WorldWideScience
 
 
1

QA/QC in pesticide residue analysis  

International Nuclear Information System (INIS)

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

2002-01-01

2

[Quantitative analysis of organochlorine pesticide residues in Chinese drugs  

UK PubMed Central (United Kingdom)

This paper reports the GC determination of 20 organochlorine pesticides in Chinese drugs Flos Ionicerae and Moluodan etc by the present method of Japan for determinaing pesticide residues. The results suggest that except Folium Isatidis, Radix Codonopsis and Sanqi Pian all accord with the for provisions pesticide residues in Japanese foodstuffs.

Han G; Chen T; Yang J; Dai J; Xu R; Zhang Y; Okano J; Yui R; Nakajima H; Hamasaki T

1996-10-01

3

[Quantitative analysis of organochlorine pesticide residues in Chinese drugs].  

Science.gov (United States)

This paper reports the GC determination of 20 organochlorine pesticides in Chinese drugs Flos Ionicerae and Moluodan etc by the present method of Japan for determinaing pesticide residues. The results suggest that except Folium Isatidis, Radix Codonopsis and Sanqi Pian all accord with the for provisions pesticide residues in Japanese foodstuffs. PMID:9772626

Han, G; Chen, T; Yang, J; Dai, J; Xu, R; Zhang, Y; Okano, J; Yui, R; Nakajima, H; Hamasaki, T

1996-10-01

4

[Identification of unknown peaks in foods during residual pesticide analysis].  

UK PubMed Central (United Kingdom)

Four unknown peaks were detected in GC chromatograms during analysis of organophosphorus pesticide residues in foods. They were identified by using GC/MS as triethyl phosphate (TEP), tributyl phosphate (TBP), diphenyl 2-ethylhexyl phosphate (DPEHP) and N-ethyltoluenesulfoneamide (NETSA), which are used as plasticizers or flame retardants in food packaging. These chemical substances were detected in the range of tr. (below 0.01 microg/g) to 11 micro/g from 29 samples, and they were also detected in the packaging. It was supposed that they were transferred to the foods from the packaging. Furthermore, they were detected in some cereals and cereal products which contain fat and had been preserved for a long time.

Tomizawa S; Takano I; Kobayashi M; Tamura Y; Tateishi Y; Sakai N; Kitayama K; Nagayama T; Kamata K; Saito K

2004-10-01

5

Agricultural pesticide residues  

International Nuclear Information System (INIS)

The utilization of tracer techniques in the study of agricultural pesticide residues is reviewed under the following headings: lysimeter experiments, micro-ecosystems, translocation in soil, degradation of pesticides in soil, biological availability of soil-applied substances, bound residues in the soil, use of macro- and microautography, double and triple labelling, use of tracer labelling in animal experiments. (U.K.).

1984-01-01

6

Pesticide Residue Monitoring Program 1998  

Science.gov (United States)

Pesticide Program Residue Monitoring 1998: annual report summarizing the results of the Food and Drug Administration's (FDA) pesticide residue ... More results from www.fda.gov/food/foodborneillnesscontaminants/pesticides

7

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

UK PubMed Central (United Kingdom)

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

Omeroglu PY; Ambrus Á; Boyacioglu D; Majzik ES

2013-01-01

8

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

Science.gov (United States)

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

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

9

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

Directory of Open Access Journals (Sweden)

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%.

Rada ?urovi?; Jelena Milinovi?; Mirjana Markovi?; Dragan Markovi?

2007-01-01

10

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

Science.gov (United States)

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

11

[Identification of chemical detected in kiwi fruit during analysis for residual pesticide].  

UK PubMed Central (United Kingdom)

An unknown peak was detected in a GC chromatogram of many kiwi fruit extracts during analysis for pesticide residues. It was identified by GC/MS as diphenyl 2-ethylhexyl phosphate (DPEHP), used as a plasticizer and flame retardant. The concentration of DPEHP was investigated in 15 samples of kiwi fruit, and it was detected at between 0.02 and 0.14 microgram/g in 10 of the samples. It might be due to migration of DPEHP into the fruit from the printed portion of the polyethylene terephthalate (PET) package.

Tamura Y; Nagayama T; Takano I; Kobayashi M; Tomizawa S; Tateishi Y; Kimura N; Kitayama K; Saito K

2002-12-01

12

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)

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

1999-01-01

13

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

International Nuclear Information System (INIS)

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

2008-01-01

14

Pesticide Residue Monitoring Program 1995  

Science.gov (United States)

... Dimethoate, the next most frequently found residue, also has tolerances on a number of fruits. ... Dimethoate*, Nitrothal-isopropyl, XMC. ... More results from www.fda.gov/food/foodborneillnesscontaminants/pesticides

15

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

Science.gov (United States)

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

16

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

International Nuclear Information System (INIS)

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

2005-01-01

17

Pesticide residues in locally available cereals and vegetables  

International Nuclear Information System (INIS)

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

1976-01-01

18

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

Directory of Open Access Journals (Sweden)

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

Seema Tahir; Tahir Anwar; Shagufta Aziz; Rauf Ahmed Werer; Karam Ahad; Ashiq Mohammed; Erik K. Kirknel; Umar Khan Baloch

1999-01-01

19

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

International Nuclear Information System (INIS)

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

2008-08-15

20

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

Directory of Open Access Journals (Sweden)

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

Raquel Garcia; Maria João Cabrita; Ana Maria Costa Freitas

2011-01-01

 
 
 
 
21

Multi-residue analysis of pesticide residues in mangoes using solid-phase microextraction coupled to liquid chromatography and UV-Vis detection.  

UK PubMed Central (United Kingdom)

A sensitive and efficient solid-phase microextraction method, based on liquid chromatography and UV-Vis detection, was developed and validated as an alternative method for sample screening prior to LC-MS analysis. It enables the simultaneous determination of ten pesticides in mango fruits. The fiber used was polydimethylsiloxane while optimum SPME conditions employed have been developed and optimized in a previous work. The desorption process was performed in static mode, using acetonitrile as a solvent. The results indicate that the DI-SPME/HPLC/UV-Vis procedure resulted in good linear range, accuracy, precision and sensibility and is adequate for analyzing pesticide residues in mango fruits. The limits of detection (0.6-3.3??g/kg) and quantification (2.0-10.0??g/kg) were achieved with values lower than the maximum residue levels (MRLs) established by Brazilian legislation for all pesticides in this study. The average recovery rates obtained for each pesticide ranged from 71.6 to 104.3% at three fortification levels, with the relative standard deviation ranging from 4.3 to 18.6%. The proposed method was applied for the determination of the aforementioned compounds in commercial mango samples and residues of azoxystrobin, fenthion, permethrin, abamectin and bifenthrin were detected in the mango samples, although below the MRLs established by Brazilian legislation.

Filho AM; dos Santos FN; Pereira PA

2011-11-01

22

The 49th Annual Florida Pesticide Residue Workshop.  

