WorldWideScience
 
 
1

QA/QC in pesticide residue analysis  

International Nuclear Information System (INIS)

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

2

Development of soybean certified reference material for pesticide residue analysis.  

Science.gov (United States)

A soybean certified reference material for pesticide residue analysis was developed by the National Metrology Institute of Japan. Three organophosphorus (diazinon, fenitrothion, chlorphyrifos) and one pyrethroid (permethrin) pesticides were sprayed on soybeans three times before harvest. These soybeans were freeze pulverized, homogenized, bottled, and sterilized by ?-irradiation to prepare the candidate material. Three isotope-dilution mass spectrometric methods that varied in terms of the solvents used for extraction of the target pesticides, the clean-up procedure, and the injection techniques and columns used for quantification via gas chromatography/mass spectrometry were applied to the characterization. Each target pesticide was quantified by two of these analytical methods, and the results were in good agreement. Homogeneity and stability assessment of the material demonstrated that the relative standard uncertainties due to the inhomogeneity and the instability for an expiry date of 55 months were 1.89-4.00% and 6.65-11.5%, respectively. The certified pesticide concentrations with expanded uncertainties (coverage factor k=2, approximate 95% confidence interval) calculated using the results of the characterization and the homogeneity and stability assessment were 21.7 ± 3.2 ?g/kg for diazinon, 88 ± 21 ?g/kg for fenitrothion, 11.1 ± 3.2 ?g/kg for chlorpyrifos, and 20.1 ± 4.3 ?g/kg for permethrin (as the sum of the constituent isomers). PMID:24401412

Yarita, Takashi; Otake, Takamitsu; Aoyagi, Yoshie; Kuroda, Youko; Numata, Masahiko; Iwata, Hitoshi; Watai, Masatoshi; Mitsuda, Hitoshi; Fujikawa, Takashi; Ota, Hidekazu

2014-02-01

3

Pesticide residue analysis of storm-drain waters, 1975  

Energy Technology Data Exchange (ETDEWEB)

Runoff-water samples for the first, third, and fourth quarters of 1975 were analyzed for pesticide residues at LLL and independently by the LFE Environmental Analysis Laboratories. For the compounds analyzed, upper limits to possible contamination were placed conservatively at the low parts-per-billion level. In addition, soil samples were also analyzed. Future work will continue to include quarterly sampling and will be broadened in scope to include quantitative analysis of a larger number of compounds. A study of recovery efficiency is planned. Because of the high backgrounds on soil samples together with the uncertainties introduced by the cleanup procedures, there is little hope of evaluating the distribution of a complex mixture of pesticides among the aqueous and solid phases in a drainage sample. No further sampling of soil from the streambed is therefore contemplated.

Distler, T. M.; Wong, C. M.

1976-03-12

4

Evaporated extracts of samples for pesticide residue analysis simplifies transport from remote places  

Digital Repository Infrastructure Vision for European Research (DRIVER)

The increasing use of pesticides demands a world-wide control of residue levels in food and the environment. However, pesticide residue analysis is challenging and needs both experience and instrumentation. Although much can be done with fairly simple means, many countries with limited resources can only perform certain analyses. Also in technologically more advanced countries, different laboratories may specialize in certain kinds of analyses and there is also a need to confirm results with ...

Terenius, Olle; A?kerblom, Malin

1997-01-01

5

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

Directory of Open Access Journals (Sweden)

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

S. Islam

2009-01-01

6

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

Directory of Open Access Journals (Sweden)

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

Sheheli Islam

2009-01-01

7

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

Science.gov (United States)

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

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

2005-01-01

8

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

Science.gov (United States)

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

Mastovská, Katerina; Lehotay, Steven J

2004-06-25

9

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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...

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

2013-01-01

10

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

International Nuclear Information System (INIS)

an 20%, except below 0.2 Rf, where the CVRf rapidly increased with decreasing Rf values. The fungi spore inhibition, chloroplast inhibition and enzyme inhibition were found most suitable for detection of pesticides primarily for confirming their identity or screening for known substances. Their use for determination of pesticide residues in samples of unknown origin is not recommended. (author)

11

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

International Nuclear Information System (INIS)

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

12

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

Science.gov (United States)

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

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

2014-07-01

13

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

International Nuclear Information System (INIS)

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

14

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

Science.gov (United States)

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

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

2014-07-01

15

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

Directory of Open Access Journals (Sweden)

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

Seema Tahir

1999-01-01

16

Pesticide residues in locally available cereals and vegetables  

International Nuclear Information System (INIS)

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

17

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

Directory of Open Access Journals (Sweden)

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

Raquel Garcia

2011-12-01

18

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

Science.gov (United States)

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

Esturk, Okan; Yakar, Yasin; Ayhan, Zehra

2014-03-01

19

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

Science.gov (United States)

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

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

2013-05-01

20

Validation of thin lay chromatographic screening methods for pesticide residue analysis  

International Nuclear Information System (INIS)

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

 
 
 
 
21

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

Science.gov (United States)

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) (pretilachlor, and ?-cyhalothrin were also found as BDL (<0.001-0.05 ?g/g) in 40 samples of Basmati rice grains and soil and 12 water samples (<0.001-0.05 ?g/L) (2010-2011). PMID:25213562

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

2014-12-01

22

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

Raquel Garcia; Maria João Cabrita; Ana Maria Costa Freitas

2011-01-01

23

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

Directory of Open Access Journals (Sweden)

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.

DRAGAN MARKOVIC

2007-08-01

24

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

Science.gov (United States)

Ten systemic pesticides, comprising methomyl, thiamethoxam, acetamiprid, carbofuran, fosthiazate, metalaxyl, azoxystrobin, diethofencarb, propiconazole, and difenoconazole, were detected in 13 baby foods (cereals, boiled potatoes, fruit and milk) using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) for sample preparation and liquid chromatography tandem mass spectrometry for analysis. The matrix-matched calibration curves showed good linearity with determination coefficients (R(2) )?>0.992. The limits of detection and quantitation were 0.0015-0.003 and 0.005-0.01 mg/kg, respectively. The mean recoveries of three different concentrations ranged from 69.2 to 127.1% with relative standard deviations <20%. The method was successfully applied to 13 actual samples collected from a local market, and none of the samples were found to contain pesticide residues. This method is suitable for the identification and quantification of systemic pesticides with matrix-matched standards in various baby foods. PMID:24861738

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

2014-06-01

25

The 49th annual Florida Pesticide Residue Workshop.  

Science.gov (United States)

The papers in this special issue of Journal of Agricultural and Food Chemistry were originally presented at the 49th annual Florida Pesticide Residue Workshop (FPRW). The FPRW is an annual meeting for scientists specializing in trace level analysis of pesticides, veterinary drug residues, and other chemical contaminants in food, animal feed, and environmental samples. PMID:23282283

Turnipseed, Sherri B; Romano, Joe

2013-03-13

26

Gas chromatographic-tandem mass spectrometric analysis of pesticides residues in produce using concurrent solvent recondensation-large volume injection.  

Science.gov (United States)

In the present work, the feasibility of the combined use of concurrent solvent recondensation-large volume injection (CSR-LVI) and interspersed calibration for pesticide residue analysis was investigated. Splitless injections of 5-20 ?L extracts containing 0.25-1g sample per mL(-1) were made into a Carbofrit packed liner and a 0.53 mm I.D., uncoated and deactivated retention gap. The determination was achieved by gas chromatography-tandem quadrupole mass spectrometry (GC-QqQ-MS/MS). The evaluation of the proposed approach was based on analysis of real samples representing a diverse range of commodities such as apples, barley malt, blackcurrants, carrots, clemetines, grapes, leek, plums, rapeseed (green plants) rucola, strawberries and tomatoes. The samples contained a total of 36 different incurred pesticides at different concentration levels. Also, analyses were carried out of artificial samples representing six differing matrices (apples, blackcurrants, carrots, huckleberry, strawberry and tomatoes) which were spiked with pesticides at known concentrations before proceeding with the extraction. When using 15 and 20 ?L CSR-LVI injection, a decrease of about 30% in peak heights compared with injection of 5 ?L was observed. In the case of 5 and 10 ?L injections, no significant difference was observed when employing to the quantification of the incurred and spiked pesticide residues. In the evaluated experimental variants, overall recoveries of the pesticides were 92 ± 5% with relative standard deviations of 12 ± 4% on average. All individual recoveries were in the range between 72 and 103 with RSD between 4 and 21%. About 15% of the instrument run time was saved by the application of interspersed calibration with standards injected between sample extracts. PMID:22204933

Walorczyk, Stanis?aw

2012-01-27

27

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

Scientific Electronic Library Online (English)

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

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

2014-04-01

28

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

Scientific Electronic Library Online (English)

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

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

29

Pesticide Residues in Food: Your Daily Dose.  

Science.gov (United States)

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

Mott, Lawrie

1985-01-01

30

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

Directory of Open Access Journals (Sweden)

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

Zuin Vânia G.

2003-01-01

31

ESTIMATION OF THE BURDEN OF PESTICIDE RESIDUES IN SLOVAK POPULATION  

Directory of Open Access Journals (Sweden)

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

Jozef Sokol

2010-07-01

32

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

International Nuclear Information System (INIS)

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

33

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

Science.gov (United States)

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

Oellig, Claudia; Schwack, Wolfgang

2012-10-19

34

Determination of pesticide residues in cannabis smoke.  

Science.gov (United States)

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

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

2013-01-01

35

Considerations on the Content of Pesticides Residues in Vegetables  

Directory of Open Access Journals (Sweden)

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

Florica Morar

2011-06-01

36

Analysis of pesticide and veterinary drug residues in baby food by liquid chromatography coupled to Orbitrap high resolution mass spectrometry.  

Science.gov (United States)

Pesticide and veterinary drug residues have been simultaneously determined in several baby foods as meat, fish and vegetable-based baby food. A generic extraction method without clean-up step was applied. Moreover, the use of a representative matrix for proper quantification of all target compounds was studied and the best results were obtained when vegetable-based baby food was used as representative matrix, allowing the reliable quantification of more than 300 compounds. The method was validated and good recoveries were obtained for most of compounds at concentrations higher than 50 µg kg(-1). Limits of detection (LOD) ranged from 0.5 to 50 µg kg(-1), whereas limits of quantification (LOQ) were established between 10 and 100 µg kg(-1). Limits of identification (LOIs) ranged from 0.5 to 50 µg kg(-1). This method was applied to the analysis of 46 different baby food samples and no positive samples were found. PMID:25281065

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

2015-01-01

37

Pesticide Instrumental Analysis  

International Nuclear Information System (INIS)

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

38

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

Science.gov (United States)

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

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

2011-09-01

39

Pesticides residue levels in selected fruits from some Ghanaian markets  

International Nuclear Information System (INIS)

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

40

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

Science.gov (United States)

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

Oellig, Claudia; Schwack, Wolfgang

2014-07-18

 
 
 
 
41

Assessment of pesticide residues on selected vegetables of Pakistan  

International Nuclear Information System (INIS)

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

42

Streamlining sample preparation and gas chromatography-tandem mass spectrometry analysis of multiple pesticide residues in tea.  

Science.gov (United States)

In this work, a new rapid method for the determination of 135 pesticide residues in green and black dry tea leaves and stalks employing gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) with a triple quadrupole was developed and validated. A substantial simplification of sample processing prior to the quantification step was achieved: after addition of water to a homogenised sample, transfer of analytes into an acetonitrile layer was aided by the addition of inorganic salts. Bulk co-extracts, contained in the crude organic extract obtained by partition, were subsequently removed by liquid-liquid extraction using hexane with the assistance of added 20% (w/w) aqueous NaCl solution. The importance of matrix hydration prior to the extraction for achieving good recoveries was demonstrated on tea samples with incurred pesticide residues. For most of the analytes, recoveries in the acceptable range of 70-120% and repeatabilities (relative standard deviations, RSDs) ?20% were achieved for both matrices at spiking levels of 0.01, 0.1 and 1 mg kg(-1). Under optimised GC-MS/MS conditions, most of the analytes gave lowest calibration level ?0.01 mg kg(-1), permitting the control at the maximum residue levels (MRLs) laid down in Regulation (EC) No 396/2005. The developed method was successfully applied to the determination of pesticide residues in real tea samples. PMID:22882823

Cajka, Tomas; Sandy, Chris; Bachanova, Veronika; Drabova, Lucie; Kalachova, Kamila; Pulkrabova, Jana; Hajslova, Jana

2012-09-19

43

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

Science.gov (United States)

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

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

2013-01-01

44

Pesticide residues in oranges from Valencia (Spain).  

Science.gov (United States)

One hundred and fifty citrus samples from an agricultural co-operative of the Valencian Community (Spain) were analysed for pre- and post-harvest pesticide residues using high performance liquid chromatography and gas chromatography. Among the residues from post-harvest treatments, imazalil was detected in 112 (74.7%) samples at a mean level of 1.2 mg/kg, thiabendazole in 21 (14.0%) samples at a mean level of 0.47 mg/kg and carbendazim in 5 (3.3%) samples at a mean level of 1.05 mg/kg. Among the residues from pre-harvest treatment, dicofol was detected in 28 (18.7%) samples at a mean level of .28 mg/kg chlorpyriphos in 19 (12.7% samples at a mean level of 0.16 mg/kg and endosulfan in 11 (7.3%) at a mean level of 0.27 mg/kg. Most of the samples contained residues of various pesticides and six samples (4.0%) exceeded the European Union Maximum Residue Limit (MRL). The pesticides that surpassed the MRLs were chlorpyriphos in five samples and dicofol in one. PMID:11469317

Fernández, M; Picó, Y; Mañes, J

2001-07-01

45

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

Science.gov (United States)

...part 180 for residues of pesticide chemicals in or on various food commodities...regulations for residues of pesticides in or on food commodities...regulations for residues of pesticides in or on food...

2011-06-22

46

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

Science.gov (United States)

...regulations for residues of pesticide chemicals in or on the food commodity...part 180 for residues of pesticide chemicals in or on the food commodity...regulations for residues of pesticides in or on the food...

2012-10-17

47

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

Science.gov (United States)

...part 180 for residues of pesticide chemicals in or on various food commodities...regulations for residues of pesticides in or on food commodities...tolerances for residues of the biochemical pesticide, 2,6-diisopropylnaphthalene...following food and...

2012-05-04

48

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

Science.gov (United States)

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

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

2008-01-01

49

A multi-residue method for pesticide residue analysis in rice grains using matrix solid-phase dispersion extraction and high-performance liquid chromatography-diode array detection.  

Science.gov (United States)

Pesticides are widely used in rice cultivation, often resulting in detection of their residues in rice grains. So far, no analytical method has been available for the simultaneous determination of most rice pesticides in rice grains. This paper reports the development and validation of such a method for the determination of eight rice pesticides (penoxsulam tricyclazole, propanil, azoxystrobin, molinate, profoxydim, cyhalofop-butyl, deltamethrin) and 3,4-dichloroaniline, the main metabolite of propanil. Pesticide extraction and clean-up was performed by an optimized matrix solid-phase dispersion (MSPD) protocol on neutral alumina (5 g) using acetonitrile as the elution solvent. Samples were analyzed in a high-performance liquid chromatography-diode array detection (HPLC-DAD) system. Pesticide separation was achieved with a mobile phase of acetonitrile/water in a linear elution gradient from 30:70% (v/v) to 100:0% (v/v) in 14 min at a flow rate of 0.8 mL min(-1). Method validation was performed by means of linearity, intra-day accuracy, inter-day precision and sensitivity. Linear regression coefficients (R(2)) were always above 0.9948. Limits of detection (LOD) and quantification (LOQ) varied from 0.002 to 0.200 mg kg(-1) and 0.006 to 0.600 mg kg(-1), respectively. Recoveries were investigated at three fortification levels and were found to be acceptable (74-127%) with relative standard deviations (RSD) below 12%. Application of the method for the analysis of five commercial rice grain samples showed that the pesticide levels were below the LOD. Overall, the method developed is suitable for the determination of residues of most rice pesticides in rice grains at levels below the established MRLs. PMID:20379813

Tsochatzis, Emmanouil D; Menkissoglu-Spiroudi, Urania; Karpouzas, Dimitrios G; Tzimou-Tsitouridou, Roxani

2010-07-01

50

Pesticide residue analysis in cereal-based baby foods using multi-walled carbon nanotubes dispersive solid-phase extraction.  

Science.gov (United States)

In the present study, a new analytical method has been developed for the simultaneous quantification of 15 organophosphorus pesticides, including some of their metabolites, (disulfoton-sulfoxide, ethoprophos, cadusafos, dimethoate, terbufos, disulfoton, chlorpyrifos-methyl, malaoxon, fenitrothion, pirimiphos-methyl, malathion, chlorpyrifos, terbufos-sulfone, disulfoton-sulfone and fensulfothion) in three different types of commercial cereal-based baby foods. Dispersive solid-phase extraction (dSPE) with multi-walled carbon nanotubes (MWCNTs) was used together with gas chromatography with nitrogen phosphorus detection. Most favorable conditions involved a previous ultrasound-assisted extraction of the sample with acetonitrile containing formic acid. After evaporation of the extract and redissolution in water, a dSPE procedure was carried out with MWCNTs. The whole method was validated in terms of repeatability, linearity, precision and accuracy and matrix effect was also evaluated. Absolute recoveries were in the range 64-105 % with relative standard deviation values below 7.6 %. Limits of quantification achieved ranged from 0.31 to 5.50 ?g/kg, which were lower than the European Union maximum residue limits for pesticide residues in cereal-based baby foods. PMID:22623047

González-Curbelo, Miguel Angel; Asensio-Ramos, María; Herrera-Herrera, Antonio V; Hernández-Borges, Javier

2012-07-01

51

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

Directory of Open Access Journals (Sweden)

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.

Terence Centner

2014-05-01

52

Quick, easy, cheap, effective, rugged and safe method with magnetic graphitized carbon black and primary secondary amine as adsorbent and its application in pesticide residue analysis.  

Science.gov (United States)

By using magnetic graphitized carbon black and primary secondary amine (GCB/PSA/MNPs) as adsorbent, a modified quick, easy, cheap, effective, rugged and safe (QuEChERS) method was proposed for pesticide residue analysis in vegetables. The magnetic adsorbent was fabricated via simple co-mixing method based on an "aggregate warp" mechanism. To achieve the optimum conditions of modified QuEChERS toward target analytes, several parameters, including the composition of analyte protectants and the amount of the adsorbents were investigated. Under the optimized conditions, a simple, rapid and effective method for the determination of 10 pesticide residues in vegetables was established by coupling modified QuEChERS to gas chromatography/mass spectrometry analysis. The detection limits of the proposed method for 10 pesticides ranged from 0.39 to 8.6ng/g. Good linearity (R value?0.990) was achieved at concentration levels of 10-200ng/g, and acceptable method reproducibility was found as intra- and inter-day precisions, yielding the relative standard deviations less than 10.7% and 13.4%, respectively. The recoveries were in the range of 69.9-125.0% at different concentrations for real samples. Compared with the reported methods for the determination of a large number of samples, the proposed method has the advantage of less time-consuming in clean-up procedure. PMID:23659978

Zheng, Hao-Bo; Zhao, Qin; Mo, Jie-Zhen; Huang, Yun-Qing; Luo, Yan-Bo; Yu, Qiong-Wei; Feng, Yu-Qi

2013-07-26

53

Progress on multi-residue determination of pesticides in food  

Directory of Open Access Journals (Sweden)

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

ZHU Pan

2013-02-01

54

Progress on multi-residue determination of pesticides in food  

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

Zhu, Pan; Miao, Hong; Du, Juan; Zhao, Yun-feng; Wu, Yong-ning

2013-01-01

55

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

Directory of Open Access Journals (Sweden)

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

Ogah C.O

2011-03-01

56

Quantification, confirmation and screening capability of UHPLC coupled to triple quadrupole and hybrid quadrupole time-of-flight mass spectrometry in pesticide residue analysis.  

Science.gov (United States)

The potential of three mass spectrometry (MS) analyzers (triple quadrupole, QqQ; time of flight, TOF; and quadrupole time of flight, QTOF) has been investigated and compared for quantification, confirmation and screening purposes in pesticide residue analysis of fruit and vegetable samples. For this purpose, analytical methodology for multiresidue determination of 11 pesticides, taken as a model, has been developed and validated in nine food matrices for the three mass analyzers coupled to ultra high pressure liquid chromatography. In all cases, limits of quantification around 0.01 mg/kg were reached, fulfilling the most restrictive case of baby-food analysis. Regarding absolute sensitivity, the lower limits of detection were obtained, as expected, for QqQ (100 fg), whereas slightly higher limits (300 fg) were obtained for both TOF and QTOF. Confirmative capacity of each analyzer was studied for each analyte based on the identification points (IPs) criterion, useful for a comprehensive comparison. QTOF mass analyzer showed the highest confirmatory capacity, although QqQ normally led to sufficient number of IPs, even at lower concentration levels. The potential of TOF MS was also investigated for screening purposes. To this aim, around 50 commercial fruits and vegetables samples were analyzed, searching for more than 400 pesticides. TOF MS proved to be an attractive analytical tool for rapid detection and reliable identification of a large number of pesticides thanks to the full spectrum acquisition at accurate mass with satisfactory sensitivity. This process is readily boosted when combined with specialized software packages, together with theoretical exact mass databases. Several pesticides (e.g. carbendazim in citrus and indoxacarb in grape) were detected in the samples. Further unequivocal confirmation of the identity was performed using reference standards and/or QTOF MS/MS experiments. PMID:20301091

Grimalt, Susana; Sancho, Juan V; Pozo, Oscar J; Hernández, Félix

2010-04-01

57

Research of pesticide residues on fruit by terahertz spectroscopy technology  

Science.gov (United States)

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

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

2011-11-01

58

Determination of organophosphorus pesticide residues in tomatoes by gas chromatography  

International Nuclear Information System (INIS)

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

59

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

Science.gov (United States)

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

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

2014-12-15

60

76 FR 22067 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...  

Science.gov (United States)

...biochemical pesticide 9,10 anthraquinone, in or on corn, field...analysis for residues of anthraquinone, 1-hydroxyanthraquinone...was ``Residue Analysis of Anthraquinone on Corn (field) including...EPA-HQ-OPP-2010-0096). DSM Food Specialties B.V.,...

2011-04-20

 
 
 
 
61

Pesticide residues in honey samples from Himachal Pradesh (India).  

Science.gov (United States)

Honey, being a natural product manufactured by honey bees is considered to be free from any extraneous material. The over-reliance on pesticides caused several environmental problems including pesticide residues in food. This constitutes a potential risk for human health, because of their sub acute and chronic toxicity. Therefore this study was carried out to know the extent of pesticide residue in honey produced in the various parts of Himachal Pradesh. Among different pesticides analysed in honey; HCH and its isomers were the most frequently detected followed by DDT and its isomers. Of the studied synthetic pyrethroids, only cypermethrin was found in honey samples. Residues of organophosphates viz. acephate, chlorpyriphos, ethion and monocrotophos were not detected, however malathion's residue was found exceeding the MRL (5 ppb) proposed by the Ministry of Commerce, Government of India. More over honey from natural vegetation contained lesser residues. It can be concluded that honey from Himachal Pradesh had low pesticide residues. PMID:18506381

Choudhary, Amit; Sharma, Duni C

2008-05-01

62

Comparison of different sample pre-treatments for multi-residue analysis of organochlorine and pyrethroid pesticides in chrysanthemum by gas chromatography with electron capture detection.  

Science.gov (United States)

The widespread use of insecticides in Chinese herbal medicines has created a compelling need for the development of a multiresidue analytical method to help assure herbs safety. The operating variables affecting the performance of the multiresidue analysis of 34 organochlorine and 12 pyrethroid pesticides in chrysanthemum, a widely used kind of Chinese herbal medicines, were evaluated. Three different extraction solvents including n-hexane and its mixtures with acetone and petroleum ether were compared, and n-hexane was found to be an appropriate option. A combination of gel permeation chromatography and SPE was selected as the optimum cleanup, in comparison with dispersive SPE, or the two former methods alone. The determination of the 46 pesticide residues in the spiked chrysanthemum samples was performed by GC with electron capture detection. The average recoveries ranged from 71.3 to 102.6% with RSDs of 1.4-15.7% for all of the pesticides. The LOQs were in the range of 0.0015-0.2 mg/kg, while the LODs were between 0.0005 and 0.1 mg/kg. The satisfactory accuracy, and precision, in combination with a good separation and few interferences, have demonstrated the strong potential of this technique for its application in chrysanthemum analysis. PMID:23471658

Xue, Jiaying; Xu, Yanjun; Liu, Fengmao; Xue, Jian; Li, Huichen; Peng, Wei

2013-04-01

63

Simultaneous determination of 103 pesticide residues in tea samples by LC-MS/MS.  

