了近年来在植物性食品中农药残留分析技术中广泛应用的气相色谱法、液相色谱法、气质联用法、液质联用法、安培检测法和免疫分析技术等几种分析检测技术,并展望了植物性食品中农药残留检测技术的发展前景。

  5. Determination of Dithiocarbamate Pesticide Residues in Tobacco by Gas Chromatography-Mass Spectroscopy%烟草中二硫代氨基甲酸酯农药残留量的测定

    边照阳; 唐纲岭; 张洪非; 李中皓; 胡清源

    2011-01-01

    为提高烟草中农药残留量的检测效率,建立了一种快速测定二硫代氨基甲酸酯类农药的方法.在密闭系统中,试样中的二硫代氨基甲酸酯在加热、超声条件下与还原性酸溶液反应,分解产生的二硫化碳经过异辛烷吸收后用气相色谱/质谱联用法(GC/MS)检测,以二硫化碳的含量表示二硫代氨基甲酸酯残留量.结果表明:方法的回收率在90.4%~106.O%之间,相对标准偏差(RSD)在3.2%~9.5%之间,定量限为0.017 mg/kg.该法可用于批量烟草样品中二硫代氨基甲酸酯类农药残留量的快速检测.%A method was presented for the analysis of dithiocarbamate pesticide residues in tobacco, in which tobacco was put into a closed-conical flask, the residues of dithiocarbamate pesticides in tobacco were extracted and hydrolyzed to CS2 under ultrasonic conditions, then CS2 trapped in a layer of iso-octane overlaying the reaction mixture was taken for gas chromatography-mass spectroscopy analysis.The recoveries ranged from 90.4% to 106.0% with the relative standard deviations (RSD) of 3.2% to 9.5% and the limit of quantification ( LOQ).of 0.017 mg/kg.This method can be used for the fast analysis of the dithiocarbamate pesticide residues in tobacco.

  6. Hair analysis to document non-fatal pesticide intoxication cases.

    Dulaurent, S; Gaulier, J M; Baudel, J L; Fardet, L; Maury, E; Lachâtre, G

    2008-03-21

    We reported two non-fatal cases of intoxication with pesticides namely alachlor and carbofuran. Hair stand samples were collected from two men approximately 1 year after alachlor intoxication for case 1, and 14 days after the last exposure for case 2. Hair analysis was performed using a liquid chromatography-tandem mass spectrometry method. In case 1, alachlor was detected in the 5 analysed hair segments (concentrations between 12 and 136 pg/mg) and its metabolites were not detected. In case 2, carbofuran and its main metabolite (3-hydroxycarbofuran) were detected in the hair strand (global analysis) at the concentrations of 207 and 164 pg/mg, respectively. However, additional data are required in order to interpret such results.

  7. Multi-residue determination of pesticides in water using multi-walled carbon nanotubes solid-phase extraction and gas chromatography-mass spectrometry.

    Wang, Shuo; Zhao, Peng; Min, Guang; Fang, Guozhen

    2007-09-21

    A reliable multi-residue method which was based on solid-phase extraction (SPE) with multi-walled carbon nanotubes (MWCNTs) as adsorbent was developed for determination and quantitation of 12 pesticides (carbofuran, iprobenfos, parathion-methyl, prometryn, fenitrothion, parathion-ethyl, isocarbofos, phenthoate, methidathion, endrin, ethion, methoxychlor) in surface water by gas chromatography-mass spectrometry (GC-MS). Parameters that might influence the extraction efficiency such as the eluent volume, the sample flow rate and the sample loading volume were optimized. The experimental results showed the excellent linearity of 12 pesticides (R(2)>0.99) over the range of 0.04-4 microg L(-1), and the precisions (RSD) were 3.1-15.1% under the optimal conditions. The detection limits of proposed method could reach 0.01-0.03 microg L(-1) based on the ratio of chromatographic signal to base line noise (S/N=3). Good recoveries achieved with spiked water samples were in the range of 82.0-103.7%. The results indicated that MWCNTs have good adsorbability to the 12 pesticides tested in this study. With less cost, less analytical time and less solvent-consuming, the developed multi-residue method could be used to determine multi-class pesticides in water simultaneously.

  8. Determination of pesticide residues in wine by membrane-assisted solvent extraction and high-performance liquid chromatography-tandem mass spectrometry.

    Moeder, M; Bauer, C; Popp, P; van Pinxteren, M; Reemtsma, T

    2012-06-01

    The determination of pesticides in food products is an essential issue to guarantee food safety and minimise health risks of consumers. A protocol based on membrane-assisted solvent extraction and liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) that allows the determination of 18 pesticides in red wine at minimum labour effort for sample preparation was developed and validated. Ten millilitres of wine were extracted using 100 μL of toluene filled in a non-porous polyethylene membrane bag which is immersed in the wine sample. After 150 min extraction under stirring, an aliquot of the extraction solution is analysed using HPLC-MS/MS. The limits of quantification ranged from 3 ng/L for Pirimicarb to 1.33 μg/L for Imidacloprid. Quantification by matrix-matched calibration provided relative standard deviations ≤16 % for most of the target pesticides. The linearity of calibration was given over three to four orders of magnitude, which enables the reliable measurement of a broad range of pesticide concentrations, and for each target pesticide, the sensitivity of the protocol meets the maximum residue levels set by legislations at least for wine grapes. Good agreement of results was found when the new method was compared with a standard liquid-liquid extraction protocol. In five wine samples analysed, Carbendazim and Metalaxyl were determined at micrograms per litre concentrations, even in some of the organic wines. Tebuconazol and Cyprodinitril were determined at lower abundance and concentration, followed by Spiroxamin and Diuron.

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

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

    2015-01-01

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

  10. [Simultaneous determination of captan and folpet pesticide residues in apples by solid-phase extraction and high performance liquid chromatography].

    Wang, Shuju; Yu, Yanbin; Tan, Peigong; Miao, Zaijing; Wei, Yishan

    2007-03-01

    A method for the simultaneous determination of captan and folpet pesticide residues in apples was developed by solid-phase extraction and high performance liquid chromatography. The sample was extracted with acetonitrile and cleaned-up by a mixture of homemade sorbent and silica gel with hexane-dichloromethane-acetonitrile (50:49: 1, v/v) as the eluent. The cleaned effects by using Florisil column, amino column, the mixed sorbent were compared, and the effect of the mixed sorbent was the best. The optimal analytical conditions were follow as: an methanol-acetonitrile-water (50: 5:45, v/v) containing 0. 1 mmol/L acetic-acetate buffer (pH 3. 80) as the mobile phase, detection at 210 nm. The method had a good linear relationship in the range of 0. 40 - 8. 00 mg/kg for captan and folpet (r > 0. 999 9). The detection limits of captan and folpet were 0. 27 mg/kg and 0. 20 mg/kg, respectively. The relative standard deviations (RSDs) of retention time were no more than 0. 60%. The average recoveries of captan and folpet from the apples spiked at three levels ranged from 69. 3% - 106% and 101% - 108%, with RSD of 3. 7% - 4. 7% and 1. 3% - 5. 4%, respectively.

  11. 茶树油清除豇豆农药残留的效果%Effects of tea tree oils on removing pesticide residue in cowpea

    林丽静; 程盛华; 李积华; 黄茂芳; 唐永富; 朱德明

    2013-01-01

    Pesticides are widely used as an insurance policy against devastating crop losses from pests and diseases. Excessive usage of pesticides may lead to contamination of the crop and the environment, eventually posing a risk of pesticide-related illnesses to humans. Previous literature has shown that water washing is only partially effective in removing pesticides, and in the case of liposoluble pesticides, a cosolvent must be used as an adjuvant. Recently, naturally occurring adjuvants are gaining prominence over synthetic chemical compounds. Tea tree oil (TTO, the oil of Melaleuca alternifolia), a natural, volatile essential oil, is mainly extracted by steam distillation from the fresh leaves and terminal branchlets of the plant. It has attracted significant interest due to its antifungal, antiviral, and antibacterial bioactivities. However, to the best of our knowledge, there are fewer experimental data evaluating its efficacy in the removal of pesticide residues. In this study, the effects of TTO on removing pesticide residue were carried out in the cowpea. Volume:volume (v:v) concentrations of 0.05%, 0.1%, 0.2%, 0.4% and 0.8% of TTO and water soluble tea tree oil (WTTO) in water were used to remove a standardized pesticide mixture (organophosphorus, pyrethroid, and carbamate compounds) from cowpeas. Sample pretreatment (pesticide application to cowpeas) was performed according to agricultural industry standards. The objective pesticide residues in cowpeas were assayed by gas chromatography (GC) and chromatography-mass spectrometry detection (GC-MS), and then the clearance rate was calculated. The results showed that TTO was able to remove the three kinds of pesticides from cowpeas. Moreover, the removal efficiency increased with increasing concentration of TTO. The effect of clearing organophosphate was much more obvious than that of either pyrethroid or carbamate. It was suggested that small liposoluble molecules of TTO rapidly infiltrate the cowpea surface to

  12. Critical assessment of extraction methods for the simultaneous determination of pesticide residues and mycotoxins in fruits, cereals, spices and oil seeds employing ultra-high performance liquid chromatography-tandem mass spectrometry.

    Lacina, Ondrej; Zachariasova, Milena; Urbanova, Jana; Vaclavikova, Marta; Cajka, Tomas; Hajslova, Jana

    2012-11-01

    This study addresses a current trend in chemical food safety control represented by an effort to integrate analyses of various groups of food contaminants/toxicants into a single, high-throughput method. The choice of optimal sample preparation step is one of the key conditions to achieve good performance characteristics. In this context, we investigated the possibility to expand the scope of the three multi-analyte extraction procedures employed earlier in other studies for rapid isolation of either pesticides or mycotoxins from plant matrices. Following procedures were tested: A - aqueous acetonitrile extraction followed by partition (QuEChERS-like method), B - aqueous acetonitrile extraction, and C - pure acetonitrile extraction. On the list of target analytes, we had 288 pesticides (including 'troublesome' acidic, basic and base-sensitive compounds) together with 38 mycotoxins (including all EU regulated ones and many 'emerging' toxins on the European Food Safety Authority (EFSA) list). The matrices selected for the experiments, apple baby food, wheat flour, spices and sunflower seeds, represented various composition categories in terms of moisture, fat and extractable compounds (e.g. pigments and essential oils) content. In preliminary experiments, acceptable recoveries (70-120%) for most of analytes were obtained by the analysis of spiked matrices, regardless which extraction procedure was used. However, when analysing dry samples with incurred pesticide residues/mycotoxins, the method C did not enable efficient extraction of some common contaminants. Procedure A, thanks to a higher matrix equivalent compared to the method B and relatively less pronounced matrix effects, enabled lower quantification limits for all analyte/matrix combinations, with the exception of polar mycotoxins and/or pesticides. Higher recoveries for the latter group of analytes could be achieved by the method B; on the other hand, extraction efficiency of non-polar pesticides from fatty

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

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

    2013-01-01

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

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

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

    2008-01-01

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

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

    Claudia R. Binder

    2013-03-01

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

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

    Lesmes-Fabian, Camilo; Binder, Claudia R

    2013-03-25

    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.

  17. The E-screen test and the MELN gene-reporter assay used for determination of estrogenic activity in fruits and vegetables in relation to pesticide residues.

    Schilirò, Tiziana; Porfido, Arianna; Longo, Annalisa; Coluccia, Sara; Gilli, Giorgio

    2013-12-01

    Endocrine-disrupting chemicals (EDCs) may lead to adverse systemic effects by interfering with normal hormone homeostasis, and diet is considered to be among the main routes of EDC exposure. The present study investigated the total estrogenic activity of fruits and vegetables by calculating the 17-β-estradiol equivalent quantity (EEQ) using two in vitro tests: the human breast cancer cell line (MCF-7 BUS) proliferation assay (E-screen test) and the luciferase-transfected human breast cancer cell line (MELN) gene-reporter assay. Of the 24 analyzed fruits and vegetables, 14 contained from 1 to 4 pesticide residues in concentrations ranging from 0.02 to 1.19 ppm, whereas the other 10 did not contain any pesticide residues. The EEQ values for all positive samples ranged from 0.010 to 0.616 μg/100g for the above in vitro tests. Our study demonstrates that estrogenic activity was present in fruits and vegetables and that the concentration of allowable pesticide residues and EEQ values were positively correlated; however, no correlation was found by comparing the estrogenic activity and the intrinsic content of phytoestrogens obtained from the available literature. A theoretical adult dietary intake of 0.7-0.9 ng EEQ/L/day from fruits and vegetables was calculated.

  18. Comparative study on maximum residue limits standards of pesticides in peanuts%花生农药最大残留限量标准比对研究

    丁小霞; 李培武; 周海燕; 李娟; 白艺珍

    2011-01-01

    It is important to protect the health of consumers and standardize the agricultural products in trading market. One essential aspect is to develop and implement a standardized scientific and applicable maximum residue limits( MRL) pesticides. A comparative study of maximum residue limits standards of pesticides in peanuts was carried out among China,Codex Alimentarius Commission (CAC) , Unite States, Japan and European Union. Corre-sponding suggestion was put forward after analyzing the problems in maximum residue limit standards of pesticides in China.%制定和实施科学合理的农药最大残留限量标准是保护消费者健康和规范农产品国际贸易的重要手段.对我国、国际食品法典委员会、花生主产国美国以及我国花生主要出口目的国日本和欧盟的花生农药最大残留限量标准进行了系统比较,分析了我国花生农药最大残留限量标准存在的问题,提出了相应的建议.

  19. Method development towards qualitative and semi-quantitative analysis of multiple pesticides from food surfaces and extracts by desorption electrospray ionization mass spectrometry as a preselective tool for food control.

    Gerbig, Stefanie; Stern, Gerold; Brunn, Hubertus E; Düring, Rolf-Alexander; Spengler, Bernhard; Schulz, Sabine

    2017-03-01

    Direct analysis of fruit and vegetable surfaces is an important tool for in situ detection of food contaminants such as pesticides. We tested three different ways to prepare samples for the qualitative desorption electrospray ionization mass spectrometry (DESI-MS) analysis of 32 pesticides found on nine authentic fruits collected from food control. Best recovery rates for topically applied pesticides (88%) were found by analyzing the surface of a glass slide which had been rubbed against the surface of the food. Pesticide concentration in all samples was at or below the maximum residue level allowed. In addition to the high sensitivity of the method for qualitative analysis, quantitative or, at least, semi-quantitative information is needed in food control. We developed a DESI-MS method for the simultaneous determination of linear calibration curves of multiple pesticides of the same chemical class using normalization to one internal standard (ISTD). The method was first optimized for food extracts and subsequently evaluated for the quantification of pesticides in three authentic food extracts. Next, pesticides and the ISTD were applied directly onto food surfaces, and the corresponding calibration curves were obtained. The determination of linear calibration curves was still feasible, as demonstrated for three different food surfaces. This proof-of-principle method was used to simultaneously quantify two pesticides on an authentic sample, showing that the method developed could serve as a fast and simple preselective tool for disclosure of pesticide regulation violations. Graphical Abstract Multiple pesticide residues were detected and quantified in-situ from an authentic set of food items and extracts in a proof of principle study.

  20. Pesticides in Urban Multiunit Dwellings: Hazard IdentificationUsing Classification and Regression Tree (CART) Analysis

    Many units in public housing or other low-income urban dwellings may have elevated pesticide residues, given recurring infestation, but it would be logistically and economically infeasible to sample a large number of units to identify highly exposed households to design interven...

  1. 果蔬汁生产中农药残留控制技术研究进展%Pesticide Residues Control Technology in Fruit and Vegetable Juice Production

    巩蓬勃; 梁宁利; 冯艳芸

    2016-01-01

    农药残留是影响果蔬汁质量的关键问题,本文对果蔬汁中农药残留控制方法研究进展进行追踪。%The pesticide residue is the key problem affecting the quality of fruit and vegetable juice.In this paper, the research progress in pesticide residues in fruit and vegetable juice control method has carried on the track.

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

    冯超; 徐骞; 金玉娥; 卢大胜; 陈冲; 熊丽蓓; 汪国权

    2015-01-01

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

  3. Performance and matrix effect observed in QuEChERS extraction and tandem mass spectrometry analyses of pesticide residues in different target crops.

    Lucini, Luigi; Molinari, Gian Pietro

    2011-10-01

    The method performance and matrix effect related to quantitative determination of pesticide residues was assessed after QuEChERS extraction and LC-MS-MS analysis. Dicloran, phosmet and phosmet-oxon, pirimiphos-methyl, and BNOA were analyzed in peach, apple, melon, cereals, tomato, and strawberry. The matrix effects, as well as recovery and process efficiencies, were determined for a fungicide, two insecticides, and a plant growth regulator. Crop samples were spiked either pre- or post-extraction, then the peak area was compared with the peak area in neat solvent. The mean recovery ranged from 73% to 98%, and repeatability (as RSD) was between 3% and 16%, depending on the compound and spiking level. The matrix effect occurred as ionic suppression and was found in the range of 5% to 22% depending on the compound. Recovery efficiencies were good and substantially comparable, being in the range of 93-96%. Although the suppression observed still appears to be acceptable considering the overall process efficiency, it seems evident that the matrix effect is important when a reliable quantitative method must be applied.

  4. Residual energy applications program systems analysis report

    Yngve, P.W.

    1980-10-01

    Current DOE plans call for building an Energy Applied Systems Test (EAST) Facility at the Savannah River Plant in close proximity to the 140 to 150/sup 0/F waste heat from one of several operating nuclear reactors. The waste water flow from each reactor, approximately 165,000 gpm, provides a unique opportunity to test the performance and operating characteristics of large-scale waste heat power generation and heat pump system concepts. This report provides a preliminary description of the potential end-use market, parametric data on heat pump and the power generation system technology, a preliminary listing of EAST Facility requirements, and an example of an integrated industrial park utilizing the technology to maximize economic pay back. The parametric heat pump analysis concluded that dual-fluid Rankine cycle heat pumps with capacities as high as 400 x 10/sup 6/ Btu/h, can utilize large sources of low temperature residual heat to provide 300/sup 0/F saturatd steam for an industrial park. The before tax return on investment for this concept is 36.2%. The analysis also concluded that smaller modular heat pumps could fulfill the same objective while sacrificing only a moderate rate of return. The parametric power generation analysis concluded that multi-pressure Rankine cycle systems not only are superior to single pressure systems, but can also be developed for large systems (approx. = 17 MW/sub e/). This same technology is applicable to smaller systems at the sacrifice of higher investment per unit output.

  5. Application of Liquid Phase Microextraction in the Determination of Pesticide Residues%液相微萃取在农药残留物检测中的应用

    熊玉宝; 张勇; 廖春华; 邱清权

    2011-01-01

    Pesticide residues were at a very low level. They also coexisted with their homologs. isomers, degradation products and metabolites etc. Pretreatment technologies of pesticide residues were the key of their analysis and detection.As a new pretreatment technology,liquid phase microextraction technology played an important role in sample preparation. Herein we would introduce three liquid phase microextraction technologies: hollow fiber liquid phase microextraction technology, head space liquid phase microextraction technology and dispersed liquid phase microextraction technology. These three kinds of technologies were compared, and their applications in pesticide residues detection being recommended. And the prospects of liquid phase microextraction technology were predicted.%残留农药的含量极低,而且还与其同系物、异构体、降解产物、代谢产物等共存.农药残留前处理技术成为农药残留分析检测中的关键.作为一种新型的样品前处理技术,液相微萃取技术扮演着重要的角色.文章将介绍3种液相微萃取技术:中空纤维液相微萃取技术、顶空液相微萃取技术和分散液相微萃取技术,对这3种技术进行了比较,重点介绍了它们在农药残留物检测中的应用,并对液相微萃取技术的发展前景予以展望.

  6. 泉州地区蔬菜农药残留现状分析%Status of pesticide residues in vegetables of Quanzhou

    许梅燕; 蔡胜茂; 高铭琪

    2015-01-01

    According to enzyme inhibition rate,480 vegetable samples randomly selected from 12 counties( city or district) of Quanzhou were detected for monitoring the pesticide residues. The results showed that the qualification rate of the vegeta-ble pesticide residue in Quanzhou was 97. 5% in the second half year of 2014,and the over-standard rate was 2. 5%. The leave vegetables were more severe in pesticide residues. The main kinds caused over-standard of pesticide residues in vegeta-bles were Methamidophos,Parathion-methyl,Isocarbophos,Folimat,and Chlorpyrifos,among which,Methamidophos and Folimat showed dozens of times of over standard rate,and two or three hundred times of over standard rate occurred in Para-thion-methyl. Aiming at the over standard of pesticide residues in vegetables,the main reason was discussed,and the corre-sponding control measures were put forward.%于2014年下半年,采用酶抑制率法对泉州12个县(市、区)随机抽取480个蔬菜样品进行农药残留情况检测,结果表明:泉州地区蔬菜农药残留抽样检测合格率为97.5%,超标率为2.5%;农药残留超标比较严重的蔬菜种类为叶菜类;造成蔬菜农药残留超标的几种农药主要是甲胺磷、甲基对硫磷、水胺硫磷、氧化乐果、毒死蜱,其中甲基对硫磷、甲胺磷和氧化乐果严重超标。针对蔬菜中农药超标问题原因进行分析,并提出相应的对策。

  7. [Determination of 51 carbamate pesticide residues in vegetables by liquid chromatography-tandem mass spectrometry based on optimization of QuEChERS sample preparation method].

