ESTIMATION OF THE BURDEN OF PESTICIDE RESIDUES IN SLOVAK POPULATION

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Jozef Sokol

2010-07-01

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

Evaluation of gas chromatography – electron ionization – full scan high resolution Orbitrap mass spectrometry for pesticide residue analysis

International Nuclear Information System (INIS)

Mol, Hans G.J.; Tienstra, Marc; Zomer, Paul

2016-01-01

Gas chromatography with electron ionization and full scan high resolution mass spectrometry with an Orbitrap mass analyzer (GC-EI-full scan Orbitrap HRMS) was evaluated for residue analysis. Pesticides in fruit and vegetables were taken as an example application. The relevant aspects for GC-MS based residue analysis, including the resolving power (15,000 to 120,000 FWHM at m/z 200), scan rate, dynamic range, selectivity, sensitivity, analyte identification, and utility of existing EI-libraries, are assessed and discussed in detail. The optimum acquisition conditions in full scan mode (m/z 50–500) were a resolving power of 60,000 and an automatic-gain-control target value of 3E6. These conditions provided (i) an optimum mass accuracy: within 2 ppm over a wide concentration range, with/without matrix, enabling the use of ±5 ppm mass extraction windows (ii) adequate scan speed: minimum 12 scans/peak, (iii) an intra-scan dynamic range sufficient to achieve LOD/LOQs ≤0.5 pg in fruit/vegetable matrices (corresponding to ≤0.5 μg kg"−"1) for most pesticides. EI-Orbitrap spectra were consistent over a very wide concentration range (5 orders) with good match values against NIST (EI-quadrupole) spectra. The applicability for quantitative residue analysis was verified by validation of 54 pesticides in three matrices (tomato, leek, orange) at 10 and 50 μg/kg. The method involved a QuEChERS-based extraction with a solvent switch into iso-octane, and 1 μL hot splitless injection into the GC-HRMS system. A recovery between 70 and 120% and a repeatability RSD <10% was obtained in most cases. Linearity was demonstrated for the range ≤5–250 μg kg"−"1. The pesticides could be identified according to the applicable EU criteria for GC-HRMS (SANTE/11945/2015). GC-EI-full scan Orbitrap HRMS was found to be highly suited for quantitative pesticide residue analysis. The potential of qualitative screening to extend the scope makes it an attractive alternative to

Evaluation of gas chromatography – electron ionization – full scan high resolution Orbitrap mass spectrometry for pesticide residue analysis

Energy Technology Data Exchange (ETDEWEB)

Mol, Hans G.J., E-mail: hans.mol@wur.nl; Tienstra, Marc; Zomer, Paul

2016-09-07

Gas chromatography with electron ionization and full scan high resolution mass spectrometry with an Orbitrap mass analyzer (GC-EI-full scan Orbitrap HRMS) was evaluated for residue analysis. Pesticides in fruit and vegetables were taken as an example application. The relevant aspects for GC-MS based residue analysis, including the resolving power (15,000 to 120,000 FWHM at m/z 200), scan rate, dynamic range, selectivity, sensitivity, analyte identification, and utility of existing EI-libraries, are assessed and discussed in detail. The optimum acquisition conditions in full scan mode (m/z 50–500) were a resolving power of 60,000 and an automatic-gain-control target value of 3E6. These conditions provided (i) an optimum mass accuracy: within 2 ppm over a wide concentration range, with/without matrix, enabling the use of ±5 ppm mass extraction windows (ii) adequate scan speed: minimum 12 scans/peak, (iii) an intra-scan dynamic range sufficient to achieve LOD/LOQs ≤0.5 pg in fruit/vegetable matrices (corresponding to ≤0.5 μg kg{sup −1}) for most pesticides. EI-Orbitrap spectra were consistent over a very wide concentration range (5 orders) with good match values against NIST (EI-quadrupole) spectra. The applicability for quantitative residue analysis was verified by validation of 54 pesticides in three matrices (tomato, leek, orange) at 10 and 50 μg/kg. The method involved a QuEChERS-based extraction with a solvent switch into iso-octane, and 1 μL hot splitless injection into the GC-HRMS system. A recovery between 70 and 120% and a repeatability RSD <10% was obtained in most cases. Linearity was demonstrated for the range ≤5–250 μg kg{sup −1}. The pesticides could be identified according to the applicable EU criteria for GC-HRMS (SANTE/11945/2015). GC-EI-full scan Orbitrap HRMS was found to be highly suited for quantitative pesticide residue analysis. The potential of qualitative screening to extend the scope makes it an attractive

Pesticide Residues in Canned Foods, Fruits, and Vegetables: The Application of Supercritical Fluid Extraction and Chromatographic Techniques in the Analysis

Directory of Open Access Journals (Sweden)

Mohamed H. EL-Saeid

2003-01-01

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

(DDT) and hexachlorohexane (HCH) pesticide residues in foodstuffs ...

African Journals Online (AJOL)

Dichloro-diphenyl-trichloro-ethane (DDT) and hexachlorohexane (HCH) pesticide residues in foodstuffs from markets in Ile-Ife, Nigeria. ... International Journal of Biological and Chemical Sciences ... Keywords: Dichlorodiphenyltrichloroethane, hexachlorocyclohexane, pesticide, residue, cowpea grain, yam chip.

Multi-pesticides residue analysis of grains using modified magnetic nanoparticle adsorbent for facile and efficient cleanup.

Science.gov (United States)

Liu, Zhenzhen; Qi, Peipei; Wang, Xiangyun; Wang, Zhiwei; Xu, Xiahong; Chen, Wenxue; Wu, Liyu; Zhang, Hu; Wang, Qiang; Wang, Xinquan

2017-09-01

A facile, rapid sample pretreatment method was developed based on magnetic nanoparticles for multi-pesticides residue analysis of grains. Magnetite (Fe 3 O 4 ) nanoparticles modified with 3-(N,N-diethylamino)propyltrimethoxysilane (Fe 3 O 4 -PSA) and commercial C18 were selected as the cleanup adsorbents to remove the target interferences of the matrix, such as fatty acids and non-polar compounds. Rice was used as the representative grain sample for method optimization. The amount of Fe 3 O 4 -PSA and C18 were systematically investigated for selecting the suitable purification conditions, and the simultaneous determination of 50 pesticides and 8 related metabolites in rice was established by liquid chromatography-tandem mass spectrometry. Under the optimal conditions, the method validation was performed including linearity, sensitivity, matrix effect, recovery and precision, which all satisfy the requirement for pesticides residue analysis. Compared to the conventional QuEChERS method with non-magnetic material as cleanup adsorbent, the present method can save 30% of the pretreatment time, giving the high throughput analysis possible. Copyright © 2017 Elsevier Ltd. All rights reserved.

Pesticide residues and bees--a risk assessment.

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Francisco Sanchez-Bayo

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

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

Science.gov (United States)

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

2014-02-01

This paper presents the first study of pesticide residue results in grain from Kazakhstan. A total of 80 samples: barley, oat, rye, and wheat were collected and tested in the accredited laboratory. Among 180 pesticides, 10 active substances were detected. Banned pesticides, such as DDTs, γ-HCH, aldrin and diazinon were found in cereal grain. Chlorpyrifos methyl and pirimiphos methyl were the most frequently detected residues. No residues were found in 77.5% of the samples, 13.75% contained pesticide residues at or below MRLs, and 8.75% above MRLs. The greatest percentage of samples with residues (29%) was noted for wheat, and the lowest for rye (20%). Obtained data were used to estimate potential health risks associated with exposure to these pesticides. The highest estimated daily intakes (EDIs) were as follows: 789% of the ADI for aldrin (wheat) and 49.8% of the ADI for pirimiphos methyl (wheat and rye). The acute risk from aldrin and tebuconazole in wheat was 315.9% and 98.7% ARfD, respectively. The results show that despite the highest EDIs of pesticide residues in cereals, the current situation could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring of pesticide residues in grain is recommended. Copyright © 2013 Elsevier Ltd. All rights reserved.

Food processing as a means for pesticide residue dissipation

Directory of Open Access Journals (Sweden)

Đorđević Tijana

2016-01-01

Full Text Available Pesticides are one of the major inputs used for increasing agricultural productivity of crops. However, their inadequate application may produce large quantities of residues in the environment and, once the environment is contaminated with pesticides, they may easily enter into the human food chain through plants, creating a potentially serious health hazard. Nowadays, consumers are becoming more aware of the importance of safe and high quality food products. Thus it is pertinent to explore simple, cost-effective strategies for decontaminating food from pesticides. Various food processing techniques, at industrial and/or domestical level, have been found to significantly reduce the contents of pesticide residues in most food materials. The extent of reduction varies with the nature of pesticides, type of commodity and processing steps. Pesticides, especially those with limited movement and penetration ability, can be removed with reasonable efficiency by washing, and the effectiveness of washing depends on pesticide solubility in water or in different chemical solvents. Peeling of fruit and vegetable skin can dislodge pesticide residues to varying degrees, depending on constitution of a commodity, chemical nature of the pesticide and environmental conditions. Different heat treatments (drying, pasteurization, sterilization, blanching, steaming, boiling, cooking, frying or roasting during various food preparation and preservation processes can cause losses of pesticide residues through evaporation, co-distillation and/or thermal degradation. Product manufactures, from the simplest grain milling, through oil extraction and processing, juicing/pureeing or canning of fruits and vegetables, to complex bakery and dairy production, malting and brewing, wine making and various fermentation processes, play a role in the reduction of pesticide contents, whereby each operation involved during processing usually adds to a cumulative effect of reduction of

Determination of Pesticide Residues in Cannabis Smoke

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Nicholas Sullivan

2013-01-01

Full Text Available 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.

Monitoring of Pesticide Residues in Commonly Used Fruits and Vegetables in Kuwait.

Science.gov (United States)

Jallow, Mustapha F A; Awadh, Dawood G; Albaho, Mohammed S; Devi, Vimala Y; Ahmad, Nisar

2017-07-25

The presence of pesticide residues in primary and derived agricultural products raises serious health concerns for consumers. The aim of this study was to assess the level of pesticide residues in commonly consumed fruits and vegetables in Kuwait. A total of 150 samples of different fresh vegetables and fruits were analyzed for the presence of 34 pesticides using the quick easy cheap effective rugged and safe (QuEChERS) multi-residue extraction, followed by gas chromatography-mass spectrometry (GC-MS) or liquid chromatography-tandem mass spectrometry (LC - MS / MS). Pesticide residues above the maximum residue limits (MRL) were detected in 21% of the samples and 79% of the samples had no residues of the pesticides surveyed or contained residues below the MRL. Multiple residues were present in 40% of the samples with two to four pesticides, and four samples were contaminated with more than four pesticide residues. Of the pesticides investigated, 16 were detected, of which imidacloprid, deltamethrin, cypermethrin, malathion, acetamiprid, monocrotophos, chlorpyrifos-methyl, and diazinon exceeded their MRLs. Aldrin, an organochlorine pesticide, was detected in one apple sample, with residues below the MRL. The results indicate the occurrence of pesticide residues in commonly consumed fruits and vegetables in Kuwait, and pointed to an urgent need to develop comprehensive intervention measures to reduce the potential health risk to consumers. The need for the regular monitoring of pesticide residues and the sensitization of farmers to better pesticide safety practices, especially the need to adhere to recommended pre-harvest intervals is recommended.

Monitoring of Pesticide Residues in Commonly Used Fruits and Vegetables in Kuwait

Directory of Open Access Journals (Sweden)

Mustapha F. A. Jallow

2017-07-01

Full Text Available The presence of pesticide residues in primary and derived agricultural products raises serious health concerns for consumers. The aim of this study was to assess the level of pesticide residues in commonly consumed fruits and vegetables in Kuwait. A total of 150 samples of different fresh vegetables and fruits were analyzed for the presence of 34 pesticides using the quick easy cheap effective rugged and safe (QuEChERS multi-residue extraction, followed by gas chromatography-mass spectrometry (GC-MS or liquid chromatography-tandem mass spectrometry (LC-MS/MS. Pesticide residues above the maximum residue limits (MRL were detected in 21% of the samples and 79% of the samples had no residues of the pesticides surveyed or contained residues below the MRL. Multiple residues were present in 40% of the samples with two to four pesticides, and four samples were contaminated with more than four pesticide residues. Of the pesticides investigated, 16 were detected, of which imidacloprid, deltamethrin, cypermethrin, malathion, acetamiprid, monocrotophos, chlorpyrifos-methyl, and diazinon exceeded their MRLs. Aldrin, an organochlorine pesticide, was detected in one apple sample, with residues below the MRL. The results indicate the occurrence of pesticide residues in commonly consumed fruits and vegetables in Kuwait, and pointed to an urgent need to develop comprehensive intervention measures to reduce the potential health risk to consumers. The need for the regular monitoring of pesticide residues and the sensitization of farmers to better pesticide safety practices, especially the need to adhere to recommended pre-harvest intervals is recommended.

Guidelines for selection and presentation of residue values of pesticides

NARCIS (Netherlands)

Velde-Koerts T van der; Hoeven-Arentzen PH van; Ossendorp BC; RIVM-SIR

2004-01-01

Pesticide residue assessments are executed to establish legal limits, called Maximum Residue Limits (MRLs). MRLs are derived from the results of these pesticide residue trials, which are performed according to critical Good Agricultural Practice. Only one residue value per residue trial may be

Assessment of pesticide residues in tomatoes and watermelons ...

African Journals Online (AJOL)

This study investigated the levels of pesticide residues in selected fruits from major markets in Dar es Salaam city. Samples of tomatoes and watermelons were analysed for eighteen organochlorine, organophosphorus and pyrethroid pesticide residues. Extraction was performed using acetone followed by dichloromethane: ...

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

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Jelena Milinović

2007-01-01

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

Qualitative screening method for pesticide residues detection in fruits and vegetables

Directory of Open Access Journals (Sweden)

Iván Mauricio Huérfano Barco

2018-01-01

Full Text Available Because of the importance of developing methodologies that allow agricultural residues analysis, a rapid screening qualitative method for the determination of pesticides residues in fruits and vegetables was validated. The methodology was based on the European QuEChERS extraction method with an additional cleaning step by gel permeation chromatography (GPC, which helped to reduce the number of matrix components in the final extract. The analysis was carried out by gas chromatography coupled to mass spectrometry with a single quadrupole analyzer. The methodology was appropriate for the qualitative analysis of 31 pesticides at their respective maximum residue limits. Consistent results were obtained with respect to a quantitative routine methodology in the analysis of real samples, hence the methodology was proven to be a good alternative for the fast analysis of these contaminants in fruits and vegetables.

Pesticide residues in orange fruit from citrus orchards in Nuevo Leon State, Mexico.

Science.gov (United States)

Suárez-Jacobo, Angela; Alcantar-Rosales, Victor Manuel; Alonso-Segura, Diana; Heras-Ramírez, Maria; Elizarragaz-De La Rosa, Dalau; Lugo-Melchor, Ofelia; Gaspar-Ramirez, Octavio

2017-09-01

Some international organisations established maximum residue limits (MRLs) in food to protect human health. Mexico lacks regulations in this matter, affecting national and international trade from agroindustry. The aim of this study was to diagnose pesticide residues in oranges from Nuevo Leon, México, in citrus orchards. In May 2014, 100 orange fruit samples were taken randomly from orchards and subjected to analysis for 93 pesticides at residual level by GC/QQQ-MS and LCQ-TOF-MS. Results showed the presence of 15 pesticide residues in the samples. The comparison of the residual levels of pesticides found in orange samples among the MRLs allowed by USA, EU and Japanese regulations demonstrated that all samples were below MRLs issued by USA and Japan. Some orange samples were above MRLs issued by the EU. This provides a basis to establish strategies in order to satisfy International Standards to protect human health and encourage Food Safety in Mexico.

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

Directory of Open Access Journals (Sweden)

Rada Đurović

2011-01-01

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.

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

International Nuclear Information System (INIS)

Ibrahim, A. B. H.

2004-03-01

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)

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

Science.gov (United States)

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

2005-01-01

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

Evaluation of Some Pesticide Residues in Stored Beans in Jos ...

African Journals Online (AJOL)

Qualitative and quantitative analysis were performed by gas chromatography with electron capture and flame ionization. All the 3 samples (100%) contained pesticide residues beyond the allowed beans maximum residue levels (MRLs) of 0.01 mg/kg and 0.2 mg/kg, respectively, for chlorpyrifos and endosulfan. The present ...

Overall and class-specific scores of pesticide residues from fruits and vegetables as a tool to rank intake of pesticide residues in United States: A validation study.

Science.gov (United States)

Hu, Yang; Chiu, Yu-Han; Hauser, Russ; Chavarro, Jorge; Sun, Qi

2016-01-01

Pesticide residues in fruits and vegetables are among the primary sources of pesticide exposure through diet, but the lack of adequate measurements hinder the research on health effects of pesticide residues. Pesticide Residue Burden Score (PRBS) for estimating overall dietary pesticide intake, organochlorine pesticide score (OC-PRBS) and organophosphate pesticide score (OP-PRBS) for estimating organochlorine and organophosphate pesticides-specific intake, respectively, were derived using U.S. Department of Agriculture Pesticide Data Program data and National Health and Nutrition Examination Survey (NHANES) food frequency questionnaire data. We evaluated the performance of these scores by validating the scores against pesticide metabolites measured in urine or serum among 3,679 participants in NHANES using generalized linear regression. The PRBS was positively associated with a score summarizing the ranks of all pesticide metabolites in a linear fashion (p for linear trend trend trend 0.07) for the OC-PRBS. The PRBS and OP-PRBS had similar performance when they were derived from fruits and vegetables with high vs. low pesticide residues, respectively (p for trend trend 0.07) than from less contaminated Fruits and vegetables (p for trend 0.63), although neither of the associations achieved statistical significance. The PRBS and the class-specific scores for two major types of pesticides were significantly associated with pesticide biomarkers. These scores can reasonably rank study participants by their pesticide residue exposures from fruits and vegetables in large-scale environmental epidemiological studies. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

DEFF Research Database (Denmark)

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

2009-01-01

Seven pesticide application strategies were investigated to control apple scab (Venturia inaequalis) and powdery mildew (Podosphaera leucotricha) and, at the same time.. fulfil the new quality standards implemented by some German retailers. These demand that pesticide residues should be below 80....... 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...

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

Science.gov (United States)

Cunha, Sara C; Lehotay, Steven J; Mastovska, Katerina; Fernandes, José O; Beatriz, Maria; Oliveira, P P

2007-03-01

This paper describes the use of a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for extraction and cleanup of 16 pesticide residues of interest in olives and olive oil. These products contain a high lipid content, which can adversely affect pesticide recoveries and harm traditional chromatographic systems. For extraction, the main factors (oil and water content) were studied and optimized in experiments to maximize pesticide recoveries. Dispersive SPE with different sorbents was also investigated to minimize matrix coextractives and interferences. For analysis, a new automated DSI device was tested in GC-MS to avoid nonvolatile coextractives from contaminating the instrument. LC-MS/MS with positive ESI was used for those pesticides that were difficult to detect by GC-MS. The final method was validated for olives in terms of recoveries, repeatabilities, and reproducibilities using both detection techniques. The results demonstrated that the method achieved acceptable quantitative recoveries of 70-109% with RSDs < 20% for DSI-GC-MS and 88-130% with RSDs < 10% for LC-MS/MS, and LOQ at or below the regulatory maximum residue limits for the pesticides were achieved.

Pesticide Residues and Bees – A Risk Assessment

Science.gov (United States)

Sanchez-Bayo, Francisco; Goka, Koichi

2014-01-01

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

Chlorinated pesticide residues in marine sediments

Digital Repository Service at National Institute of Oceanography (India)

Sarkar, A.; SenGupta, R.

of pesticide in contaminated river water into the Bay of Bengal. Con centration ranges of all these pesticide residues detected were, aldrine: 0.02-0.53, gamma BHC: 0.01-0.21, dieldrine: 0.05-0.51, and total DDT: 0.02-0.78, all in mu g g sup(-1) (wet wt)....

Pesticide Residues in Food: Attitudes, Beliefs, and Misconceptions among Conventional and Organic Consumers.

Science.gov (United States)

Koch, Severine; Epp, Astrid; Lohmann, Mark; Böl, Gaby-Fleur

2017-12-01

Pesticide use and pesticide residues in foods have been the subject of controversial public discussions and media coverage in Germany. Against this background, a better understanding of public risk perceptions is needed to promote efficient public health communication. To this end, this study captures the German public's perception of pesticide residues in foods. A representative sample of the population aged 14 years and older (n = 1,004) was surveyed via computer-assisted telephone interviewing on their attitudes and knowledge with regard to pesticide residues. Based on questions regarding their typical consumer behavior, respondents were classified into conventional and organic consumers to identify differences as well as similarities between these two consumer types. As assessed with an open-ended question, both organic and conventional consumers viewed pesticides, chemicals, and toxins as the greatest threats to food quality and safety. Evaluating the risks and benefits of pesticide use, more than two-thirds of organic consumers (70%) rated the risks as greater than the benefits, compared with just over one-half of conventional consumers (53%). Concern about the detection of pesticide residues in the food chain and bodily fluids was significantly higher among organic compared with conventional consumers. Only a minority of respondents was aware that legal limits for pesticide residues (referred to as maximum residue levels) exist, with 69% of organic and 61% of conventional consumers believing that the presence of pesticide residues in foods is generally not permitted. A lack of awareness of maximum residue levels was associated with heightened levels of concern about pesticide residues. Finally, general exposure to media reporting on pesticide residues was associated with more frequent knowledge of legal limits for pesticide residues, whereas actively seeking information on pesticide residues was not. The possible mechanisms underlying these findings are

Review of sample preparation techniques for the analysis of pesticide residues in soil.

Science.gov (United States)

Tadeo, José L; Pérez, Rosa Ana; Albero, Beatriz; García-Valcárcel, Ana I; Sánchez-Brunete, Consuelo

2012-01-01

This paper reviews the sample preparation techniques used for the analysis of pesticides in soil. The present status and recent advances made during the last 5 years in these methods are discussed. The analysis of pesticide residues in soil requires the extraction of analytes from this matrix, followed by a cleanup procedure, when necessary, prior to their instrumental determination. The optimization of sample preparation is a very important part of the method development that can reduce the analysis time, the amount of solvent, and the size of samples. This review considers all aspects of sample preparation, including extraction and cleanup. Classical extraction techniques, such as shaking, Soxhlet, and ultrasonic-assisted extraction, and modern techniques like pressurized liquid extraction, microwave-assisted extraction, solid-phase microextraction and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) are reviewed. The different cleanup strategies applied for the purification of soil extracts are also discussed. In addition, the application of these techniques to environmental studies is considered.

Review on the Influences of Bagging Treatment on Pesticide Residue in Fruits

OpenAIRE

ZHAO Xiao-yun; XIE De-fang

2018-01-01

At present, bagging technology has been widely applicated in fruit cultivation. Impact of bagging treatment on the pesticide residues have different results. On the basis of existing achievements, this paper systematically analyzed the influence of different bagging treatments on pesticide residues:such as different ways of applying pesticide, pesticide concentration, number of applying pesticide; bagging materials, bagged layer; the type of pesticide(systemic pesticide, nonendoscopic pestici...

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)

Castillo, L.E.; Ruepert, C.; Alfaro, A.R.; Solis, E.

1999-01-01

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)

Determination of Pesticides Residues in Cucumbers Grown in Greenhouse and the Effect of Some Procedures on Their Residues.

Science.gov (United States)

Leili, Mostafa; Pirmoghani, Amin; Samadi, Mohammad Taghi; Shokoohi, Reza; Roshanaei, Ghodratollah; Poormohammadi, Ali

2016-11-01

The objective of this study was to determine the residual concentrations of ethion and imidacloprid in cucumbers grown in greenhouse. The effect of some simple processing procedures on both ethion and imidacloprid residues were also studied. Ten active greenhouses that produce cucumber were randomly selected. Ethion and imidacloprid as the most widely used pesticides were measured in cucumber samples of studied greenhouses. Moreover, the effect of storing, washing, and peeling as simple processing procedures on both ethion and imidacloprid residues were investigated. One hour after pesticide application; the maximum residue levels (MRLs) of ethion and imidacloprid were higher than that of Codex standard level. One day after pesticide application, the levels of pesticides were decreased about 35 and 31% for ethion and imidacloprid, respectively, which still were higher than the MRL. Washing procedure led to about 51 and 42.5% loss in ethion and imidacloprid residues, respectively. Peeling procedure also led to highest loss of 93.4 and 63.7% in ethion and imidacloprid residues, respectively. The recovery for both target analytes was in the range between 88 and 102%. The residue values in collected samples one hour after pesticides application were higher than standard value. The storing, washing, and peeling procedures lead to the decrease of pesticide residues in greenhouse cucumbers. Among them, the peeling procedure has the greatest impact on residual reduction. Therefore, these procedures can be used as simple and effective processing techniques for reducing and removing pesticides from greenhouse products before their consumption.

Monitoring of Some Pesticides Residue in Consumed tea in Tehran Market

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Maryam Amirahmadi

2013-01-01

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

Monitoring of some pesticides residue in consumed tea in Tehran market

Directory of Open Access Journals (Sweden)

Hamedani Morteza Pirali

2013-01-01

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

Determination of Pesticide Residues in Cannabis Smoke

OpenAIRE

Nicholas Sullivan; Sytze Elzinga; Jeffrey C. Raber

2013-01-01

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

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

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Indraningsih

2006-06-01

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

Revealing Pesticide Residues Under High Pesticide Stress in Taiwan's Agricultural Environment Probed by Fresh Honey Bee (Hymenoptera: Apidae) Pollen.

Science.gov (United States)

Nai, Yu-Shin; Chen, Tsui-Yao; Chen, Yi-Cheng; Chen, Chun-Ting; Chen, Bor-Yann; Chen, Yue-Wen

2017-10-01

Significant pesticide residues are among the most serious problems for sustainable agriculture. In the beekeeping environment, pesticides not only impact a honey bee's survival, but they also contaminate bee products. Taiwan's agricultural environment has suffered from pesticide stress that was higher than that found in Europe and America. This study deciphered problems of pesticide residues in fresh honey bee pollen samples collected from 14 monitoring apiaries in Taiwan, which reflected significant contaminations within the honey bee population. In total, 155 pollen samples were screened for 232 pesticides, and 56 pesticides were detected. Among the residues, fluvalinate and chlorpyrifos showed the highest concentrations, followed by carbendazim, carbaryl, chlorfenapyr, imidacloprid, ethion, and flufenoxuron. The average frequency of pesticide residues detected in pollen samples was ca. 74.8%. The amounts and types of pesticides were higher in winter and in southwestern Taiwan. Moreover, five of these pollen samples were contaminated with 11-15 pesticides, with average levels between 1,560 and 6,390 μg/kg. Compared with the literature, this study emphasized that pollen gathered by honey bee was highly contaminated with more pesticides in Taiwan than in the America, France, and Spain. The ubiquity of pesticides in the pollen samples was likely due to the field applications of common pesticides. Recently, the Taiwanese government began to improve the pesticide policy. According to the resurvey data in 2016, there were reductions in several pesticide contamination parameters in pollen samples from west to southwest Taiwan. A long-term investigation of pollen pesticide residues should be conducted to inspect pesticides usage in Taiwan's agriculture. © The Author 2017. Published by Oxford University Press on behalf of Entomological Society of America. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

Science.gov (United States)

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

2017-01-01

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

Assessment of pesticide residues in vegetables from the Western Usambara and Uruguru Mountains in Tanzania.

Science.gov (United States)

Mtashobya, Lewis A

2017-09-25

Assessment of levels of pesticide residues in vegetables was carried out in some villages in the Western Usambara and Uluguru Mountains of Tanzania where varieties of vegetables are grown. Tomatoes and cabbages were the most popular enterprise grown all year round and therefore were selected as the model crops for this study. Analysis of the cleaned sample extracts on a gas chromatography with electron capture detector (GC-ECD) and confirmation on the Gas chromatography-mass spectrometry (GC-MS) revealed dominance of organochlorine pesticides. Organophosphorous pesticides (parathion and marathion) were only detected in some samples, however, in most cases with higher concentrations compared to organochlorine pesticides. Levels of pesticide residues detected in vegetables were up to: parathion 5.07 μg/Kg, marathion 3.73 μg/Kg, α-endosulfan 0.32 μg/Kg, β-endosulfan 0.53 μg/Kg, dieldrin 1.36 μg/Kg, γ-HCH 0.25 μg/Kg, α-HCH 0.09 μg/Kg, and p, p'-DDT 0.64 μg/Kg. These results clearly show that vegetables are contaminated with different pesticide residues. However, the total levels of pesticide residues in both tomatoes and cabbages are lower than their respective codex alimentarius maximum residue levels (MRLs). This means that the vegetables produced in the area are suitable for human consumption.

Determination of organophosphorus pesticide residues in tomatoes by gas chromatography

International Nuclear Information System (INIS)

Souissi, Sihem

2010-01-01

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

Impact of toxic heavy metals and pesticide residues in herbal products

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Nema S. Shaban

2016-03-01

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

Removal of six pesticide residues in cowpea with alkaline electrolysed water.

Science.gov (United States)

Han, Yongtao; Song, Le; An, Quanshun; Pan, Canping

2017-06-01

Reduction of six pesticide residues (isoprocarb, chlorpyrifos, bifenthrin, beta-cypermethrin, difenoconazole and azoxystrobin) in cowpea by alkaline electrolysed water (AlEW) solutions with different pH was investigated. The commonly used washing treatments in household processing were used for comparison. The residue magnitudes were determined by gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). Results showed that the removal effect of AlEW solution on the six pesticides was superior to tap water, 5% sodium chloride, 5% sodium carbonate and 5% acetic acid solution. AlEW with pH 12.2 had more potential to eliminate the six pesticides in cowpeas. Moreover, the reduction of pesticide residues gradually increased with the increase of washing time. This study demonstrated that AlEW solution with pH of 12.2 could be used to reduce pesticide residues on fresh cowpea samples. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

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

DEFF Research Database (Denmark)

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

2011-01-01

% 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...

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

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Spiridon Kintzios

2008-04-01

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

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

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Judy Y Wu

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

Washing effects of limonene on pesticide residues in green peppers.

Science.gov (United States)

Lu, Hai-Yan; Shen, Yan; Sun, Xing; Zhu, Hong; Liu, Xian-Jin

2013-09-01

The presence of pesticide residues in food has caused much concern. The low health risks and environmental impacts of limonene make it a very interesting solvent for use in green chemistry. Washing effects of limonene on pesticide residues of methyl chlorpyrifos, chlorothalonil, chlorpyrifos, fenpropathrin and deltamethrin were investigated in green pepper. Results showed that washing with a low concentration of limonene for 5 min (where LOQ is limit of quantitation) caused 53.67%, limonene for 10 min produced 55.90%, limonene for 5 min was the optimal treatment for elimination of pesticide residues in green pepper, considering effect and treatment time as well as cost. © 2013 Society of Chemical Industry.

Determination of Profenofos Pesticidal Residue in Lettuce (Lactuca sativa L. by Gas Chromatographic Method

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Yohannes Alen

2015-05-01

Full Text Available The determination of profenofos pesticidal residue in the lettuce (Lactuca sativa L. by using gas chromatography using flame photometric detector (FPD had been investigated. The lettuce was collected from Padang Luar area, Agam distric, West Sumatera. Sample for determination of profenofos residue divided into three groups: unwashed (A, washed with water (B, and washed with detergent (C. Maceration with sonication was used for the extraction using ethylacetateas a solvent. The results showed that profenofos pesticide residue in sample A, B and C were 0.204, 0.080 and 0.061 ppm, respectively. These profenofos pesticidal residue are over than the Maximum Residue Limits (MRL that established by The Japan Food Chemical Research Foundation (0.05 ppm even though World Health Organization (WHO has not established Maximum Residue Limits (MRL profenofos on lettuce. Based on the statistical analysis one-way method (Anova using SPSS 20.0 showed that there was a significant concentrations difference between lettuce A from lettuce B and lettuce C with p < 0.05.

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

Science.gov (United States)

Bajwa, Usha; Sandhu, Kulwant Singh

2014-02-01

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

Distribution of 19 organochlorinated pesticides residues in ginseng ...

African Journals Online (AJOL)

The organochlorinated pesticides widely applied and still remains in soils, has become toxic to ginseng production in Jilin Province. In this study, 19 trace organochlorinated pesticide residues in five types of ginseng products and soil samples from four ginseng production areas were analyzed using a gas ...

Types of pesticides and determination of their residues

International Nuclear Information System (INIS)

Kassem, A.R.

2010-01-01

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)

Matrix effect in analysis of pesticide residues in fruits and vegetables by high performance liquid chromatography with quadrupole-time of flight mass spectrometry

Directory of Open Access Journals (Sweden)

Andoralov A.M.

