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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

2001-08-13

2

Recent Applications of Mass Spectrometry and Combined Gas Chromatography-Mass Spectrometry to Pesticide Residue Analysis.  

Science.gov (United States)

Contents: The mass spectral fragmentation behavior of pesticides; Mass spectrometric technique: Isolation of individual residues; Applications of mass spectrometry to pesticide residue analysis; Combined gas chromatography-mass spectrometry; Applications ...

F. J. Biros

1970-01-01

3

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

2014-02-15

4

Fast gas chromatography for pesticide residues analysis using analyte protectants.  

Science.gov (United States)

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

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

2008-04-01

5

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

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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

Matrix-induced response enhancement in pesticide residue analysis by gas chromatography.  

Science.gov (United States)

The sample matrix can cause an enhancement in the observed chromatographic response for pesticide residues in a matrix extract compared with the same concentration in a matrix-free solution. The matrix increases the transfer of pesticides from hot vaporizing injectors by reducing the thermal stress for labile compounds and by masking active sites in the injector responsible for the adsorption or decomposition of polar pesticides. The use of different injector types and matrix simplification procedures can reduce matrix-induced enhancement but do not eliminate it. The most effective strategy is to use matrix-matched calibration standards or analyte protectants which equalize the response enhancement for calibration standards and sample extracts. From a practical point of view it is important that the method used to correct for matrix-induced enhancement is compatible with low system maintenance. The different approaches for correcting matrix-induced enhancement for calibration in pesticide residue analysis are discussed and compared in this review. PMID:17241638

Poole, Colin F

2007-07-27

7

Pesticide residue analysis of vegetables by gas chromatography with electron-capture detection.  

Science.gov (United States)

A new and original analytical method was developed for the routine analysis of 28 multiclass pesticide residues in vegetables (green pepper, red pepper, and tomato). The extraction was performed with acetone, and the pesticides were partitioned into ethyl acetate-cyclohexane (1 + 1, v/v). Residue levels in vegetables were determined by gas chromatography (GC) with electron-capture detection. Residue identities were confirmed by GC coupled with mass spectrometry in the selected ion monitoring mode. The average recoveries in pepper and tomato obtained for all analytes studied were 67.3 and 123.1%, respectively, with relative standard deviation between 1.8 and 7.0%. The detection limit for the pesticides studied varied from 0.1 to 2.6 microg/kg. The proposed method was applied to the analysis of these compounds in vegetables grown in experimental greenhouses. PMID:17373459

Fenoll, José; Hellín, Pilar; Martínez, Carmen M; Flores, Pilar

2007-01-01

8

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

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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

9

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

Science.gov (United States)

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

Amendola, Graziella; Pelosi, Patrizia; Dommarco, Roberto

2011-01-01

10

Development and applications of single-drop microextraction for pesticide residue analysis: A review.  

Science.gov (United States)

Single-drop microextraction (SDME) has become more popular than other microextraction techniques because it is simple, cost-effective, easy to operate and nearly solvent-free. The technique has been employed successfully for trace analysis in environmental, biomedical and food applications. In view of the increasingly stringent regulatory limits for many pesticides, which are below the LOD of the existing instruments, SDME may provide a cost-effective solution for reducing the LOD of pesticides. The present review focuses on recent development in SDME technique, and its application coupled with various analytical techniques, such as GC-MS, GC and HPLC for pesticide residue analysis in different matrices. The advantages, limitations and outlook on the future of SDME technique for its wider applications are also discussed. PMID:21077126

Pakade, Yogesh B; Tewary, Dhananjay Kumar

2010-12-01

11

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

International Nuclear Information System (INIS)

Different solid phase extraction devices were tested for the analysis of residues of eleven pesticides used in banana production in Costa Rica. The analysis was performed by using gas chromatograph equipped with NPD and ECD detectors. In general low recoveries and high variation coefficients were found for chlorothalonil, imazalil, terbufos and thiabendazole. For the other pesticides recoveries ranged between 60 and over 100%. (author)

1999-09-01

12

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

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

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Full Text Available Headspace solid phase microextraction method (HS/SPME, optimised previously for pesticide water solutions, was applied to trace residues of the pesticides chlorpyrifos, fenthion and bifenthrin in apple samples. One-hour extraction procedure was performed at 60oC extraction temperature. Nonpolar polydimethyl siloxane (PDMS fiber was used. Detection and quantification were carried out by gas chromatography/mass spectrometry (GC/MS. A non-pesticide treated apple sample was fortified with the pesticides over a 0.025-1.25 mg/kg concentration range in order to determine analytical parameters of the method applied. Linearity with regression coefficient (R values higher than 0.99 were obtained over the whole concentration range investigated for chlorpyrifos and fenthion, while linear dependence was observed in the 0.1-1.25 mg/kg range for bifenthrin. Relative recovery values for samples fortified at different levels were in the 56.68-82.91% range. Limit of detection (LOD values were determined as follows: 0.014 mg/kg for chlorpyrifos, 0.021 mg/kg for fenthion and 0.053 mg/kg for bifenthrin. Relative standard deviation (RSD values obtained for multiple analysis of the sample fortified at 0.6 mg/kg level were not higher than 20%.

Jelena Milinovi?

2007-01-01

14

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)

2008-12-13

15

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

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High-performance thin-layer chromatographic analysis of selected organophosphorous pesticide residues in tea.  

Science.gov (United States)

The separation of 9 organophosphates (monocrotophos, quinalphos, triazophos, parathion-methyl, isofenphos-methyl, temephos, parathion, phoxim-ethyl, and chlorpyrifos) by high-performance thin-layer chromatography (HPTLC) with automated multiple development was studied. The HPTLC method was developed and validated for analysis of residues of phoxim-ethyl and chlorpyrifos in tea. The sample was extracted with acetonitrile and cleaned up by ENVI-CARB solid-phase extraction. The extract was directly applied as bands to glass-backed silica gel 60F254 HPTLC plates. The plates were developed with dichloromethane-hexane (1 + 1, v/v) in a glass twin-trough chamber. Evaluation of the developed HPTLC plates was performed densitometrically. The results indicated that the detection limits of phoxim and chlorpyrifos were 5.0 x 10(-9) and 1.0 x 10(-8) g, respectively. Recoveries of the pesticides from tea by this analytical method were 90.7-105.5%, and relative standard deviations were 7.3-13.5%. The precision and accuracy of the method were generally satisfactory for analysis of pesticide residues in tea. PMID:18980143

Yue, Yongde; Zhang, Rong; Fan, Wei; Tang, Feng

2008-01-01

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

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

2003-01-01

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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

2005-01-01

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

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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

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Residue analysis of organochlorine pesticides in the Mae Klong river of Central Thailand  

Energy Technology Data Exchange (ETDEWEB)

The most natural waterways in Thailand are utilized for conventional agricultures, e.g. irrigation and wastewater discharge. Concentrations of 20 organochlorine pesticides (OCPs) were measured in surface sediments collected from the tributaries of the Mae Klong river during 2003-2005. The sampling sites chosen were nearby the rice paddy which organochlorine pesticides were intensively used for crop cultivation. Solid-liquid extraction technique was used for sediment extraction, and gas chromatography with electron capture detector was applied for pesticides determination. Total concentrations of OCPs found were ranged from 4.12 to 214.91 {mu}g g{sup -1} dw in the first year. In the second year, total residue concentrations in the surface sediments were in the range of 3.26-215.09 {mu}g g{sup -1} dw. Concentrations of pesticides were greater in dry-season rice cultivation period in both sampling years, and heptachlor epoxide was the contaminant found at highest concentration in this study. In addition, the occurrence of some selected contaminants including DDT, DDD and DDE reflects the recent contamination in the study area. This demonstrates not only that the natural waterway was polluted and contained much pesticide residues, but it also illustrates the necessity of a continuous long-term monitoring of the affected environment.

Poolpak, T. [Department of Biology, Faculty of Science, Mahidol University, Rama VI Rd., Phayathai, Bangkok 10400 (Thailand); Pokethitiyook, P. [Department of Biology, Faculty of Science, Mahidol University, Rama VI Rd., Phayathai, Bangkok 10400 (Thailand)], E-mail: scppg@mahidol.ac.th; Kruatrachue, M. [Department of Biology, Faculty of Science, Mahidol University, Rama VI Rd., Phayathai, Bangkok 10400 (Thailand); Mahidol University International College, 999 Buddhamonthon 4 Road, Salaya, Nakhonpathom 73170 (Thailand); Arjarasirikoon, U.; Thanwaniwat, N. [Department of Biology, Faculty of Science, Mahidol University, Rama VI Rd., Phayathai, Bangkok 10400 (Thailand)

2008-08-15

 
 
 
 
21

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

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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

22

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 < 20%. The limits of quantification (LOQ) for all pesticides were ?20 ng/g. The analytical results of the proposed method were in good agreement with proficiency test results (FAPAS, 19116). The recoveries and repeatabilities were in accordance with the criteria set by SANCO Guideline. The validated method was suitable for the analysis of pesticides in tea. PMID:23534490

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

2013-05-01

23

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

24

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

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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

25

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

International Nuclear Information System (INIS)

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

2005-07-01

26

A cost-effective screening method for pesticide residue analysis in fruits, vegetables, and cereal grains.  

Science.gov (United States)

This paper reports the results of studies performed to investigate the potential of applying thin layer chromatography (TLC) detection in combination with selected extraction and cleanup methods, for providing an alternative cost-effective analytical procedure for screening and confirmation of pesticide residues in plant commodities. The extraction was carried out with ethyl acetate and an on-line extraction method applying an acetone-dichloromethane mixture. The extracts were cleaned up with SX-3 gel, an adsorbent mixture of active carbon, magnesia, and diatomaceous earth, and on silica micro cartridges. The Rf values of 118 pesticides were tested in eleven elution systems with UV, and eight biotest methods and chemical detection reagents. Cabbage, green peas, orange, and tomatoes were selected as representative sample matrices for fruits and vegetables, while maize, rice, and wheat represented cereal grains. As an internal quality control measure, marker compounds were applied on each plate to verify the proper elution and detection conditions. The Rf values varied in the different elution systems. The best separation (widest Rf range) was achieved with silica gel (SG)--ethyl acetate (0.05-0.7), SG--benzene, (0.02-0.7) and reverse phase RP-18 F-254S layer with acetone: methanol: water/30:30:30 (v/v) (0.1-0.8). The relative standard deviation of Rf values (CV(Rf)) within laboratory reproducibility was generally less than 20%, except below 0.2 Rf, where the CVRf rapidly increased with decreasing Rf values. The fungi spore inhibition, chloroplast inhibition, and enzyme inhibition were found most suitable for detection of pesticides primarily for confirming their identity or screening for known substances. Their use for determination of pesticide residues in samples of unknown origin is not recommended. PMID:15825684

Ambrus, A; Füzesi, I; Susán, M; Dobi, D; Lantos, J; Zakar, F; Korsós, I; Oláh, J; Beke, B B; Katavics, L

2005-01-01

27

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

28

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

29

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)

2006-10-25

30

Uncertainty estimation in the analysis of pesticide residues in olive oil using data from proficiency tests.  

Science.gov (United States)

In this work we report the results for estimating the measurement uncertainty (MU) following up the application of two different approaches, relatively the top-down procedure, by using proficiency test data. We have focused the estimation on the olive oil matrix. We used the analytical data obtained from five selected editions of the Proficiency Tests (PTs, from 2007 to 2011) on pesticide residues in olive oil to estimate the MU. These PTs have been organized by Istituto Superiore di Sanità annually in cooperation with International Olive Council (IOC) since 1997. The number of participants in each trial ranged from 10 to 43. We used a total of 34 pesticide results. The expanded uncertainty U(c) was calculated using a covering factor k = 2 for a confidence interval of 95%. In the approach 1, the within-laboratory reproducibility standard deviation is combined with estimates of the method and laboratory bias using PTs data. In the approach 2, the way of estimating the MU is based only on the bias that the laboratory has obtained participating in a sufficient number of the IOC proficiency tests. Comparing the relative expanded uncertainty based on these different approaches we notice values quite constant and close, from 42% to 48%. Moreover, these calculated expanded uncertainties are less than the default value of 50% (corresponding to a 95% confidence level), adopted from European guidance document SANCO based on the fit-for-purpose relative standard deviation (FFP-RSD). PMID:23581684

Stefanelli, Patrizia; Generali, Tiziana; Barbini, Danilo Attard; Girolimetti, Silvana; Dommarco, Roberto

2013-01-01

31

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.

Sanchez-Bayo, Francisco; Goka, Koichi

2014-01-01

32

[Rapid screening and quantitative analysis of 144 pesticide residues in traditional Chinese medicinal herbs by gas chromatography-tandem mass spectrometry].  

Science.gov (United States)

An analytical method for the simultaneous determination of 144 pesticide residues in traditional Chinese medicinal herbs was established based on optimized QuEChERS with gas chromatography-tandem mass spectrometry (GC-MS/MS). The influences of different extraction solvents, different buffer systems and different purifying agents on the recoveries of the pesticides were investigated. The pesticide residues in the samples were extracted with acetonitrile, then cleaned-up by mixed sorbents and analyzed by GC-MS/MS in multi-reaction monitoring (MRM) mode. The external standard method was applied to quantify the pesticides. The linear range of the method was from 20 to 2 000 microg/kg with the correlation coefficients (r2) of more than 0. 983. The recoveries of the pesticides at the spiked levels of 20, 50 and 200 microg/kg ranged from 74.3% to 111.8% with the relative standard deviations lower than 15%, except for acephate, amitraz and aldrin. The method was successfully used for the analysis of target pesticides in testing samples, and had a good consistency in results with the existed standard one. This multi-residue analytical method allows for a rapid, efficient, sensitive and reliable screening and quantitative analysis of the target pesticides in traditional Chinese medicinal herbs. PMID:24783870

Cheng, Zhi; Zhang, Rong; Liu, Weihua; Wang, Jinhu; Wang, Minglin

2014-01-01

33

Radioisotopes in pesticide residues and metabolic studies  

International Nuclear Information System (INIS)

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

1994-03-01

34

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. Copyright © 2013 John Wiley & Sons, Ltd. 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

35

Determination of Pesticide Residues in Cannabis Smoke  

Digital Repository Infrastructure Vision for European Research (DRIVER)

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...

Nicholas Sullivan; Sytze Elzinga; Raber, Jeffrey C.

2013-01-01

36

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

In this work, the capability of gas chromatography coupled to time-of-flight mass spectrometry (GC–TOF MS) for quantitative analysis of pesticide residues has been evaluated. A multiclass method for rapid screening of pesticides (insecticides, acaricides, herbicides and fungicides) in fruit and vegetable matrices has been developed and validated, including detection, identification and quantification of the analytes. To this aim, several food matrices were selected: high water content (appl...

2012-01-01

37

Decline of Pesticide Residues from Barley to Malt  

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

2007-01-01

38

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

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Full Text Available The method of headspace solid phase microextraction (HS/SPME was successfully used in a simultaneous multicomponent analysis of hexachlorobenzene (HCB, tefluthrin, heptachlor, aldrin, chlorpyrifos, fenthion and bifenthrin in aqueous medium. Measurementswere performed using a nonpolar polydimethyl siloxane (PDMS fiber. Detection and quantification were done by gas chromatography/mass spectrometry (GC/MS.Optimal conditions for HS/SPME were determined both by performing extraction at different temperatures and examining extraction time profiles at constant temperature. Optimal extraction temperature for each pesticide studied was determined as follows: 60°C for HCB and for heptachlor, 80°C for aldrin and for chlorpyrifos, fenthion and tefluthrin, and temperature exceeding 80°C for bifenthrin. For the pesticide mixture studied, 60°C was identified as the optimum extraction temperature.Based on the time profiles obtained, it was confirmed that satisfactory extraction sensitivity can be obtained even for extraction times shorter than the time required to reach a sorption equilibrium. This conclusion was confirmed by linear concentration profiles obtained for the following ranges: 0.05-10 ng/ml (HCB, 0.05-25 ng/ml (tefluthrin, 0.05-40 ng/ml (heptachlor, 0.05-40 ng/ml (aldrin, 0.05-25 ng/ml (chlorpyrifos, 0.05-25 ng/ml (fenthionand 0.05-25 ng/ml (bifenthrin.Relative standard deviation (RSD values for triplicate measurements did not exceed 15%.

Rada ?urovi?

2007-01-01

39

Pesticide Residues in Food: Technologies for Detection.  

Science.gov (United States)

The report provides a brief assessment of existing, new, and emerging analytical technologies and methods to detect pesticide residues in food and addresses Federal research and programmatic issues relevant to the development and adoption of technologies ...

1988-01-01

40

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

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

2009-01-01

 
 
 
 
41

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

42

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

Scientific Electronic Library Online (English)

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

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

43

Considerations on the Content of Pesticides Residues in Vegetables  

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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

44

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 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)

2009-01-01

45

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

46

Blind analysis of fortified pesticide residues in carrot extracts using GC-MS to evaluate qualitative and quantitative performance.  

Science.gov (United States)

Unlike quantitative analysis, which must commonly undergo an extensive method validation process in labs to assure quality of results, the quality of the qualitative results in the analysis of pesticide residues in food is generally ignored in practice. Instead, chemists tend to rely on advanced MS techniques and general subjective guidelines or fixed acceptability criteria when making analyte identifications. All analytes and matrices have unique characteristics that make this current approach less effective than desirable in many real-world situations. Just as performed in quantitative method validation studies, collection of distinguishing factors of selectivity versus concentration, such as analyte retention time variabilities, ion ratios, matrix background evaluations, choice of ions, and the number of ions to use, provides specific information about the particular application to assess its quality. Empirical analysis of many blind samples to check the rates of false positives and negatives should be performed, at least to better evaluate LOD and reduce the chances of a serious qualitative problem. Familiarization training and review of results by the analyst(s) increase performance, and in any case, the traditional use of two independent analyses should still be relied upon to make chemical confirmations. In this study, an experimental approach to evaluate GC-MS using SIM with a quadrupole instrument and an MS/MS (ion trap) was conducted to assess the qualitative factors of both methods for 16 pesticides fortified (or not) in carrot extracts. Rates of false positives and negatives were compared using different identification criteria, and no single set of conditions was found to be superior for all analytes. PMID:19877146

Lehotay, Steven J; Gates, Robert A

2009-11-01

47

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)

2011-01-01

48

[A rapid multi-residual analysis for organophosphorus pesticides in the products of animal origin using gas chromatography coupled with accelerated solvent extraction and gel permeation chromatographic purification].  

Science.gov (United States)

A rapid method has been developed to determine the multi-residues of 36 organophosphorus pesticides in the products of animal origin using capillary gas chromatography with flame photometric detector (GC-FPD (P)). The organophosphorus pesticides were extracted with acetonitrile by accelerated solvent extraction, and cleaned up by auto gel permeation chromatography and primary secondary amine (PSA) packing material. The collected solution was analyzed by the GC-FPD (P) and quantified by internal standard method. The 36 organophosphorus pesticides were separated efficiently from impurity in high sensitivity and reproducibility by GC-FPD (P). The limits of detection (LODs) ranged from 0.0012 mg/kg (phorate) to 0.014 mg/kg (pyraclofos), and the limits of quantitation (LOQs) ranged from 0.004 mg/kg (phorate) to 0.047 mg/kg (pyraclofos). The recoveries ranged from 58.2% to 106.3% in blank samples spiked with 0.05, 0.1 and 0.2 mg/kg of 36 organophosphorus pesticides. The LODs, LOQs and the recoveries of the method all satisfy the requirement of pesticide residue analysis. PMID:19160756

Wu, Gang; Bao, Xiaoxia; Wang, Huaxiong; Yu, Chunyan; Wu, Huiming; Ye, Qingfu

2008-09-01

49

Use of buffering and other means to improve results of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables.  

Science.gov (United States)

A modification that entails the use of buffering during extraction was made to further improve results for certain problematic pesticides (e.g., folpet, dichlofluanid, chlorothalonil, and pymetrozine) in a simple, fast, and inexpensive method for the determination of pesticides in produce. The method, known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticide residues in foods, now involves the extraction of the sample with acetonitrile (MeCN) containing 1% acetic acid (HAc) and simultaneous liquid-liquid partitioning formed by adding anhydrous MgSO4 plus sodium acetate (NaAc). The extraction method is carried out by shaking a centrifuge tube which contains 1 mL of 1% HAc in MeCN plus 0.4 g anhydrous MgSO4 and 0.1 g anhydrous NaAc per g sample. The tube is then centrifuged, and a portion of the extract is transferred to a tube containing 50 mg primary secondary amine sorbent plus 150 mg anhydrous MgSO4/mL of extract. After a mixing and centrifugation step, the extract is transferred to autosampler vials for concurrent analysis by gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/tandem mass spectrometry. Independent of the original sample pH, the use of buffering during the extraction yields pH 5 in the water phase, which increases recoveries of both acid- and base-sensitive pesticides. The method was evaluated for 32 diverse pesticides in different matrixes, and typical percent recoveries were 95 +/- 10, even for some problematic pesticides. Optional solvent exchange to toluene prior to GC/MS analysis was also evaluated, showing equally good results with the benefit of lower detection limits, but at the cost of more time, material, labor, and expense. PMID:15859090

Lehotay, Steven J; Mastovská, Katerina; Lightfield, Alan R

2005-01-01

50

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

51

Behavior and elimination of pesticide residues during supercritical carbon dioxide extraction of essential oils of spice plants and analysis of pesticides in high-lipid-content plant extracts  

Digital Repository Infrastructure Vision for European Research (DRIVER)

With the production of pesticide-free extracts as an objective, this research investigations commenced with the extraction of spices of various provenance. Firstly, by a conventional solvent extraction and ascertaining the level of pesticide contamination. This was followed by fluid CO2 extraction. The level of pesticide contamination for these extracts from both extraction methods were compared. The work proceeded with the investigation of various parameters influencing pesticides behavior d...