    Wang, Lianzhu; Zhou, Yu; Huang, Xiaoyan; Wang, Ruilong; Lin, Zixu; Chen, Yong; Wang, Dengfei; Lin, Dejuan; Xu, Dunming

    2013-12-01

    The raw extracts of six vegetables (tomato, green bean, shallot, broccoli, ginger and carrot) were analyzed using gas chromatography-mass spectrometry (GC-MS) in full scan mode combined with NIST library search to confirm main matrix compounds. The effects of cleanup and adsorption mechanisms of primary secondary amine (PSA) , octadecylsilane (C18) and PSA + C18 on co-extractives were studied by the weight of evaporation residue for extracts before and after cleanup. The suitability of the two versions of QuEChERS method for sample preparation was evaluated for the extraction of 51 carbamate pesticides in the six vegetables. One of the QuEChERS methods was the original un-buffered method published in 2003, and the other was AOAC Official Method 2007.01 using acetate buffer. As a result, the best effects were obtained from using the combination of C18 and PSA for extract cleanup in vegetables. The acetate-buffered version was suitable for the determination of all pesticides except dioxacarb. Un-buffered QuEChERS method gave satisfactory results for determining dioxacarb. Based on these results, the suitable QuEChERS sample preparation method and liquid chromatography-positive electrospray ionization-tandem mass spectrometry under the optimized conditions were applied to determine the 51 carbamate pesticide residues in six vegetables. The analytes were quantified by matrix-matched standard solution. The recoveries at three levels of 10, 20 and 100 microg/kg spiked in six vegetables ranged from 58.4% to 126% with the relative standard deviations of 3.3%-26%. The limits of quantification (LOQ, S/N > or = 10) were 0.2-10 microg/kg except that the LOQs of cartap and thiofanox were 50 microg/kg. The method is highly efficient, sensitive and suitable for monitoring the 51 carbamate pesticide residues in vegetables.

  8. Residues of organophosphate pesticides used in vegetable cultivation in ambient air, surface water and soil in Bueng Niam Subdistrict, Khon Kaen, Thailand.

    Harnpicharnchai, Kallaya; Chaiear, Naesinee; Charerntanyarak, Lertchai

    2013-11-01

    Agricultural pesticide utilization is one of the important problems in rural and urban crop-cultivated areas, with the majority of pollutants dispersing via ambient air, water and other natural pathways. This study was therefore conducted in a specially selected village which is known to be a leading vegetable growing area in Khon Kaen Province. The aim of the study was to assess pesticide residues, and measure the seasonal fluctuations in organophosphate concentrations during 2010 in the environment of a risk area. Samples from selected sites were collected in two phases: Phase I was in summer (during March to May) and Phase II was in winter (during October to December). A total of 150 samples were analyzed using gas chromatography with flame photometric detection. The results showed that dicrotophos, chlorpyrifos, profenofos and ethion were found at the highest concentrations in soil and at the lowest concentrations in ambient air (pwater samples, the highest mean concentration of a pesticide was 1.3757 +/- 0.5014 mg/l for dicrotophos in summer and 0.3629 +/- 0.4338 mg/l for ethion in winter. The highest mean concentration of a pesticide in soil samples was 42.2893 +/- 39.0711 mg/kg ethion in summer and 90.0000 +/- 24.1644 mg/kg of ethion in winter.

  9. Research progress on storage stability of pesticide residues%农药残留储存稳定性的研究进展

    卞艳丽; 刘丰茂

    2016-01-01

    农药残留检测对农产品安全、食品卫生有十分重要的意义。残留试验样品运送到实验室后,需要根据农药的性质以及样品类型确定储存条件和储存时间,保证在储存期内待测物的性质和含量不发生变化,确保分析结果的可靠性和科学性。国内关于农药残留储存稳定性研究的规定和储存稳定性影响机制的研究较少,而国外相关机构均对农药残留储存稳定性做了详细的规定和要求。本文综述了美国环境保护署(United States Environmental Protection Agency, EPA)、经济合作与发展组织(Organization for Economic Cooperation and Development, OECD)及联合国粮食及农业组织(Food and Agriculture Organization, FAO)等机构对农药残留储存稳定性操作指南、不同样品基质中农药残留储存稳定性研究进展和农药残留储存稳定性的影响因素,并对分析样品的储存提出了建议,以期为农药残留储存稳定性的深入研究提供参考和借鉴。%Pesticide residue analysis has great significance for agricultural products’ safety and hygiene. Experimenters should determine storage conditions according to the nature of the pesticides and the type of samples, so as to ensure that the content of analytes do not change during the storage period and the results are reliable and scientific. The domestic provisions seldom conduct the research on storage stability of pesticide residues and its influence mechanism, while abroad institutions have regulations and requirements for storage stability in detail. This review summarized the operation guide for storage stability, research progress of different samples storage stability and factors which influenced the storage stability of the United States Environmental Protection Agency (EPA), Organization for Economic Cooperation and Development (OECD) and Food and Agriculture Organization (FAO), meanwhile how to store the samples was suggested, in order to provide

  10. Research progress on storage stability of pesticide residues%农药残留储存稳定性的研究进展

    卞艳丽; 刘丰茂

    2016-01-01

    农药残留检测对农产品安全、食品卫生有十分重要的意义。残留试验样品运送到实验室后,需要根据农药的性质以及样品类型确定储存条件和储存时间,保证在储存期内待测物的性质和含量不发生变化,确保分析结果的可靠性和科学性。国内关于农药残留储存稳定性研究的规定和储存稳定性影响机制的研究较少,而国外相关机构均对农药残留储存稳定性做了详细的规定和要求。本文综述了美国环境保护署(United States Environmental Protection Agency, EPA)、经济合作与发展组织(Organization for Economic Cooperation and Development, OECD)及联合国粮食及农业组织(Food and Agriculture Organization, FAO)等机构对农药残留储存稳定性操作指南、不同样品基质中农药残留储存稳定性研究进展和农药残留储存稳定性的影响因素,并对分析样品的储存提出了建议,以期为农药残留储存稳定性的深入研究提供参考和借鉴。%ABSTRACT:Pesticide residue analysis has great significance for agricultural products’ safety and hygiene. Experimenters should determine storage conditions according to the nature of the pesticides and the type of samples, so as to ensure that the content of analytes do not change during the storage period and the results are reliable and scientific. The domestic provisions seldom conduct the research on storage stability of pesticide residues and its influence mechanism, while abroad institutions have regulations and requirements for storage stability in detail. This review summarized the operation guide for storage stability, research progress of different samples storage stability and factors which influenced the storage stability of the United States Environmental Protection Agency (EPA), Organization for Economic Cooperation and Development (OECD) and Food and Agriculture Organization (FAO), meanwhile how to store the samples was suggested, in order to

  11. Pesticides for apicultural and/or agricultural application found in Belgian honey bee wax combs.

    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.

  12. 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 NPDES...

  13. Estimation of the uncertainty in a multiresidue method for the determination of pesticide residues in fruit and vegetables

    Christensen, Hanne Bjerre; Poulsen, Mette Erecius; Pedersen, Mikael

    2003-01-01

    . In the present study, recommendations from the International Organisation for Standardisation's (ISO) Guide to the Expression of Uncertainty and the EURACHEM/CITAC guide Quantifying Uncertainty in Analytical Measurements were followed to estimate the expanded uncertainties for 153 pesticides in fruit......The estimation of uncertainty of an analytical result has become important in analytical chemistry. It is especially difficult to determine uncertainties for multiresidue methods, e.g. for pesticides in fruit and vegetables, as the varieties of pesticide/commodity combinations are many...

  14. Rotenone and paraquat perturb dopamine metabolism: A computational analysis of pesticide toxicity.

    Qi, Zhen; Miller, Gary W; Voit, Eberhard O

    2014-01-06

    Pesticides, such as rotenone and paraquat, are suspected in the pathogenesis of Parkinson's disease (PD), whose hallmark is the progressive loss of dopaminergic neurons in the substantia nigra pars compacta. Thus, compounds expected to play a role in the pathogenesis of PD will likely impact the function of dopaminergic neurons. To explore the relationship between pesticide exposure and dopaminergic toxicity, we developed a custom-tailored mathematical model of dopamine metabolism and utilized it to infer potential mechanisms underlying the toxicity of rotenone and paraquat, asking how these pesticides perturb specific processes. We performed two types of analyses, which are conceptually different and complement each other. The first analysis, a purely algebraic reverse engineering approach, analytically and deterministically computes the altered profile of enzyme activities that characterize the effects of a pesticide. The second method consists of large-scale Monte Carlo simulations that statistically reveal possible mechanisms of pesticides. The results from the reverse engineering approach show that rotenone and paraquat exposures lead to distinctly different flux perturbations. Rotenone seems to affect all fluxes associated with dopamine compartmentalization, whereas paraquat exposure perturbs fluxes associated with dopamine and its breakdown metabolites. The statistical results of the Monte-Carlo analysis suggest several specific mechanisms. The findings are interesting, because no a priori assumptions are made regarding specific pesticide actions, and all parameters characterizing the processes in the dopamine model are treated in an unbiased manner. Our results show how approaches from computational systems biology can help identify mechanisms underlying the toxicity of pesticide exposure.

  15. Comparison of sample preparation methods combined with gas chromatography with electron-capture detection for the analysis of multipesticide residues in lotus seeds.

    Miao, Qing; Kong, Weijun; Yang, Shihai; Yang, Meihua

    2013-06-01

    Sample preparation is always the major bottleneck in analytical chemistry for the determination of pesticide residues. Different sample preparation methods have been proposed due to the wide variety of pesticides used and the inherent complexity of the matrices. In this study, different sample preparation methods including SPE, matrix solid-phase dispersion, the quick, easy, cheap, efficient, rugged, and safe method, and a one-step completion method were compared and evaluated for extracting pesticides from lotus seeds. Analysis was carried out using GC with electron-capture detection. The results showed that good recoveries for tested pesticides were obtained by using Florisil in the four methods, and the extraction efficiency of the one-step completion method was superior to the other three methods. The one-step completion method was confirmed to have good linearity, reproducibility, stability, and recovery for the detection of 36 pesticides in lotus seed samples. The data collected from this study are expected to prove useful in regulating the concentration of the residues in lotus seeds, as well as in protecting human health from the hazards posed by these residues.

  16. Evaluation of alternative sorbents for dispersive solid-phase extraction clean-up in the QuEChERS method for the determination of pesticide residues in rice by liquid chromatography with tandem mass spectrometry.

    Cabrera, Liziara da C; Caldas, Sergiane S; Prestes, Osmar D; Primel, Ednei G; Zanella, Renato

    2016-05-01

    Many compounds are used for pest control during the production and storage of rice, making it necessary to employ multiclass methods for pesticide residues determination. For this purpose, QuEChERS-based methods are very efficient, fast and accurate, and improvements in the clean-up step are important, especially for complex matrices, like cereals. In this work, different sorbents such as chitosan, florisil(®) , alumina, diatomaceous earth, graphitized carbon black, besides the commonly used primary secondary amine and octadecylsilane, were evaluated for dispersive solid-phase extraction clean-up in acetate-buffered QuEChERS method for the determination of residues of 20 representative pesticides and one metabolite in rice by liquid chromatography coupled to tandem mass spectrometry. The sorbent C18 presented the best results, however, chitosan showed similar results, and the best performance among the unconventional sorbents evaluated. The method limit of quantification, attending accuracy (70-120% recovery) and precision (RSD ≤20%) criteria, ranged from 5 to 20 μg/kg. Results showed that chitosan is an effective alternative to reduce analysis costs, maintaining the method reliability and accuracy.

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

    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.

  18. GC -FPD 法分析检测人参中4种有机磷农药残留%Determination of Four Organophosphorus Pesticides Residue in Ginseng by GC -FPD

    罗婧; 王玉方; 金春爱; 王峰; 刘继永; 商云帅; 何艳丽

    2013-01-01

    An analytical method for determining four organophosphorus pesticides Monocrotophos ,Dimethoate ,Malathion and Parathion residues in ginseng by GC was described .The samples were extracted with ethyl acetate ,detected by GC with FPD detector .The results showed that the linear range of four organophosphorus pesticides were from 0.02 to 5mg/L ,the correlation coefficients were 0.999 6 to 0.999 9;the minimum detectable concentration of the 4 analytes in ginseng samples were all 0.01mg/kg;average recoveries were 80.9 to 98.9% ,and the coefficient of variation ranged from 2.53 to 6.78% .The proposed method was applied to the determination of four organophosphorus pesticide residue in dried raw ginseng from market .The results of test have met the requirement of pesticide residue analysis .%建立了同时测定人参中久效磷、乐果、马拉硫磷和对硫磷4种有机磷农药残留气相色谱分析方法。以乙酸乙酯进行超声及振荡提取,用气相色谱火焰光度检测器测定。结果表明,久效磷、乐果、马拉硫磷和对硫磷4种有机磷农药的线性范围为0.02~5mg/L ,相关系数 r为0.9996~0.9999。4种有机磷农药在人参中的最低检测浓度均为0.01mg/kg ,平均回收率为80.9%~98.9%,变异系数为2.53%~6.78%,并应用该方法测定了市场上5个生晒参样品中这4种有机磷农药的残留量,符合农药残留测定要求。

  19. Pesticide exposure and risk of Alzheimer’s disease: a systematic review and meta-analysis

    Yan, Dandan; Zhang, Yunjian; Liu, Liegang; Yan, Hong

    2016-09-01

    Evidence suggests that lifelong cumulative exposure to pesticides may generate lasting toxic effects on the central nervous system and contribute to the development of Alzheimer’s disease (AD). A number of reports indicate a potential association between long-term/low-dose pesticide exposure and AD, but the results are inconsistent. Therefore, we conducted a meta-analysis to clarify this association. Relevant studies were identified according to inclusion criteria. Summary odds ratios (ORs) were calculated using fixed-effects models. A total of seven studies were included in our meta-analysis. A positive association was observed between pesticide exposure and AD (OR = 1.34 95% confidence interval [CI] = 1.08, 1.67; n = 7). The summary ORs with 95% CIs from the crude and adjusted effect size studies were 1.14 (95% CI = 0.94, 1.38; n = 7) and 1.37 (95% CI = 1.09, 1.71; n = 5), respectively. The sensitivity analyses of the present meta-analysis did not substantially modify the association between pesticide exposure and AD. Subgroup analyses revealed that high-quality studies tended to show significant relationships. The present meta-analysis suggested a positive association between pesticide exposure and AD, confirming the hypothesis that pesticide exposure is a risk factor for AD. Further high-quality cohort and case-control studies are required to validate a causal relationship.

  20. The Research Progress of Degradation Method for Organophosphorus Pesticide Residues from Vegetables%蔬菜中有机磷农药残留降解方法的研究进展

    何迪; 李明浩; 李晓东

    2012-01-01

    At present,organophosphorus pesticide is one of the most widely used chemical pesticides and mainly applied in vegetables. Organophosphorus pesticide residues brought serious threat to human health. Degradation methods for organophosphorus pesticide residues mainly include physical degradation,chemical degradation and biodegradation,during which biodegradation has the most widely application prospect.%目前有机磷农药是应用最为广泛的化学农药之一,蔬菜是其主要作用对象,有机磷农药带来的药残严重威胁人类的健康.对于有机磷药残的降解方法主要有物理降解、化学降解和生物降解,其中生物降解法是应用前景最为广泛的降解方法之一.

  1. 基于酶抑制法的农药残留快速比色检测%Rapid colormetric detection of pesticide residues based on enzyme inhibition method

    朱松明; 周晨楠; 和劲松; 张雪吟; 郭希山

    2014-01-01

    基于有机磷与氨基甲酸酯类农药对乙酰胆碱酯酶(acetylcholinesterase,AChE)的抑制作用,以吲哚酚乙酸酯为酶促水解反应的显色底物,制备了一种抛弃型农药残留快速检测酶片;通过优化试验,用物理吸附法将AChE固定到尼龙膜Hybond N+膜上,经真空冷冻干燥后,酶活回收率可达27.3%;该酶片显色结果为蓝绿色,通过比较显色强度的变化,酶片对农药标样氧乐果、毒死蜱、甲萘威与抗蚜威的检出限分别为1、0.05、1.5与0.8μg/mL,均达到食品中的最大残留限量标准;将研制的酶片用于葡萄汁与小白菜样品的检测结果证实,该酶片具有灵敏度高、准确度高、重现性好等优点,可用于农产品中有机磷与氨基甲酸酯类农药残留的快速定性筛检。%In recent years, due to the frequently reported food safety events, people generally care about the food safety. According to former research, the application amount of organophosphorus pesticides and carbamate pesticides possesses about 70% of the total application amount of pesticides. So, it is necessary to develop fast, sensitive and accurate analysis of pesticide residues to assure the quality of agricultural products. However, the existing food quality supervision system is generally based on the instrument analysis technology, which is time-consuming and high-costing, and will delay the actual release of information for the food safety determination. So it cannot provide the rapid response to the consumer queries. Therefore, there is an urgent need to develop the rapid detection techniques for food safety. A novel disposable enzyme tablet was developed for rapid colorimetric detection of pesticide residues in agricultural products, which based on the inhibition of acetylcholinesterase (AChE) activity by pesticides and the AChE-catalyzed hydrolysis of chromogenic substrate, indoxyl acetate. As known, indoxyl acetate can be catalyzed to

  2. 转基因和农药残留与食品安全的关系%The Relationship between Transgenic and Pesticide Residues and Food Safety

    周少榕

    2016-01-01

    With the development of the times, people's production technology continues to improve, in order to increase crop output per unit area, the transgenic technology and a variety of pesticides were applicated in the production process. Nobody can question the use of transgenic technology and to some extent pesticides could increase crop yields, but food safety issues attendant but also allow people to fear. Based on this, this paper discussed the relationship between pesticide residues and food safety, and food safety of transgenic relationship, hoping to provide assistance to stakeholders.%随着时代的发展,人们的生产技术不断提升,为了增加单位面积上的农作物产值,人们在生产过程中应用了转基因技术及各种各样的农药。谁也不能质疑,转基因技术及农药的使用在一定程度上增加了作物的产量,但随之而来的食品安全问题却也让人们心有余悸。鉴于此,分别讨论转基因和食品安全的关系、农药残留与食品安全的关系,希望能够为相关人士提供帮助。

  3. Probabilistic risk assessment of dietary exposure to single and multiple pesticide residues or contaminants: summary of the work performed within the SAFE FOODS project.

    van Klaveren, Jacob D; Boon, Polly E

    2009-12-01

    This introduction to the journal's supplement on probabilistic risk assessment of single and multiple exposure to pesticide residues or contaminants summarizes the objectives and results of the work performed in work package 3 of the EU-funded project SAFE FOODS. Within this work package, we developed an electronic platform of food consumption and chemical concentration databases harmonised at raw agricultural commodity level. In this platform the databases are connected to probabilistic software to allow probabilistic modelling of dietary exposure in a standardised way. The usefulness of this platform is demonstrated in two papers, which describe the exposure to pesticides and glycoalkaloids in several European countries. Furthermore, an integrated probabilistic risk assessment (IPRA) model was developed: a new tool to integrate exposure and effect modelling, including uncertainty analyses. The use of this model was shown in a paper on the cumulative exposure to anti-androgen pesticides. Combined with a health impact prioritization system, developed within this work package to compare heath risks between chemicals, the IPRA tool can also be used to compare health risks between multiple chemicals in complex risk assessment situation such as risk-benefit and risk trade-off analyses. Both the electronic platform of databases as the IPRA model may proof to be powerful tools to tackle the challenges risk managers are or will be faced with in the future.

  4. 40 CFR 180.239 - Phosphamidon; tolerances for residues.

    2010-07-01

    ...) PESTICIDE PROGRAMS TOLERANCES AND EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Specific Tolerances... residues of the insecticide phosphamidon (2-chloro-2-diethylcarbamoyl-1-methylvinyl dimethyl...

  5. 姬松茸60Co辐射新菌株J3营养成分与农药残留分析%Analysis on Nutrients and Pesticide Residues in Strain J3 Agaricus blazei Murill Irradiated by 60Co

    翁伯琦; 江枝和; 肖淑霞; 雷锦桂; 王义祥; 唐翔虬

    2011-01-01

    通过常规生产床栽,对比研究姬松茸Co辐射新菌株J和原菌株J在营养品质以及重金属含量和农药残留情况.结果表明,姬松茸Co辐射新菌株J子实体中鲜味氨基酸总量(56.5 g·kg)、甜味氨基酸总量(52.4g·kg)、硫氨基酸总量(15.8 g·kg)、支链氨基酸总量(38.1 g·kg)、芳香族氨基酸总量(16.1 g·kg)、儿童氨基酸总量(17.8 g·kg)、必需氨基酸总量(95 g·kg),分别占氨基酸总量(221.7 g·kg)的25.48%、23.64%、7.13%、17.19%、7.26%、8.03%和42.85%,分别比姬松茸J高28.12%、12.93%、0%、14.41%、12.59%、16.34%和11.76%.J的多不饱和脂肪酸(76.15%)和不饱和脂肪酸(77.55%)分别比姬松茸原菌株J高4.39%和3.82%.J子实体含镉(3.86 mg·kg)、汞(0.42 mg·kg)和砷(0.09 mg·kg),也分别比原菌株J低45.86%、32.25%和18.18%;其铅含量符合国家食用菌卫生标准GB 7096-2003;砷含量符合国家绿色食品食用菌NY/T749-2003的标准.子实体中联苯菊酯、溴氰菊酯、百菌清、六六六、多菌灵、阿维菌素、甲基托布津、甲胺磷、毒死蜱、滴滴涕和二氧化硫含量均符合国家绿色食品食用菌NY/T 749-2003的标准.%A garicus blazei Murill as rare edible fungi was adored by more and more customers.But with the increasing attention of food hygiene quality, it was important guidance of the safety production of Agaricus blazei to understand the health status of Agaricus blazei in the actual cultivation.This paper studied the difference in terms of nutritional quality, heavy metal contents and pesticide residues between strain J3 and J1.The results showed that the contents of delicious amino acid(56.5 g· kg-1), sweet amino acid(52.4 g· kg-1), sulfur amino acid( 15.8 g·kg-1), branched chain amino acid(38.1 g· kg-1), aromatic amino acid( 16.1 g·kg-1), children amino acid( 17.8 g·kg-1), necessary amino acid (95.0 g·kg-1)in the fruit bodies ofAgaricus blazei J3, occupied 25.48%, 23.64%, 7.13%, 17.19%, 7.26

  6. Accurate-mass databases for comprehensive screening of pesticide residues in food by fast liquid chromatography time-of-flight mass spectrometry.