UK PubMed Central (United Kingdom)

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

Turnipseed SB; Romano J

2013-01-01

23

Method for removing pesticide residue from tea  

UK PubMed Central (United Kingdom)

The invention discloses a method for removing pesticide residue from tea. The method adopts ozone water or ozone water-photocatalytic combined treatment to remove pesticide residue on picked tea. The treatment method can greatly lower or fully remove the pesticide residue on the tea, has easy, practical and easily controlled processing steps and low cost, is beneficial to environmental protection and hardly influences active substances in the tea.

MINNAN XIE; LI LIN; TIANGANG LUAN; WEI LIU; YINGQIAN HE

24

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

International Nuclear Information System (INIS)

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

2006-01-01

25

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

UK PubMed Central (United Kingdom)

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

Stefanelli P; Generali T; Barbini DA; Girolimetti S; Dommarco R

2013-01-01

26

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

Science.gov (United States)

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

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

2013-01-01

27

Analytical methods for pesticide residue determination in bee products.  

Science.gov (United States)

Monitoring pesticide residues in honey, wax, and bees helps to assess the potential risk of these products to consumer health and gives information on the pesticide treatments that have been used on the field crops surrounding the hives. The present review seeks to discuss the basic principles and recent developments in pesticide analysis in bee products and their application in monitoring programs. Consideration is given to extraction, cleanup, chromatographic separation, and detection techniques. PMID:12233867

Fernández, M; Picó, Y; Mañes, J

2002-09-01

28

Analytical methods for pesticide residue determination in bee products.  

UK PubMed Central (United Kingdom)

Monitoring pesticide residues in honey, wax, and bees helps to assess the potential risk of these products to consumer health and gives information on the pesticide treatments that have been used on the field crops surrounding the hives. The present review seeks to discuss the basic principles and recent developments in pesticide analysis in bee products and their application in monitoring programs. Consideration is given to extraction, cleanup, chromatographic separation, and detection techniques.

Fernández M; Picó Y; Mañes J

2002-09-01

29

Analysis of pesticide residues in rice using matrix solid-phase dispersion (MSPD)  

Scientific Electronic Library Online (English)

Full Text Available Abstract in portuguese Este trabalho apresenta um método multirresíduo de extração por dispersão da matriz em fase sólida (MSPD) para quantificação de dois inseticidas organofosforados (malation e paration metílico) e um organoclorado (beta-endosulfan) em arroz por cromatografia gasosa de alta resolução com detector por captura de elétrons. Experimentos foram realizados com adição de pesticidas na amostra, variando quantidades de amostra e de suporte, tipo de suporte e solvente de (more) eluição. A eficiência do método proposto foi demonstrada pelos valores médios de recuperação entre 75,5% e 116,0%, com valores de desvio padrão relativo entre 0,5% e 10,9%, obtidos nas análises de recuperação com amostras fortificadas nos níveis de 0,5 a 10,0 mg kg-1. Os limites de detecção foram de 20 a 105 pg para os pesticidas estudados. Arroz comercial foi analisado para a aplicação do método. Abstract in english This work reports a multi-residue extraction method based on matrix solid-phase dispersion (MSPD) and capillary gas chromatography - electron capture detection for quantification of two widely used organophosphorus insecticides (malathion and parathion-methyl) and an organochlorine pesticide (beta-endosulfan) in rice. A set of experiments was done with a spiked matrix with a standard mix, varying sample and solid phase amounts, solid phase and eluting solvent. Analyses of (more) fortified rice samples were performed at different levels (0.5-10.0 mg kg-1). Mean recoveries from three replicates ranged from 75.5% to 116.0%, with coefficients of variation from 0.5% to 10.9%. The limit of detection was in the range of 20 to 105 pg for the pesticides. Commercial rice was analyzed for method application.

Dórea, Haroldo S.; Lima Sobrinho, Ledjane

2004-10-01

30

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

Directory of Open Access Journals (Sweden)

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 (fenthion)and 0.05-25 ng/ml (bifenthrin).Relative standard deviation (RSD) values for triplicate measurements did not exceed 15%.

Rada ?urovi?; Jelena Milinovi?; Mirjana Markovi?; Dragan Markovi?

2007-01-01

31

Assessment of pesticide residues on selected vegetables of Pakistan  

International Nuclear Information System (INIS)

The present study was conducted to determine the pesticide residues on selected summer vegetables. Five vegetables were grown with three replicates in a split plot randomized complete block design. Pesticides were sprayed on vegetables thrice at regular intervals each after 15 days. At maturity the pesticides residues were extracted from edible and leaf portions using anhydrous sodium sulfate and ethyl acetate while adsorption chromatography technique was used for cleanup. The extracts were subjected to high performance liquid chromatography (HPLC) for separation and analysis of the compounds. Significant differences (p

2011-01-01

32

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

UK PubMed Central (United Kingdom)

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

Oellig C; Schwack W

2012-10-01

33

Pesticide Residue Monitoring Program 1996  

Science.gov (United States)

... Ofurace Omethoate* Ovex Oxadiazon Oxadixyl Oxamyl* Oxydemeton-methyl Oxyfluorfen Oxythioquinox Paclobutrazol Paraquat* Parathion ... More results from www.fda.gov/Food/FoodborneIllnessContaminants/Pesticides

34

[Characterizing the toxicity interaction of the binary mixture between DMSO and pesticide by the multi-effect residual analysis (MERA)].  

UK PubMed Central (United Kingdom)

Three groups of binary mixtures between dimethylsulfoxide (DMSO) and three widely used pesticides, dimethoate (DIM), dichlorvos (DIC), and metalaxyl (MET), were respectively constructed by using the direct equipartition ray design (EquRay). The luminescent inhibition toxicities of single chemical and binary mixtures to Vibrio qinghaiensis sp. -Q67 were determined by the microplate toxicity analysis (MTA). Selecting the concentration addition (CA) model as an additive reference, we developed a new multi-effect residual analysis (MERA) to quantitatively characterize the deviation of the observed toxicity from that predicted by the CA model, i. e. the degree of toxicity interaction. It was shown that the toxicity interactions between DMSO and pesticide were dominated by antagonism, and the highest antagonism distributed between -23% and -15%. The concentration ranges where antagonism existed and the degree of antagonism were influenced by the components in the mixture, the concentration ratios of the components, and the effect level. A comparison of the MERA with the conventional isobologram and the extended toxic unit summation revealed that the MERA characterizes the degree of toxicity interaction in the view of effect, with less limitation by different concentration ratios or effect levels. Therefore, the MERA can be used to evaluate the complex toxicity interactions taking place in binary mixtures.

Huo XC; Liu SS; Zhang J; Zhang J

2013-01-01

35

[Characterizing the toxicity interaction of the binary mixture between DMSO and pesticide by the multi-effect residual analysis (MERA)].  