Science.gov (United States)

A simple and sensitive method was developed and validated for the simultaneous determination of 103 pesticide residues in tea by LC-MS/MS. For the analysis of the pesticide with polarity, thermal lability or low volatility, this LC-MS/MS method has an advantage over GC. In this work, residual pesticides were extracted from the tea sample with ACN and then purified using Carb-NH(2) SPE cartridges. Using the multiple reaction monitoring mode, the pesticides were quantified and identified by the most abundant and characteristic fragment ions. The recoveries obtained for each pesticide ranged between 65 and 114% at three spiked concentration levels. The intra-day precisions were lower than 19.6%. Good linear relationships were observed with the correlation coefficients r(2) >0.996 for all analytes. The established method was successfully applied to the determination of pesticide residues in real tea samples. PMID:19399859

Huang, Zhiqiang; Zhang, Ying; Wang, Libing; Ding, Li; Wang, Meilin; Yan, Hongfei; Li, Yongjun; Zhu, Shaohua

2009-05-01

64

Determination of Pesticide Residues in Fresh and Greenhouse Vegetables  

Directory of Open Access Journals (Sweden)

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

M.H. Azizi

2008-04-01

65

Analysis of pesticides residues in environmental water samples using multiwalled carbon nanotubes dispersive solid-phase extraction.  

Science.gov (United States)

In this manuscript, a dispersive SPE method based on the use of multiwalled carbon nanotubes has been developed for the determination of 15 organophosphorus pesticides residues including some of their metabolites (disulfoton sulfoxide, ethoprophos, cadusafos, dimethoate, terbufos, disulfoton, chlorpyrifos-methyl, malaoxon, fenitrothion, pirimiphos-methyl, malathion, chlorpyrifos, terbufos sulfone, disulfoton sulfone, and fensulfothion) from real environmental waters (run-off, mineral and tap water) by GC with nitrogen phosphorus detection. Factors that affect the enrichment efficiency such as sample volume, multiwalled carbon nanotubes amount, and volume of eluent were studied. The optimized method was validated in terms of matrix-matched calibration, recovery, precision, and accuracy for the three analyzed samples. In this last case, the developed Student's t test demonstrated that there were no significant differences between real and spiked concentrations. Optimum dispersive SPE conditions (extraction of 200 mL of water, pH 6.0, with 130 mg of multiwalled carbon nanotubes, elution with 25 mL of dichloromethane for run-off and tap water and 30 mL for mineral water) allowed the quantitative extraction of analytes at levels lower than the maximum residues limits legislated by the European Union, with LODs between 1.16 and 93.6 ng/L. Absolute recovery values achieved were in the range of 67-107% (RSD values <10.1%). PMID:23303564

González-Curbelo, Miguel Ángel; Herrera-Herrera, Antonio V; Hernández-Borges, Javier; Rodríguez-Delgado, Miguel Ángel

2013-02-01

66

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

Science.gov (United States)

...part 180 for residues of pesticide chemicals in or on various food commodities...regulations for residues of pesticides in or on food various commodities...result in residues that are...additives, Food additives, Pesticides and...

2012-02-15

67

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

International Nuclear Information System (INIS)

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

68

Sample preparation method for the analysis of some organophosphorus pesticides residues in tomato by ultrasound-assisted solvent extraction followed by dispersive liquid-liquid microextraction.  

Science.gov (United States)

A very simple and economic method for organophosphorus pesticides (OPPs) residues analysis in tomato by means of gas chromatography-flame photometric detection (GC-FPD) has been developed. The method involves a rapid and small-scale extraction. The sample was homogenised and extraction of the OPPs with acetone was carried out assisted by sonication. No clean-up or evaporation were required after extraction. Pre-concentration of the OPPs from the acetone extract was done by using dispersive liquid-liquid microextraction (DLLME) technique. Chlorobenzene was added in micro-level volume as extraction solvent and triphenylphosphate as internal standard in DLLME procedure. The method showed good linearity over the range assayed (0.5-1000?gkg(-1)) and the detection limits for the pesticides studied varied from 0.1 to 0.5?gkg(-1). Repeatability studies resulted a relative standard deviation lower than 10% in all cases. The proposed method was used to determine pesticides levels in tomatoes grown in open field. PMID:25213965

Bidari, Araz; Ganjali, Mohammad Reza; Norouzi, Parviz; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub

2011-06-15

69

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

Science.gov (United States)

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

Oellig, Claudia; Schwack, Wolfgang

2011-09-16

70

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

Science.gov (United States)

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

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

2014-05-01

71

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

Science.gov (United States)

...174 or part 180 for residues of pesticide chemicals in or on various food commodities. EPA has...modification of regulations for residues of pesticides in or on food commodities. Further...requirement of a tolerance for residues of Bacillus...

2011-01-21

72

Distribution of multiple pesticide residues in apple segments after home processing  

DEFF Research Database (Denmark)

The effects of washing, storing, boiling, peeling, coring and juicing on pesticide residue were investigated for field-sprayed Discovery and Jonagold apples. Residues of chlorpyrifos, cypermethrin, deltamethrin, diazinon, endosulfan, endosulfan sulfate, fenitrothion, fenpropathrin, iprodione, kresoxim-methyl, lambda-cyhalothrin, quinalphos, tolylfluanid and vinclozolin in the processed apples were analysed by gas chromatography. Statistical analysis showed that reductions of 18-38% were required to obtain significant effects of processing practices, depending on pesticide and apple variety. Juicing and peeling the apples significantly reduced all pesticide residues. In the case of detectable pesticide residues, 1-24% were distributed in the juice and in the peeled apple. None of the pesticide residues was significantly reduced when the apples were subject to simple washing or coring. Storing significantly reduced five of the pesticide residues: diazinon, chlorpyrifos, fenitrothion, kresoxim-methyl and tolylfluanid, by 25-69%. Residues of the metabolite endosulfan sulfate were increased by 34% during storage. Boiling significantly reduced residues of fenitrothion and tolylfluanid by 32 and 81%, respectively. Only a few of the observed effects of processing could be explained by the physical or chemical characteristics of the pesticides. No differences in effect of processing due to apple variety were identified.

Rasmussen, Rie Romme; Poulsen, Mette Erecius

2003-01-01

73

Pesticide residues and bees--a risk assessment.  

Science.gov (United States)

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

Sanchez-Bayo, Francisco; Goka, Koichi

2014-01-01

74

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

Science.gov (United States)

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

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

2004-04-01

75

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

Science.gov (United States)

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

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

76

DRY–WET CYCLES INCREASE PESTICIDE RESIDUE RELEASE FROM SOIL  

Digital Repository Infrastructure Vision for European Research (DRIVER)

Soil drying and rewetting may alter the release and availability of aged pesticide residues in soils. A laboratory experiment was conducted to evaluate the influence of soil drying and wetting on the release of pesticide residues. Soil containing environmentally long-term aged (9–17 years) 14C-labeled residues of the herbicides ethidimuron (ETD) and methabenzthiazuron (MBT) and the fungicide anilazine (ANI) showed a significantly higher release of 14C activity in water extracts of previousl...

Jablonowski, Nicolai David; Linden, Andreas; Ko?ppchen, Stephan; Thiele, Bjo?rn; Hofmann, Diana; Burauel, Peter

2012-01-01

77

The 2010 European Union Report on Pesticide Residues in Food  

Digital Repository Infrastructure Vision for European Research (DRIVER)

This report presents the results of the control of pesticide residues in food commodities sampled during the calendar year 2010 in the 27 EU Member States and two EFTA countries (Iceland and Norway). The report also comprises the outcome of the consumer risk assessment of pesticide residues. EFSA presents for the first time the results of a pilot cumulative risk assessment (CRA) to multiple chemical residues. Finally, the report provides some recommendations aimed at the improvement of the fu...

European Food Safety Authority

2013-01-01

78

Public Health Implications of Pesticide Residues in Meat  

Directory of Open Access Journals (Sweden)

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

Jadhav V.J. and Waskar V.S.

2011-08-01

79

Pesticide residues in grain from Kazakhstan and potential health risks associated with exposure to detected pesticides.  

Science.gov (United States)

This paper presents the first study of pesticide residue results in grain from Kazakhstan. A total of 80 samples: barley, oat, rye, and wheat were collected and tested in the accredited laboratory. Among 180 pesticides, 10 active substances were detected. Banned pesticides, such as DDTs, ?-HCH, aldrin and diazinon were found in cereal grain. Chlorpyrifos methyl and pirimiphos methyl were the most frequently detected residues. No residues were found in 77.5% of the samples, 13.75% contained pesticide residues at or below MRLs, and 8.75% above MRLs. The greatest percentage of samples with residues (29%) was noted for wheat, and the lowest for rye (20%). Obtained data were used to estimate potential health risks associated with exposure to these pesticides. The highest estimated daily intakes (EDIs) were as follows: 789% of the ADI for aldrin (wheat) and 49.8% of the ADI for pirimiphos methyl (wheat and rye). The acute risk from aldrin and tebuconazole in wheat was 315.9% and 98.7% ARfD, respectively. The results show that despite the highest EDIs of pesticide residues in cereals, the current situation could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring of pesticide residues in grain is recommended. PMID:24316210

Lozowicka, B; Kaczynski, P; Paritova, Capital A Cyrillic ?; Kuzembekova, G B; Abzhalieva, A B; Sarsembayeva, N B; Alihan, K

2014-02-01

80

Removal of trace pesticide residues from farm produce  

International Nuclear Information System (INIS)

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

 
 
 
 
81

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

Science.gov (United States)

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

82

Survey on the pesticide residues in tea in south India.  

Science.gov (United States)

Tea is considered as a 'health beverage' due its antioxidant properties and resultant beneficial effects on human health. Such a beverage should be free from toxic elements such as pesticide residues and heavy metals. A large scale survey of teas produced in the tea factories of south India had been carried out for a period of three years from 2006 to 2008 and 912 tea samples were analysed for the residues of certain pesticides such as dicofol, ethion, quinalphos, hexaconazole, fenpropathrin, fenvalerate and propargite which are used for pest and disease control in tea in this part of the country. The analytical data proved that only less than 0.5 percentage of tea samples had residues of these pesticides. However, residues of pesticides were below their maximum limits in tea, stipulated by the European Union, Codex Alimentarius Commission of FAO/WHO and Prevention of Food Adulteration Act of Govt. of India. PMID:20640937

Seenivasan, Subbiah; Muraleedharan, NarayananNair

2011-05-01

83

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

Science.gov (United States)

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

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

2007-06-01

84

Proficiency test on incurred and spiked pesticide residues in cereals  

DEFF Research Database (Denmark)

A proficiency test on incurred and spiked pesticide residues in wheat was organised in 2008. The test material was grown in 2007 and treated in the field with 14 pesticides formulations containing the active substances, alpha-cypermethrin, bifentrin, carbendazim, chlormequat, chlorpyrifos-methyl, difenconazole, epoxiconazole, glyphosate, iprodione, malathion, pirimicarb, prochloraz, spiroxamin and trifloxystrobin. After harvest, the test material was additionally spiked in the laboratory with three pesticides, that where the residues were too low, and axozystrobin. In total, 72 laboratories submitted results and z-scores were calculated for all laboratories and pesticides, except for glyphosate where only five laboratories submitted results and summed weighted z-scores were calculated for the laboratories with a sufficient scope. For several pesticides, the submitted results were strongly depending on the extraction procedure and consequently the assigned values were calculated based on part of the results. Acceptable z-scores were obtained by 56-97% of the participants.

Poulsen, Mette Erecius; Christensen, Hanne Bjerre

2009-01-01

85

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

Science.gov (United States)

...for Residues of Pesticide Chemicals in or on Various Commodities...for residues of pesticide chemicals in or on various commodities...Federal Food, Drug, and Cosmetic Act (FFDCA), (21 U.S...for residues of pesticide chemicals in or on various food...

2013-11-27

86

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

Science.gov (United States)

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

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

2010-11-01

87

Monitoring of pesticide residues in South Indian tea.  

Science.gov (United States)

Tea is the most commonly consumed beverage in the world. Tea infusion is prepared by pouring boiling hot water over cured leaves of the Camellia sinensis plant. Such a beverage should be free from toxic chemicals. Studies on the monitoring of pesticide residues in tea of South India had been carried. Tea samples collected from different districts of South India were analysed for the residues of certain pesticide such as dicofol, ethion, quinalphos, hexaconazole, fenpropathrin, fenvalerate and propargite. These pesticides are commonly used for the control of pests and diseases in tea. The results of study indicated that among 468 samples examined, only one sample contained hexaconazole residue that exceeded the maximum residue limit (MRL). Though the residues of ethion, quinalphos, hexaconazole, dicofol, propargite and fenpropathrin were most commonly found, only one sample exceeded the MRL. PMID:23341056

Kottiappan, Madasamy; Dhanakodi, Kirubakaran; Annamalai, Satheshkumar; Anandhan, Shanmugaselvan Veilumuthu

2013-08-01

88

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

Science.gov (United States)

A comparison was made between the two versions of QuEChERS sample preparation method for the extraction of 66 organophosphorus pesticides (OPPS) in vegetables. The two QuEChERS methods were the original method without buffer published in 2003, and the AOAC Official Method 2007. 01 with acetate buffer. The adsorption behaviors of primary secondary amine (PSA) sorbent and C18 sorbent on the OPPS were studied. The method of after-extraction addition was used to evaluate matrix effects for OPPS in matrix of broccoli, tomato, green soybean, radish and shallot during liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. As a result, the QuEChERS method with acetate buffer gave higher and more consistent recoveries for some of OPPS. The PSA sorbent and C18 sorbent can adsorb dibrom, so the QuEChERS method was not suitable for the analysis of dibrom. The maximum matrix effects were in the extracts of broccoli during LC-MS/MS analysis. In this article, OPPS were extracted using the QuEChERS method with acetate buffer, and analysed by LC-MS/MS under the optimized conditions with monitoring 132 MS/MS transitions of precursor ions (two for each pesticide) in one single run. Recoveries for all but dibrom at fortification levels of 10, 40, 80 microg/kg in broccoli, tomato, green soybean, radish and shallot ranged from 55% to 122% with relative standard deviations of 1.6% - 18%. The limits of quantification (S/N > or = 10) were 0.1 - 8 microg/kg. Based on these results, the analytical method was proven to be highly efficient, robust and sensitive, and suitable for the monitoring of the maximum residue limits (MRLs) of 66 OPPS in vegetables. PMID:22679828

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

2012-02-01

89

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

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

2010-01-01

90

An optical instrument to test pesticide residues in agricultural products  

Science.gov (United States)

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

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

2005-10-01

91

Extraction of pesticide residues from biological and environmental samples  

International Nuclear Information System (INIS)

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

92

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

Directory of Open Access Journals (Sweden)

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

Kaipper Beatriz I. A.

2001-01-01

93

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

Energy Technology Data Exchange (ETDEWEB)

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

Kaipper, Beatriz I.A.; Madureira, Luiz A.S. [Santa Catarina Univ., Florianopolis, SC (Brazil). Dept. de Quimica]. E-mail: madureira@qmc.ufsc.br; Corseuil, Henry X. [Santa Catarina Univ., Florianopolis, SC (Brazil). Dept. de Engenharia Sanitaria

2001-07-01

94

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

DEFF Research Database (Denmark)

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

Poulsen, Mette Erecius; Rasmussen, Peter Have

2009-01-01

95

Residues of organochlorinated pesticides in soils from the Czech Republic  

International Nuclear Information System (INIS)

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

96

Pesticide residues in conventionally grown and organic New Zealand produce.  

Science.gov (United States)

A study was carried out to determine the prevalence and concentrations of pesticide residues in conventionally grown and organic produce (bananas, broccoli, grapes, lettuce, potatoes, tomatoes, wine). Sampling was stratified, with organic produce being over-sampled, when available. All food samples were analysed, as received, by a multi-residue pesticide residue screen. Residues were found in 130 of 307 conventionally grown food samples (42%) and in nine of 41 organic food samples (22%), including six of eleven (55%) organic tomato samples. Only four organic samples (9.8%) contained multiple residues, while 24% of conventionally grown food samples contained multiple residues. Nine conventionally grown food samples (2.6%) contained pesticide residues that exceeded the maximum residue limit (MRL). Where direct comparisons were possible between conventionally grown and organic produce, the mean concentration of residues was usually lower in the organic produce, but was generally higher than would be expected from spray drift or other adventitious sources. While the presence of these residues does not represent a significant risk to human health, their presence is inconsistent with consumer expectations for organic produce. PMID:24784963

Cressey, P; Vannoort, R; Malcolm, C

2009-01-01

97

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

Science.gov (United States)

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

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

2009-01-01

98

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

International Nuclear Information System (INIS)

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

99

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

International Nuclear Information System (INIS)

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

100

Analysis of pesticide residues in mixed fruit and vegetable extracts by direct sample introduction/gas chromatography/tandem mass spectrometry.  

Science.gov (United States)

Direct sample introduction (DSI), or "dirty sample injection," was investigated in the determination of 22 diverse pesticide residues in mixed apple, green bean, and carrot extracts by benchtop gas chromatography/tandem mass spectrometry (DSI/GC/MS-MS). The targeted pesticides, some of which were incurred in the samples, included chlorpyrifos, azinphos-methyl, parathion-methyl, diazinon, terbufos, p,p'-DDE, endosulfan sulfate, carbofuran, carbaryl, propargite, bifenthrin, dacthal, trifluralin, metalaxyl, pendimethalin, atrazine, piperonyl butoxide, diphenylamine, vinclozolin, chlorothalonil, quintozene, and tetrahydrophthalimide (the breakdown product of captan). The analytical DSI method entailed the following steps: (1) blend 30 g sample with 60 mL acetonitrile for 1 min in a centrifuge bottle; (2) add 6 g NaCl and blend 30 s; (3) centrifuge for 1-2 min; (4) add 5 mL upper layer to 1 g anhydrous MgSO4 in a vial; and (5) analyze 11 microL extract, using DSI/GC/MS-MS. Sample cleanup is not needed because GCIMS-MS is exceptionally selective for the targeted analytes, and nonvolatile coextracted matrix components do not contaminate the injector or the GC/MS-MS system. Average recoveries of the pesticides were 103 +/- 7% with relative standard deviations of 14 +/- 5% on average, and limits of detection were <2 ng/g for nearly all pesticides studied. The DSI/GC/ MS-MS approach for targeted pesticides is quantitative, confirmatory, sensitive, selective, rugged, rapid, simple, and inexpensive. PMID:10868593

Lehotay, S J

2000-01-01

 
 
 
 
101

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

Science.gov (United States)

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

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

2004-03-01

102

The 2010 European Union Report on Pesticide Residues in Food  

Directory of Open Access Journals (Sweden)

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

European Food Safety Authority

2013-03-01

103

Levels of Organochlorine Pesticide Residues in Grasscutter (Thryonomys swinderianus Tissues  

Directory of Open Access Journals (Sweden)

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

Sarah Blankson-Arthur

2011-06-01

104

Pesticide Residues Evaluation in Pulp, Juice and Nectar of Fruits  

Directory of Open Access Journals (Sweden)

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

Claudia Helena Pastor Ciscato

2012-04-01

105

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.  

Science.gov (United States)

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. PMID:24224899

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

106

Screening and evaluation of fruit samples for four pesticide residues.  

Science.gov (United States)

The occurrence of 4 pesticide residues, imidacloprid, carbendazim, methiocarb, and hexythiazox, was assessed in several fruits (oranges, tangerines, watermelons, and date plums) from the Valencian Community (Spain). A total of 227 samples--56 oranges, 134 tangerines, 13 watermelons, and 24 date plums--were taken from an agricultural cooperative representative of the area studied during 2001. The pesticides were determined by liquid chromatography/mass spectrometry after sample extraction with ethyl acetate and anhydrous sodium sulfate. Recoveries of 4 pesticides at 2 fortification levels (0.02 and 0.2 mg/kg), the lower of which was the quantification limit, ranged from 60 to 108%. Concentrations of imidacloprid, carbendazim, methiocarb, and hexythiazox ranged from 0.02 to 0.75 mg/kg in 184 samples (54 oranges, 119 tangerines, 3 watermelons, and 8 date plums). Nineteen samples contained methiocarb or hexythiazox residues that exceeded the maximum residue limits. Calculation of the estimated daily intakes of the 4 pesticides studied and their comparison with the Acceptable Daily Intakes established by the Food and Agriculture Organization of the World Health Organization demonstrated the safety of fruit consumption and showed the importance of monitoring for pesticide residues. PMID:16001861

Blasco, Cristina; Font, Guillermina; Mañes, Jordi; Picó, Yolanda

2005-01-01

107

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

Science.gov (United States)

...publication in the Pesticide Analytical Manual...06 ppm; pea, field, hay at 15 ppm; pea, field, vines at...TAED) and its degradation product diacetylethylenediamine...residues of the microbial insecticide...when used as a pesticide inert...

2013-10-25

108

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

Science.gov (United States)

...announcing the withdrawal of a pesticide petition received under section 408 of the Federal Food, Drug, and Cosmetic Act...part 174 or part 180 for residues of pesticide chemicals in or on various food commodities. Pursuant...

2011-11-09

109

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

International Nuclear Information System (INIS)

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

110

Occurrence of pesticide residues in Lebanon's water resources.  

Science.gov (United States)

Contamination of water sources by pesticides is one of the most critical environmental problems. The present work is designed to address the occurrence of 67 pesticides in the Lebanese waters. Chemical analysis was performed by a solid-phase extraction followed by a gas chromatography-mass spectrometry using programmed temperature vaporization injection. In drinking water and groundwater samples, organochlorine and organophosphate pesticides were frequently detected with a maximal sum concentration of up to 31.8 ng L(-1). High pesticide ecotoxicological risk was noticed in many surface waters, while this risk was driven mainly by diazinon, chlorpyrifos, fenpropathrin and bifenthrin insecticides. PMID:24008278

Kouzayha, Abir; Al Ashi, Aisha; Al Akoum, Rami; Al Iskandarani, Mohamad; Budzinski, Hélène; Jaber, Farouk

2013-11-01

111

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

Science.gov (United States)

...exemptions for pesticide residues in or on raw...or processed foods. 180.7...EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Procedural...levels of the pesticide chemical residue in or on the food, or for...

2010-07-01

112

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

Directory of Open Access Journals (Sweden)

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

Spiridon Kintzios

2008-04-01

113

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

Science.gov (United States)

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

Swarnam, T P; Velmurugan, A

2013-07-01

114

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

DEFF Research Database (Denmark)

The aim of this study was to investigate the amount of pesticide residues in fruits and vegetables from South America. A total of 724 samples of 46 different fruits and vegetables from eight South American countries were collected in 2007. In 19% of the samples no residues were found, 72% of samples contained pesticide residues at or below MRL, and 8.4% of samples contained pesticide residues above MRL. Thiabendazole, imazalil and chlorpyrifos were the pesticide most frequently found. Thirty-seven pesticides were found with frequencies higher that 1% in the samples. The results emphasize the need for continuous monitoring of pesticide residues, especially in imported fruits and vegetables.

Hjorth, Karen; Johansen, K.

2011-01-01

115

Reduction of pesticide residues in tomatoes and other produce.  

Science.gov (United States)

There is interest in reducing pesticide residues in fruits and vegetables in order to minimize human exposure. The objectives of this study were to (i) determine the effect of various washing treatments with and without sonication on pesticide removal from tomatoes and (ii) assess the effectiveness of a water wash on select samples using a produce-washing flume. In the first set of experiments, tomatoes were contaminated with acephate, malathion, carbaryl, bifenthrin, cypermethrin, permethrin, cyhalothrin, chlorothalonil, and imidacloprid and were dried overnight. Subsets of the tomatoes were then washed (10°C, 1 min) with one of the following: water, sodium hypochlorite (80 ?g/ml, pH 7), peroxyacetic acid (80 ?g/ml), or Tween 20 (0.1%) with and without sonication. In general, the effect of sonication depended on the washing treatment and on the pesticide. A separate experiment measured pesticide residues in contaminated samples before and after being washed in a flume (22°C, 1 min). Pesticide residues in contaminated produce were reduced from about 40 to 90% when washed for 1 min in the flume. PMID:23462090

Al-Taher, Fadwa; Chen, Yang; Wylie, Philip; Cappozzo, Jack

2013-03-01

116

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

Science.gov (United States)

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

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

2012-01-01

117

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

Scientific Electronic Library Online (English)

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

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

118

Pesticide residues in the soil of the Central Jordan Valley  

International Nuclear Information System (INIS)

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

119

Organochlorine Pesticide Residues in Fish Samples from Lagos Lagoon, Nigeria  

Directory of Open Access Journals (Sweden)

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

David Adeyemi

2008-01-01

120

Radiotracer studies of pesticide residues in stored products  

International Nuclear Information System (INIS)

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

 
 
 
 
121

Effects of different washing methods on pesticide organophosphorus residues  

Directory of Open Access Journals (Sweden)

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

WANG Xiao-Wei

2013-02-01

122

Dietary exposure to pesticide residues in Yaoundé: the Cameroonian total diet study.  