Amajuoyi, Kingsley Ifeanyi

2005-01-01

52

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

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

Influence of pesticide residues on honey bee (Hymenoptera: Apidae) colony health in France.  

Science.gov (United States)

A 3-yr field survey was carried out in France, from 2002 to 2005, to study honey bee (Apis mellifera L.) colony health in relation to pesticide residues found in the colonies. This study was motivated by recent massive losses of honey bee colonies, and our objective was to examine the possible relationship between low levels of pesticide residues in apicultural matrices (honey, pollen collected by honey bees, beeswax) and colony health as measured by colony mortality and adult and brood population abundance. When all apicultural matrices were pooled together, the number of pesticide residue detected per sampling period (four sampling periods per year) and per apiary ranged from 0 to 9, with the most frequent being two (29.6%). No pesticide residues were detected during 12.7% of the sampling periods. Residues of imidacloprid and 6- chloronicotinic acid were the most frequently detected in pollen loads, honey, and honey bee matrices. Several pairs of active ingredients were present concurrently within honey bees and in pollen loads but not in beeswax and honey samples. No statistical relationship was found between colony mortality and pesticide residues. When pesticide residues from all matrices were pooled together, a mixed model analysis did not show a significant relationship between the presence of pesticide residues and the abundance of brood and adults, and no statistical relationship was found between colony mortality and pesticide residues. Thus, although certain pesticide residues were detected in apicultural matrices and occasionally with another pesticide residual, more work is needed to determine the role these residues play in affecting colony health. PMID:19508759

Chauzat, Marie-Pierre; Carpentier, Patrice; Martel, Anne-Claire; Bougeard, Stéphanie; Cougoule, Nicolas; Porta, Philippe; Lachaize, Julie; Madec, François; Aubert, Michel; Faucon, Jean-Paul

2009-06-01

55

Types of pesticides and determination of their residues  

International Nuclear Information System (INIS)

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

2010-03-01

56

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

57

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

Science.gov (United States)

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. PMID:14668155

Rasmusssen, R R; Poulsen, M E; Hansen, H C B

2003-11-01

58

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 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.

2010-07-26

59

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

60

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

 
 
 
 
61

Organophosphorus pesticides residues in Italian raw milk.  

Science.gov (United States)

Organophosphorus pesticides (OPPs), widely used in agriculture, can cause toxic effects to humans and animals. The main purpose of the present work was to determine the contamination in raw milk by the main organophosphorus pesticides used in Italy and to evaluate the opportunity to start specific procedures of risk management along the milk production chain. The samples, collected in 4 Italian dairy plants directly from the tank trucks during the delivering, were representative of 920 tonnes of raw milk. The isolation of the OPPs (acephate, chlorpyriphos, chlorpyriphos-methyl, diazinon, methamidophos, methidathion, phorate, pirimiphos-methyl) was performed by liquid partition followed by clean-up with solid phase extraction. The analyses were carried out by dual column gas chromatography using two nitrogen-phosphorus detectors. Among the 135 samples analysed, 37 were positive in traces and 10 showed an OPP contamination ranging from 5 to 18 microg/kg. The higher results were recorded in the samples collected during the autumn-winter period. The main pollutants detected were acephate and chlorpyriphos. In every positive sample found, the OPP contamination was lower than the maximum residue level (MRL) fixed by the European Commission. PMID:16566853

Pagliuca, Giampiero; Serraino, Andrea; Gazzotti, Teresa; Zironi, Elisa; Borsari, Andrea; Rosmini, Roberto

2006-08-01

62

Determination of pesticide residues in cereal grains  

International Nuclear Information System (INIS)

The applicability of the TLC for determination of pesticide residues in cereal grains was studied using corn, rice and wheat as representative commodities and atrazine, captan, chlorpyrifos, chlortoluron, diazinon, diuron, fenitrothion, metoxuron, prochloraz, triforine as representative compounds. Following the extraction with ethyl acetate the efficiency of extraction was tested with Bio-Rad SX-3 gel, GPC, silica gel, florisil and RP-18 reverse phase silica cartridge. The GPC alone or in combination with silica or florisil cleanup were the most suitable for cleanup of the extracts. The TLC elution characteristics of 131 pesticide active ingredients were tested with eight elution systems. The detectability of the selected compounds was determined with six detection methods including two chemical and four bioassay procedures. In addition to the basic methods, the non-toxic Penicillium cyclopium fungi spore inhibition was introduced and it was found very sensitive for some fungicide compounds. The minimum detectable quantities of the tested compounds ranged from 1 ng to 100 ng. The average recoveries from rice and wheat ranged from 78% to 89%, and the limits of quantitation, LOQ, were between 0.01 and 0.2 mg/kg for the selected ten compounds. (author)

2005-07-01

63

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

Science.gov (United States)

A method to effectively remove pigments in fresh vegetables using activated carbon followed cleanup through solid phase extraction (SPE) cartridge to further reduce matrix interference and contamination, was established to determine eight organophosphorous pesticides (OPPs) by gas chromatography (GC) with nitrogen-phosphorus detection (NPD) in this study, and it has been successfully applied for the determination of eight OPPs in various fresh vegetables with the recoveries ranging from 61.8% to 107%. To evaluate eight OPPs residue level, some fresh vegetables retailed at three agricultural product markets (APM) of Nanjing in China were detected, the results showed that phorate in Shanghai green (0.0257 microg g(-1)) and Chinese cabbage (0.0398 microg g(-1)), dimethoate in Shanghai green (0.0466-0.0810 microg g(-1)), Chinese cabbage (0.077 microg g(-1)), and spinach (0.118-0.124 microg g(-1)), methyl-parathion in Shanghai green (0.0903 microg g(-1)), Chinese cabbage (0.157 microg g(-1)), and spinach (0.0924 microg g(-1)), malathion in Shanghai green (0.0342-0.0526 microg g(-1)), chorpyrifos in spinach (0.106-0.204 microg g(-1)), and Chinese cabbage (0.149 microg g(-1)), chlorfenvinfos in carrot (0.094-0.131 microg g(-1)), were found. However, fonofos and fenthion were not detected in all the collected vegetable samples. PMID:18651087

Wang, Ligang; Liang, Yongchao; Jiang, Xin

2008-10-01

64

Nuclear applications for pesticide residue studies  

International Nuclear Information System (INIS)

Radiotracer techniques offer a powerful tool in understanding the fate of pesticides in soil, plant or food and can be utilised to take suitable corrective procedures to minimise the environmental effects of pesticides. 9 refs

1994-03-01

65

Determination of pesticide residues in fruit-based soft drinks.  

Science.gov (United States)

Here we report the first worldwide reconnaissance study of the presence and occurrence of pesticides in fruit-based soft drinks. While there are strict regulations and exhaustive controls for pesticides in fruits, vegetables, and drinking water, scarce attention has been paid to highly consumed derivate products, which may contain these commodities as ingredients. In the case of the fruit-based soft drinks industry, there are no clear regulations, relating to pesticides, which address them, even when there is significant consumption in vulnerable groups such as children. In this work, we have developed a screening method to search automatically for up to 100 pesticides in fruit-based soft drinks extracts based on the application of liquid chromatography-electrospray time-of-flight mass spectrometry (LC-TOF MS). The sample extracts injected were obtained by a preliminary sample treatment step based on solid-phase extraction using hydrophilic-lipophilic balanced polymer-based reverse phase cartridges and methanol as eluting solvent. Subsequent identification, confirmation, and quantitation were carried out by LC-TOF MS analysis: the confirmation of the target species was based on retention time matching and accurate mass measurements of protonated molecules ([M + H]+) and fragment ions (obtaining accuracy errors typically lower than 2 ppm). With the proposed method, we measured over 100 fruit-based soft drink samples, purchased from 15 different countries from companies with brands distributed worldwide and found relatively large concentration levels of pesticides in most of the samples analyzed. The concentration levels detected were of the micrograms per liter level, low when considering the European maximum residue levels (MRLs) set for fruits but very high (i.e., 300 times) when considering the MRLs for drinking or bottled water. The detected pesticides (carbendazim, thiabendazole, imazalil and its main degradate, prochloraz and its main degradate, malathion, and iprodione) are mainly those applied to crops in the final stages of production (postharvest treatment), some of them contain chlorine atoms in their structures. Therefore, steps should be taken with the aim of removing any traces of pesticides in these products, in order to avoid this source of pesticide exposure on the consumer, particularly on vulnerable groups with higher exposure, such as children. PMID:19551973

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

2008-12-01

66

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

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

2011-01-01

67

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

Science.gov (United States)

A method for the determination of pesticide residues in water and sediment was developed using the QuEChERS method followed by gas chromatography – mass spectrometry. The method was validated in terms of accuracy, specificity, linearity, detection and quantification limits. The recovery percentages obtained for the pesticides in water at different concentrations ranged from 63 to 116%, with relative standard deviations below 12%. The corresponding results from the sediment ranged from 48 to 115% with relative standard deviations below 16%. The limits of detection for the pesticides in water and sediment were below 0.003 mg L?1 and 0.02 mg kg?1, respectively.

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

2010-01-01

68

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

69

Fate of pesticide residues on tea from leaf to cup  

Digital Repository Infrastructure Vision for European Research (DRIVER)

This comprehensive review of the fate of pesticides deposited on tea leaves focuses on the wide variations in MRL levels fixed by different agencies viz., EU, EPA, Codex, which may differ by as much as 200 times in individual chemicals. Hence, there is a need for harmonization of pesticide residue limits, which should be agreed to by all the stakeholders. The main factors that determine the pesticide load are the characteristics of chemicals; prevailing field conditions; the process of manufa...

2003-01-01

70

Variability in pesticides residues--the US experience.  

Science.gov (United States)

The evolution of US Environmental Protection Agency's (EPA) process for estimating potential health risks from pesticide residues in or on food is examined in light of changes in US Legislation and the variability of residue data and assumptions used to estimate dietary exposure. In the 86 years since enactment of the Insecticide Act, pesticide laws have become progressively more health-based. Passage of the 1996 Food Quality Protection Act (FQPA) requires EPA to place particular emphasis on assessing potential risk from pesticides to infants and children. Primary factors affecting the actual pesticide residues in food include frequency of application, percentage of crop treated, and the interval from treatment to harvest. Primary factors affecting the estimated pesticide residues in food include the source of the residue data, calculation techniques for non-detected residues, and the availability of data reflecting post-harvest treatments. Risk assessors must thoroughly consider these factors when assessing dietary risk to pesticides. Risk managers will need to consider these factors as a means of mitigating dietary risk from pesticides. PMID:10983571

Suhre, F B

2000-07-01

71

Bound pesticide residues in soils and plants and their determination  

International Nuclear Information System (INIS)

To assess the environmental significance of pesticide residues in soil and plants one must distinguish between two types of residues: those that are extractable with solvents, and those residues that are not extractable with solvent. The extent of bound (non-extractable) residues varies with the plant and pesticide involved and generally increases with time after treatment Bound pesticide residues have been detected in the organic matter fractions of soil, i.e. humic acid, fulvic acid and humin. Several studies have shown that lignin, hemicellulose and pectic polysaccharide are the major bound residues fraction of pesticide in plants. Attempts have been made to extract bound pesticide residues by the milder to harsher methods. Drastic extractive procedures destroy the structure of soil or plants often results in the destruction of the identity of bound residues. The High Temperature Distillation (HTD) and Supercritical Fluid Extraction (SFE) techniques may provide possible means for extraction and identification of bound residues in food products. Regulatory agencies should also consider placing further emphasis on employing more effective extraction techniques and procedures to quantitatively remove bound residues

1999-12-01

72

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

Science.gov (United States)

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

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

2007-01-01

73

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)

2004-12-01

74

New multiresidue method using solid-phase extraction and gas chromatography-micro-electron-capture detection for pesticide residues analysis in royal jelly.  

Science.gov (United States)

Royal jelly, one of the most important bee products, can be contaminated with pesticide and/or antibiotic residues resulting from treatments applied either inside beehives or in the agricultural environment. A new multiresidue method was developed and validated for analysis of nine pesticides in royal jelly. Solid-phase extraction RP-C(18) cartridges were used for sample purification and isolation of analytes. Final solution was analyzed with GC and micro-electron-capture detection. Four synthetic acaricides used by beekeepers (bromopropylate, coumaphos, malathion and tau-fluvalinate), and moreover one pyrethroid, two organochlorine, and two organophosphate insecticides were tested. Linearity is demonstrated for the range of 0.0025-1mgkg(-1), with correlation coefficients ranging from 0.99991 to 0.99846, depending on the analyte. Overall recovery rates from royal jelly blank samples spiked at five fortification levels ranged from 80.8% (lindane) to 91.3% (ethion), well above the range defined by the SANCO/10232/2006 and EC/675/2002 documents. The limit of quantification was <0.003-0.005 mg kg(-1) depending on the analyte, and the reporting level of the method, defined as the lowest recovery level, was 0.005 mg kg(-1). PMID:18804771

Karazafiris, Emmanouel; Menkissoglu-Spiroudi, Urania; Thrasyvoulou, Andreas

2008-10-31

75

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

76

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

77

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

Science.gov (United States)

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

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

2013-01-01

78

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

79

Organochlorine Pesticide Residues in Plankton, Rangsit Agricultural Area, Central Thailand  

Science.gov (United States)

Few studies have investigated organochlorine pesticide residue content in freshwater plankton communities in Thailand. As a result, this study looks to examine the concentration of organochlorine pesticide residues in plankton collected from Khlong 7 (canal) at Rangsit agricultural area, central Thailand from June 2006 to February 2007. The results from this study show that plankton communities were composed of microphytoplankton, microzooplankton, and mesozooplankton. The average method recoveries varied from 84% to 103% with a relative standard deviation between 0.20% and 3.72%. The concentrations of organochlorine pesticide residues during a one-year-period were in the range of 0.10–3.65 ng/g wet wt and contained DDT and derivatives > ? endosulfan > ? HCH > ? heptachlor > aldrin and dieldrin > endrin and endrin aldehyde > methoxychlor, respectively. Moreover, the residues of ? HCH, DDT and derivatives, and methoxychlor were higher during wet season than dry season (t-test, p ? 0.05).

Siriwong, W.; Thirakhupt, K.; Sitticharoenchai, D.; Borjan, M.; Robson, M.

2014-01-01

80

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)

2005-07-01

 
 
 
 
81

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

82

Wide-scope analysis of veterinary drug and pesticide residues in animal feed by liquid chromatography coupled to quadrupole-time-of-flight mass spectrometry.  

Science.gov (United States)

A fast and generic method has been developed for the simultaneous monitoring of >250 pesticides and veterinary drugs (VDs) in animal feed. A 'dilute-and-shoot' extraction with water and acetonitrile (1% formic acid) followed by a clean-up step with Florisil cartridges was applied. The extracts were analysed by ultra-high performance liquid chromatography coupled to hybrid analyser quadrupole-time-of-flight mass spectrometry using both positive and negative electrospray ionisation. The detection of the residues was accomplished by retention time and accurate mass using an in-house database. The identification of the detected compounds was carried out by searching of fragment ions for each compound and isotopic pattern. The optimised method was validated and recoveries ranged from 60% to 120% at three concentrations (10, 50 and 100 ?g kg(-1)) for 30%, 68% and 80% of compounds, respectively, included in the database (364) in chicken feed. Document SANCO 12495/2011 and Directive 2002/657/CE were used as guidelines for method validation. Intra-day and inter-day precisions, expressed as relative standard deviations, were lower than 20% for more than 90% of compounds. The limits of quantification ranged from 4 to 200 ?g kg(-1) for most analytes, which are sufficient to verify compliance of products with legal tolerances. The applicability of the procedure was further tested on different types of feed (chicken, hen, rabbit and horse feed), evaluating recoveries and repeatability. Finally, the method was applied to the analysis of 18 feed samples, detecting some VDs (sulfadiazine, trimethoprim, robenidin and monensin Na) and only one pesticide (chlorpyrifos). PMID:23712649

Aguilera-Luiz, María M; Romero-González, Roberto; Plaza-Bolaños, Patricia; Martínez Vidal, José Luis; Garrido Frenich, Antonia

2013-08-01

83

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)

2008-01-01

84

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

85

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

Science.gov (United States)

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

España Amórtegui, Julio C; Guerrero Dallos, Jairo A

2014-04-01

86

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

87

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

88

Graphene as dispersive solidphase extraction materials for pesticides LC-MS/MS multi-residue analysis in leek, onion and garlic.  

Science.gov (United States)

A multi-residue analytical method was validated for 24 representative pesticides residues in onion, garlic and leek. The method is based on modified QuEChERS sample preparation with a mixture of graphene, primary secondary amine (PSA), and graphitised carbon black (GCB) as reversed-dispersive solid-phase extraction (r-DSPE) material and LC-MS/MS. Graphene was first used as an r-DSPE clean-up sorbent in onion, garlic and leek. The results first show that the mixed sorbent of graphene, PSA and GCB has a remarkable ability to clean-up interfering substances in the r-DSPE procedure when compared with the mixture of PSA and GCB. Use of matrix-matched standards provided acceptable results for tested pesticides with overall average recoveries between 70.1% and 109.7% and consistent RSDs 70% recovery. PMID:24224921

Guan, Wenbi; Li, Changsheng; Liu, Xue; Zhou, Shujing; Ma, Yongqiang

2014-01-01

89

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

International Nuclear Information System (INIS)

Pesticide residues and contaminants in selected leafy vegetables, namely (lettuce, garden rocket and salad onion) were monitored at market level in Riyadh City in Saudi Arabia, during the period june to july 2001. Fifteen samples of vegetables from the City vegetable market of Riyadh were collected and subjected to multi-pesticide residue detection and analysis by gas chromatography with mass spectrometer and electron capture detectors (GC/MS,ECD). Results of sample extracts analysis showed that the two vegetables of: garden rocket and salad onion contain pesticide residues and contaminants which have no Maximum Residue Limits (MRL) prescribed by Codex Alimentarius Commission (CAC) collaborate with World Health and Food and Agriculture Organizations (WHO/FAO). Whereas lettuce vegetable was found free of any identified pesticide residues or contaminants. Garden rocket was shown to contain dibutyl phthalate (0.04 ppm)-steryl chloride (0.02 ppm) tridecane (0.06 ppm)-hexadecane (0.07 ppm)-BIS (ethylhexyl) phthalate (0.006 ppm) and pyridinium, 1-hexyl chloride (0.01 ppm). The salad onion was found to contain 9-octadecanamide (0.13 ppm)-tridecane (0.15 ppm) and tetradecane (0.16 ppm). There are no established MRL s for these pesticides and contaminants detected in garden rocket and salad onion, although when impacts on human health were reviewed some of them were found probably hazardous. (Author)

2004-01-01

90

Comparison of sample preparation methods combined with fast gas chromatography-mass spectrometry for ultratrace analysis of pesticide residues in baby food.  

Science.gov (United States)

Four sample preparation techniques were compared for the ultratrace analysis of pesticide residues in baby food: (a) modified Schenck's method based on ACN extraction with SPE cleaning; (b) quick, easy, cheap, effective, rugged, and safe (QuEChERS) method based on ACN extraction and dispersive SPE; (c) modified QuEChERS method which utilizes column-based SPE instead of dispersive SPE; and (d) matrix solid phase dispersion (MSPD). The methods were combined with fast gas chromatographic-mass spectrometric analysis. The effectiveness of clean-up of the final extract was determined by comparison of the chromatograms obtained. Time consumption, laboriousness, demands on glassware and working place, and consumption of chemicals, especially solvents, increase in the following order QuEChERS < modified QuEChERS < MSPD < modified Schenck's method. All methods offer satisfactory analytical characteristics at the concentration levels of 5, 10, and 100 microg/kg in terms of recoveries and repeatability. Recoveries obtained for the modified QuEChERS method were lower than for the original QuEChERS. In general the best LOQs were obtained for the modified Schenck's method. Modified QuEChERS method provides 21-72% better LOQs than the original method. PMID:16830724

Hercegová, Andrea; Dömötörová, Milena; Kruzlicová, Dása; Matisová, Eva

2006-05-01

91

Determination of Pesticides Residues in Selected varieties of Mango  

Directory of Open Access Journals (Sweden)

Full Text Available The present study was undertaken to access the residue of commonly used pesticides viz Cypermethrin, Methamedophos, Monocrotophos, Cyfluthrin, Dialdrin and Methyl Parathian respectively in three varieties of Mango being collected from the grower fields in Multan division. The samples were treated with organic solvent Cyclohexane and ethylacetate (1:1, cleaned on Gel Permeation Chromatograph (GPC and analyzed on auto system Gas Chromatograph (GC with electron capture detector (ECD. All the samples were found to be contaminated with a degree of variation of pesticides residue studied. However, all the samples were within permissible limits being set by FAO/WHO with reference to public health.