Science.gov (United States)

Three groups of binary mixtures between dimethylsulfoxide (DMSO) and three widely used pesticides, dimethoate (DIM), dichlorvos (DIC), and metalaxyl (MET), were respectively constructed by using the direct equipartition ray design (EquRay). The luminescent inhibition toxicities of single chemical and binary mixtures to Vibrio qinghaiensis sp. -Q67 were determined by the microplate toxicity analysis (MTA). Selecting the concentration addition (CA) model as an additive reference, we developed a new multi-effect residual analysis (MERA) to quantitatively characterize the deviation of the observed toxicity from that predicted by the CA model, i. e. the degree of toxicity interaction. It was shown that the toxicity interactions between DMSO and pesticide were dominated by antagonism, and the highest antagonism distributed between -23% and -15%. The concentration ranges where antagonism existed and the degree of antagonism were influenced by the components in the mixture, the concentration ratios of the components, and the effect level. A comparison of the MERA with the conventional isobologram and the extended toxic unit summation revealed that the MERA characterizes the degree of toxicity interaction in the view of effect, with less limitation by different concentration ratios or effect levels. Therefore, the MERA can be used to evaluate the complex toxicity interactions taking place in binary mixtures. PMID:23487948

Huo, Xiang-Chen; Liu, Shu-Shen; Zhang, Jing; Zhang, Jin

2013-01-01

36

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

Scientific Electronic Library Online (English)

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

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

2003-04-01

37

Pesticide Residue Monitoring Program 2000  

Science.gov (United States)

... (2)Pesticide Analytical Manual Volume I (3rd Ed ... Vegetable oil, refined, 1, 100.0, 0.0, Spices & condiments & flavors, 8, 37.5, 0.0, ... Olives, 10, 100.0, 0.0 ... More results from www.fda.gov/Food/FoodborneIllnessContaminants/Pesticides

38

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

UK PubMed Central (United Kingdom)

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

Gómez-Ramos MM; Ferrer C; Malato O; Agüera A; Fernández-Alba AR

2013-04-01

39

Determination of pesticide residues in cannabis smoke.  

Science.gov (United States)

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

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

2013-05-12

40

Considerations on the Content of Pesticides Residues in Vegetables  

Directory of Open Access Journals (Sweden)

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

Florica Morar; Catalina-Cristina Bloj

2011-01-01

 
 
 
 
41

Combination of analyte protectants to overcome matrix effects in routine GC analysis of pesticide residues in food matrixes.  

UK PubMed Central (United Kingdom)

Analyte protectants were previously defined as compounds that strongly interact with active sites in the gas chromatographic (GC) system, thus decreasing degradation, adsorption, or both of coinjected analytes. In this study, we evaluated various combinations of promising analyte protectants for the volatility range of GC-amenable pesticides using GC/quadrupole mass spectrometry (MS) and 1-microL hot splitless injection for sample introduction. A mixture of ethylglycerol, gulonolactone, and sorbitol (at 10, 1, and 1 mg/mL, respectively, in the injected samples) was found to be the most effective in minimizing losses of susceptible analytes and significantly improving their peak shapes (due to reduction of peak tailing). When added to final sample extracts and matrix-free calibration standards alike, these analyte protectants induced a similar response enhancement in both instances, resulting in effective equalization of the matrix-induced response enhancement effect even after a large number of fruit and vegetable extract injections. As compared to matrix-matched standardization, the analyte protectant approach offers a more convenient solution to the problems associated with calibration in routine GC/MS analysis of pesticide residues and possibly other susceptible analyte types in diverse samples. Moreover, the use of analyte protectants also substantially reduced another adverse matrix-related effect caused by gradual build-up of nonvolatile matrix components in the GC system, thus improving ruggedness and, consequently, reducing need for frequent maintenance.

Mastovská K; Lehotay SJ; Anastassiades M

2005-12-01

42

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

UK PubMed Central (United Kingdom)

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

Park Ji-Yeon; Choi Jeong-Heui; Abd El-Aty AM; Kim BoMi; Oh Jae-Ho; Do Jung-Ah; Kwon KiSung; Shim Ki-Hoon; Choi Ok-Ja; Shin SungChul; Shim Jae-Han

2011-09-01

43

Análise de resíduos de pesticidas em tomates por cromatografia em camada delgada Analysis of residue pesticide in tomatoes by thin layer chromatography  

Directory of Open Access Journals (Sweden)

Full Text Available Pesticide residues are determined by thin layer chromatography (TLC) using the Hill reaction as a detection method. Tomatoes samples without pesticide were fortified with atrazine, diuron, chloroxuron and metribuzin, and were applyed in silica gel plates with the help of a microsyringe. The pesticides were elued with ethyl acetate. There was no need of cleaning up because no interference was noticed. After the revelation of the plates, the diameters of the spots were measure by using a rule. The range of the determined concentration for all the pesticides was from 0.1 to1.0 ng/muL. The results obtained through TLC can be used for semi-quantitative analysis.The results obtained were compared to gas and liquid chromatography, showing good agreement between both techniques.

Solange Leite Moraes; Maria Olímpia Oliveira Rezende; Lia Emi Nakagawa; Luiz Carlos Luchini

2002-01-01

44

Análise de resíduos de pesticidas em tomates por cromatografia em camada delgada/ Analysis of residue pesticide in tomatoes by thin layer chromatography  

Scientific Electronic Library Online (English)

Full Text Available Abstract in english Pesticide residues are determined by thin layer chromatography (TLC) using the Hill reaction as a detection method. Tomatoes samples without pesticide were fortified with atrazine, diuron, chloroxuron and metribuzin, and were applyed in silica gel plates with the help of a microsyringe. The pesticides were elued with ethyl acetate. There was no need of cleaning up because no interference was noticed. After the revelation of the plates, the diameters of the spots were meas (more) ure by using a rule. The range of the determined concentration for all the pesticides was from 0.1 to1.0 ng/muL. The results obtained through TLC can be used for semi-quantitative analysis.The results obtained were compared to gas and liquid chromatography, showing good agreement between both techniques.

Moraes, Solange Leite; Rezende, Maria Olímpia Oliveira; Nakagawa, Lia Emi; Luchini, Luiz Carlos

2002-05-01

45

Pesticides residue levels in selected fruits from some Ghanaian markets  

International Nuclear Information System (INIS)

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

2009-01-01

46

Pesticide residues survey in citrus fruits.  

Science.gov (United States)

The use of pesticides is widespread in citrus fruits production for pre- and post-harvest protection and many chemical substances may be applied in order to control undesirable moulds or insects. A survey was carried out to evaluate levels of pesticide residues in citrus fruits. Two multiresidue analytical methods were used to screen samples for more than 200 different fungicides, insecticides and acaricides. A total of 240 samples of citrus fruits including lemon, orange, mandarin, grapefruit, lime, pomelo and kumquat were taken in various markets in the Geneva area during the year 2003. Ninety-five percent of the 164 samples issued from classical agriculture contained pesticides and 38 different compounds have been identified. This high percentage of positive samples was mainly due to the presence of two post-harvest fungicides, imazalil and thiabendazole, detected in 70% and 36% of samples respectively. Only three samples exceeded the Swiss maximum residue limits (MRLs). Fifty-three samples sold with the written indication "without post-harvest treatment" were also controlled. Among theses samples, three exceeded the Swiss MRLs for penconazole or chlorpyrifos and 18 (34%) did not respect the written indication since we found large amounts of post-harvest fungicides. Finally, 23 samples coming from certified organic production were analysed. Among theses samples, three contained small amounts of pesticides and the others were pesticides free. PMID:16019813

Ortelli, Didier; Edder, Patrick; Corvi, Claude

2005-05-01

47

Pesticide residues survey in citrus fruits.  