    Mezcua, Milagros; Malato, Octavio; García-Reyes, Juan F; Molina-Díaz, Antonio; Fernández-Alba, Amadeo R

    2009-02-01

    Because of the international trade of fruits and vegetables and the lack of harmonized regulations on the use of pesticides worldwide, the development of comprehensive screening methods for analyzing hundreds of pesticides and other banned chemicals is very convenient. This work reports the development and evaluation of a rapid automated screening method for determining pesticide residues in food using liquid chromatography electrospray time-of-flight mass spectrometry (LC-TOFMS) based on the use of an accurate-mass database. The database created includes data not only on the accurate masses of the target ions but also the characteristic in-source fragment ions (over 400 fragments included) and retention time data. This customized database was associated to commercially available software which extracted all the potential compounds of interest from the LC-TOFMS raw data of each sample and matched them against the database to search for targeted compounds in the sample. This automatic screening method requires a careful optimization of the accurate-mass window and retention time tolerances, which play a determinant role on the selectivity, accuracy, and throughput of the whole procedure. Values of 10 mDa for preliminary screening and 1 mDa/5 ppm for confirmation along with a +/-0.15 min retention time window were found to be optimum for the compounds and samples tested. The optimized methods enable the automated screening of ca. 300 compounds in less than 20 min including the LC-MS run and data processing. The proposed method was applied to 60 real samples, and the results of the positive findings compared well with those obtained using a liquid chromatography tandem mass spectrometry (LC-MS/MS) method (triple quadrupole). The rates obtained on the identification of compounds in spiked and real samples in an automated fashion at different concentration levels were over 95% of the compounds, thus revealing as a convenient tool for the large-scale screening of

  7. 2012年绵阳市蔬菜中农药残留状况%Pesticide residues in vegetables in Mianyang City in 2012

    何玲玲; 罗赟; 张代友; 吴晓红

    2013-01-01

    [Objective] To investigate the conditions of pesticide residues in vegetables in Mianyang City,and provide evidence for edible vegetables supervision.[Methods] The method of GB/T 5009-2003 was applied to determine the contents of pesticide in samples selected,the results were evaluated according to GB 2763-2005" Maximum residue limits for pesticides in food".[Results] A total of 165 vegetable samples were detected in 2012,the detection rate and the unqualified rate were 72.12% and 23.64%.The unqualified rate of leguminous,root-steam,leaf,melon vegetables and edible fungi vegetables was 8.00%,23.53%,36.00%,5.26% and 27.03%,respectively,with significant difference (x2 =11.41,P <0.01).There was no difference between pesticide residues in summer and winter(x2 =3.44,P > 0.05).[Conclusion] In Mianyang City,pesticide residues are relatively serious in the leaf vegetables.It is necessary to adopt effective measures to enhance the inspection and administration,to ban the use of highly toxic pesticides from the source,to strengthen monitoring of vegetable cultivation and marketing chain sas as to ensure the safety of the public consumption of vegetables%目的 了解绵阳市2012年市售蔬菜中农药残留情况,为食用蔬菜监管提供依据.方法 全部样品均按照GB/T 5009-2003的方法进行农药的残留检测.依据GB 2763-2005《食品中农药最大残留限量》进行判定.结果 2012年共检测蔬菜165份,农药检出率和超标率分别为72.12%和23.64%.豆类、根茎类、叶菜类、瓜果菜类和食用菌类蔬菜检测农药残留超标率分别为8.00%、23.53%、36.00%、5.26%和27.03%,差异有统计学意义(x2=11.41,P<0.01).不同种类农药超标率差异有统计学意义(x2 =62.42,P<0.01).夏季和冬季蔬菜农药超标率差异无统计学意义(x2=3.44,P>0.05).结论 绵阳市叶菜类蔬菜中农药残留情况较为严重,应采取有效措施,加强蔬菜的监督管理,从源头禁止

  8. Analysis of Food Contaminants, Residues, and Chemical Constituents of Concern

    Ismail, Baraem; Reuhs, Bradley L.; Nielsen, S. Suzanne

    The food chain that starts with farmers and ends with consumers can be complex, involving multiple stages of production and distribution (planting, harvesting, breeding, transporting, storing, importing, processing, packaging, distributing to retail markets, and shelf storing) (Fig. 18.1). Various practices can be employed at each stage in the food chain, which may include pesticide treatment, agricultural bioengineering, veterinary drug administration, environmental and storage conditions, processing applications, economic gain practices, use of food additives, choice of packaging material, etc. Each of these practices can play a major role in food quality and safety, due to the possibility of contamination with or introduction (intentionally and nonintentionally) of hazardous substances or constituents. Legislation and regulation to ensure food quality and safety are in place and continue to develop to protect the stakeholders, namely farmers, consumers, and industry. [Refer to reference (1) for information on regulations of food contaminants and residues.

  9. Determination of farm workers' exposure to pesticides by hair analysis.

    Schummer, Claude; Salquèbre, Guillaume; Briand, Olivier; Millet, Maurice; Appenzeller, Brice M R

    2012-04-25

    In the present work, a highly sensitive method based on solid phase microextraction and gas chromatography tandem (triple quadrupole) mass spectrometry was used to test hair samples for 50 pesticides including 39 molecules from different chemical families currently used in agriculture and 11 organochlorines. The population investigated was composed of 18 farm workers who provided hair samples repeatedly collected during the entire treatment period (from March to November 2009). Among the 62 hair samples that were collected, 33 different target molecules were detected. The most frequently detected agricultural pesticides were Diflufenican and Pyrimethanil, two herbicides which were detected in 13 subjects. The concentration in volunteers' hair matched with agricultural activity and the highest concentration was observed for Cyprodinil (1161pg/mg), an anilinopyrimidine used as a fungicide. For organochlorines, p,p'-DDE and γ-HCH were the most frequently detected molecules as they were present in at least one of the hair samples provided by each of the 18 volunteers. The highest concentrations detected for these chemicals reached 21.0pg/mg for p,p'-DDE and 23.5pg/mg for γ-HCH, but the highest concentration of organochlorine was observed for β-endosulfan (105pg/mg). The results suggest that farm workers have a weak, though constant exposure to organochlorine pesticides, especially to p,p'-DDE and γ-HCH, while exposure to currently used pesticides is strongly associated with occupation. Observations also suggest that spraying work would not necessarily be the only source of exposure to agricultural pesticides and that worker not directly involved in spraying can also be submitted to significant level of exposure.

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

    Rada Đurović

    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 μg/kg of each pesticide were below 8%and higher than 89%, respectively. Limits of detection (LOD for all the compounds studiedwere less than 4 μg/kg.

  11. A novel polythiophene – ionic liquid modified clay composite solid phase microextraction fiber: Preparation, characterization and application to pesticide analysis

    Pelit, Füsun Okçu, E-mail: fusun.okcu@ege.edu.tr; Pelit, Levent; Dizdaş, Tuğberk Nail; Aftafa, Can; Ertaş, Hasan; Yalçınkaya, E.E.; Türkmen, Hayati; Ertaş, F.N.

    2015-02-15

    Highlights: • A novel polythiophene – ionic liquid modified clay surface has been prepared. • Polymerization was performed electrochemically on a stainless steel wire. • This material was used as a SPME fiber in head space mode. • This new SPME fiber was applied for analysis of pesticides in juice samples. • Fiber adsorption properties were improved by modification of ionic liquids. - Abstract: This report comprises the novel usage of polythiophene – ionic liquid modified clay surfaces for solid phase microextraction (SPME) fiber production to improve the analysis of pesticides in fruit juice samples. Montmorillonite (Mmt) clay intercalated with ionic liquids (IL) was co-deposited with polythiophene (PTh) polymer coated electrochemically on an SPME fiber. The surface of the fibers were characterized by using scanning electron microscopy (SEM). Operational parameters effecting the extraction efficiency namely; the sample volume and pH, adsorption temperature and time, desorption temperature and time, stirring rate and salt amount were optimized. In order to reveal the major effects, these eight factors were selected and Plackett–Burman Design was constructed. The significant parameters detected; adsorption and temperature along with the stirring rate, were further investigated by Box–Behnken design. Under optimized conditions, calibration graphs were plotted and detection limits were calculated in the range of 0.002–0.667 ng mL{sup −1}. Relative standard deviations were no higher than 18%. Overall results have indicated that this novel PTh-IL-Mmt SPME surface developed by the aid of electrochemical deposition could offer a selective and sensitive head space analysis for the selected pesticide residues.

  12. Longitudinal study of pesticide residue levels in human milk from Western Australia during 12 months of lactation: Exposure assessment for infants

    Du, Jian; Gridneva, Zoya; Gay, Melvin C. L.; Lai, Ching T.; Trengove, Robert D.; Hartmann, Peter E.; Geddes, Donna T.

    2016-12-01

    The presence of pesticides in human milk (HM) is of great concern due to the potential health effects for the breastfed infant. To determine the relationships between HM pesticides and infant growth and development, a longitudinal study was conducted. HM samples (n = 99) from 16 mothers were collected at 2, 5, 9 and 12 months of lactation. A validated QuEChERS method and Gas chromatography-tandem mass spectrometry (GC-MS/MS) were used for the analysis of 88 pesticides in HM. Only p,p’-DDE, p,p’-DDT and β-HCH were detected with a mean concentration (±SD) of 52.25 ± 49.88 ng/g fat, 27.67 ± 20.96 ng/g fat and 48.00 ± 22.46 ng/g fat respectively. The concentrations of the detected pesticides decreased significantly throughout the first year of lactation. No significant relationships between HM p,p’-DDE and infant growth outcomes: weight, length, head circumference and percentage fat mass were detected. The actual daily intake (ADI) of total DDTs in this cohort was 14-1000 times lower than the threshold reference and significantly lower than the estimated daily intake (EDI). Further, the ADI decreased significantly throughout the first 12 months of lactation.

  13. Evaluation of relevant time-of-flight-MS parameters used in HPLC/MS full-scan screening methods for pesticide residues.

    Mezcua, Milagros; Malato, Octavio; Martinez-Uroz, Maria Angeles; Lozano, Ana; Agüera, Ana; Fernández-Alba, Amadeo R

    2011-01-01

    An automatic screening method based on HPLC/time-of-flight (TOF)-MS (full scan) was used for the analysis of 103 non-European fruit and vegetable samples after extraction by the quick, easy, cheap, effective, rugged, and safe method. The screening method uses a database that includes 300 pesticides, their fragments, and isotopical signals (910 ions) that identified 210 pesticides in 78 positive samples, with the highest number of detection being nine pesticides/sample. The concentrations of 97 pesticides were 100 microg/kg. Several parameters of the automatic screening method were carefully studied to avoid false positives and negatives in the studied samples; these included peak filter (number of chromatographic peak counts) and search criteria (retention time and error window). These parameters were affected by differences in mass accuracy and sensitivity of the two HPLC/TOF-MS systems used with different resolution powers (15 000 and 7500), the capabilities of which for resolving the ions included in the database from the matrix ions were studied in four matrixes, viz., pepper, rice, garlic, and cauliflower. Both of these mass resolutions were found to be satisfactory to resolve interferences from the signals of interest in the studied matrixes.

  14. 75 FR 53690 - Notice of Receipt of Pesticide Petition Filed for Residues of Potassium Peroxymonosulfate in or...

    2010-09-01

    ... files should avoid the use of special characters, any form of encryption, and be free of any defects or..., Antimicrobials Division (7510P), Office of Pesticide Programs, Environmental Protection Agency, 1200 Pennsylvania...: Crop production (NAICS code 111). Animal production (NAICS code 112). Food manufacturing (NAICS...

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

    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.

  16. Ionic liquid mediated sol-gel sorbents for hollow fiber solid-phase microextraction of pesticide residues in water and hair samples.

    Ebrahimi, Mahmoud; Es'haghi, Zarrin; Samadi, Fatemeh; Hosseini, Mohammad-Saeid

    2011-11-18

    An ionic liquid mediated sol-gel sorbents for hollow fiber solid-phase microextraction (HF-SPME) was developed for extraction of the pesticides: diazinon, fenitrothion, malathion, fenvalerate, phosalone and tridemorph from human hair and water samples. The analytes were subsequently analyzed with high performance liquid chromatography and diode array detection (HPLC-DAD). Preliminary experiments were carried out in order to study experimental conditions for pesticides' extraction from spiked hair and water samples with HF-SPME using hollow fiber-supported ionic liquid mediated sol-gel sorbent. The sol-gel nanocomposites were reinforced with nanoparticles such as carboxylic functionalized multi-walled carbon nanotubes (COOH-MWCNTs), amino functionalized multi-walled carbon nanotubes (NH(2)-MWCNTs), nano SiO(2), nano TiO(2) and nano MgO comparatively to promote extraction efficiency. In this device, the innovative solid sorbents were developed by the sol-gel method via the reaction of tetraethylorthosilicate (TEOS) with 2-amino-2-hydroxymethyl-propane-1,3-diol (TRIS). In the basic condition (pH 10-11), the gel growth process in the presence of ionic liquid and nanoparticles was initiated. Then, the sol was injected into a polypropylene hollow fiber segment for in situ gelation process. Parameters affecting the efficiency of HF-SPME were thoroughly investigated. Linearity was observed over a range of 0.01-25,000 ng/mL with detection limits between 0.004 and 0.095 ng/mL for the pesticides in the aqueous matrices and 0.003-0.080 ng/mL in the hair matrices. The relative recoveries in the real samples ranged from 82.0% to 94.0% for the pesticides store seller's hair and the work researchers' hair. Results are showing the great possibilities of HF-SPME-HPLC-PDA for analysis of pesticides in biological and environmental samples.

  17. Multi-residue analysis of organic pollutants in hair and urine for matrices comparison.

    Hardy, Emilie M; Duca, Radu C; Salquebre, Guillaume; Appenzeller, Brice M R

    2015-04-01

    Urine being currently the most classically used matrix for the assessment of human exposure to pesticides, a growing interest is yet observed in hair analysis for the detection of organic pollutants. The aim of the present work was to develop and to validate multi-residue analytical methods, as similar as possible, in order to determine pesticides and their metabolites in these two biological matrices despite their different nature. The list of parent compounds and their metabolites investigated here consisted of 56 compounds, including organochlorines, organophosphates, pyrethroids, carbamates, other pesticides and polychlorinated biphenyls (PCBs). Two different approaches were necessary for the analysis of non-polar compounds (mainly parents) on one hand and polar analytes (mainly metabolites) on the other hand. In the final procedure, extraction from hair was carried out with acetonitrile/water after sample decontamination and pulverization. Extract was split into two fractions, which were analyzed directly with solid phase microextraction (SPME) injection for non-polar compounds and after derivatization with liquid injection for polar compounds. In urine, non-polar compounds were analyzed directly using SPME. Polar compounds were analyzed after acidic hydrolysis, liquid-liquid extraction with acetonitrile-cyclohexane-ethyl acetate, derivatization and liquid injection. Analysis was performed with gas chromatography tandem mass spectrometry operating in negative chemical ionization (GC-MS/MS-NCI) for all the compounds (non-polar and polar) in the two matrices. In hair, limits of quantification (LOQ) ranged from 0.02 pg/mg for trifluralin to 5.5 pg/mg for diethylphosphate. In urine, LOQ ranged from 0.4 pg/mL for α-endosulfan to 4 ng/mL for dimethyldithiophosphate. The analysis of samples supplemented with standards and samples collected from an animal previously submitted to chronic exposure to pesticides confirmed that all the compounds were analyzable in both

  18. Residuos de plaguicidas organoclorados en leche pasteurizada comercializada en Ciudad de México Organochlorine pesticide residues in commercial pasteurised milk in Mexico City

    G PRADO

    1998-01-01

    Full Text Available Los residuos de algunos plaguicidas organo-clorados presentes en lasmuestras de leche pasteurizada analizadas representan un riesgo para lasalud de los consumidores. Se determinó el contenido de plaguicidas organoclorados en 96 muestras de leche pasteurizada, por cromatografía gas líquido. Las muestras fueron colectadas quincenalmente y durante un año en la Ciudad de México, de cuatro marcas comerciales.En las muestras analizadas se determinó el valor promedio X en µg/gbase grasa, la razón X/LMR y el porcentaje de muestras que sobrepasó el valor LMR. Los valores encontrados fueron los siguientes, respectivamente:(a + b-HCH, 0.22 µg/g, 2.21 y 47.9%, Lindano, 0.07 µg/g, 0.38 y 8.3%, Aldrín + Dieldrín,0.25 µg/g, 1.67 y 39.5%, Heptacloro + heptacloroepóxido, 0.15µg/g, 1.00 y 23.9%, Endrín, 0.05 µg/g, 2.70 y 37.5% y DDT + metabolitos, 0.12 µg/g, 0.10 y 0.0%. Es altamente recomendable mantener un seguimiento en el control de algunos pesticidas organoclorados presentes en la leche pasteurizada de la Ciudad de México.Milk products are frequently contaminated with toxic organochlorine pesticides.The level of organochlorine pesticide residues of 96 pasteurised milk sampleswas determined by gas-liquid chromatography. The samples were collectedfrom four milk industries in Mexico City. The pesticides found in the pasteurisedmilk samples, their average values, the average value/MRL ratio, and samplepercentages exceeding the Maximum Residue Limits (MRL were respectively:(a+b-HCH, 0.22 µg/g, 2.21, (47.9%, Lindane,0.07 µg/g, 0.38, (8.3%, Aldrin + Dieldrin, 0.25 µg/g, 1.67,(39.5%, Heptachlor + Heptachlor epoxide, 0.15 µg/g, 1.00, (23.9%,Endrin, 0.05 µg/g 2.70, (37.5%, DDT and metabolites, 0.12 µg/g,0.10, (0.0%. A follow up study in the control of organochlorine pesticides presentin Mexican pasteurised milk is recommended

  19. Determination of multiple organophosphorus pesticide residues simultaneously in fruit and vegetable by gas chromatography-mass spectrometry%气质联用法同时测定果蔬中多种有机磷农药残留

    王海凤; 王俊斌; 刘海学; 何新益; 胡毅

    2013-01-01

    Determination of organophosphorous pesticide residues in fruit and vegetable using gas chromatography-mass spectrometry was studied. Full scan was used for qualitative analysis. The total ion current was identified by scan and spectrum library search. Selected ion monitoring (SIM) was used as a quantitative method. The results showed that the analysis was finished in 20 min. The linearity of method is good with concentration range 0. 05~1. 00 mg/L (r2≥ 99%). The recoveries are generally from 72. 6% to 94. 0% with relative standard deviation (RSD) of 1.3% to 8. 8%. The method is suitable for determining multiple organophosphorous pesticide residues in fruits and vegetables.%通过气相色谱—质谱联用(GC/MS)技术对果蔬中的有机磷农药残留进行检测,采用全扫描方式(scan)进行定性,选择离子监测方式(SIM)进行定量,结合总离子流色谱图和提取离子色谱图,优化色谱条件,使分析时间控制在20 min以内,分离效果良好,在0.05~1.00 mg/L范围内线性关系良好(r2≥99%),加标回收率为72.6%~94.0%,相对标准偏差为1.3%~8.8%,符合果蔬中多种有机磷农药残留检测要求.

  20. Development, validation and application of a methodology based on solid-phase micro extraction followed by gas chromatography coupled to mass spectrometry (SPME/GC-MS) for the determination of pesticide residues in mangoes.

    Menezes Filho, Adalberto; dos Santos, Fábio Neves; Pereira, Pedro Afonso de Paula

    2010-04-15

    A method was developed for the simultaneous analysis of 14 pesticide residues (clofentezine, carbofuran, diazinon, methyl parathion, malathion, fenthion, thiabendazole, imazalil, bifenthrin, permethrin, prochloraz, pyraclostrobin, difenoconazole and azoxystrobin) in mango fruit, based on solid-phase micro extraction (SPME) coupled to gas chromatography-mass spectrometry (GC-MS). Different parameters of the method were evaluated, such as fiber type, extraction mode (direct immersion and headspace), temperature, extraction and desorption times, stirring velocities and ionic strength. The best results were obtained using polyacrylate fiber and direct immersion mode at 50 degrees C for 30 min, along with stirring at 250 rpm and desorption for 5 min at 280 degrees C. The method was validated using mango samples spiked with pesticides at concentration levels ranging from 33.3 to 333.3 microg kg(-1). The average recoveries (n=3) for the lowest concentration level ranged from 71.6 to 117.5%, with relative standard deviations between 3.1 and 12.3%, respectively. Detection and quantification limits ranged from 1.0 to 3.3 microg kg(-1) and from 3.33 to 33.33 microg kg(-1), respectively. The optimized method was then applied to 16 locally purchased mango samples, all of them containing the pesticides bifenthrin and azoxystrobin in concentrations of 18.3-57.4 and 12.7-55.8 microg kg(-1), respectively, although these values were below the MRL established by Brazilian legislation. The method proved to be selective, sensitive, and with good precision and recovery rates, presenting LOQ below the MRL admitted by Brazilian legislation.

  1. Residual Stress Analysis Based on Acoustic and Optical Methods

    Sanichiro Yoshida

    2016-02-01

    Full Text Available Co-application of acoustoelasticity and optical interferometry to residual stress analysis is discussed. The underlying idea is to combine the advantages of both methods. Acoustoelasticity is capable of evaluating a residual stress absolutely but it is a single point measurement. Optical interferometry is able to measure deformation yielding two-dimensional, full-field data, but it is not suitable for absolute evaluation of residual stresses. By theoretically relating the deformation data to residual stresses, and calibrating it with absolute residual stress evaluated at a reference point, it is possible to measure residual stresses quantitatively, nondestructively and two-dimensionally. The feasibility of the idea has been tested with a butt-jointed dissimilar plate specimen. A steel plate 18.5 mm wide, 50 mm long and 3.37 mm thick is braze-jointed to a cemented carbide plate of the same dimension along the 18.5 mm-side. Acoustoelasticity evaluates the elastic modulus at reference points via acoustic velocity measurement. A tensile load is applied to the specimen at a constant pulling rate in a stress range substantially lower than the yield stress. Optical interferometry measures the resulting acceleration field. Based on the theory of harmonic oscillation, the acceleration field is correlated to compressive and tensile residual stresses qualitatively. The acoustic and optical results show reasonable agreement in the compressive and tensile residual stresses, indicating the feasibility of the idea.