2017-03-01

Full Text Available For modern food safety control are using techniques that allow to determinate a large number of components. So for determination of pesticide residues in fruits and vegetables commonly used methods of gas and liquid chromatography with time-of-flight mass-spectrometric detection. This system allows to carry out quantitative determination several hundreds of pesticides and their identification by the characteristic fragments of the mass spectrum. The main problem when using mass spectrometric detection is a matrix effect, which is caused by the influence of matrix components extracted with pesticides from the sample. In this work, attempts have been made to reduce the influence of the matrix in the analysis of pesticide residues by high performance liquid chromatography with time of flight mass spectrometry (HPLC / TOFMS.

Effect of washing on pesticide residues in olives.

Science.gov (United States)

Guardia-Rubio, M; Ayora-Cañada, M J; Ruiz-Medina, A

2007-03-01

The present work aims at contributing to the knowledge of the fate of 5 pesticides in olives in order to evaluate how washing may affect the presence of these residues in this fruit (and consequently in olive oil). For this purpose, olives were sprayed with commercial formulations containing the active ingredients and a series of analyses were performed for 64 d by using gas chromatography with mass spectrometric detection. Selected pesticides, ranked by their importance, were diuron, terbuthylazine, simazine, alpha-endosulfan, and beta-endosulfan. The pesticide fraction, which was not removable from olives by washing, increased with time after treatment until their degradation started at week 6. Washing performed 1 d after treatment was the most effective in reducing residues, especially for simazine. Consequently, the washing step performed in olive mills could be effective in removing those herbicide residues present in olives as a consequence of contact with contaminated soil for a short time. This happens when olives are dropped and harvested off the ground by means of brushes or suction equipment.

Response of microbial communities to pesticide residues in soil restored with Azolla imbricata.

Science.gov (United States)

Lu, Xiao-Ming; Lu, Peng-Zhen

2018-01-01

Under conditions of Azolla imbricata restoration, the high-throughput sequencing technology was employed to determine change trends of microbial community structures in the soil that had undergone long-term application of pesticides. The relationship between the content of pesticide residues in the soil and the microbial community structure was analyzed. The results indicated that the microbial diversity was strongly negatively correlated with the contents of pesticide residues in the soil. At a suitable dosage of 5 kg fresh A. imbricata per square meter of soil area, the soil microbial diversity increased by 12.0%, and the contents of pesticide residues decreased by 26.8-72.1%. Sphingobacterium, Sphingopyxis, Thermincola, Sphingobium, Acaryochloris, Megasphaera, Ralstonia, Pseudobutyrivibrio, Desulfitobacterium, Nostoc, Oscillochloris, and Aciditerrimonas may play major roles in the degradation of pesticide residues. Thauera, Levilinea, Geothrix, Thiobacillus, Thioalkalispira, Desulfobulbus, Polycyclovorans, Fluviicola, Deferrisoma, Erysipelothrix, Desulfovibrio, Cytophaga, Vogesella, Zoogloea, Azovibrio, Halomonas, Paludibacter, Crocinitomix, Haliscomenobacter, Hirschia, Silanimonas, Alkalibacter, Woodsholea, Peredibacter, Leptolinea, Chitinivorax, Candidatus_Lumbricincola, Anaerovorax, Propionivibrio, Parasegetibacter, Byssovorax, Runella, Leptospira, and Nitrosomonas may be indicators to evaluate the contents of pesticide residues.

A Design of Portable Pesticide Residue Detection System Based on the Enzyme Electrode

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Xia SUN

2013-03-01

Full Text Available In this paper, a portable detection system was designed based on amperometric acetylcholinesterase biosensor for rapidly detecting pesticide residues in fruits and vegetables. There were potentiostat, three electrode system, differential amplification circuit and double integral analog to digital (A/D circuit modules in this system. The measurement principle of this system was depended on the weak current from enzyme catalyzing substrate in acetylcholinesterase biosensor for detecting pesticide residues. The weak current generated by the enzyme biosensor was changed into 0-5 V standard voltage signal by this system as an output signal. The proposed system was investigated with eight kinds of standard pesticide of different concentrations, the results showed that the detection limits were all lower than 10 ng/kg. Thus, a new effective home-made system of detecting pesticide residues with portable, easy-to-use, fast response was developed. The pesticide residues rapid detection system can collect the weak current signal generated by electrochemical reaction and on-site detect the concentration of pesticide residues in real fruits and vegetables samples.

Distribution of pesticide residues in soil and uncertainty of sampling.

Science.gov (United States)

Suszter, Gabriela K; Ambrus, Árpád

2017-08-03

Pesticide residues were determined in about 120 soil cores taken randomly from the top 15 cm layer of two sunflower fields about 30 days after preemergence herbicide treatments. Samples were extracted with acetone-ethyl acetate mixture and the residues were determined with GC-TSD. Residues of dimethenamid, pendimethalin, and prometryn ranged from 0.005 to 2.97 mg/kg. Their relative standard deviations (CV) were between 0.66 and 1.13. The relative frequency distributions of residues in soil cores were very similar to those observed in root and tuber vegetables grown in pesticide treated soils. Based on all available information, a typical CV of 1.00 was estimated for pesticide residues in primary soil samples (soil cores). The corresponding expectable relative uncertainty of sampling is 20% when composite samples of size 25 are taken. To obtain a reliable estimate of the average residues in the top 15 cm layer of soil of a field up to 8 independent replicate random samples should be taken. To obtain better estimate of the actual residue level of the sampled filed would be marginal if larger number of samples were taken.

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

Science.gov (United States)

Mekonen, Seblework; Ambelu, Argaw; Spanoghe, Pieter

2015-09-30

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

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

International Nuclear Information System (INIS)

Fianko, J.R.

2010-01-01

The Densu River Basin is one of the largest agricultural areas in Ghana. About 80% of people living in this area rely on agricultural activities for subsistence. The practice of using pesticides such as organochlorines, organophosphates, carbamates, pyrethroids and several others in agriculture and public health programs have raised concerns about potentially adverse effects on human health and the environment. Assessment of human health implications of non-point sources within a river basin include pesticide residues analysis of water, sediment and fish and monitoring of physico-chemical parameters in waters that serve as source of drinking water for the entire community within the basin. In this study, a field survey was conducted to assess farmers' knowledge of safe handling and use of pesticides. Nutrient chemistry and surface water characteristics of the Densu River and its tributaries, type and levels of pesticide residues and their trends in water, sediment and fish in the basin were also evaluated. The study also assessed the health risk associated with pesticide contamination of fish from the Basin as well as the relationship between land use and groundwater contamination. Generally surface and ground water bodies in the Densu River basin were found to be polluted with respect to nutrients and pesticides. Waters from the basin were found to be fresh, slightly acidic, and weakly mineralized with low chemical constituents. Nitrate (NO 3- N) levels in surface water ranged between 0.12 - 31.07 mgL -1 while ammonia was between 0.01 - 2.10 mgL -1 and that of phosphate was 0.012 - 2.45 mgL -1 . Pesticide residues and metabolites detected in water, sediment and fish samples from the Densu River Basin were organochlorines. In an average 96% of fish samples, 13.69% of sediment and 3.30% of water samples, at least one pesticide residue was detected per sample. Of the numerous pesticides evaluated, γ -HCH, DDT, aldrin, dieldrin, DDE, endosulfan sulphate, �

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-11-01

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

Organochlorine pesticide residues in strawberries from integrated pest management and organic farming.

Science.gov (United States)

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

2011-07-27

A rapid, specific, and sensitive method based on the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) method and a cleanup using dispersive solid-phase extraction with MgSO(4), PSA, and C18 sorbents has been developed for the routine analysis of 14 pesticides in strawberries. The analyses were performed by three different analytical methodologies: gas chromatography (GC) with electron capture detection (ECD), mass spectrometry (MS), and tandem mass spectrometry (MS/MS). The recoveries for all the pesticides studied were from 46 to 128%, with relative standard deviation of residue limits (MRL) accepted in Portugal for organochlorine pesticides (OCP). A survey study of strawberries produced in Portugal in the years 2009-2010 obtained from organic farming (OF) and integrated pest management (IPM) was developed. Lindane and β-endosulfan were detected above the MRL in OF and IPM. Other OCP (aldrin, o,p'-DDT and their metabolites, and methoxychlor) were found below the MRL. The OCP residues detected decreased from 2009 to 2010. The QuEChERS method was successfully applied to the analysis of strawberry samples.

Quantum Dots Applied to Methodology on Detection of Pesticide and Veterinary Drug Residues.

Science.gov (United States)

Zhou, Jia-Wei; Zou, Xue-Mei; Song, Shang-Hong; Chen, Guan-Hua

2018-02-14

The pesticide and veterinary drug residues brought by large-scale agricultural production have become one of the issues in the fields of food safety and environmental ecological security. It is necessary to develop the rapid, sensitive, qualitative and quantitative methodology for the detection of pesticide and veterinary drug residues. As one of the achievements of nanoscience, quantum dots (QDs) have been widely used in the detection of pesticide and veterinary drug residues. In these methodology studies, the used QD-signal styles include fluorescence, chemiluminescence, electrochemical luminescence, photoelectrochemistry, etc. QDs can also be assembled into sensors with different materials, such as QD-enzyme, QD-antibody, QD-aptamer, and QD-molecularly imprinted polymer sensors, etc. Plenty of study achievements in the field of detection of pesticide and veterinary drug residues have been obtained from the different combinations among these signals and sensors. They are summarized in this paper to provide a reference for the QD application in the detection of pesticide and veterinary drug residues.

Global Harmonization of Maximum Residue Limits for Pesticides.

Science.gov (United States)

Ambrus, Árpád; Yang, Yong Zhen

2016-01-13

International trade plays an important role in national economics. The Codex Alimentarius Commission develops harmonized international food standards, guidelines, and codes of practice to protect the health of consumers and to ensure fair practices in the food trade. The Codex maximum residue limits (MRLs) elaborated by the Codex Committee on Pesticide Residues are based on the recommendations of the FAO/WHO Joint Meeting on Pesticides (JMPR). The basic principles applied currently by the JMPR for the evaluation of experimental data and related information are described together with some of the areas in which further developments are needed.

Study of Organochlorinated Pesticide Residues and Polychlorinated Biphenyls in Soil Samples

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MSc. Vlora Gashi

2013-12-01

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

De-contamination of pesticide residues in food by ionizing radiation

International Nuclear Information System (INIS)

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

2012-01-01

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

Effectiveness of Commercial and Homemade Washing Agents in Removing Pesticide Residues on and in Apples.

Science.gov (United States)

Yang, Tianxi; Doherty, Jeffery; Zhao, Bin; Kinchla, Amanda J; Clark, John M; He, Lili

2017-11-08

Removal of pesticide residues from fresh produce is important to reduce pesticide exposure to humans. This study investigated the effectiveness of commercial and homemade washing agents in the removal of surface and internalized pesticide residues from apples. Surface-enhanced Raman scattering (SERS) mapping and liquid chromatography tandem mass spectrometry (LC-MS/MS) methods were used to determine the effectiveness of different washing agents in removing pesticide residues. Surface pesticide residues were most effectively removed by sodium bicarbonate (baking soda, NaHCO 3 ) solution when compared to either tap water or Clorox bleach. Using a 10 mg/mL NaHCO 3 washing solution, it took 12 and 15 min to completely remove thiabendazole or phosmet surface residues, respectively, following a 24 h exposure to these pesticides, which were applied at a concentration of 125 ng/cm 2 . LC-MS/MS results showed, however, that 20% of applied thiabendazole and 4.4% of applied phosmet had penetrated into the apples following the 24 h exposure. Thiabendazole, a systemic pesticide, penetrated 4-fold deeper into the apple peel than did phosmet, a non-systemic pesticide, which led to more thiabendazole residues inside the apples, which could not be washed away using the NaHCO 3 washing solution. This study gives us the information that the standard postharvest washing method using Clorox bleach solution for 2 min is not an effective means to completely remove pesticide residues on the surface of apples. The NaHCO 3 method is more effective in removing surface pesticide residues on apples. In the presence of NaHCO 3 , thiabendazole and phosmet can degrade, which assists the physical removal force of washing. However, the NaHCO 3 method was not completely effective in removing residues that have penetrated into the apple peel. The overall effectiveness of the method to remove all pesticide residues diminished as pesticides penetrated deeper into the fruit. In practical application

Evaluation of pesticide residues in oranges from São Paulo, Brazil

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Viviane Emi NAKANO

2016-01-01

Full Text Available Pesticides in “PERA” orange samples (N = 57 from São Paulo City, Brazil were assessed and the pesticide intake contribution was estimated for chronic risk assessment. Seventy-six pesticides were evaluated by the gas chromatography multi-residue method, including isomers and metabolites (4.332 determinations. The mean recoveries at the limit of quantification level were in the range of 72-115% and the relative standard deviation for five replicate samples was 1-11%. The limits of detection and quantification ranged from 0.005 to 0.4 mg.kg−1 and from 0.01 to 0.8 mg.kg−1, respectively. Pesticides were found in 42.1% of the samples at levels ranging from 0.06 to 2.9 mg.kg−1. Of the contaminated samples, 3.5% contained residues (bifenthrin and clofentezine above the maximum residue level and 12.3% contained unauthorized pesticides (azinphos-ethyl, parathion, myclobutanil, profenofos, and fenitrothion. The estimated risk characterization for orange intake by adults and children, respectively, ranged from 0.04 to 6.6% and from 0.1 to 26.5% of the acceptable daily intake. The detection of irregular residues emphasizes the need for better implementation of Good Agriculture Practices and greater control of formulated products. Other pesticides surveyed did not pose a health risk due to consumption.

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

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Korrapati Kotinagu

2015-04-01

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

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

Science.gov (United States)

Kotinagu, Korrapati; Krishnaiah, Nelapati

2015-04-01

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

Pesticide residues analysis in water samples of Nagarpur and Saturia Upazila, Bangladesh

Science.gov (United States)

Hasanuzzaman, M.; Rahman, M. A.; Islam, M. S.; Salam, M. A.; Nabi, M. R.

2018-03-01

Pesticides used to protect the crops from pest attack in the agricultural fields pose harmful effect to the non-target organisms such as human and many other aquatic and terrestrial organisms either directly or indirectly through food chain. The present study was conducted to monitor a total of seven pesticide residues under organochlorine, organophosphorus and carbamate pesticides in three different sources of pond water, paddy field water and tube-well water from Nagarpur Upazila and paddy field water in the company of Dhaleshwari and Gazikhali river water from Saturia Upazila, Bangladesh. A total of 40 water samples were analyzed using high-performance liquid chromatography equipped with ultraviolet detector. Among the organophosphorus pesticides, diazinon was detected in eight water samples at a concentration ranging from 4.11 to 257.91 μg/l whereas, malathion was detected only in one water sample at a concentration of 84.64 μg/l and chlorpyrifos pesticide was also detected only in one water sample and the concentration was 37.3 μg/l. Trace amount of carbaryl was identified but it was below the detection limit. None of the tested water samples was found to be contaminated with DDT or its metabolites (DDE and DDD). The water samples contaminated with the suspected pesticides were above the acceptable limit except for the fish pond samples of Sahabatpur and Dubaria union. To control the misuse of pesticides and to reduce the possible health risk, appropriate control systems of pests such as integrated pest management system should be implemented immediately by the authorities of the country.

Effect of processing on the disappearance of pesticide residues in fresh-cut lettuce: Bioavailability and dietary risk.

Science.gov (United States)

Camara, Miguel A; Barba, Alberto; Cermeño, Sandra; Martinez, Gracia; Oliva, Jose

2017-12-02

The aim of this research is to establish the processing factors of six pesticides durong the preparation of fresh-cut lettuce and to assess the risk of ingestion of pesticide residues associated with the consumption of the same. A field study was carried out on the dissipation of three insecticides (imidacloprid, tebufenozide, cypermethrin) and three fungicides (metalaxyl, tebuconazole, azoxystrobin) during treatment conditions simulating those used for commercial fresh-cut lettuce. A simultaneous residue analysis method is validated using QuEChERS extraction with acetonitrile and CG-MS and LC-MS/MS analysis. The residues detected after field application never exceed the established Maximum Residue Limits. The processing factors were generally less than 1 (between 0.34 for tebufenozide and 0.53 for imidacloprid), indicating that the process, as a whole, considerably reduces residue levels in processed lettuce compared to fresh lettuce. It is confirmed that cutting, followed by washing and drying, considerably reduces the residues. A matrix effect in the dialyzation of the pesticides is observed and the in vitro study of bioavailability establishes a low percentage of stomach absorption capacity (lettuce showed no concerns for consumer health.

Matrix-Matching as an Improvement Strategy for the Detection of Pesticide Residues.

Science.gov (United States)

Giacinti, Géraldine; Raynaud, Christine; Capblancq, Sophie; Simon, Valérie

2016-05-01

More than 90% of the pesticides residues in apples are located in the peel. We developed a gas chromatography/ion trap tandem mass spectrometry method for investigating all detectable residues in the peel of 3 apple varieties. Sample preparation is based on the use of the Quick Easy Cheap Effective Rugged and Safe method on the whole fruit, the flesh, and the peel. Pesticide residues were quantified with solvent-matched and matrix-matched standards, by spiking apple sample extracts. Matrix effects dependent on the type of extract (fruit, flesh, or peel) and the apple variety were detected. The best data processing methods involved normalizing matrix effect rates by matrix-matched internal/external calibration. Boscalid, captan, chlorpyrifos, fludioxonil, and pyraclostrobin were the most frequently detected pesticides. However, their concentrations in the whole fruit were below European maximum residue levels. Despite negative matrix effects, the residues in peel were detected at concentrations up to 10 times higher than those in whole fruits. Consequently, other pesticide residues present at concentrations below the limit of quantification in the whole fruit were detected in the peel. © 2016 Institute of Food Technologists®

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

Science.gov (United States)

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

2016-02-01

The pesticide residue levels of three nuts (chestnut, walnut, pinenut) collected from seven main producing areas of China were investigated. Twenty-nine pesticides, including organophosphates (OPs), organochlorines (OCs), pyrethroids (PYs) and two fungicides (triadimefon and buprofezin) were analyzed by gas chromatography (GC). Four OPs (acephate, dimethoate, chlorpyrifos and parathion-methyl) were found in 11.4% samples, with the concentrations of 19.0 µg kg(-1) to 74.0 µg kg(-1). Six OCs (DDT, HCH, endosulfan, quintozene, aldrin and dieldrin) were found in 18.2% samples, with the concentrations of 2.0 µg kg(-1) to 65.7 µg kg(-1). Among OCs, p,p-DDE and α-HCH were the dominant isomer for DDT and HCH. Five PYs (fenpropathrin, fenvalerate, cypermethrin, bifenthrin and cyhalothrin) were found in 15.9% samples, with the concentrations of 2.5 µg kg(-1) to 433.0 µg kg(-1). Fenpropathrin was the most frequently detected pesticide. In addition, triadimefon and buprofezin were detected only in two samples. For the tested nuts, 25.0% samples with multiple residues (containing more than two pesticides) were noted, even up to 9.1% samples with five pesticide residues. The residue of 15.9% samples was higher than the maximum residue limits (MRLs) of China. The short-term risks for the tested nuts were below 1.2%, and the highest long-term risk was 12.58%. The cumulative risk (cHI) for the tested pesticides were 8.43% (OPs), 0.42% (OCs), 12.82% (PYs) and 0.15% (fungicides), respectively. The total cHI was 21.82%. There was no significant health risk for consumers via nuts consumption. Copyright © 2015 Elsevier Ltd. All rights reserved.

Uncertainty of pesticide residue concentration determined from ordinary and weighted linear regression curve.

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Yolci Omeroglu, Perihan; Ambrus, Árpad; Boyacioglu, Dilek

2018-03-28

Determination of pesticide residues is based on calibration curves constructed for each batch of analysis. Calibration standard solutions are prepared from a known amount of reference material at different concentration levels covering the concentration range of the analyte in the analysed samples. In the scope of this study, the applicability of both ordinary linear and weighted linear regression (OLR and WLR) for pesticide residue analysis was investigated. We used 782 multipoint calibration curves obtained for 72 different analytical batches with high-pressure liquid chromatography equipped with an ultraviolet detector, and gas chromatography with electron capture, nitrogen phosphorus or mass spectrophotometer detectors. Quality criteria of the linear curves including regression coefficient, standard deviation of relative residuals and deviation of back calculated concentrations were calculated both for WLR and OLR methods. Moreover, the relative uncertainty of the predicted analyte concentration was estimated for both methods. It was concluded that calibration curve based on WLR complies with all the quality criteria set by international guidelines compared to those calculated with OLR. It means that all the data fit well with WLR for pesticide residue analysis. It was estimated that, regardless of the actual concentration range of the calibration, relative uncertainty at the lowest calibrated level ranged between 0.3% and 113.7% for OLR and between 0.2% and 22.1% for WLR. At or above 1/3 of the calibrated range, uncertainty of calibration curve ranged between 0.1% and 16.3% for OLR and 0% and 12.2% for WLR, and therefore, the two methods gave comparable results.

Comparison of questionnaire-based estimation of pesticide residue intake from fruits and vegetables with urinary concentrations of pesticide biomarkers.

Science.gov (United States)

Chiu, Yu-Han; Williams, Paige L; Mínguez-Alarcón, Lidia; Gillman, Matthew; Sun, Qi; Ospina, Maria; Calafat, Antonia M; Hauser, Russ; Chavarro, Jorge E

2018-01-01

We developed a pesticide residue burden score (PRBS) based on a food frequency questionnaire and surveillance data on food pesticide residues to characterize dietary exposure over the past year. In the present study, we evaluated the association of the PRBS with urinary concentrations of pesticide biomarkers. Fruit and vegetable (FV) intake was classified as having high (PRBS≥4) or low (PRBSEARTH study. Two urine samples per man were analyzed for seven biomarkers of organophosphate and pyrethroid insecticides, and the herbicide 2,4-dichlorophenoxyacetic acid. We used generalized estimating equations to analyze the association of the PRBS with urinary concentrations of pesticide biomarkers. Urinary concentrations of pesticide biomarkers were positively related to high pesticide FV intake but inversely related to low pesticide FV intake. The molar sum of urinary concentrations of pesticide biomarkers was 21% (95% confidence interval (CI): 2%, 44%) higher for each one serving/day increase in high pesticide FV intake, and 10% (95% CI: 1%, 18%) lower for each one serving/day increase in low pesticide FV intake. Furthermore, intake of high pesticide FVs positively related to most individual urinary biomarkers. Our findings support the usefulness of the PRBS approach to characterize dietary exposure to select pesticides.

How effective are common household preparations on removing pesticide residues from fruit and vegetables? A review.

Science.gov (United States)

Chung, Stephen Wc

2018-06-01

Nowadays, the use of pesticides is inevitable for pest control in crops, especially for fruit and vegetables. After the harvest from raw agricultural commodities, the amount of pesticide residues in food is mainly influenced by the storage, handling and processing that follow. If good agricultural and good manufacturing practices are enforced effectively, the amount of pesticide residues would be brought below the corresponding maximum residue level. Thus, the consumption of raw and/or prepared fruit and vegetables would be safe. Nonetheless, reports regarding pesticide residues in fruit or vegetables on mass media have been worrying consumers, who are concerned about the adverse effects of pesticide residues. As a result, consumers perform household processing before consumption to reduce any related risks. However, can these preparations effectively remove pesticide residues? Reviewing the extensive literature, it showed that, in most cases, washing and soaking can only lead to a certain degree of reduction in residue level, while other processing such as peeling, soaking in chemical baths and blanching can reduce pesticide residues more effectively. In general, the behaviour of residues during processing can be rationalised in terms of the physico-chemical properties of the pesticide and the nature of the process. In contrast, the reported studies are diversified and some areas still lack sufficient studies to draw any remarks. Recommendations are provided with respect to the available information that aims to formulate an environmental friendly, cost-effective and efficient household processing of fruit and vegetables to reduce pesticide residues. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

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

International Nuclear Information System (INIS)

Frimpong, S. K

2011-01-01

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 μg/kg), Gamma-chlordane (152.0 μg/kg), Methamidophos (18.5 μg/kg), Profenofos (31.8 μg/kg), Allethrin (10.5 μg/kg), Cypermethrin (32.0 μg/kg) and Fenvalerate (14.6 μg/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

Rapid Detection Technology for Pesticides Residues Based on Microelectrodes Impedance Immunosensor

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Wen Ping Zhao

2014-09-01

Full Text Available Compared with conventional methods, electrochemical immunosensors have many advantages, such as low cost, high sensitivity, and rapid detection, and has certain prospects for realizing real-time-monitoring. In this paper, a design of portable pesticide residues detection instrument was presented based on an electrochemical impedance immunosensor. Firstly, we studied on an impedance immunosensor based on interdigitated array microelectrode (IDAM coupled with magnetic nanobeads-antibody conjugates (MNAC for the pesticide detection. Magnetic nanobeads (diameter 150 nm coated with anti-carbofuran antibodies were used for further amplification of the binding reaction between antibody and hapten (carbofuran. Secondly, in order to develop a portable pesticide residue apparatus, we designed the impedance detection electric circuit. Main work included designing and constructing of the system circuit, designing and debugging of the system software and so on. Thirdly, the apparatus was used for the standard pesticides solutions testing combined with immunosensor to test the reliability and stability. The pesticide added standard recovery was more than 70 % and the impedance test error was less than 5 %. The results showed that the proposed instrument had a good consistence compared with the traditional analytical methods. Thus, it would be a promising rapid detection instrument for pesticide residues in agricultural products.

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

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Md. Shakhaoat Hossain

2013-02-01

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

Proficiency test on incurred and spiked pesticide residues in cereals

DEFF Research Database (Denmark)

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

2009-01-01

A proficiency test on incurred and spiked pesticide residues in wheat was organised in 2008. The test material was grown in 2007 and treated in the field with 14 pesticides formulations containing the active substances, alpha-cypermethrin, bifentrin, carbendazim, chlormequat, chlorpyrifos...

Modelling of the long-term fate of pesticide residues in agricultural soils and their surface exchange with the atmosphere: Part II. Projected long-term fate of pesticide residues.

Science.gov (United States)

Scholtz, M T; Bidleman, T F

2007-05-01

In the first part of this paper, a simple coupled dynamic soil-atmosphere model for studying the gaseous exchange of pesticide soil residues with the atmosphere is described and evaluated by comparing model results with published measurements of pesticide concentrations in air and soil. In Part II, the model is used to study the concentration profiles of pesticide residues in both undisturbed and annually tilled agricultural soils. Future trends are estimated for the measured air and soil concentrations of lindane and six highly persistent pesticides (toxaphene, p,p'-DDE, dieldrin, cis- and trans-chlordane and trans-nonachlor) over a twenty-year period due to volatilization and leaching into the deeper soil. Wet deposition and particle associated pesticide deposition (that increase soil residue concentrations) and soil erosion, degradation in the soil (other than for lindane) and run-off in precipitation are not considered in this study. Estimates of the rain deposition fluxes are reported that show that, other than for lindane, net volatilization fluxes greatly exceed rain deposition fluxes. The model shows that the persistent pesticides studied are highly immobile in soil and that loss of these highly persistent residues from the soil is by volatilization rather than leaching into the deeper soil. The soil residue levels of these six pesticides are currently sources of net volatilization to the atmosphere and will remain so for many years. The maximum rate of volatilization from the soil was simulated by setting the atmospheric background concentration to zero; these simulations show that the rates of volatilization will not be significantly increased since soil resistance rather than the atmospheric concentration controls the volatilization rates. Annual tilling of the soils increases the volatilization loss to the atmosphere. Nonetheless, the model predicts that, if only air-soil exchange is considered, more than 76% of current persistent pesticide residues

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

Science.gov (United States)

Andreou, Kostas; Semple, Kirk; Jones, Kevin

2010-05-01

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

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

Science.gov (United States)

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

2015-11-01

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

Rapid multi-residue method for the determination of pesticide ...

African Journals Online (AJOL)

Exposure to pesticides can represent a potential risk to humans. Agricultural workers are at risk of chronic toxicity. Hence, the evaluation of pesticide residues in their blood gives an indication about the extent of exposure and help in assessing adverse health effects. The aim of our study was to develop analytical method for ...

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

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Azadeh Emami

2017-02-01

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

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

Science.gov (United States)

Cabras, P; Angioni, A

2000-04-01

In this review the results obtained in the 1990s from research on the behavior of pesticide residues on grapes, from treatment to harvest, and their fate in drying, wine-making, and alcoholic beverage processing are reported. The fungicide residues on grapes (cyproconazole, hexaconazole, kresoxim-methyl, myclobutanil, penconazole, tetraconazole, and triadimenol), the application rates of which were of a few tens of grams per hectare, were very low after treatment and were not detectable at harvest. Pyrimethanil residues were constant up to harvest, whereas fluazinam, cyprodinil, mepanipyrim, azoxystrobin, and fludioxonil showed different disappearance rates (t(1/2) = 4.3, 12, 12.8, 15.2, and 24 days, respectively). The decay rate of the organophosphorus insecticides was very fast with t(1/2) ranging between 0.97 and 3.84 days. The drying process determined a fruit concentration of 4 times. Despite this, the residue levels of benalaxyl, phosalone, metalaxyl, and procymidone on sun-dried grapes equalled those on the fresh grape, whereas they were higher for iprodione (1.6 times) and lower for vinclozolin and dimethoate (one-third and one-fifth, respectively). In the oven-drying process, benalaxyl, metalaxyl, and vinclozolin showed the same residue value in the fresh and dried fruit, whereas iprodione and procymidone resides were lower in raisins than in the fresh fruit. The wine-making process begins with the pressing of grapes. From this moment onward, because the pesticide on the grape surface comes into contact with the must, it is in a biphasic system, made up of a liquid phase (the must) and a solid phase (cake and lees), and will be apportioned between the two phases. The new fungicides have shown no effect on alcoholic or malolactic fermentation. In some cases the presence of pesticides has also stimulated the yeasts, especially Kloeckera apiculata, to produce more alcohol. After fermentation, pesticide residues in wine were always smaller than those on the

Silicone Wristband Passive Samplers Yield Highly Individualized Pesticide Residue Exposure Profiles.

Science.gov (United States)

Aerts, Raf; Joly, Laure; Szternfeld, Philippe; Tsilikas, Khariklia; De Cremer, Koen; Castelain, Philippe; Aerts, Jean-Marie; Van Orshoven, Jos; Somers, Ben; Hendrickx, Marijke; Andjelkovic, Mirjana; Van Nieuwenhuyse, An

2018-01-02

Monitoring human exposure to pesticides and pesticide residues (PRs) remains crucial for informing public health policies, despite strict regulation of plant protection product and biocide use. We used 72 low-cost silicone wristbands as noninvasive passive samplers to assess cumulative 5-day exposure of 30 individuals to polar PRs. Ethyl acetate extraction and LC-MS/MS analysis were used for the identification of PRs. Thirty-one PRs were detected of which 15 PRs (48%) were detected only in worn wristbands, not in environmental controls. The PRs included 16 fungicides (52%), 8 insecticides (26%), 2 herbicides (6%), 3 pesticide derivatives (10%), 1 insect repellent (3%), and 1 pesticide synergist (3%). Five detected pesticides were not approved for plant protection use in the EU. Smoking and dietary habits that favor vegetable consumption were associated with higher numbers and higher cumulative concentrations of PRs in wristbands. Wristbands featured unique PR combinations. Our results suggest both environment and diet contributed to PR exposure in our study group. Silicone wristbands could serve as sensitive passive samplers to screen population-wide cumulative dietary and environmental exposure to authorized, unauthorized and banned pesticides.

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

Science.gov (United States)

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

1993-09-01

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

Dissipation and residue of clothianidin in granules and pesticide fertilizers used in cabbage and soil under field conditions.

Science.gov (United States)

Zhang, P W; Wang, S Y; Huang, C L; Fu, J T; Huang, R L; Li, Z H; Zhang, Z X

2018-01-01

The single application of 0.5 % clothianidin granules, a novel formulation, was used to control pests in vegetables under a high dose. In this article, residues of clothianidin in cabbage and soil samples under field conditions from Guangzhou, Nanning, and Qianjiang were determined by HPLC. The terminal residues of clothianidin in cabbage were less than the limit of detection (clothianidin residual, clothianidin granules and fertilizers of chicken manure, urea, and organic fertilizer were mixed into different pesticide fertilizers through their normal field using dosage and evaluate residual influence of clothianidin in different formula. After analysis of variance of the effect factors, the effect of different pesticide types on half-life was not significant, but the effect of sample types was significant. Clothianidin granules and pesticide fertilizers could be safely applied in cabbage under a single high-dose administration.

Pesticide residues in birds and mammals

Science.gov (United States)

Stickel, L.F.; Edwards, C.A.