Saqib Hussain

2002-01-01

92

Glove accumulation of pesticide residues for strawberry harvester exposure assessment.  

Science.gov (United States)

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

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

2011-06-01

93

Characterization of distribution of pesticide residues in crop units.  

Science.gov (United States)

The characteristic features of distribution of pesticide residues in crop units and single sample increments were studied based on more than 19,000 residue concentrations measured in root vegetables, leafy vegetables, small-, medium- and large-size fruits representing 20 different crops and 46 pesticides. Log-normal, gamma and Weibull distributions were found to provide the best fit for the relative frequency distributions of individual residue data sets. The overall best fit was provided by lognormal distribution. The relative standard deviation of residues (CV) in various crops ranged from 15-170%. The 100-120 residue values being in one data set was too small to identify potential effects of various factors such as the chemical and physical properties of pesticides and the nature of crops. Therefore, the average of CV values, obtained from individual data sets, were calculated and considered to be the best estimate for the likely variability of unit crop residues for treated field (CV = 0.8) and market samples (CV = 1.1), respectively. The larger variation of residues in market samples was attributed to the potential mixing of lots and varying proportion of non-detects. The expectable average variability of residues in composited samples can be calculated from the typical values taking into account the sample size. PMID:23638888

Horváth, Zsuzsanna; Ambrus, Arpád; Mészáros, László; Braun, Simone

2013-01-01

94

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

95

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

1977-01-01

96

Pesticide residues in fruits and vegetables from South America â?? 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

97

Organophosphorus pesticide residues in the total diet of Kuwait  

International Nuclear Information System (INIS)

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

2005-01-01

98

Analysis of phenoxyl-type N-methylcarbamate pesticide residues in vegetables by capillary zone electrophoresis with pre-column hydrolysis and amperometric detection.  

Science.gov (United States)

With systematic studies of pre-column thermalhydrolysis, a method is described for the determination of fivephenoxyl-type N-methylcarbamates (NMCs) (viz., propoxur, carbofuran, 3-hydroxy-carbofuran, carbaryl, and bendiocarb) in vegetables by capillary zone electrophoresis with amperometric detection. Effects of hydrolysis parameters such as alkali medium, temperature, and hydrolysis time, as well as separation conditions, are investigated. Under the optimum conditions, baseline separation of five hydrolysates is achieved within 16 min. Good calibration curves of propoxur, carbofuran, 3-hydroxy-carbofuran, carbaryl, and bendiocarb are obtained from 1.20x10(-7) to 5.00x10(-5) mol/L, and their detection limits (S/N=3) are 1.80x10(-8), 1.50x10(-8), 1.80x10(-8), 2.50x10(-8), and 1.80x10(-8) mol/L, respectively, which is approximately 20 approximately 50-fold more sensitive than those previously reported with a UV method. In the application of vegetable samples, the five NMCs are well determined. Average recoveries of 75 approximately 89% and 86 approximately 100% at fortified levels of 0.05 and 0.80 mg/kg are achieved with relative standard deviations of 2 approximately 6%, respectively. The method is sensitive, reproducible, and provides an alternative means for the analysis of phenoxyl-type NMC pesticide residues. PMID:18718137

Lin, Xucong; Hong, Qin; Wu, Xiaoping; Guo, Liangqia; Xie, Zenghong

2008-08-01

99

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

Chapman, S

2003-01-01

100

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

 
 
 
 
101

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

102

Pesticide residue analysis in foodstuffs applying capillary gas chromatography with mass spectrometric detection. State-of-the-art use of modified DFG-multimethod S19 and automated data evaluation.  

Science.gov (United States)

This paper focuses on recent developments in the author's laboratory and reports on the "ultimate" analysis scheme which has evolved over the last 20 years in our laboratory. This demonstrates the feasibility of screening analyses for pesticide residue identification, mainly by full scan GC-MS, down to the 0.01 ppm concentration level in plant foodstuffs. It is based on a miniaturized DFG S19 extraction applying acetone for extraction followed by liquid-liquid extraction with ethyl acetate-cyclohexane followed by gel permeation chromatography. The final chromatographic determination is carried out with a battery of three parallel operating gas chromatographic systems using effluent splitting to electron-capture and nitrogen-phosphorus detection, one with a SE-54 the other with a OV-17 capillary column and the third one with a SE-54 capillary column and mass selective detection for identification and quantitation. The method is established for monitoring more than 400 pesticides amenable to gas chromatography. These pesticide residues are identified in screening analyses by means of the dedicated mass spectral library PEST.L containing reference mass spectra and retention times of more than 400 active ingredients and also metabolites applying the macro program AuPest (Automated residue analysis on Pesticides) for automated evaluation which runs with Windows based HP ChemStation software. The two gas chromatographic systems with effluent splitting to electron-capture and nitrogen-phosphorus detection are used to check the results obtained with the automated GC-MS screening and also to detect those few pesticides which exhibit better response to electron-capture and nitrogen-phosphorus detection than to mass spectrometry in full scan. PMID:11045498

Stan, H J

2000-09-15

103

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

104

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.

105

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

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

2012-01-01

106

Organochlorine Pesticides Residues in Mussels of Greek Island Evia  

Digital Repository Infrastructure Vision for European Research (DRIVER)

A simple and effective analytical procedure was developed for the determination of some organochlorine residues inmussel samples of two sampling points in Evia Island, Greece. The sample extraction was performed on lyophilizedsamples using either the Microwave Assisted Solvent Extraction (MASE) or the Soxhlet extraction technique. Using bothtechniques aldrin, endrin and endosulfan sulfate were determined. The quantification of these pesticides was carried outby Gas Chr...

Kasiotis, Konstantinos M.

2009-01-01

107

[Sample pretreatment methods of pesticide residues in Panax notoginseng of Chinese traditional medicine].  

Science.gov (United States)

Two sample pretreatment methods of pesticide residues in Panax notoginseng of Chinese traditional medicine were developed. For Method I, the residues were extracted from homogenized tissue with n-hexane-dichloromethane (6:4) by means of ultrasonication, the crude extract was purified by an Envi-carb/NH2 solid-phase extraction (SPE) column. For Method II, matrix solid-phase dispersion (MSPD) technique was used for extracting and cleaning up. The eluates were concentrated by rotary evaporation, and then were redissolved in dichloromethane prior to GC-MS determination. The determination was performed in selected ion monitoring (SIM) mode with the external calibration for quantitative analysis. Under the optimal conditions, the results indicated that the methods are easier and faster, the recoveries of method I for the spiked standards at concentration of 0.01, 0.5, and 2.0 mg x kg(-1) were 81.90%-102.10% with the relative standard deviations (RSDs) of 3.60%-7.10%. The recoveries of method II were 96.26%-104.20% with the RSDs of 3.52%-7.94%. The detection limits (S/N) for residues of pesticides were in the range of 0.48-1.34 ng x g(-1). The results indicated that these multiresidue analysis methods can meet the requirements for determination of residue pesticides and can be appropriate for trace analysis of residue pesticides in Panax notoginseng. PMID:24417086

Wu, Na; Liu, Wei; Yan, He-Ping; Fan, Ai-Ping; Huang, Du-Shu; Zhou, Bo; Chen, Xian-Lan; Xu, Shi-Juan; Shi, Ling

2013-10-01

108

Organochlorine Pesticide Residues in Fish Samples from Lagos Lagoon, Nigeria  

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

David Adeyemi; Grace Ukpo; Chimezie Anyakora; JohnPaul Unyimadu

2008-01-01

109

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

110

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

Directory of Open Access Journals (Sweden)

Full Text Available

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

Reich H

2012-10-01

111

The Organochlorine Pesticides Residue Levels in Karun River Water  

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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

112

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

113

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

114

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)

2003-07-22

115

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

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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

116

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

117

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

118

Microwave assisted solvent extraction and coupled-column reversed-phase liquid chromatography with UV detection use of an analytical restricted-access-medium column for the efficient multi-residue analysis of acidic pesticides in soils.  

Science.gov (United States)

A screening method has been developed for the determination of acidic pesticides in various types of soils. Methodology is based on the use of microwave assisted solvent extraction (MASE) for fast and efficient extraction of the analytes from the soils and coupled-column reversed-phase liquid chromatography (LC-LC) with UV detection at 228 nm for the instrumental analysis of uncleaned extracts. Four types of soils, including sand, clay and peat, with a range in organic matter content of 0.3-13% and ten acidic pesticides of different chemical families (bentazone, bromoxynil, metsulfuron-methyl, 2,4-D, MCPA, MCPP, 2,4-DP, 2,4,5-T, 2,4-DB and MCPB) were selected as matrices and analytes, respectively. The method developed included the selection of suitable MASE and LC-LC conditions. The latter consisted of the selection of a 5-microm GFF-II internal surface reversed-phase (ISRP, Pinkerton) analytical column (50 x 4.6 mm, I.D.) as the first column in the RAM-C18 configuration in combination with an optimised linear gradient elution including on-line cleanup of sample extracts and reconditioning of the columns. The method was validated with the analysis of freshly spiked samples and samples with aged residues (120 days). The four types of soils were spiked with the ten acidic pesticides at levels between 20 and 200 microg/kg. Weighted regression of the recovery data showed for most analyte-matrix combinations, including freshly spiked samples and aged residues, that the method provides overall recoveries between 60 and 90% with relative standard deviations of the intra-laboratory reproducibility's between 5 and 25%; LODs were obtained between 5 and 50 microg/kg. Evaluation of the data set with principal component analysis revealed that the parameters (i) increase of organic matter content of the soil samples and (ii) aged residues negatively effect the recovery of the analytes. PMID:11771842

Hogendoom, E A; Huls, R; Dijkman, E; Hoogerbrugge, R

2001-12-14

119

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

120

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

Givaudan, Nicolas; Wiegand, Claudia

2014-01-01

 
 
 
 
121

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

122

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 ...

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

2008-01-01

123

[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

124

Pesticide Residues, Results from the period 2004-2011  

DEFF Research Database (Denmark)

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

Petersen, Annette; Jensen, Bodil Hamborg

2013-01-01

125

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

International Nuclear Information System (INIS)

Cocoa is a major cash crop and contributes significantly to Ghana's economy. Majority of this contribution is as a result of foreign earnings in foreign trade partnership. Cocoa products are consumed locally aside it generating foreign income for the country. Pesticide residues above allowable limits in cocoa beans have potential detrimental effects on human health, depending on the frequency of exposure and/or the potency or toxicity of the pesticide. Pesticide residues on cocoa also attract trade sanctions from international trading partners. The approved pesticides, which are used to control pests in the growing cocoa in Ghana, are: Diazinon, Cypermethrin, Deltamethrin, Acetamiprid, Imidicloprid and Pyrethrums; nevertheless some unapproved pesticides on cocoa such as Pirimiphos-methyl, Chlorpyrifos, Endosulfan, Fenitrotion, Fenvalerate, Permethrin and others find their way for use on cocoa in Ghana. The main objective of this study was to determine the levels of pesticide residues in fermented dried cocoa beans produced and ready for export in Ghana, using gas chromatography mass spectrometry. It also seeks to provide the baseline information on contamination levels of pesticide residues in semi-finished and selected finished fermented dried cocoa beans products. Fermented dried cocoa beans were sampled at random in the two main COCOBOD warehouses located in Tema and Takoradi. Semi-finished and finished cocoa products were obtained from processing industries in 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

2011-01-01

126

Monitoring of some pesticides residue in consumed tea in Tehran market  

Digital Repository Infrastructure Vision for European Research (DRIVER)

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 diffe...

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

2013-01-01

127

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

2001-01-01

128

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

129

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.

130

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

Directory of Open Access Journals (Sweden)

Full Text Available The objective of present research study was to assess the concentration of pesticide residues in fruits and vegetables from markets in Kumasi and to generate awareness about the lethal effects of these pesticides on human beings as well as to estimate the potential health risks associated with the pesticide residue with regard to consumers. A total of 350 locally produced fruits and vegetables were purchased from six main markets in Kumasi and analyzed by gas chromatography equipped with electron capture detector for organochlorine (gamma-HCH, methoxychlor, aldrin, dieldrin, endrin, p,p’-DDE, p,p’-DDT and pyrethroid (permethrin, cyfluthrin, cypermethrin, fenvalerate, deltamethrin residues. The residual concentrations of selected pesticides in the various fruit and vegetable samples and the potential health risks associated with the exposure to these pesticides were also assessed. The results obtained showed that 37.5% of the fruit and vegetable samples analyzed contained no detectable level of the monitored pesticides, 19.0% of the samples gave results with levels of insecticides residues above the MRL, while 43.5% of the samples showed results below the MRL. The analysis of health risk estimates revealed that none of the pesticides exceeded the reference dose in both fruit and vegetables except endrin which exceeded reference dose in vegetables, suggesting a great potential for systemic toxicity in children considered the most vulnerable population subgroup. Based on observations made in these studies, it is proposed that more extensive monitoring investigation covering all fruits and vegetables in all the ten regions of Ghana be carried out to find the exact position of pesticide residues.

Crentsil Kofi Bempah

2011-11-01

131

Organochlorine Pesticides Residues in Mussels of Greek Island Evia  

Directory of Open Access Journals (Sweden)

Full Text Available A simple and effective analytical procedure was developed for the determination of some organochlorine residues inmussel samples of two sampling points in Evia Island, Greece. The sample extraction was performed on lyophilizedsamples using either the Microwave Assisted Solvent Extraction (MASE or the Soxhlet extraction technique. Using bothtechniques aldrin, endrin and endosulfan sulfate were determined. The quantification of these pesticides was carried outby Gas Chromatography-Mass Spectrometry (GC-MS working in the Selected Ion Monitoring (SIM mode and therecoveries ranged from 75 to 102% at two spiking levels for 6 replicates.

Konstantinos M. Kasiotis

2009-07-01

132

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 basis for an evaluation of the state of knowledge. (orig.)

1984-01-01

133

76 FR 10584 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...  

Science.gov (United States)

...purposes and is available in the Food and Drug Administration Pesticide...residues of the insecticide zeta-cypermethrin, (S-cyano(3-phenoxyphenyl...detecting and measuring levels of cypermethrin in or on food with a limit of detection...

2011-02-25

134

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

Science.gov (United States)

...expectation of finding residues of dodine in livestock or poultry, no analytical method for animal tissues...Environmental protection, Agricultural commodities, Feed additives, Food additives, Pesticides and pests, Reporting and...

2012-08-22

135

Residues of 18 organochlorine pesticides in 30 traditional Chinese medicines.  

Science.gov (United States)

We analyzed 30 different traditional Chinese medicines (TCMs) to determine levels of contamination with organochlorine pesticides (OCPs). We tested for 18 pesticides: benzene hexachloride (BHC, including alpha-BHC, beta-BHC, gamma-BHC, delta-BHC), heptachlor, heptachlor epoxide, tecnazene, pentachloronitrobenzene (PCNB), hexachlorobenzene, aldrin, methyl pentachlorophenyl sulphide (MPCPS), alpha-endosulfan, trans-chlorodane, cis-chlorodane, p,p'-DDE, o,p'-DDT, p,p'-DDD, and p,p'-DDT. The sample extracts were analyzed by GC-ECD. A total of 280 samples of 30 different TCMs were analyzed. Our results showed that 75.8% of samples contained at least one of the above pesticides. The pesticides detected were tecnazene, hexachlorobenzene, PCNB, heptachlor, aldrin, alpha-BHC, beta-BHC, gamma-BHC, delta-BHC, p,p'-DDE, o,p'-DDT, p,p'-DDD p,p'-DDT. More than 50% of samples contained alpha-BHC (55.8%) and PCNB (55.8%); hexachlorobenzene was detected in 40.9% of samples, tecnazene in 19.5%, gamma-BHC in 16.7% and p,p'-DDE in 16.0%. Less than 10% of samples contained beta-BHC, delta-BHC, heptachlor, aldrin, o,p'-DDT, p,p'-DDT and p,p'-DDD. None of the 280 samples contained heptachlor epoxide, MPCPS, alpha-endosulfan, trans-chlorodane, or cis-chlorodane. Concentrations of OCPs in four samples exceeded the maximum allowable residue limits (MRLs) specified in the PRC Pharmacopoeia 2005. The results indicate that the most common contaminants among the 280 samples were alpha-BHC, PCNB, hexachlorobenzene, and tecnazene. Our results suggest that contamination of TCMs with OCPs is widespread. The MRLs for other OCPs commonly found in TCMs (e.g. hexachlorobenzene and tecnazene) should be set as quickly as possible, and the MRLs of OCPs in other TCMs should be established. PMID:18160094

Xue, Jian; Hao, Lili; Peng, Fei

2008-04-01

136

Performance of programmed temperature vaporizer, pulsed splitless and on-column injection techniques in analysis of pesticide residues in plant matrices.  

Science.gov (United States)

A programmed temperature vaporizer (PTV) injection technique has been recently implemented in our laboratory. In present paper its performance is compared with other GC injection techniques commonly used in trace analysis of organic contaminants. Twenty-six pesticides representing different chemical classes were selected for the study. This group comprised compounds typically subjected to discrimination in the injection port of the gas chromatograph, e.g., polar organophosphorus pesticides and thermolabile carbamates. In the first set of experiments standards in pure solvent were injected into GC systems employing different types of injection, i.e., (i) on-column, (ii) pulsed splitless, (iii) PTV solvent split, (iv) PTV splitless, and the responses of analytes were compared. Discrimination of troublesome compounds was significantly decreased with the application of PTV solvent split injection. In the second set of experiments repetitive injections of purified wheat samples were performed, with aims to evaluate the long-term stability of responses, as well as matrix effects in different stages of system contamination for each injection technique. The tolerance of the GC system to co-injected matrix components was increased in the order: on-columncompounds, while with the application of PTV matrix effects did not exceed 200% under the same conditions. PMID:11765087

Zrostlíková, J; Hajslová, J; Godula, M; Mastovská, K

2001-12-01

137

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

Science.gov (United States)

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

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

2013-05-22

138

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

Science.gov (United States)

The use and application of pesticides in vineyard is a common practice, which is important to prevent pest and diseases and improve the crop health and production, but on the other hand it could involve a potential risk for humans and the environment. For this reason, it is important to develop and validate a simple and fast multiresidue method to determine the presence of these compounds in soils. La Rioja region (Spain) is one of the most important wine-growing regions in Spain, which also entails that could be an important area of pesticide pollution. The objective of this work is to assess the temporal distribution of the possible pesticide pollution in soils from different areas of La Rioja (Spain). The pesticides selected in this study included fungicides (metalaxyl, and its metabolite CGA62826, pyrimethanil, tebuconazole, myclobutanil, kresoxim-methyl, triadimenol and flutriafol); herbicides (fluometuron, terbuthylazine and its metabolites desethylterbuthylazine and hydroxyterbuthylazine, lenacil, ethofumesate and acetochlor) and insecticides (methoxyfenozide and pirimicarb). The pesticide residues were evaluated by two analytical techniques, gas chromatography and liquid chromatography (GC-MS and LC-MS). The extraction procedure of pesticides from soils was optimized using two soil samples (blank soils) with different texture and characteristics collected from areas without pesticide application. Recoveries were studied in soil samples fortified with all pesticides at two levels of concentrations (the agronomic dose, 0.1 mg kg-1, and ten times this dose, 1 mg kg-1). Different extraction solvents were tested. The best results were obtained with methanol:acetone (50:50) mixture or methanol:CaCl2 0.01 M (50:50) mixture for hydroxyterbuthylazine and CGA62826. The accuracy (average recovery) and precision (reproducibility and repeatability) of the method were assessed using six replicates and the limits of detection (LODs) and quantification (LOQs) were estimated. Recoveries were above 70% for all pesticides. Good linear relationships of the calibration curves (0.01-1 ?g mL-1) were obtained for all the compounds by the two analytical methods with regression coefficients (r2) higher than 0.99 in the range of concentrations studied. Detection limits were pesticides studied. After the development and validation of an analytical method, the study of the temporal variability of the pesticide pollution in different periods of time (September 2011, and March, June and October 2012) were performed. Herbicide residues were found in most of the soils and an increment in concentrations of these compounds and in the number of positive samples were detected in samples collected in March 2012 in relation to those collected in September 2011. This increase in the number of positive samples was of 30 % for terbuthylazine. Fungicide residues were detected in greater concentrations in samples collected in September. Both behaviours may be related with the time of application of both types of compounds. Herbicides are commonly applied in March-April and fungicides are usually applied in summer, when different grapevine diseases like botrytis or mildiu commonly appear. Moreover, new pesticide residues were detected in March 2012, which were not detected in September 2011 in any soil sample. Further analysis of results is in course.