Science.gov (United States)

Dietary exposure to pesticide residues was assessed in Yaoundé, Cameroon, using the total diet study (TDS) method. Sixty-three composite samples, representative of the foods as consumed in Yaoundé, were collected, prepared, and analysed for residues of pesticides including organochlorine, organophosphorous, and pyrethroids. A multi-residue method was used with a limit of detection (LOD) of 0.005 mg kg(-1). Additional analyses were performed for dithiocarbamates (LOD=0.050 mg kg(-1)), glyphosate (LOD=0.005 mg kg(-1)) and chlordecone (LOD=0.0008 mg kg(-1)) on certain composites samples. The overall contamination was low with 37 out of 46 pesticides below the LOD in all samples. The estimated upper bound (for values less than the LOD equal the LOD; and values less than the LOQ equal the LOQ) of the mean dietary exposures ranged from 0.24% (cypermethrin) to 3.03% (pirimiphos-methyl) of the acceptable daily intakes (ADIs) for pesticides for which at least one analysis was greater than the LOD. This study suggests a low dietary exposure to pesticide residues in Yaoundé. PMID:18348045

Gimou, M-M; Charrondiere, U R; Leblanc, J-C; Pouillot, R

2008-04-01

123

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

International Nuclear Information System (INIS)

obtained from processing industries in Tema. Two extraction methods were used. The second extraction method was as by the QuEChERS method for vegetable oils which was used for the cocoa butter samples only, after being liquefied in water bath at 40 degrees celsius. The investigated pesticides consisted of fifteen organochlorine pesticides, thirteen organophosphorous pesticides and nine synthetic pyrethroids pesticides. Percentage recoveries ranged from 70-110 percent, with instrumental detection limits of 0.3ug/kg, 0.15ug/g and 0.15ug/g for the organochlorine, organophosphorous and synthetic pyrethroids pesticides respectively. Multivariate analysis on the residue data obtained from fermented dried cocoa beans in R-mode and Q-mode grouped the detected pesticides into currently used, previously used and drift from neighbouring crops pesticides applications. It also grouped sampled cocoa beans into four major clusters based on similarities in crop storage and farm practices. Beta-HCH (18.7 ?g/kg), Gamma-chlordane (152.0 ?g/kg), Methamidophos (18.5 ?g/kg), Profenofos (31.8 ?g/kg), Allethrin (10.5 ?g/kg), Cypermethrin (32.0 ?g/kg) and Fenvalerate (14.6 ?g/kg) were the average residues concentrations of pesticides that exceeded the Japanese maximum residue levels (MRLs). However, all the detected pesticides with exception of Allethrin were below the MRLs for European Union. From results recorded in semi-finished and finished cocoa beans products produced in Ghana, de-shelling and roasting temperatures drastically reduced the residue levels in the cocoa products, but these were not enough solution for pesticide residues in cocoa beans. And thus raises concern about the health implication of these chemicals for domestic consumption of these products. It is highly recommended that a national quality control laboratory be established to continually monitor pesticides efficacy in order to avoid overdose of pesticides application.[au

124

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

Directory of Open Access Journals (Sweden)

Full Text Available The basic principles and application possibilities of the methods based on solid phase microextraction (SPME in the analysis of pesticide residues in soil samples are presented in the paper. The most important experimental parameters which affect SPME efficacy inpesticide determination (type and thickness of microextraction fiber, duration of microextraction,temperature at which it is conducted, effect of addition of salts (the effect of efflorescence,temperature and time of desorption, the choice of optimal solvent for pesticide exctraction from the soil and the optimal number of extraction steps, as well as general guidelines for their optimization are also shown. In the end, current applications of SPMEmethods in the analysis of pesticide residues in soil samples are presented.

Rada ?urovi?

2011-01-01

125

[Rapid analysis of eight lipophilic pesticide residues in vegetables by dispersive liquid-liquid microextraction coupled with gas chromatography-tandem mass spectrometry].  

Science.gov (United States)

A novel method for rapid determination of eight lipophilic pesticides in vegetables was developed using dispersive liquid-liquid micro-extraction (DLLME) coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS). The analyte in the vegetable was extracted with water-acetone (5 : 1, v/v) solution. Then, the extract was transferred into a centrifugal tube with 25 mg primary secondary amine (PSA), 50 mg C18 and 25 mg graphitized carbon black powder. The important parameters that affected the extraction efficiency were studied, such as the extraction and dispersed solvents, and the extraction time. The results showed that a good extraction efficiency was obtained, with acetone used as the dispersed solvent and 50.0 microL chlorobenzene used as the extraction solvent. Under the optimum conditions, the enrichment factors ranged from 526 to 878. The linearity ranges of the eight targeted compounds were 0.005 - 10 mg/kg, and the limits of detection (signal/noise = 3) were 0.001 - 0.02 mg/kg, with the correlation coefficients varying from 0.992 1 to 0.998 9. The recoveries of the pesticides ranged from 60.1% to 82.5% with the relative standard deviations between 1.2% and 9.6%. The method has been used to analyze the eight lipophilic pesticide residues in vegetable samples with satisfactory results. PMID:23256389

Zhou, Min; Li, Wei; Du, Xiaoting; Xia, Zhongxing; Chen, Meichun

2012-08-01

126

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

Directory of Open Access Journals (Sweden)

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

Mohd Aslam

2013-08-01

127

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

Science.gov (United States)

Amine modified graphene is successfully synthesized via a one-pot solvothermal reaction between graphene oxide and ammonia water, methylamine or n-butyl amine. The presence of amine groups in graphene is identified by Fourier-transform infrared spectrometry, X-ray photoelectron spectroscopy and an X-ray diffractometer. The ability of amine modified graphene to cleanup fatty acids and other interfering substances from acetonitrile extracts of oil crops has been evaluated. It is found that the resulting CH3NH-G exhibits the best performance in interfering substances removal. Meanwhile, a multi-residue method is validated on 28 representative pesticide residues in four oil crops (rapeseed, peanut, sesame seeds and soybean). This method is based on modified QuEChERS sample preparation with CH3NH-G as reversed-dispersive solid phase extraction material and liquid chromatography-tandem mass spectrometry. Use of matrix-matched standards provides acceptable results for most pesticides with overall average recoveries between 70.5 and 100% and consistent RSDs70% recovery. PMID:23489497

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

2013-04-19

128

The Organochlorine Pesticides Residue Levels in Karun River Water  

Directory of Open Access Journals (Sweden)

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

Behrooz Jannat

2013-01-01

129

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

Science.gov (United States)

...section 408 of the Federal Food, Drug, and Cosmetic...part 174 or part 180 for residues of pesticide chemicals in or on various food commodities. EPA has...modification of regulations for residues of pesticides in or on food commodities....

2011-01-12

130

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

Science.gov (United States)

...section 408 of the Federal Food, Drug, and Cosmetic...part 174 or part 180 for residues of pesticide chemicals in or on various food commodities. EPA has...modification of regulations for residues of pesticides in or on food commodities....

2010-10-22

131

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

Science.gov (United States)

...section 408 of the Federal Food, Drug, and Cosmetic...part 174 or part 180 for residues of pesticide chemicals in or on various food commodities. EPA has...modification of regulations for residues of pesticides in or on food commodities....

2010-12-22

132

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

Science.gov (United States)

...section 408 of the Federal Food, Drug, and Cosmetic...in 40 CFR part 180 for residues of pesticide chemicals in or on various food commodities. The Agency...modification of regulations for residues of pesticides in or on food commodities....

2011-08-10

133

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

Science.gov (United States)

...section 408 of the Federal Food, Drug, and Cosmetic...in 40 CFR part 180 for residues of pesticide chemicals in or on various food commodities. The Agency...modification of regulations for residues of pesticides in or on food commodities....

2012-09-28

134

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

Science.gov (United States)

...section 408 of the Federal Food, Drug, and Cosmetic...part 174 or part 180 for residues of pesticide chemicals in or on various food commodities. The Agency...modification of regulations for residues of pesticides in or on food commodities....

2011-06-08

135

Simultaneous determination of 102 pesticide residues in Chinese teas by gas chromatography-mass spectrometry.  

Science.gov (United States)

An efficient and sensitive method for simultaneous determination of 102 pesticide residues in teas has been established and validated. The multi-residue analysis of the pesticides in teas involved extraction with acetone-ethyl acetate-hexane, clean-up using gel permeation chromatography (GPC) and solid-phase extraction (SPE), and subsequent identification and quantification of the selected pesticides by gas chromatography-mass spectrometry (GC-MS) under retention time locked (RTL) conditions. For most of the target analytes, the optimized pretreatment processes led to no significant interference on analysis from sample matrix, and the determination of 102 compounds was achieved in about 120 min. Pesticide residues could be determined in low sub-ppb range, from 0.01 microg/mL for hexachlorobenzene to 2.5 microg/mL for propargite, with average recoveries ranging from 59.7 to 120.9% (mean 88%) and relative standard deviations (RSDs) in the range 3.0-20.8% (mean 13.7%) for all analytes across three fortification tea levels. The limits of detection (LODs) were much lower than the maximum residue levels established by the European Union (EU) legislations. PMID:17400037

Huang, Zhiqiang; Li, Yongjun; Chen, Bo; Yao, Shouzhuo

2007-06-15

136

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

Directory of Open Access Journals (Sweden)

Full Text Available The multivariate analysis of variance MANOVA was used to analyze the data obtained from this study. No significant difference was shown between the concentrations of all parameters during four seasons and all stations based on MANOVA test. The total percentage of DDE, Kelthane, ?-BHC, and DDT detected in stations were 63, 56, 50 and 69% over the year, respectively. The maximum concentrations of ?-BHC (fall, kelthane (fall, DDE (spring and DDT (summer were 21.6, 15.4, 9.8 and 9.2µg/l, respectively. The minimum concentrations of kelthane, ?-BHC, DDE and DDT were 3, 3.1, 1.9 and 3µg/l in stations 1 (summer, 2 (fall, 3 (summer and 4 (summer, respectively. In this study, most of chemicals compounds were found in agricultural periods (spring and summer. During four seasons, the most percentage of chemicals compounds such as DDT (summer, ?-BHC (summer-fall, Kelthane (spring-summer and DDE (spring were 100, 75, 75 and 75%, respectively.

Sh. Najafpour

2010-07-01

137

Towards accreditation of MINT pesticide residue laboratory - a journey  

International Nuclear Information System (INIS)

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

138

Acetylcholinesterase Based Detection of Residual Pesticides on Cotton  

Directory of Open Access Journals (Sweden)

Full Text Available This study describes the measurement of bio-electrical signals caused by enzymatic inhibition of acetylcholinesterase (AChE for the detection of organophosphorous and carbamate pesticides which are the strong inhibitors of AChE and prevents its normal function of the rapid removal of acetylcholine (Ach. Biosensor Toxicity Analyzer (BTA was used for the testing and enzyme activity was determined by acetylthiocholine chloride (ATCCl as enzyme substrate. The monitoring of changes in bio-electrical signals caused by the interaction of biological substances and residues were evaluated. Two samples of cotton were analyzed. Cryogenic homogenization was carried out for sample pretreatment and Soxhlet extraction method (SOX was used for extraction. The resulted extracts were concentrated and then injected in the BTA. The method shows reasonable results and can successfully be utilized for the detection of residual pesticides on different types of cotton.

Jiri Militky

2012-02-01

139

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

Directory of Open Access Journals (Sweden)

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

B. ?ozowicka

2013-05-01

140

Optimization and evaluation of low-pressure gas chromatography-mass spectrometry for the fast analysis of multiple pesticide residues in a food commodity.  

Science.gov (United States)

A fast method of analysis for 20 representative pesticides was developed using low-pressure gas chromatography-mass spectrometry (LP-GC-MS). No special techniques for injection or detection with a common quadrupole GC-MS instrument were required to use this approach. The LP-GC-MS approach used an analytical column of 10 m x 0.53 mm I.D., 1 microm film thickness coupled with a 3 m x 0.15 mm I.D. restriction capillary at the inlet end. Thus, the conditions at the injector were similar to conventional GC methods, but sub-atmospheric pressure conditions occurred throughout the analytical column (MS provided the vacuum source). Optimal LP-GC-MS conditions were determined which achieved the fastest separation with the highest signal/noise ratio in MS detection (selected ion monitoring mode). Due to faster flow-rate, thicker film, and low pressure in the analytical column, this distinctive approach provided several benefits in the analysis of the representative pesticides versus a conventional GC-MS method, which included: (i) threefold gain in the speed of chromatographic analysis; (ii) substantially increased injection volume capacity in toluene; (iii) heightened peaks with 2 s peak widths for normal MS operation; (iv) reduced thermal degradation of thermally labile analytes, such as carbamates; and (v) due to larger sample loadability lower detection limits for compounds not limited by matrix interferences. The optimized LP-GC-MS conditions were evaluated in ruggedness testing experiments involving repetitive analyses of the 20 diverse pesticides fortified in a representative food extract (carrot), and the results were compared with the conventional GC-MS approach. The matrix interferences for the quantitation ions were worse for a few pesticides (acephate, methiocarb, dimethoate, and thiabendazole) in LP-GC-MS, but similar or better results were achieved for the 16 other analytes, and sample throughput was more than doubled with the approach. PMID:11556334

Mastovská, K; Lehotay, S J; Hajslová, J

2001-08-17

 
 
 
 
141

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.  

Science.gov (United States)

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

Chung, Stephen W C; Chan, Benny T P

2010-07-16

142

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

Science.gov (United States)

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

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

1993-09-01

143

COMPARISON OF CHOLINESTERASE ACTIVITY, RESIDUE LEVELS, AND URINARY METABOLITE EXCRETION OF RATS EXPOSED TO ORGANOPHOSPHORUS PESTICIDES  

Science.gov (United States)

Blood cholinesterase activity, urinary levels of phenolic and organophosphorus metabolites, and residues of intact compounds in blood and fat were determined following exposure of rats to organophosphorus pesticides. The eight pesticides studied included representative halogenate...

144

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

Science.gov (United States)

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

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

2008-01-01

145

Soil pesticide residue degradation and soil sample management procedures for environmental forensics  

Digital Repository Infrastructure Vision for European Research (DRIVER)

The overall goal of this project was to examine soil sampling procedures of each state regulatory agency that regulates pesticide use in that state, and to offer a standardized soil sampling protocol. ^ A survey of each SLA was conducted to determine the types of containers that are typically used when collecting soil samples for pesticide residue analysis and, on average, how long it takes for the soil samples to reach the laboratory once the soil sample is pulled from the field by the inv...

Saxton, George N.

2004-01-01

146

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

Science.gov (United States)

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

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

2013-01-01

147

Simultaneous determination of ten organophosphate pesticide residues in fruits by gas chromatography coupled with magnetic separation.  

Science.gov (United States)

In this study, ?-Fe2 O3 /chitosan magnetic microspheres were synthesized and evaluated by X-ray diffraction, SEM, thermogravimetric analysis, and static and kinetic adsorption experiments. Results showed that the magnetic microspheres exhibited good adsorption ability, and offered fast kinetics for the adsorption of trichlorfon, methamidophos, malathion, methyl parathion, dimethoate, omethoate, phosphamidon, phorate, isocarbophos, and chlorpyrifos. Based on magnetic separation, a simple method of magnetic SPE coupled to GC for the simultaneous determination of ten trace organophosphate pesticide residues was developed. Under the optimal conditions, the enrichment factor for ten organophosphorus pesticides was 10.1-364.7 and linear range was 0.001-10.0 mg/L. The LOD (S/N = 3) of the method for the ten pesticides was 0.31-3.59 ?g/kg. The RSD for three replicate extractions of spiked samples was between 2.5 and 6.3%. The pear and apple samples spiked with ten organophosphate pesticides at 20 and 200 ?g/kg levels were extracted and determined by this method with good recoveries ranging from 79.9 to 98.7%. Moreover, the method has been successfully applied for the determination of the ten organophosphate pesticide residues in peach samples. PMID:24470377

Tang, Qinghua; Wang, Xilong; Yu, Fan; Qiao, Xuguang; Xu, Zhixiang

2014-04-01

148

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

Science.gov (United States)

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

Loch, J P; Verdam, B

1989-01-01

149

Potential and real residues of pesticides in sugar beet  

Directory of Open Access Journals (Sweden)

Full Text Available Crops and their products can be contaminated either by direct application of pesticides for the protection of insects, acarives, agents of plant diseases and/or weeds, i.e. as the result of growing them on the soil containing pesticide residues applied in previous years. For the protection of sugar beet in our country, 23 insectisides, 17 fungicides and 18 herbicides have been registered. The pre-harvest interval (PHI ranges from 14 to 42 days i.e. they are provided by the time of application (PTA whereas the pre-harvest interval for herbicides ranges from 30 to 91 days and is ensured by the application period. Based on the results from the literature and on their own studies, the authors are of the opinion that the residues of the applied pesticides in sugar beet protection in accordance with the principles of good agricultural practice will be significantly lower than the maximum tolerable ammounts and that at the level from 1/4 to 1/10 of MRL. IT is necessary to emphasize the necessity of MRL determination both in leaves and in sugar loaf.in case they are used as animal feed.

Šovljanski Radmila A.

2006-01-01

150

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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 ...

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

2008-01-01

151

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

DEFF Research Database (Denmark)

This study investigates if acclimatization to residual pesticide contamination in agricultural soils is reflected in detoxification, antioxidant enzyme activities and energy budget of earthworms. Five fields within a joint agricultural area exhibited different chemical and farming histories from conventional cultivation to organic pasture. Soil multiresidual pesticide analysis revealed up to 9 molecules including atrazine up to 2.4 ng g -1 dry soil. Exposure history of endogeic Aporrectodea caliginosa and Allolobophora chlorotica modified their responses to pesticides. In the field, activities of soluble glutathione-S-transferases (sGST) and catalase increased with soil pesticide contamination in A. caliginosa. Pesticide stress was reflected in depletion of energy reserves in A. chlorotica. Acute exposure of pre-adapted and naïve A. caliginosa to pesticides (fungicide Opus ®, 0.1 ?g active ingredient epoxiconazole g-1 dry soil, RoundUp Flash®, 2.5 ?g active ingredient glyphosate g-1 dry soil, and their mixture), revealed that environmental pre-exposure accelerated activation of the detoxification enzyme sGST towards epoxiconazole. © 2014 Elsevier Ltd. All rights reserved.

Givaudan, Nicolas; Binet, Françoise

2014-01-01

152

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

Science.gov (United States)

This study investigates if acclimatization to residual pesticide contamination in agricultural soils is reflected in detoxification, antioxidant enzyme activities and energy budget of earthworms. Five fields within a joint agricultural area exhibited different chemical and farming histories from conventional cultivation to organic pasture. Soil multiresidual pesticide analysis revealed up to 9 molecules including atrazine up to 2.4 ng g(-1) dry soil. Exposure history of endogeic Aporrectodea caliginosa and Allolobophora chlorotica modified their responses to pesticides. In the field, activities of soluble glutathione-S-transferases (sGST) and catalase increased with soil pesticide contamination in A. caliginosa. Pesticide stress was reflected in depletion of energy reserves in A. chlorotica. Acute exposure of pre-adapted and naïve A. caliginosa to pesticides (fungicide Opus(®), 0.1 ?g active ingredient epoxiconazole g(-1) dry soil, RoundUp Flash(®), 2.5 ?g active ingredient glyphosate g(-1) dry soil, and their mixture), revealed that environmental pre-exposure accelerated activation of the detoxification enzyme sGST towards epoxiconazole. PMID:24874794

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

2014-09-01

153

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

Science.gov (United States)

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

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

2013-01-01

154

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

2008-01-01

155

Wide-scope analysis of pesticide and veterinary drug residues in meat matrices by high resolution MS: detection and identification using Exactive-Orbitrap.  

Science.gov (United States)

A multiresidue and multiclass method for the simultaneous determination of more than 350 compounds including pesticides, biopesticides and veterinary drugs in different meat matrices (beef, pork and chicken) by ultra-high performance liquid chromatography coupled to Orbitrap MS has been developed. In the present study, the determination of fragments was accomplished as an essential tool for a reliable identification of compounds using high resolution MS. To obtain these fragments, different strategies have been carried out in order to ensure an appropriate fragment assignment and identification. The analytical method is suitable for qualitative analysis, and it was also evaluated for quantitative analysis. Generic extraction conditions were optimized, obtaining adequate recovery and precision values for most of the studied analytes (>290). The limits of detection ranged from 2 to 16?µg?kg(-1). Limits of quantification were 10?µg?kg(-1) with the exception of few compounds with a higher value (50 or 100?µg?kg(-1)). Limits of identification were also established, and they ranged from 2 to 150?µg?kg(-1). This method was applied to the analysis of 18 meat samples and some veterinary drugs as enrofloxacin and sulfadiazine were detected and further identified/quantified (with triple quadrupole) in two different samples at 33?µg?kg(-1) and trace levels, respectively. No pesticides were detected in the analyzed samples. PMID:24446260

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

2014-01-01

156

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

International Nuclear Information System (INIS)

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

157

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

Scientific Electronic Library Online (English)

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

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

158

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

Scientific Electronic Library Online (English)

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

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

2013-12-01

159

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

International Nuclear Information System (INIS)

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

160

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

Science.gov (United States)

...pesticide residues in food and feed; considering...relation to the safety of food and feed containing pesticide...industrial contaminants showing chemical or other similarity to pesticides, in specific food items or groups of food...Referred to the Committee by Codex and Codex Committees...

2011-01-20

 
 
 
 
161

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

Science.gov (United States)

...sesame, sweet rocket, calendula, castor oil plant, Chinese tallowtree, cottonseed, euphorbia, evening primrose...Agency under EPA MRID number 445554-03 for the detection and measurement of the pesticide residues. Contact: Janet...

2010-09-08

162

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

Science.gov (United States)

...ADDRESSES: Submit your comments, identified by docket identification (ID) number and the pesticide petition number (PP) of...exemption as part (c) for residues of the antifungal agent Aspergillus flavus NRRL 21882 in or on cotton. The petitioner...

2010-09-30

163

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

Science.gov (United States)

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. PMID:25208400

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

2014-03-01

164

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

Public concerns over pesticide residues in food had been increasing because of their bioaccumulation effects and their great danger to the environments and human’s heath. It was therefore imperative to detect the pesticide residue using all available analytical methods, especially highly sensitive, simple, rapid and low cost. The biosensor detection strategies held a great promise for the detection of agricultural pesticides, attributing to their key features such as high sensitivity, fast ...

Yao, Xue-peng; Liu, Shao-qin

2013-01-01

165

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

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

2011-01-01

166

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

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

2004-01-01

167

Practical tracer investigations of pesticide residues in agricultural ecosystem  

International Nuclear Information System (INIS)

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

168

[Comparison of three different QuEChERS sample treatment methods in the analysis of more than one hundred pesticide residues in tobacco by gas chromatography-tandem mass spectrometry].  

Science.gov (United States)

With a combination of QuEChERS method and gas chromatography-tandem mass spectrometry (GC-MS/MS) technique, three sample treatment methods (solvent exchange method, toluene dilution method, hexane liquid-liquid extraction method) were established to analyse more than one hundred pesticide residues in tobacco. The 155 pesticide analytes contained 58 organophosphorus, 28 organochlorine, 10 pyrethroids, 10 acyl amide, 11 carbamate, 7 dinitroaniline and 31 other family pesticides. Comparison of the three treatment methods was investigated on performances including matrix effect, co-extracted matrix, peak interference, recovery and the limit of quantification (LOQ). The hexane liquid-liquid extraction method gave the cleanest extract but poorer recovery; the solvent exchange and toluene dilution method could guarantee recoveries in the range of 70% and 120% for most of the 155 pesticides. We found that organophosphorus, acyl amide and carbamate pesticides exhibited relative strong matrix effects compared with organochlorine and pyrethroid pesticides. Toluene dilution method was recommended to analyse organophosphorus pesticides, and hexane liquid-liquid extraction (LLE) method was recommended to analyse organochlorine and pyrethroid pesticides. PMID:24558850

Chen, Xiaoshui; Bian, Zhaoyang; Yang, Fei; Liu, Shanshan; Tang, Gangling; Hu, Qingyuan

2013-11-01

169

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

Science.gov (United States)

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

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

2010-12-01

170

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

Science.gov (United States)

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

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

171

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

Science.gov (United States)

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

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

2011-11-01

172

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

Science.gov (United States)

...Receipt of a Pesticide Petition Filed for Residues of Polymeric...or on All Food Commodities...part 180 for residues of polymeric...or on all food commodities...that the pesticide petition...regulation for residues of the pesticide in or on all food...