1973-01-01

SUMMARY: Residues of organochlorine pesticides and their breakdown products are present in the tissues of essentially all wild birds throughout the world. These chemicals accumulate in fat from a relatively small environmental exposure. DDE and dieldrin are most prevalent. Others, such as heptachlor epoxide, chlordane, endrin, and benzene hexachloride also occur, the quantities and kinds generally reflecting local or regional use. Accumulation may be sufficient to kill animals following applications for pest control. This has occurred in several large-scale programmes in the United States. Mortality has also resulted from unintentional leakage of chemical from commercial establishments. Residues may persist in the environment for many years, exposing successive generations of animals. In general, birds that eat other birds, or fish, have higher residues than those that eat seeds and vegetation. The kinetic processes of absorption, metabolism, storage, and output differ according to both kind of chemical and species of animal. When exposure is low and continuous, a balance between intake and excretion may be achieved. Residues reach a balance at an approximate animal body equilibrium or plateau; the storage is generally proportional to dose. Experiments with chickens show that dieldrin and heptachlor epoxide have the greatest propensity for storage, endrin next, then DDT, then lindane. The storage of DDT was complicated by its metabolism to DDE and DDD, but other studies show that DDE has a much greater propensity for storage than either DDD or DDT. Methoxychlor has little cumulative capacity in birds. Residues in eggs reflect and parallel those in the parent bird during accumulation, equilibrium, and decline when dosage is discontinued. Residues with the greatest propensity for storage are also lost most slowly. Rate of loss of residues can be modified by dietary components and is speeded by weight loss of the animal. Under sublethal conditions of continuous

Validation of a method for the determination of 120 pesticide residues in apples and cucumbers by LC-MS/MS.

Science.gov (United States)

Ramadan, Gouda; Al Jabir, Muna; Alabdulmalik, Najat; Mohammed, Ali

2016-05-01

Most countries have clearly defined regulations governing the use of pesticides in agricultural activity. The application of pesticides in agriculture usually leads to a residual amount of these pesticides on food products such as fruit and vegetables. The presence of pesticide residues on these foods destined for human consumption may pose food safety risks to consumers. To protect consumers, national authorities have established maximum limits for pesticide residues in foods. These limits can only be enforced if there are methods available to detect and monitor their concentrations in the applicable food products. To support the enforcement of this legislation, we have developed a multi-residue liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the analysis of 120 pesticide residues in apples and cucumbers which has been validated and implemented in the routine monitoring and surveillance programme for these pesticides. In this method, apple and cucumber samples are extracted using the QuEChERS method (quick, easy, cheap, effective, rugged, and safe) and the extracts were analyzed directly by LC-MS/MS. The mean recoveries at three different concentrations of 0.01 µg/g , 0.05 µg/g, and 0.1 µg/g over the analytical range varied between 70 and 120%. The repeatability of the method expressed as %RSD was less than 20%. The limit of detection (LOD) of the method ranged between 0.0014 and 0.0110 µg/g for apples and between 0.0012 and 0.0075 µg/g for cucumbers. The limit of quantification (LOQ) of the method was 0.01 µg/g for apples and cucumbers. The method has been used for the analysis of over 600 apple and 550 cucumber samples over the past two years. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

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

Directory of Open Access Journals (Sweden)

Crentsil Kofi Bempah

2012-12-01

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

Note on pesticide residues as a function of formulation used

International Nuclear Information System (INIS)

Lord, K.A.

1976-01-01

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

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

Science.gov (United States)

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

2009-04-01

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

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

OpenAIRE

FERDI BRAHUSHI; ENDRIT KULLAJ

2014-01-01

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

Organochlorine pesticide residues in the northern Indian Ocean

Digital Repository Service at National Institute of Oceanography (India)

Shailaja, M.S.; Sarkar, A.

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

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

International Nuclear Information System (INIS)

Mao Xuefei; Jiao Bining; Fu Chenmei; Qian Yongzhong; Wang Jing

2008-01-01

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)

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

Science.gov (United States)

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

2016-03-01

An analytical method based on dispersive solid-phase extraction with a multiwalled carbon nanotubes sorbent coupled with positive pulse glow discharge ion mobility spectrometry was developed for analysis of 30 pesticide residues in drinking water samples. Reduced ion mobilities and the mass-mobility correlation of 30 pesticides were measured. The pesticides were divided into five groups to verify the separation capability of pulse glow discharge in mobility spectrometry. The extraction conditions such as desorption solvent, ionic strength, conditions of adsorption and desorption, the amounts of multiwalled carbon nanotubes, and solution pH were optimized. The enrichment factors of pesticides were 5.4- to 48.7-fold (theoretical enrichment factor was 50-fold). The detection limits of pesticides were 0.01∼0.77 μg/kg. The linear range was 0.005-0.2 mg/L for pesticide standard solutions, with determination coefficients from 0.9616 to 0.9999. The method was applied for the analysis of practical and spiked drinking water samples. All results were confirmed by high-performance liquid chromatography with tandem mass spectrometry. The proposed method was proven to be a commendably rapid screening qualitative and semiquantitative technique for the analysis of pesticide residues in drinking water samples on site. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

International Nuclear Information System (INIS)

Kammerbauer, J.; Moncada, J.

1999-01-01

There is a basic lack of information about the presence of pesticide residues in the environment in Central America. Over the period of February 1995 to June 1997, river, well, lagoon and spring water samples, as well as soil, fish tissue, lagoon bed sediments and some foodstuffs were taken from the greater Cholutecan River Basin of Honduras and analyzed for pesticide residues. These were collected at three separate sites (La Lima, Zamorano and Choluteca), each characterized by differing agricultural production systems. The main pesticide residues found in soil samples were dieldrin and p,p'-DDT, while river water samples were found to have detectable levels of heptachlor, endosulfan and chlorpyrifos, with lagoon and well water also being shown to contain heptachlor. These pesticides detected were in more than 20% of the samples assessed. In river water samples more pesticide residues at higher concentrations were found to be associated with areas of more intensive agricultural production. The fewest pesticides with lowest concentrations were found in the small subwatershed associated with traditional agricultural production. Although the pesticides found in the soils at the three sites were generally similar they tended to be higher in the southern part of the Cholutecan watershed, followed by the central zone, with the lowest concentrations being found in the more traditional production zone. In lagoon and well water samples more pesticides, but mostly in lower concentrations were detected at the traditional production site than at the others. Ten pesticide compounds were detected in fish tissue, mainly organochlorines, some of which were also found in lagoon sediments. In terms of food products, almost no pesticides were detected in vegetables, but the kidney adipose tissue taken from slaughtered cows was shown to have a tendency to contain some organochlorines. Spring water in the traditional agricultural production zone contained three organochlorine compounds

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

Science.gov (United States)

Walorczyk, Stanisław; Drożdżyński, Dariusz; Kowalska, Jolanta; Remlein-Starosta, Dorota; Ziółkowski, Andrzej; Przewoźniak, Monika; Gnusowski, Bogusław

2013-08-15

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. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

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Md. Nur Alam

2015-01-01

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

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

Science.gov (United States)

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

2016-11-01

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

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

Directory of Open Access Journals (Sweden)

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

2012-10-01

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

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

DEFF Research Database (Denmark)

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

2012-01-01

. None of the results for the pesticides residues measured in individual apples exceeded the EU Maximum Residue Levels (MRLs). However, there was a large variation in the residues levels in the apples, with levels from 0.01 to 1.4 mg kg−1 for captan, the pesticide with the highest variation, and from 0.......01 to 0.2 mg kg−1 for pyraclostrobin, the pesticide with the lowest variation. Residues of fenoxycarb and indoxacarb were only found in a few apples, probably due to the early application time of these two compounds. The evaluation of the effect of spray quality did not show any major difference between......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...

Identification and concentration of selected pesticide residues in Ghanaian cocoa beans

International Nuclear Information System (INIS)

Sefakor, Adzo Fialor

2017-07-01

three matrices, it was only the shells that had recordable concentrations of pyrethroids being present and these were Cypermethrin (0.013 mg/kg) and Permethrin (0.012 mg/kg). Regional analysis also showed Permethrin to be present in bean shells from both Ashanti and Western South Region at concentrations of 0.01 mg/kg and 0.02 mg/kg respectively. Cypermethrin on the other hand was present in bean shells from four regions ranging in concentrations of 0.011 mg/kg to 0.020 mg/kg. Chlorpyrifos which was the only organophosphorous compound tested for was found to be present in about 42% of the cocoa shell samples analysed at concentrations ranging from 0.0108 to 0.0396 mg/kg with an average concentration of 0.0184 mg/kg being recorded. Eastern Region had the highest concentration of Chlorpyrifos in the shells (0.026 mg/kg), while Western North Region recorded the highest concentration in the whole beans (0.027 mg/kg) and Central Region recorded the highest concentration in the nibs (0.015 mg/kg). On the whole, all the pesticide residue concentrations measured were below the established EU and Japan MRLs. Principal Component Analysis (PCA) used to assess the associations amongst the various pesticides and between the pesticides and the regions revealed that Imidacloprid/Thiamethoxam; Thiamethoxam/Cypermethrin and Chlorpyrifos/Imidacloprid were in comparable proportions and prevalence in the cocoa nibs. For the shells however, Imidacloprid/Cypermethrin and Deltamethrin/Permethrin/Thiamethoxam were of similar proportions. PCA of the whole cocoa beans also indicated a close association between Cypermethrin/Thiamethoxam and Permethrin/Clothianidin. Out of all the regions, Central Region had the highest association with all the 10 pesticides in the shells and with Imidacloprid in the whole beans whilst Western South Region showed an association with Chlorpyrifos in the nibs. (author)

Evaluation of Some Pesticide Residues in Fruits import by High Performance Liquid Chromatography

Directory of Open Access Journals (Sweden)

Lamees Munef Abdul-Latef

2017-02-01

Full Text Available Pesticide residues have been found in various fruits and vegetables.  This studycollected 24 samples and reported a method based on High Performance Liquid Chromatography (HPLC. For determination of pesticide residues used in Some fruits which were collected from different markets of Baghdad city to make 24 samples from (peel , core, mixture for each type of fruits markets as:  Oranges( Egypt , Africa, Pomegranate ( Egypt, Mango ( Kenya , Pears (China,  Plum fruits ( Africa , Kiwi (Turkey .That detective of ( 5 different  pesticides (diazinon,  malathion, chlorpyrifos ,parathion  and cypermethrin. The results were detected of multi-residues of  pesticides on the fruit in ( peel , core , mixture may be in the limit of Maximum residue limits(MRL or higher of it   . The pesticides detected that exceeding the limits are: cypermethrin  in Kiwi (peel, core and mixtureat(0.204,0.038, 0.537, in pomegranate detected in (peel and mixture at (0.509,0.189 mg/kg , Diazinondetccted in Egyptian orange in (peel ,core and mixture at (0.031,0.207, 0.099 mg/kg . Malathion and Parathion was not detected at any type of fruits and  that results was compared with codex of FAO/WHO(2013. That data is important to monitor residues in food and to fill gaps in current knowledge would be helpful in assessing human exposure risks from ingestion of contaminated Fruits Imported to our country .

Role of Sample Processing Strategies at the European Union National Reference Laboratories (NRLs) Concerning the Analysis of Pesticide Residues

DEFF Research Database (Denmark)

Hajeb, Parvaneh; Herrmann, Susan Strange; Poulsen, Mette Erecius

2017-01-01

to the European Union Reference Laboratory on Cereals and Feedingstuff (EURL) for the determination of the particle size distribution and pesticide residue recovery. The results showed that the NRLs used several different brands and types of mills. Large variations in the particle size distributions and pesticide...

Distribution of multiple pesticide residues in apple segments after home processing

DEFF Research Database (Denmark)

Rasmussen, Rie Romme; Poulsen, Mette Erecius; Hansen, H. C. B.

2003-01-01

The effects of washing, storing, boiling, peeling, coring and juicing on pesticide residue were investigated for field-sprayed Discovery and Jonagold apples. Residues of chlorpyrifos, cypermethrin, deltamethrin, diazinon, endosulfan, endosulfan sulfate, fenitrothion, fenpropathrin, iprodione, kre...

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

International Nuclear Information System (INIS)

He Jiang; Huang Min; Chen Hao; Wu Ling; Gao Peng; Wang Yan; Lei Qing

2011-01-01

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

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

Directory of Open Access Journals (Sweden)

Husniye Imamoglu

2016-01-01

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

An Innovative Rapid Method for Analysis of 10 Organophosphorus Pesticide Residues in Wheat by HS-SPME-GC-FPD/MSD.

Science.gov (United States)

Du, Xin; Ren, YongLin; Beckett, Stephen J

2016-01-01

The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/PDMS fiber increased with increasing spiking levels, yielding significant (R(2) > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity.

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

International Nuclear Information System (INIS)

Costinel, Diana; Lazar, Roxana Elena; Vremera, Raluca; Irimescu, Rodica; Saros-Rogobete, Gili

2006-01-01

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)

Status of persistent organic pesticide residues in water and food and their effects on environment and farmers: a comprehensive review in Nigeria

Directory of Open Access Journals (Sweden)

Norida Mazlan

2017-08-01

Full Text Available Pesticide helps to enhance agricultural production, however, it significantly affect both socio and environmental entities of a country. In Nigeria, pesticide is widely used, thus its traces have been detected in water, soil and air. Several studies have already indicated that most of the environmental ecology (air, water, and soil in Nigeria has been contaminated by persistent organic pesticides like organochlorine and organophosphate. Other reasons of high pesticide residues present in Nigeria environment is due to inappropriate dosage applied of pesticides that leaves behind excess. However, its residues are found above safety levels in the air, water, and soil across the nation. Based on previous analysis, it is indicated that 125,000-130,000 metric ton pesticides are being applied annually in Nigeria. Despite banned of some pesticides such as dichlorodiphenyltrichloroethane- and -Hexachlorocyclohexane, they are still being used by farmers in their agricultural production. Many of the Class 1 (high extremely toxic pesticides are still being used in developing countries like Nigeria. Hence, there is need to sensitize and educate the general public especially the end-users (farmers particularly on management practices of pesticides. Considering these entire hazardous situations, in this article the history of pesticide used in Nigeria has been reviewed in detail. The article also discussed the effects of pesticide use in Nigerian waters, soil and on crops. The risk of residual pesticide on agricultural workers, pesticide residue risk preventive measures by the Federal Government of Nigeria, banned and restricted pesticides in Nigeria, Nigerian Government and its efforts to eliminate persistent organic pesticides in use are also reviewed in details.

Fruit and vegetable intake and their pesticide residues in relation to semen quality among men from a fertility clinic.

Science.gov (United States)

Chiu, Y H; Afeiche, M C; Gaskins, A J; Williams, P L; Petrozza, J C; Tanrikut, C; Hauser, R; Chavarro, J E

2015-06-01

Is consumption of fruits and vegetables with high levels of pesticide residues associated with lower semen quality? Consumption of fruits and vegetables with high levels of pesticide residues was associated with a lower total sperm count and a lower percentage of morphologically normal sperm among men presenting to a fertility clinic. Occupational and environmental exposure to pesticides is associated with lower semen quality. Whether the same is true for exposure through diet is unknown. Men enrolled in the Environment and Reproductive Health (EARTH) Study, an ongoing prospective cohort at an academic medical fertility center. Male partners (n = 155) in subfertile couples provided 338 semen samples during 2007-2012. Semen samples were collected over an 18-month period following diet assessment. Sperm concentration and motility were evaluated by computer-aided semen analysis (CASA). Fruits and vegetables were categorized as containing high or low-to-moderate pesticide residues based on data from the annual United States Department of Agriculture Pesticide Data Program. Linear mixed models were used to analyze the association of fruit and vegetable intake with sperm parameters accounting for within-person correlations across repeat samples while adjusting for potential confounders. Total fruit and vegetable intake was unrelated to semen quality parameters. High pesticide residue fruit and vegetable intake, however, was associated with poorer semen quality. On average, men in highest quartile of high pesticide residue fruit and vegetable intake (≥1.5 servings/day) had 49% (95% confidence interval (CI): 31%, 63%) lower total sperm count and 32% (95% CI: 7%, 58%) lower percentage of morphologically normal sperm than men in the lowest quartile of intake (vegetable intake was associated with a higher percentage of morphologically normal sperm (P, trend = 0.04). Surveillance data, rather than individual pesticide assessment, was used to assess the pesticide residue

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

Science.gov (United States)

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

2013-01-04

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.

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

Directory of Open Access Journals (Sweden)

Faqir Muhammad

2013-01-01

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

Association Between Pesticide Residue Intake From Consumption of Fruits and Vegetables and Pregnancy Outcomes Among Women Undergoing Infertility Treatment With Assisted Reproductive Technology.

Science.gov (United States)

Chiu, Yu-Han; Williams, Paige L; Gillman, Matthew W; Gaskins, Audrey J; Mínguez-Alarcón, Lidia; Souter, Irene; Toth, Thomas L; Ford, Jennifer B; Hauser, Russ; Chavarro, Jorge E

2018-01-01

Animal experiments suggest that ingestion of pesticide mixtures at environmentally relevant concentrations decreases the number of live-born offspring. Whether the same is true in humans is unknown. To examine the association of preconception intake of pesticide residues in fruits and vegetables (FVs) with outcomes of infertility treatment with assisted reproductive technologies (ART). This analysis included 325 women who completed a diet assessment and subsequently underwent 541 ART cycles in the Environment and Reproductive Health (EARTH) prospective cohort study (2007-2016) at a fertility center at a teaching hospital. We categorized FVs as having high or low pesticide residues using a validated method based on surveillance data from the US Department of Agriculture. Cluster-weighted generalized estimating equations were used to analyze associations of high- and low-pesticide residue FV intake with ART outcomes. Adjusted probabilities of clinical pregnancy and live birth per treatment cycle. In the 325 participants (mean [SD] age, 35.1 [4.0] y; body mass index, 24.1 [4.3]), mean (SD) intakes of high- and low-pesticide residue FVs were 1.7 (1.0) and 2.8 (1.6) servings/d, respectively. Greater intake of high-pesticide residue FVs was associated with a lower probability of clinical pregnancy and live birth. Compared with women in the lowest quartile of high-pesticide FV intake (<1.0 servings/d), women in the highest quartile (≥2.3 servings/d) had 18% (95% CI, 5%-30%) lower probability of clinical pregnancy and 26% (95% CI, 13%-37%) lower probability of live birth. Intake of low-pesticide residue FVs was not significantly related to ART outcomes. Higher consumption of high-pesticide residue FVs was associated with lower probabilities of pregnancy and live birth following infertility treatment with ART. These data suggest that dietary pesticide exposure within the range of typical human exposure may be associated with adverse reproductive consequences.

Chlorinated pesticide residues in sediments from the Arabian Sea along the Central West coast of India

Digital Repository Service at National Institute of Oceanography (India)

Sarkar, A.; SenGupta, R.

Environmental contamination by persistent chlorinated pesticides has evoked major concern due to the presence of their residues in the environment. The quantitative distribution of chlorinated pesticides residues in the marine sediments from...

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

Science.gov (United States)

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

2013-01-01

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

Pesticide Residues in Canned Foods, Fruits, and Vegetables: The Application of Supercritical Fluid Extraction and Chromatographic Techniques in the Analysis

OpenAIRE

EL-Saeid, Mohamed H.

2003-01-01

Multiple pesticide residues have been observed in some samples of canned foods, frozen vegetables, and fruit jam, which put the health of the consumers at risk of adverse effects. It is quite apparent that such a state of affairs calls for the need of more accurate, cost-effective, and rapid analytical techniques capable of detecting the minimum concentrations of the multiple pesticide residues. The aims of this paper were first, to determine the effectiveness of the use of Supercritical Flui...

Pesticide Residues in Commercial Lettuce, Onion, and Potato Samples From Bolivia—A Threat to Public Health?

DEFF Research Database (Denmark)

Skovgaard, Marlene; Renjel, Susana; Jensen, Olaf Chresten

2017-01-01

lettuce samples from La Paz were sampled on August 15, 2015 at a local market and screened for 283 pesticides. Residues of cypermethrin, chlorpyrifos, difenoconazol, or/and λ-cyhalothrin were detected in 50% of the lettuce samples, whereas no pesticides were found in potatoes and onions. In 20......% of the lettuce samples, the measurements were above the maximum residue limits, and 2 or 3 pesticides were identified simultaneously. Washing almost halved the pesticide levels, but still 20% of the samples showed measurements above the limits. No samples contained concentrations of pesticides which alone...

Towards accreditation of MINT pesticide residue laboratory - a journey

International Nuclear Information System (INIS)

Nashriyah Mat; Salmah Moosa; Misman Sumin; Maizatul Akmam Mohd Nasir; Norimah Yusof

2005-01-01

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)

T-REX Version 1.5 User's Guide for Calculating Pesticide Residues on Avian and Mammalian Food Items - Appendix B - Initial Pesticide Residues on Arthropods

Science.gov (United States)

Obtain empirical data from the scientific literature and registrant-submitted studies to refine the initial residue assumptions of pesticides on arthropods that are simulated with TIM, T-REX, and T-HERPS

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

DEFF Research Database (Denmark)

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

2015-01-01

Fruits and vegetables from Souteast Asia were analysed for the presence of pesticide residues. A total of 721 samples of 63 different commodities were collected in 2011. The products were imported to Denmark, Finland, Norway and Sweden from ten countries; about 80% were imported from Thailand....... The reason for the increased control for certain food products from Southeast Asia was that the official control had revealed many products with too high levels of pesticide residues. In 60% of the samples we did not find any residues, while 28% had residues below or at the MRLs. Results above the MRLs were...

Residues of Organochlorinated Pesticides in Soil from Tomato ...

African Journals Online (AJOL)

This work presents the concentrations of five pesticide residues, lindane, chlorpyrifos, endosulfan, p, p'-DDE and p, p'-DDD in soil samples collected from tomato fields in Ngarenanyuki, Tanzania. Endosulfan sulphate was detected in 100 % of the sample analysed with mean concentration of 0.2407 mg/kg dw. Chlorpyrifos ...

Persistent Organochlorine Pesticide Residues in Some Selected Cocoa Beverages in Nigeria

Directory of Open Access Journals (Sweden)

Olayinka A. Ibigbami

2017-12-01

Full Text Available This study evaluates the quality of the cocoa beverages produced in Nigeria with respect to the occurrence and levels of organochlorine pesticides OCPs residues in order to ascertain the potential health risks to the general public. Seven cocoa-based beverages were analysed for 17 OCP residues using gas chromatography coupled with an Electron Captured Detector (GC-ECD after extraction and silica-gel clean-up. The study reveals the presence of ten OCP residues in the cocoa beverages, with a concentration range from not detected ND—0.256 mg/kg, while α-BHC, β-BHC, methoxychlor, p,p′-DDE, dieldrin, endrin aldehyde, and endosulfan sulphate were not detected in any of the analysed samples. The contamination pattern of OCPs in the beverages was in the following order: Ovaltine > Milo > Cadbury-choco > Bournvita > Cowbell-coffee > Richoco > Oluji, with p,p′-DDT being the most frequently found pesticide. Heptachlor and endosulfan II showeda residual level above the European Union (EU Maximum Residual Limits (MRLs in only one sample.

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

Science.gov (United States)

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

2016-09-02

An automated multi-plug filtration cleanup (m-PFC) method on modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts was developed. The automatic device was aimed to reduce labor-consuming manual operation workload in the cleanup steps. It could control the volume and the speed of pulling and pushing cycles accurately. In this work, m-PFC was based on multi-walled carbon nanotubes (MWCNTs) mixed with other sorbents and anhydrous magnesium sulfate (MgSO4) in a packed tip for analysis of pesticide multi-residues in crop commodities followed by liquid chromatography with tandem mass spectrometric (LC-MS/MS) detection. It was validated by analyzing 25 pesticides in six representative matrices spiked at two concentration levels of 10 and 100μg/kg. Salts, sorbents, m-PFC procedure, automated pulling and pushing volume, automated pulling speed, and pushing speed for each matrix were optimized. After optimization, two general automated m-PFC methods were introduced to relatively simple (apple, citrus fruit, peanut) and relatively complex (spinach, leek, green tea) matrices. Spike recoveries were within 83 and 108% and 1-14% RSD for most analytes in the tested matrices. Matrix-matched calibrations were performed with the coefficients of determination >0.997 between concentration levels of 10 and 1000μg/kg. The developed method was successfully applied to the determination of pesticide residues in market samples. Copyright © 2016 Elsevier B.V. All rights reserved.

[Rapid screening and confirmation of 205 pesticide residues in rice by QuEChERS and liquid chromatography-mass spectrometry].

Science.gov (United States)

Chen, Xi; Cheng, Lei; Qu, Shichao; Huang, Daliang; Liu, Jiacheng; Cui, Han; Jia, Yanbo; Ji, Mingshan

2015-10-01

A method for rapid screening and confirmation of 205 pesticide residues in rice was developed by combining QuEChERS and high performance liquid chromatography-triple quadrupole-linear ion trap mass spectrometry (LC-Q-TRAP/MS). The rice samples were extracted with acetonitrile, and then cleaned up with primary secondary amine (PSA), anhydrous magnesium sulfate (MgSO4) and C18 adsorbent. Finally, the samples were detected by LC-Q-TRAP/MS in multiple reaction monitoring with information-dependent acquisition of enhanced product ion (MRM-IDA-EPI) mode followed with database searching. A total of 205 pesticide residues were confirmed by retention times, ion pairs and the database searching using EPI library, and quantified by external standard method. All the pesticides showed good linearities with linear correlation coefficients all above 0.995. The limits of quantification (LOQs) for the 205 pesticides were 0.5-10.0 μg/kg. The average recoveries of the 205 pesticides ranged from 62.4% to 127.1% with the relative standard deviations (RSDs) of 1.0% - 20.0% at spiked levels of 10 μg/kg and 50 μg/kg, and only 20 min were needed for the analysis of an actual rice sample. In brief, the method is fast, accurate and highly sensitive, and is suitable for the screening and confirmation of pesticide residues in rice.

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

Science.gov (United States)

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

2005-01-01

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.

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

Science.gov (United States)

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

Pesticide residues in nut-planted soils of China and their relationship between nut/soil.

Science.gov (United States)

Han, Yongxiang; Mo, Runhong; Yuan, Xinyue; Zhong, Donglian; Tang, Fubin; Ye, Caifen; Liu, Yihua

2017-08-01

Twenty-nine pesticide residues in nut-planted soils from China were investigated. One organophosphate (chlorpyrifos) was detected in 5.3% soils, and the residue levels of 7.2 μg/kg to 77.2 μg/kg. The concentrations of six organochlorines (DDT, HCH, endosulfan, quintozene, aldrin and dieldrin) detected in 78.9% soils were 0.6 μg/kg to 90.1 μg/kg. The residue levels of six pyrethroids (bifenthrin, fenpropathrin, cyhalothrin, cypermethrin, fenvalerate and deltamethrin) detected in 65.8% soils were 1.5 μg/kg to 884.3 μg/kg. Triadimefon and buprofezin were found in 71.1% and 52.6% samples, respectively, with the corresponding concentrations of 9.8 μg/kg to 193.7 μg/kg and 87.9 μg/kg to 807.4 μg/kg. The multiple residues were found in 76.3% soils. A significant correlation between pesticide residues in nuts and soils was observed, with the correlation coefficient (r) 0.83 (P < 0.001). In addition, the bioconcentration factor (BCF) values for the explanation of pesticides from soils into nuts were ranged from 0.8 to 16.5. The results showed that some pesticides could accumulate in nut by the uptake effect from soil. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

International Nuclear Information System (INIS)

Sanchez, Andres Garcia; Martos, Natividad Ramos; Ballesteros, Evaristo

2006-01-01

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 μg/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

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

Science.gov (United States)

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

2017-10-01

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

Analytical Method Development for the Determination of Α-Endosulfan and Bifenthrin Pesticide Residues in Tea

Directory of Open Access Journals (Sweden)

Dyah Styarini

2014-03-01

Full Text Available The development of analytical method for the determination of α-endosulfan and bifenthrin residues in tea has been done. The complex matrices and also the pigment were the challenge in doing quantification of the pesticide residues in tea matrices. In order to get appropriate analysis method for the determination of pesticide residues in tea, the modification was done in the analytical method for the determination of organochlorine multiresidue in non fat matrices: seasoning and spicy that is published by Directorate General of Food Crops, Directorate of Food Plant Protection. The modification was done particularly in clean-up step to remove the interferences from the extract of tea matrices such as the pigment that usually interfere the measurement with Gas Chromatography (GC. The result showed that the MDL value for both analytes were 0.5 ng/g that were much lower than MRLs. The percent recovery obtained from the method was 78.58 and 90.19% for α-endosulfan and bifenthrin, respectively. The precision of the analysis method for both analytes were good since the % RSD values were below than the Horwitz’s value that was 19.18% at spiking level concentration of 300 ng/g.

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

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

2014-07-01

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

Successive monitoring surveys of selected banned and restricted pesticide residues in vegetables from the northwest region of China from 2011 to 2013.

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Yu, Yan; Hu, Senke; Yang, Yuxuan; Zhao, Xiaodan; Xue, Jianjun; Zhang, Jinghua; Gao, Song; Yang, Aimin

2017-08-02

A wide range of pesticides is applied for crop protection in vegetable cultivation in China. Regulation of pesticide maximum residue limits (MRLs) in vegetables is established but not fully enforced. And pesticide residues in vegetables were not well monitored. This study conducted the monitoring surveys from 2011 to 2013 to investigate the pesticides in vegetables in the northwest region of China. A multi-residue gas chromatography/mass spectrometry method (GC/MS) was used in determination of pesticides in vegetable samples. The χ 2 test was used to compare the concentration of pesticide residues. A total of 32 pesticide residues were detected in 518 samples from 20 types of vegetables in this study. 7.7% of the detected pesticide residues exceeded the MRLs. The percentages of residues that exceeded the MRLs for leafy, melon and fruit, and root vegetables were 11.2%, 5.1%, and 1.6%, respectively. There was no seasonal difference in the proportion of samples that exceeded the MRLs in different vegetables. A total of 84.3% (27/32) pesticides were detected at concentrations that exceeded MRLs. And of the 27 pesticides that exceeded the MRLs, 11 (40.7%) were banned for use in agriculture. The most frequently detected pesticides were Malathion (9.4%), Dichlorvos (8.7%), and Dimethoate (8.1%). The observed high rate of pesticides detected and high incidence of pesticide detection exceeding their MRLs in the commonly consumed vegetables indicated that the Good Agricultural Practices (GAP) may not be well followed. The management of pesticide use and control should be improved. Well-developed training programs should be initiated to improve pesticide application knowledge for farmers.

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

Science.gov (United States)

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

2016-11-04

A rapid method to screen and quantify multi-class analytic targets in red wine has been developed by direct analysis in real time (DART) coupled with triple quadruple tandem mass spectrometry (QqQ-MS). A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure was used for increasing analytical speed and reducing matrix effect, and the multiple reaction monitoring (MRM) in DART-MS/MS ensured accurate analysis. One bottle of wine containing 50 pesticides and 12 adulterants, i.e., preservatives, antioxidant, sweeteners, and azo dyes, could be totally determined less than 12min. This method exhibited proper linearity (R 2 ≥0.99) in the range of 1-1000ng/mL for pesticides and 10-5000ng/mL for adulterants. The limits of detection (LODs) were obtained in a 0.5-50ng/mL range for pesticides and 5-50ng/mL range for adulterants, and the limits of quantification (LOQs) were in a 1-100ng/mL range for pesticides and 10-250ng/mL range for adulterants. Three spiked levels for each analyte in wine were evaluated, and the recoveries were in a scope of 75-120%. The results demonstrated DART-MS/MS was a rapid and simple method, and could be applied to rapid analyze residual pesticides and illegal adulterants in a large quantities of red wine. Copyright © 2016 Elsevier B.V. All rights reserved.

Pesticide residues in fish from the Densu River Basin in Ghana ...

African Journals Online (AJOL)

The Densu River is a typical river flowing through agricultural areas in Southern Ghana. Six fish species from different locations in the river were sampled and analyzed for residues of pesticides and metabolites using GC with ECD/FID. The results of the study indicate that all the detected residues and metabolites in fish ...

Levels of pesticides residues in the White Nile water in the Sudan.