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

2013-04-01

139

A Survey of Determination for Organophosphorus Pesticide Residue in Agricultural Products  

Directory of Open Access Journals (Sweden)

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

Wen Li

2013-04-01

140

[Study on the detection and pattern classification of pesticide residual on vegetable surface by using visible/near-infrared spectroscopy].  

Science.gov (United States)

A nondestructive testing based on visible/near-infrared reflectance spectroscopy was put forward for the common high pesticide residues of green plants in the wavelength range from 600 to 1100 nm. Firstly, spectral features were extracted by wavelet transform from original spectral data. Secondly, the principal component analysis (PCA) was done in the further analysis of spectral characteristics. Thirdly, the two PCs were applied as inputs of artificial neural network, and a multi-neuron perceptron neural network was established. Finally, It was proved that the type of pesticide residues was effectively identified and showed by classification results. In short, the study provides a new approach to the detection of pesticide residues in vegetables and fruits. PMID:22827060

Chen, Rui; Zhang, Jun; Li, Xiao-long

2012-05-01

 
 
 
 
141

Effect of sampling size on the determination of accurate pesticide residue levels in Japanese agricultural commodities.  

Science.gov (United States)

The uncertainty in pesticide residue levels (UPRL) associated with sampling size was estimated using individual acetamiprid and cypermethrin residue data from preharvested apple, broccoli, cabbage, grape, and sweet pepper samples. The relative standard deviation from the mean of each sampling size (n = 2(x), where x = 1-6) of randomly selected samples was defined as the UPRL for each sampling size. The estimated UPRLs, which were calculated on the basis of the regulatory sampling size recommended by the OECD Guidelines on Crop Field Trials (weights from 1 to 5 kg, and commodity unit numbers from 12 to 24), ranged from 2.1% for cypermethrin in sweet peppers to 14.6% for cypermethrin in cabbage samples. The percentages of commodity exceeding the maximum residue limits (MRLs) specified by the Japanese Food Sanitation Law may be predicted from the equation derived from this study, which was based on samples of various size ranges with mean residue levels below the MRL. The estimated UPRLs have confirmed that sufficient sampling weight and numbers are required for analysis and/or re-examination of subsamples to provide accurate values of pesticide residue levels for the enforcement of MRLs. The equation derived from the present study would aid the estimation of more accurate residue levels even from small sampling sizes. PMID:22475588

Fujita, Masahiro; Yajima, Tomonari; Iijima, Kazuaki; Sato, Kiyoshi

2012-05-01

142

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

143

Removal of chloropyrifos ethyl, tetradifon and chlorothalonil pesticide residues from citrus by using ozone.  

Science.gov (United States)

The removal of chloropyrifos ethyl, tetradifon and chlorothalonil pesticide residues from the lemon, orange and grapefruit matrices were achieved by ozonation. All of chlorothalonil residues adsorbed onto the orange matrix were completely removed after 5 min ozonation. The highest removal percentages of tetradifon and chloropyrifos ethyl were achieved as 98.6 and 94.2%, respectively for the lemon and grapefruit matrices. All of diffused chlorothalonil and chloropyrifos ethyl residues were completely removed from both orange and grapefruit matrices after 5 min ozonation. Increasing of applied ozone dosage was not significantly effect on the removal percentages of pesticides whereas increasing of ozonation temperature caused a negative effect on the removal percentages of pesticides. The washing of the matrices with tap water was not as effective as ozonation in the removal of residual pesticides. Our results show that ozone treatment has a great potential for removing of residual pesticides from lemon, orange and grapefruit matrices. PMID:23058925

Kusvuran, Erdal; Yildirim, Deniz; Mavruk, Funda; Ceyhan, Mehmet

2012-11-30

144

Investigation of pesticide residues in vegetables and fruits grown in various regions of Hatay, Turkey.  

Science.gov (United States)

In this study, 175 pesticide residues in various vegetable and fruit samples grown in different regions of Hatay, Turkey, were investigated. Residue analyses were performed using liquid chromatography-tandem mass spectrometry with the QuEChERS method. In tomato, plum and apricot samples, pesticide residues were below the limits of detection. In other samples, at least one pesticide residue was detected. Twelve pesticides (acetamiprid, carbendazim, chlorpyrifos, fenarimol, fludioxonil, hexythiazox, imidacloprid, metalaxyl, pyridaben, pyriproxyfen, thiabendozole, triadimenol) were found at levels between 0.003 and 0.759 mg kg(-1). Only in cucumber samples, acetamiprid residues were found at levels greater than the maximum acceptable limit in Turkish Food Codex and European Union maximum residue limits (EU MRLs). In other samples, the detected residue amounts are less than the MRLs declared in the Turkish Food Codex and EU MRLs. PMID:24786407

Sungur, Sana; Tunur, Cetin

2012-01-01

145

Enzyme inhibition-based determination of pesticide residues in vegetable and soil in centrifugal microfluidic devices.  

Science.gov (United States)

Pesticide residue is of concern as an environmental pollutant when present at medium to high concentrations. Such residue was quantified in both vegetable and soil samples by an enzyme inhibition technique. The multistep reactions were integrated into centrifugal microfluidic devices allowing automated simultaneous analysis of several samples or of replicates. The small sample size inherent to microfluidic devices allowed for less reagent to be used including less of the expensive enzyme which is key to this method. Liquid-solid magnetically actuated extraction, filtration, sedimentation, and detection were all integrated on the same device. Several parameters were optimized including the concentration of enzyme, substrate, chromatic agent, and reaction time. In this environmental application of centrifugal microfluidics, the percent inhibition of enzyme activity is logarithmically proportional to the demonstration pesticide concentration (in this case carbofuran). This meant that as the pesticide concentration increased in the samples, the reaction was more inhibited and the final product absorbed less light at 525 nm. Two versions of the centrifugal microfluidic devices were made. One version was designed for the analysis of vegetable samples (cabbage) and the other for the analysis of soil samples. Each version provided results that were statistically similar to the conventional benchtop method with a carbofuran limit of detection of 0.1 ppm or 0.1 ?g g(-1) (5 ng absolute limit of detection). PMID:23865536

Duford, David A; Xi, Yongqing; Salin, Eric D

2013-08-20

146

Solid phase microextraction of pesticide residues from strawberries.  

Science.gov (United States)

A new solid phase microextraction method for the determination of pesticide residues in strawberries for 16 commonly used compounds was described. The strawberries were crushed and centrifuged. An aliquot of the well agitated aqueous supernatant (4 ml) was extracted with a fibre coated with polydimethylsiloxane (PDMS, 100 microns) for 45 min at room temperature. Identification and quantification were achieved using a gas chromatography-mass spectrometry (GC-MS) system and selective ion monitoring (SIM). The method was tested for the following pesticides: carbofuran, diethofencarb, penconazole, hexaconazole, metalaxyl, folpet, bromopropylate, dichlofluanid, alpha-endosulfan, beta-endosulfan, parathion ethyl, procymidone, iprodione, vinclozolin, myclobutanil and chlorothalonil. Limits of detection, repeatability and linearity for standard calibration in strawberries were obtained. Positive and negative effects of the matrix between the extracting solution of strawberries and water were observed. Stabilities of these compounds in the extracting solution of strawberries were determined. The solvent-free SPME procedure was found to be quicker and more cost effective than the solvent extraction methods commonly used. PMID:10492703

Hu, R; Hennion, B; Urruty, L; Montury, M

1999-03-01

147

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

Science.gov (United States)

A rapid method using programmed temperature vaporiser injection-low-pressure gas chromatography-high-resolution time-of-flight mass spectrometry (PTV-LP-GC-HR-TOF-MS) for the analysis of multiple pesticide residues in fruit-based baby food was developed. The fast and inexpensive buffered QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction method and "conventional" approach that employs ethyl acetate extraction followed by gel permeation chromatography (GPC) cleanup were employed for sample preparation. A PTV injector in solvent venting mode was used to reduce volume of acetonitrile and acetic acid (from the buffered QuEChERS extracts) that caused higher column bleed without their elimination. Otherwise, the time-to-digital converter would become saturated in HR-TOF-MS. For fast GC separation allowing analysis of 100 analytes within a 7 min runtime, both a high temperature programming rate and vacuum conditions in a megabore GC column were employed. The use of HR-TOF-MS allowed the unbiased identification and reliable quantification of target analytes through the application of a narrow mass window (0.02 Da) for extracting analyte ions and the availability of full spectral information even at very low levels. With only a few exceptions, the lowest calibration levels for the pesticides tested were foods and baby foods (2003/13/EC). PMID:18164024

Cajka, Tomas; Hajslova, Jana; Lacina, Ondrej; Mastovska, Katerina; Lehotay, Steven J

2008-04-01

148

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

Science.gov (United States)

...for residues of pesticides in or on food commodities. Further information...residues of the insecticide zeta-cypermethrin, in or on pistachio at 0.05 parts...measuring levels of cypermethrin in or on food with a limit of detection that...

2010-08-04

149

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.

2009-10-06

150

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; Otle?, Semih

2014-10-01

151

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

152

Catanionic surfactant ambient cloud point extraction and high-performance liquid chromatography for simultaneous analysis of organophosphorus pesticide residues in water and fruit juice samples.  

Science.gov (United States)

A mixed anionic-cationic surfactant cloud point extraction (CPE) has been developed using sodium dodecyl sulfate (SDS) and tetrabutylammonium bromide (TBABr) for the extraction and preconcentration of organophosphorus pesticides (OPPs) at ambient temperature before analysis by high-performance liquid chromatography. The studied OPPs were azinphos-methyl, parathion-methyl, fenitrothion, diazinon, chlorpyrifos, and prothiophos. The optimum conditions of the mixed anionic-cationic CPE were 50 mmol L(-1) SDS, 100 mmol L(-1) TBABr, and 10% (w/v) NaCl. The extracted OPPs were successfully separated within 11 min using the conditions of a Waters Symmetry C8 column, a flow rate of 0.8 mL min(-1), a gradient elution of methanol and water, and detection at 210 nm. Linearity was found over the range 0.05-5 ?g mL(-1), with the correlation coefficients higher than 0.996. The enrichment factor of the target analytes was in the range 6-11, which corresponds to their limits of detection from 1 to 30 ng mL(-1). High precisions (intra-day and inter-day) were obtained with relative standard deviation <1.5% (t(R)) and 10% (peak area). Accuracies (% recovery) of the different spiked OPP concentrations were 82.7-109.1% (water samples) and 80.3-113.3% (fruit juice samples). No contamination by the OPPs was observed in any studied samples. PMID:21744237

Seebunrueng, Ketsarin; Santaladchaiyakit, Yanawath; Soisungnoen, Phimpha; Srijaranai, Supalax

2011-09-01

153

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

Science.gov (United States)

...already granted for such residue. (14) Information concerning any maximum residue level established by the Codex Alimentarius Commission for the pesticide chemical residue addressed in the petition. If a Codex maximum residue level...

2010-07-01

154

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

155

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

156

Effect of background derivatization on the signal enhancement of pesticide residues extracted from edible oils.  

Science.gov (United States)

The effect of background derivatization on the signal enhancement of pesticide residues extracted from edible oil samples was studied by GC with negative chemical ionization MS. The analytes were extracted by a solvent extraction process, and the extract was subjected to rapid low-temperature fat precipitation. The residual fatty acids were silylated by derivatization with N,O-bis(trimethylsilyl)trifluoroacetamide. The chromatograms obtained from the derivatized samples showed higher signal intensity and lower detection levels when compared to the direct analysis without derivatization. The sensitivity levels of the method are either better or comparable to that of previously reported methodologies. The LODs of the analyzed organochlorine, organophosphorus, and synthetic pyrethroid residues in sunflower, rice bran, and ground oil samples were in the range of 0.02–0.5 ng/g, and the LOQs were in the range of 0.1–2 ng/g. The intraday and interday accuracies were in the range of 81–116% with RSDs less than 14%. The recoveries obtained were in the range of 53–89% with the RSD values less than 13% for all the studied pesticide residues. PMID:24132997

Deme, Pragney; Azmeera, Tirupathi; Bethala, Prabhavathi Devi L A; Jonnalagadda, Padmaja R; Rachapudi, Prasad B N; Upadhyayula, Vijaya Sarathi V R

2013-12-01

157

Monitoring of Some Pesticides Residue in Consumed tea in Tehran Market  

Digital Repository Infrastructure Vision for European Research (DRIVER)

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 group...

2013-01-01

158

Monitoring of some pesticides residue in consumed tea in Tehran market  

Digital Repository Infrastructure Vision for European Research (DRIVER)

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 group...

2013-01-01

159

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 prepa...

Mol, Hans G. J.; Rooseboom, Astrid; Dam, Ruud; Roding, Marleen; Arondeus, Karin; Sunarto, Suryati

2007-01-01

160

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

 
 
 
 
161

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

162

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

163

Analysis of pesticide residues in fruit and vegetables after cleanup with solid-phase extraction using ENV+ (Polystyrene-divinylbenzene) cartridges.  

Science.gov (United States)

A rapid and simple cleanup procedure for the existing multimethod using solid-phase extraction columns to measure pesticide concentrations in fruit and vegetables is presented. After extraction with ethyl acetate, the sample is passed through ENV+, polystyrene-divinylbenzene extraction column, and eluted with ethyl acetate and injected on to capillary GC columns connected to various detectors. The extraction column has the capacity to retain a broad range of pesticides and is widely used in environmental water samples. In this paper, the sample is extracted in an organic solvent. In contrast to what could be expected, it has been found that the column has the capacity to retain pesticides when used as the normal phase. PMID:10552525

Pihlström, T; Osterdahl, B G

1999-07-01

164

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

Directory of Open Access Journals (Sweden)

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

Md. Shakhaoat Hossain

2013-02-01

165

Evaluation of organophosphorus pesticide residues in citrus fruits from the Valencian community (Spain).  

Science.gov (United States)

Approximately 200 citrus samples from markets of the Valencian Community (Spain) were analyzed to establish their residue levels in 12 organophosphorus pesticide residues during the 1994-1995 campaign. The organophosphorus pesticides carbophenothion, chlorpyriphos, chlorfenvinphos, diazinon, ethion, fenitrothion, malathion, methidation, methylparathion, phosmet, quinalphos, and tetradifon were simultaneously extracted by matrix solid-phase dispersion and determined by gas chromatography-mass spectrometry using selected ion monitoring mode. A total of 32.25% contained pesticide residues and 6.9% exceeded the European Union Maximum Residue Levels (MRLs). The pesticides found in the samples with residues above MRLs were carbophenothion, ethion, methidathion, and methyl parathion. Lower level residues of these and the other pesticides studied (except diazinon) were frequently found. The estimated daily intake of the 12 organophosphorus pesticide residues during the studied period was 4.87 x 10(-4) mg/kg body weight/day. This value is lower than the provisional tolerances dairy intakes proposed by the Food and Agriculture Organization and the World Health Organization. PMID:9325585

Torres, C M; Picó, Y; Marín, R; Mañes, J

1997-01-01

166

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

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

2013-01-01

167

Status and effect of pesticide residues in soils under different land uses of Andaman Islands, India.  

Science.gov (United States)

Pesticides are shown to have a great effect on soil organisms, but the effect varies with pesticide group and concentration, and is modified by soil organic carbon content and soil texture. In the humid tropical islands of Andaman, India, no systematic study was carried out on pesticide residues in soils of different land uses. The present study used the modified QuEChERS method for multiresidue extraction from soils and detection with a gas chromatograph. DDT and its various metabolites, ?-endosulfan, ?-endosulfan, endosulfan sulfate, aldrin, and fenvalerate, were detected from the study area. Among the different pesticide groups detected, endosulfan and DDT accounted for 41.7 % each followed by aldrin (16.7 %) and synthetic pyrethroid (8.3 %). A significantly higher concentration of pesticide residues was detected in rice-vegetable grown in the valley followed by rice-fallow and vegetable-fallow in the coastal plains. Soil microbial biomass carbon is negatively correlated with the total pesticide residues in soils, and it varied from 181.2 to 350.6 mg?kg(-1). Pesticide residues have adversely affected the soil microbial populations, more significantly the bacterial population. The Azotobacter population has decreased to the extent of 51.8 % while actinomycetes were the least affected though accounted for 32 % when compared to the soils with no residue. PMID:23553417

Murugan, A V; Swarnam, T P; Gnanasambandan, S

2013-10-01

168

[Survey of pesticide residues in imported vegetable products (1992.4-2006.3)].  

Science.gov (United States)

Pesticide residues in 165 imported vegetable products on the Tokyo market from Apr. 1992 to Mar. 2006 were investigated. Seven kinds of pesticides were detected at levels between Tr (below 0.01 ppm) and 1.0 ppm from 16 samples. There was no sample in which pesticide residues exceeded the MRLs. The salt leaf of grape imported from Greece contained chlorpyrifos and quinalphos, and there was some doubt as to whether the residue levels exceeded the MRLs when the Japanese positive list system for pesticide residues in food was applied. Pesticides were detected from pickles and dehydrated vegetable, but not from products that had been treated with heat and water, such as boiled vegetables and purees. Many samples of products from Asia, and North America area contained detectable levels of pesticides. Residue levels of these pesticides were calculated as between 0.006 and 20.3% of their ADI values according to the daily intake of vegetable products. Therefore, these vegetable products should be safe when eaten in a normal manner. PMID:19602863

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

2009-06-01

169

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

Science.gov (United States)

...Docket No. FSIS-2010-0044] Codex Alimentarius Commission: Meeting of the...Pesticide Residues (CCPR) of the Codex Alimentarius Commission (Codex), which...Stuck, U.S. Manager for Codex Alimentarius. [FR Doc. 2011-1143...

2011-01-20

170

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

Science.gov (United States)

...Docket No. FSIS-2013-0012] Codex Alimentarius Commission: Codex Committee...Pesticide Residues (CCPR) of the Codex Alimentarius Commission (Codex), which...INFORMATION: Background The Codex Alimentarius (Codex) was established...

2013-03-14

171

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

Science.gov (United States)

...Docket No. FSIS-2011-0035] Codex Alimentarius Commission: Codex Committee...Pesticide Residues (CCPR) of the Codex Alimentarius Commission (Codex), which...Stuck, U.S. Manager for Codex Alimentarius. [FR Doc. 2012-1160...

2012-01-23

172

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

173

Pesticide residue dynamics in passion fruits: Comparing field trial and modelling results  

DEFF Research Database (Denmark)

We evaluated the exposure to pesticides from the consumption of passion fruits and subsequent human health risks by combining several methods: (i) experimental field studies including the determination of pesticide residues in/on passion fruits, (ii) dynamic plant uptake modelling, and (iii) human health risk assessment concepts. Eight commonly used pesticides were applied onto passion fruits cultivated in Colombia. Pesticide concentrations were measured periodically (between application and harvest) in whole fruits and fruit pulp. Measured concentrations were compared with predicted residues calculated with a dynamic and crop-specific pesticide uptake model, namely dynamiCROP. The model accounts for the time between pesticide application and harvest, the time between harvest and consumption, the amount of spray deposition on plant surfaces, uptake processes, dilution due to crop growth, degradation in plant components, and reduction due to food processing (peeling). Measured and modelled residues correspond well (r2=0.88â??0.99), with all predictions falling within the 90% confidence interval of the measured values. A mean error of 43% over all studied pesticides was observed between model estimates and measurements. The fraction of pesticide applied during cultivation that is eventually ingested by humans is on average 10â??4â??10â??6, depending on the time period between application and ingestion and the processing step considered. Model calculations and intake fractions via fruit consumption based on experimental data corresponded well for all pesticides with a deviation of less than a factor of 2. Pesticide residues in fruits measured at recommended harvest dates were all below European Maximum Residue Limits (MRLs) and therefore do not indicate any violation of international regulatory thresholds.

Juraske, Ronnie; Fantke, Peter

2012-01-01

174

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)

2008-02-01

175

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

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

2013-01-01

176

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

In this study, field trials on fine and coarse spray quality application of pesticides on apples were performed. The main objectives were to study the variation of pesticide residue levels in individual fruits versus composite samples, and the effect of standard fine spray quality application versus coarse spray quality application on residue levels. The applications included boscalid, bupirimate, captan, fenoxycarb, indoxacarb, pirimicarb, pyraclostrobin and thiophanate-methyl. Apples were c...

2012-01-01

177

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

Science.gov (United States)

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

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

2013-10-01

178

Determination of pesticide residues in honey by single-drop microextraction and gas chromatography.  