2010-01-13

173

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

Science.gov (United States)

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

Baker, Brian P., 1958-; Benbrook, Charles.; Benbrook, Karen L.; Groth, Edward, 1944-

2002-01-01

174

Nondestructive detection pesticide residue on navel orange surface using laser image  

Science.gov (United States)

To detect pesticide residue on navel orange surface by nondestructive means, five group oranges sprayed water, fenvalerate, isocarbophos, fenpropathrin, carbendazim pesticides respectively were chosen as experimental samples. Laser imaging system was built for acquiring images of fruits. Unitary nonlinear regression function was fitted by analyzing gray histogram curves of images within 12-40 range. The coefficient or eigenvalue of functions was different about every navel orange. The threshold coefficient was confirmed by data processing, which can establish fruits surface sprayed pesticide or not. The result showed that laser imaging technique is feasible for detecting pesticide residue on navel orange surface.

Yao, Mingyin; Liu, Muhua; Yao, Lintao

2009-07-01

175

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

International Nuclear Information System (INIS)

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

176

FINGER PRINTING TECHNIQUE FOR DETECTION OF PESTICIDE RESIDUES IN VEGETABLE CROPS  

Directory of Open Access Journals (Sweden)

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

Syeda Azeem Unnisa

2014-06-01

177

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

Science.gov (United States)

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

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

2014-10-01

178

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

Energy Technology Data Exchange (ETDEWEB)

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.

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

1996-12-31

179

Cumulative risk assessment of pesticide residues in food.  

Science.gov (United States)

There is increasing need to address the potential risks of combined exposures to multiple residues from pesticides in the diet. The available evidence suggests that the main concern is from dose addition of those compounds that act by the same mode of action. The possibility of synergy needs to be addressed on a case-by-case basis, where there is a biologically plausible hypothesis that it may occur at the levels of residues occurring in the diet. Cumulative risk assessment is a resource-intense activity and hence a tiered approach to both toxicological evaluation and intake estimation is recommended, and the European Food Safety Authority (EFSA) has recently published such a proposal. Where assessments have already been undertaken by some other authority, full advantage should be taken of these, subject of course to considerations of quality and relevance. Inclusion of compounds in a cumulative assessment group (CAG) should be based on defined criteria, which allow for refinement in a tiered approach. These criteria should include chemical structure, mechanism of pesticidal action, target organ and toxic mode of action. A number of methods are available for cumulating toxicity. These are all inter-related, but some are mathematically more complex than others. The most useful methods, in increasing levels of complexity and refinement, are the hazard index, the reference point index, the Relative Potency Factor method and physiologically based toxicokinetic modelling, although this last method would only be considered should a highly refined assessment be necessary. Four possible exposure scenarios are of relevance for cumulative risk assessment, acute and chronic exposure in the context of maximum residue level (MRL)-setting, and in relation to exposures from the actual use patterns, respectively. Each can be addressed either deterministically or probabilistically. Strategies for dealing with residues below the limit of detection, limit of quantification or limit of reporting need to be agreed. A number of probabilistic models are available, but some of there are geographically constrained due to the underlying datasets used in their construction. Guidance on probabilistic modelling needs to be finalised. Cumulative risk assessments have been performed in a number of countries, on organophosphate insecticides alone (USA) or together with carbamates (UK, DK, NL), triazines, chloroacetanilides, carbamates alone (USA), and all pesticides (DE). All identifiable assumptions and uncertainties should be tabulated and evaluated, at least qualitatively. Those likely to have a major impact on the outcome of the assessment should be examined quantitatively. In cumulative risk assessment, it is necessary, as in other risk assessments, for risk managers to consider what level of risk would be considered "acceptable", for example what percentile of the population should be below the reference value. Criteria for prioritising CAGs for cumulative risk assessment include frequency of detection in monitoring programmes, high usage, high exposure relative to the reference value, large number of compounds (e.g. five or more) in a group. PMID:18585444

Boobis, Alan R; Ossendorp, Bernadette C; Banasiak, Ursula; Hamey, Paul Y; Sebestyen, Istvan; Moretto, Angelo

2008-08-15

180

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

Science.gov (United States)

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

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

2014-01-01

 
 
 
 
181

Public Health Implications of Pesticide Residues in Meat  

Digital Repository Infrastructure Vision for European Research (DRIVER)

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...

Jadhav V.J. and Waskar V.S.

2011-01-01

182

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

Directory of Open Access Journals (Sweden)

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

M. I. Bhanger

2011-12-01

183

Organochlorine pesticide residues in wheat and drinking water samples from Jaipur, Rajasthan, India.  

Science.gov (United States)

The organochlorine pesticide contamination in dietary sources has caused serious threat to the human progeny. The present study was therefore conducted to evaluate the pesticide contamination in wheat flour and drinking water from Jaipur City, Rajasthan, India using Gas Chromatograph. All the wheat and water samples were found to be contaminated with various organochlorine pesticide residues of DDT and its metabolites, HCH and its isomers, heptachlor and its expoxide and aldrin. The amount of pesticide detected in wheat flour was higher than the permissible limits prescribed by WHO/FAO. In drinking water only a few pesticides exceeded the permissible limits. Seasonal variations of pesticides residues were also observed during the study period. PMID:15473547

Bakore, Neela; John, P J; Bhatnagar, Pradeep

2004-11-01

184

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

The ethyl acetate-based multi-residue method for determination of pesticide residues in produce has been modified for gas chromatographic (GC) analysis by implementation of dispersive solid-phase extraction (using primary¿secondary amine and graphitized carbon black) and large-volume (20 ¿L) injection. The same extract, before clean-up and after a change of solvent, was also analyzed by liquid chromatography with tandem mass spectrometry (LC¿MS¿MS). All aspects related to sample preparati...

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

2007-01-01

185

Perspective on Dietary Risk Assessment of Pesticide Residues in Organic Food  

Directory of Open Access Journals (Sweden)

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

Charles M. Benbrook

2014-05-01

186

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

Science.gov (United States)

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

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

2013-05-01

187

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

Science.gov (United States)

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

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

2013-01-01

188

MONITORING THE TRANSFER OF PESTICIDE RESIDUES FROM SOFT SURFACES TO FOODS  

Science.gov (United States)

The Food Quality Protection Act of 1996 requires assessing pesticide residue exposures to children. Contact of soft surfaces by foods and the ingestion of the food represents a pesticide exposure pathway. Chlorpyrifos has widespread use indoors and would be protected from envir...

189

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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...

2008-01-01

190

Monitoring of pesticide residues of five notable vegetables at Agbogbloshie market in Accra, Ghana.  

Science.gov (United States)

The study monitored the concentrations of pesticide residues in vegetables arriving at Agbogbloshie, a central market in the Accra Metropolis from different parts of Ghana and beyond. A total of 810 samples of 5 different vegetables from Central, Volta, Greater Accra, Ashanti, Eastern Regions, and neighboring country (Togo) were collected from January 2009 through to December 2011. In all, 18 % of the samples had no detectable residues, 62 % were below the maximum residue limits (MRLs), and 20 % also exceeded the EU (MRLs) adopted values. Overall, lettuce contained the highest number of residues above their MRLs besides cucumber and cabbage. The pesticide residues were mainly organophosphates and synthetic pyrethroids. The results demonstrate the need for continuous monitoring of pesticide residues in vegetables arriving at the various major markets in Ghana. PMID:25007773

Osei-Fosu, P; Donkor, A K; Nyarko, S; Nazzah, N K; Asante, I K; Kingsford-Adabo, R; Arkorful, N A

2014-11-01

191

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

International Nuclear Information System (INIS)

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

192

Residual Component Analysis  

CERN Document Server

Probabilistic principal component analysis (PPCA) seeks a low dimensional representation of a data set in the presence of independent spherical Gaussian noise, Sigma = (sigma^2)*I. The maximum likelihood solution for the model is an eigenvalue problem on the sample covariance matrix. In this paper we consider the situation where the data variance is already partially explained by other factors, e.g. covariates of interest, or temporal correlations leaving some residual variance. We decompose the residual variance into its components through a generalized eigenvalue problem, which we call residual component analysis (RCA). We show that canonical covariates analysis (CCA) is a special case of our algorithm and explore a range of new algorithms that arise from the framework. We illustrate the ideas on a gene expression time series data set and the recovery of human pose from silhouette.

Kalaitzis, Alfredo A

2011-01-01

193

Modelling regional transport of pesticide residues in groundwater  

Digital Repository Infrastructure Vision for European Research (DRIVER)

The movement of pesticides through soil and groundwater to pumping wells for drinking-water supply was modelled. Most of the retardation and transformation occurs when a pesticide moves through the unsaturated zone. Computed leaching to groundwater increased when soil heterogeneity was taken into account. A column method was developed to measure the rate of pesticide transformation in the aquifer as input for models. The fluctuation of the concentration in the pumping well due to the applicat...

Leistra, M.; Beltman, W. H. J.; Boesten, J. J. T. I.; Matser, A. M.; Zee, S. E. A. T. M.

1996-01-01

194

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

Science.gov (United States)

Tea is an agricultural product of the leaves, leaf buds, and internodes of various cultivars and sub-varieties of the Camellia sinensis plant, processed and vulcanized using various methods. Tea is a main beverage in Iranian food basket so should be free from toxic elements such as pesticides residue. There is no data bank on the residue of pesticides in the consumed black tea in Iran. The present study is the first attempt for monitoring of 25 pesticide residues from different chemical groups in tea samples obtained from local markets in Tehran, I.R. Iran during the period 2011. A reliable and accurate method based on spiked calibration curve and QuEChERS sample preparation was developed for determination of pesticide residues in tea by gas chromatography-mass spectrometry (GC/MS). The using of spiked calibration standards for constructing the calibration curve substantially reduced adverse matrix-related effects and negative recovery affected by GCB on pesticides. The recovery of pesticides at 3 concentration levels (n = 3) was in range of 81.4 - 99.4%. The method was proved to be repeatable with RSDr lower than 20%. The limits of quantification for all pesticides were ?20 ng/g. 53 samples from 17 imported and manufactured brand were analyzed. Detectable pesticides residues were found in 28.3% (15 samples) of the samples. All of the positive samples were contaminated with unregulated pesticides (Endosulfan Sulfate or Bifenthrin) which are established by ISIRI. None of the samples had contamination higher than maximum residue limit set by EU and India. PMID:23369650

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

2013-01-01

195

Monitoring of some pesticides residue in consumed tea in Tehran market  

Directory of Open Access Journals (Sweden)

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

Hamedani Morteza Pirali

2013-01-01

196

Monitoring of Some Pesticides Residue in Consumed tea in Tehran Market  

Directory of Open Access Journals (Sweden)

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.

Maryam Amirahmadi

2013-01-01

197

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

Science.gov (United States)

...chemicals in or on various food commodities. The Agency...of pesticides in or on food commodities. Further...analytical method using chemical derivatization followed...including an applicable CODEX MRL. Per the 2011 Final...residues of metaldehyde in food crops including...

2012-09-28

198

The Concept of Withholding Period and Pesticide Residue in Grain Storage  

Directory of Open Access Journals (Sweden)

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.

Adegbola, J. A.

2012-12-01

199

Dietary exposure to pesticide residues from commodities alleged to contain the highest contamination levels.  

Science.gov (United States)

Probabilistic techniques were used to characterize dietary exposure of consumers to pesticides found in twelve commodities implicated as having the greatest potential for pesticide residue contamination by a United States-based environmental advocacy group. Estimates of exposures were derived for the ten most frequently detected pesticide residues on each of the twelve commodities based upon residue findings from the United States Department of Agriculture's Pesticide Data Program. All pesticide exposure estimates were well below established chronic reference doses (RfDs). Only one of the 120 exposure estimates exceeded 1% of the RfD (methamidophos on bell peppers at 2% of the RfD), and only seven exposure estimates (5.8 percent) exceeded 0.1% of the RfD. Three quarters of the pesticide/commodity combinations demonstrated exposure estimates below 0.01% of the RfD (corresponding to exposures one million times below chronic No Observable Adverse Effect Levels from animal toxicology studies), and 40.8% had exposure estimates below 0.001% of the RfD. It is concluded that (1) exposures to the most commonly detected pesticides on the twelve commodities pose negligible risks to consumers, (2) substitution of organic forms of the twelve commodities for conventional forms does not result in any appreciable reduction of consumer risks, and (3) the methodology used by the environmental advocacy group to rank commodities with respect to pesticide risks lacks scientific credibility. PMID:21776262

Winter, Carl K; Katz, Josh M

2011-01-01

200

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

Directory of Open Access Journals (Sweden)

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

YAO Xue-Peng

2013-02-01

 
 
 
 
201

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

Science.gov (United States)

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

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

2013-01-01

202

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

Directory of Open Access Journals (Sweden)

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

2007-01-01

203

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

Science.gov (United States)

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

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

2009-04-01

204

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

Science.gov (United States)

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 >20?m, 20-2?m and 2-0.1?m 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 20-2?m and 2-0.1?m 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 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.

Andreou, Kostas; Semple, Kirk; Jones, Kevin

2010-05-01

205

Organochlorine pesticide residues in European sardine, horse mackerel and Atlantic mackerel from Portugal.  

Science.gov (United States)

This paper reports the results for the surveillance of nine organochlorine pesticides (HCH isomers (alpha, beta, e, gamma), p,p'-DDD, p,p'-DDT, p,p'-DDE, p,p'-DDD, HCB and aldrin) in muscle of three fish species, European pilchard (Sardina pilchardus), Atlantic horse mackerel (Trachurus trachurus) and Atlantic mackerel (Scomber scombrus). Analytical methodology included n-hexane extraction, clean-up with 2% deactivated Florisil, and quantification with gas chromatography-electron capture detection (GC-ECD). The highest mean concentrations were found for p,p'-DDT in sardine and mackerel at levels of 30.1 and 109.9 microg kg(-1), respectively, and for p,p'-DDD in horse mackerel at 51.9 microg kg(-1). Three species had higher levels for S-DDT than S-HCH. The estimated daily intake of organochlorine pesticides in the three species showed that in sardine, the highest EDIs were found for aldrin, at 1.8 ng kg(-1) bw day(-1), which represents 1.8% of the acceptable daily intake (ADI), and for ss-HCH, at 4.0 ng kg(-1) bw day(-1), representing 0.4% of ADI. Lowest values were found for Atlantic mackerel. Statistical analysis to determine the differences in mean concentrations of pesticides between species, and any correlation between groups of residues related with each one of the species, was undertaken. PMID:16019839

Campos, A; Lino, C M; Cardoso, S M; Silveira, M I N

2005-07-01

206

Radiotracer studies of pesticide residues in food plants  

International Nuclear Information System (INIS)

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

207

[Survey of pesticide residues in imported cereal products (1994.4 approximately 2006.3)].  

Science.gov (United States)

A survey of pesticide residues in 490 imported cereal products on the Tokyo market from April 1994 to March 2006 was carried out. Eight kinds of organophosphorus pesticides (chlorpyrifos, chlorpyrifos-methyl, DDVP, diazinon, etrimfos, malathion, MEP and pirimiphos-methyl) were detected at levels between Tr (below 0.01 ppm) and 0.82 ppm from 91 samples. In our investigations, chlorpyrifos-methyl and malathion tended to be detected in samples from America, pirimiphos-methyl in those from Europe, and MEP in those from Oceania. Thus, pesticide residues seemed to be different in produce from different areas. Residue levels of these pesticides were calculated as between 0.08 and 13.2% of their ADI values according to the daily intake of cereal products. Therefore, these cereal products should be safe for normal usage. PMID:18633211

Kobayash, Maki; Takano, Ichiro; Tamura, Yasuhiro; Tomizawa, Sanae; Tateishi, Yukinari; Sakai, Naoko; Kamijo, Kyoko; Ibe, Akihiro; Nagayama, Toshihiro

2008-06-01

208

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

International Nuclear Information System (INIS)

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

209

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

Science.gov (United States)

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

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

2013-09-01

210

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

Directory of Open Access Journals (Sweden)

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

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

2012-10-01

211

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

Directory of Open Access Journals (Sweden)

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

D.K. Essumang

2009-04-01

212

Plant uptake of pesticides and human health: Dynamic modeling of residues in wheat and ingestion intake  

DEFF Research Database (Denmark)

Human intake of pesticide residues from consumption of processed food plays an important role for evaluating current agricultural practice. We take advantage of latest developments in crop-specific plant uptake modeling and propose an innovative dynamic model to estimate pesticide residues in the wheat-environment system, dynamiCROP. We used this model to analyze uptake and translocation of pesticides in wheat after foliar spray application and subsequent intake fractions by humans. Based on the evolution of residues in edible parts of harvested wheat we predict that between 22 mg and 2.1 g per kg applied pesticide are taken in by humans via consumption of processed wheat products. Model results were compared with experimentally derived concentrations in wheat ears and with estimated intake via inhalation and ingestion caused by indirect emissions, i.e. the amount lost to the environment during pesticide application. Modeled and measured concentrations in wheat fitted very well and deviate from less than a factor 1.5 for chlorothalonil to a maximum factor 3 for tebuconazole. Main aspects influencing pesticide fate behavior are degradation half-life in plant and time between pesticide application and crop harvest, leading to variations in harvest fraction of at least three orders of magnitude. Food processing may further reduce residues by approximately 63%. Intake fractions from residues in sprayed wheat were up to four orders of magnitude higher than intake fractions estimated from indirect emissions, thereby demonstrating the importance of exposure from consumption of food crops after direct pesticide treatment. © 2011 Elsevier Ltd. All rights reserved.

Fantke, Peter; Charles, Raphaël

2011-01-01

213

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

International Nuclear Information System (INIS)

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

214

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

Directory of Open Access Journals (Sweden)

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

Yawar Latif

2011-12-01

215

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

Directory of Open Access Journals (Sweden)

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

FERDI BRAHUSHI

2014-06-01

216

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

Directory of Open Access Journals (Sweden)

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

Tong Dewen

2007-01-01

217

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

Science.gov (United States)

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

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

2011-01-01

218

Gas chromatography with flame photometric detection of 31 organophosphorus pesticide residues in Alpinia oxyphylla dried fruits.  

Science.gov (United States)

A simple, rapid and effective gas chromatography-flame photometric detection method was established for simultaneous multi-component determination of 31 organophosphorus pesticides (OPPs) residues in Alpinia oxyphylla, which is widely consumed as a traditional medicine and food in China. Sample preparation was completed in a single step without any clean-up procedure. All pesticides expressed good linear relationships between 0.004 and 1.0 ?g/mL with correlation coefficients higher than 0.9973. The method gave satisfactory recoveries for most pesticides. The limits of detection varied from 1 to 10 ng/mL, and the limits of quantification (LOQs) were between 4 and 30 ng/mL. The proposed method was successfully applied to 55 commercial samples purchased from five different areas. Five pesticide residues were detected in four (7.27%) samples. The positive samples were confirmed by gas chromatography with tandem mass spectrometry (GC-MS/MS). PMID:24874387

Zhao, Xiangsheng; Kong, Weijun; Wei, Jianhe; Yang, Meihua

2014-11-01

219

Reduction of pesticide residues on fresh vegetables with electrolyzed water treatment.  

Science.gov (United States)

Degradation of the 3 pesticides (acephate, omethoate, and dimethyl dichloroviny phosphate [DDVP]) by electrolyzed water was investigated. These pesticides were commonly used as broad-spectrum insecticides in pest control and high-residual levels had been detected in vegetables. Our research showed that the electrolyzed oxidizing (EO) water (pH 2.3, available chlorine concentration:70 ppm, oxidation-reduction potential [ORP]: 1170 mV) and the electrolyzed reducing (ER) water (pH 11.6, ORP: -860 mV) can reduce the pesticide residues effectively. Pesticide residues on fresh spinach after 30 min of immersion in electrolyzed water reduced acephate by 74% (EO) and 86% (ER), omethoate by 62% (EO) and 75% (ER), DDVP by 59% (EO) and 46% (ER), respectively. The efficacy of using EO water or ER water was found to be better than that of using tap water or detergent (both were reduced by more than 25%). Besides spinach, the cabbage and leek polluted by DDVP were also investigated and the degradation efficacies were similar to the spinach. Moreover, we found that the residual level of pesticide residue decreased with prolonged immersion time. Using EO or ER water to wash the vegetables did not affect the contents of Vitamin C, which inferred that the applications of EO or ER water to wash the vegetables would not result in loss of nutrition. PMID:22420563

Hao, Jianxiong; Wuyundalai; Liu, Haijie; Chen, Tianpeng; Zhou, Yanxin; Su, Yi-Cheng; Li, Lite

2011-05-01

220

Kuwait's total diet study: dietary intake of organochlorine, carbamate, benzimidazole and phenylurea pesticide residues.  

Science.gov (United States)

The State of Kuwait in cooperation with the U.S. Food and Drug Administration (FDA) conducted a Total Diet Study (TDS) to estimate intakes of pesticide residues by the population. The levels of organochlorine (OC) pesticides, carbamates, benzimidazoles, and phenylureas in the TDS core list are reported here. The TDS core list was established through a national food consumption survey. All food items (140 for the Kuwaiti adult) were prepared as eaten and analyzed for the pesticides mentioned above. The FDA's multiresidue methods in Volume I of the Pesticide Analytical Manual were used in gas, liquid, and gel permeation chromatographic analyses. Only vegetable and fruit samples contained pesticide residues (mg/kg), including the carbamates 1-naphthol (1.4) and 3H-carbofuran (0.94) in carrots; the OC pesticide vinclozolin (0.47), 3H-carbofuran (0.66), and fenuron (0.6) in kiwi fruit; the OC pesticide procymidone (0.32) and carbendazim (0.5) in grapes; 3H-carbofuran (5.0) in apricots; the OC pesticides captan (0.013) and thiabendazole (0.63) in pears; captan (0.035) in plums; and carbendazim (0.4) in mandarin oranges. The levels of 3H-carbofuran found in both apricots and kiwi fruit exceeded the maximum residue limits (MRLs) of the Food and Agriculture Organization/World Health Organization (FAO/WHO) of the United Nations. The daily intakes of pesticides by the different population groups are discussed in light of the FAO/WHO acceptable daily intakes. PMID:10589497

Sawaya, W N; al-Awadhi, F A; Saeed, T; al-Omair, A; Ahmad, N; Husain, A; Khalafawi, S; al-Omirah, H; Dashti, B; al-Amiri, H; al-Saqer, J

1999-01-01

 
 
 
 
221

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

Crentsil Kofi Bempah; Jacob Asomaning; Juliana Boateng

2012-01-01

222

Regulatory science and uncertainty in the risk assessment of pesticide residues  

Digital Repository Infrastructure Vision for European Research (DRIVER)

In this thesis I examine how the scientific advisory system in England and Wales has responded to concerns about the risks of pesticide residues in food and demands for wider engagement in the formulation of advice. Specifically, I explore how the Advisory Committee on Pesticides (ACP) frames scientific uncertainties in risk assessment, and why some bodies outside and within government are critical of the ACP’s approach that is centred in the conventional single-chemical, high-dose-respons...

Diggle, Rebecca

2010-01-01

223

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

International Nuclear Information System (INIS)

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

224

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

International Nuclear Information System (INIS)

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

225

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

Directory of Open Access Journals (Sweden)

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

Helena BAŠA ?ESNIK

2006-10-01

226

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

Science.gov (United States)

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

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

2011-11-18

227

Pesticides Residues in Smoked Fish Samples from North-Eastern Nigeria  

Directory of Open Access Journals (Sweden)

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

A. Mustapha

2010-01-01

228

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

Science.gov (United States)

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.

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

2014-08-01

229

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

Science.gov (United States)

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

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

2013-01-01

230

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

Directory of Open Access Journals (Sweden)

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

A Allahresani

2010-02-01

231

MONITORING OF PESTICIDE RESIDUES IN AGRICULTURAL PRODUCTS IN THE YEARS 2001 AND 2002  

Directory of Open Access Journals (Sweden)

Full Text Available Agricultural Institute of Slovenia has been monitoring the pollution of agricultural products with residues of pesticides as part of professional projects in agriculture since 1987, and as part of national monitoring programme since 1999. Constant measurements are necessary because of intensive production of agricultural products and expanded use of chemical substances for plant protection. In the years 2001 and 2002 we have analysed the presence of pesticide residues in 301 samples of fruit and vegetables from eight different growing areas of Slovenia as part of national monitoring.