Science.gov (United States)

Nesser, Gibreel A A; Abdelbagi, Azhari O; Hammad, Ahmed Mohammed Ali; Tagelseed, Mirghani; Laing, Mark D

2016-06-01

Twenty-two commonly used pesticides were monitored during autumn, winter, and summer of 2004-2005 in 27 water samples from three sites along the White Nile in Sudan (former Sudan). Sites were selected to reflect pesticides gathered from drainage canals in central Sudan and from upstream sources. Collected samples were extracted and subjected to gas chromatographic analysis. Pesticides levels were measured in nanograms per liter. Pesticides residues were detected in 96 % of the samples with a total residue burden of 4132.6 ng L(-1), and an overall mean concentration and range of 50.99 and not detected-1570 ng L(-1), respectively. Ororganochlorines were the most frequently detected contaminants, which were found in 70 % of the samples, causing a total burden of 2852.8 ng L(-1), followed by pyrethroids 15 % of the samples, with a total burden of 926.5 ng L(-1). The tested herbicides were detected in ˂4 % of the samples with a total burden of 353.3 ng L(-1), while organophosphorus levels were below the detection limit. The most frequent contaminants were the following: heptachlor and its epoxide (52 % of samples), followed by DDTs (dichlorodiphenyltrichloroethanes) (DDT and DDE, in 19 % of the samples), cypermethrin and fenvalerate (in 11 % of the samples), and pendimethalin (in oxyfluorfen were not detected in the analyzed samples. Generally, levels were least in autumn, and followed by summer and winter. Sources of contamination might include agricultural lands in central Sudan and upstream sources. Both recent and old contaminations were indicated.

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

International Nuclear Information System (INIS)

Blankson-Arthur, S.

2009-06-01

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

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

Science.gov (United States)

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

2012-05-09

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

Variability of pesticide residues in eggplant units collected from a field trial and marketplaces in Greece.

Science.gov (United States)

Prodhan, Mohammad Dalower Hossain; Papadakis, Emmanouil-Nikolaos; Papadopoulou-Mourkidou, Euphemia

2018-04-01

Variability of pesticide residues among food items is very important when assessing the risks and food safety for the consumers. Therefore, the present study was undertaken to estimate the unit-to-unit residue variability factors for eggplant. In total, 120 samples from a trial field and 142 samples from different marketplaces in Thessaloniki, Greece, were collected to estimate the variability of pesticide residues in eggplant units. They were extracted by the QuEChERS method and the residues were determined by LC-MS/MS. For the field samples, the unit-to-unit variability factors (VFs) obtained for cypermethrin and deltamethrin residues were 2.54 and 2.51, respectively. The mean residue levels of both pesticides were higher in the composite samples than in the individual samples. The average VFs for the marketplace samples was 3.89. The eggplant units exposed to pesticides were higher in residues than the non-exposed units. The variability factors obtained in the marketplace samples were higher than those in the samples collected from the field trial. A default VF value of 3 for field trials is appropriate for use when assessing the acute dietary intake but a VF for the marketplace samples should be reconsidered with a larger data. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Increased occurrence of pesticide residues on crops grown in protected environments compared to crops grown in open field conditions.

Science.gov (United States)

Allen, Gina; Halsall, Crispin J; Ukpebor, Justina; Paul, Nigel D; Ridall, Gareth; Wargent, Jason J

2015-01-01

Crops grown under plastic-clad structures or in greenhouses may be prone to an increased frequency of pesticide residue detections and higher concentrations of pesticides relative to equivalent crops grown in the open field. To test this we examined pesticide data for crops selected from the quarterly reports (2004-2009) of the UK's Pesticide Residue Committee. Five comparison crop pairs were identified whereby one crop of each pair was assumed to have been grown primarily under some form of physical protection ('protected') and the other grown primarily in open field conditions ('open'). For each pair, the number of detectable pesticide residues and the proportion of crop samples containing pesticides were statistically compared (n=100 s samples for each crop). The mean concentrations of selected photolabile pesticides were also compared. For the crop pairings of cabbage ('open') vs. lettuce ('protected') and 'berries' ('open') vs. strawberries ('protected') there was a significantly higher number of pesticides and proportion of samples with multiple residues for the protected crops. Statistically higher concentrations of pesticides, including cypermethrin, cyprodinil, fenhexamid, boscalid and iprodione were also found in the protected crops compared to the open crops. The evidence here demonstrates that, in general, the protected crops possess a higher number of detectable pesticides compared to analogous crops grown in the open. This may be due to different pesticide-use regimes, but also due to slower rates of pesticide removal in protected systems. The findings of this study raise implications for pesticide management in protected-crop systems. Copyright © 2014 Elsevier Ltd. All rights reserved.

Evaluation of pesticide residue dynamics in Chinese cabbage, head cabbage and cauliflower.

Science.gov (United States)

Kocourek, František; Stará, Jitka; Holý, Kamil; Horská, Tereza; Kocourek, Vladimír; Kováčová, Jana; Kohoutková, Jana; Suchanová, Marie; Hajšlová, Jana

2017-06-01

Pesticide residues from the time of application until harvest were analysed for 20, 17 and 18 active insecticidal and fungicidal substances in Chinese cabbage, head cabbage and cauliflower, respectively. In total, 40 mathematical models of residue degradation were developed using a first-order kinetic equation, and from these models it was possible to forecast the action pre-harvest interval for a given action threshold for low-residue production in Brassica vegetables as a percentage of the maximum residue level. Additionally, it was possible to establish an action pre-harvest interval based on an action threshold of 0.01 mg kg ‒1 for the production of Brassica vegetables for baby food. Among the evaluated commodities, the speed of residue degradation was highest in head cabbage, medium in Chinese cabbage and lowest in cauliflower. The half-lives of pesticide in various vegetables were also determined: they ranged from 1.55 to 5.25 days in Chinese cabbage, from 0.47 to 6.54 days in head cabbage and from 1.88 to 7.22 days in cauliflower.

Evaluation of Patterns and Spatial Trends of Pesticide Residues

African Journals Online (AJOL)

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PCA of the data sets for pesticide residues in water, soil and sediments samples from ..... J. Sci. 38(3), 2012. 189. 0.00. 0.20. 0.40. 0.60. 0.80. 1.00. Comp[1]. Comp[2]. R. 2. X. (c u m. ) & ..... Environmental Management, 60: 215-. 225. Wiberg K ...

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

Science.gov (United States)

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

2014-01-01

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

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

Directory of Open Access Journals (Sweden)

M. H. EL-Saeid

2013-01-01

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

Validation Study on a Rapid Method for Simultaneous Determination of Pesticide Residues in Vegetables and Fruits by LC-MS/MS.

Science.gov (United States)

Sato, Tamaki; Miyamoto, Iori; Uemura, Masako; Nakatani, Tadashi; Kakutani, Naoya; Yamano, Tetsuo

2016-01-01

A validation study was carried out on a rapid method for the simultaneous determination of pesticide residues in vegetables and fruits by LC-MS/MS. Preparation of the test solution was performed by a solid-phase extraction technique with QuEChERS (STQ method). Pesticide residues were extracted with acetonitrile using a homogenizer, followed by salting-out and dehydration at the same time. The acetonitrile layer was purified with C18 and PSA mini-columns. The method was assessed for 130 pesticide residues in 14 kinds of vegetables and fruits at the concentration level of 0.01 μg/g according to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan. As a result 75 to 120 pesticide residues were determined satisfactorily in the tested samples. Thus, this method could be useful for a rapid and simultaneous determination of multi-class pesticide residues in various vegetables and fruits.

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

Science.gov (United States)

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

2016-02-01

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

Evaluation of regulatory variation and theoretical health risk for pesticide maximum residue limits in food.

Science.gov (United States)

Li, Zijian

2018-08-01

To evaluate whether pesticide maximum residue limits (MRLs) can protect public health, a deterministic dietary risk assessment of maximum pesticide legal exposure was conducted to convert global MRLs to theoretical maximum dose intake (TMDI) values by estimating the average food intake rate and human body weight for each country. A total of 114 nations (58% of the total nations in the world) and two international organizations, including the European Union (EU) and Codex (WHO) have regulated at least one of the most currently used pesticides in at least one of the most consumed agricultural commodities. In this study, 14 of the most commonly used pesticides and 12 of the most commonly consumed agricultural commodities were identified and selected for analysis. A health risk analysis indicated that nearly 30% of the computed pesticide TMDI values were greater than the acceptable daily intake (ADI) values; however, many nations lack common pesticide MRLs in many commonly consumed foods and other human exposure pathways, such as soil, water, and air were not considered. Normality tests of the TMDI values set indicated that all distributions had a right skewness due to large TMDI clusters at the low end of the distribution, which were caused by some strict pesticide MRLs regulated by the EU (normally a default MRL of 0.01 mg/kg when essential data are missing). The Box-Cox transformation and optimal lambda (λ) were applied to these TMDI distributions, and normality tests of the transformed data set indicated that the power transformed TMDI values of at least eight pesticides presented a normal distribution. It was concluded that unifying strict pesticide MRLs by nations worldwide could significantly skew the distribution of TMDI values to the right, lower the legal exposure to pesticide, and effectively control human health risks. Copyright © 2018 Elsevier Ltd. All rights reserved.

Residue analysis of sixty pesticides in red swamp crayfish using QuEChERS with high-performance liquid chromatography-tandem mass spectrometry

Science.gov (United States)

In this study, a multi-residue analytical method using QuEChERS extraction and dispersive solid-phase extraction (d-SPE) cleanup followed by high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS) was developed for rapid determination of 60 pesticide residues in whole crayfish a...

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

International Nuclear Information System (INIS)

Latif, Y.; Sherazi, S.T.H.; Bhanger, M.I.

2011-01-01

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

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

Directory of Open Access Journals (Sweden)

M. I. Bhanger

2011-12-01

Full Text Available A very sensitive analytical method for the determination of 26 pesticides in some fruits based on solid phase extraction (SPE cleanup was developed using gas chromatography (GC coupled with micro electron capture detector (μECD. 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 μECD 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 μg g-1 in analyzed fruits were above 90% with relative standard deviations (RSD less than 6

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

International Nuclear Information System (INIS)

Andrea, M.M.; Peres, T.B.; Luchini, L.C.; Marcondes, M.A.; Pettinelli, A. Jr.; Nakagawa, L.E.

2001-01-01

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 ([ 14 C]-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 [ 14 C]-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)

Pesticide Residues on Three Cut Flower Species and Potential Exposure of Florists in Belgium

Directory of Open Access Journals (Sweden)

Khaoula Toumi

2016-09-01

Full Text Available In order to assess the prevalence of pesticide contamination and the risk of florists’ exposure when handling cut flowers, sampling and analysis of 90 bouquets of the most commonly sold cut flowers in Belgium (50 bouquets of roses; 20 of gerberas, and 20 of chrysanthemums were carried out. The bouquets were collected from 50 florists located in the seven largest cities of Belgium (Antwerp, Brussels, Charleroi, Ghent, Leuven, Liege, and Namur and from five supermarkets located in the different regions. To have a better understanding of the route of exposure and professional practices a questionnaire was also addressed to a group of 25 florists who volunteered to take part in the survey. All florists were interviewed individually when collecting the questionnaire. The residual pesticide deposit values on cut flowers were determined in an accredited laboratory using a multi-residue (QuEChERS Quick Easy Cheap Effective Rugged Safe method and a combination of gas chromatography (GC and liquid chormatograhphy (LC analysis. A total of 107 active substances were detected from all samples; i.e., an average of about 10 active substances per bouquet. The most severely contaminated bouquet accumulated a total concentration of residues up to 97 mg/kg. Results show that roses are the most contaminated cut flowers; with an average of 14 substances detected per sample and a total concentration per rose sample of 26 mg/kg. Some active substances present an acute toxicity (acephate, methiocarb, monocrotophos, methomyl, deltamethrin, etc. and exposure can generate a direct effect on the nervous system of florists. Nevertheless, fungicides (dodemorph, propamocarb, and procymidone were the most frequently detected in samples and had the highest maximum concentrations out of all the active substances analysed. Dodemorph was the most frequently detected substance with the highest maximum concentration (41.9 mg/kg measured in the rose samples. It appears from the

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

Directory of Open Access Journals (Sweden)

Yuningsih

2006-03-01

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

Risk Analysis on Organochlorine Pesticides Residue in Potato and Carrot from Conventional and Organic Farms in Citarum Watershed Area, West Java Province, Indonesia

Directory of Open Access Journals (Sweden)

Suphia Rahmawati

2017-03-01

Full Text Available Six samples of carrot and potatoes were collected from conventional and organic farms. Organochlorine pesticides (OCPs residue was analyzed using liquid-liquid extraction. The concentration of OCPs residue together with the consumption pattern were used to calculate the potential risk. Estimated Daily Intake (EDI of OCPs residue in carrots and potatoes both from conventional and organic farms were below the standard given in SNI 7313:2008 and the Maximum Residue Limit (MRLs from USEPA . Hazard quotient (HQ and Hazard Index (HI as effect analysis were below the unity, thus there may not be a concern for non-carcinogenic effect. Risk analysis on cancer effects indicated that potatoes samples were above the recommended risk by EPA (10-6. In addition, risk of potatoes samples from organic samples was higher compare to that of the conventional farm. Cancer risk analysis of carrot samples were found below the recommended risk by EPA. Cancer risk effect of carrot samples from conventional farm was slightly higher compare to that of the organic farm.

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

Science.gov (United States)

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

2014-05-01

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

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

Science.gov (United States)

2010-07-01

... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Experimental use permit microbial....2172 Experimental use permit microbial pesticides residue data requirements table. (a) General. Sections 158.100 through 158.130 describe how to use this table to determine the residue chemistry data...

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

Science.gov (United States)

Wang, Jian; Cheung, Wendy; Leung, Daniel

2014-01-29

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

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

Science.gov (United States)

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

2016-01-15

Extreme and uncontrolled usage of pesticides produces a number of problems for vegetation and human health. In this study, the existence of organophosphates (OPs), organochlorines (OCs), pyrethroids (PYs) and fungicides (FUs) were investigated in persimmons/jujubes and their planted soils, which were collected from China. One OP (dimethoate), three OCs (DDT, quintozene and aldrin), six PYs (bifenthrin, fenpropathrin, cyhalothrin, cypermethrin, fenvalerate and deltamethrin) and two FUs (triadimefon and buprofezin) were found in 36.4% of persimmons and 70.8% of jujubes, with concentrations from 1.0 μg/kg to 2945.0 μg/kg. The most frequently detected pesticides in the two fruits were fenpropathrin in persimmons and cypermethrin in jujubes, with the detection frequencies of 30.0% and 22.7%, respectively. The residues of 4.5% (persimmon) and 25.0% (jujube) of samples were higher than the maximum residue limits (MRLs) of China. Compared with the fruits, more types of pesticides and higher residues were observed in their planted soils. The most frequently detected pesticides were HCH in persimmon soil and DDT in jujube soil, with the detection frequencies of 10.9% and 12.7%, respectively. For the tested samples, 39.1% of fruit samples and 63.0% of soil samples with multiple residues (containing more than two pesticides) were noted, even up to 8 residues in fruits and 14 residues in soils. Except for cyhalothrin, the other short-term risks for the tested pesticides in the fruits were below 10%, and the highest long-term risk was 14.13% for aldrin and dieldrin. There was no significant health risk for consumers via consumption of the two fruits. Copyright © 2015 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2007-06-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Masiá, Ana [Food and Environmental Safety Research Group, Department of Preventive Medicine and Public Health, Food Science, Toxicology and Legal Medicine, University of Valencia, Valencia (Spain); Research Center on Desertification (CIDE, UV-CSIC-GV), Carretera Moncada-Náquera, Moncada (Spain); Suarez-Varela, Maria Morales; Llopis-Gonzalez, Agustin [Unit of Public Health, Hygiene and Environmental Health, Department of Preventive Medicine and Public Health, Food Science, Toxicology and Legal Medicine, University of Valencia, Valencia (Spain); CIBER Epidemiología y Salud Pública (CIBERESP), Madrid (Spain); Center for Advanced Research in Public Health (CSISP-FISABIO), Valencia (Spain); Picó, Yolanda, E-mail: Yolanda.Pico@uv.es [Food and Environmental Safety Research Group, Department of Preventive Medicine and Public Health, Food Science, Toxicology and Legal Medicine, University of Valencia, Valencia (Spain); Research Center on Desertification (CIDE, UV-CSIC-GV), Carretera Moncada-Náquera, Moncada (Spain); CIBER Epidemiología y Salud Pública (CIBERESP), Madrid (Spain)

2016-09-14

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

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

International Nuclear Information System (INIS)

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

2016-01-01

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

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

OpenAIRE

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

2012-01-01

Milk of cattle was collected from various localities of Faisalabad, Pakistan. Pesticides concentration was determined by HPLC using solid phase microextraction. The residue analysis revealed that about 40% milk samples were contaminated with pesticides. The mean±SE levels (ppm) of cyhalothrin, endosulfan, chlorpyrifos and cypermethrin were 0.38±0.02, 0.26±0.02, 0.072±0.01 and 0.085±0.02, respectively. Quantitative structure activity relationship (QSAR) models were used to predict the residues...

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

Science.gov (United States)

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

2014-05-01

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

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

Science.gov (United States)

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

Assessment of the effect of washing and boiling on the levels of pesticide residues in vegetables cultivated in Akuapem North Municipality

International Nuclear Information System (INIS)

Opare-Boafo, Maame Serwa

2016-07-01

Vegetables play an important role in human nutrition and health. Pesticides are extensively used by vegetable farmers in crop production and this may contaminate the crop. Traditional method of washing vegetables prior to consumption has been assumed to reduce pesticide residues. The study seeks to assess the effect of washing with various solutions and with boiling on the concentration of pesticide residues in vegetables and to estimate the potential human health risk associated with pesticide ingestion via vegetable diet using the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method. Results of the study indicated that the farmers involved in vegetable farming in the Akwapim North Municipality are in the middle age group and use pesticides in their farming activities. Majority (65%) of them have no formal training in pesticide usage and apply pesticides in mixtures made of combinations of up to four (4) pesticides in a single tank mixture. The farmers do not use any protective clothing and stores agrochemicals in multipurpose storage structures together with food containers and farm implements. As a result of pesticide exposure, 67% of farmers experienced various kinds of discomfort including headache, tingling or burning of skin, irritation of eyes or skin. Chloropyrifos residue was the only pesticide residue that gave positive detection in the analysed vegetable samples. The raw (non-spiked) vegetable samples (cabbage, lettuce and squash) had 0.29 mg kg -1 , 0.19 mg kg -1 and 0.14 mg kg -1 of Chloropyrifos residue in cabbage, squash and lettuce respectively. The level of chloropyrifos residues detected in raw cabbage samples from the study area was below the maximum permissible limit (MPLs) of 1 mg/kg (Codex, 2003) but the residues found in raw squash was above the maximum permissible limit of 0.01 mg/kg and that of lettuce was also above the maximum permissible limit (0.05mg/kg). Washing of vegetables vigorously in water for 2 minutes before

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

DEFF Research Database (Denmark)

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

2007-01-01

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......(-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....

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

International Nuclear Information System (INIS)

Jimenez, V.; Ramos de Jimenez, J.; Rojas, B.

1999-01-01

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 18 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 μg/L carbofuran, 0.016 μg/L chlorothalonil, 0.007 μg/L ametryn and 0.003 μg/L chlorpyrifos, when using standard spiked solutions. Recovery (%) was high when standard mixtures were used for the test runs but low when real surface water samples were tested, especially for chlorothalonil which was not recovered at all. (author)

9 CFR 318.16 - Pesticide chemicals and other residues in products.

Science.gov (United States)

2010-01-01

..., DEPARTMENT OF AGRICULTURE AGENCY ORGANIZATION AND TERMINOLOGY; MANDATORY MEAT AND POULTRY PRODUCTS INSPECTION... ingredients. Residues of pesticide chemicals, food additives and color additives or other substances in or on ingredients (other than meat, meat byproducts, and meat food products) used in the formulation of products...

Pesticide residues in leafy vegetables and human health risk assessment in North Central agricultural areas of Chile.

Science.gov (United States)

Elgueta, Sebastian; Moyano, Stella; Sepúlveda, Paulina; Quiroz, Carlos; Correa, Arturo

2017-06-01

To investigate pesticide residue concentrations and potential human health risk, a study was conducted in 118 leafy vegetable samples collected in 2014-2015 from the North Central agricultural areas of Chile. The pesticide residues were determined using the multiresidue QuEChERS method by gas chromatography as well as high-performance liquid chromatography. The results indicated that 27% of the total samples contained pesticide residues above the maximum residue limits of each active ingredient. The maximum estimated daily intake obtained for carbon disulphide (CS 2 ), methamidophos, azoxystrobin and cypermethrin were 0.57, 0.07, 0.06 and 0.05 mg kg -1 , respectively, which was higher than their acceptable daily intake. It is concluded that inhabitants of the North Central agricultural area of Chile are not exposed to health risks through the consumption of leafy vegetables with the exception of methamidophos. Nevertheless, the high levels of methamidophos detected in leafy vegetables could be considered a potential chronic health risk.

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

Science.gov (United States)

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

2015-01-01

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

Removal of acidic interferences in multi-pesticides residue analysis of fruits using modified magnetic nanoparticles prior to determination via ultra-HPLC-MS/MS

International Nuclear Information System (INIS)

Qi, Peipei; Wang, Zhiwei; Yang, Guiling; Wang, Xinquan; Shang, Chunqing; Xu, Hao; Wang, Xiangyun; Zhang, Hu; Wang, Qiang

2015-01-01

The authors describe magnetite (Fe 3 O 4 ) nanoparticles modified with 3-(N,N-diethylamino) propyltrimethoxysilane (Fe 3 O 4 -PSA NPs) for use as a sorbent for dispersive solid phase extraction of pesticide residues. The Fe 3 O 4 -PSA NPs were prepared by silanizing Fe 3 O 4 NPs and modifying them with 3-(N,N-diethylamino) propyltrimethoxysilane. Field-emission scanning electron microscopy, FTIR and zeta potential measurements were employed to characterize the modified NPs. They were then used as an adsorbent to remove acidic interferences (such as malic acid and succinic acid), which are major interferences in LC-MS/MS analysis in causing ion suppression in the MS spectra of pesticides. In addition, graphitized carbon black (GCB) was used as an adsorbent to eliminate interferences by pigments. The use of Fe 3 O 4 -PSA NPs can replace time-consuming centrifugation as used in the so-called QuEChERS (quick, easy, cheap, effective, rugged and safe) method. This improvement is particularly significant in high-throughput analysis. Following the optimization of the quantities of Fe 3 O 4 -PSA NPs and GCB, the method was applied to the determination of 56 pesticides in (spiked) fruits (apple, kiwi, orange and pear) by ultra-HPLC-MS/MS. The analytical ranges typically extend from 1 to 200 ng∙mL −1 , and recoveries range from 60.2 to 130 % at different concentrations of all four kinds of fruits. The LOQs for the pesticides are 10 ng∙kg −1 , which makes the method a viable tool for pesticide monitoring in fruits. (author)

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

Energy Technology Data Exchange (ETDEWEB)

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

1996-12-31

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

Organic amendments for risk mitigation of organochlorine pesticide residues in old orchard soils

Science.gov (United States)

Centofantia, Tiziana; McConnell, Laura L.; Chaney, Rufus L.; Beyer, W. Nelson; Andradea, Natasha A.; Hapeman, Cathleen J.; Torrents, Alba; Nguyen, Anh; Anderson, Marya O.; Novak, J. M.; Jackson, Dana

2015-01-01

Performance of compost and biochar amendments for in situ risk mitigation of aged DDT, DDE and dieldrin residues in an old orchard soil was examined. The change in bioavailability of pesticide residues to Lumbricus terrestris L. relative to the unamended control soil was assessed using 4-L soil microcosms with and without plant cover in a 48-day experiment. The use of aged dairy manure compost and biosolids compost was found to be effective, especially in the planted treatments, at lowering the bioavailability factor (BAF) by 18–39%; however, BAF results for DDT in the unplanted soil treatments were unaffected or increased. The pine chip biochar utilized in this experiment was ineffective at lower the BAF of pesticides in the soil. The US EPA Soil Screening Level approach was used with our measured values. Addition of 10% of the aged dairy manure compost reduced the average hazard quotient values to below 1.0 for DDT + DDE and dieldrin. Results indicate this sustainable approach is appropriate to minimize risks to wildlife in areas of marginal organochlorine pesticide contamination. Application of this remediation approach has potential for use internationally in areas where historical pesticide contamination of soils remains a threat to wildlife populations.

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

International Nuclear Information System (INIS)

1990-01-01

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 14 C 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

Intake of Fruits and Vegetables with Low-to-Moderate Pesticide Residues Is Positively Associated with Semen-Quality Parameters among Young Healthy Men123

Science.gov (United States)

Gaskins, Audrey J; Williams, Paige L; Mendiola, Jaime; Levine, Hagai; Hauser, Russ; Swan, Shanna H; Chavarro, Jorge E

2016-01-01

Background: Numerous studies have shown that occupational or environmental pesticide exposure can affect male fertility. There is less evidence, however, regarding any potentially adverse effects of pesticide residues in foods on markers of male fertility potential. Objectives: We examined the relations between fruit and vegetable intake, considering pesticide residue status, and semen quality and serum concentrations of reproductive hormones in healthy young men. Methods: The Rochester Young Men's Study is a cross-sectional study that recruited men aged 18–22 y (n = 189) in Rochester, New York. Participants completed a questionnaire, provided a semen sample, had a blood sample drawn, and underwent a physical examination at enrollment. Semen samples were analyzed for total sperm count, sperm concentration, morphology, motility, ejaculate volume, total motile count, and total normal count. Dietary intake during the previous year was assessed by a validated food-frequency questionnaire. Fruit and vegetables were categorized as having high [Pesticide Residue Burden Score (PRBS) ≥4] or low-to-moderate (PRBS vegetable intake with semen variables and reproductive hormones while adjusting for potential confounding factors. Results: The total intake of fruit and vegetables was unrelated to semen quality. However, the intake of fruit and vegetables with low-to-moderate pesticide residues was associated with a higher total sperm count and sperm concentration, whereas the intake of fruit and vegetables with high pesticide residues was unrelated to semen quality. On average, men in the highest quartile of low-to-moderate-pesticide fruit and vegetable intake (≥2.8 servings/d) had a 169% (95% CI: 45%, 400%) higher total sperm count and a 173% (95% CI: 57%, 375%) higher sperm concentration than did men in the lowest quartile (vegetables, regardless of pesticide-residue status, was not associated with reproductive hormone concentrations. Conclusions: The consumption of fruit

Development of methods for screening pesticide residues in plant matrices in Ghana

International Nuclear Information System (INIS)

Lowor, Samuel Tetteh

1999-12-01

TLC has been used in combination with micro-extraction and clean-up methods to provide an alternative cost effective analytical procedure for screening pesticide residues in plant matrices. Thirty-five (35) agrochemicals, which are used in priority crops in Ghana, were used in this study. Ethylacetate extraction in the presence of anhydrous sodium sulphate, followed by gel permeation chromatographic clean up and additional purification on silica gel cartridges provided clean extracts enabling the application of 300mg sample equivalent on the TLC plates. Detection method involving the use of O-tolidine was found to be suitable for general screening of residues, having medium sensitivity for several compounds. The method involving the use of silver nitrate was the only one found to be most suitable for detecting the organo chlorine pesticides. Lindane was the most sensitive to this reagent and had a Minimum Detectable Quantity (MDQ) value of 5ng/5 uL. This method was suitable for use on only alumina plates and detection was also possible even under sunlight. The enzyme inhibition methods were very sensitive to the carbamate and phosphoric acid type insecticides with MDQ values between 0.2 and 2000ng. Other detection methods involving p-nitrobenzene, p-dimethylaminobenzaldehyde and photosynthesis inhibition were also tried and discussed. The database developed has been successfully used for screening and semiquantitative determination of some ranges of pesticide residue in soil and plant matrices. (au)

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

International Nuclear Information System (INIS)

Talukder, F.A.; Dahmani, J.H.A.; Kaakeh, W.; Deadman, M.L.

2008-01-01

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)

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

International Nuclear Information System (INIS)

Anwar, T.; Ahmad, I.; Tahir, S.

2011-01-01

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)

pesticide residues in water from tpc sugarcane plantations

African Journals Online (AJOL)

ABSTRACT. We report herein, the analysis of water samples collected from TPC Sugarcane Plantation and its environs in Kilimanjaro region, which is the earliest intensive user of pesticides in Tanzania. A total of 50 water samples collected from 18 sampling sites between 2000 and 2001 were analyzed for pesticide ...

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

NARCIS (Netherlands)

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

2012-01-01

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

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

International Nuclear Information System (INIS)

Sheng Guangyao; Yang Yaning; Huang Minsheng; Yang Kai

2005-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Sheng Guangyao [Department of Crop, Soil, and Environmental Sciences, University of Arkansas, Fayetteville, AR 72701 (United States)]. E-mail: gsheng@uark.edu; Yang Yaning [Department of Crop, Soil, and Environmental Sciences, University of Arkansas, Fayetteville, AR 72701 (United States); Huang Minsheng [Department of Environmental Science and Technology, East China Normal University, Shanghai 200062 (China); Yang Kai [Department of Environmental Science and Technology, East China Normal University, Shanghai 200062 (China)

2005-04-01

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 {approx}3.0 and {approx}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 {approx}7.0 than at pH {approx}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 {approx}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 {approx}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 {approx}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.

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

Science.gov (United States)

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

2014-11-01

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 μg/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). Copyright © 2014 Elsevier Ltd. All rights reserved.

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

Science.gov (United States)

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

2012-11-01

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

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

Science.gov (United States)

2010-09-23

... (NAICS code 111). Animal production (NAICS code 112). Food manufacturing (NAICS code 311). Pesticide..., Cheshire CH65 4EY, United Kingdom, proposes to establish an exemption from the requirement of a tolerance... residues harmful to plants and animals is highly unlikely to occur when it is applied as part of the...

Pesticide Residues in Commercial Lettuce, Onion, and Potato Samples From Bolivia—A Threat to Public Health?

DEFF Research Database (Denmark)

Skovgaard, Marlene; Renjel, Susana; Jensen, Olaf Chresten

2017-01-01

Bolivia does not have a surveillance program for pesticide residues in food. The few published studies have suggested that pesticide contamination in food may present a public health problem. Data are lacking for all foods except tomatoes and breast milk. In this study 10 potato, 10 onion, and 10...... or together would lead to exposures that exceeded the acceptable daily intake or the acute reference dose. To protect consumers from pesticide poisonings and chronic effects, the development of measures for prevention, control, and monitoring of food contamination by pesticides in Bolivia is suggested....

Determination of pesticide residues in cereal grains

International Nuclear Information System (INIS)

Fuzesi, I.; Susan, M.

2005-01-01

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)

[An experimental proficiency test for ability to screen 104 residual pesticides in agricultural products].

Science.gov (United States)

Tsumura, Yukari; Ishimitsu, Susumu; Otaki, Kayo; Uchimi, Hiroyuki; Matsumoto, Nobuyuki; Daba, Masaki; Tsuchiya, Tetsu; Ukyo, Masaho; Tonogai, Yasuhide

2003-10-01

An experimental proficiency test program for ability to screen 104 residual pesticides in agricultural products has been conducted. Eight Japanese laboratories joined the program. Items tested in the present study were limit of detection, internal proficiency test (self spike) and external proficiency test (blind spike). All 104 pesticides were well detected and recovered from agricultural foods in the internal proficiency test. However, the results of the external proficiency test did not completely agree with those of the internal proficiency tests. After 5 rounds of the blind spike test, the ratio of the number of correctly detected pesticides to that of actually contained ones (49 total) ranged from 65% to 100% among laboratories. The numbers of mistakenly detected pesticides by a laboratory were 0 to 15. Thus, there was a great difference among the laboratories in the ability to screen multiresidual pesticides.

Organic amendments for risk mitigation of organochlorine pesticide residues in old orchard soils

International Nuclear Information System (INIS)

Centofanti, Tiziana; McConnell, Laura L.; Chaney, Rufus L.; Beyer, W. Nelson; Andrade, Natasha A.; Hapeman, Cathleen J.; Torrents, Alba; Nguyen, Anh; Anderson, Marya O.; Novak, Jeffrey M.

2016-01-01

Performance of compost and biochar amendments for in situ risk mitigation of aged DDT, DDE and dieldrin residues in an old orchard soil was examined. The change in bioavailability of pesticide residues to Lumbricus terrestris L. relative to the unamended control soil was assessed using 4-L soil microcosms with and without plant cover in a 48-day experiment. The use of aged dairy manure compost and biosolids compost was found to be effective, especially in the planted treatments, at lowering the bioavailability factor (BAF) by 18–39%; however, BAF results for DDT in the unplanted soil treatments were unaffected or increased. The pine chip biochar utilized in this experiment was ineffective at lower the BAF of pesticides in the soil. The US EPA Soil Screening Level approach was used with our measured values. Addition of 10% of the aged dairy manure compost reduced the average hazard quotient values to below 1.0 for DDT + DDE and dieldrin. Results indicate this sustainable approach is appropriate to minimize risks to wildlife in areas of marginal organochlorine pesticide contamination. Application of this remediation approach has potential for use internationally in areas where historical pesticide contamination of soils remains a threat to wildlife populations. - Highlights: • Historical applications of organochlorine pesticides are a risk to local ecosystems. • Low cost and sustainable mitigation measures are needed to reduce risks. • Organic matter rich amendments were added to contaminated soil. • Earthworms microcosms were used to measure bioaccumulation factors. • Aged composts were most effective at mitigating risks to ecosystems. - Incorporation of aged dairy manure and biosolids compost amendments is an effective, low cost approach to mitigate risks to terrestrial wildlife from organochlorine pesticides in soils.