UK PubMed Central (United Kingdom)

The use of pesticides is widespread in citrus fruits production for pre- and post-harvest protection and many chemical substances may be applied in order to control undesirable moulds or insects. A survey was carried out to evaluate levels of pesticide residues in citrus fruits. Two multiresidue analytical methods were used to screen samples for more than 200 different fungicides, insecticides and acaricides. A total of 240 samples of citrus fruits including lemon, orange, mandarin, grapefruit, lime, pomelo and kumquat were taken in various markets in the Geneva area during the year 2003. Ninety-five percent of the 164 samples issued from classical agriculture contained pesticides and 38 different compounds have been identified. This high percentage of positive samples was mainly due to the presence of two post-harvest fungicides, imazalil and thiabendazole, detected in 70% and 36% of samples respectively. Only three samples exceeded the Swiss maximum residue limits (MRLs). Fifty-three samples sold with the written indication "without post-harvest treatment" were also controlled. Among theses samples, three exceeded the Swiss MRLs for penconazole or chlorpyrifos and 18 (34%) did not respect the written indication since we found large amounts of post-harvest fungicides. Finally, 23 samples coming from certified organic production were analysed. Among theses samples, three contained small amounts of pesticides and the others were pesticides free.

Ortelli D; Edder P; Corvi C

2005-05-01

48

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

UK PubMed Central (United Kingdom)

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

Omeroglu PY; Ambrus A; Boyacioglu D

2013-01-01

49

Pesticide residue removal from vegetables by ozonation  

UK PubMed Central (United Kingdom)

A novel machine was developed to remove pesticide residues from vegetables using ozone. This domestic-scale vegetable cleaner consists of a closed cleaning chamber, an ozone generator, a water recirculation pump, and an oxidation–reduction potential (ORP) electrode. Two vegetables, Chinese white cabbage and green-stem bok choy, and three pesticides, permethrin (trans-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarboxylate), chlorfluazuron (1-[3,5-dichloro-4-(3-chloro-5-trifluoromethyl-2-pyridyloxy)phenyl]-3-(2,6-difluorobenzoyl) urea), and chlorothalonil (tetrachloroisophthalonitrile) were used in tests. Cleaning for 15min with pump recirculation removed 51% of chlorfluazuron and 53% of chlorothalonil. When the ozone production rate was 250mg/h, removal efficiencies were 60% for chlorfluazuron and 55% for chlorothalonil, increases of 2–9% over pump recirculation only. When the ozone production rate was 500mg/h, removal efficiencies were 75% for chlorfluazuron and 77% for chlorothalonil; increases of 24% over pump recirculation only. After the ozone treatment, all the pesticide residuals met the Standards for Pesticide Residue Limits in Foods.

Chen JY; Lin YJ; Kuo WC

2013-02-01

50

Clean up of pesticide residues by Gel- Permeation chromatography  

International Nuclear Information System (INIS)

Use of the semi-automatic gel chromatographic system, Type : KL-SX-3 ( GPC) was evaluated for pesticide residue analysis. The clean up procedure was found efficient for large column use (28 mm id. x 20 cm). Recoveries of linuron and pirimiphos-methyl were found 84.3 and 79.8 percent respectively. Fat and pesticide contents are clearly separable. About eighty percent of DDT (88.8%), 91.4% of carbaryl and 98% of carbofuran were recovered in 80-190 ml of cyclohexane-dichloromethane 1 : 1 eluent. In the small column more than 70% of pesticides come out in the initial fractions ( 0-30 ml) of eluent. From this study it is thus concluded that GPC (KL-SX-C) with large column is suitable to separate pesticides from fat and other co-extracts from grain samples, but small column technique is of limited use. (author)

2003-01-01

51

Pesticide residue analysis of fruit juices by LC-MS/MS direct injection. One year pilot survey.  

UK PubMed Central (United Kingdom)

For this work, thirteen types of fruit juices (orange, pineapple, peach, apple, multifruit, mango, strawberry, tomato, pear, mandarin, grape, banana and grapefruit) were selected to develop an analytical method for the analysis of 53 pesticides by direct injection in LC-MS/MS. The preparation of the samples was very simple: an aliquot of the juice was centrifuged and it was ten-times diluted prior to analysis, which allowed reducing considerably the time and cost of the analyses. Besides, dilution of the samples permits reducing the amount of matrix going into the system, and thus, decreasing the matrix effects, so common in this type of commodities, opening the possibility to perform quantification with solvent based standards. Validation of the method was carried out in accordance with EU guidelines. Calibration curves covering three orders of magnitude were performed, and they were linear over the concentration range studied for all the matrices (from 0.1 to 100 ?g L(-1)). Practical limits of quantification were in the low ?g L(-1) range, far below the maximum residue levels (MRLs) of the EU regulations, which do not set specific MRLs for juices, and in this cases of processed food, MRLs of the raw product are applied. Repeatability of the instrumental method was studied in all matrices, obtaining good intra- and inter-day relative standard deviations (RSDs). The proposed method was applied to 106 real fruit juice samples purchased in different local markets during a one-year survey in order to validate the suitability for routine analysis. 43% of the analysed samples gave positive results (higher than the practical limits of quantification).

Ferrer C; Martínez-Bueno MJ; Lozano A; Fernández-Alba AR

2011-02-01

52

Streamlined pretreatment and GC-FPD analysis of multi-pesticide residues in perennial Morinda roots: A tropical or subtropical plant.  

UK PubMed Central (United Kingdom)

In this study, a simple and rapid multi-pesticide residues analytical method has been developed and evaluated for simultaneous identification and quantification of 30 organophosphorus pesticides (OPPs) present at trace levels in perennial Morinda roots. Samples were firstly extracted and cleaned up with a streamlined method (modified QuEChERS), and then detected by gas chromatography with flame photometric detector (GC-FPD). For accurate quantification, representative matrix-matched calibration curves were applied to compensate matrix effects. Reasonable linearity was found in the concentration ranges of 0.04 and 1.28?gmL(-1), with correlation coefficients r better than 0.9921 (0.9921-0.9998). The limits of detection (LODs) were between 0.005 and 0.02?gmL(-1) for all investigated pesticides, while the limits of quantification (LOQs) were in the range of 0.01-0.04?gmL(-1), below the regulatory maximum residue limits (MRL) suggested. Acceptable quantitative recoveries of 75.01-118.89% (96.0% on average) were achieved with relative standard deviations (RSD) varying from 0.89% to 9.80% (5.39% on average) at three different concentration levels of 0.05, 0.1 and 1.0mgkg(-1). Out of all 40 batches of real samples, only fenitrothion was found in two samples, which was successfully confirmed by GC-MS. Based on these results, this analytical method has been proven to be fast, robust, accurate, selective, sensitive and easy to operate in the analysis of multiple pesticide residues in Morinda roots. Meanwhile, it also draws attention to the need of pesticide monitoring programs in local soils.