H BAŠA ?ESNIK

2004-04-01

232

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

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

2012-01-01

233

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

The active involvement of EFSA in the area of pesticide residues assessment started in 2006 following the adoption of new legislation on maximum residue levels (MRLs) of pesticides in food (Regulation (EC) No 396/2005). EFSA took on a new role as an independent risk assessment body in the process of MRL setting, providing important contributions in the EU-wide harmonisation of MRLs. With the development of a risk assessment model (EFSA PRIMo) the risk assessment process has become mo...

Reich H; Brocca D; Dujardin B; Bergman P; Fontier H

2012-01-01

234

Residues of five pesticides in field-treated alfalfa seeds and alfalfa sprouts.  

Science.gov (United States)

Residues of five different pesticides applied to alfalfa seed crops were determined in the harvested seeds and in sprouts grown from these seeds. Although seeds are usually used for future production of alfalfa plants, some of these seeds may be sprouted for human food consumption. The pesticides studied--aldicarb (Temik), chlorothalonil (Bravo), chlorpyrifos (Lorsban), methamidophos (Monitor) and propargite (Comite)--were applied at a normal usage rate and at two to three times that rate. Residues on the seeds and sprouts, if any, were insignificant at rates of application. PMID:2413099

Archer, T E; Gauer, W O

1985-08-01

235

[Determination of organic phosphorus pesticide residues in scallion by gas chromatography coupled with microwave clean-up].  

Science.gov (United States)

A method for the determination of organic phosphorus pesticide residues is described. It covers 25 residues in scallion including dichlorvos, ethoprophos, phorate, diazinon, disulfoton, dimethoate, pirimiphos-methyl, chlorpyrifos, malathion, fenitrothion, parathion, chlorfenvinphos, ethion, EPN, dyfonate, chlorpyrifos-methyl, parathion-methyl, fenthion, quinalphos, gardona, methidathion, carbophenothion, phosmet, phosalone, and coumaphos. After the scallion samples were heated for 30 s in microwave oven, the residues were extracted with acetonitrile, and then the organic phase was salted out from the matrix. As a result, most of the interfering impurities were abolished in the heating process. In this study, these pesticides were categorized into two groups for analysis. The gas chromatographic analysis was performed on a capillary column (DB-1701, 30 m x 0.25 mm x 0.25 microm) and determined with a flame photometric detector. Linear correlation coefficients of the 25 organic phosphorus pesticides were not lower than 0.991 0 and the linear ranges for most of the compounds were between 0.1 to 5.0 mg/L. The detection limits were between 0.025 and 0.200 mg/L. In recovery study, average recoveries ranged from 85.2% to 119.6% at the fortification levels of 0.05, 0.2 and 0.5 mg/kg and the relative standard deviations were in the range of 2.1% and 14.8%. The method is a simple, rapid and highly efficient one to determine organic phosphorus pesticide residues in scallion. PMID:17679438

Jiang, Jun; Li, An; Li, Haiyan; Tong, Kexing; Zhou, Lili; Zhou, Huimin; Zhao, Tong

2007-05-01

236

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

International Nuclear Information System (INIS)

ts. Nitrate (NO3-N) levels in surface water ranged between 0.12 - 31.07 mgL-1 while ammonia was between 0.01 - 2.10 mgL-1 and that of phosphate was 0.012 - 2.45 mgL-1. Pesticide residues and metabolites detected in water, sediment and fish samples from the Densu River Basin were organochlorines. In an average 96% of fish samples, 13.69% of sediment and 3.30% of water samples, at least one pesticide residue was detected per sample. Of the numerous pesticides evaluated, ? -HCH, DDT, aldrin, dieldrin, DDE, endosulfan sulphate, ?-chlordane, endrin and ?-HCH were detected in fish, water and sediment samples. Aldrin and dieldrin levels detected were above the recommended limit of 0.03 ?L-1 with endosulfan, endrin and chlordane registering levels above their recommended limits of 20.0?L-1 and 0.2 ?L-1 respectively for drinking water. Pesticide residues in fish samples varied between 0.10 ?gKg-1 to 30.90 ?gKg-1. The highest level was detected in Hepsetus odoe (HO-N). Contamination pattern of pesticide residues in fish samples was generally in the order of p'p'-DDE > heptachlor > ?- HCH > p'p'-DDT > endosulfan Sulphate > ?-endosulfan > ?- HCH > ?-chlordane > dieldrin > endrin ketone > methoxychlor > endrin > aldrin > endrin aldehyde. Data obtained from the field survey regarding safe use of pesticides, toxicity awareness and symptoms among farmers indicated that a very high proportion of farmers were at high risk of pesticide poisoning from occupational exposure. More than 90% of farm workers did not practice safety precaution during pesticide formulation and application leading to considerable prevalence of pesticide related illness in this agricultural community. The presence of pesticide residues in fish was of further concern because fish is the main protein diet for humans in the basin. The estimated dose for aldrin, methoxychlor, ?-chlordane, endrin aldehyde, endrin ketone, endrin, p'p'-DDT and ?-HCH do not pose a direct hazard to human health, although present in fish samples since the values registered were lower than the reference doses. However, ?- HCH, heptachlor, ?-endosulfan, endosulfan sulphate, p'p'-DDE and dieldrin levels exceeded the reference dose, indicating a great potential for systemic toxicity in children who are considered to be the most vulnerable population subgroup. In children, between the ages of 0 - 1year, the hazard indices of 2.64, 1.720, 1.736 and 0.792 were computed for ?-endosulfan, heptachlor, endosulfan sulphate and dieldrin respectively while for children between the ages 1 -11years, hazard indices for heptachlor, ?-endosulfan and endosulfan were 0.573, 0.880 and 0.576 respectively. Although residue levels of pesticide residues were below the maximum permissible intake of Codex Alimentarius Committee of Food and Agricultural Organization on pesticides residues, there was no zero risk because there were pesticide residues present in fish. The results implicitly revealed that improper land use in the basin has led to poor groundwater and surface water quality. (au)

237

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

Science.gov (United States)

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

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

2014-06-15

238

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

International Nuclear Information System (INIS)

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

239

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

Science.gov (United States)

...section 408 of the Federal Food, Drug, and Cosmetic...part 174 or part 180 for residues of pesticide chemicals in or on various food commodities. EPA has...modification of regulations for residues of pesticides in or on food commodities....

2010-09-01

240

Compound specific isotope analysis of organophosphorus pesticides.  

Science.gov (United States)

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

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

2014-09-01

 
 
 
 
241

Residual pesticide detection on food with particle-enhanced Raman scattering  

Science.gov (United States)

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

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

2014-08-01

242

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

Science.gov (United States)

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

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

2015-03-01

243

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

Directory of Open Access Journals (Sweden)

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

Crentsil Kofi Bempah

2012-12-01

244

Consumer exposure to pesticide residues in apples from the region of south-eastern Poland.  

Science.gov (United States)

The production of apples in Poland is the largest among the countries of the European Union, and therefore, the consumption of these fruits is high in our country. The aim of this study was to determine the presence of pesticide residues in Polish apples and to assess if these residues pose a risk to the health of the consumer. Furthermore, compliance with legal regulations concerning the use of plant protection products in crop cultivation was ascertained. Pesticide residues were found in 192 samples (61.5% of tested samples). In six samples (1.9%), residues exceeded maximum residue limits. Violations concerned the insecticides: indoxacarb, diazinon and fenitrothion. The highest long-term consumer exposure was found in the case of consumption of apples with diazinon residue for both groups, adults and toddlers [4% acceptable daily intake (ADI), adults; 21% ADI, toddlers]. The highest values of short-term exposure were obtained in the case of consumption of apples with indoxacarb [5% acute reference dose (ARfD), adults; 27% ARfD, toddlers] and fenitrothion (4% ARfD, adults; 23% ARfD, toddlers). Although fungicides are the pesticides found most often in apples, the consumption of apples with insecticide residues constitutes the greatest hazard to human health. PMID:23666120

Szpyrka, Ewa; Kurdziel, Anna; S?owik-Borowiec, Magdalena; Grzegorzak, Magdalena; Matyaszek, Aneta

2013-11-01

245

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

DEFF Research Database (Denmark)

The differences in residue pattern between Italy and South Africa, the main exporters of table grapes to the Danish market, were investigated. The results showed no major differences with respect to the number of samples with residues, with residues being found in 54-78% of the samples. Exceedances of the European Union maximum residue limit (MRL) were found in five samples from Italy. A number of samples were rinsed to study the possible reduction of residues. For copper, iprodione, procymidone and dithiocarbamates a significant effect of rinsing was found (20-49% reduction of residues). However, no significant effect was found for organophosphorus pesticides and pyrethroids, whereas the number of samples with residues of benzilates, phenylamids and triazoles was insufficient to demonstrate any significant effects. An intake calculation showed that the average intake from Italian grapes was 3.9 mu g day(-1) for pesticides and 21 mu g day(-1) for copper. Correspondingly, the intakes from South African grapes were 2.6 and 5.7 mu g day(-1) respectively. When the total exposure of pesticides from grapes were related to acceptable daily intake, expressed as the sum of Hazard Quotients, the exposure were approximately 0.5% for Italian samples and 1% for South African samples.

Poulsen, Mette Erecius; Sloth, Jens JØrgen

2007-01-01

246

Identification of residual pesticides in water by GC/QPMS.  

Science.gov (United States)

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

Murata, T; Takahashi, S

1991-10-01

247

Optical instrument development for detection of pesticide residue in apple surface  

Science.gov (United States)

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

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

2013-05-01

248

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

2007-01-01

249

Survey of pesticide residues in maize, cowpea and millet from northern Cameroon: part I.  

Science.gov (United States)

In northern Cameroon, the misuse of pesticides for pest control is common among small-scale farmers. Therefore, monitoring of pesticide residues was carried out on stored maize, cowpea and millet from eight localities. The determination of residues of organochlorines (lindane, ?-endosulfan and ?-endosulfan), organophosphorus compounds (malathion and pirimiphos-methyl), synthetic pyrethroids (permethrin) and carbamates (carbufuran) was performed using GC-ECD/NPD and GC-MS for confirmation. Organochlorine pesticides were detected more frequently and in higher concentrations, ranging from 0.02 ± 0.01 mg kg(-1) for ?-endosulfan in millet to 9.53 ± 4.00 mg kg(-1) lindane in maize, than organophosphorus compounds, with concentrations varying from 0.04 ± 0.03 mg kg(-1) for pirimiphos methyl to 0.23 ± 0.38 mg kg(-1) for malathion in maize. Permethrin was found only in maize at 0.39 ± 0.23 mg kg(-1). No carbofuran was found. More than 75% of samples contained pesticide residues above the maximum residue limit (MRL); showing a potential human dietary risk related to consumption of these grains. PMID:24779572

Sonchieu, Jean; Benoit Ngassoum, Martin; Bosco Tchatchueng, Jean; Srivastava, Ashutosh Kumar; Srivastava, Laxman Prasad

2010-01-01

250

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

Science.gov (United States)

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

Lorenzin, Michele

2007-01-01

251

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

Science.gov (United States)

...Filing of a Pesticide Petition for Residues of a Aspergillus...AF36 on Corn Food/Feed Commodities...part 180 for residues of a pesticide chemical in or on various food commodities...regulations for residues of a pesticide in or on food...

2010-03-03

252

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

Directory of Open Access Journals (Sweden)

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.

Faqir Muhammad

2013-01-01

253

De-contamination of pesticide residues in food by ionizing radiation  

International Nuclear Information System (INIS)

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

254

Assessment of Organochlorine Pesticide Residues in the Surface Sediments of River Yamuna in Delhi, India  

Directory of Open Access Journals (Sweden)

Full Text Available The present study reports the concentration levels and distribution patterns of the organochlorine pesticide residues in the surface sediments of river Yamuna in the Indian capital state, Delhi. Analytical measurements were carried out for twenty organochlorine pesticides (OCPs in the Pre-monsoon, Monsoon and Post-monsoon seasons, at six different sampling locations along the 22 km stretch of the river Yamuna in Delhi. The results revealed contamination of the surface sediments with several persistent organochlorine pesticides. Endrin aldehyde, Endosulfan sulfate and DDT showed the highest percentage composition of OCP at all the sampling sites in all the three seasons. The total organochlorine pesticides level ranged from 157.71 - 307.66 ng/g in Pre-monsoon to 195.86 - 577.74 ng/g in Monsoon and 306.9 - 844.45 ng/g in the Post-monsoon season. This not only demonstrates the pollution of the river with pesticide residues, but also the necessity of a continuous long-term monitoring of the affected environment.

Puneeta Pandey

2011-07-01

255

Stability of pesticides' residues under ultraviolet germicidal irradiation.  

Science.gov (United States)

Legislation for food safety is limited mostly to pesticides monitoring and no attention is paid to the presence and toxicity of by-products formed after pesticide application. Stability studies of three selected transformation products: IMP - 2-isopropyl-6-methyl-4-pyrimidinol (diazinon hydrolysis product), TCP - 3,5,6-trichloro-2-pyridinol (chlorpyrifos transformation product), and 6CNA - 6-chloronicotinic acid (imidacloprid and acetamiprid transformation product) were performed under exposure to sunlight at room temperature (22 °C) and in the dark at 4 °C over 90 days. The results showed slight change in concentration with samples under refrigeration in darkness.Alternatively, an aqueous solution of TCP exposed to sunlight resulted in a high decrease of initial concentration within time. The toxicity assessment was performed using luminescent bacteria Vibrio fischeri and the results expressed low toxicity in the case of IMP and 6CNA. However, for TCP the calculated EC50 value after 30 minutes of exposure equated to roughly 15.1 mg L-1. Stability of the selected transformation products upon 245 nm irradiation indicated little decrease in concentration for IMP and 6CNA in deoxygenated and oxygenated aqueous solutions. In the case of TCP, the photochemical behaviour appeared to depend on oxygen concentration in the medium. For more detailed comparison, the degradation quantum yields were calculated. PMID:24062043

Zabar, Romina; Sarakha, Mohamed; Chung, Pascal Wong Wah; Trebše, Polonca

2011-06-01

256

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

Science.gov (United States)

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

257

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

Directory of Open Access Journals (Sweden)

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

Ademola F. Aiyesanmi

2012-05-01

258

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

Science.gov (United States)

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

Wang, Jian; Cheung, Wendy; Leung, Daniel

2014-01-29

259

Effects of ozone microbubble treatment on removal of residual pesticides and quality of persimmon leaves.  

Science.gov (United States)

This study investigated the effects of ozone microbubble (OMCB) treatment on the removal of residual fenitrothion (FT) and benomyl pesticides from red and green persimmon leaves, and also the treatment effect on the leaf colours, physical properties and flavour. The continuous bubbling OMCB treatment was more effective than the non-bubbling OMCB treatments at reducing the FT and benomyl agricultural pesticide residues from both the red and green persimmon leaves. Moreover, the bubbling OMCB treatment had no effect on the colour and pulling strength of the leaves. These results indicate that the treatment by bubbling OMCB is an extremely effective method for removing the residues of FT and benomyl in persimmon leaves and has relatively little effect on leaf quality characteristics. PMID:23265500

Ikeura, Hiromi; Hamasaki, Sadahiro; Tamaki, Masahiko

2013-05-01

260

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

Science.gov (United States)

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

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

2014-07-01

 
 
 
 
261

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

Directory of Open Access Journals (Sweden)

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

Botwe, B. O.

2011-08-01

262

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

International Nuclear Information System (INIS)

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

263

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

Science.gov (United States)

In agricultural fields, soil and water quality preservation is strongly influenced by pesticides use and behavior. To limit the environmental impacts of agricultural activities, best management practices such as the use of cover crops are encouraged. Cover crops during the fallow period were found to be efficient in reducing nitrate leaching, controlling soil erosion, improving soil organic content and enhancing soil biological activity. This technique was also found to modify soil water dynamics in the following crop. According to these effects, modifications on pesticide behavior in soil, such as sorption, degradation and transport, are expected (Alletto et al., 2012 ; 2013). In this study, the impact of the nature and level of decomposition of cover crop was studied on the sorption characteristics of three pesticides. These pesticides differed in their physicochemical characteristics (hydrophobicity, solubility, persistence) and were two herbicides, S-metolachlor and glyphosate, which are largely used in maize production and predominantly found as pollutants in water; and one fungicide, epoxiconazole. Correlations between pesticide sorption and physicochemical characteristics of the cover crop residues were studied. Residues of oat, turnip rape, red clover and phacelia were collected in March 2011 and incubated at 28°C and at the water holding capacity during 0, 6, 28 or 56 days. For each date, adsorption of the three radiolabeled pesticides was measured in batch on the different cover crop residues, and their biochemical composition (Van Soest fractionation), hydrophobicity (contact angle measurement) and C/N ratio were determined. Results showed that the adsorption of the pesticides differed significantly according to (i) the pesticide, (ii) the nature of cover crop, (iii) the decomposition level of the cover crop and the interaction cover crop x decomposition time. Epoxiconazole was the most adsorbed molecule, with Kd values ranging from 161 ± 30 L/Kg (oat, turnip rape, phacelia) to 206 ± 45 L/Kg (red clover); and glyphosate was the less adsorbed, with Kd values ranging from 1 ± 1 L/Kg (oat, red clover) to 9 ± 1 L/Kg (phacelia) at day 0. Differences between pesticides were expected considering the hydrophobicity of these molecules. Adsorption of the three pesticides increased with decomposition time (up to sevenfold for glyphosate on oat), and was negatively correlated with C/N ratio (-0.73glyphosate on oat and turnip rape (?=-0.99 and ?=-0.62, psoil surface influenced the mobility of pesticides as it was observed in decomposing mulch of crop residues (Aslam et al., 2013). As a result, the type of cover crop and the changes of cover crop residues composition during decomposition in field may control differently the movement of non-ionic pesticides compared to ionic compounds such as glyphosate, largely used in conservation agriculture practices. Keywords : Cover crops ; Glyphosate ; S-metolachlor ; Epoxiconazole ; Mulch; Sorption ; Biochemical composition References Alletto L., Benoit P., Justes E., Coquet Y. 2012. Effects of tillage and fallow period management on the fate of the herbicide isoxaflutole in an irrigated continuous-maize field. Agriculture, Ecosystems Environment, 153, 40- 49. http://dx.doi:10.1016/j.agee.2012.03.002 Alletto L., Benoit P., Coufignal M., Bergheaud V., Dumény V., Longueval D., Barriuso E. 2013. Sorption and mineralization of S-metolachlor in 51 fields cultivated with conservation tillage. Soil Tillage Research 128, 97-103. http://dx.doi.org/10.1016/j.still.2012.11.005 Aslam S., Garnier P., Rumpel C., Parent S., Benoit P. 2013. Adsor

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

2013-04-01

264

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

International Nuclear Information System (INIS)

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

265

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

International Nuclear Information System (INIS)

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

266

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

International Nuclear Information System (INIS)

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

267

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

The specific objectives are: i) to determine the level of awareness of pesticide residue in locally available food among food sellers in Ile Ife area of Osun state, Nigeria; ii) to identify the demographic and socio-economic characteristics of food sellers who use pesticides, natural means in preserving their foodstuff from getting spoilt; iii) to determine the level of understanding of food sellers who use pesticides about the likely health implications that could result. The design of the s...

Samson Ayo Deji

2012-01-01

268

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

Directory of Open Access Journals (Sweden)

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

Gevany P. Pinho

2009-01-01

269

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

Scientific Electronic Library Online (English)

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

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

270

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.  

Science.gov (United States)

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 ?g/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 ?g/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 ?g/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 ?g/kg ww for carp and perch, respectively. Contamination of fish reflected generally concentrations in surroundings. Isoproturon was the most concentrated and its main source was water for perch while carp was exposed through both water and sediments, highlighting their life strategies in pond. PMID:22961490

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

2013-01-01

271

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

Science.gov (United States)

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

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

2011-12-01

272

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

International Nuclear Information System (INIS)

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

273

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

Energy Technology Data Exchange (ETDEWEB)

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

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

2009-12-15

274

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

Science.gov (United States)

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

275

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

Science.gov (United States)

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

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

2006-01-01

276

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

Directory of Open Access Journals (Sweden)

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

VALENTINA L. CHRISTOVA-BAGDASSARIAN

2014-07-01

277

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

Science.gov (United States)

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. PMID:22864634

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

2012-10-01

278

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

International Nuclear Information System (INIS)

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

279

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

Science.gov (United States)

...use permit microbial pesticides product analysis data requirements table. ...use permit microbial pesticides product analysis data requirements table. ...this table to determine the product analysis data requirements and...

2010-07-01

280

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

Science.gov (United States)

...false Microbial pesticides product analysis data requirements table. ...2120 Microbial pesticides product analysis data requirements table. ...use this table to determine the product analysis data requirements and...

2010-07-01

 
 
 
 
281

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

Efsa, Panel On Plant Protection Products And Their Residues

2012-01-01

282

Endocrine disrupting activity in fruits and vegetables evaluated with the E-screen assay in relation to pesticide residues.  

Digital Repository Infrastructure Vision for European Research (DRIVER)

Food is likely to be one of the most important routes of human exposure to endocrine disrupting compounds (EDCs). In the present study, we evaluated the total estrogenic activity of fruits and vegetables, which was calculated using the human breast cancer cell line (MCF-7 BUS) proliferation assay (E-screen), in relation to pesticide residues. We analysed 44 food samples, 30 fruits and 14 vegetables. Of these samples, 10 did not contain any pesticide residues. The other 34 samples contained fr...

Gilli, Giorgio; Schiliro, Tiziana

2011-01-01

283

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

International Nuclear Information System (INIS)

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

284

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

Science.gov (United States)

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

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

2013-01-01

285

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

International Nuclear Information System (INIS)

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

286

Determination of pesticide residues in integrated pest management and nonintegrated pest management samples of apple (Malus pumila Mill.).  

Science.gov (United States)

Studies were undertaken to analyze the residues of commonly used pesticides viz. chlorpyrifos, endosulfan, dicofol, cypermethrin, fenvalerate, propargite, malathion, phorate, carbendazim, carbosulfan, thiamethoxam, and mancozeb in apple of integrated pest management (IPM) and non-IPM samples collected from the IPM and non-IPM fields of Shimla. We also present a method for the determination of these pesticides in apple samples. Residues of chlorpyrifos, endosulfan, dicofol, cypermethrin, fenvalerate, and propargite were analyzed by gas chromatography, while residues of carbendazim, carbosulfan, and thiamethoxam were analyzed by high-performance liquid chromatography. Residues of mancozeb were determined by a colorimetric method. Recoveries of all of the pesticides ranged from 61.30 to 95.46% at 0.1, 0.2, and 1.0 microg g(-1) levels of fortification with relative standard deviations ranging between 0.8 and 8.7. Apples from IPM and non-IPM orchards were analyzed for these pesticides using a developed method. Except for carbendazim and chlorpyrifos, the residues of all of the pesticides analyzed were below detectable limits. Although residues of carbendazim and chlorpyrifos were below the prescribed limits of maximum residue levels in both IPM and non-IPM orchards, residues were lower in apples from IPM orchards. PMID:19904932

Singh, Shashi Bala; Mukherjee, Irani; Maisnam, Jaya; Kumar, Praveen; Gopal, Madhuban; Kulshrestha, Gita

2009-12-01

287

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

International Nuclear Information System (INIS)

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

288

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

Directory of Open Access Journals (Sweden)

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

F. Upadhi

2012-11-01

289

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

Science.gov (United States)

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

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

2000-11-01

290

Dietary exposure of Hong Kong adults to pesticide residues: results of the first Hong Kong total diet study.  