Sensitivity analysis of the STICS-MACRO model to identify cropping practices reducing pesticides losses.

Science.gov (United States)

Lammoglia, Sabine-Karen; Makowski, David; Moeys, Julien; Justes, Eric; Barriuso, Enrique; Mamy, Laure

2017-02-15

STICS-MACRO is a process-based model simulating the fate of pesticides in the soil-plant system as a function of agricultural practices and pedoclimatic conditions. The objective of this work was to evaluate the influence of crop management practices on water and pesticide flows in contrasted environmental conditions. We used the Morris screening sensitivity analysis method to identify the most influential cropping practices. Crop residues management and tillage practices were shown to have strong effects on water percolation and pesticide leaching. In particular, the amount of organic residues added to soil was found to be the most influential input. The presence of a mulch could increase soil water content so water percolation and pesticide leaching. Conventional tillage was also found to decrease pesticide leaching, compared to no-till, which is consistent with many field observations. The effects of the soil, crop and climate conditions tested in this work were less important than those of cropping practices. STICS-MACRO allows an ex ante evaluation of cropping systems and agricultural practices, and of the related pesticides environmental impacts. Copyright © 2016 Elsevier B.V. All rights reserved.

Organochlorine Pesticides Residues in Human Breast Milk from the Middle Governorates in Jordan in 2013/2014.

Science.gov (United States)

Al Antary, Tawfiq M; Alawi, Mahmoud A; Estityah, Hussein; Haddad, Nizar

2017-07-01

One hundred samples of mother breast milk were gathered from six middle governorates and districts in Jordan in 2013/2014 to monitor Organochlorine pesticides pollutants. The results showed clearly that banned organochlorine pesticides are still detected in the monitored samples in low concentration despite banning of these persistent pollutants in Jordan since 36 years ago. However, the results indicated that 1% of the contaminated samples contained β-HCH, 5% γ-HCH, 3% p,p'-DDD, 2% heptachlor, 45% p,p'-DDE and 3% p,p'-DDT. In addition, these monitored samples had no residues of aldrin, dieldrin, α-endosulfan, β-endosulfan, HCB, o,p'-DD, o,p'-DDT and o,p'-DDE. In conclusion, there was a decline in the residues of Organochlorine pesticides, particularly DDT group members.

Pesticide residues in fruit samples: comparison of different QuEChERS methods using liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Christia, C; Bizani, E; Christophoridis, C; Fytianos, K

2015-09-01

Acetate- and citrate-buffered quick, easy, cheap, effective, rugged, safe (QuEChERS) pretreatment methods were evaluated for the determination of various pesticides in peaches, grapes, apples, bananas, pears, and strawberries from various regions of Greece, using LC-MS/MS. The purposes of this study were (i) to evaluate which type of QuEChERS method was the most appropriate and effective for each matrix; (ii) to apply the selected QuEChERS method for each matrix, in order to detect and quantify pesticide residues in various fruit samples using UPLC-MS/MS; (iii) to examine the concentration distribution of pesticide classes among fruit originating from various areas; and (iv) to assess pesticide concentration distribution between peel and flesh of fruit in order to evaluate the penetration of pesticide residues in the fruit flesh. Acetate-buffered QuEChERS was found to be the most suitable technique for most of the fruit matrices. According to the recovery values at two different concentration levels, peaches should preferably be treated by the citrate-buffered type, whereas grapes, bananas, apples, pears, and strawberries are best treated by the acetate-buffered version, although the differences in efficiency were small. The addition of graphitized carbon black significantly decreases the recovery of specific pesticides in all matrices except for strawberries. The majority of values do not exceed the official maximum residue levels set by the European Commission. Organophosphates proved to be the most commonly detected category along with triazines-triazoles-conazoles group and by carbamates. Apples and pears seem to be the most contaminated fruit matrices among those tested. Distribution of pesticide classes shows variations between different regions, suggesting different pesticide application practices. In the case of peaches and pears, there is an equal distribution of detected pesticides between peel and flesh, indicating penetration of contaminants into the

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

Science.gov (United States)

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

2014-10-22

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

Residue analysis of organochlorine pesticides in water and ...

African Journals Online (AJOL)

Mr Willims

2013-05-12

May 12, 2013 ... and public health purposes because of their low cost and versatility in ... water, air and sediment or in biota. ... Pesticides II EPA Method 8081A was employed for the analyses. ..... Ize-Iyamu OK, Asia IO, Egwakhide PA (2007).

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

DEFF Research Database (Denmark)

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

2011-01-01

We are working on the development of a real-time electrochemical sensor based on an immunoassay detection system to detect and quantify the presence of pesticide residues in ground water. Highly selective and sensitive immuno-reactions are being investigated to be optimized in order to bring them...

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

International Nuclear Information System (INIS)

Baysoyu, D.; Tiryaki, O.; Secer, E.; Aydin, G.

2009-01-01

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 1 4C-carbaryl by radioisotope tracer technique. 1 4C-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.

Factors Affecting Transfer of Pyrethroid Residues from Herbal Teas to Infusion and Influence of Physicochemical Properties of Pesticides

Directory of Open Access Journals (Sweden)

Jin-Jing Xiao

2017-09-01

Full Text Available The transfer of pesticide residues from herbal teas to their infusion is a subject of particular interest. In this study, a multi-residue analytical method for the determination of pyrethroids (fenpropathrin, beta-cypermethrin, lambda-cyhalothrin, and fenvalerate in honeysuckle, chrysanthemum, wolfberry, and licorice and their infusion samples was validated. The transfer of pyrethroid residues from tea to infusion was investigated at different water temperatures, tea/water ratios, and infusion intervals/times. The results show that low amounts (0–6.70% of pyrethroids were transferred under the different tea brewing conditions examined, indicating that the infusion process reduced the pyrethroid content in the extracted liquid by over 90%. Similar results were obtained for the different tea varieties, and pesticides with high water solubility and low octanol–water partition coefficients (log Kow exhibited high transfer rates. Moreover, the estimated values of the exposure risk to the pyrethroids were in the range of 0.0022–0.33, indicating that the daily intake of the four pyrethroid residues from herbal tea can be regarded as safe. The present results can support the identification of suitable tea brewing conditions for significantly reducing the pesticide residue levels in the infusion.

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

Science.gov (United States)

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

2010-04-01

The potential of three mass spectrometry (MS) analyzers (triple quadrupole, QqQ; time of flight, TOF; and quadrupole time of flight, QTOF) has been investigated and compared for quantification, confirmation and screening purposes in pesticide residue analysis of fruit and vegetable samples. For this purpose, analytical methodology for multiresidue determination of 11 pesticides, taken as a model, has been developed and validated in nine food matrices for the three mass analyzers coupled to ultra high pressure liquid chromatography. In all cases, limits of quantification around 0.01 mg/kg were reached, fulfilling the most restrictive case of baby-food analysis. Regarding absolute sensitivity, the lower limits of detection were obtained, as expected, for QqQ (100 fg), whereas slightly higher limits (300 fg) were obtained for both TOF and QTOF. Confirmative capacity of each analyzer was studied for each analyte based on the identification points (IPs) criterion, useful for a comprehensive comparison. QTOF mass analyzer showed the highest confirmatory capacity, although QqQ normally led to sufficient number of IPs, even at lower concentration levels. The potential of TOF MS was also investigated for screening purposes. To this aim, around 50 commercial fruits and vegetables samples were analyzed, searching for more than 400 pesticides. TOF MS proved to be an attractive analytical tool for rapid detection and reliable identification of a large number of pesticides thanks to the full spectrum acquisition at accurate mass with satisfactory sensitivity. This process is readily boosted when combined with specialized software packages, together with theoretical exact mass databases. Several pesticides (e.g. carbendazim in citrus and indoxacarb in grape) were detected in the samples. Further unequivocal confirmation of the identity was performed using reference standards and/or QTOF MS/MS experiments. Copyright 2010 John Wiley & Sons, Ltd.

Tracking residual organochlorine pesticides (OCPs) in green, herbal, and black tea leaves and infusions of commercially available tea products marketed in Poland.

Science.gov (United States)

Witczak, Agata; Abdel-Gawad, Hassan; Zalesak, Michal; Pohoryło, Anna

2018-03-01

The content of residual organochlorine pesticides (OCPs) was examined in green, herbal, and black tea leaves as well as in their infusions prepared from tea products marketed in the main supermarkets in Poland. It was found that the detected mean levels of organochlorine residues in tea leaves ranged from tea occurred in the highest concentrations. Among dichlorodiphenyltrichloroethane (DDT) metabolites the highest level of p,p'DDT (1.96 ng g -1 dw) was in green tea samples. The transfer of OCPs from tea leaves to brew was investigated. The present study revealed that during the infusion process, a significant percentage of the residues, particularly pesticides with high water solubility, were transferred to the infusions. The obtained results show that the percentage transfer of each pesticides from tea to the tea infusions ranged from 6.74% (heptachlor) to 86.6% (endrin). The detected residues were below current MRLs for these pesticides.

Intake of Fruits and Vegetables with Low-to-Moderate Pesticide Residues Is Positively Associated with Semen-Quality Parameters among Young Healthy Men.

Science.gov (United States)

Chiu, Yu-Han; Gaskins, Audrey J; Williams, Paige L; Mendiola, Jaime; Jørgensen, Niels; Levine, Hagai; Hauser, Russ; Swan, Shanna H; Chavarro, Jorge E

2016-05-01

Numerous studies have shown that occupational or environmental pesticide exposure can affect male fertility. There is less evidence, however, regarding any potentially adverse effects of pesticide residues in foods on markers of male fertility potential. We examined the relations between fruit and vegetable intake, considering pesticide residue status, and semen quality and serum concentrations of reproductive hormones in healthy young men. The Rochester Young Men's Study is a cross-sectional study that recruited men aged 18-22 y (n = 189) in Rochester, New York. Participants completed a questionnaire, provided a semen sample, had a blood sample drawn, and underwent a physical examination at enrollment. Semen samples were analyzed for total sperm count, sperm concentration, morphology, motility, ejaculate volume, total motile count, and total normal count. Dietary intake during the previous year was assessed by a validated food-frequency questionnaire. Fruit and vegetables were categorized as having high [Pesticide Residue Burden Score (PRBS) ≥4] or low-to-moderate (PRBS sperm count and sperm concentration, whereas the intake of fruit and vegetables with high pesticide residues was unrelated to semen quality. On average, men in the highest quartile of low-to-moderate-pesticide fruit and vegetable intake (≥2.8 servings/d) had a 169% (95% CI: 45%, 400%) higher total sperm count and a 173% (95% CI: 57%, 375%) higher sperm concentration than did men in the lowest quartile (sperm counts in young men unselected by fertility status. This suggests that pesticide residues may modify the beneficial effects of fruit and vegetable intake on semen quality. © 2016 American Society for Nutrition.

Pesticide Residues, Results from the period 2004-2011

DEFF Research Database (Denmark)

Petersen, Annette; Jensen, Bodil Hamborg; Andersen, Jens Hinge

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...

Screening of 439 Pesticide Residues in Fruits and Vegetables by Gas Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry Based on TOF Accurate Mass Database and Q-TOF Spectrum Library.

Science.gov (United States)

Li, Jian-Xun; Li, Xiao-Ying; Chang, Qiao-Ying; Li, Yan; Jin, Ling-He; Pang, Guo-Fang; Fan, Chun-Lin

2018-05-03

Because of its unique characteristics of accurate mass full-spectrum acquisition, high resolution, and fast acquisition rates, GC-quadrupole-time-of-flight MS (GC-Q-TOF/MS) has become a powerful tool for pesticide residue analysis. In this study, a TOF accurate mass database and Q-TOF spectrum library of 439 pesticides were established, and the parameters of the TOF database were optimized. Through solid-phase extraction (SPE), whereby pesticides are extracted from fruit and vegetable substrates by using 40 mL 1% acetic acid in acetonitrile (v/v), purified by the Carbon/NH₂ SPE cartridge, and finally detected by GC-Q-TOF/MS, the rapid analysis of 439 pesticides in fruits and vegetables can be achieved. The methodology verification results show that more than 70 and 91% of pesticides, spiked in fruits and vegetables with concentrations of 10 and 100 μg/kg, respectively, saw recoveries that conform to the European Commission's criterion of between 70 and 120% with RSD ≤20%. Eighty-one percent of pesticides have screening detection limits lower than 10 μg/kg, which makes this a reliable analysis technology for the monitoring of pesticide residues in fruits and vegetables. This technology was further validated for its characteristics of high precision, high speed, and high throughput through successful detection of 9817 samples during 2013-2015.

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

International Nuclear Information System (INIS)

Cheah Uan Boh; Lum Keng Yeang

2002-01-01

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

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

Science.gov (United States)

Farré, M; Picó, Y; Barceló, D

2014-02-07

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. Copyright © 2013 Elsevier B.V. All rights reserved.

Evaluating organochlorine pesticide residues in the aquatic environment of the Lake Naivasha River basin using passive sampling techniques.

Science.gov (United States)

Abbasi, Yasser; Mannaerts, Chris M

2018-05-18

Passive sampling techniques can improve the discovery of low concentrations by continuous collecting the contaminants, which usually go undetected with classic and once-off time-point grab sampling. The aim of this study was to evaluate organochlorine pesticide (OCP) residues in the aquatic environment of the Lake Naivasha river basin (Kenya) using passive sampling techniques. Silicone rubber sheet and Speedisk samplers were used to detect residues of α-HCH, β-HCH, γ-HCH, δ-HCH, heptachlor, aldrin, heptachlor epoxide, pp-DDE, endrin, dieldrin, α-endosulfan, β-endosulfan, pp-DDD, endrin aldehyde, pp-DDT, endosulfan sulfate, and methoxychlor in the Malewa River and Lake Naivasha. After solvent extraction from the sampling media, the residues were analyzed using gas chromatography electron capture detection (GC-ECD) for the OCPs and gas chromatography-mass spectrometry (GC-MS) for the PCB reference compounds. Measuring the OCP residues using the silicone rubber samplers revealed the highest concentration of residues (∑OCPs of 81 (± 18.9 SD) μg/L) to be at the Lake site, being the ultimate accumulation environment for surficial hydrological, chemical, and sediment transport through the river basin. The total OCP residue sums changed to 71.5 (± 11.3 SD) μg/L for the Middle Malewa and 59 (± 12.5 SD) μg/L for the Upper Malewa River sampling sites. The concentration sums of OCPs detected using the Speedisk samplers at the Upper Malewa, Middle Malewa, and the Lake Naivasha sites were 28.2 (± 4.2 SD), 31.3 (± 1.8 SD), and 34.2 (± 6.4 SD) μg/L, respectively. An evaluation of the different pesticide compound variations identified at the three sites revealed that endosulfan sulfate, α-HCH, methoxychlor, and endrin aldehyde residues were still found at all sampling sites. However, the statistical analysis of one-way ANOVA for testing the differences of ∑OCPs between the sampling sites for both the silicone rubber sheet and Speedisk samplers

Association between blood cholinesterase activity, organophosphate pesticide residues on hands, and health effects among chili farmers in Ubon Ratchathani Province, northeastern Thailand

Science.gov (United States)

Nganchamung, Thitirat; Robson, Mark G; Siriwong, Wattasit

Use of pesticides has been documented to lead to several adverse health effects. Farmers are likely to be exposed to pesticides through dermal exposure as a result of mixing, loading, and spraying. Organophosphate pesticides (OPs) are widely used in most of the agricultural areas throughout Thailand. OPs are cholinesterase inhibitors and blood cholinesterase activity is used as a biomarker of OP effects. This study aims to determine the association between blood cholinesterase activity and organophosphate pesticide residues on chili farmer’s hands and their adverse health effects. Ninety chili farmers directly involved with pesticide applications (e.g. mixing, loading, spraying) were recruited and were interviewed face to face. Both enzymes, erythrocyte acetylcholinesterase (AChE) and plasma cholinesterase (PChE), were tested with the EQM Test-mate Cholinesterase Test System (Model 400). Hand wipe samples were used for collecting residues on both hands and OP residues for chlorpyrifos and profenofos were quantified using gas chromatography equipped with a flame photometric detector (GC-FPD). The average activity (±SD) of AChE and PChE was 2.73 (±0.88) and 1.58 (±0.56) U/mL, respectively. About 80.0% of the participants had detectable OP residues on hands. The median residues of chlorpyrifos and profenofos were found to be 0.02 and 0.03 mg/kg/two hands, respectively. Half of participants reported having some acute health symptoms within 48 hours after applying pesticides. When adjusted for gender, number of years working in chili farming, and frequency of pesticide use, AChE activity (Adjusted OR = 0.03, 95%CI: 0.01-0.13) and detected OP residues on hands (Adjusted OR = 0.15, 95%CI: 0.02-0.95) were significantly associated with having health effects, but no significant association was found in PChE activity (Adjusted OR = 2.09, 95%CI: 0.63-6.99). This study suggests that regular monitoring for blood cholinesterase and effective interventions to reduce pesticide

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

NARCIS (Netherlands)

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

1998-01-01

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

Assessment of organochlorine pesticides and atrazine residues in Maize Produced in Ghana using GC-ECD/ GC-MS

International Nuclear Information System (INIS)

Miensah, E.D.

2015-07-01

Maize is consumed by over 95% of the Ghanaian populace and the practice of using atrazine, lindane and other organochlorine pesticides in its production has raised concerns about potential adverse effects on human health and the environment. A field survey was conducted in this study to assess farmers’ knowledge of safe handling and use of these chemicals as well as toxicity awareness and symptoms among farmers and traders. Residues of the pesticides in maize samples as well as the potential health risk associated with exposure to them were also evaluated. Data obtained from the field survey indicate that a large proportion of farmers are at risk of pesticide poisoning through occupational exposure. Over 80 % of applicators do not apply safety precautions during pesticide mixing and application; resulting in considerable prevalence of pesticide related illnesses in the study area. Residues of lindane and atrazine were below detection limits of 0.005 mg/kg and 0.010 mg/kg respectively of the GC-ECD/MS used for the analysis; except in the Ashanti region where atrazine was 0.05 mg/kg which is within the EU-MRL of 0.1 mg/kg. However, minute concentrations of other organochlorines (endrin- 0.007 mg/kg; heptachlor- 0.023 mg/kg; alpha-endosulfan- 0.013 mg/kg) were found in maize samples from Brong Ahafo, Eastern, Central and Upper west regions. Though endrin and alpha-endosulfan were below the EU-MRL of 0.01 mg/kg and 0.10 mg/kg respectively, heptachlor was slightly above the EU-MRL of 0.01 mg/kg. The estimated doses for all these other organochlorines pesticides do not pose direct hazard to human health because their estimated dose values were lower than toxic thresholds and reference doses. However, due to the unsafe application practices by applicators, there exists a potential risk for systemic and carcinogenic health effects by these chemicals in the study area. (au)

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)

1995-08-01

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 14 C-compound pesticide residues. Refs, figs and tabs

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

Energy Technology Data Exchange (ETDEWEB)

NONE

1995-08-01

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 {sup 14}C-compound pesticide residues.

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

Directory of Open Access Journals (Sweden)

Nurul Karim

2012-09-01

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

Contribution to the food products' analysis: A research and evaluation on the hemolytic effect of some pesticides used in Lebanon.

Science.gov (United States)

Al-Alam, Josephine; Millet, Maurice; Chbani, Asma; Fajloun, Ziad

2015-01-01

Pesticides are a real concern for the society as their use has become critical, leading sometimes to their accumulation as residues in fruits and vegetables. After examining the pesticides sold in Northern Lebanon, this study is focused on the analysis and identification of pesticides residues in fruits and vegetables that are harvested in this region and treated with the locally sold pesticides. Results show: first, (i) a use of Zineb by the name of another pesticide Micronized Sulfur to avoid prosecution; (ii) a significant presence of Metalaxyl in lemons and oranges; (iii) a significant presence of Trifluralin in strawberries; and (iv) a significant presence of Zineb in lemons and tomatoes. Second, with the use of hemolytic tests on human blood results show: (i) a critical concentration and a significant hemolytic effect of some pesticides used in Lebanon; and (ii) an absence of hemolytic effect in the collected fractions of the different analyzed fruit extracts containing pesticides. Finally, this work is the first step for pesticides' analysis in vegetables and fruits in Lebanon, initiating a wider analytical study in order to control and examine the use of pesticides which, according to our results, could have an adverse effect on human health over a long term.

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

Science.gov (United States)

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

2011-11-01

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

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

International Nuclear Information System (INIS)

Luo Yuzhou; Zhang Minghua

2009-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-12-15

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

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

Science.gov (United States)

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

2013-05-01

Public concern in Vietnam is increasing with respect to pesticide pollution of the environment and of drinking water resources. While established monitoring programs in the Mekong Delta (MD) focus on the analysis of organochlorines and some organophosphates, the environmental concentrations of more recently used pesticides such as carbamates, pyrethroides, and triazoles are not monitored. In the present study, household level pesticide use and management was therefore surveyed and combined with a one year environmental monitoring program of thirteen relevant pesticides (buprofezin, butachlor, cypermethrin, α-endosulfan, β-endosulfan, endosulfan-sulfate, fenobucarb, fipronil, isoprothiolane, pretilachlor, profenofos, propanil, and propiconazole) in surface water, soil, and sediment samples. The surveys showed that household level pesticide management remains suboptimal in the Mekong Delta. As a consequence, a wide range of pesticide residues were present in water, soil, and sediments throughout the monitoring period. Maximum concentrations recorded were up to 11.24 μg l(-1) in water for isoprothiolane and up to 521 μg kg(-1) dm in sediment for buprofezin. Annual average concentrations ranged up to 3.34 μg l(-1) in water and up to 135 μg kg(-1) dm in sediment, both for isoprothiolane. Occurrence of pesticides in the environment throughout the year and co-occurrence of several pesticides in the samples indicate a considerable chronic exposure of biota and humans to pesticides. This has a high relevance in the delta as water for drinking is often extracted from canals and rivers by rural households (GSO, 2005, and own surveys). The treatment used by the households for preparing surface water prior to consumption (flocculation followed by boiling) is insufficient for the removal of the studied pesticides and boiling can actually increase the concentration of non-volatile pollutants. Copyright © 2012 Elsevier B.V. All rights reserved.

Pesticide Instrumental Analysis

International Nuclear Information System (INIS)

Samir, E.; Fonseca, E.; Baldyga, N.; Acosta, A.; Gonzalez, F.; Felicita, F.; Tomasso, M.; Esquivel, D.; Parada, A.; Enriquez, P.; Amilibia, M.

2012-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2005-01-01

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

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

International Nuclear Information System (INIS)

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

2005-01-01

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

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

Science.gov (United States)

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

2005-10-01

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

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

Science.gov (United States)

Luo, Yuzhou; Zhang, Minghua

2009-12-01

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

Long-term persistence of various 14C-labeled pesticides in soils

International Nuclear Information System (INIS)

Jablonowski, Nicolai D.; Linden, Andreas; Köppchen, Stephan; Thiele, Björn; Hofmann, Diana; Mittelstaedt, Werner; Pütz, Thomas; Burauel, Peter

2012-01-01

The fate of the 14 C-labeled herbicides ethidimuron (ETD), methabenzthiazuron (MBT), and the fungicide anilazine (ANI) in soils was evaluated after long-term aging (9–17 years) in field based lysimeters subject to crop rotation. Analysis of residual 14 C activity in the soils revealed 19% (ETD soil; 0–10 cm depth), 35% (MBT soil; 0–30), and 43% (ANI soil; 0–30) of the total initially applied. Accelerated solvent extraction yielded 90% (ETD soil), 26% (MBT soil), and 41% (ANI soil) of residual pesticide 14 C activity in the samples. LC-MS/MS analysis revealed the parent compounds ETD and MBT, accounting for 3% and 2% of applied active ingredient in the soil layer, as well as dihydroxy-anilazine as the primary ANI metabolite. The results for ETD and MBT were matching with values obtained from samples of a 12 year old field plot experiment. The data demonstrate the long-term persistence of these pesticides in soils based on outdoor trials. - Highlights: ► The environmental persistence of three 14 C-labeled pesticides in soils is presented. ► Extract analysis revealed the pesticides and metabolites after 9–17 years of aging. ► Pesticide residues may represent a long-term soil burden. ► The bioaccessibility and/or bioavailability of long-term aged pesticide residues remain unknown. - Residual fractions of the pesticides ethidimuron, methabenzthiazuron, and metabolites of anilazine are highly persistent in soils and remain extractable after long-term environmental aging.

PHYSICOCHEMICAL CHARACTERISTICS, PESTICIDE RESIDUE AND AFLATOXIN CONTAMINATION OF COLD PRESSED PUMPKIN SEED (Cucurbita pepo L. OILS FROM CENTRAL ANATOLIA REGION OF TURKEY

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FATMA NUR ARSLAN

2017-06-01

Full Text Available In this study, physicochemical characteristics, pesticide residues and aflatoxin contaminations of cold pressed pumpkin seed (Cucurbita pepo L. oils cultivated in four different central Anatolia regions of Turkey, were investigated. Lab-scale screw press machine was used to produce cold pressed pumpkin seed oils and the oil contents were found between 42.8%−47.4% for naked seeds. The physicochemical characteristic (refractive index, viscosity, color value, triglyceride profile analysis, peroxide value, iodine value, free fatty acid, saponification number, unsaponified matter, specific extinction values at 232 and 270 nm of cold pressed oils were determined by using different analytical techniques. The results showed that there was a non-significant difference between cold pressed pumpkin seed oils from different regions, in terms of physicochemical characteristics. The contents of pesticide residue and aflatoxin B1, B2, G1 and G2 contamination were determined by using validated UHPLC-MS/MS method. The chlorpyrifos pesticide residue was detected under the limit value declared by official authorities for the quality assessment of edible oils. Aflatoxins weren’t detected in any of studied pumpkin seed oils. Therefore, in food industry the positive effect of screw-pressing application could be useful for preservation of bioactive compounds during edible oil production and also enhancing of their functional properties.

Pesticide exposure - Indian scene

International Nuclear Information System (INIS)

Gupta, P.K.

2004-01-01

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

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

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Isioma Tongo

2015-01-01

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

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

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Faustin Vidogbéna

2015-10-01

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

Practical tracer investigations of pesticide residues in agricultural ecosystem

International Nuclear Information System (INIS)

Fuehr, F.

1984-01-01

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 14 C-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.)

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

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

2016-11-01

Residues of 14 pesticides were determined in 150 cowpea samples collected in five southern Chinese provinces in 2013 and 2014.70% samples were detected one or more residues. 61.3% samples were illegal mainly because of detection of unauthorized pesticides. 14.0% samples contained more than three pesticides. Deterministic and probabilistic methods were used to assess the chronic and acute risk of pesticides in cowpea to eight subgroups of people. Deterministic assessment showed that the estimated short-term intakes (ESTIs) of carbofuran were 1199.4%-2621.9% of the acute reference doses (ARfD) while the rates were 985.9%-4114.7% using probabilistic assessment. Probabilistic assessment showed 4.2%-7.8% subjects may suffer from unacceptable acute risk from carbofuran contaminated cowpeas from the five provinces (especially children). But undue concern is not necessary, because all the estimations are based on conservative assumption. Copyright © 2016 Elsevier Inc. All rights reserved.

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

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

2016-05-01

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

Determination of Levels of Organochlorine, Organophosphorus, and Pyrethroid Pesticide Residues in Vegetables from Markets in Dar es Salaam by GC-MS

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John A. M. Mahugija

2017-01-01

Full Text Available This study investigated the levels of pesticides and metabolites in vegetables from major markets in Dar es Salaam city, Tanzania. Samples of fresh cabbage, spinach, and onions from the markets were analysed for pesticide residues. Extraction was performed using acetone followed by dichloromethane : cyclohexane mixture and the extracts were cleaned up using Florisil. The compounds were determined by gas chromatography-mass spectrometry (GC-MS. Pesticides and metabolites were detected in 72.2% of the samples. The detected pesticide residues and their highest mean concentrations were p,p′-DDT 4.00 × 10−3 mg/kg, p,p′-DDD 6.40 × 10−1 mg/kg, o,p′-DDD 1.00 × 10−2 mg/kg, α-endosulfan 6.00 × 10−1 mg/kg, β-endosulfan 2.10 × 10−1 mg/kg, chlorpyrifos 3.00 mg/kg, and cypermethrin 4.00 × 10−2 mg/kg. The most frequently detected compounds were p,p′-DDD and chlorpyrifos. The order of contamination was spinach > cabbage > onions. Generally, there were no significant variations in concentrations of pesticide residues among samples and sampling sites, which indicated similarities in contamination patterns. The concentrations of contaminants were above the maximum residue limits (MRLs in 33.3–50% of the samples. The findings indicated risks and concerns for public health.

Pesticide residue determination in surface waters by stir bar sorptive extraction and liquid chromatography/tandem mass spectrometry.

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Giordano, A; Fernández-Franzón, M; Ruiz, M J; Font, G; Picó, Y

2009-03-01

In this stir bar sorptive extraction (SBSE) method, 16 pesticides were extracted from surface water samples by sorption onto 1 mm polydimethylsiloxane layer coated on a 10-mm-length stir bar magnet. After liquid desorption of the analytes with 1 ml of methanol, the detection was performed on a liquid chromatography-tandem mass spectrometry with a triple quadrupole (QqQ) analyzer using selected reaction monitoring mode via electrospray ionization. Parameters affecting SBSE operation, including sample volume, salt addition, extraction time, stirring rate, and desorption conditions, have been evaluated. The optimized SBSE method required two 50 ml aliquots of surface water samples, one aliquot was added of 30% NaCl and stirred at 900 rpm during 1 h for testing five pesticides with log K(o/w) 3. The method was validated in spiked surface water samples at limits of quantifications (LOQs) and ten times the LOQs showing recoveries Albufera Lake and surrounding channels, showing that SBSE is a powerful tool for routine control analysis of pesticide residues in surface water.

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

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Sompon Wanwimolruk

2016-09-01

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

[High throuput analysis of organophosphorus pesticide residues and their metabolites in animal original foods by dual gas chromatography-dual pulse flame photometric detection].

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Yang, Lixin; Li, Heli; Miao, Hong; Zeng, Fangang; Li, Ruifeng; Chen, Huijing; Zhao, Yunfeng; Wu, Yongning

2011-10-01

A method was established for the quantitative determination of 54 organophosphorus pesticide residues and their metabolites in foods of animal origin by dual gas chromatography-dual pulse flame photometric detection. Homogenized samples were extracted with acetone and methylene chloride, and cleaned-up by gel permeation chromatography (GPC). The response of each analyte showed a good linearity with a correlation coefficient not less than 0. 99. The recovery experiments were performed by a blank sample spiked at low, medium and high fortification levels. The recoveries for beef, mutton, pork, chicken were in the range of 50. 5% -128. 1% with the relative standard deviations (n = 6) of 1. 1% -25. 5%, which demonstrated the good precision and accuracy of the present method. The limits of detection for the analytes were in the range of 0. 001 -0. 170 mg/kg, and the limits of quantification were in the range of 0. 002 -0. 455 mg/kg. Animal food samples collected from markets such as meat, liver and kidney were analyzed, and the residues of dichlorovos and disulfoton-sulfoxide were found in the some samples. The established method is sensitive and selective enough to detect organophosphorus pesticide residues in animal foods.

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

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

2015-01-01

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

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)

Chai, Mee Kin; Tan, Guan Huat

2008-01-01

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)

Evaluation of various soaking agents as a novel tool for pesticide residues mitigation from cauliflower (Brassica oleracea var. botrytis).

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Abdullah; Randhawa, Muhammad Atif; Asghar, Ali; Pasha, Imran; Usman, Rabia; Shamoon, Muhammad; Bhatti, Muhammad Arslan; Irshad, Muhammad Asim; Ahmad, Naveed

2016-08-01

The increasing use of pesticides for boosting the yield of agricultural crops also impart toxic residues which ultimately extend to numerous physiological disorders upon consumption. The present study was designed as an effort to assess the reduction potential of various chemical solutions and to minimize the pesticide residues in cauliflower ( Brassica oleracea var. botrytis ). The samples were soaked in various solutions along with tap water to mitigate pesticide residues. Afterwards, the extracted supernatant was passed through column containing anhydrous sodium sulfate trailed by activated carbon for clean-up. Eluents were first evaporated and then completely dried under gentle stream of Nitrogen. Finally, the residues were determined using gas chromatography equipped with electron capture detector (GC-ECD). Results revealed the highest reduction of endosulfan, bifenthrin and cypermethrin residues with acetic acid (10 %) was 1.133 ± 0.007 (41 %), 0.870 ± 0.022 (60 %) and 0.403 ± 0.003 (75 %), respectively among the tested solutions. However, simple tap water treatment also resulted in 0.990 ± 0.02 (12 %), 1.323 ± 0.015 (14 %) and 1.274 ± 0.002 (21 %) elimination of endosulfan, bifenthrin and cypermethrin residues, respectively. Moreover, among various solutions, acetic acid depicted maximum reduction potential followed by citric acid, hydrogen peroxide, sodium chloride and sodium carbonate solutions. The percent reduction by various solutions ranged from 12 to 41, 14 to 60 and 21 to 75 % for the elimination of endosulfan, bifenthrin and cypermethrin residues, respectively.