Science.gov (United States)

A novel, simple, and rapid single-drop microextraction (SDME) procedure combined with GC has been developed, validated, and applied for the determination of multiclass pesticide residues in honey samples. The SDME was optimized using a Plackett-Burman screening design considering all parameters that may influence an SDME procedure and a consequent central composite design to control the parameters that were found to significantly influence the pesticide determination. The developed analytical method required minimal volumes of organic solvents and exhibited good analytical characteristics with enrichment factors ranging from 3 for alpha-endosulfan to 10 for lindane, procymidone, and captan and method quantification limits ranging from 0.03 microg/kg for phosalone to 10.6 microg/kg for diazinon. The relative recoveries obtained ranged from 70.8% for captan to 120% for fenarimol, and the precision (RSD) ranged from 3 to 15%. The proposed SDME procedure followed by GC with an electron capture detector for quantification and GC/MS for identification was applied with success to the analysis of 17 honey samples. Monitoring results indicated a low level of honey contamination by diazinon, chlorpyrifos-ethyl, procymidone, bromopropylate, and endosulfan (alpha-, beta-, and endosulfan sulfate) residues that were far below the maximum residue limit values specified by the European Union for endosulfan (10 microg/kg) and bromopropylate (100 microg/kg) in honey samples. PMID:21563700

Tsiropoulos, Nikolaos G; Amvrazi, Elpiniki G

2011-01-01

179

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

180

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

 
 
 
 
181

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.

2013-01-01

182

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

183

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

184

Monitoring of pesticide residues in Egyptian fruits and vegetables during 1996.  

Science.gov (United States)

Samples of the most common fruits and vegetables were collected from 8 local markets in 6 governorates. These 1,579 samples were analyzed for residues of 53 pesticides, which included organophosphorus and organonitrogen compounds and some synthetic pyrethroids. Samples were also analyzed for residues of organochlorine pesticides, although they had been prohibited from use several years ago. Only 510 of the 1,579 samples were analyzed for dithiocarbamate pesticide residues, which were determined as CS2. Overall, 76.1 % of the total analyzed samples had no detectable residues, 23.9% contained detectable residues, and 2.59% contained residues that exceeded maximum residue limits. For individual crops, contaminated samples ranged from 0 to 96% of the number of samples analyzed. However, the highest violative percentage for samples of individual crops was 12.5. Chlorpyrifos, carbaryl, dimethoate, bromopropylate, and profenofos were the violative pesticides determined in fruit and vegetable samples. The results of the current study demonstrated that no restricted or banned pesticides such as DDT, HCH, and their isomers were found in any of the samples analyzed. Dithiocarbamate residues were detected in 9.4% of the 510 samples analyzed, with a violative percentage of 0.39, representing one grape sample and one peach sample. PMID:11324620

Dogheim, S M; Gad Alla, S A; El-Marsafy, A M

2001-01-01

185

Microcomputer programming in basic for the evaluation of capillary gas chromatography in the analysis of pesticide residues. I. MATRIXCOMP--a program that facilitates the recognition of interfering peaks from the biological matrix.  

Science.gov (United States)

Chromatograms of pesticide residues in food include peaks produced by pesticides and matrix compounds. Pesticide peaks are recognized by means of relative retention times and response factors; two detectors are used and internal standard methods are applied. Chromatograms of reference samples for all types of food are stored as raw data in a reduced format, together with tables of all chromatographic data for the matrix compounds. MATRIXCOMP provides the analyst with the chromatograms of the actual sample and the reference in parallel on a visual display screen for visual comparison. Simultaneously, the relevant chromatographic data for the sample, the reference and the calibration tables are displayed on a second screen page in a condensed form. PMID:3841352

Stan, H J; Lipinski, J

1985-12-01

186

Determination of pesticide residue in selected fruits and vegetable  

International Nuclear Information System (INIS)

Food contamination due to indiscriminate use of pesticides has become a serious problem. Fruits samples of tomato, grapes, musk melon, parsimen and vegetable samples of potato, pea, spinach, cabbage and pumpkin ere collected from local market of Peshawar, coming from different regions. All samples were extracted, purified and analyzed for the commonly used pesticides. Dichlorovas, BHC, Atrazine, Daizinon, Methadiathion and Cypermethrin were detected by Gas Chromatography. These pesticides were detected in vegetable samples Id Atrazine were found in potato sample and not detected in other samples. Large concentration of Cypermethrin (44.6) was detected in the pea sample. All the vegetables samples have maximum concentration of pesticides, which is higher than their MRLs, but in pumpkin no one of the above pesticides were detected. In fruits samples, dichlorovas, atrazine, diazinon, methadiathion. Cypermethrin were detected. BHC was not present in fruits samples. All these pesticides were above the MRLs. The study concluded that agriculture crops are highly contaminated due to the uncontrolled use of pesticides in project area and suggested that pesticides should be applied in calculated dose to avoid resistance and persistence due to over and under dose application. (author)

2004-06-07

187

Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate: collaborative study.  

Science.gov (United States)

A collaborative study was conducted to determine multiple pesticide residues in fruits and vegetables using a quick, simple, inexpensive, and effective sample preparation method followed by concurrent analysis with gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/ tandem mass spectrometry (LC/MS/MS). For short, the method is known as QuEChERS, which stands for quick, easy, cheap, effective, rugged, and safe. Twenty representative pesticides were fortified in 3 matrixes (grapes, lettuces, and oranges) at 3 duplicate levels unknown to the collaborators ranging from 10 to 1000 ng/g. Additionally, 8 incurred pesticide residues were determined. Thirteen laboratories from 7 countries provided results in the study, and a variety of different instruments were used by collaborators. The QuEChERS procedure simply entails 3 main steps: (1) a 15 g homogenized sample is weighed into a 50 mL centrifuge tube to which 15 mL acetonitrile containing 1% HOAc is added along with 6 g MgSO4 and 1.5 g NaOAc, and the tube is shaken and centrifuged; (2) a portion of the extract is mixed with 3 + 1 (w/w) MgSO4-primary secondary amine sorbent (200 mg/mL extract) and centrifuged; and (3) the final extract is analyzed by GC/MS and LC/MS/MS. To detect residues kresoxim-methyl (9.2 +/- 3.2 ng/g) and cyprodinil (112 +/- 18) were found in the grapes; permethrins (112 +/- 41), lamda-cyhalothrin (58 +/- 11), and imidacloprid (12 +/- 2) were determined in the lettuces; and ethion (198 +/- 36), thiabendazole (53 +/- 8), and imazalil (13 +/- 4) were determined in the oranges. Chlorpyrifosmethyl (200 ng/g) was used as a quality control standard added during sample homogenization and yielded 86% recovery and 19% RSD(R). Intralaboratory repeatabilities for the method averaged 9.8% RSD for all analytes. The results demonstrate that the method is fit-for-purpose to monitor many pesticide residues in fruits and vegetables, and the Study Director recommends that it be adopted Official First Action. PMID:17474521

Lehotay, Steven J

2007-01-01

188

Pesticide residues in raspberries (Rubus idaeus L.) and dietary risk assessment.  

Science.gov (United States)

The aim of this study was to evaluate the residues of 140 pesticides in raspberries from north-eastern Poland (2005-2010). Gas chromatography with electron capture detector (GC-ECD) and nitrogen phosphorous detector (GC-NPD) was used. Among the 128 samples, 66 (51.6%) were found to detect residues: 14.1% contained one pesticide and around 38% multiple pesticide residues. The most frequently detected were pyrimethanil residues (36.0%). Twenty-seven (21.1%) raspberry samples exceeded the maximum residue limits. The estimated daily intakes ranged from 0.003% to 3.183% of the acceptable daily intake (ADI) for adults 0.008% and 9.7% for toddlers, respectively. The most critical case is procymidone, the acute risk was 180.9% of acute reference dose (ARfD) for toddlers and for adults (83% of ARfD) which is high. PMID:24779781

Lozowicka, B; Kaczy?ski, P; Jankowska, M; Rutkowska, E; Hrynko, I

2012-09-01

189

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 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

190

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

Science.gov (United States)

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

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

2014-06-01

191

Pesticide residues in grapes from vineyards included in integrated pest management in Slovenia.  

Science.gov (United States)

Although the list of pesticides used in integrated pest management (IPM) in grape growing and their annual application rates are limited, we are still confronted with the problem of pesticide residues in grapes. This paper presents the results of pesticide monitoring of 47 samples of wine grapes (Vitis vinifera L.) from the 2006 vintage from vineyards included in IPM. The grape samples were analysed for the presence of 67 pesticides. Among them 20 were allowed in IPM in 2006. Grapes were sampled at harvest. Two internal analytical methods were used for the determination of pesticides: gas chromatography-mass spectrometry (GC-MS) method for the determination of dithiocarbamates and a multi-residue GC-MS method. One grape sample (2.1%) contained no residues or they were below the limit of detection, 28 samples (59.6%) contained residues lower or equal than maximum residue levels (MRLs), and 18 samples (38.3%) exceeded national MRLs for cyprodinil (the concentration range was 0.03-0.40 mg kg(-1) of cyprodinil) and fludioxonil (concentration was 0.03 mg kg(-1) of fludioxonil). Multiple residues were found in 41 samples (87.2%). The highest number of pesticides detected per sample was seven. No violation of pesticides allowed in IPM was observed. Folpet (97.9%), cyprodinil (51.1%), dithiocarbamates (44.7%), chlorothalonil (23.4%), chlorpyriphos (19.1%) and pyrimethanil (14.9%) were the most frequently found pesticides in grapes. Risk assessment showed that the exceeded concentrations of cyprodinil and fludioxonil did not represent any risk for consumer's health (the national estimate of short-term intake as a percentage of the acceptable daily intake was below 100%). PMID:18348043

Cesnik, H Basa; Gregorcic, A; Cus, F

2008-04-01

192

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 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

1996-07-01

193

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

Science.gov (United States)

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

Young, S J; Kamps, L R

1982-07-01

194

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

195

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

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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

196

Pesticide residues determination in Polish organic crops in 2007-2010 applying gas chromatography-tandem quadrupole mass spectrometry.  

Science.gov (United States)

A sensitive, accurate and reliable multiresidue method based on the application of gas chromatography-tandem quadrupole mass spectrometry (GC-QqQ-MS/MS) has been established for screening, identification and quantification of a large number of pesticide residues in produce. The method was accredited in compliance with PN-EN ISO/IEC 17025:2005 standard and it was operated under flexible scope as PB-11 method. The flexible scope of accreditation allowed for minor modifications and extension of the analytical scope while using the same analytical technique. During the years 2007-2010, the method was used for the purpose of verification of organic crop production by multiresidue analysis for the presence of pesticides. A total of 528 samples of differing matrices such as fruits, vegetables, cereals, plant leaves and other green parts were analysed, of which 4.4% samples contained pesticide residues above the threshold value of 0.01 mg/kg. A total of 20 different pesticide residues were determined in the samples. PMID:23561134

Walorczyk, Stanis?aw; Dro?d?y?ski, Dariusz; Kowalska, Jolanta; Remlein-Starosta, Dorota; Zió?kowski, Andrzej; Przewo?niak, Monika; Gnusowski, Bogus?aw

2013-08-15

197

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

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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

198

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

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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

199

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

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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

200

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

 
 
 
 
201

[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

202

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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 ...

Puneeta Pandey; Khillare, P. S.; Krishan Kumar

2011-01-01

203

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

204

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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 ...

Aiyesanmi, Ademola F.; Idowu, Gideon A.

2012-01-01

205

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

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Full Text Available A variety of pesticides is used in alfalfa field to control pests. Biological control agents are also used to control these pests, therefore it is important to understand the effects of such pesticides on these beneficial insects. The present study was carried out to examine the residual effects of Dursban and Fenvalerate as conventional pesticides as well as Bio-Fly and Bio-Neem as biorational pesticides on ladybird beetle, Adonia variegata Goeze using panel exposure technique. Dursban was highly toxic to ladybird beetles at ?, 1 and 2 folds of the recommended dosages, where mortality percentages ranging from 46.7-50, 50 and 55-55.33%, respectively during the period of 1-120 h. Fenvalerate produced moderate toxic effects on the coccinellids, where mortality percentages were 10-47.7, 20-50 and 13.33-50% following the residual exposure of ?, 1 and 2 folds of the recommended dosages. On the other hand, the biorational pesticides Bio-Neem and Bio-Fly showed slight toxicity of a maximum of 10% mortality, produced after 5-day exposure of their recommended and half the recommended dosages. When the dose was doubled the toxicity of Bio-Fly did not increase, however, that of Bio-Neem reached 26.7 after 5 days. It can be concluded that in IPM programs, the application of conventional pesticides must be considered carefully for use, whereas biorational pesticides can be used with natural enemies with minimum effects.

Mohammed A. Al-Doghairi

2004-01-01

206

Pesticide residue level in tea ecosystems of Hill and Dooars regions of West Bengal, India.  

Science.gov (United States)

In the present study we quantified the residues of organophosphorus (e.g. ethion and chlorpyrifos), organochlorine (e.g. heptachlor, dicofol, alpha-endosulfan, beta-endosulfan, endosulfan sulfate) and synthetic pyrethroid (e.g. cypermethrin and deltamethrin) pesticides in made tea, fresh tea leaves, soils and water bodies from selected tea gardens in the Dooars and Hill regions of West Bengal, India during April and November, 2006. The organophosphorus (OP) pesticide residues were detected in 100% substrate samples of made tea, fresh tea leaves and soil in the Dooars region. In the Hill region, 20% to 40% of the substrate samples contained residues of organophosphorus (OP) pesticides. The organochlorine (OC) pesticide residues were detected in 33% to 100% of the substrate samples, excluding the water bodies in the Dooars region and 0% to 40% in the Hill region. The estimated mean totals of studied pesticides were higher in fresh tea leaves than in made tea and soils. The synthetic pyrethroid (SP) pesticide residues could not be detected in the soils of both the regions and in the water bodies of the Dooars. Sixteen percent and 20% of the made tea samples exceeded the MRL level of chlorpyrifos in Dooars and Hill regions respectively. The residues of heptachlor exceeded the MRL in 33% (April) and 100% (November) in the Dooars and 40% (April) and 20% (November) in the Hill region. Based on the study it was revealed that the residues of banned items like heptachlor and chlorpyrifos in made tea may pose health hazards to the consumers. PMID:18286381

Bishnu, Avhik; Chakrabarti, Kalyan; Chakraborty, Ashis; Saha, Tapan

2009-02-01

207

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

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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

208

Effect of household and industrial processing on the levels of pesticide residues and degradation products in melons.  

Science.gov (United States)

Two varieties of melons (Cucumis melo) were treated with two fungicides (carbendazim and maneb) and four insecticides (acetamiprid, cyromazin, imazalil and thiamethoxam) to quantify the effect of household processing on the pesticide residues. To ensure sufficiently high levels of residues in flesh and peel, the most concentrated formulations were applied observing good agricultural practice. The peeling step decreased the concentration of pesticide residues for maneb, imazalil and acetamiprid by more than 90%. Cyromazin, carbendazim and thiamethoxam were reduced by approximately 50%. The reduction of the pesticides could not be fully explained by the systemic character of the pesticides. However, the agricultural practices (time of application), solubility and mode of action (systemic versus contact pesticide) of the pesticides could be used to explain the difference in processing factors for the studied pesticides. Degradation products (melamine and ethylenethiourea) were also investigated in this study, but were not detected. PMID:22489844

Bonnechère, A; Hanot, V; Bragard, C; Bedoret, T; van Loco, J

2012-01-01

209

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

210

Analysis of pesticide residues using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) pesticide multiresidue method in traditional Chinese medicine by gas chromatography with electron capture detection.  

Science.gov (United States)

The Quick Easy Cheap Effective Rugged and Safe multiresidue method (QuEChERS) has been validated for the extraction of 15 organochlorine pesticides (OCPs) in completely different matrices of traditional Chinese medicine (TCM). The method employed a rapid, simple and cost-effective procedure. The spiking levels for the recovery experiments were 0.1, 0.5 and 2.0 mg kg(-1). Mean recoveries mostly ranged between 76.0% and 114.0% (96.0% on average), and relative standard deviations (RSD) were generally below 10% (4.72% on average). Based on these results, the methodology has been proven to be highly efficient and robust and thus suitable for monitoring the MRL compliance of a wide range of commodity. The contamination status of 15 OCPs on 80 different TCMs marketed in China, and a total of 400 samples were also performed using a previously validated method. 15 OCPs were benzene hexachloride (BHC, including ?-BHC, ?-BHC, ?-BHC, ?-BHC), hexachlorobenzene, heptachlor, heptachlor epoxide, aldrin, p, p'-DDE, p, p'-DDD, o, p'-DDT, p, p'-DDT, mirex, endrin, dieldrin. This study indicates that the proposed method is useful for analyzing OCPs in TCM. PMID:21741067

Xu, Rong; Wu, Jianwei; Liu, Yougang; Zhao, Runhuai; Chen, Bo; Yang, Meihua; Chen, Jun

2011-08-01

211

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

Science.gov (United States)

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

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

2013-10-01

212

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

213

[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

214

Monitoring the Residue Level of Three Selected Pesticides in Red Amaranth  

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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 ?...

Jahan Ara Khatoon; Md. Shariful Islam; Nur Mohammad Talukder; Md. Afzal Hossain

2004-01-01

215

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

216

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

International Nuclear Information System (INIS)

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

1982-06-11

217

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

Science.gov (United States)

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

Stoner, Kimberly A.; Eitzer, Brian D.

2013-01-01

218

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

Science.gov (United States)

Analysis of pollen trapped from honey bees as they return to their hives provides a method of monitoring fluctuations in one route of pesticide exposure over location and time. We collected pollen from apiaries in five locations in Connecticut, including urban, rural, and mixed agricultural sites, for periods from two to five years. Pollen was analyzed for pesticide residues using a standard extraction method widely used for pesticides (QuEChERS) and liquid chromatography/mass spectrometric analysis. Sixty pesticides or metabolites were detected. Because the dose lethal to 50% of adult worker honey bees (LD50) is the only toxicity parameter available for a wide range of pesticides, and among our pesticides there were contact LD50 values ranging from 0.006 to >1000 ?g per bee (range 166,000X), and even among insecticides LD50 values ranged from 0.006 to 59.8 ?g/bee (10,000X); therefore we propose that in studies of honey bee exposure to pesticides that concentrations be reported as Hazard Quotients as well as in standard concentrations such as parts per billion. We used both contact and oral LD50 values to calculate Pollen Hazard Quotients (PHQ = concentration in ppb ÷ LD50 as ?g/bee) when both were available. In this study, pesticide Pollen Hazard Quotients ranged from over 75,000 to 0.01. The pesticides with the greatest Pollen Hazard Quotients at the maximum concentrations found in our study were (in descending order): phosmet, Imidacloprid, indoxacarb, chlorpyrifos, fipronil, thiamethoxam, azinphos-methyl, and fenthion, all with at least one Pollen Hazard Quotient (using contact or oral LD50) over 500. At the maximum rate of pollen consumption by nurse bees, a Pollen Hazard Quotient of 500 would be approximately equivalent to consuming 0.5% of the LD50 per day. We also present an example of a Nectar Hazard Quotient and the percentage of LD50 per day at the maximum nectar consumption rate. PMID:24143241

Stoner, Kimberly A; Eitzer, Brian D

2013-01-01

219

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

International Nuclear Information System (INIS)

A study was done on the speciation and analysis of organochlorine pesticides in sediment collected from coastal water of Peninsular Malaysia along the Straits of Malacca, namely the coastal water areas of Kedah, Perlis and Perak. Sediment samples were collected using a box coring device at four stations in coastal waters along the Muda rice granary area and four other stations outside the area. The main objective of the study was to monitor the level of contamination by compounds that have been used to control pests particularly in rice granary areas. The detection and quantification of the compounds were done with the GC-ECD. The capability of the method used was examined by analysis of Standard Reference Material obtained from NIST, USA. The mean concentrations of organochlorine pesticide compounds in the coastal water area along the Muda area was 11.17 ± 3.76 ng/g, dry weight (range 7.64-19.86 ng/g, dry weight) whilst those in other areas was 4.14 ± 1.36 ng/g, dry weight (range 2.29-5.10 ng/g, dry weight). The average concentration of the DDT group in the Muda area was 4.22 ± 2.39 ng/g, dry weight, whilst the non-DDT group was 6.94 ± 2.01 ng/g, dry weight. Outside the Muda area, the average concentration of the DDT group was 1.26 ± 0.58 ng/g, dry weight. The non-DDTgroup had a mean concentration of 2.88 ± 0.80 ng/g, dry weight. Even though the concentration of the organochlorinated pesticides in the Muda area was higher, it was still lower than levels reported worldwide. For example, at the Gulf of Mexico (range DDT<0.02-454.00 ng/g, dry weight), Arabian Sea (range DDT 7.4-179.1 ng/g), Gulf of Bengal (range DDT<0.22-720.0 ng/g, dry weight) and Colombian Caribbean (range DDT 38.0-266.0 ng/g, dry weight). Being aware of the sensitivity of marine life, especially crustacean to organochlorines and ensuring the sustainability of rice production in the Muda area, continued monitoring of the level of pesticides residues of the coastal water of the Muda granary area should be undertaken, lack of which could be damaging to the marine ecosystem as the compounds are persistent in the environment. (Author)

2002-01-01

220

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

 
 
 
 
221

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; Hansen, H.K.