Science.gov (United States)

The use of pesticides and other chemicals has become a common practice in modern agriculture to enhance and stabilise crop yield, protect the nutritional integrity of food, facilitate food storage to assure year-round supplies, and provide attractive and appealing food products. With the adoption of strict good agricultural practice (GAP), only minimal amounts of pesticide residues should remain on the crops or in connected foods of animal origin up the food chain. To assess their associated health risk to local people, the dietary exposure of Hong Kong adults to residues of four groups of pesticides or their metabolites - organophosphorus pesticides (OPPs), carbamates, pyrethrins and pyrethroids, and dithiocarbamate (DTC) metabolites - is estimated in the first Hong Kong Total Diet Study (TDS). A total of 150 commonly consumed food items were collected and prepared "as consumed". A total of 600 composite food samples were analysed for 85 pesticides or their metabolites by liquid chromatography-tandem mass spectrometry (LC-MS/MS). These pesticides were primarily found at low levels (highest mean = 350 ?g kg(-1)) in food samples of plant origin such as vegetables and fruits. Dietary exposures to pesticide residues were estimated based on the analytical results and the food consumption data of the local residents. The estimated dietary exposures of Hong Kong adults to all individual pesticides were well below their respective acceptable daily intakes (ADIs). The percentage contributions of the estimated mean and 95th percentile dietary exposures to the ADIs of individual pesticides were <6% and <24% for the OPPs, <1% for the carbamates and pyrethrins and pyrethroids, and <1% and <4% for the DTC metabolites, respectively. The findings indicate that dietary exposures to all the pesticide residues analysed in this study were unlikely to pose unacceptable health risks to the Hong Kong population. PMID:24588687

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

2014-01-01

291

Use, analysis, and regulation of pesticides in natural extracts, essential oils, concretes, and absolutes.  

Science.gov (United States)

Natural extracts used by the fragrance and cosmetics industries, namely essential oils, concretes, resinoids, and absolutes, are produced from natural raw materials. These are often cultivated by use of monoculture techniques that involve the use of different classes of xenobiotica, including pesticides. Because of these pesticides’ potential effect on public health and the environment, laws regarding permitted residual levels of pesticides used in cultivation of raw materials for fragrance and cosmetic products are expected to become stricter. The purpose of this review is to present and classify pesticides commonly used in the cultivation of these natural raw materials. We will summarize the most recent regulations, and discuss publications on detection of pesticides via chemical analysis of raw natural extracts. Advances in analytical chemistry for identification and quantification of pesticides will be presented, including both sample preparation and modern separation and detection techniques, and examples of the identification and quantification of individual pesticides present in natural extracts, for example essential oils, will be provided. PMID:23797908

Tascone, Oriane; Roy, Céline; Filippi, Jean-Jacques; Meierhenrich, Uwe J

2014-02-01

292

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

International Nuclear Information System (INIS)

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

293

Survey of organophosphorus pesticide residues in virgin olive oils produced in Chile.  

Science.gov (United States)

Dimethoate, diazinon, parathion methyl, pirimiphos methyl, malathion, fenthion, chlorpyriphos, methidathion and azinphos methyl were determined in 71 olive oil samples produced in Chile from different varieties of olives (arbequina, frantoio, picual, lechino and blend) at three different harvest periods (2007, 2008 and 2009). The target pesticides were determined using a validated analytical method based on microwave-assisted liquid-liquid and solid-phase extraction with subsequent GC-FPD detection and GC-MS/MS for confirmation purposes. In 79% of the samples, five of the nine pesticides tested were detected with a frequency of one pesticide per sample. The highest detection rates were observed for the residues of chlorpyriphos and diazinon. The average concentration of chlorpyriphos, diazinon, azinphos methyl and methidathion were 0.084, 0.057, 0.024 and 0.010 µg g(-1), respectively. Higher contents of organophosphorus pesticides (OPPs) were found in regions where intensive agriculture is practiced. However, the levels of OPPs were reassuringly low and indicate that olive oil produced and exported from Chile does not currently represent any risk for consumers. PMID:24785499

Fuentes, Edwar; Báez, María E; Díaz, Juan

2010-01-01

294

De-contamination of pesticide residues in food by ionizing radiation  

Science.gov (United States)

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

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

2012-04-01

295

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

Science.gov (United States)

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

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

2010-10-01

296

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

Scientific Electronic Library Online (English)

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

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

297

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

Directory of Open Access Journals (Sweden)

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

Isabel Cristina Sales Fontes Jardim

2009-01-01

298

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

International Nuclear Information System (INIS)

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

299

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

Directory of Open Access Journals (Sweden)

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.

Aamand Jens

2011-01-01

300

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

DEFF Research Database (Denmark)

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.

Bache, Michael; Taboryski, Rafael Jozef

2011-01-01

 
 
 
 
301

Simultaneous determination of 405 pesticide residues in grain by accelerated solvent extraction then gas chromatography-mass spectrometry or liquid chromatography-tandem mass spectrometry.  

Science.gov (United States)

A new method has been established for simultaneous determination of 405 pesticide residues in grain, using accelerated solvent extraction (ASE), solid-phase extraction (SPE), and GC-MS and LC-MS-MS. The method was based on appraisal of the GC-MS and LC-MS-MS characteristics of 660 pesticides, their efficiency of extraction from grain, and their purification. Samples of grain (10 g) were mixed with Celite 545 (10 g) and the mixture was placed in a 34-mL cell of an accelerated solvent extractor and extracted with acetonitrile in the static state for 3 min with two cycles at 1,500 psig and at 80 degrees C. For the 362 pesticides determined by GC-MS, half of the extracts were cleaned with an Envi-18 cartridge and then further cleaned with Envi-Carb and Sep-Pak NH2 cartridges in series. The pesticides were eluted with acetonitrile-toluene, 3:1, and the eluates were concentrated and used for analysis after being exchanged with hexane twice. For the 43 pesticides determined by LC-MS-MS the other half of the extracts were cleaned with Sep-Pak Alumina N cartridge and further cleaned with Envi-Carb and Sep-Pak NH2 cartridges. Pesticides were eluted with acetonitrile-toluene, 3:1. After evaporation to dryness the eluates were diluted with acetonitrile-water, 3:2, and used for analysis. In the linear range of each pesticide the linear correlation coefficient r was equal to or greater than 0.956 and 94% of linear correlation coefficients were greater than 0.990. At low, medium, and high fortification levels, at the limit of detection (LOD), twice the LOD and ten times LOD, respectively, recoveries ranged from 42 to 132%; for 382 pesticides, or 94.32%, recovery was from 60 to 120%. The relative standard deviation (RSD) was always below 38% and was below 30% for 391 pesticides, or 96.54%. The LOD was 0.0005-0.3000 mg kg(-1). The proposed method is suitable for determination of 405 pesticide residues in grain such as maize, wheat, oat, rice, and barley, etc. PMID:16520938

Pang, Guo-Fang; Liu, Yong-Ming; Fan, Chun-Lin; Zhang, Jin-Jie; Cao, Yan-Zhong; Li, Xue-Min; Li, Zeng-Yin; Wu, Yan-Ping; Guo, Tong-Tong

2006-03-01

302

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

Directory of Open Access Journals (Sweden)

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

Yao Xin

2010-06-01

303

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

Science.gov (United States)

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. PMID:24184045

Masci, Maurizio; Orban, Elena; Nevigato, Teresina

2014-01-01

304

Dispersive microextraction based on magnetic polypyrrole nanowires for the fast determination of pesticide residues in beverage and environmental water samples.  

Science.gov (United States)

In this study, magnetic polypyrrole nanowires (mPPYs) were fabricated via a simple co-mixing method based on an "aggregation-wrap" mechanism. The polypyrrole (PPy) nanowires were synthesized by in situ chemical oxidative polymerization using cetyltrimethylammonium bromide as the "soft template" and the magnetic nanoparticles (MNPs) prepared using solvothermal methods. Typically, when these two nanomaterials were vortically mixed in a solvent, the MNPs were wrapped into the PPy nanowire networks that formed during the aggregation process, leading to the formation of mPPYs which can be separated from the solvent rapidly and conveniently by a magnet. Due to the better permeability, good adsorption ability, and magnetic separability of the resultant material, mPPYs were applied for the enrichment of 11 pesticides including organophosphorus, organochlorine, and pyrethroid using magnetic solid phase extraction (MSPE) to test their feasibility in sample preparation. Several parameters affecting the extraction efficiency were investigated, and under the optimized conditions, a simple and effective method for the determination of pesticide residues was established by coupling with gas chromatography/mass spectrometry (GC/MS) analysis. The whole pretreatment process was rapid and can be accomplished within 15 min. The linearity range of the proposed method was 0.2-10 ?g/L, with correlation coefficients (R) of 0.995-0.999; the limits of quantification for the target compounds were in the range of 0.09-0.29 ?g/L. In addition, an acceptable reproducibility was achieved by evaluating the intra- and inter-day precisions with relative standard deviations of less than 14 and 16 %, respectively. Finally, the established MSPE-GC/MS method was successfully applied for the determination of pesticide residues in beverage teas, juices, and environmental water samples. PMID:23515608

Zhao, Qin; Lu, Qian; Feng, Yu-Qi

2013-05-01

305

Pesticide residues in honeybees, honey and bee pollen by LC-MS/MS screening: reported death incidents in honeybees.  

Science.gov (United States)

The aim of this study was to investigate reported cases of honeybee death incidents with regard to the potential interrelation to the exposure to pesticides. Thus honeybee, bee pollen and honey samples from different areas of Greece were analyzed for the presence of pesticide residues. In this context an LC-ESI-MS/MS multiresidue method of total 115 analytes of different chemical classes such as neonicotinoids, organophosphates, triazoles, carbamates, dicarboximides and dinitroanilines in honeybee bodies, honey and bee pollen was developed and validated. The method presents good linearity over the ranges assayed with correlation coefficient values r(2)?0.99, recoveries ranging for all matrices from 59 to 117% and precision (RSD%) values ranging from 4 to 27%. LOD and LOQ values ranged - for honeybees, honey and bee pollen - from 0.03 to 23.3 ng/g matrix weight and 0.1 up to 78 ng/g matrix weight, respectively. Therefore this method is sufficient to act as a monitoring tool for the determination of pesticide residues in cases of suspected honeybee poisoning incidents. From the analysis of the samples the presence of 14 active substances was observed in all matrices with concentrations ranging for honeybees from 0.3 to 81.5 ng/g, for bee pollen from 6.1 to 1273 ng/g and for honey one sample was positive to carbendazim at 1.6 ng/g. The latter confirmed the presence of such type of compounds in honeybee body and apicultural products. PMID:24747255

Kasiotis, Konstantinos M; Anagnostopoulos, Chris; Anastasiadou, Pelagia; Machera, Kyriaki

2014-07-01

306

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

Science.gov (United States)

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

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

2008-06-01

307

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

International Nuclear Information System (INIS)

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

308

Monitoring the Residue Level of Three Selected Pesticides in Red Amaranth  

Directory of Open Access Journals (Sweden)

Full Text Available A study was undertaken in the Department of Biochemistry, Bangladesh Agricultural University, Mymensingh to monitor the level of three selected pesticides at various dose levels. In this case edible part of red amaranth was extracted and analyzed for applied pesticide residues. It was found that after one day 0.0065 ?g of cypermethrin retained per g of plant sample, which was 0.23% of the applied dose. While on the 3rd day of spray the level of residue was found to decrease (0.0024 ?g g1-1 which accounted for 0.085% of the applied dose. In case of higher dose applied, the residue level of chlorpyrifos was 0.0173 ?g g-1 whereas the level increased to 0.0237 ?g g1-1 on 3rd day of application. It seemed that the uptake of chlorpyrifos by red amaranth from soil and its accumulation therein was higher on 3rd day of application. The residue level of carbofuran was very low both at 1st and 3rd day of application. However, an increasing trend of incorporation was observed on 3rd day of application. It is remarkable to note that when higher level of chlorpyrifos and carbofuran were jointly applied, the amount of chlorpyrifos as residue increased but the level of carbofuran decreased. Finally carbofuran could not be traced after 72 h of joint application. So study indicated that chlorpyrifos might exert antagonistic effect on the uptake/accumulation of carbofuran in plant system.

Jahan Ara Khatoon

2004-01-01

309

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

Science.gov (United States)

The levels of dichlorodiphenyltrichloroethane (DDT), dichlorodiphenyldichloroethylene (DDE), endosulfan, endosulfan sulfate, carbofuran, and cartap which were estimated in the flesh of Catla catla sampled from ten sites of Ravi River between its stretches from Shahdara to Head Balloki were studied to know the level of contamination of the selected pesticides by GC-ECD method. All fish samples were found contaminated with different concentrations of DDT, DDE, endosulfan, and carbofuran; however, DDT and DDE concentrations were more than the maximum residue limits (MRLs) about food standards, while endosulfan sulfate and cartap were not detected. Pesticide concentrations in the fish flesh were ranged from 3.240 to 3.389 for DDT, 2.290 to 2.460 for DDE, 0.112 to 0.136 for endosulfan, and 0.260 to 0.370??g?g?1 for carbofuran. The findings revealed that the pesticide concentrations in the fish flesh decreased in the order: DDT > DDE > carbofuran > endosulfan. After Degh fall and After Hudiara nulla fall river sampling sites were found severely contaminated. It is proposed that a constant monitoring programs are needed to be initiated to overcome the present alarming situation. PMID:25003148

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

2014-01-01

310

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

Science.gov (United States)

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

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

2011-05-01

311

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

Scientific Electronic Library Online (English)

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

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

312

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

Directory of Open Access Journals (Sweden)

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

Mário Sérgio Galhiane

2012-01-01

313

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

Science.gov (United States)

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. PMID:11697784

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

2001-01-01

314

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

Science.gov (United States)

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

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

2014-01-01

315

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

Directory of Open Access Journals (Sweden)

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

Djouaka Rousseau F

2006-03-01

316

Pesticides  

Science.gov (United States)

... exposure, as well as on the treatment and prevention of pesticide poisoning. Evaluating Chemicals: Is It ... Student Edition Lesson: Arsenic and Lead Scavenger Hunt (357KB) EHP Student Edition ...

317

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

Directory of Open Access Journals (Sweden)

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.

Wanpen Mesomya

2012-11-01

318

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

Science.gov (United States)

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

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

2012-05-01

319

Determination of organochlorine pesticide residues in fatty foods: a critical review on the analytical methods and their testing capabilities.  

Science.gov (United States)

Organochlorine pesticide (OCP) residues in foods have been of concern for several decades. However, the analysis of some of the OCPs and their metabolites or derivatives, such as endrin aldehyde, endrin ketone, nonachlor, etc. in fatty foods (including foods of animal and plant origin), was not commonly included in routine monitoring programme. Recently, the Stockholm Convention introduced nine plus one new persistent organic pollutants (POPs) that included chlordecone and some other OCPs. Is there a method available that can analyze both traditional OCPs, together with their metabolites and derivatives in fatty foods? Furthermore, is there a suitable method that can monitor OCPs and the newly added POPs including chlordecone in fatty foods together in a pot? This review aims to provide some background information to answer these questions. PMID:21742333

Chung, Stephen W C; Chen, Benedict L S

2011-08-19

320

Determination of Pesticide Residues in Soil by Modified Matrix Solid-Phase Dispersion and Gas Chromatography  

International Nuclear Information System (INIS)

Modified matrix solid-phase dispersion (MMSPD) and gas chromatography have been developed for quantitative analysis of various classes of pesticides (pirimicarb, metalaxyl, metolachlor, isopropalin and pendimethalin) in soil. MMSPD used Florisil as dispersant and acetone as solvent. Determination was carried out by gas chromatography with nitrogen-phosphorus detection (GC-NPD). The effect of the residence time of pesticides in soil on the recoveries was studied. MMSPD was compared with continuous liquid-solid extraction (LSE). MMSPD had good extraction efficiency and cleanup efficiency and the extract obtained could be directly subjected to GC analysis without further purification. The method gave recoveries ranging from 93% to 100% with relative standard deviations (RSDs) lower than 10%. The limits of detection (LODs) ranged from 0.2 to 2.0 ng g-1

 
 
 
 
321

Overall calibration procedure via a statistically based matrix-comprehensive approach in the stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry analysis of pesticide residues in fruit-based soft drinks.  

Science.gov (United States)

Stir bar sorptive extraction (SBSE)-thermal desorption (TD) procedure combined with gas chromatography mass spectrometry (GC-MS) and the statistical variance component model (VCM) is applied to the determination of semi-volatile compounds including organochlorine and organophosphorus pesticides in various synthetic and real fruit-based soft drink matrices. When the matrix effects are corrected using isotopically labelled or non labelled internal standard, but matrix/calibration run-induced deviations are still present in the measurements, the adoption of a variance component model (VCM) in the quantitative analysis of various matrices via an overall calibration curve is successful. The method produces an overall calibration straight line for any analyte accounting for the uncertainty due to all the sources of uncertainty, namely matrix-induced deviations, calibration runs performed at different times, measurement errors. Small increases in the detection limits and in uncertainty in the concentration values obtained in the inverse regression face favourably the decrease in times and costs for routine analyses. PMID:21238780

Lavagnini, Irma; Urbani, Alessandro; Magno, Franco

2011-02-15

322

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

Science.gov (United States)

An atmospheric pressure chemical ionization source has been used to enhance the potential of gas chromatography coupled with quadrupole time-of-flight (QTOF) mass spectrometry (MS) for screening and quantification purposes in pesticide residue analysis. A screening method developed in our laboratory for around 130 pesticides has been applied to fruit and vegetable samples, including strawberries, oranges, apples, carrots, lettuces, courgettes, red peppers, and tomatoes. Samples were analyzed together with quality control samples (at 0.05 mg/kg) for each matrix and for matrix-matched calibration standards. The screening strategy consisted in first rapid searching and detection, and then a refined identification step using the QTOF capabilities (MS(E) and accurate mass). Identification was based on the presence of one characteristic m/z ion (Q) obtained with the low collision energy function and at least one fragment ion (q) obtained with the high collision energy function, both with mass errors of less than 5 ppm, and an ion intensity ratio (q/Q) within the tolerances permitted. Following this strategy, 15 of 130 pesticides were identified in the samples. Afterwards, the quantitation capabilities were tested by performing a quantitative validation for those pesticides detected in the samples. To this aim, five matrices were selected (orange, apple, tomato, lettuce, and carrot) and spiked at two concentrations (0.01 and 0.1 mg/kg), and quantification was done using matrix-matched calibration standards (relative responses versus triphenyl phosphate used as an internal standard). Acceptable average recoveries and relative standard deviations were obtained for many but not all pesticide-matrix combinations. These figures allowed us to perform a retrospective quantification of positives found in the screening without the need for additional analysis. Taking advantage of the accurate-mass full-spectrum data provided by QTOF MS, we searched for a higher number of compounds (up to 416 pesticides) in a second stage by performing extra data processing without any new sample injection. Several more pesticides were detected, confirmed, and/or tentatively identified when the reference standard was unavailable, illustrating in this way the potential of gas chromatography-QTOF MS to detect pesticides in addition to the ones targeted in quantitative analysis of pesticides in food matrices. PMID:24828980

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

2014-11-01

323

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

Science.gov (United States)

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

324

Occurrence and possible fate of organochlorine pesticide residues at Manzala Lake in Egypt as a model study.  

Science.gov (United States)

Persistence of the residue of organochlorine pesticides (OCPs) became a great danger to our environment long ago. In this study, the persistence of OCPs at Manzala Lake in Egypt was determined. Four different sites were investigated: the El-Gamel, El-Kowar, El-Rasoah, and Janb El-Timsah regions. Among these, the El-Kowar region had the highest concentration of total OCPs in the sediment samples when compared to other regions during both 2012 and 2013. In fact, generally, the residues of OCPs in the sediment samples were significantly higher in all tested sites in comparison with other compartments. Conversely, OCP residues were undetectable in water samples at both the El-Gamel region and the El-Rasoah site in the studied seasons. The data proved that the sediment layer plays a sourcing role in OCP persistence in the aquatic ecosystem. Data analysis also indicated that there was an external source for OCP contamination in the Manzala Lake ecosystem that most likely comes from Nile Basin countries and which extends the expected half-life of these compounds. It could be exemplified by DDT, the half-life of which increased from 30 to approximately 47 years. PMID:25424498

Kamel, Essam; Moussa, Saad; Abonorag, Mostafa A; Konuk, Muhsin

2015-01-01

325

Validation of pestice multi residue analysis method on cucumber  

International Nuclear Information System (INIS)

In this study we aimed to validate the method of multi pesticide residue analysis on cucumber. Before real sample injection, system suitability test was performed in gas chromatography (GC). For this purpose, a sensitive pesticide mixture was used for GC-NPD and estimated the performance parameters such as number of effective theoretical plates, resolution factor, asymmetry, tailing and selectivity. It was detected that the system was suitable for calibration and sample injection. Samples were fortified at the level of 0.02, 0.2, 0.8 and 1 mg/kg with mixture of dichlorvos, malathion and chloropyrifos pesticides. In the fortification step 14C-carbaryl was also added on homogenized analytical portions to make use of 14C labelled pesticides for the determining extraction efficiency. Then the basic analytical process, such as ethyl acetate extraction, filtration, evaporation and cleanup, were performed. The GPC calibration using 14C- carbaryl and fortification mixture (dichlorvos, malathion and chloropyrifos) showed that pesticide fraction come through the column between the 8-23 ml fractions. The recovery of 14C-carbaryl after the extraction and cleanup step were 92.63-111.73 % and 74.83-102.22 %, respectively. The stability of pesticides during analysis is an important factor. In this study, stability test was performed including matrix effect. Our calculation and t test results showed that above mentioned pesticides were not stabile during sample processing in our laboratory conditions and it was found that sample comminution with dry ice may improve stability. In the other part of the study, 14C-chloropyrifos was used to determine homogeneity of analytical portions taken from laboratory samples. Use of 14C labelled pesticides allows us for quick quantification analyte, even with out clean-up. The analytical results show that after sample processing with waring blender, analytical portions were homogenous. Sample processing uncertainty depending on quantity of analytical portions was calculated from sampling constant equation (Ks=WxCVsp2). CVsp for 50 g was 4.539% and 8.033% for 5 g analytical portions.

326

Residuos de plaguicidas organoclorados en 4 tipos de aceites vegetales / Organochlorine pesticide residues in 4 types of vegetable oils.  

Scientific Electronic Library Online (English)

Full Text Available SciELO Venezuela | Language: Spanish Abstract in spanish Esta investigación tuvo como objetivos identificar y cuantificar residuos de los plaguicidas organoclorados (POC) hexaclorobenceno (HCB), lindano, cis-clordano, heptacloro, aldrín, dieldrín, endrín y o,p’-diclorodifeniltricloroetano (o,p’-DDT) en aceites de maíz, soya, girasol y mezclas de aceites, [...] que se expenden en la ciudad de Maracaibo, Venezuela. Se analizaron 30 muestras de 4 tipos de aceites de 10 marcas comerciales. La extracción de residuos de POC se realizó según la técnica de la AOAC. Para la identificación y cuantificación se utilizó un cromatógrafo de gases con detector de captura electrónica (GC-ECD), y para la confirmación, un cromatógrafo de gases acoplado a un espectrómetro de masas (GCMS). Todos los residuos de POC investigados fueron detectados en las muestras analizadas. Se detectaron en mayor concentración (mg/ g) aldrín (0,0088), lindano (0,0054) y o,p’-DDT (0,0035). El análisis estadístico demostró diferencias significativas (P Abstract in english The present study had as objectives to identify and to quantify organochlorine pesticide residues (OCP) hexachlorobenzene (HCB), lindane, cis-chlordane, heptachlor, aldrín, dieldrín, endrín and o,p’-DDT in vegetable oils of corn, soybean, sunflower and mixtures of oils, sold in the city of Maracaibo [...] , Venezuela. 30 samples of 4 types of vegetable oils of 10 commercial brands were analyzed. The extraction of OCP residues was done according to the Official Method of AOAC. A gas chromatograph with an electronic capture detector (GC-ECD) was used for identification and quantification of OCP residues and confirmation was done with a gas chromatograph coupled with a mass spectrometer (GC-MS). All the OCP residues investigated were detected in the analyzed samples. Aldrin (0.0088), lindane (0.0054) and o,p’-DDT (0.0035) were the OCP residues detected in higher concentrations (mg/g). The statistical analysis showed significant differences (P

María, Piñero González; Pedro, Izquierdo Córser; María, Allara Cagnasso; Aiza, García Urdaneta.

327

Residuos de plaguicidas organoclorados en 4 tipos de aceites vegetales / Organochlorine pesticide residues in 4 types of vegetable oils.  