  2. Rapid Detection of Pesticide Residues in Chinese Herbal Medicines by Fourier Transform Infrared Spectroscopy Coupled with Partial Least Squares Regression

    Tianming Yang

    2016-01-01

    Full Text Available This paper reports a simple, rapid, and effective method for simultaneous detection of cartap (Ca, thiocyclam (Th, and tebufenozide (Te in Chinese herbal medicines including Radix Angelicae Dahuricae and Liquorices using Fourier transform infrared spectroscopy (FT-IR coupled with partial least squares regression (PLSR. The proposed method can handle the intrinsic interferences of herbal samples; satisfactory average recoveries attained from near-infrared (NIR and mid-infrared (MIR PLSR models were 99.0±10.8 and 100.2±1.0% for Ca, 100.2±6.9 and 99.7±2.5% for Th, and 99.1±6.3 and 99.6±1.0% for Te, respectively. Furthermore, some statistical parameters and figures of merit are fully investigated to evaluate the performance of the two models. It was found that both models could give accurate results and only the performance of MIR-PLSR was slightly better than that of NIR-PLSR in the cases suffering from herbal matrix interferences. In conclusion, FT-IR spectroscopy in combination with PLSR has been demonstrated for its application in rapid screening and quantitative analysis of multipesticide residues in Chinese herbal medicines without physical or chemical separation pretreatment step and any spectral processing, which also implies other potential applications such as food and drug safety, herbal plants quality, and environmental evaluation, due to its advantages of nontoxic and nondestructive analysis.

  3. Direct surface analysis of pesticides on soil, leaves, grass, and stainless steel by static secondary ion mass spectrometry

    Ingram, J.C.; Groenewold, G.S.; Appelhans, A.D.; Delmore, J.E.; Olson, J.E.; Miller, D.L. [Idaho National Engineering Lab., Idaho Falls, ID (United States)

    1997-02-01

    Direct surface analyses by static secondary ion mass spectrometry (SIMS) were performed for the following pesticides adsorbed on dandelion leaves, grass, soil, and stainless steel samples: alachlor, atrazine, captan, carbofuran, chlorpyrifos, chlorosulfuron, chlorthal-dimethyl, cypermethrin, 2,4-D, diuron, glyphosate, malathion, methomyl, methyl arsonic acid, mocap, norflurazon, oxyfluorfen, paraquat, temik, and trifluralin. The purpose of this study was to evaluate static SIMS as a tool for pesticide analysis, principally for use in screening samples for pesticides. The advantage of direct surface analysis compared with conventional pesticide analysis methods is the elimination of sample pretreatment including extraction, which streamlines the analysis substantially; total analysis time for SIMS analysis was ca. 10 min/sample. Detection of 16 of the 20 pesticides on all four substrates was achieved. Of the remaining four pesticides, only one (trifluralin) was not detected on any of the samples. The minimum detectable quantity was determined for paraquat on soil in order to evaluate the efficacy of using SIMS as a screening tool. Paraquat was detected at 3 pg/mm{sup 2} (c.a. 0.005 monolayers). The results of these studies suggest that SIMS is capable of direct surface detection of a range of pesticides, with low volatility, polar pesticides being the most easily detected. 25 refs., 2 figs., 2 tabs.

  4. 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

    Marcos Zatti da Silva

    2007-04-01

    ão 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.

  5. Homogeneous liquid-liquid extraction combined with gas chromatography-electron capture detector for the determination of three pesticide residues in soils

    Wang Xuedong [School of Environmental Science and Public Health, Wenzhou Medical College, Wenzhou 325035 (China)], E-mail: zjuwxd@yahoo.com.cn; Zhao Xinna; Liu Xiujuan; Li Yanyan; Fu Lingyan; Hu Jia [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, Central China Normal University, Wuhan 430079 (China); Huang Changjiang [School of Environmental Science and Public Health, Wenzhou Medical College, Wenzhou 325035 (China)

    2008-07-14

    In this study, a new method was developed for analyzing malathion, cypermethrin and lambda-cyhalothrin from soil samples by using homogeneous liquid-liquid extraction (HLLE) and gas chromatography with electron capture detector (GC-ECD). Acetone was used as extraction solvent for the extraction of target pesticides from soil samples. When the extraction process was finished, the target analytes in the extraction solvent were rapidly transferred from the acetone extract to carbon tetrachloride, using HLLE. Under the optimum conditions, linearity was obtained in the range of 0.05-40 {mu}g kg{sup -1} for malathion, 0.04-10 {mu}g kg{sup -1} for lambda-cyhalothrin and 0.05-50 {mu}g kg{sup -1} for cypermethrin, respectively. Coefficients of correlation (r{sup 2}) ranged from 0.9993 to 0.9998. The repeatability was carried out by spiking soil samples at concentration levels of 2.5 {mu}g kg{sup -1} for lambda-cyhalothrin, and 10 {mu}g kg{sup -1} for malathion and cypermethrin, respectively. The relative standard deviations (RSDs) varied between 2.3 and 9.6% (n = 3). The limits of detection (LODs), based on signal-to-noise ratio (S/N) of 3, varied between 0.01 and 0.04 {mu}g kg{sup -1}. The relative recoveries of three pesticides from soil A1, A2 and A3 at spiking levels of 2.5, 5 and 10 {mu}g kg{sup -1} were in the range of 82.20-91.60%, 88.90-110.5% and 77.10-98.50%, respectively. In conclusion, the proposed method can be successfully applied for the determination of target pesticide residues in real soil samples.

  6. Determination of Organophosphorous Pesticide Residues in Aquatic Products by Gas Chromatography%固相净化气相色谱法测定水产品中多种有机磷农药残留

    万译文; 刘丽; 李小玲; 黄华伟

    2012-01-01

    Established an analytical method for the determination of 8 organophosphorous pesticide residues in aquatic products by GC/FPD. The sample was extracted by acetonitrile, purified by ENVI-C18 and PSA solid-phase extraction, cartridges using acetone/n-hexane ( 1:1, V:V) as eluent. The eluent was blown to dryness under a stream of nitrogen,was then injected into the GC system to quantitative analysis. Calibration curves of high cor-relation were for 8 organophosphorous pesticide residues in a range between 0.050 mg/L and 1.00 mg/L,detec-tion limits were in the range of 1. 8μg/kg~2.5 (μg/kg,RSD of spiked replicate samples ranged from 1.1%~ 5.7% and the recovery rates were from 69.8%~116%.%建立了水产品中8种有机磷农药残留同时测定的方法,选择乙腈提取,ENVI-C18串联PSA固相萃取柱净化,经丙酮/正己烷混合溶液(体积比1∶1)洗脱,洗脱液氮吹浓缩后采用气相色谱外标法定量.8种有机磷农药在0.050 mg/L~1.00 mg/L范围内线性良好,检出限在1.8 μg/kg~2.5 μg/kg之间,3个添加水平加标样品平行测定的相对标准偏差为1.1% ~5.7%,回收率为69.8%~116%.

  7. Combustion Analysis of Different Olive Residues

    Antonio Ruiz

    2008-04-01

    Full Text Available The Thermogravimetric Analysis (TGA techniques and concretely the study of the burning profile provide information that can be used to estimate the behaviour of the combustion of carbonous materials. Commonly, these techniques have been used for the study of carbons, but are also interesting for the analysis of biomass wastes, due to the different species present on the wastes affect directly to its thermal properties. In this work, techniques of thermal analysis have been applied to compare the behaviour of different wastes coming from olive oil mills. From these results, it is remarkable that the Concentrated Olive Mill Waste Water (COMWW presents more unfavourable conditions for its combustion.

  8. Application of the QuEChERS method for the determination of organochlorine pesticide residues in Brazilian fruit pulps by GC-ECD.

    Paz, Mário; Correia-Sá, Luísa; Vidal, Carla B; Becker, Helena; Longhinotti, Elisane; Domingues, Valentina F; Delerue-Matos, Cristina

    2017-01-02

    The Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method was applied to the extraction of 14 organochlorine pesticides (OCPs) residues from commercial fruit pulps available in supermarkets in Fortaleza, Northeastern Brazil. The analyses were carried out by gas chromatography (GC), coupled to an electron-capture detector (ECD), and were confirmed by GC-tandem mass spectrometry (MS). The parameters of the analytical method, such as accuracy, precision, linear range, limits of detection and quantification, were determined for each pesticide. The results showed good linearity (R(2) ≥ 0.9916) and the overall average recoveries were considered satisfactory obtaining values between 69 and 110%, RSD of 2-15 %, except for hexachlorobenzene (HCB) in açai, acerola and guava pulp samples. The OCPs were detected in guava (α-HCH; lindane) and soursop (α, β-HCH isomers) samples. The QuEChERS method and GC-ECD were successfully used to analyze OCPs in commercially available Brazilian fruit pulps and can be applied in routine analytical laboratories.

  9. Analysis of bioremediation of pesticides by soil microorganisms

    Ruml, Tomas; Klotz, Dietmar; Tykva, Richard

    1995-10-01

    The application of new pesticides requires careful monitoring of their distribution in the environment. The effect of the soil microflora on the stability of the [14C]- labelled juvenoid hormone analogue W-328 was estimated. The micro-organisms from two different soil samples were isolated and tested for their ability to decompose W-328. One bacterial strain, yeast and mold isolates, exhibited the degradation activity. The growth characteristics such as pH and temperature optima were determined. The degradation products were estimated using HPLC.

  10. Effects of different washing methods on pesticide organophosphorus residues%洗涤方法对有机磷农药残留的影响

    刘振华; 王小伟; 于瑞祥; 沈一萍; 丁卓平

    2013-01-01

    Objective To compare the effects of different washing methods for removing of organophos-phorus 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 clean-ing effect were flour water concentration for 3.5 g per 500 mL water, soaking time for 17 min, soaking tem-perature for 32 ℃, and the pesticide removal rate reached to 83%. A good linear range was obtained between 0.8~32.0μg/mL, and the linear equation was Y=0.011X-0.005 with correlation coefficient of 0.9955, the limit of detection was 0.8μg/mL. Conclusion It is effective to reduce pesticide residues on the fruits and vegeta-bles by using flour water, and the method is simple, convenient and cheap, and suitable for use in daily life.%  目的比较不同洗涤方法对果蔬表面有机磷农药去除效果的影响.方法利用可食用的无毒物质洗米水、面粉水、小苏打和食用碱4种洗涤溶液,对残留有机磷类农药(以氧化乐果为例)的蔬菜样品(白菜)进行清洗,经萃取、浓缩后,用磷钼蓝比色法进行测定.结果面粉水的清洗效果最好,通过对面粉水清洗效果进行单因素实验和正交实验,得出最佳清洗效果条件为面粉水浓度为3.5 g/500 mL、浸泡时间为17 min、浸泡温度为32℃,农药去除率达到83%.氧化乐果在为0.8~32.0μg/mL范围内线性范围良好,线性方程为Y=0.011X−0.005,相关系数为0.9955,检出限为0.8μg/mL.结论用面粉水对果蔬进行清洗,能够有效减少农药残留,此法简单、便捷、价廉,适合在日常生活中使用.

  11. Accelerated solvent extraction -gas chromatography to the residue of pesticides measurement%加速溶剂萃取-气相色谱法对土壤中农药残留的测定

    孙志伟

    2015-01-01

    文章论述了加速溶剂萃取-气相色谱法对土壤中农药残留的测定方法.%This paper introduced the accelerated solvent extraction -gas chromatography to the residue of pesticides measurement.

  12. Laboratory assessment by combined z score values in proficiency tests: experience gained through the European Union proficiency tests for pesticide residues in fruits and vegetables.

    Medina-Pastor, P; Mezcua, M; Rodríguez-Torreblanca, C; Fernández-Alba, A R

    2010-08-01

    The obligation for accredited laboratories to participate in proficiency tests under ISO 17025, performing multiresidue methods (MRMs) for pesticide residues, involves the reporting of a large number of individual z scores making the evaluation of the overall performance of the laboratories difficult. It entails, time and again, the need for ways to summarise the laboratory's overall assessment into a unique combined index. In addition, the need for ways to continually evaluate the performance of the laboratory over the years is equally acknowledged. For these reasons, following 14 years of the European Union Reference Laboratory for Pesticide Residues in Fruits and Vegetables (EUPT-FV), useful formulas have been designed to globally evaluate the assessment of the participating laboratories. The aim is to achieve a formula which is easy to understand, which can be applied and which fits the purposes of long-term evaluation detecting positive and negative trends. Moreover, consideration is needed for a fair compensation of bad results in MRM, taking into account the large number of compounds that are covered. It is therefore important to be aware of the difficulties in getting satisfactory values from a wide range of compounds. This work presents an evaluation of the main well-established combined z score formulas together with those new ones developed here which have been applied to the European proficiency test results (EUPTs) over the years. Previous formulas such as the rescaled sum of z score (RSZ), the sum squared of z score (SSZ) and the relative laboratory performance (RLP) are compared with the newer ones: the sum of weighted z scores (SWZ) and the sum of squared z scores (SZ2). By means of formula comparisons, conclusions on the advantages, drawbacks and the most fit-for-purpose approach are achieved.

  13. Finite Element Residual Stress Analysis of Planetary Gear Tooth

    Jungang Wang

    2013-01-01

    Full Text Available A method to simulate residual stress field of planetary gear is proposed. In this method, the finite element model of planetary gear is established and divided to tooth zone and profile zone, whose different temperature field is set. The gear's residual stress simulation is realized by the thermal compression stress generated by the temperature difference. Based on the simulation, the finite element model of planetary gear train is established, the dynamic meshing process is simulated, and influence of residual stress on equivalent stress of addendum, pitch circle, and dedendum of internal and external meshing planetary gear tooth profile is analyzed, according to non-linear contact theory, thermodynamic theory, and finite element theory. The results show that the equivalent stresses of planetary gear at both meshing and nonmeshing surface are significantly and differently reduced by residual stress. The study benefits fatigue cracking analysis and dynamic optimization design of planetary gear train.

  14. Residual Displacements‘ Progresive Analysis of the Multisupported Beam

    Liudas Liepa

    2014-12-01

    Full Text Available This paper focuses on a shakedown behaviour of the ideally elasto-plastic beams system under variable repeated load. The mathematical models of the analysis problems are created using numerical methods, extremum energy principles and mathematic programming. It is shown that during the shakedown process the residual displacements vary non-monotonically. By solving analysis problem, where the load locus is being progressively expanded, it is possible to determine the upper and lower bounds of residual displacements. Suggested methods are ilustrated by solving multisupported beam example problem. The results are obtained considering principle of the small displacements.

  15. Occupational exposure to pesticides and prostate cancer: a systematic review and meta-analysis.

    Lewis-Mikhael, Anne-Mary; Bueno-Cavanillas, Aurora; Ofir Guiron, Talia; Olmedo-Requena, Rocío; Delgado-Rodríguez, Miguel; Jiménez-Moleón, José Juan

    2016-02-01

    Epidemiological studies on exposure to pesticides and risk of prostate cancer (PC) provide inconsistent results. We aimed to explore various potential sources of heterogeneity not previously assessed and to derive updated risk estimates from homogenous studies. We searched PubMed, Web of Science and Scopus databases for case-control and cohort studies published from 1985 to April 2014. We assessed the quality of the articles using the Newcastle-Ottawa Scale. Pooled estimates were calculated using random-effects models. Heterogeneity was explored using subset analyses and metaregression. Fifty-two studies were included in the review and 25 in the meta-analysis. No association was found between low exposure to pesticides and PC, but association was significant for high exposure, pooled OR 1.33 (1.02 to 1.63), I(2)=44.8%, p=0.024. Heterogeneity was explained by a number of variables including method used to assess exposure. Pooled OR was weak and non-significant for studies measuring serum pesticide level, 1.12 (0.74 to 1.50), I(2)=0.00%, p=0.966. For studies applying self-reporting of exposure, pooled estimate was 1.34 (0.91 to 1.77), I(2)=0.00%, p=0.493, while a high significant association was detected for grouped exposure assessment, 2.24 (1.36 to 3.11), I(2)=0.00%, p=0.955. In spite of a weak significant association detected when pooling ORs for high occupational exposure to pesticides, the magnitude of the association was related to the method of exposure assessment used by the original studies. A family history-pesticide exposure interaction was also observed for a number of pesticides.

  16. Radionuclides in Bayer process residues: previous analysis for radiological protection

    Cuccia, Valeria; Rocha, Zildete, E-mail: vc@cdtn.b, E-mail: rochaz@cdtn.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil); Oliveira, Arno H. de, E-mail: heeren@nuclear.ufmg.b [Universidade Federal de Minas Gerais (DEN/UFMG), Belo Horizonte, MG (Brazil). Dept. de Engenharia Nuclear

    2011-07-01

    Natural occurring radionuclides are present in many natural resources. Human activities may enhance concentrations of radionuclides and/or enhance potential of exposure to naturally occurring radioactive material (NORM). The industrial residues containing radionuclides have been receiving a considerable global attention, because of the large amounts of NORM containing wastes and the potential long term risks of long-lived radionuclides. Included in this global concern, this work focuses on the characterization of radioactivity in the main residues of Bayer process for alumina production: red mud and sand samples. Usually, the residues of Bayer process are named red mud, in their totality. However, in the industry where the samples were collected, there is an additional residues separation: sand and red mud. The analytical techniques used were gamma spectrometry (HPGe detector) and neutron activation analysis. The concentrations of radionuclides are higher in the red mud than in the sand. These solid residues present activities concentrations enhanced, when compared to bauxite. Further uses for the residues as building material must be more evaluated from the radiological point of view, due to its potential of radiological exposure enhancement, specially caused by radon emission. (author)

  17. A mobile App for military operational entomology pesticide applications

    Multiple field studies conducted for the Deployed War Fighter Protection (DWFP) research program have generated over 80 specific guidance points for innovative combinations of pesticide application equipment, pesticide formulations, and application techniques for aerosol and residual pesticide treat...

  18. Pesticides and honey bees

    Amaro, Pedro; Godinho, Joana

    2012-01-01

    After the analysis of the criterion of toxicological classification (TC) of pesticides to honeybees and of the evolution of TC and of legislation related to the theme, in Portugal, it is demonstrated how the absence of rigor of the Portuguese Pesticide Regulation Authority (AFN) and of the pesticides suppliers contribute to the very high probability of mortality of honeybees by pesticides and finally are presented proposals for the optimization of perspectives to...

  19. Comparison of solid phase- and liquid/liquid-extraction for the purification of hair extract prior to multi-class pesticides analysis.

    Duca, Radu-Corneliu; Salquebre, Guillaume; Hardy, Emilie; Appenzeller, Brice M R

    2014-04-01

    The present study focuses on the influence of a purification step - after extraction of pesticides from hair and before analysis of the extract - on the sensitivity of analytical methods including compounds from different chemical classes (both parent and metabolites). Sixty-seven pesticides and metabolites from different chemical classes were tested here: organochlorines, organophosphates, carbamates, pyrethroids, ureas, azoles, phenylpyrazoles and neonicotinoids. Two gas chromatography-negative chemical ionization-tandem mass spectrometry methods and one based on ultra-performance liquid chromatography-electrospray tandem mass spectrometry were used. Seven solid-phase extraction cartridges: C18, S-DVB, PS-DVB, GCB, GCB/PSA, SAX/PSA and Florisil/PSA were tested and compared to more classical liquid-liquid extraction procedures using ethyl acetate, hexane and dichloromethane. Although LLE allowed obtaining good results for some compounds, on the whole, SPE clearly provided better recovery for the majority of the pesticide residues tested in the present study. GCB/PSA was clearly the best suited to non-polar compounds such as organochlorines, pyrethroids and organophosphates, with recovery ranging from 45.9% (diflufenican) to 117.1% (parathion methyl). For hydrophilic metabolites (e.g. dialkyl phosphates and other organophosphate metabolites, pyrethroid metabolites, phenols and carbamate metabolites), the best results were obtained with PS-DVB, with recovery ranged from 10.3% (malathion monocarboxylic acid) to 93.1% (para-nitrophenol). For hydrophilic parent pesticides (e.g. neonicotinoids, carbamates, azoles) and metabolites without nucleophilic functions, the best recovery was obtained with SAX/PSA, with recovery ranging from 52.1% (3-hydroxycarbofuran) to 100.9% (3,4-dichloroaniline). Solid phase extraction was found to be more suitable than the liquid-liquid extraction for pesticides and their metabolites determination in terms of number of extracted compounds

  20. Use of the EFSA Standard Sample Description (SSD for the reporting of data on the control of pesticide residues in food and feed according to Regulation (EC No 396/2005 (Version: 2013 Data Collection

    European Food Safety Authority

    2014-01-01

    Full Text Available Regulation (EC No 396/2005 on Maximum Residue Levels of pesticides in or on food and feed of plant and animal origin requires the Member States to monitor pesticide residue levels in food commodities and submit the monitoring results to EFSA and the European Commission. In 2009, EFSA developed the Standard Sample Description (SSD, which is a standardised model for the reporting of harmonised data on analytical measurements of chemical substances occurring in food, feed and water. This document is intended to provide the Member States with specific guidance on how to use the SSD for the reporting of the national results of the pesticide monitoring in the framework of Article 32 of Regulation (EC No 396/2005. In particular, this document is meant to provide SSD users with support in selecting the appropriate codes for the elements which pertain to pesticide residues monitoring data. This document shall complement the EFSA guidance document “Standard sample description for food and feed”.