Liu H; Kong W; Qi Y; Gong B; Miao Q; Wei J; Yang M

2013-09-01

53

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

UK PubMed Central (United Kingdom)

Gas and liquid chromatography (GC and LC) coupled to mass spectrometry (MS) serve as the most powerful analytical tools commonly used to monitor pesticide residues in food, among other applications. However, both GC-MS and LC-MS are susceptible to matrix effects which can adversely affect quantification depending on the analyte, matrix, sample preparation, instrumentation, and operating conditions. Among the approaches that reduce matrix effects, the most common in pesticide residue applications is matrix-matched calibration because it is relatively inexpensive and simple. Also, it has been shown to work well during method validation when fortified samples are exactly matched with samples used for calibration. However, the quality of matrix-matched results in real-world analyses depends on the consistency of matrix effects among diverse samples. In this study, the variability of matrix effects was measured for 38 representative pesticides in 20 samples each (including different varieties) of rice, orange, apple, and spinach extracted using the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) method for analysis by LC-MS/MS and low-pressure GC-MS. Using LC-MS/MS, only oranges gave >20% matrix effects for a few pesticides. GC-MS exhibited larger matrix effects, but as in LC-MS/MS, the differences were reasonably consistent among the 20 samples tested. Main conclusions of this study are that for the conditions utilized: (1) matrix-matching was not needed for most pesticides in the simpler food matrices; and (2) for the more complex orange matrix, acceptably accurate quantitative results were achieved by using matrix-matching even with a different sample of the same type. However, full confidence cannot be extended to matrix-matched results, and for consequential applications such as regulatory enforcement, confirmatory analyses using alternate quantitative determinations should also be conducted.

Kwon H; Lehotay SJ; Geis-Asteggiante L

2012-12-01

54

Pesticide residues in some commodities: dietary risk for children.  

UK PubMed Central (United Kingdom)

The objective of this study was to identify pesticides found in infants' and children's diets. Fruits and vegetables were collected from 2004 to 2007 and analyzed using a multiresidue method. The most frequently detected residues were procymidone, captan, chlorpyrifos and chlorothalonil. Twenty-eight percent of the samples contained pesticide residues. Strawberry, pear, apple, peach and tomato contained pesticide levels of concern. Twenty-one pesticides were found with the estimated total mean daily intake greater than the acceptable daily intake for four of the pesticides. Residues of carbaryl, diazinon and methidathion exceeded regulatory levels in (apple, strawberry, and orange).

Gebara AB; Ciscato CH; Monteiro SH; Souza GS

2011-05-01

55

[Organochlorine pesticide residues in cow's milk, Nicaragua  

UK PubMed Central (United Kingdom)

This work reports on a preliminary study carried out in Nicaragua to build a profile of the contamination of cow's milk with 10 organochlorine pesticides and make recommendations based on the findings. Between December 1993 and March 1994, milk samples were collected from 48 different sites in the country. The samples were analyzed for residues of hexachlorobenzene (HCB), alpha-BHC, lindane, aldrin, dieldrin, oxychlordane, heptachlor epoxide, and the principal metabolites of DDT (p,p'-TDE, p,p'-DDE, and p,p'-DDT) by means of solid-phase extraction from milk fat, and the quantity of the residues was determined by gas chromatography with electron capture detection. Heptachlor epoxide was found in 1 milk sample, dieldrin in 1, lindane in 3, oxychlordane in 3, alpha-BHC in 3, aldrin in 6, HCB in 9, and metabolites of DDT in 39 (81% of the samples). The six samples most heavily contaminated with by-products of DDT came from the departments of León and Chinandega, in the Pacific region, where there used to be intensive cotton production. The highest concentration was found in the sample from Malpaisillo, with 1105 micrograms of pesticide per kg of milk fat. The authors recommend that studies should be done so that the risk of contamination of other food products can be estimated, and that the public's health should be protected through strict control of the production or importation, storage, sale, and use of organochlorine pesticides.

Zapata Morán AL; Santamaría Ríos MM; Alvarez Irías M; Salazar Vanegas S; Müller U

1996-06-01

56

[Organochlorine pesticide residues in human adipose tissue in Costa Rica  

UK PubMed Central (United Kingdom)

Organochlorine pesticide residues were found in 82 samples of human adipose material from 82 surgical cases in 16 Costa Rica hospitals. Identification was made by gas-liquid chromatography. The highest pesticide concentration was that of DDT and its metabolites (33.16 micrograms/g). Residues of almost all commercial pesticides were also found. Concentrations of alpha-chlordane. Aldrin and Polychlorinated biphenyls were not significant.

Barquero M; Constenla MA

1986-06-01

57

Application of isotope dilution gas chromatography-mass spectrometry in analysis of organochlorine pesticide residues in ginseng root.  

Science.gov (United States)

A highly accurate and precise method based on isotope dilution gas chromatography-mass spectrometry was developed for the determination of five matrix-bound organochlorine pesticides, namely, hexachlorobenzene and hexachlorocyclohexanes (alpha-, beta-, delta-, and gamma- isomers), in a reference sample of Panax gingseng. Identification of the analytes was confirmed under selective ion monitoring mode by the presence of two dominant ion fragments within the specific time windows (+/-1% of the relative retention time with respect to the calibration standards) and matching of relative ion intensities of the concerned ions in samples and calibration standards (within +/-5%). Quantification was based on the measurement of concentration ratios of the natural and isotopic analogues in the sample and calibration blends. To circumvent the tedious iterative process of exact isotope matching that is often used in isotope dilution mass spectrometry analysis, a single-point calibration procedure was adopted with the isotopic amount ratios in the sample and calibration blends close to unity (0.9-1.1). Under the described approach, intraday and interday repeatability of replicate analyses of organochlorine pesticides in the ginseng root sample were below 1.4%. The expanded relative uncertainty ranging from 4.0 to 6.5% at a coverage factor of 2 was significantly lower than those of conventional gas chromatographic methods using other calibration techniques (internal or external standards). A deviation of less than 2.0% from the certified values was achieved when applying the developed method to determine hexachlorobenzene, alpha-, and beta-hexachlorocyclohexane in a certified reference material (CRM), BCR-CRM 115. Because of the unavailability of relevant CRMs of herbal origins, the concerned ginseng root sample, after verification of the "true values" of the concerned organochlorine pesticides by the valid primary method, is suitable for serving as an in-house reference material for quality assurance and method validation purposes. PMID:17407316

Chan, Serena; Kong, Mei-Fong; Wong, Yiu-Chung; Wong, Siu-Kay; Sin, Della W M

2007-04-04

58

Distribution of multiple pesticide residues in apple segments after home processing  

DEFF Research Database (Denmark)

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

Rasmussen, Rie Romme; Poulsen, Mette Erecius

2003-01-01

59

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

UK PubMed Central (United Kingdom)

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

Pizzutti IR; de Kok A; Dickow Cardoso C; Reichert B; de Kroon M; Wind W; Weber Righi L; Caiel da Silva R

2012-08-01

60

Determination of pesticide residues in cereal grains  

International Nuclear Information System (INIS)

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

2005-01-01

 
 
 
 
61

Organochlorine pesticide (OCP) residues in mountain soils from Tajikistan.  