Scientific Electronic Library Online (English)

Full Text Available SciELO Venezuela | Language: Spanish Abstract in spanish Esta investigación tuvo como objetivos identificar y cuantificar residuos de los plaguicidas organoclorados (POC) hexaclorobenceno (HCB), lindano, cis-clordano, heptacloro, aldrín, dieldrín, endrín y o,p’-diclorodifeniltricloroetano (o,p’-DDT) en aceites de maíz, soya, girasol y mezclas de aceites, [...] que se expenden en la ciudad de Maracaibo, Venezuela. Se analizaron 30 muestras de 4 tipos de aceites de 10 marcas comerciales. La extracción de residuos de POC se realizó según la técnica de la AOAC. Para la identificación y cuantificación se utilizó un cromatógrafo de gases con detector de captura electrónica (GC-ECD), y para la confirmación, un cromatógrafo de gases acoplado a un espectrómetro de masas (GCMS). Todos los residuos de POC investigados fueron detectados en las muestras analizadas. Se detectaron en mayor concentración (mg/ g) aldrín (0,0088), lindano (0,0054) y o,p’-DDT (0,0035). El análisis estadístico demostró diferencias significativas (P Abstract in english The present study had as objectives to identify and to quantify organochlorine pesticide residues (OCP) hexachlorobenzene (HCB), lindane, cis-chlordane, heptachlor, aldrín, dieldrín, endrín and o,p’-DDT in vegetable oils of corn, soybean, sunflower and mixtures of oils, sold in the city of Maracaibo [...] , Venezuela. 30 samples of 4 types of vegetable oils of 10 commercial brands were analyzed. The extraction of OCP residues was done according to the Official Method of AOAC. A gas chromatograph with an electronic capture detector (GC-ECD) was used for identification and quantification of OCP residues and confirmation was done with a gas chromatograph coupled with a mass spectrometer (GC-MS). All the OCP residues investigated were detected in the analyzed samples. Aldrin (0.0088), lindane (0.0054) and o,p’-DDT (0.0035) were the OCP residues detected in higher concentrations (mg/g). The statistical analysis showed significant differences (P

María, Piñero González; Pedro, Izquierdo Córser; María, Allara Cagnasso; Aiza, García Urdaneta.

2007-12-01

328

Simultaneous determination of 50 residual pesticides in Flos Chrysanthemi using accelerated solvent extraction and gas chromatography.  

Science.gov (United States)

A gas chromatographic method for simultaneous determination of 50 organochlorine (OCP) and pyrethroid (PP) pesticides in Flos Chrysanthemi was established. Accelerated solvent extraction (ASE) technique was used to extract the target compounds, cleaned with alumina neutral-florisil column, and eluted by mixed solvents of ethyl acetate and hexane (15:85, v/v). Selected pesticides were identified using HP-5 and DB1701 capillary dual column and detected by electron-capture detector. Quantitative analysis was performed using an external standard by HP-5 capillary column. Results showed that recoveries were 73.4-120.1%, and the relative standard deviations (RSDs) were 1.6-12.4%. The limits of detection of the method were 0.0021-0.0069 mg/kg, and the limits of quantity were 0.0064-0.0210 mg/kg. PMID:25062509

Huang, Xiaohui; Zhao, Xinghui; Lu, Xiaotong; Tian, Huaiping; Xu, Ajing; Liu, Yan; Jian, Zhang

2014-09-15

329

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

Science.gov (United States)

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. PMID:22891938

Loos, Martin; Krauss, Martin; Fenner, Kathrin

2012-09-18

330

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

International Nuclear Information System (INIS)

A method for the multiresidue analysis of olive oil samples for 26 pesticides is proposed. Residual pesticides are extracted from oil using an n-hexane/acetonitrile mixture, extracts being cleaned-up by gel permeation chromatography (GPC) for analysis by gas chromatography-tandem mass spectrometry (GC-MS/MS). Electron ionization and chemical ionization are employed in a single analysis for the determination of pesticides. Pesticide recoveries from virgin and refined olive oil spiked with 10, 100 and 250 ?g/kg concentrations of the pesticides ranged from 83.8 to 110.3%. The proposed method features good sensitivity: its limits of quantification are low enough to allow pesticide residues to be determined at concentrations below the maximum residue levels legally accepted. The precision, expressed as relative standard deviation, ranges from 4.93 to 8.11%. Applicability was tested on 40 olive oil samples. Several pesticides were detected in most of the virgin olive oil samples. By contrast, refined olive samples contained few pesticides, and only endosulfan sulphate was detected in all

331

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

Science.gov (United States)

The integrated pest management (IPM) modules of pesticide schedule on Basmati rice were validated at field experiments conducted in Northern India for consecutive 3 years (2005-2008). The pesticide residues were found below the detectable limit (carbendazim in rice grains and soil were detected below Carbendazim applied as seed treatment at Dehradun and Kaithal field trials was found below detectable limit in both IPM and non-IPM rice grains (carbendazim (carbendazim (0.001-0.01 ?l/L) in water samples each from IPM and non-IPM fields of Uttar Pradesh. The results of 3-year trials of IPM module indicated basmati rice as safe and economical with pesticide residue-free rice grains. PMID:23996682

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

2014-01-01

332

Pesticide residues in two frog species in a paddy agroecosystem in palakkad district, kerala, India.  

Science.gov (United States)

Pesticides residues were quantified in 109 frogs comprising two species (Fejervarya limnocharis and Hoplobatrachus crassus) from organic and conventional paddy farms in Kerala, India. Seven frogs from conventional but none from the organic farms revealed deformities. Levels of total Organochlorines (OCs) (33.22 ng/g) and Synthetic Pyrethroid, Fenvalerate-II (26.91/42.15 ng/g) in deformed F. limnocharis and H. crassus were significantly greater than in healthy frogs. Among OCs in healthy frogs, traces of ? (gamma)-HCH (hexachlorocyclohexane) (2.12 ng/g) were found only in F. limnocharis from organic farm. Among Organophosphates, Phorate (1.02 ng/g) and Quinalphos (2.62 ng/g) were present in traces in deformed F. limnocharis, while Parathion ethyl (1.02 ng/g) was detected in deformed H. crassus. The data indicate that the high level of pesticides may have contributed to the deformity of frogs. Therefore, an elaborative study will be essential to conserve amphibians in India. PMID:25173364

Kittusamy, Ganesan; Kandaswamy, Chandrasekar; Kandan, Nambirajan; Subramanian, Muralidharan

2014-12-01

333

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

Scientific Electronic Library Online (English)

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

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

2013-11-15

334

Study of the effect of gamma irradiation on phenolic compounds and pesticides residues  

International Nuclear Information System (INIS)

The aim of this study was to show the effects of this process of conservation on the polyphenol rate and the antioxidant capacity of polyphenols of quince, of the cocoa and those of sage, then to study its effects on the pesticides residues in the sage sheets. The irradiation of quince polyphenols, increased the polyphenols rate as well as the antioxidant capacity. In the case of cocoa polyphenols, we don't have ace observed many differences between the irradiated and not irradiated samples, and in the case of sage polyphenols, the polyphenol rate as well as the antioxidant capacity decreased. Finally, irradiation of parathion caused degradation of this molecule, and the polyphenol rate as well as the antioxidant capacity pf polyphenols of the sheets of sage soaked with parathion was a less decreased than polyphenols of the sheets not soaked with parathion. (Author). 37 refs

335

Investigation of organochlorine pesticide residues in samples of 40 nursing mothers residing in Tehran  

Directory of Open Access Journals (Sweden)

Full Text Available Organochlorine pesticides are a group of persistant compounds which have been used for a long time. Due to their stability, some of them such as DDT, BHC and their derivatives are still used in the areas with malaria epidemic condition, hence the chance of food contamination always exists. The present survey demonstrated that human milk is one of the best indicator substances in monitoring the environment and human body contamination by organochlorine compounds. We studied the level of residues in the milk of nursing mothers who could be exposed to these compounds through food chain in their contaminated environment. In this investigation, we collected 40 samples from the nursing mothers of two hospitals located in the north and south of Tehran. Detection was carried out by Gas chromatography (GC with 3% OV17 column and Ni63 ECD (Electron Capture Detector. Reference substances were obtained from WHO. Results are discussed in the text.

Afshar M

1997-09-01

336

The determination of pesticide residues in local vegetables by means of neutron activation technique  

International Nuclear Information System (INIS)

Analytical methods based on neutron activation have been developed for studying pesticides residues of bromine, arsenic and mercury in local vegetables and fruits. The concentration of bromine, arsenic and mercury in samples are enriched prior to neutron irradiations by a technique of dry-ashing and freeze-drying for the determination of arsenic, bromine and mercury respectively. The element bromine is determined instrumentally while arsenic and mercury are determined destructively using a distillation technique. The limit of detection under the conditions used for bromine, arsenic and mercury as obtained are 0.01, 0.001 and 0.0001 microgram respectively. A total of 45 varieties of vegetables and 20 varieties of fruits are analyzed. The results of the investigation and the concentration range in part per million of bromine, arsenic and mercury are also presented

337

Effect of ?- ray, Microwave Heating and Solar Irradiation of Apple Juice on Organochlorinated Pesticides Residues  

Directory of Open Access Journals (Sweden)

Full Text Available This study was conducted to evaluate the effect of solar radiation, microwave heating and ?-irradiation on the Organochlorinated Pesticide (OCP's in apple juice. The solar radiation caused a destruction of 20% after 20 hr exposure to sunlight compared to 12% reduction for the tested OCP's after microwave heating for 10 min. On the other hand, the use of ?- irradiation leads to a degradation percentage of 30% after treatment with 25 kGray, while the irradiation with 5 kGray was found to produce insignificant effect on OCP?s residues when compared with the control treatments. The degradation was found to increase with increasing exposure time and all treatments were found to be not effective in complete destruction of OCP?s.

K. Al-Ismail

2009-01-01

338

Development of a fieldable rapid pesticide exposure analysis sensing system  

Science.gov (United States)

Despite the recent interest in organically grown foods, most agricultural crops use multiple pesticides to optimize yield. There are many persons whose health may be affected by the spraying; there is the active applicator and the passive neighbors. In between these extremes are the farm workers who pick the crops anywhere from days to weeks after application. How much pesticide residue are these workers exposed to during a workday and how much is transferred back to the residence? Despite the low vapor pressures, what is the true concentration of pesticides surrounding a person when pesticides adsorbed to particulate matter are included? What is the relationship between the concentration around an individual and the amount adsorbed/ingested? To answer these questions on a statistically significant scale in actual field conditions, a portable, fast, inexpensive measurement device is required. We present herein results obtained using Surface-Enhanced Raman Spectroscopy (SERS) that demonstrate the capability to detect < 100 organophosphate, organochlorine and carbamate-based pesticides in the vapor phase as well as the ability of SERS sensors to detect a particular analyte in a synthetic urine matrix. We will also present data collected from CDC quantified urine samples and will present results obtained in a field test wherein SERS sensors wore worn as dosimeters in the field and real-time vapor sampling of the farm workers barracks was performed. The issue of potential interferences will also be discussed.

Spencer, Kevin M.; Clauson, Susan L.; Spencer, Sarah A.; Sylvia, James M.; Vallejos, Quirina M.; Quandt, Sara A.; Arcury, Thomas A.

2010-04-01

339

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

DEFF Research Database (Denmark)

We are working on the development of a real-time electrochemical sensor based on an immunoassay detection system to detect and quantify the presence of pesticide residues in ground water. Highly selective and sensitive immuno-reactions are being investigated to be optimized in order to bring them into the level of real-time in-line sensors. In this project a competitive immunoassay between surface immobilized 2,6-dichlorobenzamide (BAM) haptens and BAM present in the water sample using an anti-BAM monoclonal antibody is being described. 2,6-Dichlorobenzamide (BAM) is a degradation product of the herbicide, dichlobenil which has been used extensively in the past and it is among the most frequently found pesticide residues in European ground water. BAM is highly resistant to further degradation and is fairly soluble in water. We have synthesized and immobilized a small library of BAM haptens and compared the affinity constants of the antibody towards this library. Furthermore, since regeneration of the BAM-hapten surface is a prerequisite for the development of a real-time electrochemical sensor with immunoassay-based detection, studies on regeneration of surfaces, modified with the newly synthesized BAM-haptens has been preformed and compared and correlated to the measured affinity constants. By using conventional ELISA we were able to indicate that one of the immobilized BAM haptens with an intermediate affinity towards the anti-BAM antibody was better in terms of regeneration. Design and fabrication of a fully automated microfluidic based on this immunoassay and electrochemical detection are in progress.

Uthuppu, Basil; Kostesha, Natalie

2011-01-01

340

Distribution of pesticide residues in rice grain and in its coproducts  

Scientific Electronic Library Online (English)

Full Text Available SciELO Brazil | Language: English Abstract in portuguese Os agrotóxicos são usados em muitas culturas para prevenir e preservar os grãos de possíveis ataques de pragas. O objetivo deste trabalho foi avaliar a distribuição dos agrotóxicos bispiribaque de sódio, carbofurano, clomazona e tebuconazol nas diferentes frações do arroz beneficiado (arroz branco, [...] farelo de arroz, arroz com casca, arroz parboilizado beneficiado, farelo de arroz parboilizado e arroz parboilizado com casca), o qual foi cultivado em campos experimentais sob condições controladas de aplicação. Para tanto, o método QuEChERS foi otimizado para a extração dos agrotóxicos e validou-se um método utilizando CLAE-DAD para quantificação e CL-EM para confirmação. O método QuEChERS modificado foi adequado na extração dos agrotóxicos, bem como as condições cromatográficas para identificação e quantificação, conforme os indicativos de eficiência determinados: LOD de 0,07 mg kg-1 e LOQ de 0,2 mg kg-1 para a mistura dos agrotóxicos, e recuperação para arroz e farelo de arroz de 119 e 116%, 84 e 119%, 113 e 96%, 103 e 97% para carbofurano, bispiribaque de sódio, clomazona e tebuconazol, respectivamente. O método desenvolvido foi aplicado nas frações do beneficiamento e o farelo apresentou maior concentração de resíduo dos agrotóxicos, quando comparado ao arroz beneficiado, sendo 8,0, 2,3, 2,2 e 1,6 vezes mais contaminado, em média, para tebuconazol, clomazona, carbofurano e bispiribaque de sódio, respectivamente. Apenas o clomazona e o tebuconazol apresentaram concentrações dentro do limite aceitável estabelecidos pelo Codex Alimentarius (0,1 mg kg-1) para o arroz beneficiado nas safras analisadas. Abstract in english Pesticides are used to prevent pests from attacking grains in order to preserve the crops. This paper aims at evaluating the distribution of the pesticides bispyribac-sodium, carbofuran, clomazone and tebuconazole in different fractions of milled rice (white rice, rice bran, husked rice, parboiled r [...] ice, parboiled rice bran, and husked parboiled rice) which is planted on experimental fields under controlled conditions. The QuEChERS method was adapted to the extraction of pesticides and validated by using HPLC-DAD for quantification and LC-MS for confirmation. The analytical method of extracting pesticides, as well as the chromatographic conditions for identification and quantification, were suitable, according to certain efficiency indicators: 0.07 mg kg-1 LOD and 0.2 mg kg-1 LOQ for the mixture of pesticides and rice and rice bran recoveries of 119 and 116%, 84 and 119%, 113 and 96%, 103 and 97% for carbofuran, bispyribac-sodium, clomazone and tebuconazole, respectively. The method under development was applied to rice fractions: bran had the highest residue concentration of the studied pesticides, when compared to milled rice, showing 8.0, 2.3, 2.2 and 1.6 times more contamination, in average, with tebuconazole, clomazone, carbofuran and bispyribac-sodium, respectively. Only clomazone and tebuconazole were in the acceptable limits established by Codex Alimentarius (0.1 mg kg-1) for milled rice.

Giniani C., Dors; Ednei G., Primel; Carlos A. A., Fagundes; Carlos H. P., Mariot; Eliana, Badiale-Furlong.

1921-19-01

 
 
 
 
341

Distribution of pesticide residues in rice grain and in its coproducts  

Scientific Electronic Library Online (English)

Full Text Available SciELO Brazil | Language: English Abstract in portuguese Os agrotóxicos são usados em muitas culturas para prevenir e preservar os grãos de possíveis ataques de pragas. O objetivo deste trabalho foi avaliar a distribuição dos agrotóxicos bispiribaque de sódio, carbofurano, clomazona e tebuconazol nas diferentes frações do arroz beneficiado (arroz branco, [...] farelo de arroz, arroz com casca, arroz parboilizado beneficiado, farelo de arroz parboilizado e arroz parboilizado com casca), o qual foi cultivado em campos experimentais sob condições controladas de aplicação. Para tanto, o método QuEChERS foi otimizado para a extração dos agrotóxicos e validou-se um método utilizando CLAE-DAD para quantificação e CL-EM para confirmação. O método QuEChERS modificado foi adequado na extração dos agrotóxicos, bem como as condições cromatográficas para identificação e quantificação, conforme os indicativos de eficiência determinados: LOD de 0,07 mg kg-1 e LOQ de 0,2 mg kg-1 para a mistura dos agrotóxicos, e recuperação para arroz e farelo de arroz de 119 e 116%, 84 e 119%, 113 e 96%, 103 e 97% para carbofurano, bispiribaque de sódio, clomazona e tebuconazol, respectivamente. O método desenvolvido foi aplicado nas frações do beneficiamento e o farelo apresentou maior concentração de resíduo dos agrotóxicos, quando comparado ao arroz beneficiado, sendo 8,0, 2,3, 2,2 e 1,6 vezes mais contaminado, em média, para tebuconazol, clomazona, carbofurano e bispiribaque de sódio, respectivamente. Apenas o clomazona e o tebuconazol apresentaram concentrações dentro do limite aceitável estabelecidos pelo Codex Alimentarius (0,1 mg kg-1) para o arroz beneficiado nas safras analisadas. Abstract in english Pesticides are used to prevent pests from attacking grains in order to preserve the crops. This paper aims at evaluating the distribution of the pesticides bispyribac-sodium, carbofuran, clomazone and tebuconazole in different fractions of milled rice (white rice, rice bran, husked rice, parboiled r [...] ice, parboiled rice bran, and husked parboiled rice) which is planted on experimental fields under controlled conditions. The QuEChERS method was adapted to the extraction of pesticides and validated by using HPLC-DAD for quantification and LC-MS for confirmation. The analytical method of extracting pesticides, as well as the chromatographic conditions for identification and quantification, were suitable, according to certain efficiency indicators: 0.07 mg kg-1 LOD and 0.2 mg kg-1 LOQ for the mixture of pesticides and rice and rice bran recoveries of 119 and 116%, 84 and 119%, 113 and 96%, 103 and 97% for carbofuran, bispyribac-sodium, clomazone and tebuconazole, respectively. The method under development was applied to rice fractions: bran had the highest residue concentration of the studied pesticides, when compared to milled rice, showing 8.0, 2.3, 2.2 and 1.6 times more contamination, in average, with tebuconazole, clomazone, carbofuran and bispyribac-sodium, respectively. Only clomazone and tebuconazole were in the acceptable limits established by Codex Alimentarius (0.1 mg kg-1) for milled rice.

Giniani C., Dors; Ednei G., Primel; Carlos A. A., Fagundes; Carlos H. P., Mariot; Eliana, Badiale-Furlong.

342

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

Directory of Open Access Journals (Sweden)

Full Text Available Pesticides provide the primary means for controlling organisms that compete with man for food and fibre or cause injury to man, livestock and crops. They played a vital role in the economic production of wide ranges of vegetable, fruit, cereal, forage, fibre and oil crops which now constitute a large part of successful agricultural industry in many countries. After application to the target areas, pesticide residues are removed from applicators by rinsing with water which results in the formation of a toxic wastewater that represents a disposal problem for many farmers. Pesticides can adversely affect people, pets, livestock and wildlife in addition to the pests they are intended to destroy. The phenomenon of biomagnification of some pesticides has resulted in reproductive failure of some fish species and egg shell thinning of birds such as peregrine falcons, sparrow hawk and eagle owls. Pesticide toxicity to humans include skin and eye irritation and skin cancer. Therefore, care must be exercised in the application, disposal and treatment of pesticides. Currently, disposal of pesticide wastewater is carried out by: 1 land cultivation, 2 dumping in soil pits, plastic pits and concrete pits or on land and in extreme cases in streams near the rinsing operation, 3 use of evaporation beds and 4 land filling. These methods of disposal are unsafe as the surface run off will reach streams, rivers and lakes and the infiltration of the wastewater into the local soil will eventually reach ground water. The treatment methods currently used for pesticide wastewater include: 1 incineration (incinerators and open burning, 2 chemical treatments (O3/UV, hydrolysis, Fenton oxidation and KPEG, 3 physical treatments (inorganic, organic absorbents and activated carbon and 4 biological treatments (composting, bioaugmentation and phytoremediation. Therefore, the choice of safe, on farm disposal techniques for agricultural pesticides is very important. A comparative analysis was performed on 18 methods of pesticide disposal/treatment using six criteria: containment, detoxification ability, cost, time, suitability for on farm use, size and evaporation efficiency. The results indicated that of the 18 methods evaluated, 9 scored above 80/100 and can be used on farm. They were organic absorbents (97, composting (94, bioaugmentation (92, inorganic absorbents (90, Fenton oxidation (86, O3/UV (83, activated carbon (82, hydrolysis (82, and land cultivation (80. The other methods are not suitable for on farm use as they suffered from containment problems, high cost and variability of effectiveness.

Mariam T. Al Hattab

2012-05-01

343

Total diet study on pesticide residues in France: levels in food as consumed and chronic dietary risk to consumers.  

Science.gov (United States)

Chronic dietary exposure to pesticide residues was assessed for the French population using a total diet study (TDS) to take into account realistic levels in foods as consumed at home (table-ready). Three hundred and twenty-five pesticides and their transformation products, grouped into 283 pesticides according to their residue definition, were sought in 1235 composite samples corresponding to 194 individual food items that cover 90% of the adult and child diet. To make up the composite samples, about 19,000 food products were bought during different seasons from 2007 to 2009 in 36 French cities and prepared according to the food preparation practices recorded in the individual and national consumption survey (INCA2). The results showed that 37% of the samples contained one or more residues. Seventy-three pesticides were detected and 55 quantified at levels ranging from 0.003 to 8.7mg/kg. The most frequently detected pesticides, identified as monitoring priorities in 2006, were the post-harvest insecticides pirimiphos-methyl and chlorpyrifos-methyl-particularly in wheat-based products-together with chlorpyrifos, iprodione, carbendazim and imazalil, mainly in fruit and fruit juices. Dietary intakes were estimated for each subject of INCA2 survey, under two contamination scenarios to handle left-censored data: lower-bound scenario (LB) where undetected results were set to zero, and upper-bound (UB) scenario where undetected results were set to the detection limit. For 90% of the pesticides, exposure levels were below the acceptable daily intake (ADI) under the two scenarios. Under the LB scenario, which tends to underestimate exposure levels, only dimethoate intakes exceeded the ADI for high level consumers of cherry (0.6% of children and 0.4% of adults). This pesticide, authorised in Europe, and its metabolite were detected in both cherries and endives. Under the UB scenario, that overestimates exposure, a chronic risk could not be excluded for nine other pesticides (dithiocarbamates, ethoprophos, carbofuran, diazinon, methamidophos, disulfoton, dieldrin, endrin and heptachlor). For these pesticides, more sensitive analyses of the main food contributors are needed in order to refine exposure assessment. PMID:22595191

Nougadère, Alexandre; Sirot, Véronique; Kadar, Ali; Fastier, Antony; Truchot, Eric; Vergnet, Claude; Hommet, Frédéric; Baylé, Joëlle; Gros, Philippe; Leblanc, Jean-Charles

2012-09-15

344

Pesticide residues in fruits and vegetables from Pakistan: a review of the occurrence and associated human health risks.  

Science.gov (United States)

The main objective of the review is to document, assess and analyze the results of the previously reported data on levels of different pesticides in selected fruits and vegetables from Pakistan. The findings of the previous studies clearly indicated that more than 50 % of the samples were contaminated with organophosphate, pyrethroids and organochlorine pesticides. Many studies reported that among fresh fruits and vegetables tomato, apple, melon, mango, grapes, and plum crossed the FAO/WHO permissible limits for these contaminants residual levels. The comparison of other regions showed that observed levels were found above maximum residue limits (MRLs) in 50 % of the samples but were in agreement with the studies from neighboring countries like China and Bangladesh. Higher hazard risk index (HRI) values were calculated for dieldrin, methamidophos, o,p'-DDT, diazinon and p,p'-DDT in apple, mango, banana, melon, potato and onion. The review also highlights that data on pesticide residues in foodstuff is scarce which should be overcome by further extending studies from different areas of Pakistan. In order to ascertain the provision of food suitable for human consumption, it is imperative to monitor pesticides in food commodities by the country's authorities and enforce guidelines based on permissible limits. PMID:24958529

Syed, Jabir Hussain; Alamdar, Ambreen; Mohammad, Ashiq; Ahad, Karam; Shabir, Zunera; Ahmed, Haroon; Ali, Syeda Maria; Sani, Syed Gul Abbas Shah; Bokhari, Habib; Gallagher, Kevin D; Ahmad, Iftikhar; Eqani, Syed Ali Musstjab Akber Shah

2014-12-01

345

Analytical method for simultaneous determination of pesticide and veterinary drug residues in milk by CE-MS.  