Characterizing pesticide dissipation in food crops

DEFF Research Database (Denmark)

Fantke, Peter; Juraske, R.; Jolliet, O.

2013-01-01

Ingestion of residues via consumption of food crops is the predominant exposure route of the general population toward pesticides. However, pesticide dissipation in crops constitutes a main source of uncertainty in estimating residues in harvested crop parts and subsequent human exposure. Neverth......Ingestion of residues via consumption of food crops is the predominant exposure route of the general population toward pesticides. However, pesticide dissipation in crops constitutes a main source of uncertainty in estimating residues in harvested crop parts and subsequent human exposure....... Nevertheless, dissipation is a key mechanism in models assessing pesticide distribution in the cropenvironment and the magnitude of residues in harvest. We provide a consistent framework for characterizing pesticide dissipation in food crops for use in modeling approaches applied in health risk and impact...... degradation is dominating. We are currently testing the regression to predict degradation half-lives in crops. By providing mean degradation half-lives at 20°C for more than 300 pesticides, we reduce uncertainty and improve assumptions in current practice of health risk and impact assessments....

Rapid and sensitive suspension array for multiplex detection of organophosphorus pesticides and carbamate pesticides based on silica–hydrogel hybrid microbeads

International Nuclear Information System (INIS)

Wang, Xuan; Mu, Zhongde; Shangguan, Fengqi; Liu, Ran; Pu, Yuepu; Yin, Lihong

2014-01-01

Highlights: • Silica–hydrogel hybrid microbeads were used to develop suspension array. • The results in detecting pesticides agree well with those from LC–MS/MS. • The method showed the good capability for multiplex analysis of pesticides residues. - Abstract: A technique for multiplex detection of organophosphorus pesticides and carbamate pesticides has been developed using a suspension array based on silica–hydrogel hybrid microbeads (SHHMs). The main advantage of SHHMs, which consist of both silica and hydrogel materials, is that they not only could be distinguished by their characteristic reflection peak originating from the stop-band of the photonic crystal but also have low non-specific adsorption of proteins. Using fluorescent immunoassay, the LODs for fenitrothion, chlorpyrifos-methyl, fenthion, carbaryl and metolcarb were measured to be 0.02 ng/mL, 0.012 ng/mL, 0.04 ng/mL, 0.05 ng/mL and 0.1 ng/mL, respectively, all of which are much lower than the maximum residue limits, as reported in the European Union pesticides database. All the determination coefficients for these five pesticides were greater than 0.99, demonstrating excellent correlations. The suspension array was specific and had no significant cross-reactivity with other chemicals. The results for the detection of pesticide residues collected from agricultural samples using this method agree well with those from liquid chromatography–tandem mass spectrometry. Our results showed that this simple method is suitable for simultaneous detection of these five pesticides residues in fruits and vegetables

Rapid and sensitive suspension array for multiplex detection of organophosphorus pesticides and carbamate pesticides based on silica–hydrogel hybrid microbeads

Energy Technology Data Exchange (ETDEWEB)

Wang, Xuan [Key Laboratory of Environmental Medicine Engineering, Ministry of Education, School of Public Health, Southeast University, Nanjing, Jiangsu (China); Mu, Zhongde; Shangguan, Fengqi [State Key Laboratory of Bioelectronics, School of Biological Science and Medical Engineering, Southeast University, Nanjing, Jiangsu (China); Liu, Ran; Pu, Yuepu [Key Laboratory of Environmental Medicine Engineering, Ministry of Education, School of Public Health, Southeast University, Nanjing, Jiangsu (China); Yin, Lihong, E-mail: lhyin@seu.edu.cn [Key Laboratory of Environmental Medicine Engineering, Ministry of Education, School of Public Health, Southeast University, Nanjing, Jiangsu (China)

2014-05-01

Highlights: • Silica–hydrogel hybrid microbeads were used to develop suspension array. • The results in detecting pesticides agree well with those from LC–MS/MS. • The method showed the good capability for multiplex analysis of pesticides residues. - Abstract: A technique for multiplex detection of organophosphorus pesticides and carbamate pesticides has been developed using a suspension array based on silica–hydrogel hybrid microbeads (SHHMs). The main advantage of SHHMs, which consist of both silica and hydrogel materials, is that they not only could be distinguished by their characteristic reflection peak originating from the stop-band of the photonic crystal but also have low non-specific adsorption of proteins. Using fluorescent immunoassay, the LODs for fenitrothion, chlorpyrifos-methyl, fenthion, carbaryl and metolcarb were measured to be 0.02 ng/mL, 0.012 ng/mL, 0.04 ng/mL, 0.05 ng/mL and 0.1 ng/mL, respectively, all of which are much lower than the maximum residue limits, as reported in the European Union pesticides database. All the determination coefficients for these five pesticides were greater than 0.99, demonstrating excellent correlations. The suspension array was specific and had no significant cross-reactivity with other chemicals. The results for the detection of pesticide residues collected from agricultural samples using this method agree well with those from liquid chromatography–tandem mass spectrometry. Our results showed that this simple method is suitable for simultaneous detection of these five pesticides residues in fruits and vegetables.

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

Science.gov (United States)

Sapbamrer, Ratana; Hongsibsong, Surat

2014-07-01

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

Solid-phase extraction combined with high-performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry analysis of pesticides in water: method performance and application in a reconnaissance survey of residues in drinking water in Greater Cairo, Egypt.

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Potter, Thomas L; Mohamed, Mahmoud A; Ali, Hannah

2007-01-24

Monitoring of water resources for pesticide residues is often needed to ensure that pesticide use does not adversely impact the quality of public water supplies or the environment. In many rural areas and throughout much of the developing world, monitoring is often constrained by lack of testing facilities; thus, collection of samples and shipment to centralized laboratories for analysis is required. The portability, ease of use, and potential to enhance analyte stability make solid-phase extraction (SPE) an attractive technique for handling water samples prior to their shipment. We describe performance of an SPE method targeting a structurally diverse mixture of 25 current-use pesticides and two common degradates in samples of raw and filtered drinking water collected in Greater Cairo, Egypt. SPE was completed in a field laboratory in Egypt, and cartridges were shipped to the United States for elution and high-performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry analysis. Quantitative and reproducible recovery of 23 of 27 compounds (average = 96%; percent relative standard deviation = 21%) from matrix spikes (1 microg L-1 per component) prepared in the field and from deionized water fortified similarly in the analytical laboratory was obtained. Concurrent analysis of unspiked samples identified four parent compounds and one degradate in drinking water samples. No significant differences were observed between raw and filtered samples. Residue levels in all cases were below drinking water and "harm to aquatic-life" thresholds, indicating that human and ecological risks of pesticide contamination were relatively small; however, the study was limited in scale and scope. Further monitoring is needed to define spatial and temporal variation in residue concentrations. The study has demonstrated the feasibility of performing studies of this type using SPE to extract and preserve samples in the field. The approach should be broadly

Pesticide residues in cauliflower, eggplant, endive, lettuce, pepper, potato and wheat of the slovene origin found in 2009.

Science.gov (United States)

Baša-Česnik, Helena; Velikonja-Bolta, Spela; Gregorčič, Ana

2010-12-01

In the year 2009, 170 cauliflower, eggplant, endive, lettuce, pepper, potato and wheat samples from Slovene producers were analysed for pesticide residues. The samples were analysed for the presence of 214 different active compounds using three analytical methods. MRL exceedances have not been observed, which is better than the results obtained from the monitoring of pesticide residues in the products of plant origin in the European Union, Norway, Iceland and Liechtenstein for the years 2004 to 2006. We have observed that MRL exceedances in Slovenia have been reduced in recent times. We assume that the farmers have learned how to use PPP safely in accordance with good agricultural practice.

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)

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

2001-12-14

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.

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

Science.gov (United States)

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

2012-01-01

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

EVALUATION OF FARMERS APPRECIATION IN REDUCING PESTICIDE BY ORGANIC FARMING PRACTICE

Directory of Open Access Journals (Sweden)

Indraningsih Indraningsih

2016-10-01

Full Text Available Vegetables and dairy milk are important commodities in Pangalengan and Lembang, West Java. However, agrochemicals are used intensively and excessively in production system. Therefore, pesticide residues and contamination commonly occurred in agricultural products and environments. The study aimed to assess farmers’ attitudes on pesticide toxicity and reducing pesticide residues in animal and food crops products, and investigate the attitude changes of farmers on pesticide use. It was an on-farm research and farmers were directly involved in the study. The attitude change was analyzed on questionnaire and interview base for over 99 respondents in Pangalengan and Lembang between 2001 and 2003. Samples of soils, weeds, cabbages and milk were collected for pesticide residue analysis. Results showed that farmers did not aware on toxicity effects of pesticides in both animal and human health. There was misinterpretation among the farmers where pesticides were regarded as drugs rather than toxic compound to increase productivity. The organochlorines/OCs (lindane and heptachlor were common pesticide contaminants found in soils of 7.9- 11.4 ppb, but no organophospates (OPs were detected. Both OCs and OPs were also detected in soils of Lembang at a range of 11.53-65.63 ppb and 0.6-2.6 ppb, respectively. There were pesticide residues detected in weeds collected from Pangalengan (8.93 ppb lindane, 2.05 ppb heptachlor, and 33.27 ppb chlorpyriphos methyl/CPM and Lembang (6.45 ppb lindane, 2.65 ppb endosulfan, 6.85 ppb diazinon, and 0.5 ppb CPM. Only endosulfan with least residue level (0.1 ppb was detected in organic cabbages, whereas lindane was detected much higher (3.7 ppb in non-organic cabbages. Pesticide residues were not detected in milk of dairy cattle fed on by-products of organic cabbages, but lindane was still present in milk of dairy cattle fed on non-organic cabbages for 7 days subsequently. The present study indicates that the organic farming

Evaluation of abamectin, diazinon and chlorpyrifos pesticide residues in apple product of Mahabad region gardens: Iran in 2014.

Science.gov (United States)

Pirsaheb, Meghdad; Fattahi, Nazir; Rahimi, Rahim; Sharafi, Kiomars; Ghaffari, Hamid Reza

2017-09-15

The purpose of this study was to investigate abamectin, diazinon and chlorpyrifos in apple from the Mahabad of Iran. The influences of several parameters including shadow and sun, geographical directions and varieties of apples, whether they are golden or red type, was also taken into account on the residuals of the pesticides in the samples. The results indicated that sun considerably decreased the concentrations of diazinon and chlorpyrifos in samples exposed to it. Geographical directions are showed to be non-influential on diazinon while they are influential on chlorpyrifos ones. This can be attributed to pesticide spraying time and prevailing wind direction in Mahabad. The pesticides in golden and red varieties showed no significant relations. The apple samples from Mahabad did not contain any abamectin while they contained residuals of diazinon and chlorpyrifos. In some samples the diazinon and chlorpyrifos were above allowed limit according to World Health Organization (WHO) standard. Copyright © 2017 Elsevier Ltd. All rights reserved.

Earthworm tolerance to residual agricultural pesticide contamination

DEFF Research Database (Denmark)

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

2014-01-01

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...

Survey of Diazinon and Chlorpyrifos Pesticide Residues in the Corp of Apple (Red Delicious Variety of Miyandoab’s Springhouses by Using HPLC-PDA

Directory of Open Access Journals (Sweden)

H. Shahyan

2017-07-01

Full Text Available In this research to investigate the probable contamination of the apple tree to pesticides that is used by farmers in Miandoab, the residues of Diazinon and Chlorpirifos were investigated in this crop. First, the sampling is carried out by using the simple random sampling method and then, after Solid Phase Extraction (SPE through High-Performance Liquid Chromatography (HPLC, the residues of Diazinon and chlorpirifos were measured. So that, the pesticides residues in apples that were washed with skin, without skin and, in peeled apples were measured 0.08, 0.31, 0.68 ppm for Diazinon and 0.24, 0.54, 0.98 ppm for Chlorpirifos, respectively. Comparison of the statistical results with global standards reveals that the residues of Diazinon in Apples with the skin, and the residues of Chlorpirifos in three modes: Unwashed with the skin, washed with the skin and peeled is more than global standards (Diazinon 0.5 ppm and Chlorpirifos 0.01 ppm Therefore, it is required that the authorities and farmers of this region pay special attention to residues and the time of applying pesticides; thereby, they can prevent endangering health society.

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

Science.gov (United States)

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

2010-11-01

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

Improvement of the Raman detection system for pesticide residues on/in fruits and vegetables

Science.gov (United States)

Li, Yan; Peng, Yankun; Zhai, Chen; Chao, Kuanglin; Qin, Jianwei

2017-05-01

Pesticide residue is one of the major challenges to fruits safety, while the traditional detection methods of pesticide residue on fruits and vegetables can't afford the demand of rapid detection in actual production because of timeconsuming. Thus rapid identification and detection methods for pesticide residue are urgently needed at present. While most Raman detection systems in the market are spot detection systems, which limits the range of application. In the study, our lab develops a Raman detection system to achieve area-scan thorough the self-developed spot detection Raman system with a control software and two devices. In the system, the scanning area is composed of many scanning spots, which means every spot needs to be detected and more time will be taken than area-scan Raman system. But lower detection limit will be achieved in this method. And some detection device is needed towards fruits and vegetables in different shape. Two detection devices are developed to detect spherical fruits and leaf vegetables. During the detection, the device will make spherical fruit rotate along its axis of symmetry, and leaf vegetables will be pressed in the test surface smoothly. The detection probe will be set to keep a proper distance to the surface of fruits and vegetables. It should make sure the laser shins on the surface of spherical fruit vertically. And two software are used to detect spherical fruits and leaf vegetables will be integrated to one, which make the operator easier to switch. Accordingly two detection devices for spherical fruits and leaf vegetables will also be portable devices to make it easier to change. In the study, a new way is developed to achieve area-scan result by spot-scan Raman detection system.

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

International Nuclear Information System (INIS)

Meyer, D.E.

1999-01-01

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

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

Science.gov (United States)

Mekonen, Seblework; Ambelu, Argaw; Spanoghe, Pieter

2014-06-01

Samples of maize, teff, red pepper, and coffee (green bean and coffee bean with pulp) were collected from a local market in the Jimma Zone, Ethiopia. Samples were analyzed for the occurrence of cypermethrin, permethrin, deltamethrin, chlorpyrifos ethyl, DTT and its metabolites, and endosulfan (α, β). In the analytical procedure, the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction methodology with dispersive solid phase extraction clean up (d-SPE) technique was applied. Validation of the QuEChERS method was satisfactory. Recovery percentages of most pesticides were in the range of 70% to 120%, with good repeatability (%relative standard deviation coffee bean. Residues of DDT in coffee pulp significantly differed (p < 0.01) from other food items except for red pepper. The concentration of pesticides in the food items varied from 0.011 mg/kg to 1.115 mg/kg. All food items contained 1 or more pesticides. Two-thirds of the samples had residues below corresponding maximum residue limits, and the remaining one-third of samples were above the maximum residue limits. These results indicate the need for a good pesticide monitoring program to evaluate consumer risk for the Ethiopian people. © 2014 SETAC.

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

Science.gov (United States)

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

2014-07-01

The aim of this study was to investigate reported cases of honeybee death incidents with regard to the potential interrelation to the exposure to pesticides. Thus honeybee, bee pollen and honey samples from different areas of Greece were analyzed for the presence of pesticide residues. In this context an LC-ESI-MS/MS multiresidue method of total 115 analytes of different chemical classes such as neonicotinoids, organophosphates, triazoles, carbamates, dicarboximides and dinitroanilines in honeybee bodies, honey and bee pollen was developed and validated. The method presents good linearity over the ranges assayed with correlation coefficient values r(2)≥0.99, recoveries ranging for all matrices from 59 to 117% and precision (RSD%) values ranging from 4 to 27%. LOD and LOQ values ranged - for honeybees, honey and bee pollen - from 0.03 to 23.3 ng/g matrix weight and 0.1 up to 78 ng/g matrix weight, respectively. Therefore this method is sufficient to act as a monitoring tool for the determination of pesticide residues in cases of suspected honeybee poisoning incidents. From the analysis of the samples the presence of 14 active substances was observed in all matrices with concentrations ranging for honeybees from 0.3 to 81.5 ng/g, for bee pollen from 6.1 to 1273 ng/g and for honey one sample was positive to carbendazim at 1.6 ng/g. The latter confirmed the presence of such type of compounds in honeybee body and apicultural products. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2015-05-15

A quick and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method, using dynamic multiple reaction monitoring and a 1.8-μm particle size analytical column, was developed to determine 57 pesticides in tomato in a 13-min run. QuEChERS (quick, easy, cheap, effective, rugged, and safe) method for samples preparations and validations was carried out in compliance with EU SANCO guidelines. The method was applied to 58 tomato samples. More than 84% of the compounds investigated showed limits of detection equal to or lower than 5 mg kg(-1). A mild (50%) matrix effect was observed for 72%, 25%, and 3% of the pesticides studied, respectively. Eighty-one percent of the pesticides showed recoveries ranging between 70% and 120%. Twelve pesticides were detected in 35 samples, all below the maximum residue levels permitted in the Brazilian legislation; 15 samples exceeded the maximum residue levels established by the EU legislation for methamidophos; and 10 exceeded limits for acephate and four for bromuconazole. Copyright © 2014 Elsevier Ltd. All rights reserved.

Validation of pestice multi residue analysis method on cucumber

International Nuclear Information System (INIS)

2011-01-01

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 1 4C-carbaryl was also added on homogenized analytical portions to make use of 1 4C 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 1 4C- 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 1 4C-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, 1 4C-chloropyrifos was used to determine homogeneity of analytical portions taken from laboratory samples. Use of 1 4C 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

Pesticide residues in berries harvested from South-Eastern Poland (2009-2011).

Science.gov (United States)

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

2013-01-01

Poland is a leading grower/producer of berries in Europe that are either eaten raw or processed. As well as berries this includes fruit such as grapes, strawberries and other small fruits. Testing for the presence of active substances in Plant Protection Products, (PPP), in such fruit is however important, as part of measures taken to minimise human intake. To determine the incidence of pesticide residues in berries harvested from South-Eastern Poland in 2009-2011. . Chromatographic separation followed by analytical detection was performed on 250 samples of various test fruits using an accredited methodology: GC/ECD/NPD, together with spectrophotometric detection wherever necessary, according to PN-EN ISO/IEC 17025. As part of previous monitoring, 126 active substances were identified in 2009, 132 in 2010 and 153 in 2011; levels were compared to Maximum Residue Limits (MRLs). RESULTS;. Analyses showed that 46.4% of samples contained PPPs of which 4% exceeded the MRL. The most were found in raspberries, (58.8% of all tested), followed by 58.3% redcurrants, and gooseberries as well as 50% grapes. The most frequently found active substances of PPPs were pyrimethanil (15.6%), dithiocarbamates (12.4%), procymidone (8%), cyprodinil (5.6%) and difenoconazole (5.2%). The highest MRL exceedances were found in blackcurrants. Testing also revealed many examples of pesticides not recommended for the protection of specific crops: propiconazole in gooseberries, cyprodinil, flusilazole, iprodione, pyrimethanil in blackcurrants and folpet and captan in raspberries. Furthermore, active substances whose use in PPPs have been forbidden since 2008 were also detected, ie. endosulfan in blackcurrants and strawberries, fenitrothion in black and red currants as well as procymidone in raspberries, blackcurrants and strawberries. These data are consistent to those obtained from the whole of Poland and the European Union (EU). Most pesticides were present in raspberries, redcurrants

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

Science.gov (United States)

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

Screening of 485 Pesticide Residues in Fruits and Vegetables by Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry Based on TOF Accurate Mass Database and QTOF Spectrum Library.

Science.gov (United States)

Pang, Guo-Fang; Fan, Chun-Lin; Chang, Qiao-Ying; Li, Jian-Xun; Kang, Jian; Lu, Mei-Ling

2018-03-22

This paper uses the LC-quadrupole-time-of-flight MS technique to evaluate the behavioral characteristics of MSof 485 pesticides under different conditions and has developed an accurate mass database and spectra library. A high-throughput screening and confirmation method has been developed for the 485 pesticides in fruits and vegetables. Through the optimization of parameters such as accurate mass number, time of retention window, ionization forms, etc., the method has improved the accuracy of pesticide screening, thus avoiding the occurrence of false-positive and false-negative results. The method features a full scan of fragments, with 80% of pesticide qualitative points over 10, which helps increase pesticide qualitative accuracy. The abundant differences of fragment categories help realize the effective separation and qualitative identification of isomer pesticides. Four different fruits and vegetables-apples, grapes, celery, and tomatoes-were chosen to evaluate the efficiency of the method at three fortification levels of 5, 10, and 20 μg/kg, and satisfactory results were obtained. With this method, a national survey of pesticide residues was conducted between 2012 and 2015 for 12 551 samples of 146 different fruits and vegetables collected from 638 sampling points in 284 counties across 31 provincial capitals/cities directly under the central government, which provided scientific data backup for ensuring pesticide residue safety of the fruits and vegetables consumed daily by the public. Meanwhile, the big data statistical analysis of the new technique also further proves it to be of high speed, high throughput, high accuracy, high reliability, and high informatization.

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

OpenAIRE

Tentu. Nageswara Rao; A. Muralidhar Reddy; SNVS. Murthy; Prathipati Revathi; K. Suneel Kumar

2016-01-01

The silica nanoparticles prepared by stober’s mechanism by reaction of tetraethylorthosilicate (TEOS) with ammonia was tested for their adsorption capacity in the pre-concentration of residues of pesticides in water. The synthesized nanoparticles were characterized by Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM) and X-Ray Diffraction (XRD). The size of the silica nanoparticles were 50 to 250 nm. The solid phase extraction (SPE) cartridges were prepared by filling...

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

Science.gov (United States)

Raina-Fulton, Renata

2014-01-01

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

Development of multi-residue method for the determination of pesticides in cereal matrices by isotopic dilution associated to liquid chromatography coupled to tandem mass spectrometry after pressurized liquid extraction

International Nuclear Information System (INIS)

El Mrabet, Khadija

2008-01-01

Pesticides are nowadays considered as toxic for human health. The maximal residues levels authorized in water and foodstuff are more and more strict. Therefore, selective analytical techniques are necessary for their identification and their quantification. The aim of this thesis was to develop a multi-residue method for the determination of pesticides by isotopic dilution associated to liquid chromatography (LC) coupled with tandem mass spectrometry (MS"2) after pressurized liquid extraction. In a first step, an analysis method of phenyl-ureas and triazines in groundwater by isotopic dilution associated to LC/MS"2 after solid phase extraction has been developed. The method has been validated and evaluated by participating to an inter-laboratory study. Concerning cereals, an extraction method of pesticides associated to an analysis by LC/MS"2 has been developed for thirty-eight pesticides representative of twenty-six chemicals families and fourteen labeled compounds in wheat. The analysis has been carried out in reversed phase chromatography. Separation and detection conditions have been optimized. A global analytical protocol consisting of a pressurized liquid extraction step using acetonitrile at 100 deg. C and at 100 bars and followed by purification step of the resulting extract on a polymeric sorbent was developed. The developed method enables to extract thirty-eight pesticides and fourteen labeled compounds from wheat with recovery yield about 85% (RSD =4%, n=3). Moreover, the results show that the application of isotopic dilution can be complex. Although some improvements need to be added regarding experimentation of aged matrices or contaminated samples, the potential of the method has been demonstrated. (author) [fr

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

International Nuclear Information System (INIS)

Henry, L.; Kishimba, M.A.

2006-01-01

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

Citizen's Guide to Pest Control and Pesticide Safety

Science.gov (United States)

... contain pesticide residues. In addition, birds such as ducks and geese may absorb pesticide residues if they ... Where do you store your pesticides? A nationwide study conducted by EPA revealed that almost half (approximately ...

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

Science.gov (United States)

2010-03-03

... ENVIRONMENTAL PROTECTION AGENCY [EPA-HQ-OPP-2010-0111; FRL-8811-2] Notice of Filing of a Pesticide Petition for Residues of a Aspergillus flavus AF36 on Corn Food/Feed Commodities AGENCY: Environmental... for residues of the antifungal [[Page 9598

Classification of different kinds of pesticide residues on lettuce based on fluorescence spectra and WT-BCC-SVM algorithm

Science.gov (United States)

Zhou, Xin; Jun, Sun; Zhang, Bing; Jun, Wu

2017-07-01

In order to improve the reliability of the spectrum feature extracted by wavelet transform, a method combining wavelet transform (WT) with bacterial colony chemotaxis algorithm and support vector machine (BCC-SVM) algorithm (WT-BCC-SVM) was proposed in this paper. Besides, we aimed to identify different kinds of pesticide residues on lettuce leaves in a novel and rapid non-destructive way by using fluorescence spectra technology. The fluorescence spectral data of 150 lettuce leaf samples of five different kinds of pesticide residues on the surface of lettuce were obtained using Cary Eclipse fluorescence spectrometer. Standard normalized variable detrending (SNV detrending), Savitzky-Golay coupled with Standard normalized variable detrending (SG-SNV detrending) were used to preprocess the raw spectra, respectively. Bacterial colony chemotaxis combined with support vector machine (BCC-SVM) and support vector machine (SVM) classification models were established based on full spectra (FS) and wavelet transform characteristics (WTC), respectively. Moreover, WTC were selected by WT. The results showed that the accuracy of training set, calibration set and the prediction set of the best optimal classification model (SG-SNV detrending-WT-BCC-SVM) were 100%, 98% and 93.33%, respectively. In addition, the results indicated that it was feasible to use WT-BCC-SVM to establish diagnostic model of different kinds of pesticide residues on lettuce leaves.

Personal exposure to pesticide among workers engaged in pesticide container recycling operations.

Science.gov (United States)

Guidotti, T L; Yoshida, K; Clough, V

1994-12-01

Pesticide container handling operations in western Canada were examined to determine the exposure of workers to residual pesticide in sorting, metal-container crushing, metal-container shredding, plastic-container shredding, metal washing, and metal melting. Environmental exposure monitoring and biological monitoring were applied, including measurement of pesticide deposition density on outer clothing (test coveralls and other protective wear), deposition on fabric and gauze patches under the outer clothing, inhalation of airborne pesticide residues, dislodgement of pesticide residues by hand washing, and pre- and postexposure urinary excretion of pesticide (2,4-D). Exposure levels were highly variable; some variability was accounted for by work practices or lapses in protection. The highest levels of exposure were observed for metal washing, metal crushing, and metal shredding; sorting and plastic shredding were intermediate, and metal melting was associated with very little exposure. Urinary 2,4-D excretion, as an indicator of internal dose, correlated most closely with exposure by the inhalation route, and both were highest for metal washing and shredding. Deposition of pesticide on garments was highest for metal crushing. Melting of washed metal does not appear to present a significant hazard of exposure. Recommendations are proposed for the protection of workers emphasizing health and safety guidelines, worker education, personal hygiene, exposure and health monitoring, and record-keeping, and specific recommendations for each process. These recommendations apply to all pesticide container recycling operations except melting of washed metal containers.

Pesticides in the propolis at São Saulo State, Brazil - doi: 10.4025/actascianimsci.v34i4.15859 Pesticides in the propolis at São Saulo State, Brazil - doi: 10.4025/actascianimsci.v34i4.15859

Directory of Open Access Journals (Sweden)

Samir Moura Kadri

2012-10-01

Full Text Available The increasing demand for propolis has caused a raise in its production. However, an increasingly pesticide-dependent agriculture is a great concern with regard to bees, their produce and environmental contamination. Current analysis evaluates the presence of pesticides (organochlorines, organophosphates, pyrethroids, carbamates, herbicides, fungicides and acaricides in samples of propolis from the state of São Paulo, Brazil. Beekeepers from several localities in the state provided samples of propolis (50, which were collected, stored in non-toxic plastic bags and maintained in a freezer for analyses. Possible pesticide residues were examined by gas chromatography method but no pesticide residues were detected in the examined propolis samples. Propolis analyzed in the state of São Paulo did not show any pesticide contamination. The increasing demand for propolis has caused a raise in its production. However, an increasingly pesticide-dependent agriculture is a great concern with regard to bees, their produce and environmental contamination. Current analysis evaluates the presence of pesticides (organochlorines, organophosphates, pyrethroids, carbamates, herbicides, fungicides and acaricides in samples of propolis from the state of São Paulo, Brazil. Beekeepers from several localities in the state provided samples of propolis (50, which were collected, stored in non-toxic plastic bags and maintained in a freezer for analyses. Possible pesticide residues were examined by gas chromatography method but no pesticide residues were detected in the examined propolis samples. Propolis analyzed in the state of São Paulo did not show any pesticide contamination.

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

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Svetlana Hrouzková

2012-09-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2004-09-15

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

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

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Mobeen Akhtar

2014-01-01

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

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

Science.gov (United States)

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

2014-01-01

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

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)

Neves Bettencourt da Silva, Ricardo Jorge; Gomes Ferreira Crujo Camoes, Maria Filomena

2010-01-01

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2006-03-15

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

[Determination of 250 pesticide residues in vegetables using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry].

Science.gov (United States)

Zhang, Aizhi; Wang, Quanlin; Cao, Lili; Li, Yu; Shen, Hao; Shen, Jian; Zhang, Shufen; Man, Zhengyin

2016-02-01

A multiresidue analytical method for the determination of 250 pesticide residues in vegetables was developed by using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target compounds were extracted with acetonitrile containing 1% (v/v) acetic acid, purified by a mixed sorbent of MgSO4, primary secondary amine (PSA), graphitized carbon black (GCB) and C18, separated on a Waters ACQUITY™ UPLC BEH C18 column (100 mm x 2. 1 mm, 1.7 µm) and detected by UPLC-MS/MS. Anhydrous magnesium sulfate was used as a dewatering agent. The effects of the amounts of MgSO4, PSA, GCB and C18 added on the recoveries of 250 pesticides were investigated. The results showed that the purification effect was best when 300 mg MgSO4, 200 mg PSA, 10 mg GCB and 100 mg C18 in 2 mL of the extract were added. For the 250 pesticide residues, the limits of detection (LODs) of the method were from 0. 01 to 50. 00 g/kg. The recoveries obtained ranged from 60. 1% to 120% at three spiked levels in Chinese chives with the relative standard deviations between 3. 5% and 19. 5% using matrix matched external standard method. The results showed that the method is able to meet requirements of the multiresidue detection of the 250 pesticides in vegetable. The method has the advantages of rapidity, simplicity, high sensitivity and better purification effect. It is suitable for the rapid determination of the common pesticides in vegetables, and it provides a strong guarantee for the risk assessments of the quality and safety of vegetables.

Fate of iprovalicarb, indoxacarb, and boscalid residues in grapes and wine by GC-ITMS analysis.

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Angioni, Alberto; Dedola, Fabrizio; Garau, Vincenzo Luigi; Schirra, Mario; Caboni, Pierluigi

2011-06-22

The behavior in field and the transfer from grapes to wine during winemaking of iprovalicarb, indoxacarb, and boscalid was studied. The residue levels found in grapes were far below the MRLs set for grapes in EU, accounting at harvest time 0.81, 0.43, and 4.23 mg/kg for iprovalicarb, indoxacarb, and boscalid, respectively. The residue levels in the samples treated with boscalid may have residual problems (due to an accumulation effect) if repeated field treatments will be performed. Winemaking experiments showed a complete transfer of all pesticide from grapes to the must, while in wine the residues were low or negligible due to the adsorbing effect of lees and pomace. The clarification experiments showed a good removal of pesticide residues from the wine media, for all pesticides. The GC-ITMS method showed good performance with adequate recoveries ranging from 75 to 115%, and good method limits of quantitation (LOQs) and of determination (LODs) far below MRLs.

Effect of clarification process on the removal of pesticide residues in red wine and comparison with white wine.