UK PubMed Central (United Kingdom)

The concentrations and spatial distribution of organochlorine pesticides (OCPs) in surface soils of different altitudes (570–4656 m) from Tajikistan were determined. OCPs were detected in all samples with concentrations in the range 52.83–247.98 ng g(-1) dry weight (ng g(-1) dw). Aldrins were the most predominant compounds followed by chlordanes, hexachlorocyclohexanes (HCHs) and endosulfans, while dichlorodiphenyltrichloroethanes (DDTs) and methoxychlor were detected at much lower concentrations. Composition analysis indicated that OCPs mainly came from the atmospheric transport of historically used pesticides. OCP residues in the west and northwest parts of Tajikistan were higher than the east and the southeast due to the proximity to the potential sources and anthropogenic activity intensities around. Additionally, correlation analysis between OCPs and altitudes indicated that the more volatile pollutants, such as HCH isomers, seemed to become enriched more easily in regions with higher altitudes relative to the less volatile ones, such as DDTs.

Zhao Z; Zeng H; Wu J; Zhang L

2013-03-01

62

Fast analysis of multiple pesticide residues in apple juice using dispersive liquid-liquid microextraction and multidimensional gas chromatography-mass spectrometry.  

UK PubMed Central (United Kingdom)

A method for the rapid trace analysis of 24 residual pesticides in apple juice by multidimensional gas chromatography-mass spectrometry (MD-GC/MS) using dispersive liquid-liquid microextraction (DLLME) was developed and optimized. Several parameters of the extraction procedure such as type and volume of extraction solvent, type and volume of dispersive solvent and salt addition were evaluated to achieve the highest yield and to attain the lowest detection limits. The DLLME procedure optimized consists in the formation of a cloudy solution promoted by the fast addition to the sample (5 ml) of a mixture of carbon tetrachloride (extraction solvent, 100 microl) and acetone (dispersive solvent, 400 microl). The tiny droplets formed and dispersed among the aqueous sample solution are further joined and sedimented (85 microl) in the bottom of the conical test tube by centrifugation. Once extracted, all the 24 pesticides were directly injected and separated by a dual GC column system, comprising a short wide-bore DB-5 capillary column with low film thickness connected by a Deans switch system to a second chromatographic narrower column, with identical stationary phase. The instrumental setting used, in combination with carefully optimized operational fast GC and MS parameters, markedly decreased the retention times of the targeted analytes. The total chromatographic run was 8 min. Mean recoveries for apple juice spiked at three concentrations ranged from 60% to 105% and the intra-repeatability ranged from 1% to 21%. The limits of detection of the 24 pesticides ranged from 0.06 to 2.20 microg/L. In 2 of a total of 28 analysed samples were found residues of captan, although at levels below the maximum limit legal established.

Cunha SC; Fernandes JO; Oliveira MB

2009-12-01

63

Public Health Implications of Pesticide Residues in Meat  

Directory of Open Access Journals (Sweden)

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

Jadhav V.J. and Waskar V.S.

2011-01-01

64

Note on pesticide residues as a function of formulation used  

International Nuclear Information System (INIS)

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).

1976-01-01

65

[Advances in determination of multi-residue pesticides in traditional Chinese medicine by GC-MS].  

UK PubMed Central (United Kingdom)

The current methods of preparation of pesticide residue analysis in traditional Chinese medicine were summarized in this paper. And the new preparation techniques used in recent years were reviewed, which included solid-phase micro-extraction (SPME), QuECHERS, matrix solid-phase dispersion (MSPD). In addition, the determination method of the pesticide residue methods in the traditional Chinese medicine were also included in the paper, and analysed the problem in the determination based on the characteristics of TCMs.

Liu D; Xue J; Wu X

2011-02-01

66

[Organochlorine pesticide residues in 4 types of vegetable oils].  

UK PubMed Central (United Kingdom)

The present study had as objectives to identify and to quantify organochlorine pesticide residues (OCP) hexachlorobenzene (HCB), lindane, cis-chlordane, heptachlor, aldrin, dieldrin, endrin and o,p'-DDT in vegetable oils of corn, soybean, sunflower and mixtures of oils, sold in the city of Maracaibo, Venezuela. 30 samples of 4 types of vegetable oils of 10 commercial brands were analyzed. The extraction of OCP residues was done according to the Official Method of AOAC. A gas chromatograph with an electronic capture detector (GC-ECD) was used for identification and quantification of OCP residues and confirmation was done with a gas chromatograph coupled with a mass spectrometer (GC-MS). All the OCP residues investigated were detected in the analyzed samples. Aldrin (0.0088), lindane (0.0054) and o,p'-DDT (0.0035) were the OCP residues detected in higher concentrations (microg/g). The statistical analysis showed significant differences (P<0.05) for the concentration of OCP in the different types and commercial brands of vegetable oils. Lindane concentration in the corn oil (0.0125 microg/g), as well as cischlordane (0.0091 microg/g) and aldrín (0.0287 microg/g) in the soybean oil exceeded maximal residual limits (MRL) established by Food and Agriculture Organization of the United Nations/World Health Organization (FAO/WHO). In conclusion, it was detected a high incidence of OCP residues in vegetable oils analyzed.

Piñero González M; Izquierdo Córser P; Allara Cagnasso M; García Urdaneta A

2007-12-01

67

Pesticides  

Energy Technology Data Exchange (ETDEWEB)

This review covers the literature on pesticide analysis published or abstracted in the period between December 15, 1984, and December 15, 1986. The major sources of information were the primary abstracting journals Chemical Abstracts and Analytical Abstracts. Journals that were searched directly include the Journal of the Association of Official Analytical Chemists, Journal of Agricultural and Food Chemistry, Bulletin of Environmental Contamination and Toxicology, Analytical Chemistry, and the Journal of Chromatography (including its bibliography issues). The review is devoted mainly to methods for the determination of residues of pesticides and related compounds in a wide variety of samples and the analysis of pesticide standards. Analyses of pesticide formulations are not covered. The attempt was made to choose the most important publications describing methodology, instrumentation, and applications that would be readily available to readers to this Journal. Abstract citations are given for references from the more obscure journals and those not published in English.

Sherma, J.

1987-06-15

68

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

Science.gov (United States)

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

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

2007-01-01

69

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

Science.gov (United States)

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

70

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

UK PubMed Central (United Kingdom)

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

Karazafiris E; Menkissoglu-Spiroudi U; Thrasyvoulou A

2008-10-01

71

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

Science.gov (United States)

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

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

2008-09-11

72

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

Science.gov (United States)

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

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

2007-06-01

73

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

UK PubMed Central (United Kingdom)

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

Cho SK; Abd El-Aty AM; Park YS; Choi JH; Khay S; Kang CA; Park BJ; Kim SJ; Shim JH

2007-06-01

74

Survey on the pesticide residues in tea in south India.  