2007-01-01

222

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

Science.gov (United States)

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

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

2012-09-01

223

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

Science.gov (United States)

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

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

2006-01-01

224

Pesticide residue analysis in foodstuffs applying capillary gas chromatography with atomic emission detection state-of-the-art use of modified multimethod S19 of the Deutsche forschungsgemeinschaft and automated large-volume injection with programmed-temperature vaporization and solvent venting.  

Science.gov (United States)

Atomic emission detection (AED) provides high element-specific detection of all compounds amenable to gas chromatography (GC). The heteroatoms nitrogen, chlorine, phosphorus, sulfur, bromine and fluorine, which are important elements in pesticide residue analysis, are of major interest. A main drawback of AED is its lower sensitivity with respect to other selective detection methods used in pesticide residue analysis such as electron-capture and nitrogen-phosphorus detection. This holds true especially for the important nitrogen trace. For this reason, more sensitive detection can be achieved by injection of larger volumes or higher concentrations of sample extracts, because matrix compounds were usually registered only in the carbon, hydrogen and oxygen traces. This paper focuses on recent developments from the authors' laboratory in order to demonstrate the feasibility of screening analyses with the identification of pesticide residues down to the 0.01 ppm concentration level in plant foodstuffs. This has been achieved by means of automated large volume injection with programmed-temperature vaporization and solvent venting as well as careful optimization of make-up and reactant gases with AED. Clean up follows the principle of multimethod S19 of the Deutsche Forschungsgemeinschaft in a reduced procedure. After elimination of lipids and waxes by gel permeation chromatography, extracts from 10 g of the food samples were concentrated to 200 microliters, of which 12.5 microliters were introduced into the GC-AED system. Two analyses were usually performed with the element traces of sulfur, phosphorus, nitrogen and carbon in the first run and chlorine and bromine in the second run. Fluorine and oxygen were not detected in any screening analyses. The method has proved to be of great value especially with "problem foodstuffs". The limits of detection were determined for 385 pesticides and are presented together with their retention data. PMID:8938393

Stan, H J; Linkerhägner, M

1996-10-25

225

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

226

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

Science.gov (United States)

The detection and quantification of different pesticides in the goat milk samples collected from different localities of Faisalabad, Pakistan was performed by HPLC using solid phase microextraction. The analysis showed that about 50% milk samples were contaminated with pesticides. The mean±SEM levels (ppm) of cyhalothrin, endosulfan, chlorpyrifos and cypermethrin were 0.34±0.007, 0.063±0.002, 0.034±0.002 and 0.092±0.002, respectively; whereas, methyl parathion was not detected in any of the analyzed samples. Quantitative structure activity relationship (QSAR) models were suggested to predict the residues of unknown pesticides in the goat milk using their known physicochemical characteristics including molecular weight (MW), melting point (MP), and log octanol to water partition coefficient (Ko/w) in relation to the characteristics such as pH, % fat, specific gravity and refractive index of goat milk. The analysis revealed good correlation coefficient (R2 = 0.985) for goat QSAR model. The coefficients for Ko/w and refractive index for the studied pesticides were higher in goat milk. This suggests that these are better determinants for pesticide residue prediction in the milk of these animals. Based upon the determined pesticide residues and their provisional tolerable daily intakes, risk analysis was also conducted which showed that daily intake levels of pesticide residues including cyhalothrin, chlorpyrifos and cypermethrin in present study are 2.68, 5.19 and 2.71 times higher, respectively in the goat milk. This intake of pesticide contaminated milk might pose health hazards to humans in this locality. PMID:23369514

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

2013-01-01

227

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

228

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

229

Assessment of pesticide residues in Karabo?az Lake from K?z?l?rmak Delta, Turkey.  

Science.gov (United States)

Monitoring of pesticide residues in water and sediments was conducted for the coastal shallow Karabo?az Lake, northern Turkey. During a one-year study period, eight pesticides (malathion, etofenprox, molinate, oxamyl, propamocarb hydrochloride, tebufenozide, linuron, piperonyl butoxide) were detected in water and in sediments, all at ?g/L and ?g/kg concentrations, respectively. Temporal variation in pesticide concentrations was observed. Highest pesticide concentrations in water and sediment were from tebufenozide and etofenprox, respectively. Aquatic risk assessments revealed that out of eight pesticides detected, three showed unaccaptable risk: malathion, oxamyl and etofenprox. PMID:23775316

Yurtkuran, Zeynep; Sayg?, Yasemin

2013-08-01

230

Effect of home processing on the distribution and reduction of pesticide residues in apples.  

Science.gov (United States)

The effect of home processing (washing, peeling, coring and juicing) on residue levels of chlorpyrifos, ?-cypermethrin, tebuconazole, acetamiprid and carbendazim in apple segments was investigated. The pesticide residues were determined by UPLC-MS/MS and GC with a flame photometric (FPD) and electron capture detection (ECD). The results indicated that the pesticide residue levels in the apple peel and core were higher compared with in the apple flesh. After peeled and cored apple was processed into apple juice and pomace, chlorpyrifos, ?-cypermethrin and tebuconazole were concentrated in the apple pomace. However, residues of acetamiprid and carbendazim were exceptions. The apple pomace was free of acetamiprid, which was mainly present in the apple juice. After washing the mean loss of chlorpyrifos, ?-cypermethrin, tebuconazole, acetamiprid and carbendazim from apples under recommended dosage and twofold higher dosage were 17-21%, 6.7-7.1%, 13-32%, 42-67% and 47-50%, respectively. The pesticide residues were significantly reduced in the edible part of the apple except for ?-cypermethrin during peeling and coring process. The removal effect of apple juicing was found to be the most pronounced on ?-cypermethrin residue, which was reduced in the range of 81-84%, and the reductions of chlorpyrifos, tebuconazole, acetamiprid and carbendazim upon apple juicing were in the range of 15-36%. PMID:22738391

Kong, Z; Shan, W; Dong, F; Liu, X; Xu, J; Li, M; Zheng, Y

2012-08-01

231

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

Science.gov (United States)

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

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

2014-08-01

232

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.

2012-04-01

233

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

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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

234

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 ...

235

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

DEFF Research Database (Denmark)

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

Poulsen, Mette E.; Wenneker, Marcel

2012-01-01

236

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

237

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

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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

238

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

International Nuclear Information System (INIS)

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

2005-04-01

239

Assessment of the impact of pesticide residues on microbiological and biochemical parameters of tea garden soils in India.  

Science.gov (United States)

The main aim of this study was to assess the impact of pesticidal residues on soil microbial and biochemical parameters of the tea garden soils. The microbial biomass carbon (MBC), basal (BSR) and substrate induced respirations (SIR), beta-glucosidase activity and fluorescein diacetate hydrolyzing activity (FDHA) of six tea garden soils, along with two adjacent forest soils (control) in West Bengal, India were measured. The biomass and its activities and biochemical parameters were generally lower in the tea garden soils than the control soils. The MBC of the soils ranged from 295.5 to 767.5 micro g g(- 1). The BSR and SIR ranged from 1.65 to 3.08 mu g CO2-C g(- 1) soil h(- 1) and 3.08 to 10.76 micro g CO2-C g(- 1)h(- 1) respectively. The beta-glucosidase and FDHA of the soils varied from 33.3 and 76.3 micro g para-nitrophenol g(- 1) soil h(- 1) and 60.5 to 173.5 micro g fluorescein g(- 1)h(- 1)respectively. The tea garden soils contained variable residues of organophosphorus and organochlorine pesticides, which negatively affected the MBC, BSR, SIR, FDHA and beta -glucosidase activity. Ethion and chlorpyriphos pesticide residues in all the tea garden soils varied from 5.00 to 527.8 ppb and 17.6 to 478.1 ppb respectively. The alpha endosulfan, beta endosulfan and endosulfan sulfate pesticide residues in the tea garden soils ranged from 7.40 to 81.40 ppb, 8.50 to 256.1 ppb and 55 to 95.9 ppb respectively. Canonical correlation analysis shows that 93% of the total variation was associated with the negative impact of chlorpyriphos, beta and alpha endosulfan and endosulfan sulfate on MBC, BSR and FDHA. At the same time ethion had negative impact on SIR and beta-glucosidase. Data demonstrated that the pesticide residues had a strong impact on the microbial and biochemical components of soil quality. PMID:18941998

Bishnu, A; Saha, T; Mazumdar, D; Chakrabarti, K; Chakraborty, A

2008-11-01

240

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

Directory of Open Access Journals (Sweden)

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

B Shabankhani

2006-01-01

 
 
 
 
241

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

Directory of Open Access Journals (Sweden)

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

Yawar Latif

2012-08-01

242

A rapid spectrophotometric assay of some organophosphorus pesticide residues in vegetable samples  

Science.gov (United States)

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

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

2007-08-01

243

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)

2008-01-01

244

Applicability of some mass spectrometric criteria for the confirmation of pesticide residues.  

Science.gov (United States)

This study was initiated to demonstrate the impact of tolerance intervals calculated based on experimental data and standard criteria on the capability to detect and identify pesticide residues by GC-MS in plant extract. The tolerance intervals specified by the current guidelines and standards (EU, EPA, ISO, EC) result in a large number of false negative values. The tolerance intervals calculated based on the actually measured ion ratios at 2 different probability levels did not provide a better estimate. Based on experimental findings a 2-phase procedure for confirmation of pesticide residues is recommended. The first screening phase comprises identification of those pesticide residues that are likely to be present avoiding false negatives as far as possible. Relatively large tolerance intervals, +/-30% of absolute ion abundances ratios, have to be used at this point. When 2 or 3 selected ion ratios are within the established tolerance intervals the residue is confirmed. When the ions detected still indicate the possible presence of a residue the result may be reported as tentatively identified. However, when the result would lead to regulatory action, second confirmatory phase has to be undertaken. This can be achieved with the same GC-MS equipment, by injecting matrix-matched standards of the suspected analyte, in order to compensate for matrix influence on ion ratios. Alternatively, methods using different physico-chemical properties of the compound have to be used. The choice of the technique depends on their availability, time and cost. PMID:15508043

Soboleva, Eugenia; Ahad, Karam; Ambrus, Arpád

2004-11-01

245

Residues and enantiomeric profiling of organochlorine pesticides in sediments from Xinghua Bay, southern East China Sea.  

Science.gov (United States)

The spatial distribution and chiral signatures of organochlorine pesticides (OCPs) in the surface sediments of Xinghua Bay, southern East China Sea, were investigated. The total OCP concentrations ranged from 9.15 to 40.5 ng/g dry weight, with a predominance of hexachlorocyclohexanes (HCHs) and dichlorodiphenyltrichloroethanes (DDTs). The isomer ratios of ?-HCH/?-HCH (less than 1.0) and the predominant ?-HCH implied that HCH residues were derived not only from historical technical HCH use but also from the additional use of lindane in this area. The isomer ratios of p,p'-DDT/(p,p'-DDD + p,p'-DDE) and o,p'-DDT/p,p''-DDT, and a strong correlation (R = 0.83, P dicofol-type DDT and technical DDT. Moreover, the fact that only cis-chlordane was detectable for all sampling stations suggested the past application of technical chlordane. Based on the sediment quality guidelines (SQG), ?-HCH is the main OCP species of ecotoxicological concern in Xinghua Bay. Enantiomeric analysis showed that the (+)-enantiomers of ?-HCH and o,p'-DDT were more prevalent than the (-)-enantiomers in most samples, whereas both racemic and nonracemic residues existed for o,p'-DDD. These results implied that the SQG of chiral OCPs should be reassessed using concentrations of their individual enantiomers. PMID:24328544

Xue, Bin; Tang, Qiao Z; Jin, Mei Q; Zhou, Shan S; Zhang, Hai S

2014-01-01

246

Analysis of organochlorine pesticide residues in human and cow's milk in the towns of Asendabo, Serbo and Jimma in South-Western Ethiopia.  

Science.gov (United States)

The level of some OCPs in human and cow milk collected from Asendabo, Serbo and Jimma in South-West Ethiopia were analyzed using GC-ECD. Results of the analysis indicated that all samples contained detectable quantities of p,p'-DDT and its metabolites, p,p-DDE and p,p-DDD, but none of the other OCPs analyzed. Mean levels of total DDT in the human and cow milk samples in the three areas were 12.68 and 0.389 ?g g(-1) respectively. The distributions of p,p-DDT, p,p-DDE and p,p-DDD in the human milk samples from the three locations followed the same trend in which the proportion of p,p-DDT was the highest in all the three cases, comprising 55-71% of total DDT, followed by p,p-DDE, 26-39%, and the least, p,p-DDD of 2-5%. The mean ratio of DDT/DDE concentration for the three areas was calculated to be 2.01. This value was much higher than the values reported from other countries in earlier studies and indicates the existence of a higher quantity of DDT from a fresh input in the three study areas. The mean estimated daily intake of DDT by infants from mother's milk in the three locations was found to be 62.17 ?g kg(-1) body weight, which is about three times higher than the acceptable daily intake set by WHO/FAO for total DDT, 20 ?g kg(-1) of body weight. This alarmingly high daily intake value is a cause for concern, since children are highly susceptible to effects from such environmental contaminants. The study has revealed that people in the study areas are facing exposure to DDT from recent use. The observed contamination of mother's milk and the possible transfer of the contaminant from mother to child is an obvious risk associated with breast-feeding in the study areas and possibly in other parts of the country too. PMID:23062941

Gebremichael, Sosina; Birhanu, Tarekegn; Tessema, Dejene A

2013-02-01

247

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

Science.gov (United States)

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

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

2011-01-01

248

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

Science.gov (United States)

The positive list system became effective from May 29, 2006 to improve the regulation of residual agricultural chemicals (pesticides, feed additives and veterinary drugs) in foods. In accordance with the system, we investigated pesticide residues in 50 agricultural products purchased in Morioka city from March to November 2006. Analyses were performed according to the "Multiresidue Method for Agricultural Chemicals by GC/MS", the Notice of the Ministry of Health, Labour and Welfare. Five pesticides and two non-agricultural chemicals were detected from 16 samples. Ortho-phenylphenol (OPP) was detected from 8 samples: immature pea, snap bean, kiwi, plain-boiled bamboo shoot, mango, white asparagus, lemon and domestic shiitake mushroom. Maximum residue limits (MRLs) have not been established for these products, and they exceeded the uniform level of 0.01 ppm. DDT was detected from Philippines banana (0.30 ppm) and Korean paprika (0.45 ppm). The residual level in Philippines banana was lower than the MRL, but Korean paprika exceeded its MRL. Chlorpyrifos, Thiabendazole and Imazaril were detected from citrus imported from the U.S.A., but their residue levels were lower than the respective MRLs. Aniline and 2-pyrrolidone were detected from several imported products. These two may not be regulated by the positive list system because they are not agricultural chemicals, although their derivatives are used as pesticides or veterinary drugs. Three problems have been revealed from this survey: 1) application of the uniform level to minor agricultural products, 2) residues of non-agricultural chemicals whose toxicity is uncertain, 3) metabolites of agricultural chemicals, which are also regulated by the positive list system, have not been clearly defined. PMID:17538241

Iwasaki, Mariko; Sato, Itaru; Jin, Yihe; Saito, Norimitsu; Tsuda, Shuji

2007-05-01

249

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

Science.gov (United States)

...in 40 CFR part 180 for the residues of the herbicide sulfentrazone...allows monitoring of food with residues at or above the levels set...of acid and cleaned up with solid phase extraction prior to analysis...CFR part 180 for the combined residues of the insecticide...

2013-12-30

250

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)

2001-11-01

251

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 C_1_8 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 (Q_L) 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)

1999-09-01

252

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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 0.0...

2012-01-01

253

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

254

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 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

1988-06-03

255

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

256

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

Science.gov (United States)

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

Watanabe, Eiki; Kobara, Yuso; Yogo, Yasuhiro

2012-09-12

257

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

258

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.

2009-12-01

259

Comparison of the variability in the levels of pesticide residue observed in Japanese cabbage and grape units.  

Science.gov (United States)

To estimate variations in pesticide residue levels in crops, the variability factors (VFs, the 97.5th percentile of the residue levels in the sample divided by the average residue levels in the lot) in residue levels of acetamiprid and cypermethrin applied to cabbage and grapes were investigated, respectively. The VFs in the residue levels of both pesticides in cabbage (2.00 and 2.39, respectively) were clearly higher than those in grapes (1.82 and 1.63, respectively). Although the residue levels of both pesticides in grapes showed a normal distribution, those values in cabbage were slightly skewed at lower residue levels. Individual residue levels in grapes had a good agreement between acetamiprid and cypermethrin. In contrast, the distribution of cypermethrin residue levels in cabbage was slightly skewed at higher residue levels as compared to that of acetamiprid. These results indicate that the difference in the relative distribution of the two pesticides between cabbage and grapes might be due to the influence of various factors such as differences in crop species, plant cultivation methods, and physicochemical properties of the pesticides. PMID:22263932

Fujita, Masahiro; Yajima, Tomonari; Iijima, Kazuaki; Sato, Kiyoshi

2012-02-15

260

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.

 
 
 
 
261

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

262

Development of methodology for determination of pesticides residue in water by SPE/HPLC/DAD.  

Science.gov (United States)

To boost crop yield, sugarcane growers are using increasing amounts of pesticides to combat insects and weeds. But residues of these compounds can pollute water resources, such as lakes, rivers and aquifers. The present paper reports the results of a study of water samples from the Feijão River, which is the source of drinking water for the city of São Carlos, São Paulo, Brazil. The samples were evaluated for the presence of four leading pesticides--ametryn, atrazine, diuron and fipronil--used on sugarcane, the dominant culture in the region. The samples were obtained from three points along the river: the headwaters, along the middle course of the river and just before the municipal water intake station. The pesticides were extracted from the water samples by solid-phase extraction (SPE) and then analyzed by liquid chromatography with diode array detection (LC-DAD). The analytical method was validated by traditional methods, obtaining recovery values between 90 and 95%, with precision deviations inferior to 2.56%, correlation coefficients above 0.99 and detection and quantification limits varying from 0.02 to 0.05 mg L(-1) and 0.07 to 0.17 mg L(-1), respectively. No presence of residues of the pesticides was detected in the samples, considering the detection limits of the method employed. PMID:23393971

Cappelini, Luciana Teresa Dias; Cordeiro, Daniela; Brondi, Silvia Helena Govoni; Prieto, Kátia Roberta; Vieira, Eny Maria

2012-01-01

263

Monitoring of pesticide residues in dairy cattle farms from NW Spain.  

Science.gov (United States)

The consequences of the use of pesticides in agricultural activities for food and feed product safety are subjects of major concern. In the present work, simple and environmentally friendly methodologies were applied to the analysis of soil and cattle feed samples collected in dairy cattle farms from Galicia (NW Spain). This forms part of an integrated study aiming to investigate the global impact of the use of pesticides in such farms. The target compounds were 36 plant protection products belonging to different families. Organochlorine and organophosphorus pesticides were the most commonly detected compounds in the analyzed samples; pyrethroid and chloroacetanilide pesticides were also found in some of them, but not so frequently. Detected levels were rarely above the established legal limits. PMID:20721413

Fernandez-Alvarez, Maria; Lamas, J Pablo; Garcia-Chao, Maria; Garcia-Jares, Carmen; Llompart, Maria; Lores, Marta; Dagnac, Thierry

2010-10-01

264

Pesticide analysis in rose wines by micellar electrokinetic chromatography.  

Science.gov (United States)

In this work, the determination of 11 pesticides (pirimicarb, metalaxyl, pyrimethanil, procymidone, nuarimol, azoxystrobin, tebufenozide, fenarimol, benalaxyl, penconazole, and tetradifon) in rose wines by micellar EKC (MEKC) using reversed electrode polarity stacking mode (REPSM) as online preconcentration strategy is described. The MEKC buffer consisted of 100 mM sodium tetraborate and 30 mM SDS at pH 8.5 with 6% v/v 1-propanol. A solid-phase microextraction (SPME) procedure using PDMS/divinylbenzene (PDMS/DVB) fibers was applied to extract the selected pesticides from the rose wine samples. The comparison between the calibration curves obtained from hydroalcoholic solutions (12% v/v ethanol) and from rose wines (matrix matched calibration) showed the existence of a strong matrix effect. Furthermore, a comparison with calibration curves obtained with white wine samples also showed significant differences for most of the analyzed pesticides. As a result, a matrix matched calibration was developed. Quantitative extraction from spiked wine samples was carried out in triplicate at two levels of concentration (range 0.18-6.00 mg/L). LODs between 0.040 and 0.929 mg/L were achieved, which are below the maximum residue limits (MRLs) established for wine grapes (except for pirimicarb) by the EU and Spain legislation as well as by the Codex Alimentarius. The established method - which is solvent free, cost effective, and fast - was also applied to the analysis of several homemade rose wine samples and a commercial one. Two of the selected pesticides were found in some of the analyzed samples. PMID:18027361

Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Borges-Miquel, Teresa M; Rodríguez-Delgado, Miguel Angel

2007-12-01

265

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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 residu...