Science.gov (United States)

This study reports a method based on CE-MS/MS detection developed for the multiresidue determination of seven pesticides (amidosulfuron, cyprodinil, cyromazine, imazaquin, pirimicarb, demethyl pirimicarb, procymidone) and eight residues of veterinary drugs (ciprofloxacin, enrofloxacin, sulfacetamide, sulfabenzamide, sulfachlorpyridazine, sulfaquinoxaline, sulfathiazole, sulfisoxazole), whose contents are regulated by the EU Council Regulations no. 396/2005 and no. 2377/90, in animal edible tissues. Milk samples were extracted with ACN and the extract was cleaned up using an Oasis hydrophilic-lipophilic balance SPE cartridge. The proposed method was validated in accordance with the European Commission Decision 657/2002. MS/MS experiments, using an IT analyzer, operating in multiple reaction monitoring mode, were carried out to achieve the minimum number of required identification points. Recovery data were also satisfactory, with values higher than 78% for most pesticides and veterinary drugs extracted from milk spiked at half the maximum residue limit established for the studied compounds. The RSD% (n = 5) were lower than 13 and 15% for intra-day and inter-day assays, respectively. The method was applied to establish the occurrence of the studied pesticides in 100 milk samples, attaining the determination of pesticide and veterinary drug residues in milk in the low microg/kg range. PMID:19384986

Blasco, Cristina; Picó, Yolanda; Andreu, Vicente

2009-05-01

346

Resíduos de agrotóxicos em frutos de tomate / Pesticide residues in tomato fruits  

Scientific Electronic Library Online (English)

Full Text Available SciELO Brazil | Language: Portuguese Abstract in portuguese O uso intensivo de agrotóxicos em culturas de tomates tem causado preocupações quanto à provável contaminação do produto final. Este trabalho teve como objetivo monitorar, por dois anos consecutivos, em quatro propriedades de uma área altamente tecnificada, o uso de agrotóxicos em tomate irrigado du [...] rante seu desenvolvimento, quantificar os resíduos dos principais princípios ativos utilizados, e avaliar o grau de contaminação dos frutos colhidos. Foram analisados metamidofós, clorpirifós, captan, clorotalonil, endosulfan, lambda-cialotrina, e cobre. Para avaliar o grau de contaminação dos frutos foi validado um método de análise de resíduos múltiplos capaz de quantificar esses compostos. Os resíduos encontrados foram de fungicidas e inseticidas aplicados nas fases de frutificação e maturação: captan, 0,35 mg/kg, na Fazenda 2; clorotalonil, 0,16 mg/kg e 0,95 mg/kg, nas Fazendas 1 e 2, respectivamente; lambda-cialotrina, 0,03 mg/kg, na Fazenda 2; cobre, 2,03 mg/kg, 3,75 mg/kg e 1,44mg/kg, nas Fazendas 1, 2 e 3, respectivamente, e 0,95 mg/kg, 1,70 mg/kg e 2,31 mg/kg, na Fazenda 4. Não ocorreram resíduos dos inseticidas organofosforados, aplicados principalmente durante o desenvolvimento vegetativo da cultura. Não houve contaminação dos tomates pelos agrotóxicos analisados. Os resíduos que devem ser monitorados são os dos agrotóxicos aplicados na fase de maturação da cultura. Abstract in english The intensive use of pesticide in tomato crops have been causing concern about a possible contamination of the final product. This work aimed at monitoring, for two years, in four farms located in a high technology area, the use of pesticides in irrigated tomato crops, quantifying the main active in [...] gredient residues and evaluating the contamination level of the fruits. The components analised were: methamidophos, chlorpyrifos, captan, chlorothalonil, endosulfan, lambda-cyhalothrin and copper oxychloride. In order to evaluate the contamination level, a multiresidue method was validated. The residues found were from fungicides and insecticides used during the frutification and maturation stages of the crop: captan, 0.35 mg/kg, at Farm 2; chlorothalonil, 0.16 mg/kg and 0.95 mg/kg, at Farms 1 and 2, respectively; lambda-cyhalothrin, 0.03 mg/kg, at Farm 2; copper, 2.03 mg/kg, 3.75 mg/kg and 1.44 mg/kg, at Farms 1, 2 and 3, respectively, and 0.95 mg/kg, 1.70 mg/kg and 2.31 mg/kg, at Farm 4. Residues of organophosphorous components applied mainly during the vegetative growing were not found. There was no contamination in the tomatos. The residues to be monitored are those from the pesticides used in the crop maturation stage.

Leslie Maria Segura, Zavatti; Rosângela Blotta, Abakerli.

347

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

Directory of Open Access Journals (Sweden)

Full Text Available O uso intensivo de agrotóxicos em culturas de tomates tem causado preocupações quanto à provável contaminação do produto final. Este trabalho teve como objetivo monitorar, por dois anos consecutivos, em quatro propriedades de uma área altamente tecnificada, o uso de agrotóxicos em tomate irrigado durante seu desenvolvimento, quantificar os resíduos dos principais princípios ativos utilizados, e avaliar o grau de contaminação dos frutos colhidos. Foram analisados metamidofós, clorpirifós, captan, clorotalonil, endosulfan, lambda-cialotrina, e cobre. Para avaliar o grau de contaminação dos frutos foi validado um método de análise de resíduos múltiplos capaz de quantificar esses compostos. Os resíduos encontrados foram de fungicidas e inseticidas aplicados nas fases de frutificação e maturação: captan, 0,35 mg/kg, na Fazenda 2; clorotalonil, 0,16 mg/kg e 0,95 mg/kg, nas Fazendas 1 e 2, respectivamente; lambda-cialotrina, 0,03 mg/kg, na Fazenda 2; cobre, 2,03 mg/kg, 3,75 mg/kg e 1,44mg/kg, nas Fazendas 1, 2 e 3, respectivamente, e 0,95 mg/kg, 1,70 mg/kg e 2,31 mg/kg, na Fazenda 4. Não ocorreram resíduos dos inseticidas organofosforados, aplicados principalmente durante o desenvolvimento vegetativo da cultura. Não houve contaminação dos tomates pelos agrotóxicos analisados. Os resíduos que devem ser monitorados são os dos agrotóxicos aplicados na fase de maturação da cultura.The intensive use of pesticide in tomato crops have been causing concern about a possible contamination of the final product. This work aimed at monitoring, for two years, in four farms located in a high technology area, the use of pesticides in irrigated tomato crops, quantifying the main active ingredient residues and evaluating the contamination level of the fruits. The components analised were: methamidophos, chlorpyrifos, captan, chlorothalonil, endosulfan, lambda-cyhalothrin and copper oxychloride. In order to evaluate the contamination level, a multiresidue method was validated. The residues found were from fungicides and insecticides used during the frutification and maturation stages of the crop: captan, 0.35 mg/kg, at Farm 2; chlorothalonil, 0.16 mg/kg and 0.95 mg/kg, at Farms 1 and 2, respectively; lambda-cyhalothrin, 0.03 mg/kg, at Farm 2; copper, 2.03 mg/kg, 3.75 mg/kg and 1.44 mg/kg, at Farms 1, 2 and 3, respectively, and 0.95 mg/kg, 1.70 mg/kg and 2.31 mg/kg, at Farm 4. Residues of organophosphorous components applied mainly during the vegetative growing were not found. There was no contamination in the tomatos. The residues to be monitored are those from the pesticides used in the crop maturation stage.

Leslie Maria Segura Zavatti

1999-03-01

348

Residues of endosulfan and other selected organochlorine pesticides in farm areas of the Lower Fraser Valley, British Columbia, Canada.  

Science.gov (United States)

Crop soils, ditch sediments, and water flowing from several farm areas to salmon tributary streams of the Fraser River in the Lower Fraser Valley (LFV) of British Columbia, Canada, were sampled in 2002-2003 to quantify for residues of an organochlorine cyclodiene pesticide, endosulfan (END = alpha-endosulfan + beta-endosulfan + endosulfan sulfate). Residues from historical use of other selected organochlorine pesticides, namely, cyclodienes (aldrin, alpha-chlordane, gamma-chlordane, dieldrin, endrin, endrin aldehyde, heptachlor, and heptachlor epoxide), hexachlorocyclohexanes [alpha-benzene-hexachloride (alpha-BHC), beta-BHC, delta-BHC, and gamma-BHC (lindane)], and DDT-related compounds (p,p-DDT, p,p-DDD, p,p-DDE, and methoxychlor) were also determined. Reference and background levels of these pesticides in ditches leading to fish streams were obtained from pristine watershed areas. Varying amounts of END residues were detected in soils (<0.02-5.60 mg kg(-1) dry wt.) and ditch sediments (<0.02-3.33 mg kg(-1) dry wt.) in mainly three of five farm areas sampled. Likewise, residues (excluding END) of other selected organochlorine compounds such as aldrin, BHC, chlordane, endrin, p,p-DDT, methoxychlor, and their respective major transformation products (endosulfan sulfate, dieldrin, endrin aldehyde, heptachlor, heptachlor epoxide, p,p-DDD, and p,p-DDE) were found in crop soils (<0.02-16.2 mg kg(-1) dry wt.) and sediments (<0.02-9.73 mg kg(-1) dry wt.). Most of these pesticides (END: <0.01-1.86 microg L(-1); other selected organochlorine pesticides: <0.0.1-1.50 microg L(-1)) were also found in ditch water leading to salmon streams in several farms. The END levels of crop soils from the same LFV study farms in 1994 and 2003 indicated an estimated decline of 22% to 1.35 mg kg(-1) dry wt. during that period. This reduction was probably due to the increasing use of alternate pesticides (e.g., organophosphorus compounds). Some possible biological implications of these pesticide residues on nontarget organisms in the LFV are discussed. PMID:15942037

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

2005-01-01

349

Statistical assessment of organochlorine pesticides residues in surface water penetrated into caspian sea  

International Nuclear Information System (INIS)

Multivariate statistical techniques, such as factor analysis (FA) and discriminant analysis (DA) were used for evaluation of temporal/spatial variations and interpretation of organochlorine pesticides (OCPs) data from Shiroud River (Iran). Eight sites were selected along the river and fifteen OCPs components were measured. FA was applied to determine the interrelationship between various variables and also to identify any possible pollution sources. FA has identified six factors were responsible for explaining 73.39 % of the total variance in OCPs data. DA has identified tour discriminant functions (DFs) responsible for spatial variations and two DFs were responsible for temporal variations. It has provided important information about allocation of all observations, since more than 80 % correct assignations in spatial analysis and 76 % correct assignations in temporal analysis DA indicates that some parameters contribute highly in discriminating the eight sites and also in discriminating the four seasons for both spatial/temporal and OCPs variations. (author)

350

Study On The Procedures For Determining Of Pesticide Residues In Green Vegetables  

International Nuclear Information System (INIS)

Researches presented in this work are divided into two main parts. One part embraces the residue analytical methods. The other part comprises applying of these residue analytical methods for analysis of plant material. Part I: Residue analytical methods (Analytical procedures): Determination of Endosulphan in plant material by GC/ECD; Determination of Methamidofos in plant material by GC/FTD; Determination of Deltamethrin, Cyhalothrin, Cyfluthrin in plant material by GC/ECD; Determination of Maneb in plant material by HPLC/UV; Determination of Zineb in plant material by F-AAS; Determination of Organo-Asenic and Mercury in plant material by RNAA; The limits of detection and determination (LOD, LOQ), Recovery, Efficiency, the Calibration curve are validated. Part II: Applying of Residue Analytical Methods for analysis of endosulphan, methamidofos, maneb, zineb, cyhalothrin, deltamethrin, cyfluthrin, metallo-organic compounds in Spinach, Cabbage, Pimento, Japanese Bean, Japanese Pumpkin, Tomato, Potato, Sweet Potato. The results and conclusion are present in this work. (author)

351

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

Science.gov (United States)

Flow injection combined with tandem mass spectrometry (MS/MS) was investigated for the rapid detection of highly polar pesticides that are not amenable to multi-residue methods because they do not partition into organic solvents and require dedicated chromatographic conditions. The pesticides included in this study were amitrole, chlormequat, cyromazine, daminozide, diquat, ethephon, fosetyl-Al, glufosinate, glyphosate and its metabolite aminomethylphosphonic acid, maleic hydrazide, mepiquat and paraquat. The composition of the flow-injection solvent was optimized to achieve maximum MS/MS sensitivity. Instrumental limits of detection varied between substantially reduces the liquid chromatography-MS/MS capacity demand which for many laboratories is prohibitive for inclusion of these pesticides in their monitoring and surveillance programmes. PMID:24518902

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

2014-11-01

352

Response surface optimization for determination of pesticide residues in grapes using MSPD and GC-MS: assessment of global uncertainty.  

Science.gov (United States)

In this work, a simple and low-cost method based on matrix solid-phase dispersion (MSPD) and gas chromatography to determine eight multi-class pesticides such as vinclozolin, dichlofluanid, penconazol, captan, quinoxyfen, fluquinconazol, boscalid, and pyraclostrobin in grapes is described. Fungicide residues were identified and quantified using gas chromatography-mass spectrometry in selected ion monitoring mode (GC-MS, SIM). The experimental variables that affect the MSPD method, such as the amount of solid phase, solvent nature and elution volume were optimized using an experimental design. The best results were obtained using 0.5 g of grapes, 1.0 g of silica as clean-up sorbent, 1.50 g of C(18) as bonded phase and 10 mL of dichloromethane/ethyl acetate (1:1, v/v) as eluting solvent. Significant matrix effects observed for most of the pesticides tested were eliminated using matrix-matched standards. The pesticide recoveries in grapes samples were better than 80% except for captan. Intra-laboratory precision in terms of Horwitz ratio of the pesticides evaluated was below 0.5, suggesting ruggedness of the method. The quantification limits of the pesticides were in the range of 3.4-8.7 microg kg(-1), which were lower than the maximum residue limits (MRLs) of the pesticides in grapes samples established by the European legislation. Decision limits (CCalpha) and detection capability (CCbeta) have been calculated. The expanded uncertainties at two levels of concentration were <20% for all analytes. PMID:20694812

Lagunas-Allué, L; Sanz-Asensio, J; Martínez-Soria, M T

2010-10-01

353

Validation of a multi-residue method for the determination of residuals pesticides in cabbage (Brassica Oleracea var. Capitata) for gases chromatography  

International Nuclear Information System (INIS)

This study describes the validation of a multi-residue method for the determination of most used organo chlorine, organophosphorus and organonitrogen pesticides in cabbage in the Cundinamarca Department (Colombia). The extraction process includes blending of small sample quantity with ethyl acetate in presence of Na2SO4 and NaHCO3, filtration and concentration. The clean up steps include GPC and mini-column chromatography using silica gel. Final determination was carried out by gas chromatography with: pulsed splitless injection, HP-5 capillary column, and a parallel detection system with micro electron capture detection (? - ECD) and Nitrogen-Phosphorus Detection (NPD). The methodology is specific, selective, accurate and robust. Recovery values of majority of pesticides were in the range 70-120% at spiking levels ranging 0.05-10.73 mg/kg. Limits of detection were less than 0.10 mg/kg for most of the studied compounds. The distribution of the analyses in the laboratory sample was evaluated and it was found its homogeneity. The evaluation of pesticide residues was made in a specific area of municipality of Madrid-Cundinamarca, (Colombia). No residues of the studied analyses were founded

354

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

Science.gov (United States)

...combined residues of the herbicide saflufenacil (2-chloro-5-[3,6-dihydro-3-methyl-2...as the stoichiometric equivalent of saflufenacil, in or on oilseeds, cottonseed subgroup...combined residues of the herbicide saflufenacil...

2010-09-23

355

Quantitative analysis of three chiral pesticide enantiomers by high-performance column liquid chromatography.  

Science.gov (United States)

Methods for the enantiomeric quantitative determination of 3 chiral pesticides, paclobutrazol, myclobutanil, and uniconazole, and their residues in soil and water are reported. An effective chiral high-performance liquid chromatographic (HPLC)-UV method using an amylose-tris(3,5-dimethylphenylcarbamate; AD) column was developed for resolving the enantiomers and quantitative determination. The enantiomers were identified by a circular dichroism detector. Validation involved complete resolution of each of the 2 enantiomers, plus determination of linearity, precision, and limit of detection (LOD). The pesticide enantiomers were isolated by solvent extraction from soil and C18 solid-phase extraction from water. The 2 enantiomers of the 3 pesticides could be completely separated on the AD column using n-hexane isopropanol mobile phase. The linearity and precision results indicated that the method was reliable for the quantitative analysis of the enantiomers. LODs were 0.025, 0.05, and 0.05 mg/kg for each enantiomer of paclobutrazol, myclobutanil, and uniconazole, respectively. Recovery and precision data showed that the pretreatment procedures were satisfactory for enantiomer extraction and cleanup. This method can be used for optical purity determination of technical material and analysis of environmental residues. PMID:18980112

Wang, Peng; Liu, Donghui; Gu, Xu; Jiang, Shuren; Zhou, Zhiqiang

2008-01-01

356

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

Directory of Open Access Journals (Sweden)

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.

Samson Ayo Deji

2012-10-01

357

Vegephy: impact of vegetable oils used as extemporaneous additives on pesticide residues and their crop protection potential.  

Science.gov (United States)

Within the framework of the VEGEPHY project set up to assess the effect of refined oils used as extemporaneous additives, both alone and in combination with oligosaccharides (guar, xanthan and carboxymethyl cellulose), on the quality of plant protection treatments for wheat, a study was conducted on the effect of combinations of additives on the level of pesticide residues in wheat plants and grain and their impact on treatment efficiency. The use of some of these additives gave efficiency results that were comparable with those obtained with additives that are currently used but are not bio-based. The use of refined oils as extemporaneous additives, both alone and combined with oligosaccharides, led to better penetration by the pesticide as well as longer persistence of its activity. The experiments were conducted with fungicides, herbicides, plant growth regulators and various types of formulation (EC, SC and WG). The results obtained were conclusive, but they did depend on the physico-chemical properties of the active substance. The risk of exceeding the maximum residue levels (MRLs) of pesticides was also evaluated. Even where the MRLs had not been not exceeded, the experiments showed that in some cases the treatment with these additives could lead to pesticide residues up to two times higher than those measured for the treatment without additives. It would be necessary, therefore, to reduce the treatment dose associated with the additive and/or have a long enough pre-harvest interval to avoid exceeding the MRLs. The use of green additives could be a useful and easy way to attain the European Union (EU) goal of reducing pesticide use by improving the retention of active substances on the plant and reducing the number of treatments. PMID:25145232

Rousseau, G; Coutanceau, P; Lebeau, F; Pigeon, O; Ducat, N; De Vos, P

2013-01-01

358

[Application of a rapid and simple multi-residue method for determination of pesticide residues in drinking water and beverages using liquid chromatography-tandem mass spectrometry].  

Science.gov (United States)

A rapid and simple multi-residue method for determination of pesticides has been applied to drinking water and beverages. To a disposable polypropylene tube containing 10.0 g sample, 20 mL acetonitrile was added and the mixture was shaken vigorously for 1 min to extract pesticides. Then, 1 g sodium chloride and 4 g magnesium sulfate anhydrous were added, followed by vigorous shaking for 1 min and centrifugation to obtain the organic phase. The organic phase was processed with a graphite carbon black/PSA solid phase column. After concentration and reconstitution with 25% methanol containing aqueous solution, the test solution was analyzed with LC-MS/MS. Recovery tests of 91 pesticides fortified (0.02 ?g/g) in 35 kinds of drinking water and beverages were conducted. The decline of recoveries in alcoholic beverages is considered to be due to the increase of organic phase volume owing to ethanol included in the alcoholic beverages. A simulation study was carried out with simulated alcoholic beverages, which consisted of 50% grape juice, with various amounts of ethanol and water, to examine pesticides recoveries and volume of the organic phase. The results suggested this method would be applicable both to alcoholic beverages containing less than 10% ethanol and to alcoholic beverages containing over 10% ethanol after dilution with water to below 10% ethanol prior to the addition of acetonitrile. A sample could be processed and analyzed by LC-MS/MS within 2 h. Thus, this method should be useful for monitoring and screening pesticide residues in drinking water and various beverages. PMID:23132358

Fukui, Naoki; Takatori, Satoshi; Kitagawa, Yoko; Okihashi, Masahiro; Osakada, Masakazu; Nakatsuji, Naoto; Nakayama, Yukiko; Kakimoto, You; Obana, Hirotaka

2012-01-01

359

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

Science.gov (United States)

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

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

2014-12-01

360

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

Science.gov (United States)

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

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

2014-05-01

 
 
 
 
361

Monitoring of Certain Pesticide Residues and Some Heavy Metals in Fresh Cow`s Milk at Gharbia Governorate, Egypt  

Digital Repository Infrastructure Vision for European Research (DRIVER)

This monitoring study of 40 samples of cow`s milk collected from different locations at Gharbia Governorate during the four different seasons of the years 2005-2006, was conducted to determine the contamination levels of seven pesticide residues including four organophosphorus (chlorpyrifos, diazinon, dimethoate and malathion) and three synthetic pyrethroides (cypermethrin, deltamethrin and fenvelerate), as well as five heavy metals (copper, iron, cadmium, zinc and lead). The results showed t...

Nasr, I. N.; Sallam, A. A. A.; Abd El-khair, A. A.

2007-01-01

362

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

Science.gov (United States)

This study investigated organophosphorus (OP) residues in vegetables from 27 farms, 106 markets, and 1 supermarket around Kwan Phayao Lake, Northern Thailand, between August and September 2013. Types of vegetables sampled were all vegetables cultivated or sold around the study site. The most common OP pesticides detected in farm samples were chlorpyrifos (50 %), malathion (31.8 %), monocrotophos (31.8 %), diazinon (13.6 %), omethoate (13.6 %), and dicrotophos (9.1 %). The most common OP pesticides detected in market samples were chlorpyrifos (33.9 %), diazinon (18.6 %), parathion-methyl (3.4 %), profenofos (3.4 %), primiphos-ethyl (3.4 %), and fenitrothion (1.7 %). The OP pesticides detected in supermarket samples were chlorpyrifos (33.3 %), and diazinon (66.7 %). Among the compounds detected, chlorpyrifos was detected in most of the vegetable samples from all sources. The highest chlorpyrifos level in farm samples were found in lemon balm (2.423 mg/kg) followed by Vietnamese coriander (0.835 mg/kg), and cowpea (0.027 mg/kg). The highest level in markets samples were found in garlic (7.785 mg/kg) followed by Chinese cabbage (2.864 mg/kg) and Vietnamese coriander (1.308 mg/kg). Residues from supermarket samples were found only in parsley (0.027 mg/kg). The findings showed that 16 samples (59.3 %) from farms and 14 samples (13.2 %) from markets contained OP residues at or above the maximum residue limits established by the European Union. It is concluded that awareness, safety education, and strict regulation of pesticide use are necessary. PMID:24609615

Sapbamrer, Ratana; Hongsibsong, Surat

2014-07-01

363

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

Science.gov (United States)

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

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

2014-07-01

364

Estimation of sampling uncertainty for pesticide residues in root vegetable crops.  

Science.gov (United States)

The sampling uncertainty for pesticide residues in carrots, parsley leaves and selected medium size crops was estimated with simple random sampling by applying range statistics. The primary samples taken from treated fields consisted of individual carrots or a handful of parsley leaves. The samples were analysed with QUEChERs extraction method and LCMS/MS detection with practical LOQ of 0.001 mg/kg. The results indicate that the average sampling uncertainties estimated with simple random sampling and range statistics were practically the same. The confidence interval for the estimated sampling uncertainty decreased with the number of replicate samples taken from one lot and the number of lots sampled. The estimated relative ranges of sampling uncertainty are independent from the relative standard deviation of the primary samples. Consequently the conclusions drawn from these experiments are generally applicable. There is no optimum for sample size and number of lots to be tested for estimation of sampling uncertainty. Taking a minimum of 6 replicate samples from at least 8-12 lots is recommended to obtain a relative 95% range of sampling uncertainty within 50%. The cost of sampling/analyses, the consequences of wrong decision should also be taken into account when a sampling plan is prepared. PMID:24138463

Farkas, Zsuzsa; Horváth, Zsuzsanna; Kerekes, Kata; Ambrus, Árpád; Hámos, András; Szabó, Mária Szeitzné

2014-01-01

365

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

Science.gov (United States)

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

Malhat, Farag; Nasr, Islam

2011-12-01

366

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

Science.gov (United States)

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