UK PubMed Central (United Kingdom)

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

Seenivasan S; Muraleedharan N

2011-05-01

75

Survey on the pesticide residues in tea in south India.  

Science.gov (United States)

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

Seenivasan, Subbiah; Muraleedharan, NarayananNair

2010-07-20

76

Characteristics and alteration of pesticide residues in surface soils of agricultural fields and public parks  

Science.gov (United States)

Organic contents of agricultural soils are major sources of organic compounds and pesticides into atmosphere. Therefore, surface soil samples from different locations in the city of Corvallis, USA were collected over a course of 1 year (2004/2005). The samples were subject to chemical extraction and analysis by gas chromatography-mass spectrometry (GC-MS). The results of the chemical analysis showed pesticide residues were present in soils and varied seasonally. For example, the highest total relative concentration of pesticide residues in Canola field was 0.16% in January 2005, and was 0.56% in Wheat Field in August 2005, and was 0.14% in the River Front Park in December 2004 and was 0.33 in Rose Garden. Sometimes in the year, these pesticide residues were not detected in the same sites.

Al-Mutlaq, Khalid F.

2006-12-01

77

Pesticide Residue Monitoring Program Results and ...  

Science.gov (United States)

... HEXYTHIAZOX. IBP +. IMAZALIL *. IMAZAMETHABENZ METHYL ESTER (AC 222,2. IMIDACLOPRID. IN-B2838 +. IOXYNIL +. IPRODIONE *. ... More results from www.fda.gov/food/foodborneillnesscontaminants/pesticides

78

Pesticide Residue Monitoring Database User's Manual - List ...  

Science.gov (United States)

... pyrethrins, pyridaben, pyridaphenthion, pyrimethanil, pyripoxyfen, quinalphos, quinclorac, quinoxyfen, quintozene, part of quintozene (total), ... More results from www.fda.gov/Food/FoodborneIllnessContaminants/Pesticides

79

Pesticide Residue Monitoring Database User's Manual - List ...  

Science.gov (United States)

... tri-allate, triazamate, triazophos, tribufos, tributyl phosphate, trichlorfon, trichloroethylene, trichloronat, trichloronat oxygen analog, trichloronat ... More results from www.fda.gov/food/foodborneillnesscontaminants/pesticides

80

Proficiency test on incurred and spiked pesticide residues in cereals  

DEFF Research Database (Denmark)

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

Poulsen, Mette Erecius; Christensen, Hanne Bjerre

2009-01-01

 
 
 
 
81

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

UK PubMed Central (United Kingdom)

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

Cervera MI; Portolés T; Pitarch E; Beltrán J; Hernández F

2012-06-01

82

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

UK PubMed Central (United Kingdom)

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

Yao LX; Huang LX; Li GL; He ZH; Zhou CM; Yang BM; Guo B

2010-11-01

83

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

Science.gov (United States)

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

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

2010-11-01

84

[Determination of 6 kinds of pesticides residue in Dioscoreae rhizoma slices by GC-MS].  

UK PubMed Central (United Kingdom)

OBJECTIVE: To determine the 6 residues including organophosphorus, organochlorinated and pyrethroid pesticides simultaneously in crude yam slices, yam slices stir-fried with bran and sulfur fumigation yam. METHODS: The compounds were ready for GC-MS analysis after being extracted with acetonitrile and purified. Determinations were performed with selected ion monitoring mode and external standard method was adopted in the quantificaticon. RESULTS: The contents of 6 kinds pesticides residue had good linear correlation with the peak area in the rang of 0.01-0.5 microg/mL. The average recoveries of 6 kinds pesticides residue were 87.5%-95.5%. The method detection limits ranged from 0.002-0.005 microg/g. Organochlorine and pyrethroid pesticides were detected in the three samples except the parathion residue. CONCLUSION: Stir-fried with bran and sulphur fumigation had nearly no effects on the pesticides residue in yam. The method is sensitive and accurate and can be used in determination of multiresidual pesticides residue in yam.

Jiang YH; Liu W; Cao H; Yu LR; Xiang FJ

2011-12-01

85

Monitoring of pesticide residues in South Indian tea.  

Science.gov (United States)

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

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

2013-01-23

86

Monitoring of pesticide residues in South Indian tea.  

UK PubMed Central (United Kingdom)

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

Kottiappan M; Dhanakodi K; Annamalai S; Anandhan SV

2013-08-01

87

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

UK PubMed Central (United Kingdom)

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

Tang S; Liang J; Tan Y; Cheke RA

2013-01-01

88

Extraction of pesticide residues from biological and environmental samples  

International Nuclear Information System (INIS)

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

1997-01-01

89

A review of organochlorine pesticide residues in ferruginous hawk eggs  

Science.gov (United States)

Ten Ferruginous Hawk nests in northeast Oregon were studied from 1978 to 1980. Pesticide residues, eggshell thickness, and reproductive success from these nests will be reviewed. In addition, egg residues from other published studies in the Pacific Northwest and elsewhere will be discussed.

Henny, C. J.

1985-01-01

90

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

Directory of Open Access Journals (Sweden)

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

Neff Roni A; Hartle Jennifer C; Laestadius Linnea I; Dolan Kathleen; Rosenthal Anne C; Nachman Keeve E

2012-01-01

91

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

UK PubMed Central (United Kingdom)

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

Neff RA; Hartle JC; Laestadius LI; Dolan K; Rosenthal AC; Nachman KE

2012-01-01

92

Monitoring of pesticide residue in bovine milk from Nadia district, West Bengal.  

Science.gov (United States)

Monitoring of 210 bovine milk samples collected from local markets in the Nadia district of West Bengal during 2011 was performed. Samples were collected in summer and winter seasons. Analysis of pesticides was performed by using a multiresidue method validated in the laboratory. The quantification was performed using GC-ECD. Analysis revealed the presence of lindane in less than 1 % of milk samples. Endosulfan I and II were also detected and were found to exceed MRL recommended by Codex. Overall 1.90 % of the analyzed samples showed trace to measurable amount of pesticide residues. The monitored area provided pesticide residues data of milk, assisting in future scientific assessment on pesticide usage. PMID:23708263

Singh, Aruna Kumari; Sar, Tapas Kumar; Mandal, Tapan Kumar

2013-05-26

93

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

DEFF Research Database (Denmark)

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

Poulsen, Mette Erecius; Naef, A.