Science.gov (United States)

Doulia, Danae S; Anagnos, Efstathios K; Liapis, Konstantinos S; Klimentzos, Demetrios A

2018-04-30

The aim of this study was to determine the potential of seven clarifying agents to remove pesticides in red wine. The presence of pesticides in wine consists a great problem for winemakers and therefore, results on pesticide removal by clarification are very useful for taking a decision on the appropriate adsorbent. The selection of an efficient adsorbent can be based on data correlating pesticide removal in red wine to pesticides' properties, given the great number and variety of pesticides used. So, this experimental work is focused on the collection of results with regard to pesticide removal by clarification using a great number of pesticides and fining agents. A Greek red wine, fortified with single solutions and mixtures of 23 or 9 pesticides was studied. The seven fining agents, used at two concentrations, were activated carbon, bentonite, polyvinylpolypyrrolidone (PVPP), gelatin, egg albumin, isinglass-fish glue, and casein. Pesticides were selected with a wide range of properties (octanol-water partition coefficient (log K ow ) 2.7-6.3 and water solubility 0.0002-142) and belong to 11 chemical groups. Solid phase extraction (SPE) followed by gas chromatography (GC) with electron capture detector (ECD) were performed to analyze pesticide residues of the clarified fortified wine. The correlation of the clarifying agents' effectiveness to pesticide's chemical structure and properties (log K ow , water solubility) was investigated. The antagonistic and/or synergistic effects, occurring among the pesticides in the mixtures, were calculated by indices. Pesticide removal effectiveness results of the red wine were compared to those obtained from a white wine under the same experimental conditions and discussed. The order of decreasing adsorbent effectiveness (mixture of 23 pesticides) was: activated carbon 40% > gelatin 23% > egg albumin 21% > PVPP 18% > casein 12% > bentonite 7%. Isinglass showed 12% removal at the highest permitted concentration. In the case of

Pesticide contamination of fruits and vegetables - A market basket survey from selected regions in Ghana

International Nuclear Information System (INIS)

Asiedu, Eric

2013-07-01

A market - basket survey was carried out with the aim of determining the concentration levels of pesticides, in lettuce, garden eggs, pineapple and mango from some selected regions in Ghana and to assess the potential health risk associated with exposure to the pesticide residues from fruits and vegetables consumption. A total of 192 fresh samples of fruits and vegetables were randomly collected under normal purchase conditions from 12 major towns and cities in the three regions of Ghana. The samples were extracted and analyzed for organophosphates, synthetic pyrethroids and organo chlorine pesticides. The percentage of samples of fruits and vegetables with pesticide residues in Lettuce, Garden eggs, Pineapple and Mango were 52%, 40%, 45%, 48% respectively and concentrations of pesticides did not vary significantly in samples as well as the sampling areas (p>0.05) even though there were differences in residual concentrations of pesticides . The differences in residual concentrations of pesticides could be due to different agricultural practices adopted by farmers and also accessibility of the pesticides. The average residue concentrations range from 0.01-0.45 mg/kg, 0.01-0.30 mg/kg and 0.01-1.27 mg/kg for organophosphates, synthetic pyrethroids and organo chlorine pesticides respectively. Lindane, chloropyrifos and cypermethrin were the most frequent organo chlorine, organophosphate and synthetic pyrethroid pesticides respectively while lettuce was the most frequently contaminated sample. Comparing the concentration levels of organo chlorine pesticides residue with the maximum residue limits (MRLs) adopted by the FAO/WHO Codex Alimentarious Commission shows that some of the fruits and vegetables sold on Ghanaian markets are contaminated even though the levels are generally low. Health risk analysis indicates that heptachlor in particular may be of public concern since its concentration levels exceeded the reference dose in all the four different types of samples

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

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Wanpen Mesomya

2012-11-01

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

Determination of pesticide residue in selected fruits and vegetable

International Nuclear Information System (INIS)

Tabbasum, R.; Aman, A.

2005-01-01

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)

2011 EPA Pesticide General Permit (PGP)

Data.gov (United States)

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

Compensation of matrix effects in gas chromatography-mass spectrometry analysis of pesticides using a combination of matrix matching and multiple isotopically labeled internal standards.

Science.gov (United States)

Tsuchiyama, Tomoyuki; Katsuhara, Miki; Nakajima, Masahiro

2017-11-17

In the multi-residue analysis of pesticides using GC-MS, the quantitative results are adversely affected by a phenomenon known as the matrix effect. Although the use of matrix-matched standards is considered to be one of the most practical solutions to this problem, complete removal of the matrix effect is difficult in complex food matrices owing to their inconsistency. As a result, residual matrix effects can introduce analytical errors. To compensate for residual matrix effects, we have developed a novel method that employs multiple isotopically labeled internal standards (ILIS). The matrix effects of ILIS and pesticides were evaluated in spiked matrix extracts of various agricultural commodities, and the obtained data were subjected to simple statistical analysis. Based on the similarities between the patterns of variation in the analytical response, a total of 32 isotopically labeled compounds were assigned to 338 pesticides as internal standards. It was found that by utilizing multiple ILIS, residual matrix effects could be effectively compensated. The developed method exhibited superior quantitative performance compared with the common single-internal-standard method. The proposed method is more feasible for regulatory purposes than that using only predetermined correction factors and is considered to be promising for practical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2009-06-01

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

Organochlorine pesticides and PCBs in air of southern Mexico (2002-2004)

Science.gov (United States)

Alegria, Henry A.; Wong, Fiona; Jantunen, Liisa M.; Bidleman, Terry F.; Figueroa, Miguel Salvador; Bouchot, Gerardo Gold; Moreno, Victor Ceja; Waliszewski, Stefan M.; Infanzon, Raul

Air samples were collected in southern Mexico in 2002-2004 to determine the extent of contamination with organochlorine (OC) pesticides and polychlorinated biphenyls (PCBs). The ΣDDTs ranged from 239 to 2360 pg m -3. Other prominent OC pesticides were endosulfans, toxaphene and lindane. Pesticides detected in lower concentrations include chlordanes, dieldrin, and heptachlor. Proportions of DDT compounds suggested fresh use of DDT in some locations and a mix of fresh and aged residues at others. Ratios of trans-chlordane/ cis-chlordane were consistent with fresh chlordane usage or emission of residues from former termiticide applications. The ΣPCBs was relatively low at all sites. Concentrations of OC pesticides measured with passive samplers agreed well with those measured using high-volume samplers. Air back trajectory analysis suggests a complex pattern of regional atmospheric transport.

Determination of pesticide residues in blood samples of villagers ...

African Journals Online (AJOL)

user

The spray-workers, during the activity of spraying crops, are ... cholinesterase inhibitor, it was recorded as a potent neurotoxic agent ... organic pesticide poisoning, of which around 73% were males and 27% ... analysis of blood will provide evidence of exposure of the body to ...... Occupational illness from cholinesterase ...

Retraction: Adyel et al. Health Risk Assessment of Pesticide Residues via Dietary Intake of Market Vegetables from Dhaka, Bangladesh. Foods 2013, 2, 64–75

Directory of Open Access Journals (Sweden)

Md. Shakhaoat Hossain

2013-07-01

Full Text Available The following article [1], doi: 10.3390/foods2010064, website: http://www.mdpi.com/2304-8158/2/1/64, has been retracted by the authors because of some major errors in broad field of pesticide residues identification and concentrations. During random cross check retention time of pesticides by HPLC did not match with the standards of detected pesticides. As a result concentration of all detected pesticides, maximum residue limits (MRLs and health risk assessments were changed. All these errors made the article [1] as a wrong one. All authors have confirmed that the reported results produced using quite inappropriate procedures. As first author herein, I take full responsibility for the retraction of our experiments and any other errors in its contents, and would like to offer my apologies on behalf of my co-authors to the readership of Foods for any inconveniences caused by this retraction.

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

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Yao Xin

2010-06-01

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

Serum organochlorine pesticide residues and risk of testicular germ cell carcinoma: a population-based case-control study.

Science.gov (United States)

Biggs, Mary L; Davis, Mark D; Eaton, David L; Weiss, Noel S; Barr, Dana B; Doody, David R; Fish, Sherianne; Needham, Larry L; Chen, Chu; Schwartz, Stephen M

2008-08-01

Testicular germ cell carcinoma (TGCC) is the most common malignancy among men ages 20 to 34 years. Although the pathogenesis of TGCC is poorly understood, suboptimal androgen levels or impaired androgen signaling may play a role. Some persistent organochlorine pesticides commonly found in human tissue possess antiandrogenic properties. We examined whether the risk of TGCC is associated with serum levels of 11 organochlorine pesticides, including p,p'-DDE, and whether the p,p'-DDE-TGCC association is modified by CAG or GGN repeat polymorphisms in the androgen receptor gene. We conducted a population-based case-control study among 18- to 44-year-old male residents of three Washington State counties. Cases (n = 246) were diagnosed during 1999 to 2003 with a first, primary TGCC. Controls (n = 630) were men of similar age with no history of TGCC from the same population identified through random-digit telephone dialing. Questionnaires elicited information on demographic, medical, and lifestyle factors. A blood specimen provided serum for gas chromatography-high-resolution mass spectrometry analysis of organochlorine pesticide residues and DNA for genotyping. We observed no clear patterns between TGCC risk and concentrations of any of the organochlorines measured, nor did we observe that the risk associated with p,p'-DDE was modified by androgen receptor CAG ( or =23 repeats) or GGN ( or =17 repeats) genotype. This study does not provide support for the hypothesis that adult exposure to organochlorine pesticides is associated with risk of TGCC. Due to uncertainty regarding how well organochlorine levels measured in adulthood reflect exposures during early life, further research is needed using exposure measurements collected in utero or during infancy.

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-01-15

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

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

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Rada Đurović

2007-01-01

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

Residues of Organochlorine Pesticides in Lake Mariut

International Nuclear Information System (INIS)

Saad, M.A.H.; Abu-Elamayem, M.M.; El-Sebae, A.B.; Sharaf, I.P.

1981-01-01

Lake Mariut, a brackish water lake adjoining the Mediterranean Coast of Egypt, has suffered much from intensive pollution in recent years due to the successive increase of human population and industry around it (Saad, 1980). The occurrence and distribution of organochlorine pesticides in the water of Lake Mariut during a period of one year were studied. This study represents an essential part of a pilot project on pollution of Lake Mariut supported by IAEA. The major organochlorine pesticides detected in the water of Lake Mariut were Lindane, p, p'-DDE, o,p'-DDT and p, p'-DDT. The mean concentrations of these pesticides were 2.091, 4.493, 0.009 and 0.134 ppb, respectively. The mean concentration of the calculated total DDT (Σ DDT) was 5.1 PPb

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

Directory of Open Access Journals (Sweden)

Aamand Jens

2011-01-01

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

Development of a fieldable rapid pesticide exposure analysis sensing system

Science.gov (United States)

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

2010-04-01

Despite the recent interest in organically grown foods, most agricultural crops use multiple pesticides to optimize yield. There are many persons whose health may be affected by the spraying; there is the active applicator and the passive neighbors. In between these extremes are the farm workers who pick the crops anywhere from days to weeks after application. How much pesticide residue are these workers exposed to during a workday and how much is transferred back to the residence? Despite the low vapor pressures, what is the true concentration of pesticides surrounding a person when pesticides adsorbed to particulate matter are included? What is the relationship between the concentration around an individual and the amount adsorbed/ingested? To answer these questions on a statistically significant scale in actual field conditions, a portable, fast, inexpensive measurement device is required. We present herein results obtained using Surface-Enhanced Raman Spectroscopy (SERS) that demonstrate the capability to detect issue of potential interferences will also be discussed.

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

Science.gov (United States)

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

2013-01-01

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

Development and validation of a multiresidue method for pesticide analysis in honey by UFLC-MS

Directory of Open Access Journals (Sweden)

Adriana M. Zamudio S.

2017-05-01

Full Text Available A method for the determination of pesticide residues in honey by ultra fast liquid chromatography coupled with mass spectrometry was developed. For this purpose, different variations of the QuECHERS method were performed: (i amount of sample, (ii type of salt to control pH, (iii buffer pH, and (iv different mixtures for cleaning-up. In addition, to demonstrate that the method is reliable, different validation parameters were studied: accuracy, limits of detection and quantification, linearity and selectivity. The results showed that by means of the changes introduced it was possible to get a more selective method that improves the accuracy of about 19 pesticides selected from the original method. It was found that the method is suitable for the analysis of 50 pesticides, out of 56. Furthermore, with the developed method recoveries between 70 and 120% and relative standard deviation below 15% were found.

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

Science.gov (United States)

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

2008-01-01

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

Farm workers' health and pesticide residue analysis of three farms in ...

African Journals Online (AJOL)

Cross sectional survey on the health status of the farm workers, engaged with pesticide use, at three agricultural farms; one in Debre zeit and two in Meki, Ethiopia, was conducted. A low prevalence of respiratory symptoms, chronic cough = 2.4%, in the farm workers as well as, chronic cough = 2.7%, in the control group was ...

40 CFR 180.564 - Indoxacarb; tolerances for residues.

Science.gov (United States)

2010-07-01

... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Indoxacarb; tolerances for residues...) PESTICIDE PROGRAMS TOLERANCES AND EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Specific Tolerances § 180.564 Indoxacarb; tolerances for residues. (a) General. Tolerances are established for residues of...

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

Energy Technology Data Exchange (ETDEWEB)

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

1997-09-01

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

Bee pollen as a bioindicator of environmental pesticide contamination.

Science.gov (United States)

de Oliveira, Renata Cabrera; Queiroz, Sonia Claudia do Nascimento; da Luz, Cynthia Fernandes Pinto; Porto, Rafael Silveira; Rath, Susanne

2016-11-01

Honeybees and bee products are potential bioindicators of the presence of contaminants in the environment, enabling monitoring of large areas due to the long distances travelled by bees. This work evaluates the use of bee pollen as a bioindicator of environmental contamination by pesticides. A GC-MS/MS analytical method for multiresidue determination of 26 different pesticides in pollen was developed and validated in accordance with the recommendations of the European Union SANCO guide. Environmental monitoring was conducted using the analysis of 145 pollen samples collected from ten beehives in the experimental apiary of Embrapa in Jaguariúna (São Paulo State, Brazil). Bioallethrin and pendimethalin were identified in four and eighteen samples, respectively, at concentrations below the LOQ of the method (25 ng g(-1)). Passive sampling with polyurethane foam discs was used as a control, and no pesticides were found. The detection of pesticide residues in seven samples (33%) from commercial apiaries in Ribeirão Preto (São Paulo State) confirmed the efficiency of the analytical method and the need for environmental monitoring for the presence of pesticide residues. The results demonstrated the potential of bee pollen as a bioindicator of environmental contamination by pesticides. Copyright © 2016 Elsevier Ltd. All rights reserved.

Determination of some selected pesticide residues in apple juice by solid-phase microextraction coupled to gas chromatography – mass spectrometry

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Andrea Hercegová

2011-01-01

Full Text Available The performance of solid phase microextraction (SPME for enrichment of pesticides from apple juice was investigated. Samples were diluted with water, extracted by solid-phase microextraction and analysed by gas chromatography using mass-spectrometry detector (MSD in selected ion monitoring mode (SIM. The method was tested for the following pesticides used mostly in fruit culturing at Slovakia: tebuthylazine, fenitrothion, chlorpyrifos, myclobutanil, cyprodinil, phosalone, pyrimethanil, tebuconazole, kresoxim-methyl, methidathion, penconazole. All pesticides were extracted with polydimethylsiloxane fibre 100 μm thickness. The linear concentration range of application was 0.05 μg dm−3–10 μg dm−3. The method described provides detectabilities complying with the maximum residue levels (MRLs set by regulatory organizations for pesticides in apple juice matrices. The solvent – free SPME procedure was found to be quicker and more cost effective then the solvent extraction methods commonly used.

77 FR 74003 - Pesticides; Draft Guidance for Pesticide Registrants on Antimicrobial Pesticide Products With...

Science.gov (United States)

2012-12-12

... Insecticide, Fungicide, and Rodenticide Act (FIFRA) or are required to register pesticides. The following list... remediation, on nonporous and porous surfaces, for residual activity, for mold prevention, and in heating...

In-hive Pesticide Exposome: Assessing risks to migratory honey bees from in-hive pesticide contamination in the Eastern United States

Science.gov (United States)

Traynor, Kirsten S.; Pettis, Jeffery S.; Tarpy, David R.; Mullin, Christopher A.; Frazier, James L.; Frazier, Maryann; Vanengelsdorp, Dennis

2016-09-01

This study measured part of the in-hive pesticide exposome by analyzing residues from live in-hive bees, stored pollen, and wax in migratory colonies over time and compared exposure to colony health. We summarized the pesticide burden using three different additive methods: (1) the hazard quotient (HQ), an estimate of pesticide exposure risk, (2) the total number of pesticide residues, and (3) the number of relevant residues. Despite being simplistic, these models attempt to summarize potential risk from multiple contaminations in real-world contexts. Colonies performing pollination services were subject to increased pesticide exposure compared to honey-production and holding yards. We found clear links between an increase in the total number of products in wax and colony mortality. In particular, we found that fungicides with particular modes of action increased disproportionally in wax within colonies that died. The occurrence of queen events, a significant risk factor for colony health and productivity, was positively associated with all three proxies of pesticide exposure. While our exposome summation models do not fully capture the complexities of pesticide exposure, they nonetheless help elucidate their risks to colony health. Implementing and improving such models can help identify potential pesticide risks, permitting preventative actions to improve pollinator health.

[Surface-enhanced Raman spectroscopy analysis of thiabendazole pesticide].

Science.gov (United States)

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

2015-02-01

Surface-enhanced Raman spectroscopy (SERS) technique was used to analyze the Raman peaks of thiabendazole pesticides in the present paper. Surface enhanced substrates of silver nanoparticle were made based on microwave technology. Raman signals of thiabendazole were collected by laser Micro-Raman spectrometer with 514. 5 and 785 nm excitation wavelengths, respectively. The Raman peaks at different excitation wavelengths were analyzed and compared. The Raman peaks 782 and 1 012 at 785 nm excitation wavelength were stronger, which were C--H out-of-plane vibrations. While 1284, 1450 and 1592 cm(-1) at 514.5 nm excitation wavelength were stronger, which were vng and C==N stretching. The study results showed that the intensity of Raman peak and Raman shift at different excitation wavelengths were different And strong Raman signals were observed at 782, 1012, 1284, 1450 and 1592 cm(-1) at 514.5 and 785 nm excitation wavelengths. These characteristic vibrational modes are characteristic Raman peaks of carbendazim pesticide. The results can provide basis for the rapid screening of pesticide residue in agricultural products and food based on Raman spectrum.

Studies on organochlorine pesticide residues in human breast milk of primparae mothers from selected areas in the Greater Accra Region

International Nuclear Information System (INIS)

Osei Tutu, A.

2009-06-01

A study was conducted to determine the types and levels of organochlorine pesticide residuals in the human milk samples of 42 nursing mothers from Ada and Accra. The milk samples were analyzed for 14 different organochlorine pesticides residue (Aldrin, Dieldrin, p,p'-DDT, p,p'-DDE, Endrin, Endrin Aldehyde, Endrin Ketone, Endosulphan sulfate,' Alpha Endosulphan, Gamma-HCH, Delta-HCH, Gamma Chlordane, Heptachlor and Methoxychlor) using Gas chromatography with electron capture detector. The mean concentrations for the organochlorine pesticide residues detected in the human milk samples from Accra are; Gamma-HCH (4.207µg/kg fat), Delta-HCH (13.855µg/kg fat), Heptachlor (11.791µg/kg fat), Aldrin (2.962µg/kg fat), Gamma- Chlordane (1.839µg/kg fat), Alpha-Endosulfan (4.740µg/kg fat), p,p'-DDE (23.367µg/kg fat), Dieldrin (2.407µg/kg fat), p,p'-DDT (3.085µg/kg fat), Endrin (7.669µg/kg fat), Endrin Aldehyde (7.769µg/kg fat), Endosulfan-Sulphate (99.052µg/kg fat), Endrin Ketone (63.846µg/kg fat), and Methoxychlor (20.116µg/kg fat). The mean concentrations of the various organochlorine pesticide residues detected in the human milk samples from Ada are; Gamma-HCH (5.438µg/kg fat), DeIta-HCH (6.728µg/kg fat), Heptachlor (0.682µg/kg fat), Aldrin (2.38µg/kg fat), Gamma- Chlordane (1.304µg/kg fat), Alpha-Endosulfan (2.588µg/kg fat), p,p'-DDE (24.165µg/kg fat), Dieldrin (2.222µg/kg fat), p,p'-DDT (3.468µg/kg fat), Endrin (6.339 µg/kg fat), Endosulfan-Sulphate (63.803)µg/kg fat), Endrin Ketone (11.167)µg/kg fat), and Methoxychlor (0.703µg/kg fat). The mean concentration of Endosulfan Sulfate was (99.052Iµ g/kg fat) was highest for the milk samples from Accra. Gamma chlordane recorded the least mean concentration (1.839 µg/kg fat) in the milk samples from Accra. The mean concentration of Endosulfan sulfate (63.803 µg/kg fat) was still the highest as compared to the other organochlorines analyzed for in the milk samples from Ada. Endrin Aldehyde was not

pH-dependence of pesticide adsorption by wheat-residue-derived black carbon.

Science.gov (United States)

Yang, Yaning; Chun, Yuan; Sheng, Guangyao; Huang, Minsheng

2004-08-03

The potential of black carbon as an adsorbent for pesticides in soils may be strongly influenced by the properties of the adsorbent and pesticides and by the environmental conditions. This study evaluated the effect of pH on the adsorption of diuron, bromoxynil, and ametryne by a wheat (Triticum aestivum L.) residue derived black carbon (WC) as compared to a commercial activated carbon (AC). The pH drift method indicated that WC had a point of zero charge of 4.2, much lower than that of 7.8 for AC. The density of oxygen-containing surface functional groups, measured by the Boehm titration, on WC was 5.4 times higher than that on AC, resulting in a pesticide adsorption by WC being 30-50% of that by AC, due to the blockage of WC surface by the waters associated with the functional groups. A small decrease (5.5%/unit pH) in diuron adsorption by WC with increase in pH resulted from increased deprotonation of surface functional groups at higher pH values. A much larger decrease (14-21%/unit pH) in bromoxynil adsorption by WC with increase in pH resulted from the deprotonation of both the adsorbate and surface functional groups of the adsorbent. The deprotonation reduced the adsorptive interaction between bromoxynil and the neutral carbon surface and increased the electrical repulsion between the negatively charged WC surface and bromoxynil anions. Deprotonation of ametryne with increase in pH over the low pH range increased its fraction of molecular form and thus adsorption on WC by 15%/unit pH. Further increase in pH resulted in a 20%/unit pH decrease in ametryne adsorption by WC due primarily to the development of a negative charge on the surface of WC. The pH-dependent adsorption of pesticides by black carbon may significantly influence their environmental fate in soils.

[Determination of eight pesticide residues in tea by liquid chromatography-tandem mass spectrometry and its uncertainty evaluation].

Science.gov (United States)

Hu, Beizhen; Cai, Haijiang; Song, Weihua

2012-09-01

A method was developed for the determination of eight pesticide residues (fipronil, imidacloprid, acetamiprid, buprofezin, triadimefon, triadimenol, profenofos, pyridaben) in tea by liquid chromatography-tandem mass spectrometry. The sample was extracted by accelerated solvent extraction with acetone-dichloromethane (1:1, v/v) as solvent, and the extract was then cleaned-up with a Carb/NH2 solid phase extraction (SPE) column. The separation was performed on a Hypersil Gold C, column (150 mm x 2. 1 mm, 5 microm) and with the gradient elution of acetonitrile and 0. 1% formic acid. The eight pesticides were determined in the modes of electrospray ionization (ESI) and multiple reaction monitoring (MRM). The analytes were quantified by matrix-matched internal standard method for imidacloprid and acetamiprid, by matrix-matched external standard method for the other pesticides. The calibration curves showed good linearity in 1 - 100 microg/L for fipronil, and in 5 -200 microg/L for the other pesticides. The limits of quantification (LOQs, S/N> 10) were 2 p.g/kg for fipronil and 10 microg/kg for the other pesticides. The average recoveries ranged from 75. 5% to 115.0% with the relative standard deviations of 2.7% - 7.7% at the spiked levels of 2, 5, 50 microg/kg for fipronil and 10, 50, 100 microg/kg for the other pesticides. The uncertainty evaluation for the results was carried out according to JJF 1059-1999 "Evaluation and Expression of Uncertainty in Measurement". Items constituting measurement uncertainty involved standard solution, weighing of sample, sample pre-treatment, and the measurement repeatability of the equipment were evaluated. The results showed that the measurement uncertainty is mainly due to sample pre-treatment, standard curves and measurement repeatability of the equipment. The method developed is suitable for the conformation and quantification of the pesticides in tea.

Quantitative Multiclass Pesticide Residue Analysis in Apple, Pear, and Grape by Modified QuEChERS and Liquid Chromatography Coupled to High-Resolution Mass Spectrometry.

Science.gov (United States)

Munaretto, Juliana S; Viera, Mariela de S; Martins, Manoel L; Adaime, Martha B; Zanella, Renato

2016-11-01

Most of the analytical methods currently applied in food control laboratories are focused on the determination of target compounds using LC coupled to tandem MS, which is an effective technique, but low-resolution MS is limited. Thus, a method for determination of pesticide multiresidues in fruits (pear, apple, and grape) using a modified quick, easy, cheap, effective, rugged, and safe method and LC coupled to quadrupole time-of-flight (Q-TOF) MS was developed and validated. The proposed method showed good linearity (r2 > 0.99) from 1 to 100 μg/L. Recoveries for blank samples spiked at 0.01, 0.04, and 0.10 mg/kg were between 66 and 122%, with RSDs apple, pear, and grape matrixes were 0.01 mg/kg for 112, 120, and 118 compounds, and 0.04 mg/kg for 22, 12, and 17 compounds, and average mass accuracy error was 3.2 ppm. LC with Q-TOF MS detection using protonated molecular ion and/or adducts and mass accuracy provided reliability for the method. The proposed method is effective for pesticide residue determination in apple, pear, and grape samples, proving that high-resolution MS using full scan mode can be a powerful and reliable technique for quantification purposes, being adequate for application in the surveillance of maximum residue limits set by different legislations.

[Exposure pathways to pesticides in schoolchildren in the Province of Talca, Chile].

Science.gov (United States)

Muñoz-Quezada, María Teresa; Lucero, Boris; Iglesias, Verónica; Muñoz, María Pía

2014-01-01

To describe pesticide concentrations in distinct environmental matrices at two time points (low and high seasons in local agricultural production) and to estimate the association between the presence of pesticide residues in matrices and the use of pesticides in the home with the sociodemographic variables of schoolchildren in the Province of Talca, Chile. A cross-sectional study was conducted in 190 schoolchildren. Families were surveyed about their children's vegetable consumption in school and at home, the use of pesticides in the home, and other sociodemographic variables. Additionally, we measured pesticide residues in vegetables and water consumed by the schoolchildren and in the soil of 14 schools. At both time points, the vegetable matrix had the highest pesticide concentration, both in urban and rural schoolchildren. The most common pesticide residues in vegetables were chlorpyrifos, diphenylamine, pyrimethanil, and thiabendazole. In the home, pyrethroid and organophosphate pesticides were mainly used in summer. Dangerous pesticide residues such as azinphos methyl and dimethoate were found in vegetables consumed by the children in schools and households, and organochlorines were found in the soil in some schools. Pesticide exposure should be limited and the health effects related to pesticide exposure should be assessed in the school population. Copyright © 2013 SESPAS. Published by Elsevier Espana. All rights reserved.

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

Science.gov (United States)

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

2014-01-01

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

Contamination of Dining Tables with Pesticides in Kibirigwi Irrigation Scheme

International Nuclear Information System (INIS)

Kimani, V.W; McDermont, J.J

1999-01-01

Kibirigwi irrigation scheme is a small holder area in Central Kenya, where the main activity is production of horticultural crops. Pesticides are widely misused. This study investigated the extent of house hold pesticide exposure in 40 randomly selected farms in JUly-August, 1995. Exposure measures collected included pesticide levels on dining table swabs. Fifty coytton clothes measuring 30 cm *30cm were prepared in the laboratory by soaking overnight in methanol. In each of the selected homesteads, the table used for meals was swabbed with the piece of cloth. In the laboratory, the residues chemicals extracted from these swabs using conventional residual analysis procedures and the extracts were analysed by gas liquid chromatography. Information on which pesticide (s) were recently handled in the home and when, were also recorded. Cypermethrin (9/40), malathion (9/40), Diazinon (5/40), dimethoate (4/40), chloropyrifos (4/40) and fenitrothion (1/40) were detected in these samples. The range of individual organophosphate pesticides detected was 0.01-8.7ug/cm 2 of table area and for cypermethrin the range was 0.0024 ng-5.8 ng/cm 2 . It was concluded that farmers and their family members are likely to be contaminated with pesticides from tables either dermally or through contamination of food placed on such tables

A gas/liquid chromatographic-mass spectrometric method for the rapid screening of 250 pesticides in aqueous matrices

Energy Technology Data Exchange (ETDEWEB)

Chandramouli, B.; Harvan, D.; Brittain, S.; Hass, R. [Eno River Labs, LLC. Durham, NC (United States)

2004-09-15

Pesticide residues in food present a potentially serious and significant cause for concern. Many pesticides have been associated with significant health effects to the nervous and endocrine systems and some have been deemed carcinogenic. There are many well-established techniques for pesticide analysis. However, commercial pesticide methods have traditionally only been available for specific pesticide families, such as chlorinated pesticides or herbicides, and at detection limits ranging from 0.05 ppb to 1 ppm in aqueous matrices. Techniques that can quickly screen for the presence/absence of pesticide residues in food matrices are critical in ensuring the safety of food and water. This paper outlines a combined Gas Chromatographic-High Resolution Mass Spectrometric (GC-HRMS) and Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) screening assay for 250 pesticides that was developed for use in water, and soda samples at screening levels ranging from 0.1-5 ppb. The pesticides selected have been identified by the European Union as being of concern and the target of possible legislation. The list encompasses a variety of pesticide classes and compound groupings.

Risk assessment of mixtures of pesticides. Current approaches and future strategies

DEFF Research Database (Denmark)

Reffstrup, Trine Klein; Larsen, John Christian; Meyer, Otto A.

2010-01-01

The risk assessment of pesticide residues in food is based on toxicological evaluation of the single compounds and no internationally accepted procedure exists for evaluation of cumulative exposure to multiple residues of pesticides in crops, except for a few groups of pesticides sharing a group...... several approaches are available for the risk assessment of mixtures of pesticides. However, no single simple approach is available to judge upon potential interactions at the low doses that humans are exposed to from pesticide residues in food. In these cases, PBTK models could be useful as tools...... to assess combined tissue doses and to help predict potential interactions including thresholds for such effects. This would improve the quality of the risk assessment....

Pesticide use and application: An Indian scenario

International Nuclear Information System (INIS)

Abhilash, P.C.; Singh, Nandita

2009-01-01

Agricultural development continues to remain the most important objective of Indian planning and policy. In the process of development of agriculture, pesticides have become an important tool as a plant protection agent for boosting food production. Further, pesticides play a significant role by keeping many dreadful diseases. However, exposure to pesticides both occupationally and environmentally causes a range of human health problems. It has been observed that the pesticides exposures are increasingly linked to immune suppression, hormone disruption, diminished intelligence, reproductive abnormalities and cancer. Currently, India is the largest producer of pesticides in Asia and ranks twelfth in the world for the use of pesticides. A vast majority of the population in India is engaged in agriculture and is therefore exposed to the pesticides used in agriculture. Although Indian average consumption of pesticide is far lower than many other developed economies, the problem of pesticide residue is very high in India. Pesticide residue in several crops has also affected the export of agricultural commodities in the last few years. In this context, pesticide safety, regulation of pesticide use, proper application technologies, and integrated pest management are some of the key strategies for minimizing human exposure to pesticides. There is a dearth of studies related to these issues in India. Therefore, the thrust of this paper was to review the technology of application of pesticides in India and recommend future strategies for the rational use of pesticides and minimizing the problems related to health and environment.

Validation of Analysis Method of pesticides in fresh tomatoes by Gas Chromatography associated to a liquid scintillation counting

International Nuclear Information System (INIS)

Dhib, Ahlem

2011-01-01

Pesticides are nowadays considered as toxic for human health. The maximum residues levels (MRL) in foodstuff are more and more strict. Therefore, selective analytical techniques are necessary for their identification and their quantification. The aim of this study is to set up a multi residue method for the determination of pesticides in tomatoes by gas chromatography with μECD detector (GC/μECD) associated to liquid scintillation counting. A global analytical protocol consisting of a QuECHERS version of the extraction step followed by purification step of the resulting extract on a polymeric sorbent was set up. The 14 C-chloropyrifos used as an internal standard proved excellent to control the different steps needed for the sample preparation. The method optimized is specific, selective with a recovery averaged more than 70 pour cent, repetitive and reproducible. Although some others criteria need to be checked regarding validation before its use in routine analysis, the potential of the method has been demonstrated.

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

Science.gov (United States)

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

2007-04-01

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.