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

    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 org

  2. Pesticide residues, heavy metals, and DNA damage in sentinel oysters Crassostrea gigas from Sinaloa and Sonora, Mexico.

    Vázquez-Boucard, Celia; Anguiano-Vega, Gerardo; Mercier, Laurence; Rojas del Castillo, Emilio

    2014-01-01

    Pesticides and heavy metals were analyzed in sentinel Crassostrea gigas oysters placed in six aquaculture sites close to a contaminated agricultural region. Each site was sampled twice. Tests revealed the presence of organochlorine (OC) pesticides in the oysters at concentrations varying from 31.8 to 72.5 μg/kg for gamma-hexachlorocyclohexane (γ-HCH); from 1.2 to 3.1 μg/kg for dichlorodiphenyldichloroethylene (4,4-DDE); from 1.6 to 2.3 μg/kg for endosulfan I; and from 1.4 to 41.2 μg/kg for endosulfan II, as well as heavy metals in concentrations that exceeded Mexican tolerance levels (405.5 to 987.8 μg/g for zinc; 4.2 to 7.3 μg/g for cadmium; and 7.2 to 9.9 μg/g for lead). Significant levels of DNA damage in oyster hemocytes were also detected. There was a significant, positive correlation between genotoxic damage and concentration of nickel or the presence of endosulfan II. Cellular viability evaluated by cytotoxic analyses was found to be high at 80%. Marked inhibition in activity of acetylcholinesterase (AChE ) and induction of glutathione S-transferase (GST) activity was noted. Data demonstrated a significant relation between AChE activity inhibition and presence of endosulfan II, γ-HCH, copper, lead, and 4,4-DDE, as well as between AChE and GST activity at different sites.

  3. 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.

    González-Curbelo, Miguel Ángel; Lehotay, Steven J; Hernández-Borges, Javier; Rodríguez-Delgado, Miguel Ángel

    2014-09-01

    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 and other nonvolatile compounds for salting out in the method is not ideal for mass spectrometry. In this study, we developed and evaluated three new different versions of the QuEChERS method using more volatile salts (ammonium chloride and ammonium formate and acetate buffers) to induce phase separation and extraction of 43 representative pesticide analytes of different classes. Fast low-pressure gas chromatography tandem mass spectrometry (LPGC-MS/MS) and liquid chromatography (LC)-MS/MS were used for analysis. The QuEChERS AOAC Official Method 2007.01 was also tested for comparison purposes. Of the studied methods, formate buffering using 7.5g of ammonium formate and 15mL of 5% (v/v) formic acid in acetonitrile for the extraction of 15g of sample (5g for wheat grain) provided the best performance and practical considerations. Method validation was carried out with and without the use of dispersive solid-phase extraction for cleanup, and no significant differences were observed for the majority of pesticides. The method was demonstrated in quantitative analysis for GC- and LC-amenable pesticides in 4 representative food matrices (apple, lemon, lettuce, and wheat grain). With the typical exceptions of certain pH-dependent and labile pesticides, 90-110% recoveries and food applications.

  4. Residuals analysis of the generalized linear models for longitudinal data.

    Chang, Y C

    2000-05-30

    The generalized estimation equation (GEE) method, one of the generalized linear models for longitudinal data, has been used widely in medical research. However, the related sensitivity analysis problem has not been explored intensively. One of the possible reasons for this was due to the correlated structure within the same subject. We showed that the conventional residuals plots for model diagnosis in longitudinal data could mislead a researcher into trusting the fitted model. A non-parametric method, named the Wald-Wolfowitz run test, was proposed to check the residuals plots both quantitatively and graphically. The rationale proposedin this paper is well illustrated with two real clinical studies in Taiwan.

  5. A meta-analysis comparing the sensitivity of bees to pesticides.

    Arena, Maria; Sgolastra, Fabio

    2014-04-01

    The honey bee Apis mellifera, the test species used in the current environmental risk assessment procedure, is generally considered as extremely sensitive to pesticides when compared to other bee species, although a quantitative approach for comparing the difference in sensitivity among bees has not yet been reported. A systematic review of the relevant literature on the topic followed by a meta-analysis has been performed. Both the contact and oral acute LD50 and the chronic LC50 reported in laboratory studies for as many substances as possible have been extracted from the papers in order to compare the sensitivity to pesticides of honey bees and other bee species (Apiformes). The sensitivity ratio R between the endpoint for the species a (A. mellifera) and the species s (bees other than A. mellifera) was calculated for a total of 150 case studies including 19 bee species. A ratio higher than 1 indicated that the species s was more sensitive to pesticides than honey bees. The meta-analysis showed a high variability of sensitivity among bee species (R from 0.001 to 2085.7), however, in approximately 95 % of the cases the sensitivity ratio was below 10. The effect of pesticides in domestic and wild bees is dependent on the intrinsic sensitivity of single bee species as well as their specific life cycle, nesting activity and foraging behaviour. Current data indicates a need for more comparative information between honey bees and non-Apis bees as well as separate pesticide risk assessment procedures for non-Apis bees.

  6. Genetic Alterations in Pesticide Exposed Bolivian Farmers: An evaluation by analysis of chromosomal aberrations and the comet assay

    Erik Jørs

    2007-01-01

    Full Text Available Background: Pesticides are of concern in Bolivia because of increasing use. Frequent intoxications have been demonstrated due to use of very toxic pesticides, insufficient control of distribution and sale and little knowledge among farmers of protective measures and hygienic procedures.Method: Questionnaires were applied and blood tests taken from 81 volunteers from La Paz County, of whom 48 were pesticide exposed farmers and 33 non-exposed controls. Sixty males and 21 females participated with a mean age of 37.3 years (range 17–76. Data of exposure and possible genetic damage were collected and evaluated by well known statistical methods, controlling for relevant confounders. To measure genetic damage chromosomal aberrations and the comet assay analysis were performed.Results: Pesticide exposed farmers had a higher degree of genetic damage compared to the control group. The number of chromosomal aberrations increased with the intensity of pesticide exposure. Females had a lower number of chromosomal aberrations than males, and people living at altitudes above 2500 metres seemed to exhibit more DNA damage measured by the comet assay.Conclusions: Bolivian farmers showed signs of genotoxic damage, probably related to exposure to pesticides. Due to the potentially negative long term health effects of genetic damage on reproduction and the development of cancer, preventive measures are recommended. Effective control with imports and sales, banning of the most toxic pesticides, education and information are possible measures, which could help preventing the negative effects of pesticides on human health and the environment.

  7. Analysis of fenbendazole residues in bovine milk by ELISA.

    Brandon, David L; Bates, Anne H; Binder, Ronald G; Montague, William C; Whitehand, Linda C; Barker, Steven A

    2002-10-09

    Fenbendazole residues in bovine milk were analyzed by ELISAs using two monoclonal antibodies. One monoclonal antibody (MAb 587) bound the major benzimidazole anthelmintic drugs, including fenbendazole, oxfendazole, and fenbendazole sulfone. The other (MAb 591) was more specific for fenbendazole, with 13% cross-reactivity with the sulfone and no significant binding to the sulfoxide metabolite. The limit of detection of the ELISA method in the milk matrix was 7 ppb for MAb 587 and 3 ppb for MAb 591. Fenbendazole was administered in feed, drench, and paste form to three groups of dairy cattle. Milk was collected immediately before dosing and then every 12 h for 5 days. The ELISA indicated that residue levels varied widely among individual cows in each group. Fenbendazole levels peaked at approximately 12-24 h and declined rapidly thereafter. Metabolites were detected at much higher levels than the parent compound, peaked at approximately 24-36 h, and declined gradually. Residue levels were undetectable by 72 h. The ELISA data correlated well with the total residues determined by chromatographic analysis, but the use of the two separate ELISAs did not afford an advantage over ELISA with the single, broadly reactive MAb 587. The ELISA method could be used to flag high-residue samples in on-site monitoring of fenbendazole in milk and is a potential tool for studying drug pharmacokinetics.

  8. Mass balance and composition analysis of shredder residue.

    Pomykala, J. A., Jr.; Jody, B. J.; Spangenberger, J. S.; Daniels, E. J.; Energy Systems

    2007-01-01

    The process of shredding end-of-life vehicles to recover metals results in a byproduct commonly referred to as shredder residue. The four-and-a-half million metric tons of shredder residue produced annually in the United States is presently land filled. To meet the challenges of automotive materials recycling, the U.S. Department of Energy is supporting research at Argonne National Laboratory in cooperation with the Vehicle Recycling Partnership (VRP) of the United States Council for Automotive Research (USCAR) and the American Plastics Council. This paper presents the results of a study that was conducted by Argonne to determine variations in the composition of shredder residue from different shredders. Over 90 metric tons of shredder residues were processed through the Argonne pilot plant. The contents of the various separated streams were quantitatively analyzed to determine their composition and to identify materials that should be targeted for recovery. The analysis established a reliable mass balance for the different materials in shredder residue.

  9. Residual stress analysis of drive shafts after induction hardening

    Lemos, Guilherme Vieira Braga; Rocha, Alexandre da Silva; Nunes, Rafael Menezes, E-mail: lemos_gl@yahoo.com.br [Universidade Federal do Rio Grande do Sul (UFRS), Porto Algre, RS (Brazil); Hirsch, Thomas Karl [Stiftung Institut für Werkstofftechnik (IWT), Bremen (Germany)

    2014-08-15

    Typically, for automotive shafts, shape distortion manifests itself in most cases after the induction hardening by an effect known as bending. The distortion results in a boost of costs, especially due to machining parts in the hardened state to fabricate its final tolerances. In the present study, residual stress measurements were carried out on automotive drive shafts made of DIN 38B3 steel. The samples were selected in consequence of their different distortion properties by an industrial manufacturing line. One tested shaft was straightened, because of the considerable dimensional variation and the other one not. Firstly, the residual stress measurements were carried out by using a portable diffractometer, in order to avoid cutting the shafts and evaluate the original state of the stresses, and afterwards a more detailed analysis was realized by a conventional stationary diffractometer. The obtained results presented an overview of the surface residual stress profiles after induction hardening and displayed the influence of the straightening process on the redistribution of residual stresses. They also indicated that the effects of the straightening in the residual stresses cannot be neglected. (author)

  10. Analysis of Recent Situation of Pesticide Poisoning in Bangladesh: Is There a Proper Estimate?

    Gourab Dewan

    2014-06-01

    Conclusion: Pesticide poisoning is responsible for great number of admissions and deaths in Bangladesh. Creating a register of commercially available pesticides in each region for rapid identification of nature of the pesticide is recommended.

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

    Christian Nansen

    2010-03-01

    Full Text Available 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 food and feed items. As a model system, we investigated detection of a miticide applied to maize leaves and its miticidal bioactivity over time, and we compared two types of reflectance data: fourier transformed infrared (FTIR data and hyperspectral imaging (HI data. The miticide (bifenazate was applied at a commercial field rate to maize leaves in the field, with or without application of a surfactant, and with or without application of a simulated “rain event”. In addition, we collected FTIR and HI from untreated control leaves (total of five treatments. Maize leaf data were collected at seven time intervals from 0 to 48 hours after application. FTIR data were analyzed using conventional analysis of variance of miticide-specific vibration peaks. Two unique FTIR vibration peaks were associated with miticide application (1,700 cm−1 and 763 cm−1. The integrated intensities of these two peaks, miticide application, surfactant, rain event, time between miticide application, and rain event were used as explanatory variables in a linear multi-regression fit to spider mite mortality. The same linear multi-regression approach was applied to variogram parameters derived from HI data in five selected spectral bands (664, 683, 706, 740, and 747 nm. For each spectral band, we conducted a spatial structure analysis, and the three standard variogram parameters (“sill”, “range”, and “nugget” were examined as possible “indicators” of miticide

  12. Residual Effect of Pesticides used in Integrated Apple Production on Chrysoperlaexterna (Hagen (Neuroptera: Chrysopidae Larvae Efecto Residual de los Pesticidas utilizados en la Producción integrada de Manzanas en las Larvas de Chrysoperla externa (Hagen (Neuroptera: Chrysopidae

    Alexandre P Moura

    2012-06-01

    Full Text Available Temperate fruit crops are an important economic activity for growers in southern Brazil. However, several pest species are associated to apple (Malus domestica Borkh. crops in Brazil. Pesticides are largely used to control them and one way to change this is to combine selective pesticides and predator insects. The goal of this research was to evaluate the effects of the abamectin, carbaryl, fenitrothion, methidathion, sulfur, and trichlorfon pesticides on the survival and stage length of larvae and pupae, adult oviposition from treated larvae, and hatched eggs of two Chrysoperla externa (Hagen, 1861 (Neuroptera: Chrysopidae populations. The compounds were sprayed on glass plates in accordance with the International Organization for Biological Control (IOBC recommendations. First- and second-instar larvae were exposed to pesticide residues. Carbaryl, fenitrothion, and methidathion caused 100% mortality of first- and second-instar larvae. Changes in the number of eggs laid by females from first- and second-instar larvae exposed to residues of abamectin and sulfur, or abamectin, sulfur, and trichlorfon, respectively, were not observed. Only abamectin reduced the number of hatched eggs laid by females in Bento Gonçalves from treated first-instar larvae. Sulfur reduced the viability of C. externa eggs in Bento Gonçalves and Vacaria females from treated second-instar larvae, whereas trichlorfon and abamectin reduced the viability of eggs in Vacaria females. In conclusion, carbaryl, fenitrothion and methidathion were harmful to C. externa. Trichlorfon was harmful to first-instar larvae and slightly harmful to second-instar larvae. Abamectin and sulfur were slightly harmful to first-instar larvae and harmless to second-instar larvae.El cultivo de frutas de clima templado es una actividad económica importante para agricultores del Sur de Brasil. Sin embargo, varias especies de plagas están asociadas al cultivo de la manzana (Malus domestica Borkh. en

  13. Study on Experiment of Absorption Spectroscopy Detection of Pesticide Residues of Carbendazim in Orange Juice%橙汁中多菌灵农药残留吸收光谱特征研究

    季仁东; 陈梦岚; 赵志敏; 朱星玥; 王乐新; 刘全金

    2014-01-01

    coefficient was 0 .996 ,and the recovery was :81% ~102% .According to the regression model ,we can ob-tain the amount of carbendazim pesticide residues in orange juice .It was verified that the method of using ultraviolet-visible ab-sorption spectra was feasible to detect the carbendazim residues in orange juice .The result proved that it is possible to detect pesticide residues of carbendazim in orange juice ,and it can meet the needs of rapid analysis .This study provides a new way for the detection of pesticide residues .

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

    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 res

  15. Human health risk of dietary intake of organochlorine pesticide residues in bovine meat and tissues from Veracruz, México.

    Pardío, Violeta; Martínez, David; Flores, Argel; Romero, Dora; Suárez, Víctor; López, Karla; Uscanga, Roxana

    2012-12-01

    Tissue distribution patterns of organochlorine pesticides in bovine carcasses varied significantly among seasons, geographic locations and tissues. The highest concentrations of Σ-DDT during the dry season were detected in lungs from Paso de Ovejas (2,834.90μg/kg lipid) and, during the rainy season, Lindane and Σ-HCH in muscle and lung samples from Paso de Ovejas (995.80 and 1,690.10μg/kg lipid). Estimated daily intakes of γ-HCH and Σ-DDT (3.35 and 1.22μg/kg bw/day) through consumption of muscle tissues from Paso de Ovejas and Puente Nacional during the rainy season showed the highest contribution. During the rainy season the highest non-cancer Hazard Ratios estimated corresponded to γ-HCH (3.97) and Σ-DDT (4.39) detected in muscle samples from Puente Nacional. The highest Hazard Ratios of cancer risk to the 95th centile daily consumption through meat corresponded to p,p'-DDT from Alvarado (7.76E+06) and from Paso de Ovejas for γ-HCH (1.50E+05) during rainy season. The results indicate potential non- and carcinogenic risks to consumer health through meat consumption.

  16. Detection of Exposure to Environmental Pesticides During Pregnancy by the Analysis of Maternal Hair Using GC–MS

    Posecion, N.; Ostrea, E.; Bielawski, D.; Corrion, M.; Seagraves, J.; Jin, Y.

    2006-01-01

    Several classes of pesticides were extracted from maternal hair by solid-liquid extraction. Analysis of their selected metabolites involved a methanolic/hydrochloric acid methyl ester derivatization and liquid–liquid extraction. Gas chromatography electron impact mass spectrometry was used to detect and quantify the pesticides and metabolites. Recovery of parent compounds and metabolites from the analysis of spiked hair ranged from 87 to 112% with coefficients of variation less than 11%. Limi...

  17. Influence of ripening stages of tomatoes in the analysis of pesticides by gas chromatography

    Sousa,Flaviane A. de; Neves,Antônio A.; Maria Eliana L. R. Queiroz; Heleno,Fernanda F.; Teófilo, Reinaldo F.; Pinho,Gevany P.

    2014-01-01

    Some parameters of tomato fruits ripening such as color, pH, ºBrix, acidity and lycopene and β-carotene content were evaluated during the ripening of fruits. Five pesticides were quantified in organic extracts derived from tomatoes at different stages of maturation. The solid-liquid extraction technique with partition at low temperature (SLE-PLT) was used to obtain these organic extracts. The matrix effect of tomato was calculated from the results of analysis by gas chromatography with e...

  18. Health and environmental hazards of pesticides.

    Iyaniwura, T T

    1991-01-01

    The increase in world population and in demand for food and economic crops has put a pesticide burden on man and the environment. Pesticide residues from vector control and agricultural uses contaminate the terrestrial and aquatic surroundings and contribute to the pollution problem of the environment. Various human toxicoses have resulted from pesticide use. The major pathogenic pesticides are chlorinated hydrocarbons and organophosphates. With careful and enlightened use, pesticide toxicity, to both man and the environment, could be significantly reduced.

  19. Evaluation of zirconium dioxide-based sorbents to decrease the matrix effect in avocado and almond multiresidue pesticide analysis followed by gas chromatography tandem mass spectrometry.

    Lozano, Ana; Rajski, Łukasz; Uclés, Samanta; Belmonte-Valles, Noelia; Mezcua, Milagros; Fernández-Alba, Amadeo R

    2014-01-01

    Two sorbents containing ZrO₂ (Z-Sep and Z-Sep+) were tested as a d-SPE clean-up in combination with the QuEChERS and ethyl acetate multiresidue method in the pesticide residues extraction in avocado. All extracts were analysed using gas chromatography coupled with a triple quadrupole mass spectrometer working in multi-reaction monitoring mode. GC QToF was used to compare the amount of matrix compounds present in the final extracts, prepared according to different protocols. The highest number of pesticides with acceptable recoveries and the lowest amount of coextracted matrix compounds were provided by QuEChERS with Z-Sep. Subsequently, this method was fully validated in avocado and almonds. Validation studies were carried out according to DG Sanco guidelines including: the evaluation of recoveries at two levels (10 and 50 μg/kg), limit of quantitation, linearity, matrix effects, as well as interday and intraday precision. In avocado, 166 pesticides were fully validated compared to 119 in almonds. The method was operated satisfactorily in routine analysis and was applied to real samples.

  20. Meta-analysis of scientific studies related to pesticide application techniques - air assistance and adjuvant addition

    Gustavo Migliorini de Oliveira

    Full Text Available ABSTRACT: The aim of this study was to investigate the effects of air-assisted boom sprayers and addition of adjuvants in the spray solution on control levels of pesticide sprays against weeds and pathogenic fungi by meta-analysis of scientific literature. To perform the meta-analysis, data were collected from the results presented in scientific papers. By these data, a variable was created, denominated as relative control that was used to quantify and test whether the use of air assistance or adjuvants affects the effectiveness of pesticide sprays. This variable was calculated as a difference between percentage of pesticide control in treatments with air assistance or adjuvants and treatments without these spray techniques. Data were analyzed statistically using the Comprehensive Meta-Analysis software. Results showed that the use of air assistance did not have any effect on the control levels of weeds and pathogenic fungi; whereas, the addition of adjuvants increased these levels by 6.45%.

  1. Organochlorine pesticides and polychlorinated biphenyl congeners in wild terrestrial mammals from Croatia: Interspecies comparison of residue levels and compositions.

    Herceg Romanić, Snježana; Klinčić, Darija; Kljaković-Gašpić, Zorana; Kusak, Josip; Reljić, Slaven; Huber, Đuro

    2015-10-01

    In this pilot study, we investigated levels of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in the adipose tissues of two free-ranging terrestrial carnivores from Croatia sampled in 2010 and 2011: the brown bear (Ursus arctos; N=32) and the grey wolf (Canis lupus; N=29). Concentrations of ∑OCPs and ΣPCBs ranged from 0.45 to 4.09 ng g(-1) lipid mass (lm) and from 0.93 to 8.52 ng g(-1) lm in brown bear, and from 1.18 to 5.67 ng g(-1) lm and 2.68 to 48.9 ng g(-1) lm in grey wolf adipose tissues, respectively. PCBs were dominant accounting for over 72% of total analyzed persistent organic pollutants (POPs). The sum of six indicator non-dioxin-like PCBs (Σ6IndNDL PCBs) made up 60-93% and 58-85% of the total congener concentrations in brown bears and wolves, respectively. Although the levels of the measured parameters were significantly higher in grey wolves than in bears, the contaminant profiles of the two species were similar, with γ-HCH, HCB, β-HCH and DDE as major OCP contaminants, and PCB-153>PCB-180≈PCB-170>PCB-138 as the dominant congeners. The sum of hexachlorocyclohexanes (ΣHCHs) and 8 toxicologically relevant dioxin-like PCBs (Σ8ToxDL PCBs) was higher in the males than in the females of the brown bear. Concentrations of ΣDDTs, HCB, ΣOCP, ΣPCBs, Σ6IndNDL PCBs, and toxicologically relevant non-dioxin-like PCBs (ΣToxNDL PCBs) were significantly positively correlated with lipid content in the grey wolf. Concentrations of OCPs and PCBs in brown bears and wolves from Croatia were low and normal for large terrestrial mammals.