Afshar M; Tahery E; Alasty D

1997-01-01

266

Assessment of Pesticide Residues in Honey Samples from Portugal and Spain  

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

2003-01-01

267

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...

2012-01-01

268

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

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

1984-01-01

269

Monitoring of pesticide residues in vegetables marketed in Al-Qassim region, Saudi Arabia.  

Science.gov (United States)

A total of 23 pesticides from different chemical groups in 160 different domestic vegetables collected from four major big supermarkets located in Al-Qassim region, Saudi Arabia, were identified by gas chromatography with mass spectrometry (GC-MS). Residues were found in 89 of the 160 samples and 53 samples were above the maximum residue levels (MRLs). The most frequently found pesticides were carbaryl followed by biphenyl and then carbofuran. Cabbage was the most positive and violated MLRs (16 and 11 samples), followed by carrot and green pepper (12 and 7 samples), cucumber (12 and 6 samples), egg-plant (12 and 5 samples), squash (11 and 7 samples), lettuce (11 and 6 samples) and tomato (11 and 4 samples). The highest concentrations were found in lettuce (ethiofencarb, 7.648), followed by tomato (tolclofos-methyl, 7.312 mg/kg), cabbage (chlropyrifos, 6.207 mg/kg), carrot (heptanophos, 3.267 mg/kg), green pepper (carbaryl, 2.228 mg/kg) and egg-plant (carbaryl, 1.917 mg/kg). These findings pointed to the following recommendation: the need for a monitoring program for pesticide residues in vegetables cultivated under greenhouse conditions at the national level to protect consumers' health. PMID:20627311

Osman, K A; Al-Humaid, A M; Al-Rehiayani, S M; Al-Redhaiman, K N

2010-09-01

270

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)

2011-04-01

271

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

272

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)

1982-06-11

273

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

2005-01-01

274

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

Science.gov (United States)

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

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

2007-06-01

275

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

Energy Technology Data Exchange (ETDEWEB)

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

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

2004-09-15

276

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

2014-05-01

277

Preparation of activated carbons from agricultural residues for pesticide adsorption.  

Science.gov (United States)

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

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

2010-09-01

278

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

279

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)

1982-01-01

280

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

Energy Technology Data Exchange (ETDEWEB)

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

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

2002-12-01

 
 
 
 
281

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

International Nuclear Information System (INIS)

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

2002-12-01

282

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

1994-02-04

283

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  

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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

284

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

285

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

286

Organochlorine pesticide residues in breastmilk: difficulties in sample collection and in assessing intakes.  

Science.gov (United States)

Organochlorine pesticides are highly lipophilic and stable resulting both in their persistence in the environment and their tendency to pass up the food chain. Residues of these compounds are detectable in breastmilk and have been monitored since the 1950s. Samples can be collected using non-invasive techniques and the results are frequently used to assess degradation in the environment as well as risks to recipient infants. As a food, breastmilk is unique. It is manufactured entirely for an individual consumer with some of its constituents driven by its recipient. It can form the sole source of nutrition for a considerable period of an infant's life. Standard calculations of exposure to residues rely on consumption of 750-850 ml breastmilk day(-1) containing 3.5% fat for a 5-kg infant. The fat content of breastmilk, however, is highly variable, which means that that using fixed breastmilk volumes and fat can lead to an imprecise calculation of individual risk. The fat concentration of breastmilk changes throughout a single feed, between feeds and as lactation progresses. This variation therefore raises the methodological problem of how to secure a representative sample of breastmilk. Furthermore, maternal factors such as age and parity also affect concentrations because of the persistence of organochlorine pesticide residues in maternal fat stores. It is therefore critical that samples are collected in a systematic manner taking account of these variables, particularly if the results not only are to be used for risk assessment, but also in comparing changes in environmental concentrations. Reviews of the literature have shown that these variables have often been disregarded in drawing up sampling strategies and methodologies are poorly reported in publications. The paper discusses the literature currently available on monitoring organochlorine pesticide residues in breastmilk and presents an overview of some of the factors that need to be taken into account when collecting samples and assessing infant exposure. PMID:12042020

Harris, Caroline A; Woolridge, Michael W; Hay, Alastair W M

2002-06-01

287

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

Science.gov (United States)

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

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

2011-11-01

288

Monitoring of selected pesticides residue levels in water samples of paddy fields and removal of cypermethrin and chlorpyrifos residues from water using rice bran.  

Science.gov (United States)

Consumption of pesticides associated foods increased in recent decades in Bangladesh. Most of the pesticides come from paddy, as rice is the main food items here and about 70 % pesticides are used only on paddy fields. Water samples of paddy fields and Kaliganga River of Manikganj district were analyzed to provide base line data on cypermethrin, chlorpyrifos and diazinon residue by using high performance liquid chromatography. Levels of Cypermethrin, chlorpyrifos and diazinon detected in the paddy field water samples were (0.605 ± 0.011 ?g/L), (0.06 ± 0.001 ?g/L) and (0.039 ± 0.002 ?g/L), respectively. 0.11 ± 0.003 ?g/L of cypermethrin and 0.012 ± 0.0006 ?g/L of chlorpyrifos were also identified in the water samples of Kaligonga River. Diazinon residue was not detected in the river water samples. The detected concentrations of pesticide residues in the river water were below the accepted maximum residue limit (MRL) value of drinking water (0.1 ?g/l) adopted by the FAO/WHO Codex Alimentarius Commission. Cypermethrin and chlorpyrifos were chosen for decontamination through rice bran, as it was found in river water. Two gm rice bran could easily decontaminated 95.6 % and 96.4 % of cypermethrin and chlorpyrifos. The result of this study showed that pesticide residue was detected in water samples were below the MRLs value, which can easily be decontaminated through absorption of rice bran. PMID:22627618

Bhattacharjee, Shubhra; Fakhruddin, A N M; Chowdhury, M A Z; Rahman, M A; Alam, M K

2012-08-01

289

Rapid and effective sample clean-up based on magnetic multiwalled carbon nanotubes for the determination of pesticide residues in tea by gas chromatography-mass spectrometry.  

Science.gov (United States)

In this work, amine-functionalised magnetic nanoparticles and multiwalled carbon nanotubes (MNPs/MWCNTs) composites were synthesised by a simple method and applied as an adsorbent for rapid clean-up of acetonitrile extracts of tea samples prior to analysing eight pesticide residues by gas chromatography-mass spectrometry. Several parameters affecting the sampling and treatment efficiency were investigated, including extraction solvent, sonication time, weight ratio of MWCNTs to MNPs in the composites, amount of adsorbent, clean-up time and washing solution. Under the optimised conditions, the recoveries obtained for each pesticide ranged from 72.5% to 109.1% with relative standard deviations lower than 12.6%. Limit of quantification ranged from 0.02 to 0.08 mg kg?¹. The established method was successfully applied to the analysis of pesticide residues in real tea samples. The results indicated that the use of MNPs/MWCNTs composites allowed the simple and expeditious clean-up of complex tea samples for subsequent determination of pesticide residues. PMID:24128556

Deng, Xiaojuan; Guo, Qianjin; Chen, Xiaoping; Xue, Tao; Wang, Hui; Yao, Pei

2014-02-15

290

Microbiological quality and organochlorine pesticide residue in commercially available ready-to-eat raisins.  

Science.gov (United States)

Microbiological quality and organochlorine pesticide residual contamination in raisins in a restricted area of Lucknow city, India was assessed in 20 samples. Total bacterial count was found in both open and packed raisin samples within the acceptable range (10(5)-<10(6)). The presence of food pathogens like Salmonella spp. and Enterobacteriaceae was detected more in open samples whereas Staphylococcus spp. and Pseudomonas spp. were absent. Lactobacilli spp. was found in all open samples and two packed samples. Presence of OCP residue was also found below the MRL although low levels of alpha-HCH and gamma-HCH were detected in samples. The study shows presence of spoilage and pathogenic microorganisms as well as OCP residue within permissible limits which was more in open samples than in packed ones. PMID:18668188

Sharma, Sapna; Chandra, Prachi; Mishra, Chetna; Kakkar, Poonam

2008-10-01

291

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 23.3ng/g matrix weight and 0.1 up to 78ng/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 81.5ng/g, for bee pollen from 6.1 to 1273ng/g and for honey one sample was positive to carbendazim at 1.6ng/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

292

A survey of pesticide residues in pollen loads collected by honey bees in France.  

Science.gov (United States)

In 2002, a field survey was initiated on French apiaries to monitor weakness of honey bee, Apis mellifera L., colonies. Apiaries were evenly distributed in five sites located on continental France. Five colonies were randomly selected in each apiary, leading to a total of 125 studied honey bee colonies. For 3 yr (starting in autumn 2002), colonies were visited four times per year: after winter, before summer, during summer, and before winter. Pollen loads from traps were collected at each visit. Multiresidue analyses were performed in pollen to search residues of 36 different molecules. Specific analyses were conducted to search fipronil and metabolites and also imidacloprid and metabolites. Residues of 19 searched compounds were found in samples. Contamination by pesticides ranged from 50 to 0%. Coumaphos and tau-fluvalinate residues were the most concentrated of all residues (mean concentrations were 925.0 and 487.2 microg/kg, respectively). Fipronil and metabolite contents were superior to the limit of detection in 16 samples. Residues of fipronil were found in 10 samples. Nine samples contained the sulfone compound, and three samples contained the desulfinyl compound. Residues of imidacloprid and 6-chloronicotinic acid were found in 69% of samples. Imidacloprid contents were quantified in 11 samples with values ranging from 1.1 to 5.7 microg/kg. 6-Chloronicotinic acid content was superior to the limit of quantification in 28 samples with values ranging from 0.6 to 9.3 microg/kg. Statistical tests showed no difference between places of sampling with the exception of fipronil. Possible origins of these contaminations, concentration and toxicity of pesticides, and the possible consequences for bees are discussed. PMID:16686121

Chauzat, Marie-Pierre; Faucon, Jean-Paul; Martel, Anne-Claire; Lachaize, Julie; Cougoule, Nicolas; Aubert, Michel

2006-04-01

293

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

294

Stir Bar Sorptive Extraction (SBSE) in sample preparation from heterogeneous matrices: determination of pesticide residues in pear pulp at ppb (ng/g) level  

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

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

2003-01-01

295

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

296

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

297

Residual gas analysis device  

Energy Technology Data Exchange (ETDEWEB)

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

Thornberg, Steven M. (Peralta, NM)

2012-07-31

298

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 LC_5_0 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 (< 0.050 ppm) or very low concentrations (< 0.010 ppm). The Nacaome and Choluteca Rivers, which include Tegucigalpa and other urban centers within their drainage basins, had the greatest number of pesticide detections and the highest concentrations among all the water samples tested. Carbofuran at 9.23 ppm and propiconizole at 1.79 ppm were detected in the sample taken from the Choluteca River in February of 1995. The April '95 sample from the Choluteca River contained 2.80 ppm of diallate and 0.26 ppm of heptachlor-epoxide. Samples from the Nacaome River contained high concentrations of diallate (1.400 ppm), carbaryl (0.560 ppm), 2,4-D (0.230 ppm) and quinomethinate (0.320 ppm). Intensive cultivation of melons and other export crops occurs throughout the drainage basin of this river in southern Honduras. All river and lake bottom sediments contained DDT or its metabolites. Four sediment samples had extremely high concentrations of these compounds in excess of 2.000 ppm. The insecticides endosulfan and lindane had much lower LC_5_0 values and were therefore found to be much more toxic to the post-larval shrimp than the fungicides tridemorph and propiconazole. (author)

1999-09-01

299

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

Science.gov (United States)

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

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

2010-11-01

300

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

 
 
 
 
301

Application of ultra-high pressure liquid chromatography linear ion-trap orbitrap to qualitative and quantitative assessment of pesticide residues.  

Science.gov (United States)

The analysis of pesticides residues using a last generation high resolution and high mass accuracy hybrid linear ion trap-Orbitrap mass spectrometer (LTQ-Orbitrap-MS) was explored. Pesticides were extracted from fruits, fish, bees and sediments by QuEChERS and from water by solid-phase with Oasis HLB cartridges. Ultra-high pressure liquid chromatography (UHPLC)-LTQ-Orbitrap mass spectrometer acquired full scan MS data for quantification, and data dependent (dd) MS(2) and MS(3) product ion spectra for identification and/or confirmation. The regression coefficients (r(2)) for the calibration curves (two order of magnitude up to the lowest calibration level) in the study were ?0.99. The LODs for 54 validated compounds were ?2ngmL(-1) (analytical standards). The relative standard deviation (RSD), which was used to estimate precision, was always lower than 22%. The recovery of extraction and matrix effects ranged from 58 to 120% and from -92 to 52%, respectively. Mass accuracy was always ?4ppm, corresponding to a maximum mass error of 1.6millimass units (mmu). This procedure was then successfully applied to pesticide residues in a set of the above-mentioned food and environmental samples. In addition to target analytes, this method enables the simultaneous detection/identification of non-target pesticides, pharmaceuticals, drugs of abuse, mycotoxins, and their metabolites. PMID:24438835

Farré, M; Picó, Y; Barceló, D

2014-02-01

302

Rapid multiplug filtration cleanup with multiple-walled carbon nanotubes and gas chromatography-triple-quadruple mass spectrometry detection for 186 pesticide residues in tomato and tomato products.  

Science.gov (United States)

This study reports the development and validation of a novel rapid cleanup method based on multiple-walled carbon nanotubes in a packed column filtration procedure for analysis of pesticide residues followed by gas chromatography-triple-quadruple tandem mass spectrometry detection. The cleanup method was carried out by applying the streamlined procedure on a multiplug filtration cleanup column with syringes. The sorbent used for removing the interferences in the matrices is multiple-walled carbon nanotubes mixed with anhydrous magnesium sulfate. The proposed cleanup method is convenient and time-saving as it does not require any solvent evaporation, vortex, or centrifugation procedures. It was validated on 186 pesticides and 3 tomato product matrices spiked at two concentration levels of 10 and 100 ?g kg(-1). Satisfactory recoveries and relative standard deviations are shown for most pesticides using the multiplug filtration cleanup method in tomato product samples. The developed method was successfully applied to the determination of pesticide residues in market samples. PMID:24512455

Zhao, Pengyue; Huang, Baoyong; Li, Yanjie; Han, Yongtao; Zou, Nan; Gu, Kejia; Li, Xuesheng; Pan, Canping

2014-04-30

303

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

Scientific Electronic Library Online (English)

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

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

304

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

305

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

Science.gov (United States)

A laboratory experiment was conducted to evaluate the effect of alternating soil drying and wetting on the release of aged 14C-labeled pesticide residues and their distribution in soil organic fractions (humic acids, fulvic acids, and humin substances). The used soils (gleyic cambisol; Corg 1.2%, pH 7.2) were obtained from the upper soil layer of two individual outdoor lysimeter studies containing either environmentally long-term aged 14C residues of the herbicide ethidimuron (ETD; 0-10 cm depth; time of aging: 9 years) or methabenzthiazuron (MBT; 0-30 cm depth; time of aging: 17 years). Triplicate soil samples (10 g dry soil equivalents) were (A=dry/wet) previously dried (45° C) or (B=wet/wet) directly mixed with pure water (1+2, w:w), shaken (150 rpm, 1 h), and centrifuged (~2000 g). The resulting supernatant was removed, filtered (0.45 ?m) and subjected to 14C activity analysis via liquid scintillation counter (LSC), dissolved organic carbon (DOC) analysis, and LC-MS-MS analysis. This extraction procedure was repeated 15 individual times, for both setups (A) and (B). To determine the distribution of the aged 14C labelled pesticide residues in the soil organic matter fractions, the soil samples were subject to humic and fulvic acids fractionations at cycles 0, 4, 10, and 15. The residual pesticide 14C activity associated with the humic, fulvic, and humin substances (organic fraction remaining in the soil) fractions was determined via LSC. The water-extracted residual 14C activity was significantly higher in the extracts of the dry/wet, compared to the wet/wet soil samples for both pesticides. The total extracted 14C activity in the dry/wet soil extracts accounted for 51.0% (ETD) and 15.4% (MBT) in contrast to 19.0% (ETD) and 4.7% (MBT) in the wet/wet extracts after 15 water extractions. LC-MS-MS analysis revealed the parent compound ETD 27.9 ?g kg-1 soil (dry/wet) and 10.7 ?g kg-1 soil (wet/wet), accounting for 3.45 and 1.35% of total parent compound initially applied after a total of 10 water extractions, respectively. MBT was detected but not quantified, whereas its metabolite MABT (2-methylamino-benzothiazole) was detected (0.8 vs 0.3 ?g kg-1, in dry/wet vs wet/wet soil water extracts, respectively) after 10 water extractions. These results demonstrate the long-term persistence of ETD and MBT and metabolites and their remobilization potential facilitated by soil drying and rewetting. For all samples, the DOC content was significantly higher for the water extracts obtained after dry/wet cycles compared to values obtained from the constantly moistened soil samples. The DOC and water extracted residual 14C activity correlated positively. This result indicates that pesticide residues are associated with DOC which might function as a shuttle for the distribution of pesticide residues. This molecular association can be released into solution where it might be degraded co-metabolically. Overall, the results suggest that intermittent soil drying and rewetting alters the disaggregation of soil aggregates, resulting in a release of entrapped organic carbon and pesticide molecules. Furthermore, analysis of the organic fractions obtained from the 14C pesticide residues containing soil revealed that 14C residues were mainly associated with the humin fraction. The analysis of the organic fractions revealed that extractable residual 14C activity of ETD was more associated with the fulvic acid fraction compared to the residual pesticide 14C activity of MBT, being more associated with the humic acid fraction. For 14C MBT residues, the distribution of the 14C residues in the organic fractions remained rather equal throughout the water extraction cycles. This observation can be supported by the non-mobile character of MBT in soil and its higher KOC value of 247-587 compared to the rather mobile pesticide ETD with a KOC value of 37.1-149. However, for both pesticides a decrease of residual 14C activity in the humic and fulvic acid fractions throughout the water extractions cycles was observed. This observation was more pronounced

Jablonowski, N. D.; Mucha, M.; Thiele, B.; Hofmann, D.; Burauel, P.

2012-04-01

306

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

2007-08-01

307

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

Science.gov (United States)

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

2013-01-30

308

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.

2011-01-01

309

Pesticide residues on the external surfaces of field-crop sprayers: environmental impact.  

Science.gov (United States)

There is increased awareness of the need to clean the external surfaces of sprayers, but the extent to which the washings may impact on the environment is not known. Quantification of the levels of external residues on sprayers could give an indication of the potential environmental impact of sprayer cleaning. The presence of azoxystrobin, carbendazim, chlorothalonil, cyanazine, cypermethrin, epoxiconazole, flusilazole, isoproturon, kresoxim-methyl, metazachlor, pendimethalin, pirimicarb and tebuconazole on thirteen sprayers, sampled on two occasions was investigated. Composite samples were taken from the boom, nozzles and spray tank (delivery system) and the mudguard, cab door, rear window and windscreen (tractor body). Despite being subject to some form of cleaning, pesticides were detected on all sprayers. Residues were found at higher quantities and with greater frequency on the nozzles and booms, but the mean dose on the spray tank was equal to that on the mudguard (7.2 mg m(-2)). Isoproturon, pendimethalin, metazachlor, chlorothalonil and azoxystrobin were all detected above 1000 mg m(-2) on the delivery system, whereas on the tractor body the highest concentrations were between 100 and 1000 mg m(-2) (isoproturon, pendimethalin, chlorothalonil and carbendazim). On the whole, azoxystrobin was detected on the least number of occasions. However, there was great variation within and between compounds and sampling sites. Generally sprayers were not cleaned frequently or efficiently, enabling residues to accumulate on the external surfaces where they can remain for years. The findings here indicate that the quantity of these residues may be sufficient to be harmful to aquatic organisms should the residues enter a watercourse. In addition, if all the residues were removed by cleaning in the field and the washings catchment area was 15 m2 or less, overdosing could occur. Further work is required to assess whether a more frequent cleaning regime would reduce the overall environmental impact of cleaning sprayers. Implications for potential occupational exposure are considered elsewhere. PMID:15307671

Ramwell, Carmel T; Johnson, Paul D; Boxall, Alistair; Rimmer, Duncan A

2004-08-01

310

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

2006-02-03

311

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

Energy Technology Data Exchange (ETDEWEB)

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

Sanchez, Andres Garcia [Department of Physical and Analytical Chemistry, E.P.S. of Linares, University of Jaen, E-23700 Linares, Jaen (Spain); Martos, Natividad Ramos [Department of Physical and Analytical Chemistry, Faculty of Sciences, University of Jaen, E-23071 Jaen (Spain); Ballesteros, Evaristo [Department of Physical and Analytical Chemistry, E.P.S. of Linares, University of Jaen, E-23700 Linares, Jaen (Spain)]. E-mail: eballes@ujaen.es

2006-02-03

312

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

Science.gov (United States)

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

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

2009-12-18

313

Residual levels and identify possible sources of organochlorine pesticides in Korea atmosphere  

Science.gov (United States)

The nationwide monitoring program was established in 2008 to monitor of persistent organic pollutants (POPs) in Korea. Under this program, it was observed air concentrations of organochlorine pesticides (OCPs) at 37 sites from January to October of 2008, to determine the residue levels and identify possible sources in Korea atmosphere. Samples of OCPs including HCB, aldrin, dieldrin, endrin, p, p'-DDT, o, p'-DDT, p, p'-DDE, o, p'-DDE, p, p'-DDD, o, p'-DDD, trans-chlordane, cis-chlordane, trans-nonachlor, cis-nonachlor, oxychlordane, heptachlor, heptachlor epoxide were collected with high volume air sampler and analyzed by HRGC/HRMS. The concentrations were in the range of 41.2-344.3 pg m -3 for HCB, ND-47.55 pg m -3 for DDTs (sum of p, p'-DDT, o, p'-DDT, p, p'-DDE, o, p'-DDE, p, p'-DDD, o, p'-DDD), ND-38.97 pg m -3 for chlordanes (sum of trans-chlordane, cis-chlordane, trans-nonachlor, cis-nonachlor, oxychlordane), ND-9.19 pg m -3 for heptachlors (sum of heptachlor and heptachlor epoxide) and ND-4.32 pg m -3 for dieldrin. The predominant compound in air was HCB. However, HCB itself has not ever been registered and used as a pesticide in Korea. The elevated concentration of HCB in Korea might be contributed to geographical location and long range transport. For DDTs, it was found that no more fresh input occurred recently and technical type DDTs was prevailing in Korea. Higher concentration of chlordane was observed in winter, which was contributed to the fresh input technical chlordane and long range transport. Relatively lower levels of heptachlor and dieldrin despite much more consumption than other pesticides were resulted from shorter half-lives in environment.