Green Aspects of Techniques for the Determination of Currently Used Pesticides in Environmental Samples

OpenAIRE

Maciej Tankiewicz; Jacek Namieśnik; Jolanta Stocka; Marek Biziuk

2011-01-01

Pesticides are among the most dangerous environmental pollutants because of their stability, mobility and long-term effects on living organisms. Their presence in the environment is a particular danger. It is therefore crucial to monitor pesticide residues using all available analytical methods. The analysis of environmental samples for the presence of pesticides is very difficult: the processes involved in sample preparation are labor-intensive and time-consuming. To date, it has been standa...

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

Science.gov (United States)

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

2009-04-10

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

Evaluation of supercritical fluid chromatography coupled to tandem mass spectrometry for pesticide residues in food.

Science.gov (United States)

Cutillas, Víctor; Galera, María Martínez; Rajski, Łukasz; Fernández-Alba, Amadeo R

2018-04-13

Supercritical fluid chromatography coupled to triple quadrupole mass spectrometry has been evaluated for pesticide residues in food. In order to check its advantages and limitations it was developed a method to identify and quantify 164 pesticides in three different matrices (tomato, orange and leek). A carbon dioxide gradient with methanol (containing 1 mM ammonium formate) was used allowing a flow rate of 1.5 mL/min that made the total run time of 12 min without any problem of overpressure. Addition of a post column flow 150 μL/min of Methanol with ammonium formate/formic acid was necessary to improve the ionization. The matrix effect study revealed that the percentages of pesticides with irrelevant matrix effect (suppression lower than 20%) was 99% in tomato, 87% in orange and 62% in leek, whereas significant suppression (higher than 50%) was not found in tomato and only 1% of the compounds in orange and 3% in leek.These results compare favorably with that typically obtained in LC-MS/MS. The absence of water in the mobile phase, also provided some important advantages regarding LC-MS/MS as (i) higher retention of polar compounds in the column, which elute with high sensitivity and good peak shape and (ii) a general increase of the sensitivity of the analysis, consequence of the high ionization and ion extraction efficiency. Pesticides evaluated were identified following the SANTE/11813/2017. At the spiking concentration of 5 μg/kg, 98% of the pesticides were identified in tomato, 98% in orange and 94% in leek, whereas for the concentration of 10 μg/kg all the compounds were identified in tomato and only spiromesifen was not identified in orange and leek. At the concentration of 20 μg/kg, spiromesifen was also identified in these two matrices. The linearity and reproducibility of the method were evaluated with results which guarantee high quality in the analytical measurements. Even though only 2 μL of final extract were injected, the

Residues, Sources and Potential Biological Risk of Organochlorine Pesticides in Surface Sediments of Qiandao Lake, China.

Science.gov (United States)

Yang, Huayun; Zhou, Shanshan; Li, Weidong; Liu, Qi; Tu, Yunjie

2015-10-01

Sediment samples were analyzed to comprehensively characterize the concentrations, distribution, possible sources and potential biological risk of organochlorine pesticides in Qiandao Lake, China. Concentrations of sumHCH and sumDDT in sediments ranged from 0.03 to 5.75 ng/g dry weight and not detected to 14.39 ng/g dry weight. The predominant β-HCH and the α-HCH/γ-HCH ratios indicated that the residues of HCHs were derived not only from historical technical HCH use but also from additional usage of lindane. Ratios of o,p'-DDT/p,p'-DDT and DDD/DDE suggested that both dicofol-type DDT and technical DDT applications may be present in most study areas. Additionally, based on two sediment quality guidelines, γ-HCH, o,p'-DDT and p,p'-DDT could be the main organochlorine pesticides species of ecotoxicological concern in Qiandao Lake.

Organophosphate Pesticide Residues in Okra and Brinjal Grown in Peri-Urban Environment of Big Cities of Punjab

International Nuclear Information System (INIS)

Randhawa, M.A.; Zaman, M.; Anjum, F.M.; Asghar, A.

2015-01-01

Peri urban farming system is main supplier of vegetables to urban population and organophosphate pesticides exposure due to consumption of okra and brinjal to urban population has been estimated in this study. Okra and brinjal samples (90 samples for each vegetable) were collected from peri-urban farming area of Faisalabad, Multan and Gujranwala and were analysed by GC-ECD for quantification of chlorpyrifos, profenophos and triazophos residues. Data were statistically analyzed to calculate, mean and standard deviation. Quantification of pesticides residues revealed that 85 (47.22 percentage) samples were contaminated and 15 (8.33 percentage of total samples and 17.64 percentage of contaminated) samples showed residues value higher than MRL'S. Out of 85 contaminated samples 27 (31.76 percentage) samples were contaminated with chlorpyrifos, 30 (35.29 percentage) samples with profenofos and 29 (34.11) were contaminated with triazophos. The mean concentration of chlorpyrifos in okra was 0.192 mg Kg-1 and brinjal 0.197 mg Kg-1. The mean concentration for profenofos in okra was 0.02 mg Kg-1 and brinjal 0.035 mg Kg-1. Similarly mean concentration for triazophos in okra was 0.009 mg Kg-1 and brinjal 0.01 mg Kg-1. Overall, 6.67 percentage samples of okra and 6.66 percentage samples of brinjal contaminated with chlorpyrifos exceeded EU MRL of 0.05 mg kg-1. Okra samples were found contaminated at frequency of 4.44 percentage and brinjal samples at frequency of 5.56 percentage with higher profenofos residues level than MRL of 0.05 mg kg-1. Approximately, 6.67 percentage samples of okra and 5.6 percentage samples of brinjal had profenofos residue level above MRL of 0.01 mg kg-1. This study may be helpful for building database regarding regional exposure of urban population and facilitate in estimation of possible risk to their health in our daily life. (author)

Multiresidue levels of pesticides in selected fruits in Ghana; a preliminary study in the Yilo and Lower Manya Krobo Districts of the Eastern Region of Ghana

International Nuclear Information System (INIS)

Krokroko, W.

2011-01-01

Locally produced fruits (mango, pineapple and banana) were sampled and purchased from farms and markets with the Yilo and Lower Manya Krobo districts and analyzed for pesticide residues by gas chromatography equipped with an Electron Capture Detector (GC-ECD). In all, 80 samples made up of 40 mango samples and 20 samples each of pineapples and bananas were extracted and analyzed for mainly organochlorine residues (γ-HCH, δ-HCH, aldrin, dieldein, heptachlor, γ-chlordane, endosulfan s, p, p'-DDE etc.) and synthetic pyrethroid residues (allethrin, bifenthrin, fenpropathrin, permethrin, cyfluthrin, etc.). Analysis indicates that about 88% of the mangoes sampled from the farms contained one or more of these pesticide residues. 75% and 65% of the pineapples and bananas respectively from farms and markets had one or more of the analyzed pesticide residues. The data revealed that about 6.2% of the fruit samples analyzed contained organochlorine pesticide residues of γ-HCH (0.013mg/kg and 0.038mg/kg respectively in mangoes and pineapples); δ-HCH [0.014mg/kg (mango) and 0.024mg/kg (pineapple)]; methoxychlor [0.027 mg/kg (mango) and 0.048mg/kg (pineapple)]. Synthetic pyrethoid residues of cyfluthrin [0.078mg/kg (mango) and 0.059 mg/kg (pineapple) and fenvalerate [0.025 mg/kg and 0.028 mg/kg respectively for mango and pineapple] were also found above their respective maximum residue limits (Table 4.8) whereas 78.2% of detected pesticide residues were below the MRLs. Nonetheless, the continuous consumption of these fruits with even the modest pesticide levels can result in accumulation that could result in deadly chronic effects. In assessing the consumers' perception of pesticide residues in fruits, about 69% of the respondents were aware of pesticide residues in fruits and the corresponding adverse effect on human health. Some have experienced pesticide poising after fruit consumption. Thus many wish pesticide usage in fruit and crop cultivation in general is curbed or

Influence of pesticide applications on degradation of the herbicide 14C - 2,4-D in different soils

International Nuclear Information System (INIS)

Marcondes, Marcilio Amaral

2001-01-01

Despite the importance of pesticide usage for the food production, its indiscriminate use may cause changes in the soil fertility, because pesticides influence soil microorganisms which are important for the biogeochemical cycles. The influence of applications of several pesticides, as recommended for cotton culture, was studied on the bioactivity of different soils (from Sao Paulo and Tatui, SP) by using radiometric techniques and a closed system for detection of bio mineralization of ''1 4 C-2,4-D ( 14 C-2,4-dichlorophenoxyacetic acid) and production of 14 C-volatile compounds. The 14 C-2,4-D dissipation under influence of other pesticide applications was also studied by determination of 14 C-extractable residues, 14 C-bound residues and qualitative and quantitative analysis of the 14 C-extractable residues by high pressure liquid chromatography (HPLC) and thin layer chromatography (TLC). 14 C-volatile compounds were never detected but increases and decreases of bio mineralization were detected in both soils after different treatments. The mixture of deltamethrin + methyl parathion increased significantly the bioactivity in both soils; nevertheless, monocrotophos did not have any influence. The applications of different pesticides have also influenced the 14 C-2,4-D dissipation, because the radiocarbon recovered as 14 C-extractable residues differed between the treated and untreated samples of both soils. On the other hand, the pesticide applications did not influence the production of 14 C-bound residues. This 14 C-residue was produced in larger amounts by the richest in organic matter soil (Sao Paulo). Although radiocarbon had been detected not only as 14 'C-2,4-D but also as a 14 C-metabolite, in both soils and treatments, results indicate that the ' 14 C-2,4-D dissipation varied in the two studied soils and was influenced by treatments with others pesticides. (author)

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

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Gómez-Almenar, M. C.

2015-06-01

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

Residues in food derived from animals

International Nuclear Information System (INIS)

Grossklaus, D.

1989-01-01

The first chapter presents a survey of fundamentals and methods of the detection and analysis of residues in food derived from animals, also referring to the resulting health hazards to man, and to the relevant legal provisions. The subsequent chapters have been written by experts of the Federal Health Office, each dealing with particular types of residues such as those of veterinary drugs, additives to animal feeds, pesticide residues, and with environmental pollutants and the contamination of animal products with radionuclides. (MG) With 35 figs., 61 tabs [de

Pesticide residue levels in green beans cultivated in Souss Masa valley (Morocco) after multiple applications of bifenthrin and λ-cyhalothrin.

Science.gov (United States)

Bouri, M; Salghi, R; Bazzi, Lh; Zarrouk, A; Rios, A; Zougagh, M

2012-09-01

Dissipation of bifenthrin and λ-cyhalothrin pyrethroid insecticides, under environmental conditions, was evaluated on green beans grown in experimental greenhouses (Souss Massa valley, Morocco). Pesticide residues were determined by gas chromatography with micro electron-capture detector (GC-μECD) after dichloromethane extraction and cleanup on florisil phase cartridges. In the case of field experiments, a random block scheme was employed. Each block contained 25 plants in a single row and tests were carried out in triplicates applying pesticides at the recommended doses by the manufacturers. Fruit samples were periodically taken until the end of the preharvest interval (p.i.). The results obtained showed that the p.i of bifenthrin in green bean were 4 days in the winter and 3.5 days in the spring, whereas that for λ-cyhalothrin 8 days was found in the winter and 7.5 days in the spring. Consequently, it is possible to consider the European Union maximum residue limit (EU MRL) values compatible with the proper agricultural practices used for growing green bean in the plastic greenhouse of Souss Massa valley in South Morocco. Bifenthrin had a degradation of first-order kinetics, whereas that of levels for λ-cyhalothrin residue can not be interpreted by the use of a first order model.

[Meta-analysis of association between organophosphorus pesticides and aplastic anemia].

Science.gov (United States)

Zhang, Ji; Yang, Tubao

2015-09-01

To evaluate the association between organophosphorus pesticides and aplastic anemia, and provide scientific evidence for the primary prevention of aplastic anemia. The published papers of case control studies on the association between organophosphorus pesticides and aplastic anemia from January 1990 to August 2014 were collected from Chinese BioMedical Literature Base (CBM), Chinese National Knowledge Infrastructure (CNKI), PubMed and EMBASE. The papers which met the inclusion criteria were evaluated. The pooled odds ratios (OR) and 95% confidence interval (CI) of organophosphorus pesticides were calculated with software Review Manager 5.0. Subgroup analysis were conducted for different population and different usage of organophosphorus pesticides. A total of 9 papers were selected, involving 5 833 subjects (1 404 cases and 4 429 controls). The results showed that organophosphorus pesticides could increase the risk of aplastic anemia (OR=1.97, 95% CI: 1.60-2.44) . Subgroup analysis showed that Asian (OR=2.01, 95% CI: 1.52-2.66) had higher risk of aplastic anemia than American or European (OR=1.93, 95% CI: 1.39-2.67) . Using pure organophosphorus pesticides (OR=2.15, 95% CI: 1.60-2.88) was more prone to cause aplastic anemia than using the mixture of organophosphorus pesticides (OR=1.82, 95% CI: 1.34-2.47). The analysis indicated that organophosphorus pesticides might be a risk factor for aplastic anemia. Reducing organophosphorus pesticides exposure in daily life and industrial or agricultural production could prevent the incidence of aplastic anemia.

Tracer work in pesticide research

International Nuclear Information System (INIS)

Gonzales, B.P.

1989-01-01

Innumerable studies on the large number of pesticides being used throughout the world led to some adverse findings on the properties and behavior of these chemicals and their degradation products in revelation to potential toxicity and environmental pollution. However, it is also a fact (difficult to accept as it may) that the use of pesticides as an indirect means of increasing food production cannot yet be dispensed with despite the potential dangers attributed to it. What can be done is to insure its judicious application which means minimizing its effectiveness in controlling pest infestations. To be able to do this it is necessary to know not only what pesticide is to be used against a given pest but also the fate of pesticide after application to a particular environment under prevailing conditions. Knowledge of the distribution and persistence of the parent compounds under metabolites will also help either, to confirm or to dispel the alleged dangers posed by them. Radiotracer methodology is particularly effective for this type of work because it permits highly sensitive analysis with minimum clean-up and permits one to determine even the bound residues which defies ordinary extraction procedures. Some studies made are studies on fate of pesticides in plant after foliar application to plant needs, uptake and translocation of systemic pesticides, fate of pesticides in soil, bioaccumulation of pesticide by aquatic organisms, etc. This particular study is on distribution of pesticide among the components of a rice/fish ecosystem. This project aims to generate data from experiments conducted in a model ecosystem using radiolabelled lindane and carbo-furan. In both cases, results show a decline in extractable species from the recommended dosage of pesticide application although they tend to imbibe a considerable amount of pesticide. It is hoped that depuration in additional experiments will bring useful results. (Auth.)

A mobile App for military operational entomology pesticide applications

Science.gov (United States)

Multiple field studies conducted for the Deployed War Fighter Protection (DWFP) research program have generated over 80 specific guidance points for innovative combinations of pesticide application equipment, pesticide formulations, and application techniques for aerosol and residual pesticide treat...

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

Science.gov (United States)

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

2014-09-01

The objective of this study was to validate (SANCO/12495/2011 and NTC-ISO/IEC 17025) multi-residue multi-class methods using QuEChERS sample preparation and GC-MS for the analysis of regulated pesticides in tomatoes (Solanum lycopersicum), tamarillos (Solanum betaceum) and goldenberries (Physalis peruviana). These Latin American products are representative and widely produced in Antioquia (Colombia). Sample preparation followed the UNE-EN 15662 method (150 mg MgSO4, 25mg primary secondary amines and 25mg of octadecylsiloxane for cleanup; graphitized carbon black was added for tomatoes). Extracts were injected using a programmed temperature-vaporizing injector. The residues were validated over a range from 0.02 mg/kg to 0.20 mg/kg, with 24 analytes validated in tomatoes, 33 in tamarillos and 28 in goldenberries. An initial risk assessment was enabled by monitoring 24 samples in the municipalities of El Peñol, Marinilla and San Vicente Ferrer. Risks were found for tomatoes, but no significant risks were found for tamarillos or goldenberries. Copyright © 2014 Elsevier Ltd. All rights reserved.

[Ecotoxicological study of chlorinated pesticides].

Science.gov (United States)

Rosival, L; Szokolay, A; Uhnák, J

1980-01-01

The authors describe a model for the ecotoxicological investigation of pesticide residues guided by the analysis of various links of the food chain and of human materials. It is pointed to the possibility of studying the dynamics of the exposure to human beings by analyzing gynaecological material (prenatal stage) and samples obtained at necropsy from human beings of varying age (different durations of exposure). The observations of the relative accumulation of hexachlorobenzene, beta-BHC and DDT in butter, human milk and human fat in a region with intensive cultivation revealed a considerble accumulation of hexachlorobenzene which reaches the level of DDT. The conclusion drawn from ecotoxicological studies indicates that a reduction of the tolerances of pesticide residues in raw materials for baby foods is imperative. The analyses of gynaecological material (202 samples of the available content of the uterus and 24 placental and embryonic specimens) permitted to evidence a significant difference between two regions and a specific relationship of the observed substances and their metabolites to the fat-dissolving power of the analyzed materials.

Nanomaterials-Based Optical Techniques for the Detection of Acetylcholinesterase and Pesticides

Directory of Open Access Journals (Sweden)

Ning Xia

2014-12-01

Full Text Available The large amount of pesticide residues in the environment is a threat to global health by inhibition of acetylcholinesterase (AChE. Biosensors for inhibition of AChE have been thus developed for the detection of pesticides. In line with the rapid development of nanotechnology, nanomaterials have attracted great attention and have been intensively studied in biological analysis due to their unique chemical, physical and size properties. The aim of this review is to provide insight into nanomaterial-based optical techniques for the determination of AChE and pesticides, including colorimetric and fluorescent assays and surface plasmon resonance.

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

Science.gov (United States)

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

Multiresidue analysis of 47 pesticides in cooked wheat flour and polished rice by liquid chromatography with tandem mass spectrometry.

Science.gov (United States)

Lee, Sung Jung; Park, Hyeong Jin; Kim, Wooseong; Jin, Jong Sung; Abd El-Aty, A M; Shim, Jae-Han; Shin, Sung Chul

2009-04-01

Liquid chromatography in conjunction with tandem mass spectrometry was used to directly quantify of 47 pesticide residues from cooked wheat flour and polished rice, which are the most widely consumed cereals in the Republic of Korea. The sample clean-up was carried out according to the method established by the Korea Food and Drug Administration. The mobile phase for liquid chromatography separation consisted of water and 5 mm methanolic ammonium formate. Tandem mass spectroscopy experiments were performed in electrospray ionization positive mode and the multiple reaction monitoring mode. The matrix effects estimated for the 47 pesticides had a mean value of 99% and ranged from 45 to 147%. High recoveries (70-140%) and relative standard deviations (flour and polished rice samples. Of the screened pesticide residues, only tricyclazole and fenobucarb were found in polished rice samples. However, no samples contained residues above the MRL established by the Korea Food and Drug Administration.

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

Directory of Open Access Journals (Sweden)

Marcos Zatti da Silva

2007-04-01

ão necessários para se compreender melhor o efeito desses agrotóxicos sobre o ácaro predador.This study was carried out to evaluate the residual toxicity of some pesticides used in citrus orchards, on Neoseiulus californicus (McGregor under laboratory conditions. The residual contact bioassay method was adopted. Citrus leaves of the variety "Pêra" were sprayed in a Potter tower. The products' residual toxicity was evaluated at two hours and 1, 3, 5, 7, 10, 14 and 21 days after treatment. Ten adult females of N. californicus were transferred to each arena together with an enough amount of Tetranychus urticae to feed the predator. Mortality evaluations were performed at 72 hours after transferring the predaceous mites to the arenas. The pesticides acrinathrin, deltamethrin, dinocap, sulphur, fenpropathrin, fenbutatin oxide and propargite did not cause significant mortalities to the adults of N. californicus. Abamectim, azocyclotin and cyhexatin caused mortalities of 29.8, 24.0 and 34.1%, respectively, for N. californicus adults exposed to two-hour pesticide residues. Dicofol, pyridaben and chlorfenapyr caused 100% of mortality to the predators exposed to the two-hour acaricide residues. Abamectin provoked significant mortalities for a period shorter than one day. Residues of azocyclotin, cyhexatin, dicofol, pyridaben and chlorfenapyr caused significant mortalities for periods of 1, 1, 10, 10 and 21 days, respectively. The results of this study provided basic information for choosing the adequate pesticides to be used in citrus orchards in which N. californicus is present, or in those the predator will be released. The results are also useful for the decision of the best releasing time for N. californicus in the field, after pesticide applications. Studies carried out in the field are still necessary to understand better the effect of these pesticides under the predaceous mite.

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

Science.gov (United States)

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

2016-10-26

One of the recent trends in Analytical Chemistry is the development of economic, quick and easy hyphenated methods to be used in a field that includes analytes of different classes and physicochemical properties. In this work a multi-residue method was developed for the simultaneous determination of 28 xenobiotics (polar and hydrophilic) using hydrophilic interaction liquid chromatography technique (HILIC) coupled with triple quadrupole mass spectrometry (LC-MS/MS) technology. The scope of the method includes plant growth regulators (chlormequat, daminozide, diquat, maleic hydrazide, mepiquat, paraquat), pesticides (cyromazine, the metabolite of the fungicide propineb PTU (propylenethiourea), amitrole), various multiclass antibiotics (tetracyclines, sulfonamides quinolones, kasugamycin and mycotoxins (aflatoxin B1, B2, fumonisin B1 and ochratoxin A). Isolation of the analytes from the matrix was achieved with a fast and effective technique. The validation of the multi-residue method was performed at the levels: 10 μg/kg and 100 μg/kg in the following representative substrates: fruits-vegetables (apples, apricots, lettuce and onions), cereals and pulses (flour and chickpeas), animal products (milk and meat) and cereal based baby foods. The method was validated taking into consideration EU guidelines and showed acceptable linearity (r ≥ 0.99), accuracy with recoveries between 70 and 120% and precision with RSD ≤ 20% for the majority of the analytes studied. For the analytes that presented accuracy and precision values outside the acceptable limits the method still is able to serve as a semi-quantitative method. The matrix effect, the limits of detection and quantification were also estimated and compared with the current EU MRLs (Maximum Residue Levels) and FAO/WHO MLs (Maximum Levels) or CXLs (Codex Maximum Residue Limits). The combined and expanded uncertainty of the method for each analyte per substrate, was also estimated. Copyright © 2016 Elsevier B

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

International Nuclear Information System (INIS)

Haron, S. H.; Ismail, B. S.

2015-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-09-25

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

Organochlorine pesticide contamination of ground water in the city of Hyderabad.

Science.gov (United States)

Shukla, Gangesh; Kumar, Anoop; Bhanti, Mayank; Joseph, P E; Taneja, Ajay

2006-02-01

Organochlorine pesticides are ubiquitous and persistent organic pollutants used widely throughout the world. Due to the extensive use in agriculture, organic environmental contaminants such as HCH, DDT along with other organochlorine pesticides are distributed globally by transport through air and water. The main aim of present study is to determine contamination levels of organochlorine pesticides in the ground water of Hyderabad City. Water samples were collected from 28 domestic well supplies of the city. For this study, random sampling technique was applied, all the samples were collected in high purity glass bottles and refrigerated at 4 degrees C until analysis. Solid Phase Extraction (SPE) is used for the extraction of organochlorine pesticide residues in water sample. The collected water samples were pre-filtered through a 0.45 microg glass fiber filter (Wattman GF/F) to remove particulate matter and were acidified with hydrochloric acid (6N) to pH 2.5. Methanol modifier (BDH, for pesticide residue analysis, 10 mL) was added to water sample for better extraction. SPE using pre-packed reversed phase octadecyl (C-18 bonded silica) contained in cartridges was used for sample preparation. Prior to the extraction, the C-18 bonded phase, which contains 500 mg of bonded phase, was washed with 20 mL methanol. The sample was mixed well and allowed to percolate through the cartridges with flow rate of 10-15 mL/min under vacuum. After sample extraction, suction continued for 15 min to dry the packing material and pesticides trapped in the C-18 bonded phases were eluted by passing 10 mL hexane and fraction was evaporated in a gentle steam of Nitrogen. In all samples pesticide residues were analyzed by GC (Chemito-8510) with Ni63 ECD detector. Helium was used as carrier gas and nitrogen was used as make up gas. The injection technique was split/split less. All the samples analyzed were found to be contaminated with four pesticides i.e. DDT, beta-Endosulfan, alpha

Assessment of herbicides and organochlorine pesticides contamination in agricultural soils using gas chromatography-mass spectrometry.

Science.gov (United States)

Wang, Wan-Hong; Wang, Shi-Cheng; Wang, Yan-Hong

2008-01-01

A rapid multi-residue method for the simultaneous analysis of 3 herbicides and 8 organochlorine pesticides (OCPs) in agricultural soils has been developed, using ultrasonic solvent extraction coupled with gas chromatography-mass spectrometry (GC-MS). The recoveries ranged from 81% to 117% with a relative standard deviation (R.S.D) lower than 15%. The limits of quantification (LOQs) ranged from 0.03 to 1.06 microg x kg(-1) dry weight for different pesticides studied. The proposed method has been applied to investigate the 11 pesticide residues in agricultural soils collected from Liaoning Province, northeast of China. 3 OCPs and 3 herbicides were identified. Acetochlor, atrazine, butachtor were measured in the relatively high level with values ranging from 0.53 to 203.18 microg x kg(-1), 0.14 to 21.20 microg x kg(-1), pesticides in this study was compared with the date of other countries reported and the corresponding limiting values used in Netherland, USA, Canada, Vietnam and Thailand. Among the herbicide residues, there was a significant relativity between soil utilizing types and their residue concentration. It seems that the monitoring action for soil contamination caused by commonly-used herbicides should be enhanced according to soil utilizing types, especially acetochlor in maize field.

Pesticide residues in sediments from the west coast of India

Digital Repository Service at National Institute of Oceanography (India)

Sarkar, A.; SenGupta, R.

An average of 55,000 t of pesticides (including or organochlorine compounds) are used every year in India for agricultural purposes. The cumulative effects of these pesticides on the coastal environment can be expected to be considerable...

Multivariate study of parameters in the determination of pesticide residues in apple by headspace solid phase microextraction coupled to gas chromatography-mass spectrometry using experimental factorial design.

Science.gov (United States)

Abdulra'uf, Lukman Bola; Tan, Guan Huat

2013-12-15

Solid-phase microextraction (SPME) is a solvent-less sample preparation method which combines sample preparation, isolation, concentration and enrichment into one step. In this study, multivariate strategy was used to determine the significance of the factors affecting the solid phase microextraction of pesticide residues (fenobucarb, diazinon, chlorothalonil and chlorpyrifos) using a randomised factorial design. The interactions and effects of temperature, time and salt addition on the efficiency of the extraction of the pesticide residues were evaluated using 2(3) factorial designs. The analytes were extracted with 100 μm PDMS fibres according to the factorial design matrix and desorbed into a gas chromatography-mass spectrometry detector. The developed method was applied for the analysis of apple samples and the limits of detection were between 0.01 and 0.2 μg kg(-)(1), which were lower than the MRLs for apples. The relative standard deviations (RSD) were between 0.1% and 13.37% with average recovery of 80-105%. The linearity ranges from 0.5-50 μg kg(-)(1) with correlation coefficient greater than 0.99. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

Science.gov (United States)

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

2014-07-01

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

Determination of pesticides in fruits and vegetables using acetonitrile extraction and GC/MS technique

International Nuclear Information System (INIS)

Hussain, Z.

2010-01-01

A selection of oranges, guava and spinach were purchased from the local markets of Lahore, Pakistan. Extraction of the samples was carried out using an acetonitrile/toluene extraction procedure to determine the residual concentration of pesticides which may have been used during seasonal growth. Gas chromatography/mass spectrometry (GC/MS) was used for quantitative and confirmatory analysis of GC-amenable pesticides. The data obtained was compared with that of a referenced pesticide by matching molecular weight to a library of known pesticides. For comparison the same non-sprayed fruits/vegetable were extracted as a control reference. Factors studied were retention time, elution time, relative abundance and molecular weight. The results showed that low molecular weight pesticides were eluted before the high molecular weight pesticides. Pesticides identified included crotoxyphos, fenoxycarb and methoxyfenozide. (author)

Transfer rates of 19 typical pesticides and the relationship with their physicochemical property.

Science.gov (United States)

Chen, Hongping; Pan, Meiling; Pan, Rong; Zhang, Minglu; Liu, Xin; Lu, Chengyin

2015-01-21

Determining the transfer rate of pesticides during tea brewing is important to identify the potential exposure risks from pesticide residues in tea. In this study, the transfer rates of 19 typical pesticides from tea to brewing were investigated using gas chromatography tandem mass and ultraperformance liquid chromatography tandem mass. The leaching rates of five pesticides (isocarbophos, triazophos, fenvalerate, buprofezin, and pyridaben) during tea brewing were first reported. The pesticides exhibited different transfer rates; however, this result was not related to residual concentrations and tea types. Pesticides with low octanol-water partition coefficients (Logkow) and high water solubility demonstrated high transfer rates. The transfer rates of pesticides with water solubility > 29 mg L(-1) (or 25% (or 2.48) were >65% (or <35%). This result indicates that water solubility at approximately 20 mg L(-1) and LogKow at approximately 2.0 could be the demarcation lines of transfer rate. The results of this study can be used as a guide in the application of pesticides to tea trees and establishment of maximum residue limits of pesticides in tea to reduce pesticide exposure in humans.

Bioaccumulation and distribution of organochlorine residues across ...

African Journals Online (AJOL)

Eighteen organochlorine pesticide (OCP) residues were measured in the water, sediment, plankton, benthic invertebrates and fish in various sections of the Lagos Lagoon in 2014 to investigate their bioaccumulation and distribution in the food web. The analysis was done using gas chromatography with an electron capture ...

Determination of pesticides in coconut (Cocos nucifera Linn.) water and pulp using modified QuEChERS and LC-MS/MS.

Science.gov (United States)

Ferreira, Jordana Alves; Ferreira, Joana Maria Santos; Talamini, Viviane; Facco, Janice de Fátima; Rizzetti, Tiele Medianeira; Prestes, Osmar Damian; Adaime, Martha Bohrer; Zanella, Renato; Bottoli, Carla Beatriz Grespan

2016-12-15

The use of pesticides is directly linked to improvements in productivity and to the preservation of coconut palms. However pesticide analysis is necessary to determine whether pesticide residues in the food products containing coconut are within the maximum residue limits (MRLs), ensuring the quality of these products. This work aimed to develop a method for multiresidue determination of ten pesticides in coconut water and pulp using QuEChERS and LC-MS/MS. The method was effective in terms of selectivity, linearity, matrix effect, accuracy and precision, providing LOD of 3μgkg(-1), LOQ of 10μgkg(-1) and recoveries between 70 and 120% with RSD lower than 20%. The developed method was applied to 36 samples in which residues of carbendazim, carbofuran, cyproconazole and thiabendazole were found below the LOQ in coconut water and pulp. Copyright © 2016 Elsevier Ltd. All rights reserved.

[Determination of 51 carbamate pesticide residues in vegetables by liquid chromatography-tandem mass spectrometry based on optimization of QuEChERS sample preparation method].

Science.gov (United States)

Wang, Lianzhu; Zhou, Yu; Huang, Xiaoyan; Wang, Ruilong; Lin, Zixu; Chen, Yong; Wang, Dengfei; Lin, Dejuan; Xu, Dunming

2013-12-01

The raw extracts of six vegetables (tomato, green bean, shallot, broccoli, ginger and carrot) were analyzed using gas chromatography-mass spectrometry (GC-MS) in full scan mode combined with NIST library search to confirm main matrix compounds. The effects of cleanup and adsorption mechanisms of primary secondary amine (PSA) , octadecylsilane (C18) and PSA + C18 on co-extractives were studied by the weight of evaporation residue for extracts before and after cleanup. The suitability of the two versions of QuEChERS method for sample preparation was evaluated for the extraction of 51 carbamate pesticides in the six vegetables. One of the QuEChERS methods was the original un-buffered method published in 2003, and the other was AOAC Official Method 2007.01 using acetate buffer. As a result, the best effects were obtained from using the combination of C18 and PSA for extract cleanup in vegetables. The acetate-buffered version was suitable for the determination of all pesticides except dioxacarb. Un-buffered QuEChERS method gave satisfactory results for determining dioxacarb. Based on these results, the suitable QuEChERS sample preparation method and liquid chromatography-positive electrospray ionization-tandem mass spectrometry under the optimized conditions were applied to determine the 51 carbamate pesticide residues in six vegetables. The analytes were quantified by matrix-matched standard solution. The recoveries at three levels of 10, 20 and 100 microg/kg spiked in six vegetables ranged from 58.4% to 126% with the relative standard deviations of 3.3%-26%. The limits of quantification (LOQ, S/N > or = 10) were 0.2-10 microg/kg except that the LOQs of cartap and thiofanox were 50 microg/kg. The method is highly efficient, sensitive and suitable for monitoring the 51 carbamate pesticide residues in vegetables.