  2. Multiresidue analysis of 50 pesticides in grape, pomegranate, and mango by gas chromatography-ion trap mass spectrometry.

    Savant, Rahul H; Banerjee, Kaushik; Utture, Sagar C; Patil, Sangram H; Dasgupta, Soma; Ghaste, Manoj S; Adsule, Pandurang G

    2010-02-10

    A selective and sensitive multiresidue analysis method is reported for simultaneous determination of 50 pesticides of different chemical classes in three commercially important fruits of different nature viz. grape, pomegranate, and mango. The sample preparation method involves extraction of a 10 g sample with 10 mL of ethyl acetate; cleanup by dispersive solid phase extraction with primary secondary amine (PSA, 25 mg) for grape and PSA + graphitized carbon black (25 + 5 mg) for pomegranate and mango; and determination by gas chromatography-ion trap mass spectrometry through multiple reaction monitoring (MRM). Sample preparation under acidified (pH 4) and cold (<4 degrees C) conditions, use of PTV-large volume injection (20 microL) through multibaffled liner and chromatographic separation on a short 10 m VF-5MS capillary column gave a satisfactory response for all of the analytes including relatively unstable compounds such as captan, captafol, folpet, endrine, and iprodione within 31.8 min. The limit of quantification (LOQ) of most of the compounds was pesticide in samples within 20% tolerance range at the LOQ level. Use of matrix-matched standards could minimize the matrix effect, which was lowest in grape, followed by pomegranate and mango. Recoveries ranged within 70-120% at 10, 20, and 50 ng g(-1) in all three matrixes with associated relative standard deviations <20% (n = 6). The method could be successfully applied to the screening of 100 farm samples for compliance to EU maximum residue limits.

  3. Pesticides in the propolis at São Saulo State, Brazil - doi: 10.4025/actascianimsci.v34i4.15859 Pesticides in the propolis at São Saulo State, Brazil - doi: 10.4025/actascianimsci.v34i4.15859

    Samir Moura Kadri

    2012-10-01

    Full Text Available The increasing demand for propolis has caused a raise in its production. However, an increasingly pesticide-dependent agriculture is a great concern with regard to bees, their produce and environmental contamination. Current analysis evaluates the presence of pesticides (organochlorines, organophosphates, pyrethroids, carbamates, herbicides, fungicides and acaricides in samples of propolis from the state of São Paulo, Brazil. Beekeepers from several localities in the state provided samples of propolis (50, which were collected, stored in non-toxic plastic bags and maintained in a freezer for analyses. Possible pesticide residues were examined by gas chromatography method but no pesticide residues were detected in the examined propolis samples. Propolis analyzed in the state of São Paulo did not show any pesticide contamination. The increasing demand for propolis has caused a raise in its production. However, an increasingly pesticide-dependent agriculture is a great concern with regard to bees, their produce and environmental contamination. Current analysis evaluates the presence of pesticides (organochlorines, organophosphates, pyrethroids, carbamates, herbicides, fungicides and acaricides in samples of propolis from the state of São Paulo, Brazil. Beekeepers from several localities in the state provided samples of propolis (50, which were collected, stored in non-toxic plastic bags and maintained in a freezer for analyses. Possible pesticide residues were examined by gas chromatography method but no pesticide residues were detected in the examined propolis samples. Propolis analyzed in the state of São Paulo did not show any pesticide contamination.

  4. Study on the interaction of catalase with pesticides by flow injection chemiluminescence and molecular docking.

    Tan, Xijuan; Wang, Zhuming; Chen, Donghua; Luo, Kai; Xiong, Xunyu; Song, Zhenghua

    2014-08-01

    The interaction mechanisms of catalase (CAT) with pesticides (including organophosphates: disulfoton, isofenphos-methyl, malathion, isocarbophos, dimethoate, dipterex, methamidophos and acephate; carbamates: carbaryl and methomyl; pyrethroids: fenvalerate and deltamethrin) were first investigated by flow injection (FI) chemiluminescence (CL) analysis and molecular docking. By homemade FI-CL model of lg[(I0-I)/I]=lgK+nlg[D], it was found that the binding processes of pesticides to CAT were spontaneous with the apparent binding constants K of 10(3)-10(5) L mol(-1) and the numbers of binding sites about 1.0. The binding abilities of pesticides to CAT followed the order: fenvalerate>deltamethrin>disulfoton>isofenphos-methyl>carbaryl>malathion>isocarbophos>dimethoate>dipterex>acephate>methomyl>methamidophos, which was generally similar to the order of determination sensitivity of pesticides. The thermodynamic parameters revealed that CAT bound with hydrophobic pesticides by hydrophobic interaction force, and with hydrophilic pesticides by hydrogen bond and van der Waals force. The pesticides to CAT molecular docking study showed that pesticides could enter into the cavity locating among the four subdomains of CAT, giving the specific amino acid residues and hydrogen bonds involved in CAT-pesticides interaction. It was also found that the lgK values of pesticides to CAT increased regularly with increasing lgP, Mr, MR and MV, suggesting that the hydrophobicity and steric property of pesticide played essential roles in its binding to CAT.

  5. Study on The New Methods of Degradation of Pesticide Residues in Vegetables%蔬菜残留农药降解新方法的研究

    董建民; 吕微; 刘红伟

    2011-01-01

    The residues of pesticides is one of the major problems influencing food safety of China.The simulation model of the degradation of three kinds of pesticides(dichlorvos,imethamidophos,carbofuran) in vegetables was established.The degradation way of closed turbocharged dynamic high concentration ozone was independent developmented.The results showed,the effect of degradation is significant,the degradation rates of organic phosphorus exceeded 93%,the degradation rates of carbofuran exceeded 88%.%农药残留是影响我国食物安全的一大关键问题。文中建立了蔬菜农药降解效果分析体系,自主研发了高浓度臭氧密闭动态增压降解方法,分析了该方法对蔬菜中常见的敌敌畏、甲胺磷和呋喃丹等3种农药残留的降解效果。结果表明,该降解方法在进行多农药高浓度残留降解时其降解效果显著,有机磷降解率均超过93%,呋喃丹降解率超过88%。

  6. Multi-analyte high performance liquid chromatography coupled to high resolution tandem mass spectrometry method for control of pesticide residues, mycotoxins, and pyrrolizidine alkaloids.

    Dzuman, Zbynek; Zachariasova, Milena; Veprikova, Zdenka; Godula, Michal; Hajslova, Jana

    2015-03-10

    A new reliable and highly sensitive method based on high performance liquid chromatographic (HPLC) separation and high resolution tandem mass spectrometric detection (HRMS/MS) has been developed and validated for determination of 323 pesticide residues, 55 mycotoxins, and 11 plant toxins represented by pyrrolizidine alkaloids. The method was validated for three matrices, leek, wheat, and tea differing in nature/amount of co-extracts that may cause various matrix effects. For target analytes isolation, optimized QuEChERS-based (quick, easy, cheap, effective, rugged, and safe) extraction procedure was employed. Spectral HRMS/MS library has been established providing an entire spectrum of fragment ions for each analyte, which allows unbiased identification and confirmation of target compounds. The limits of quantification (LOQs) of target analytes were below 10 μg kg(-1) for 82%, 81%, and 61% for matrices leek, wheat, and tea, respectively. Recoveries were in the acceptable range (70-120%) according to SANCO/12571/2013 for most of target analytes, except for highly polar 'masked' mycotoxin deoxynivalenol-3-glucoside with recoveries 35%, 47%, and 42% for matrices leek, wheat, and tea, respectively. The linearities of calibration curves expressed as coefficients of determination were in the range of 0.9661-1.000, and repeatabilities expressed as relative standard deviations (RSDs) at LOQs lied in the range of 0.25-13.51%. The trueness of the method was verified using several certified reference materials (CRMs) and proficiency test samples.

  7. 40 CFR 180.467 - Carbon disulfide; tolerances for residues.

    2010-07-01

    ...) PESTICIDE PROGRAMS TOLERANCES AND EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Specific Tolerances..., insecticide, and fungicide carbon disulfide, from the application of sodium tetrathiocarbonate, in or on...

  8. 40 CFR 180.198 - Trichlorfon; tolerances for residues.

    2010-07-01

    ...) PESTICIDE PROGRAMS TOLERANCES AND EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Specific Tolerances... the insecticide trichlorfon (dimethyl (2,2,2-trichloro-1-hydroxyethyl) phosphonate) in or on...

  9. [Study on usage of pesticides in various countries].

    Yamamoto, Miyako; Toda, Miou; Tanaka, Keiko; Sugita, Takiko; Sasaki, Shiho; Uneyama, Chikako; Morikawa, Kaoru

    2007-01-01

    Usage of pesticides in food items in export countries was studied, focusing items which Japan imports in large quantity. Japan has imported field crops such as wheat, corn and soy bean, and also grapefruit in large quantity on a weight base, mainly from United States, Australia and Canada. While, Japan has imported various kinds of vegetables in which China had the largest share. We collected usage data of pesticides for 44 food items of 17 countries of 2004. Pesticides which were used frequently (usage rank within top ten in each item/country) were dichlorvos, carbofuran, chlorpyrifos, dimethoate (insecticides), mancozeb, carbendazim, thiophanate-methyl, chlorthalonil (fungicides), glyphosate, 2,4-D, paraquat, acetochlor (herbicides). Carbendazim, thiophanate-methyl, acetochlor and dichlorvos were mainly used in China. Dithiocarbamates are used frequently in various food items in various countries, and also frequently detected in monitoring in foreign countries. Some pesticides such as bisultap, monosultap, etaboxam and triazmate were used only in certain countries, and available information on toxicity or analytical method was very limited. Some of pesticides described above have not been analyzed in the pesticide residue monitoring in Japan before 2005,however, many of them are subjects of analysis for import food after 2006 with the enforcement of positivelist system for residues of pesticide and veterinary medicines in food in Japan.

  10. Control Efficiency of Oats Seed-coating with Thiamethoxam on Aphids and Red Leaf and Analysis of Pesticide Residue%噻虫嗪种子包衣对燕麦蚜虫和红叶病的控制效果及农药残留分析

    李惠霞; 张海英; 郭建国; 郭满库; 何苏琴; 刘永刚; 赵桂琴

    2012-01-01

    The red leaf of oat caused by yellow dwarf virus(BYDV) is an important disease and it could be prevented by controlling of aphids.The control effects and efficacy duration of oat seeds coated with thiamethoxam on aphids and red leaf were investigated in the field.The dynamic of residue in plants and seeds were detected using high performance liquid chromatography(HPLC).The results showed that both the aphid number on each plant and disease index of red leaf were lower in the plants of seed coating treatment than those of control.During seedling to jointing stage,the control effects on aphids were 77.71%~87.91% and the control effects on red leaf were 65.79%~82.89%.During booting to flowering stage,the control effects on aphids were 58.45%~68.61% and the control effects on red leaf were 62.98%~64.14%.So the efficacy duration was as long as 90 days.The residue dynamic of thiamethoxam residue in plants was accorded with the first-order dynamic equation C=13.218e-0.0971t based on the thiamethoxam residue 9.86 mg·kg-1 at the 60th day after planting,and the half-life period was 7.14 d.The thiamethoxam residue in plants were 0.43~9.86 mg·kg-1 at 60~100 d after planted,it was close to or exceeded the maximum residue limits(MRLs) for forage,so the plants could not be mowed as green feed.The residue was less or equal to 0.06 at 110 d after planted and could be mowed as green feed or hay.The thiamethoxam residue was not detected in oat kernels.%红叶病是由蚜虫传播黄矮病毒(BYDV)引起的燕麦上的重要病害,有效防治蚜虫可控制燕麦红叶病的发生。为了明确噻虫嗪种衣剂的应用效果和安全性,通过田间试验研究了噻虫嗪种子包衣对燕麦蚜虫和红叶病的防效及持效期,并采用高效液相色谱法测定了药物在植株和籽粒上的残留动态。结果表明,种子包衣处理后,燕麦单株蚜量和红叶病病情指数均低于对照,苗期至拔节期的蚜虫防效为77.71%~87.91%,

  11. Compound specific isotope analysis to investigate pesticide degradation in lysimeter experiments at field conditions

    Ryabenko, Evgenia; Elsner, Martin; Bakkour, Rani; Hofstetter, Thomas; Torrento, Clara; Hunkeler, Daniel

    2015-04-01

    The frequent detection of organic micropollutants such as pesticides, consumer care products or pharmaceuticals in water is an increasing concern for human and ecosystem health. Degradation analysis of these compounds can be challenging in complex systems due to the fact that metabolites are not always found and mass balances frequently cannot be closed. Many abiotic and biotic degradation pathways cause, however, distinct isotope fractionation, where light isotopes are transferred preferentially from the reactant to the product pool (normal isotope fractionation). Compound-specific isotope analysis (CSIA) of multiple elements is a particularly powerful method to evaluate organic micropollutant transformation, because it can even give pathway-specific isotope fractionation (1,2). Available CSIA field studies, however, have focused almost exclusively on volatile petroleum and chlorinated hydrocarbons, which are present in high concentrations in the environment and can be extracted easily from water for GC-IRMS analysis. In the case of micropollutants, such as pesticides, CSIA in more challenging since it needs to be conducted at lower concentrations and requires pre-concentration, purification and high chromatographic performance (3). In this study we used lysimeters experiments to analyze transformation of atrazine, acetochlor, metolachlor and chloridazone by studying associated isotope fractionation. The project combines a) analytical method development for CSIA, b) identification of pathways of micropollutant degradation and c) quantification of transformation processes under field condition. The pesticides were applied both, at the soil surface and below the top soil under field-relevant concentrations in May 2014. After typical irrigation of the lysimeters, seepage water was collected in 50L bottles and stored for further SPE and CSIA. Here we present the very first result of a) analytical method development, b) improvement of SPE methods for complex pesticide

  12. Quality of potatoes grown in various regions of Serbia as influenced by heavy metal and pesticide residues concentrations

    Rajković Miloš B.

    2002-01-01

    export of products based on potatoes containing Cd. Analyses of lindane and bensultap (Bancol pesticides indicate that they are not within critical values, nor in such quantities to affect human health, so, from this aspect, the analysed potato samples from all sites are absolutely suitable for consumation.

  13. Analysis of sulphonamide residues in edible animal products: a review.

    Wang, S; Zhang, H Y; Wang, L; Duan, Z J; Kennedy, I

    2006-04-01

    The methods of analysis for sulphonamide residues in edible animal products are reviewed. Sulphonamides are widely used for therapeutic and prophylactic purposes in both humans and animals, sometimes as growth promoters as additives in animal feed. As a result of their widespread use, there is concern about whether the levels used of these drugs can generate serious problems in human health, e.g., allergic or toxic reactions. Several methods for the determination of sulphonamides have been reported in the literature and this review considers high-performance liquid chromatography (HPLC), liquid chromatography-mass spectrometry (LC/MS), gas chromatography (GC), thin-layer chromatography (TLC), high-performance capillary electrophoresis (HPCE), enzyme-linked immunosorbant assay (ELISA), biosensor immunoassay (BIA) and microbiological methods. Specific aspects of analysing sulphonamides, such as sample handling, chromatographic conditions and detection methods are discussed. Methods for drug residue monitoring should be accurate, simple, economical in both time and cost, and capable of detecting residues below the maximum residue limits (MRL). The current sulphonamide detection technologies are based on chromatographic methods or bacteriological growth inhibition. The instrumental methods such as HPLC and GC are both sensitive and specific, but are laborious and expensive. Because of the labour-intensive processes, only a few cases of GC methods applied to residue analysis have been published. These methods are suitable for confirmation but not for screening of large numbers of samples. Microbiological methods do not require highly specialized and expensive equipment. They also use highly homogeneous cell populations for testing and thus result in better assay precision. Although HPCE has powerful separation ability, the precision is poor and the instrument still needs to be improved. To date, this technique has not been widely applied to routine analysis. Currently

  14. Prevention of food poisoning due to pesticide residues in vegetables of Guangdong province%广东省预防蔬菜农残中毒工作研究

    黄伟雄; 邓峰; 江月碧; 罗建波; 梁春穗; 戴昌芳

    2001-01-01

    为预防蔬菜农药中毒的发生和提高蔬菜食用的安全性,广东省卫生防疫站开展了预防蔬菜农残引起食物中毒的系统工作,包括:加强部门间合作,研究消除蔬菜中农药残留物的方法,提高监测技术水平。结果表明,此系统的工作是科学的、有效的,广东省因农药引起的食物中毒呈逐年下降趋势。%A prevention system in Guangdong province was developed by the Station of Health and Anti|epidemic to prevent the food poisoning due to pesticide residues in vegetables.It includes the reinforcement of the cooperation between departments,research on the method for removing pesticide residues in vegetables and improvement of the level of inspection.The work indicated the scientific and efficient of the system,and the downtrend of food poisoning due to pesticide residues.

  15. PRICE, QUALITY, AND PESTICIDE RELATED HEALTH RISK CONSIDERATIONS IN FRUIT AND VEGETABLE PURCHASES: AN HEDONIC ANALYSIS OF TUCSON, ARIZONA SUPERMARKETS

    Estes, Edmund A.; Smith, V. Kerry

    1996-01-01

    National opinion polls indicate that pesticide residues on fresh fruits and vegetables remain an important concern of American consumers, despite a decade-long increase in per capita consumption levels for fresh fruits and vegetables. Increased availability of organically grown fruits and vegetables may change consumer produce purchase behavior which is often dominated by appearance considerations. Domestic consumers likely consider and tradeoff price, visual appearance, and health risk when ...

  16. 不同剂型戊唑醇在土壤中的残留消解动态%Residue and Degradation of Tebuconazole with Different Pesticide Formulations in Soil

    陈丽霞; 许丽建; 文海花

    2015-01-01

    以悬浮剂﹑乳油﹑水分散粒剂﹑可湿性粉剂和水乳剂5种不同剂型为研究对象,探讨不同剂型戊唑醇在土壤中的残留消解动态. 在高剂量(有效成分浓度300 mg /kg)施药1次后,不同剂型戊唑醇的消解半衰期为11~12 d. 分别以高剂量和低剂量(有效成分浓度300 mg/kg和450 mg/kg,两个浓度水平在土壤中进行残留试验,在最后一次施药的28﹑35和42 d后,分别测定5种剂型戊唑醇的最终残留量,结果表明,不同剂型戊唑醇在土壤中的最终残留水平无显著差异.%The degradation and residue of tebuconazole with different pesticide formulations in soil were studied, and the main pesticide formulations were aqueous suspension concentrate, emulsifiable concentrate,water dispersible granule,wettable powder and emulsion.The half-lives of tebuconazole with different pesticide formulations at higher dosage(300 mg/kg) in ba-nana were in ranges of 11~12 d,respectively.With the higher and lower dosage (300 mg/kg and 450 mg/kg),the final residues of tebuconazole with different pesticide formulations at 28,35 and 42 d after the last spraying were also investigated.The results showed that there was no significant difference in the three different pesticide formulations in soil.

  17. Determination of organophosphorus pesticides and their major degradation product residues in food samples by HPLC-UV.

    Peng, Guilong; He, Qiang; Lu, Ying; Mmereki, Daniel; Zhong, Zhihui

    2016-10-01

    A simple method based on dispersive solid-phase extraction (DSPE) and dispersive liquid-liquid microextraction method based on solidification of floating organic droplets (DLLME-SFO) was developed for the extraction of chlorpyrifos (CP), chlorpyrifos-methyl (CPM), and their main degradation product 3,5,6-trichloro-2-pyridinol (TCP) in tomato and cucumber samples. The determination was carried out by high performance liquid chromatography with ultraviolet detection (HPLC-UV). In the DSPE-DLLME-SFO, the analytes were first extracted with acetone. The clean-up of the extract by DSPE was carried out by directly adding activated carbon sorbent into the extract solution, followed by shaking and filtration. Under the optimum conditions, the proposed method was sensitive and showed a good linearity within a range of 2-500 ng/g, with the correlation coefficients (r) varying from 0.9991 to 0.9996. The enrichment factors ranged from 127 to 138. The limit of detections (LODs) were in the range of 0.12-0.68 ng/g, and the relative standard deviations (RSDs) for 50 ng/g of each analytes in tomato samples were in the range of 3.25-6.26 % (n = 5). The proposed method was successfully applied for the extraction and determination of the mentioned analytes residues in tomato and cucumber samples, and satisfactory results were obtained.

  18. 40 CFR 180.157 - Methyl 3-[(dimethoxyphos-phinyl) oxy]butenoate, alpha and beta isomers; tolerances for residues.

    2010-07-01

    ... PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS TOLERANCES AND EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN.... (a) General. Tolerances are established for residues of the insecticide methyl 3- butenoate,...

  19. 75 FR 26668 - Flutriafol; Pesticide Tolerances

    2010-05-12

    ... class of pesticides. Although conazoles act similarly in plants (fungi) by inhibiting ergosterol... are no currently established Codex, Canadian, or Mexican maximum residue limits for flutriafol...

  20. Mineral analysis, anthocyanins and phenolic compounds in wine residues flour

    Bennemann Gabriela Datsch

    2016-01-01

    Full Text Available This study analyzed the mineral content (N, P, K, S, Ca, Fe, Mg, Mn, Fe and Zn, anthocyanins and phenolic compounds in flours produced from residues of different grape cultivars from the wineries in the Southern region of Brazil. Mineral analysis showed a significant difference for all grape cultivar, with the exception for phosphorus content. Residues from cv. Seibel showed higher levels of N, Cu and Mg. The cultivars Ancelotta, Tanat and Bordô present higher contents of K, Zn, Mn, Fe and Ca. For the concentration of anthocyanins, cultivars Cabernet Sauvignon (114.7 mg / 100g, Tannat (88.5 mg / 100 g and Ancelotta (33.8 mg/100 g had the highest concentrations. The cultivars Pinot Noir (7.0 g AGE / 100 g, Tannat (4.3 g AGE / 100 g, and Ancelotta (3.9 g AGE / 100 g had the highest content of phenolic compounds. Considering these results, it became evident the potential of using the residue of winemaking to produce flour for human consumption, highlighting the grapes ‘Tannat' and ‘Ancellotta'.