Park, Jin Soo; Shin, Sun Kyoung; Kim, Woo Il; Kim, Byung Hoon

2011-12-01

314

[Determination of the trace residues of four organochlorine pesticides in agricultural products by high performance liquid chromatography with modified multi-walled carbon nanotubes as solid phase extraction adsorbent].  

Science.gov (United States)

A novel method for the simultaneous determination of the trace residues of four organochlorine pesticides such as p,p'-DDD, p,p'-DDT, o,p'-DDT and p,p'-DDE in agricultural products by multi-walled carbon nanotubes (MWNTs) modified by acid oxidation on the surface as solid phase extraction (SPE) adsorbent coupled with high performance liquid chromatography (HPLC) was developed. The effects of the surface acid oxidation, SPE operations and HPLC conditions on the determination of the four pesticide residues were investigated. Under the optimized experimental conditions, the novel method provided wide linear ranges for the pesticides with correlation coefficients of 0. 997 8 - 0. 999 5, the detection limit was 0.050 mg/L for each pesticides. The recoveries from the samples spiked with the pesticide standards at three concentration levels of 0.10, 2.0 and 50 mg/L were in the range of 78% - 104% with the relative standard deviations (RSDs) of 2.7% -7.6%. This study indicated the MWNTs SPE was an efficient clean-up method to agricultural products (included dried orange peel, ginseng, cabbage and tea). The proposed method showed the advantages of accuracy and sensitivity, and can meet the requirements for the determination of low residue pesticide in agricultural products. The study provides a useful method for the analysis of trace substance of agricultural products. PMID:23285982

Peng, Xiaojun; Pang, Jinshan; Deng, Aihua; Liang, Weihua; Liang, Youzhen; Wen, Qijing

2012-09-01

315

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

316

Use of liquid chromatography coupled to quadrupole time-of-flight mass spectrometry to investigate pesticide residues in fruits.  

Science.gov (United States)

In this paper, the potential of coupling liquid chromatography with hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF) for the determination of pesticides in a variety of fruit samples (orange peel and flesh, banana skin and flesh, strawberry and pear) has been explored. The quantitative application at residue levels has been proven for two insecticides (buprofezin and hexythiazox), which were satisfactorily determined at three concentration levels, 0.1, 1, and 5 mg/kg, obtaining a suitable linearity range (correlation coefficient>0.99) of more than 2 orders of magnitude. Satisfactory recoveries have been obtained for both compounds at the three levels tested in all sample matrices, with lowest calibration levels (LCL) of 0.075 and 0.01 mg/kg. The excellent potential of QTOF for identification purposes is illustrated by the high number of identification points (IPs) earned, up to 21, at the highest concentration of 5 mg/kg, or between 11 and 21 at the 0.1 and 1 mg/kg levels. The application of LC-QTOF MS to real samples revealed the presence of several positives at concentrations close to the LCL, all of which were confirmed with more than 11 IPs. The potential of QTOF for elucidation of nontarget analytes has also been demonstrated by the finding of one transformation product (TP) of buprofezin in a banana skin sample. This TP was identified by obtaining the full scan product ion spectra at different collision energies with acceptable accurate mass deviation. The work performed in this paper illustrates the suitability and excellent confirmatory potential of LC-QTOF MS for pesticides residues analysis in food samples. PMID:17309229

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

2007-04-01

317

Development and validation of methodology for the determination of residues of organophosphorus pesticides in tomatoes  

Scientific Electronic Library Online (English)

Full Text Available SciELO Brazil | Language: English Abstract in portuguese Os pesticidas organofosforados são freqüentemente aplicados no cultivo de tomate no Brasil. No presente trabalho uma metodologia analítica foi desenvolvida e validada para a quantificação de resíduos dos pesticidas organofosforados acefato, chlorpyrifós, malation, metamidofós and paration metílico e [...] m tomate, empregando Cromatografia Gasosa com Detector de Nitrogênio e Fósforo (GC-NPD). A possibilidade de ocorrência de efeito matriz foi estudada. As curvas analíticas, preparadas nos extratos da matriz, foram lineares de 0,006 até 0,80 mg L-1. Os estudos de precisão forneceram resultados com RSD Abstract in english The organophosphorus pesticides are frequently applied in tomato cultivation in Brazil. In the present work an analytical methodology for quantification of the organophosphorus pesticides: acephate, chlorpyrifos, malathion, methamidophos and parathion-methyl residues in tomatoes was developed and va [...] lidated using Gas Chromatography with a Nitrogen-Phosphorus Detector (GC-NPD). The possibility of a matrix effect was studied. Analytical curves prepared in an extract of the matrix were linear from 0.006 to 0.80 mg L-1. The precision studies supplied results with RSD

Anagilda B., Gobo; Márcia H. S., Kurz; Ionara R., Pizzutti; Martha B., Adaime; Renato, Zanella.

318

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

Science.gov (United States)

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

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

2008-07-01

319

77 FR 25954 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...  

Science.gov (United States)

...linear C 8 -C 18 fatty acids. The following materials...petition is based on coconut fatty acid, dimethylamidopropylamide...biochemical pesticide, methyl jasmonate (CAS No. 1211-29-6...2-pentenyl)-, methyl ester, in or on canola,...

2012-05-02

320

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

Science.gov (United States)

...www.epa.gov/dockets. FOR FURTHER INFORMATION CONTACT: Olga Odiott, Registration Division (7505P), Office of Pesticide...telephone number: (703) 308-9369; email address: odiott.olga@epa.gov. SUPPLEMENTARY INFORMATION: I. General...

2013-11-27

 
 
 
 
321

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

Science.gov (United States)

...correction of the glyphosate tolerance in the commodity poultry, meat from 4 ppm to 0.1 ppm. Adequate enforcement...Environmental protection, Agricultural commodities, Feed additives, Food additives, Pesticides and pests, Reporting and...

2010-03-24

322

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

1975-01-01

323

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

324

[Application of near-infrared spectroscopy to detection of pesticide phoxim residues].  

Science.gov (United States)

Near-infrared (NIR) spectroscopy technique was applied directly to the detection of pesticide phoxim residues. A sample pretreatment method was introduced. Samples were mixed with silica gel. Silica gel as a sorbent was employed to extract and enrich the low-concentration samples. Subsequently, diffuse reflection spectrum was measured on silica gel. Calibration models were developed using partial least square regression (PLSR) algorithm. Leave-one-out cross-validation was used to evaluate and compare the models. Two experiments were carried out, and the results show that 21 samples with the concentration gradient of 0.5 mg x L(-1) exhibited a high correlation coefficient of cross-validation of 0. 958, and a root mean square error of cross validation (RMSECV) of 0.872 mg x L(-1), while 41 samples with the concentration gradient of 0.25 mg x L(-1) gave a correlation coefficient of cross-validation of 0.924 and RMSECV of 1.15 mg x L(-1). It is indicated that with the reduction in concentration gradient, the prediction capacity of models dropped, but there still existed a high correlation coefficient with the concentration of phoxim in the samples. The experiments proved that the sample pretreatment method with the introduction of silica gel as an absorber to enrich low concentration analyte was effective. The method was able to lower the detection limit of NIR. The developed technique has a potential application in low-concentration sample detection by NIR spectroscopy, such as pesticide residues. PMID:19950643

Shen, Fei; Yan, Zhan-ke; Ye, Zun-zhong; Ying, Yi-bin

2009-09-01

325

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

326

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

327

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.

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

328

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

Science.gov (United States)

Organochlorine pesticides were intensively used in Mexico from 1950 until their ban and restriction in 1991. However, the presence of these compounds is commonly reported in many regions of the country. The aim of the present study was to identify and quantify residual organochlorine and organophosphorus pesticides in agricultural soil in Rio Verde region, San Luis Potosi state, which has been identified as possibly polluted by pesticides. Composed samples from 24 zones covering an area of approximately 5,440 ha were analyzed. The most frequently found pesticides were p,p´-DDT followed by ,p,p´-DDE, heptachlor, endosulfan and ?-HCH whose frequency rates were 100, 91, 83 and 54%, respectively. The concentration of p,p´-DDT in the crops grown in these soils was in the following order: chili > maize > tomato > alfalfa. The results obtained in this study show that p,p´-DDT values are lower or similar to those found in other agricultural regions of Mexico. Methyl and ethyl parathion were the most frequent organophosphate pesticide detected in 100% and 62.5% of the samples with average concentrations of 25.20 and 47.48 ?g kg(-1), respectively. More research is needed to establish the background levels of pesticides in agricultural soils and their potential ecological and human health effects in this region. PMID:24813984

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

2014-07-01

329

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

330

77 FR 43562 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...  

Science.gov (United States)

...part 180 for residues of the herbicide quinclorac (3,7-dichloro-8-quinolinecarboxylic...refined oil, as no concentration of quinclorac residues is expected in these commodities...determinations was designed to measure quinclorac residues present as the...

2012-07-25

331

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

Science.gov (United States)

...combined residues of the fungicide propiconazole, (1-[[2-(2,4- dichlorophenyl...for the determination of residues of propiconazole and its metabolites containing the...combined residues of the fungicide propiconazole,...

2010-03-19

332

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

Science.gov (United States)

...part 180 for residues of the fungicide propiconazole, 1-[[2-(2,4-dichlorophenyl...for the determination of residues of propiconazole and its metabolites containing...434 for residues of the fungicide propiconazole, 1-[[2-(2,4-...

2011-07-20

333

Pesticide residue analyses and biomarker responses of native Costa Rican fish of the Poeciliidae and Cichlidae families to assess environmental impacts of pesticides in Palo Verde National Park.  

Science.gov (United States)

Pesticide chemical residues in water samples and biomarker responses in transplanted fish were used to monitor environmental hazards of pesticides in Palo Verde National Park (Costa Rica). The Costarican fish, Parachromis dovii (Ciclhidae) and Poecilia gillii (Poecillidae), were selected as sentinel species. Contaminant analyses detected up to 15 different pesticide residues in water with hexachlobenzene (2261 ng l(-1)), phorate (473 ng l(-1)), epoxiconazole (314) and bromacil (117 ng l(-1)) being the compounds found in higher concentrations. Biomarker responses evidenced impacts on cholinesterase activities in transplanted fish at Barbudal site probably due to the presence of organophosphate insecticides such as phorate. High enzyme activities of glutathione S-transferase and catalase and elevated levels of lipid peroxides were also observed at a site impacted by rice fields (Cabuyo); those effects could be associated with the presence of hexachloro benzene and triazole fungicides. In general, P. dovii biomarkers were affected to a greater extent than those of P. gillii in fish transplanted to sites associated with agriculture, which suggests the former species is a good candidate for future surveys. PMID:24579517

Mena, F; Fernández San Juan, M; Campos, B; Sánchez-Avila, J; Faria, M; Pinnock, M; de la Cruz, E; Lacorte, S; Soares, A M V M; Barata, C

2014-01-01

334

[Simultaneous determination of 103 pesticide residues in cabbages and apples using programmable temperature vaporizer-based large volume injection by gas chromatography-negative chemical ionization mass spectrometry].  

Science.gov (United States)

A gas chromatography-mass spectrometric (GC-MS) method has been established for the simultaneous determination of 103 pesticide residues in cabbages and apples using programmable temperature vaporizer-based large volume injection (PTV-LVI) and negative chemical ionization (NCI). It was found that much lower detection limits for the investigated pesticides can be obtained. Prior to GC-NCI/MS analysis, the optimized parameters of PTV-LVI were as follows: inlet temperature was set at 45 degrees C, split vent flow rate was 20 mL/min, evaporation time was 1 min and evaporation temperature was set at 60 degrees C. The volume of injection was 10 microL. Co-extractives were removed from the acetonitrile extracts using solid phase extraction with octadecyl (200 mg) and primary secondary amine (100 mg) sorbents. Matrix matched calibration solutions were used for all the analyses. To evaluate performance of the method, validation experiments were carried out in cabbages and apples at two spiking levels (5 and 10 microg/kg). The average recoveries ranged from 58.5% to 113.2%, and the relative standard deviations (RSDs, n = 6) were in the range of 3.3% - 14.5%. The limits of detection (S/N = 3) were less than 5 microg/kg for all the pesticides. The results show that this method is simple, rapid, sensitive and specific. It is appropriate for the simultaneous identification and quantification of the multi-residues in cabbages and apples. PMID:21046783

Dong, Jing; Pan, Yuxiang; Qin, Yaping; Lü, Jianxia; Yu, Qiongwei

2010-07-01

335

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

336

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.

337

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

Science.gov (United States)

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

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

2014-06-01

338

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)

2009-06-01

339

75 FR 35801 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...  

Science.gov (United States)

...hydrolyzed to released conjugated residues and purified by C18 solid phase extraction. Residues are quantified by LC/MS/MS using...conjugated residues and purified by C18 solid phase extraction. Residues are quantified by LC/MS/MS...

2010-06-23

340

Application of QuEChERS method for simultaneous determination of pesticide residues and PAHs in fresh herbs.  

Science.gov (United States)

The aim of this study was to evaluate the application of quick, easy, cheap, effective, rugged and safe method for simultaneous determination of polycyclic aromatic hydrocarbons and pesticide residues in fresh herbs. In the experiment two extraction solvents and standard types of sorbents were used. The extracts were analyzed using GC-SIM-MS. The results suggest that acetonitrile is more suitable extraction solvent giving more purified samples and better recovery values (71.6 %-116.9 %) with RSD lower than 15 % for most of the compounds. In real samples pesticides were identified in the samples of parsley, tarragon and lovage. In few samples the pesticide levels exceeded the MRL established by EU. PMID:23292488

Sadowska-Rociek, Anna; Surma, Magdalena; Cie?lik, Ewa

2013-04-01

 
 
 
 
341

Gel Permeation Chromatography Purification and Gas Chromatography-Mass Spectrometry Detection of Multi-Pesticide Residues in Traditional Chinese Medicine  

Digital Repository Infrastructure Vision for European Research (DRIVER)

The measurement of 23 organochlorine, organophosphorus, and pyrethroid pesticides in typical traditional Chinese medicine (TCM), flos lonicerae, was made using gel permeation chromatography (GPC) purification and gas chroma- tography-mass spectrometry (GC-MS) detection. The pesticides were extracted with ultrasonic device and 5.0 mL mixture of ethyl acetate and cyclohexane (1:1, v/v). Coextractants from sample matrices which may have interfere to the qualitative and quantitative analysis, suc...

Wan-E Zhuang; Zhen-Bin Gong

2012-01-01

342

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

343

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)

2007-11-01

344

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

2002-01-01

345

Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection.  

Science.gov (United States)

Validation experiments were conducted of a simple, fast, and inexpensive method for the determination of 229 pesticides fortified at 10-100 ng/g in lettuce and orange matrixes. The method is known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticide residues in foods. The procedure involved the extraction of a 15 g sample with 15 mL acetonitrile, followed by a liquid-liquid partitioning step performed by adding 6 g anhydrous MgSO4 plus 1.5 g NaCl. After centrifugation, the extract was decanted into a tube containing 300 mg primary secondary amine (PSA) sorbent plus 1.8 g anhydrous MgSO4, which constituted a cleanup procedure called dispersive solid-phase extraction (dispersive SPE). After a second shaking and centrifugation step, the acetonitrile extract was transferred to autosampler vials for concurrent analysis by gas chromatography/mass spectrometry with an ion trap instrument and liquid chromatography/tandem mass spectrometry with a triple quadrupole instrument using electrospray ionization. Each analytical method was designed to analyze 144 pesticides, with 59 targeted by both instruments. Recoveries for all but 11 of the analytes in at least one of the matrixes were between 70-120% (90-110% for 206 pesticides), and repeatabilities typically <10% were achieved for a wide range of fortified pesticides, including methamidophos, spinosad, imidacloprid, and imazalil. Dispersive SPE with PSA retained carboxylic acids (e.g., daminozide), and <50% recoveries were obtained for asulam, pyridate, dicofol, thiram, and chlorothalonil. Many actual samples and proficiency test samples were analyzed by the method, and the results compared favorably with those from traditional methods. PMID:15859089

Lehotay, Steven J; de Kok, André; Hiemstra, Maurice; Van Bodegraven, Peter

2005-01-01

346

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

Science.gov (United States)

...residues of 5-chloro- 2-methyl-4-isothiazolin-3-one (in combination with 2-methyl-4- isothiazolin-3-one) (CAS Reg. Nos. 26172-55-4...tolerance for residues of 2-methyl- 4-isothiazolin-3-one (CAS Reg. No....

2010-12-22

347

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

Science.gov (United States)

...tolerances in 40 CFR part 180 for residues of the fungicide 5-chloro-3-methyl-4-nitro-1H-pyrazole...In all plant matrices, the residue of concern, parent CMNP and...to its aglycone, CHNP) and solid-phase cleanup. Contact...indirect or inadvertent combined residues of the insecticide...

2010-10-27

348

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

Science.gov (United States)

...developed to determine the residues of flonicamid and its three...TFNA-AM in various crops. The residue analytical method for the majority...partition with ethyl acetate. The residue method for wheat straw is similar, except that a C 18 solid phase extraction (SPE)...

2012-03-14

349

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

Science.gov (United States)

...CFR part 180 for residues of the insecticide...aliquot was purified by solid phase extraction...leaf lettuce and HAX solid phase extraction...CFR part 180 for residues of the fungicide...from preliminary residues trials in Europe...standard followed by solid phase...

2011-12-08

350

76 FR 39358 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...  

Science.gov (United States)

...CFR part 180 for residues of the fungicide...involves extraction, solid phase cleanup of...and cleaned up with solid phase extraction...CFR part 180 for residues of the herbicide...acibenzolar-S-methyl residues convertible to benzo...involves extraction and solid phase cleanup...

2011-07-06

351

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

Science.gov (United States)

...180 for residues of the insecticide metaflumizone, in or on the raw agricultural commodities...developed to determine residues of metaflumizone and its metabolites M320I04, and M320I23...matrices. In this method, residues of metaflumizone are extracted from plant matrices...

2011-08-10

352

Quantification, nature and bioavailability of bound "1"4C-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

1985-03-25

353

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

2012-01-01

354

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

355

Determination of organochlorine pesticide residues in honey from the central zone of Portugal and the Valencian community of Spain  

Digital Repository Infrastructure Vision for European Research (DRIVER)

In this study nine organochlorine pesticide residues ([alpha]-, [beta]-, and [gamma]-hexachlorocyclohexane (HCH), hexachlorobenzene (HCB), aldrin, p,p'-DDE, p,p'-DDD, o,p'-DDT, and p,p'-DDT) in forty nine samples of honey collected from markets of Portugal and Spain during 2001 and 2002, respectively, were evaluated. For this evaluation, three analytical procedures were studied. The analytical procedure, based on LLE extraction with ethyl acetate followed by gas chromatography-electron-captur...

2004-01-01

356

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

2013-01-01

357

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.

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

2014-05-01

358

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

359

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

360

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

"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; whi...

Khodadadi, M.; Samadi, M. T.; Rahmani, A. R.; Maleki, R.; Allahresani, A.; Shahidi, R.

2010-01-01

 
 
 
 
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