  1. 气相色谱法测定蔬菜中9种有机磷农药残留%GC-detection of 90rganophosphorous Pesticide Residues in Vegetables

    孙卓然; 娜仁高娃; 张海燕; 蒙成华

    2011-01-01

    To establish a method for detection of 9 organophosphorous pesticide residues in vegetables by capillary column gas chromatography. After homogenization of vegetables, organophosphorous pesticides were extracted by aceto-nitrile, cleaned by CARB/NH2, solubilized by acetone and made up to volume, detected by DB-1701 capillary column and flame photometric detector. Nine organophosphorous pesticide residues in vegetables could be detected in the same time. The recovery was 80.2%-102.2% with relative standard deviation between the 2.15% and 5.32%. The detection limit was 0.004 2-0.027 mg/kg. The method is simple, rapid, sensitive and accurate. The technical specifications are suitable for the detection of 9 organophosphorous pesticide residues in vegetables.%建立毛细管柱气相色谱法测定蔬菜中9种有机磷农药残留的分析方法.蔬菜经均质,用乙腈提取,CARB/NH2柱净化,丙酮溶解定容,采用DB - 1701毛细管柱和火焰光度检测器测定,一次进行9种有机磷农药残留检测.样品加标回收率在80.2%~102.2%之间,相对标准偏差在2.15%~5.32%之间,检出限在0.0042~0.027 mg/kg之间.实验结果表明,该方法简便、快速、灵敏、准确,各项技术指标满足蔬菜中9种有机磷农药残留检测要求.

  2. 气相色谱/质谱法测定蔬菜中44种农药残留%Determination of 44 Pesticide Residues in Vegetables Using Chromatography-gas Chromatography/mass Spectrometry

    王爱霞; 张静; 罗建民; 陈俊宇

    2013-01-01

    A rapid,simple and sensitive method was developed for the simultaneous determining of pesticide residues in vegetables.The target pesticides in vegetables were purified by PSA powder and graphon dispersive sorbent.The drugs were analysed by GPC-GC/MS,which removed most of macromolecule such as pigment and fat.For the 44 pesticide residues in level of 0.008 mg/kg-0.064 mg/kg,the average recoveries (n=5)were in range of 65%-120%and the RSD was less than 15%.The limits of detection were in range of 0.000 5 mg/kg-0.2 mg/kg.The method in this study could be used for detecting the pesticide residues in vegetables.%建立了蔬菜中多种农药残留同时检测的分析方法。样品中残留农药采用乙腈提取,使用PSA粉和石墨炭黑吸附剂净化,再经在线凝胶渗透色谱-气相色谱/质谱(GPC-GC/MS)分析,进一步除去样液中色素和脂肪等大分子干扰物质。加标水平为0.008 mg/kg~0.064 mg/kg时,回收率为65%~120%,相对标准偏差小于15%;44种农药的检出限为0.0005 mg/kg~0.02 mg/kg。实验证明,该方法操作简单快速、准确度高,能够满足蔬菜中多种农药残留限量标准的检测要求。

  3. Rapid Detection of Trace Dimethoate Pesticide Residues Based on Colorimetric Spectroscopy%微量乐果农药残留比色光谱快速检测方法

    李文; 孙明; 李民赞; 孙红

    2015-01-01

    In order to detect dimethoate pesticide residues rapidly and safely ,a feasible method based on colorimetric spectrosco‐py was developed .Because dimethoate is one of organophosphorus pesticides containing sulfur ,its sulfenyl can react with Pd2+to produce a yellow complex named palladium sulfide .PdCl2 was used as the color agent ,which was dissolved in acetic acid in‐stead of the common concentrated hydrochloric acid .The dimethoate solution was prepared by dissolving the commercial pesti‐cides into distilled water at different concentrations .The pesticide samples were reacted with the same amount of PdCl2 solution respectively .The absorbance spectra of the samples after coloring reaction were measured in the region of 300~900 nm by a spectrophotometer .The result showed that the effect of using acetic acid instead of concentrated hydrochloric acid was not only safe but also preferable ,and 0.5 mg・ kg -1 was the minimum concentration of the pesticide that could be distinguished in the spectra . The result met the pesticide residue detecting requirements of part fruits and vegetables in the national standard GB2763—2012 regulations .Further studies on random 40 dimethoate samples from 0.5 to 88 mg・kg -1 were carried out .Thirty samples were randomly selected to establish the training model and remaining 10 samples were used to test the model .The pre‐processing methods were carried on the spectrum data such as normalization and smoothing to get a better effect through compar‐ison their prediction results with the correlation coefficient (r) and the root mean square error of cross‐validation (RMSEP) .The principal component analysis (PCA) method and partial least squares(PLS)method were used to establish prediction models re‐spectively in the different wave ranges .By calculating the correlation coefficient of dimethoate samples in 350~900 nm the maxi‐mum of 0.957 2 was obtained at wavelength 458 nm ,so 453~463 and 400~600 nm were selected

  4. Solid state fermentation of biogas residues for production of Bacillus thuringiensis based bio-pesticide%以沼渣为原料固态发酵生产Bt生物农药

    张玮玮; 弓爱君; 邱丽娜; 要如磊

    2013-01-01

    used as a substrate for bio-pesticides production by solid state fermentation. Principal component analysis of biogas residue indicated that it was well suited for the growth of Bacillus thuringiensis in the experiments. The culture medium recipe was optimized by the orthogonal test. Brewer's grain, corn meal, soybean cake power and mixed ions were chosen to carry out the study. The results showed that brewer’s grain had the biggest effects on the growth of Bacillus thuringiensis and then followed the growth effects of corn meal, soybean cake power and mixed ions. Ultimately, the optimum media were 50% biogas residues, 35% brewer's grain, 10% corn meal, and 5% soybean cake power. This article compared the fermentation process among conventional media, only biogas residues media and the optimum media, under the optimized conditions. Spore counts of 5.23×1010 CFU/g and entomotoxicity of 16100 IU/mg were obtained after 48h fermentation, while 2.55×1010 CFU/g spore counts and 12500 IU/mg entomotoxicity were obtained in the conventional medium, and 1.74×108 CFU/g spore counts and 6000 IU/mg entomotoxicity were found in the only biogas residue medium. At last, by comparing the cost between conventional medium and the optimum media, the cost could be lowered by 36.3%. The present study proved the feasibility of using kitchen waste for the production of bio-pesticides, and it seemed to be a promising alternative for the use of conventional mediums to reduce the costs.

  5. 不同栽培方式下豇豆中4种农药的残留消解%Degradation of Four Pesticide Residues in Cowpea among Different Planting Patterns

    李建国; 韩丙军; 谢德芳; 吕岱竹; 任红; 许如意

    2012-01-01

    The protected and open field experiments were conducted to study the degradation of beta cypermethrin, difenoconazole, dimethoate and acephate residues in cowpea. The GC with ECD and FPD were used to determine the residues of the four pesticides. The four pesticide residues degradation dynamics equations were calculated by a simple first-order kinetics equation. Compared with the open field planting pattern, the degradation rates of the four pesticides under protected field were slower. The pesticides used in cowpea under protected field could control the pests longer, but there was more safety risks in cowpea. In order to ensure the safety of cowpea, the rational use of pesticides must be paid attention to and the shorter half-life pesticides should be used in cowpea planting.%为了研究保护地和露地2种栽培模式下高效氯氰菊酯、苯醚甲环唑、乐果和乙酰甲胺磷4种农药在豇豆中降解残留规律,分别采用气相色谱法电子捕获检测器和火焰光度检测器测定豇豆中高效氯氰菊酯、苯醚甲环唑和乐果、乙酰甲胺磷的残留量.结果表明:4种农药在豇豆中的消解都遵循指数型降解规律.保护地栽培下农药的降解速率总体上比露地的慢,一方面可更长时间的对害虫产生防治作用,但另一方面可能更易引起农药残留的安全隐患.因此,在豇豆的种植中,应当规范农药的使用,选用半衰期较短、降解较快的农药.

  6. EVALUATION OF FARMERS APPRECIATION IN REDUCING PESTICIDE BY ORGANIC FARMING PRACTICE

    Indraningsih Indraningsih

    2016-10-01

    Full Text Available Vegetables and dairy milk are important commodities in Pangalengan and Lembang, West Java. However, agrochemicals are used intensively and excessively in production system. Therefore, pesticide residues and contamination commonly occurred in agricultural products and environments. The study aimed to assess farmers’ attitudes on pesticide toxicity and reducing pesticide residues in animal and food crops products, and investigate the attitude changes of farmers on pesticide use. It was an on-farm research and farmers were directly involved in the study. The attitude change was analyzed on questionnaire and interview base for over 99 respondents in Pangalengan and Lembang between 2001 and 2003. Samples of soils, weeds, cabbages and milk were collected for pesticide residue analysis. Results showed that farmers did not aware on toxicity effects of pesticides in both animal and human health. There was misinterpretation among the farmers where pesticides were regarded as drugs rather than toxic compound to increase productivity. The organochlorines/OCs (lindane and heptachlor were common pesticide contaminants found in soils of 7.9- 11.4 ppb, but no organophospates (OPs were detected. Both OCs and OPs were also detected in soils of Lembang at a range of 11.53-65.63 ppb and 0.6-2.6 ppb, respectively. There were pesticide residues detected in weeds collected from Pangalengan (8.93 ppb lindane, 2.05 ppb heptachlor, and 33.27 ppb chlorpyriphos methyl/CPM and Lembang (6.45 ppb lindane, 2.65 ppb endosulfan, 6.85 ppb diazinon, and 0.5 ppb CPM. Only endosulfan with least residue level (0.1 ppb was detected in organic cabbages, whereas lindane was detected much higher (3.7 ppb in non-organic cabbages. Pesticide residues were not detected in milk of dairy cattle fed on by-products of organic cabbages, but lindane was still present in milk of dairy cattle fed on non-organic cabbages for 7 days subsequently. The present study indicates that the organic farming

  7. A gas/liquid chromatographic-mass spectrometric method for the rapid screening of 250 pesticides in aqueous matrices

    Chandramouli, B.; Harvan, D.; Brittain, S.; Hass, R. [Eno River Labs, LLC. Durham, NC (United States)

    2004-09-15

    Pesticide residues in food present a potentially serious and significant cause for concern. Many pesticides have been associated with significant health effects to the nervous and endocrine systems and some have been deemed carcinogenic. There are many well-established techniques for pesticide analysis. However, commercial pesticide methods have traditionally only been available for specific pesticide families, such as chlorinated pesticides or herbicides, and at detection limits ranging from 0.05 ppb to 1 ppm in aqueous matrices. Techniques that can quickly screen for the presence/absence of pesticide residues in food matrices are critical in ensuring the safety of food and water. This paper outlines a combined Gas Chromatographic-High Resolution Mass Spectrometric (GC-HRMS) and Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) screening assay for 250 pesticides that was developed for use in water, and soda samples at screening levels ranging from 0.1-5 ppb. The pesticides selected have been identified by the European Union as being of concern and the target of possible legislation. The list encompasses a variety of pesticide classes and compound groupings.

  8. Progress in pesticide and POPs hair analysis for the assessment of exposure.

    Tsatsakis, Aristidis; Tutudaki, Maria

    2004-10-29

    The present paper reviews the work that has been done in the field of pesticide and persistent organic pollutants (POPs) hair analysis during the last 15 years. It summarizes the compounds of interest, the methods of analyte extraction from the hair matrix, the analytical techniques employed and the results obtained. The most widely studied POPs are the polychlorinated dibenzodioxins (PCDDs), the dibenzofurans (PCDFs) the co-planar biphenyls (co-PCBs) and total biphenyls (PCBs). The most widely studied pesticides are the organochlorine ones, like the hexachlorocyclohexanes and the DDTs, which nowadays are only found as environmental pollutants, some organophosphates, selected pyrethroids and the carbamate methomyl. The most widely applied technique was gas chromatography (GC) coupled to mass spectrometry (MS). Other detectors like the ECD in the case of organochlorine analysis and the NPD in the case of organophosphate analysis were also used. The presented data concern human and animal studies. The levels of DDTs detected in hair were between 19 and 400 ng/g, of co-PCBs 0.27 and 0.45 ng/g, of total PCBs 5-13 ng/g of PCDDs and PCDFs 0.1-10 pg/g of lindane 20-400 ng/g of HCHs 14-40 ng/g of diazinon 110-520 ng/g and of methomyl 900-1800 ng/g. These results strongly support the possibility of using hair as a suitable indicator for the assessment of long-term exposure to POPs and pesticides.

  9. Combination of solid-phase extraction with dispersive liquid-liquid microextraction followed by GC-MS for determination of pesticide residues from water, milk, honey and fruit juice.

    Shamsipur, Mojtaba; Yazdanfar, Najmeh; Ghambarian, Mahnaz

    2016-08-01

    In this work, an effective preconcentration method for the extraction and determination of traces of multi-residue pesticides was developed using solid-phase extraction (SPE) coupled with dispersive liquid-liquid microextraction and gas chromatography-mass spectrometry (GC-MS). Variables affecting the performance of both extraction steps such as type and volume of elution and extraction solvents, breakthrough volume, salt addition, extraction time were thoroughly investigated. The proposed method resulted in good linearities (R(2)>0.9915) over the ranges of 1-10,000ngkg(-1), limits of detection (LODs) in the range of 0.5-1.0ngkg(-1) at S/N=3, and precision of RSD% of ⩽11.8. Under optimal conditions, the preconcentration factors were obtained in the range of 2362-10,593 for 100mL sample solutions. Comparison of the proposed method with other ones demonstrated that SPE-DLLME method provides higher extraction efficiency and larger preconcentration factor for determination of pesticides residues. Further, it is simple, inexpensive, highly sensitive, and can be successfully applied to separation, preconcentration and determination of the pesticides (and other noxious materials) in different real food samples.

  10. Detection of Exposure to Environmental Pesticides During Pregnancy by the Analysis of Maternal Hair Using GC-MS.

    Posecion, N; Ostrea, E; Bielawski, D; Corrion, M; Seagraves, J; Jin, Y

    2006-12-01

    Several classes of pesticides were extracted from maternal hair by solid-liquid extraction. Analysis of their selected metabolites involved a methanolic/hydrochloric acid methyl ester derivatization and liquid-liquid extraction. Gas chromatography electron impact mass spectrometry was used to detect and quantify the pesticides and metabolites. Recovery of parent compounds and metabolites from the analysis of spiked hair ranged from 87 to 112% with coefficients of variation less than 11%. Limits of detection ranged from 0.031 to 5.88 μg g(-1). Analysis of hair samples from pregnant women in the Philippines showed maternal exposure during pregnancy to bioallethrin, propoxur, chlorpyrifos, pretilachlor and malathion.

  11. Fatigue Strength and Residual Stress Analysis of Deep Rolled Crankshafts

    Imran M Quraishi

    2012-12-01

    Full Text Available The endurance life of an engine crankshaft is closely related to its fatigue strength, in addition to other material properties and shape parameters. Deep rolling, moreover, enhances the fatigue limit by applying compressive residual stress within the fillet radius area as a major surface hardening technique. The objective of this paper isto maximize fatigue life of engine through crankshaft design optimization by quantifying fatigue strength for microalloyed steels versus Cr-Mo alloy steel, and to examine the effects of deep rolling load and rolled fillet geometry. Fatigue tests have been made with standard rotary bending test samples from both bar and forged blanks. Rig tests for actual crankshafts have been made to show how the fatigue strength correlates with different sample types. A correlation of stress distribution with bending moment was demonstrated by applying a strain gauging technique on crankshaft specimens. Therefore, an analysis of combined stresses could be made by considering the effect of static residual stress in addition to the applied dynamic bending stress. Optimum conditions for rolling load, fillet geometry and material were identified. Consequently, these results will be adapted to CAE analysis database to enable an optimization of safety factors.

  12. Examining the feasibility of mixture risk assessment: A case study using a tiered approach with data of 67 pesticides from the Joint FAO/WHO Meeting on Pesticide Residues (JMPR).

    Evans, Richard M; Scholze, Martin; Kortenkamp, Andreas

    2015-10-01

    The way in which mixture risk assessment (MRA) should be included in chemical risk assessment is a current topic of debate. We used data from 67 recent pesticide evaluations to build a case study using Hazard Index calculations to form risk estimates in a tiered MRA approach in line with a Framework proposed by WHO/IPCS. The case study is used to illustrate the approach and to add detail to the existing Framework, and includes many more chemicals than previous case studies. A low-tier MRA identified risk as being greater than acceptable, but refining risk estimates in higher tiers was not possible due to data requirements not being readily met. Our analysis identifies data requirements, which typically expand dramatically in higher tiers, as being the likely cause for an MRA to fail in many realistic cases. This forms a major obstacle to routine implementation of MRA and shows the need for systematic generation and collection of toxicological data. In low tiers, hazard quotient inspection identifies chemicals that contribute most to the HI value and thus require attention if further refinement is needed. Implementing MRA requires consensus on issues such as scope setting, criteria for performing refinement, and decision criteria for actions.

  13. Níveis de resíduos de praguicidas organoclorados em produtos cárneos sob inspeção federal Levels of organochlorine pesticide residue in meat products inspected by the federal government

    João Pessoa de Paula Carvalho

    1980-09-01

    Full Text Available Com objetivo de evidenciar a freqüência e os níveis de resíduos de praguiddas organoclorados, foram analisadas 445 unidades amostrais de matéria prima (gordura bovina provenientes de carcaças de bovinos de frigoríficos e 132 unidades amostrais de carne bovina já processada (enlatados, tais como "corned beef" e "roast beef". Apresentaram-se com resíduos de praguicidas acima dos limites de tolerância estipulados, 77 unidades amostrais de gordura bovina e 5 de produto processado. Resíduos de praguiddas, sem contudo ultrapassar os limites de tolerância, foram identificados em, praticamente, todas as amostras, sendo que 27% das unidades amostrais de gordura bovina e 10,6% de produto processado apresentaram resíduos de praguicidas em violação aos limites estabelecidos na legislação. Heptacloro, BHC e Dieldrin foram os praguiddas mais freqüentes e Lindane e DDT os menos evidenciados.To bring attention to the frequency and the levels of organochlorine pesticide residue in meat, 445 samples of raw material (bovine fat from bovine carcasses collected from meat packing plants and 132 samples of preserved meat (canned, such as corned or roast beef were analyzed. Seventy-seven samples of bovine fat and 8 of preserved meat were discovered to have pesticide residue above the maximum acceptable limits. Pesticide residue was found in practically all the samples without, however, exceeding the acceptable limits. Twenty-seven percent of the bovine fat samples and 10.6% of the preserved meat contained residue above the legal tolerance levels. Heptachlor, BHC, and Dieldrin were the most frequent; Lindane and DDT, the least.

  14. Assessment of pesticide residues in army cutworm moths (Euxoa auxiliaris) from the Greater Yellowstone Ecosystem and their potential consequences to foraging grizzly bears (Ursus arctos horribilis).

    Robison, Hillary L; Schwartz, Charles C; Petty, Jim D; Brussard, Peter F

    2006-09-01

    During summer, a grizzly bear (Ursus arctos horribilis) in the Greater Yellowstone Ecosystem (GYE) (USA) can excavate and consume millions of army cutworm moths (Euxoa auxiliaris) (ACMs) that aggregate in high elevation talus. Grizzly bears in the GYE were listed as threatened by the US Fish and Wildlife Service in 1975 and were proposed for delisting in 2005. However, questions remain about key bear foods. For example, ACMs are agricultural pests and concern exists about whether they contain pesticides that could be toxic to bears. Consequently, we investigated whether ACMs contain and transport pesticides to bear foraging sites and, if so, whether these levels could be toxic to bears. In 1999 we collected and analyzed ACMs from six bear foraging sites. ACMs were screened for 32 pesticides with gas chromatography with electron capture detection (GC-ECD). Because gas chromatography with tandem mass spectrometry (GC-MS/MS) can be more sensitive than GC-ECD for certain pesticides, we revisited one site in 2001 and analyzed these ACMs with GC-MS/MS. ACMs contained trace or undetectable levels of pesticides in 1999 and 2001, respectively. Based on chemical levels in ACMs and numbers of ACMs a bear can consume, we calculated the potential of chemicals to reach physiological toxicity. These calculations indicate bears do not consume physiologically toxic levels of pesticides and allay concerns they are at risk from pesticides transported by ACMs. If chemical control of ACMs changes in the future, screening new ACM samples taken from bear foraging sites may be warranted.

  15. Analysis of diazinon pesticide using potentiometric biosensor based on enzyme immobilized cellulose acetate membrane in gold electrode

    Mashuni; Ramadhan, L. O. A. N.; Jahiding, M.; Herniati

    2016-02-01

    Biosensor for analysis of diazinon pesticide using Potentiometric transducer has been developed. The basic element of this biosensor was a gold electrode modified with an immobilized acetylcholinesterase enzyme layer formed by entrapment with glutaraldehyde crosslinked-cellulose acetate. The aim of the research is to determine the composition of glutaraldehyde crosslinked-cellulose acetate in the gold electrode which provide optimum performance of biosensors of diazinon pesticide analysis on characterization include a range of working concentration, sensitivity, and detection limit. The results showed the composition of the cellulose acetate 15% and glutaraldehyde 25% that obtain optimum performance in the measurement of diazinon pesticide with a range of working concentration of 10-6 ppm to 1 ppm, the value of sensitivity 20.275 mV/decade and detection limit 10-6 ppm. The use of cellulose acetate provides highly sensitive devices allowing the efficient analysis of pesticides. The response time of electrode is on the measurement of pesticide diazinon with concentration variation of 10-6 ppm to 1 ppm with response time is about 5 minutes.

  16. 酶试剂法快速检测常用农药残留的比较研究%Comparative Study on Enzyme Reagent Method for Rapid Detection of Common Pesticide Residues

    易涛; 赵明明; 路磊; 丁华; 周有祥; 李书谦

    2012-01-01

    根据果蔬中农药残留检出的实际情况,采用市场上的3个商品化农残酶速测试剂盒对常见农药(水胺硫磷、敌敌畏、呋喃丹、毒死蜱、三唑磷、灭多威、氯氟氰菊酯、甲氰菊酯、百菌清、腐霉利和三唑酮)进行了灵敏度试验.结果表明,酶试剂对腐霉利、氯氟氰菊酯、甲氰菊酯、百菌清、三唑酮5种农药无抑制反应或灵敏度较差,而对其余6种农药的反应较为灵敏,其灵敏度依次为敌敌畏、呋喃丹、三唑磷、毒死蜱、水胺硫磷和灭多威.%The common residue of pesticides in fruits and vegetables, including isocarbophos, dichlorvos, carbofuran, chlor-pyrifos, triazophos, methomyl, cyhalothrin, fenpropathrin, chlorothalonil, procymidone and triazolone, were analyzed by the 3 commercial enzyme inhibition kits with the pesticide residue rapid analyzer The results showed that any enzyme reagent inhibition kit was not sensitive to procymidone, cyhalothrin, fenpropathrin, chlorothalonil and triazolone, it was only sensitive to six pesticides, the sensitivity to the six pesticides in order was dichlorvos, carbofuran, triazophos, chlorpyrifos, isocarbophos and methomyl.

  17. GC/MS方法分析豇豆中水胺硫磷等37种农药残留%Determination of 37 pesticides residues included Isocarbophos in cowpeas by GC/MS

    易盛国; 杨晓凤; 侯雪; 韩梅

    2011-01-01

    A method based on GC/MS was developed to detect 37 pesticides residues included isocarbophos in cowpeas. Pesticides were extracted with acetonitrile, cleaned up by an NH2/CARBON SPE column, separated on a capillary column (HP-5MS, 30 m ×0. 25 mm ×0. 25 μm) and determined with GC/MS/SIM. The linear ranges of the determination were 0. 020 ~0. 500 mg/L (r2 >0. 99). The recoveries of all pesticides were in the range of 73% ~ 126% with RSD (n =3) of 4. 3% ~ 14% at the spiked level of 0. 10 mg/kg. This method is suitable for the detection of multi-pesticide residues in cowpeas.%建立了GC/MS法同时测定豇豆中水胺硫磷等37种农药残留的方法.农药经过乙腈提取,NH2/CARBON复合固相萃取小柱净化,HP-5MS(30 m×0.25 mm×0.25 μm)弹性石英毛细管柱分离后,用GC/MS选择离子模式进行测定.农药在0.020~0.500 mg/L时与峰面积有良好的线性关系(r2>0.990).农药在0.10 mg/kg的添加水平时,回收率为73%~126%,RSD(n=3)为4.3%~14%.方法适用于豇豆中多种农药残留的测定要求.

  18. Image Analysis to Estimate Mulch Residue in Soil

    Carmen Moreno

    2014-01-01

    Full Text Available Mulching is used to improve the condition of agricultural soils by covering the soil with different materials, mainly black polyethylene (PE. However, problems derived from its use are how to remove it from the field and, in the case of it remaining in the soil, the possible effects on it. One possible solution is to use biodegradable plastic (BD or paper (PP, as mulch, which could present an alternative, reducing nonrecyclable waste and decreasing the environmental pollution associated with it. Determination of mulch residues in the ground is one of the basic requirements to estimate the potential of each material to degrade. This study has the goal of evaluating the residue of several mulch materials over a crop campaign in Central Spain through image analysis. Color images were acquired under similar lighting conditions at the experimental field. Different thresholding methods were applied to binarize the histogram values of the image saturation plane in order to show the best contrast between soil and mulch. Then the percentage of white pixels (i.e., soil area was used to calculate the mulch deterioration. A comparison of thresholding methods and the different mulch materials based on percentage of bare soil area obtained is shown.

  19. Determination of organophosphorus pesticides residues in carrot juice by SBSE -LC -MS/MS%SBSE -LC -MS/MS 法检测胡萝卜汁中有机磷农药残留

    倪永付; 闫秋成; 王勇; 朱莉萍; 高洁

    2015-01-01

    建立了搅拌棒吸附萃取(SBSE)—液相色谱串联质谱法检测胡萝卜汁中有机磷农药残留。样品经搅拌棒萃取,解析液解析后,上机检测。采用 ZORBAX Eclipse Plus C18色谱柱分离,在多反应监测模式下进行检测,用外标法定量。结果表明:3种有机磷药物在浓度0.5~50μg/L 范围内线性关系良好,相关系数 r =0.9953~0.9999,方法检测限为0.5μg/kg。在不同添加水平下,其平均回收率为86.8%~95%,变异系数为4.3%~12.8%。%The organophosphorus pesticides residues in carrot juice was determined by stir bar sorptive extraction (SBSE)combining with liquid chromatography -tandem mass spectrometry.The sample was extracted by SBSE.After being desorbed,the sample was performed on ZORBAX Eclipse Plus C18 col-umn.The analysis was carried out in the multiple reaction monitoring mode and external standard method was used for quantification.The calibration curve of the three organophosphorus pesticides showed a good linear relationship as concentrations in the range of 0.5 ~50 μg/L with the correlation coefficient r =0.995 3~0.999 9,the detection limit of this method was 0.5 μg/kg.In different concentrations,the average recovery rate of this method was 86.8% ~95% and the coefficient of variation 4.3% ~12.8%.

  20. Determination of Pesticide Residues in Honeybees using Modified QUEChERS Sample Work-Up and Liquid Chromatography-Tandem Mass Spectrometry

    Żaneta Bargańska

    2014-03-01

    Full Text Available Increasing emissions of chemical compounds to the environment, especially of pesticides, is one of factors that may explain present honeybee colony losses. In this work, an analytical method employing liquid chromatography-tandem mass spectrometry (LC-MS/MS was optimized for the simultaneous screening of 19 pesticides which have not been yet determined in honeybee samples from northern Poland (Pomerania. The sample preparation, based on the QuEChERS method combining salting-out liquid-liquid extraction to acetonitrile and a dispersive-SPE clean-up, was adjusted to honeybee samples by adding a small amount of hexane to eliminate beeswax. The recovery of analytes ranged from 70% to 120% with relative standard deviation ≤20%. The limits of detection were in the range of 0.91–25 ng/g. A total of 19 samples of honeybees from suspected pesticide poisoning incidents were analyzed, in which 19 different pesticides were determined.

  1. Progress in the biodegradation of pyrethroid pesticides residues by microorganism%微生物降解拟除虫菊酯类农药残留的研究进展

    冯海燕; 崔志峰

    2011-01-01

    随着拟除虫菊酯类农药使用量不断增加,产生的农药残留问题对生态环境和人类健康造成了危害.对降解拟除虫菊酯类农药的微生物种类、降解酶和降解机制及降解酶基因克隆和构建工程菌等方面进行综述,旨在为研究和开发微生物降解拟除虫菊酯类农药残留提供参考.%Pyrethroid insecticide is widely used in agriculture which bringing great benefits to the agricultural production. With the rapidly increase of pyrethroid requirement, the residues has bring hazard to ecological environment and human health. Biodegradation the pesticide residues by microorganisms is an appropriate way to solve this problem. In this paper.recent progress in microbial degradation of pyrethroid pesticide residues were reviewed,including the microbial species, pyrethroid-degrading enzymes,degradation mechanisms and the construction of genetically engineered microorganisms. This paper would provide some references for the advanced research and exploitation of pyrethroid biodegradation.

  2. Quantifying Residual Stresses by Means of Thermoelastic Stress Analysis

    Gyekenyesi, Andrew L.; Baaklini, George Y.

    2001-01-01

    This study focused on the application of the Thermoelastic Stress Analysis (TSA) technique as a tool for assessing the residual stress state of structures. TSA is based on the fact that materials experience small temperature changes when compressed or expanded. When a structure is cyclically loaded, a surface temperature profile results which correlates to the surface stresses. The cyclic surface temperature is measured with an infrared camera. Traditionally, the amplitude of a TSA signal was theoretically defined to be linearly dependent on the cyclic stress amplitude. Recent studies have established that the temperature response is also dependent on the cyclic mean stress (i.e., the static stress state of the structure). In a previous study by the authors, it was shown that mean stresses significantly influenced the TSA results for titanium- and nickel-based alloys. This study continued the effort of accurate direct measurements of the mean stress effect by implementing various experimental modifications. In addition, a more in-depth analysis was conducted which involved analyzing the second harmonic of the temperature response. By obtaining the amplitudes of the first and second harmonics, the stress amplitude and the mean stress at a given point on a structure subjected to a cyclic load can be simultaneously obtained. The experimental results showed good agreement with the theoretical predictions for both the first and second harmonics of the temperature response. As a result, confidence was achieved concerning the ability to simultaneously obtain values for the static stress state as well as the cyclic stress amplitude of structures subjected to cyclic loads using the TSA technique. With continued research, it is now feasible to establish a protocol that would enable the monitoring of residual stresses in structures utilizing TSA.

  3. Rapid determination of residues of pesticides in honey by µGC-ECD and GC-MS/MS: Method validation and estimation of measurement uncertainty according to document No. SANCO/12571/2013.

    Paoloni, Angela; Alunni, Sabrina; Pelliccia, Alessandro; Pecorelli, Ivan

    2016-01-01

    A simple and straightforward method for simultaneous determination of residues of 13 pesticides in honey samples (acrinathrin, bifenthrin, bromopropylate, cyhalothrin-lambda, cypermethrin, chlorfenvinphos, chlorpyrifos, coumaphos, deltamethrin, fluvalinate-tau, malathion, permethrin and tetradifon) from different pesticide classes has been developed and validated. The analytical method provides dissolution of honey in water and an extraction of pesticide residues by n-Hexane followed by clean-up on a Florisil SPE column. The extract was evaporated and taken up by a solution of an injection internal standard (I-IS), ethion, and finally analyzed by capillary gas chromatography with electron capture detection (GC-µECD). Identification for qualitative purpose was conducted by gas chromatography with triple quadrupole mass spectrometer (GC-MS/MS). A matrix-matched calibration curve was performed for quantitative purposes by plotting the area ratio (analyte/I-IS) against concentration using a GC-µECD instrument. According to document No. SANCO/12571/2013, the method was validated by testing the following parameters: linearity, matrix effect, specificity, precision, trueness (bias) and measurement uncertainty. The analytical process was validated analyzing blank honey samples spiked at levels equal to and greater than 0.010 mg/kg (limit of quantification). All parameters were satisfactorily compared with the values established by document No. SANCO/12571/2013. The analytical performance was verified by participating in eight multi-residue proficiency tests organized by BIPEA, obtaining satisfactory z-scores in all 70 determinations. Measurement uncertainty was estimated according to the top-down approaches described in Appendix C of the SANCO document using the within-laboratory reproducibility relative standard deviation combined with laboratory bias using the proficiency test data.

  4. Modelling pesticide volatilization after soil application using the mechanistic model Volt'Air

    Bedos, Carole; Génermont, Sophie; Le Cadre, Edith; Garcia, Lucas; Barriuso, Enrique; Cellier, Pierre

    Volatilization of pesticides participates in atmospheric contamination and affects environmental ecosystems including human welfare. Modelling at relevant time and spatial scales is needed to better understand the complex processes involved in pesticide volatilization. Volt'Air-Pesticides has been developed following a two-step procedure to study pesticide volatilization at the field scale and at a quarter time step. Firstly, Volt'Air-NH 3 was adapted by extending the initial transfer of solutes to pesticides and by adding specific calculations for physico-chemical equilibriums as well as for the degradation of pesticides in soil. Secondly, the model was evaluated in terms of 3 pesticides applied on bare soil (atrazine, alachlor, and trifluralin) which display a wide range of volatilization rates. A sensitivity analysis confirmed the relevance of tuning to K h. Then, using Volt'Air-Pesticides, environmental conditions and emission fluxes of the pesticides were compared to fluxes measured under 2 environmental conditions. The model fairly well described water temporal dynamics, soil surface temperature, and energy budget. Overall, Volt'Air-Pesticides estimates of the order of magnitude of the volatilization flux of all three compounds were in good agreement with the field measurements. The model also satisfactorily simulated the decrease in the volatilization rate of the three pesticides during night-time as well as the decrease in the soil surface residue of trifluralin before and after incorporation. However, the timing of the maximum flux rate during the day was not correctly described, thought to be linked to an increased adsorption under dry soil conditions. Thanks to Volt'Air's capacity to deal with pedo-climatic conditions, several existing parameterizations describing adsorption as a function of soil water content could be tested. However, this point requires further investigation. Practically speaking, Volt'Air-Pesticides can be a useful tool to make

  5. Image Analysis to Estimate Mulch Residual on Soil

    Moreno Valencia, Carmen; Moreno Valencia, Marta; Tarquis, Ana M.

    2014-05-01

    Organic farmers are currently allowed to use conventional polyethylene mulch, provided it is removed from the field at the end of the growing or harvest season. To some, such use represents a contradiction between the resource conservation goals of sustainable, organic agriculture and the waste generated from the use of polyethylene mulch. One possible solution is to use biodegradable plastic or paper as mulch, which could present an alternative to polyethylene in reducing non-recyclable waste and decreasing the environmental pollution associated with it. Determination of mulch residues on the ground is one of the basic requisites to estimate the potential of each material to degrade. Determination the extent of mulch residue on the field is an exhausting job while there is not a distinct and accurate criterion for its measurement. There are several indices for estimation the residue covers while most of them are not only laborious and time consuming but also impressed by human errors. Human vision system is fast and accurate enough in this case but the problem is that the magnitude must be stated numerically to be reported and to be used for comparison between several mulches or mulches in different times. Interpretation of the extent perceived by vision system to numerals is possible by simulation of human vision system. Machine vision comprising image processing system can afford these jobs. This study aimed to evaluate the residue of mulch materials over a crop campaign in a processing tomato (Solanum lycopersicon L.) crop in Central Spain through image analysis. The mulch materials used were standard black polyethylene (PE), two biodegradable plastic mulches (BD1 and BD2), and one paper (PP1) were compared. Meanwhile the initial appearance of most of the mulches was sort of black PE, at the end of the experiment the materials appeared somewhat discoloured, soil and/or crop residue was impregnated being very difficult to completely remove them. A digital camera

  6. Purification process of Industrialization preparation of pesticide residue grade n-hexane%农残级正己烷的产业化制备纯化工艺研究

    鄢雄伟; 全灿; 金君素; 黄挺; 李红梅

    2012-01-01

    以工业级正已烷为原料,通过脱色-连续精馏-过滤等一系列纯化工艺制备农残级正己烷,用紫外吸光度、纯度( GC-FID)和杂质峰高(GC-ECD)等检测值作为农残质量控制指标.产品质量与占当前国内垄断市场的进口试剂水平相当.通过试验确定了较为合适的工艺条件:二氧化硅为脱色剂,用量是原料质量的2%,然后用10%的蒸馏水水洗一次,连续精馏装置的导热油加热温度为98℃,脱轻塔和成品塔的回流比分别为10∶1和4∶1,重组分放料速率20 mL/min,产率可达70%左右.%Pesticide residue grade solvents have the characteristic of ultra high purity, low U V value, low pH value, low moisture content and low evaporation residue, which do not have those controlled impurity peak in pesticide chromato-graphic detection. This project funded by the China government, in which the industrialization process of pesticide residue grade n-hexane was studied, the industrial n-hexane as crude after purification approaches including decoloration,distillation and filtration. The optimized process parameters are: firstly utilizing 2% of silicon dioxide as decoloration agent then is rinsed with distilled water before distillation. The heating temperature of two distillation towers is 88 ℃ with reflux ratio of 10:1 and 4:1 for both respectively, the discharge rate of heavy component is 20 mLAnin.the yield is approximately 70%. This patented technique will meet pesticide residue grade n-hexane market in China or globally.

  7. Conformational analysis of a flexible oligosaccharide using residual dipolar couplings.

    Tian, F; Al-Hashimi, H M; Craighead, J L; Prestegard, J H

    2001-01-24

    We present a new approach to the analysis of the conformational and the motional properties of an oligosaccharide, methyl 3,6-di-O-(alpha-D-mannopyranosyl)-alpha-D-mannopyranoside. The approach relies on an order matrix analysis of residual dipolar couplings in the solution state. By combining a number of different types of couplings, (1)D(CH), (2)D(CH), and D(HH), an order matrix is solved for each ring of the trimannoside. The resulting order parameters indicate the internal motion at the alpha (1,3) linkage to be limited, while significant motion is suggested at the alpha (1,6) linkage. Two structures for the trimannoside were determined by aligning the order tensor principal axes obtained from two different orienting media, bicelles and phage. The very similar conformations at the alpha (1,3) linkage of these two structures confirm that the internal motion at the alpha (1,3) linkage is small and the conformation is a good representation of a single preferred structure. The different conformations at the alpha (1,6) linkage suggest that the motional amplitudes are large and the conformations must be viewed as virtual conformers. Compared with traditional NMR methods, data acquisition is easy and data analysis is straightforward.

  8. Comparative Proteomic Analysis of Carbonylated Proteins from the Striatum and Cortex of Pesticide-Treated Mice

    Coughlan, Christina; Walker, Douglas I.; Lohr, Kelly M.; Richardson, Jason R.; Saba, Laura M.; Caudle, W. Michael; Fritz, Kristofer S.; Roede, James R.

    2015-01-01

    Epidemiological studies indicate exposures to the herbicide paraquat (PQ) and fungicide maneb (MB) are associated with increased risk of Parkinson's disease (PD). Oxidative stress appears to be a premier mechanism that underlies damage to the nigrostriatal dopamine system in PD and pesticide exposure. Enhanced oxidative stress leads to lipid peroxidation and production of reactive aldehydes; therefore, we conducted proteomic analyses to identify carbonylated proteins in the striatum and cortex of pesticide-treated mice in order to elucidate possible mechanisms of toxicity. Male C57BL/6J mice were treated biweekly for 6 weeks with saline, PQ (10 mg/kg), MB (30 mg/kg), or the combination of PQ and MB (PQMB). Treatments resulted in significant behavioral alterations in all treated mice and depleted striatal dopamine in PQMB mice. Distinct differences in 4-hydroxynonenal-modified proteins were observed in the striatum and cortex. Proteomic analyses identified carbonylated proteins and peptides from the cortex and striatum, and pathway analyses revealed significant enrichment in a variety of KEGG pathways. Further analysis showed enrichment in proteins of the actin cytoskeleton in treated samples, but not in saline controls. These data indicate that treatment-related effects on cytoskeletal proteins could alter proper synaptic function, thereby resulting in impaired neuronal function and even neurodegeneration. PMID:26345149

  9. Comparative Proteomic Analysis of Carbonylated Proteins from the Striatum and Cortex of Pesticide-Treated Mice

    Christina Coughlan

    2015-01-01

    Full Text Available Epidemiological studies indicate exposures to the herbicide paraquat (PQ and fungicide maneb (MB are associated with increased risk of Parkinson’s disease (PD. Oxidative stress appears to be a premier mechanism that underlies damage to the nigrostriatal dopamine system in PD and pesticide exposure. Enhanced oxidative stress leads to lipid peroxidation and production of reactive aldehydes; therefore, we conducted proteomic analyses to identify carbonylated proteins in the striatum and cortex of pesticide-treated mice in order to elucidate possible mechanisms of toxicity. Male C57BL/6J mice were treated biweekly for 6 weeks with saline, PQ (10 mg/kg, MB (30 mg/kg, or the combination of PQ and MB (PQMB. Treatments resulted in significant behavioral alterations in all treated mice and depleted striatal dopamine in PQMB mice. Distinct differences in 4-hydroxynonenal-modified proteins were observed in the striatum and cortex. Proteomic analyses identified carbonylated proteins and peptides from the cortex and striatum, and pathway analyses revealed significant enrichment in a variety of KEGG pathways. Further analysis showed enrichment in proteins of the actin cytoskeleton in treated samples, but not in saline controls. These data indicate that treatment-related effects on cytoskeletal proteins could alter proper synaptic function, thereby resulting in impaired neuronal function and even neurodegeneration.

  10. Transport of bromide and pesticides through an undisturbed soil column: A modeling study with global optimization analysis

    Dusek, Jaromir; Dohnal, Michal; Snehota, Michal; Sobotkova, Martina; Ray, Chittaranjan; Vogel, Tomas

    2015-04-01

    The fate of pesticides in tropical soils is still not understood as well as it is for soils in temperate regions. In this study, water flow and transport of bromide tracer and five pesticides (atrazine, imazaquin, sulfometuron methyl, S-metolachlor, and imidacloprid) through an undisturbed soil column of tropical Oxisol were analyzed using a one-dimensional numerical model. The numerical model is based on Richards' equation for solving water flow, and the advection-dispersion equation for solving solute transport. Data from a laboratory column leaching experiment were used in the uncertainty analysis using a global optimization methodology to evaluate the model's sensitivity to transport parameters. All pesticides were found to be relatively mobile (sorption distribution coefficients lower than 2 cm3 g- 1). Experimental data indicated significant non-conservative behavior of bromide tracer. All pesticides, with the exception of imidacloprid, were found less persistent (degradation half-lives smaller than 45 days). Three of the five pesticides (atrazine, sulfometuron methyl, and S-metolachlor) were better described by the linear kinetic sorption model, while the breakthrough curves of imazaquin and imidacloprid were more appropriately approximated using nonlinear instantaneous sorption. Sensitivity analysis suggested that the mo