2009-01-01

94

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

International Nuclear Information System (INIS)

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

2008-01-01

95

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

UK PubMed Central (United Kingdom)

Amine modified graphene is successfully synthesized via a one-pot solvothermal reaction between graphene oxide and ammonia water, methylamine or n-butyl amine. The presence of amine groups in graphene is identified by Fourier-transform infrared spectrometry, X-ray photoelectron spectroscopy and an X-ray diffractometer. The ability of amine modified graphene to cleanup fatty acids and other interfering substances from acetonitrile extracts of oil crops has been evaluated. It is found that the resulting CH3NH-G exhibits the best performance in interfering substances removal. Meanwhile, a multi-residue method is validated on 28 representative pesticide residues in four oil crops (rapeseed, peanut, sesame seeds and soybean). This method is based on modified QuEChERS sample preparation with CH3NH-G as reversed-dispersive solid phase extraction material and liquid chromatography-tandem mass spectrometry. Use of matrix-matched standards provides acceptable results for most pesticides with overall average recoveries between 70.5 and 100% and consistent RSDs<13%, except for pymetrozine, thidiazuron and diuron. In any case, this method still meets the 0.1-8.3 ?g/kg detection limit needs for most pesticides and may be used for qualitative screening applications, in which any identified pesticides can be quantified and confirmed by a more intensive method that achieves >70% recovery.

Guan W; Li Z; Zhang H; Hong H; Rebeyev N; Ye Y; Ma Y

2013-04-01

96

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

UK PubMed Central (United Kingdom)

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

Wan MT

2013-01-01

97

Studies on organochlorine pesticide residue in fishes from the Densu river basin, Ghana.  

UK PubMed Central (United Kingdom)

The study was carried out to determine the levels of organochlorine pesticide residue in five fish species Chrysichthys nigrodigitatus, Hepsetus odoe, Tilapia zilli, Heterotis niloticus and Oreochromis niloticus from the Densu river basin (Weija) in Ghana. The fishes sampled from the Weija fish landing site were selected on the basis of their importance to local human fish consumption. The detectable organochlorine pesticides were ?-Hexachlorocyclohexane (HCH), ?-Hexachlorocyclohexane, aldrin and dieldrin. Others investigated were alpha endosulfan, endosulfan sulfate, p,p'-DDT and its metabolite p,p'-DDE, endrin and its metabolite endrin aldehyde and endrin ketone. The total contamination levels of the individual fishes varied in the decreasing order of 9.19 ng g(-1) (O. niloticus), 4.16 ng g(-1) (T. zilli), 3.69 ng g(-1) (C. nigrodigitatus), 3.68 ng g(-1) (H. odoe) and 3.09 ng g(-1) (H. niloticus). The highest organochlorine pesticide residue recorded in the study was alpha-endosulfan while dieldrin was the least pesticide observed. Analysis of variance indicated significant statistical differences for most organochlorine pesticide residues in the samples. The levels of organochlorine pesticides found in fish samples in the study were below maximum residue limit for food safety stipulated by EU, US FDA, FAO, Italy and Australia and thus safe for human consumption.

Kuranchie-Mensah H; Yeboah PO; Nyarko E; Golow AA

2013-04-01

98

Pesticide persistence and bound residues in soil - regulatory significance  

International Nuclear Information System (INIS)

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

2005-01-01

99

Levels of Organochlorine Pesticide Residues in Grasscutter (Thryonomys swinderianus) Tissues  

Directory of Open Access Journals (Sweden)

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

Sarah Blankson-Arthur; P. Owiredu Yeboah; Abledze Golow; Anita Osei Tutu; Dzifa Denutsui

2011-01-01

100

Glove accumulation of pesticide residues for strawberry harvester exposure assessment.  

UK PubMed Central (United Kingdom)

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

Li Y; Chen L; Chen Z; Coehlo J; Cui L; Liu Y; Lopez T; Sankaran G; Vega H; Krieger R

2011-06-01

 
 
 
 
101

Glove accumulation of pesticide residues for strawberry harvester exposure assessment.  

Science.gov (United States)

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

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

2011-04-19

102

[Determination of organochlorine pesticide residues in Microcos paniculata by GC].  

UK PubMed Central (United Kingdom)

OBJECTIVE: To establish a method for determination 9 organochlorine pesticide residue in Microcos paniculata by gas chromatography. METHODS: The sample was infiltrated with water and extracted with hexane by ultrasonic. The extract solvent was purified by concentrated sulphuric acid. DB-1701 capillary column was used to separate the sample. GC-ECD was applied to determine the residues of organochlorine pesticide. RESULTS: The percentage recoveries were ranged from 78.1% to 97.8% and RSD were from 2.4% to 8.8%. CONCLUSION: The method established is quick, simple and low in cost.

Lu P; Chen WT; Chen HA; Long Y; Yang LW; Ye WC; Jiang RW

2012-08-01

103

Food and Drug Administration Pesticide Program Residue ...  

Science.gov (United States)

Text Version... (2) Pesticide Analytical Manual Volume I ... 7 28.6 0.0 Olives 45 75.6 4.4 2 Peaches ... 30 96.7 3.3 Vegetable oil, crude 1 100.0 0.0 Vegetable oil, refined ... More results from www.fda.gov/downloads/Food/FoodSafety

104

Automated QuEChERS Tips for Analysis of Pesticide Residues in Fruits and Vegetables by GC-MS.  

UK PubMed Central (United Kingdom)

This paper reports the development of an automated method of QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) using pipet tips fitted with filtration screens and containing primary-secondary amine, magnesium sulfate, and graphitized carbon black. These tips are referred to as "QuEChERS Tips". Using loosely contained sorbent, dispersive solid phase extraction (dSPE) cleanup was performed with the QuEChERS Tips and automation. The main advantage of the QuEChERS Tips is that they are readily automated because this dSPE method does not require centrifugation. High recoveries (70-117%) and good reproducibilities (<12%) are shown for over 200 pesticides using automated QuEChERS Tips and GC-MS in various sample matrices.

Kaewsuya P; Brewer WE; Wong J; Morgan SL

2013-02-01

105

MSPD Sample Preparation Approach for Reversed-Phase Liquid Chromatographic Analysis of Pesticide Residues in Stem of Coconut Palm.  

UK PubMed Central (United Kingdom)

A method was developed using matrix solid-phase dispersion, together with liquid chromatography with ultraviolet diode array detector for determination of carbofuran, difenoconazole, ?-cyfluthrin, spirodiclofen and thiophanate-methyl in stem of coconut palm. The best results were obtained using 2.0 g of stem, 1.6 g of Florisil as sorbent and cyclohexane:acetone mixture (4:1). The method was validated using stem samples spiked with pesticides at four concentration levels (0.05-2.0 ?g/g). Average recoveries ranged from 70 % to 114.3 %, with relative standard deviations between 1.2 % and 19.2 %. Detection and quantification limits were in the ranges 0.02-0.03 and 0.05-0.1 ?g/g, respectively.

Ferreira JA; Santos LF; Souza NR; Navickiene S; de Oliveira FA; Talamini V

2013-08-01

106

MSPD sample preparation approach for reversed-phase liquid chromatographic analysis of pesticide residues in stem of coconut palm.  

Science.gov (United States)

A method was developed using matrix solid-phase dispersion, together with liquid chromatography with ultraviolet diode array detector for determination of carbofuran, difenoconazole, ?-cyfluthrin, spirodiclofen and thiophanate-methyl in stem of coconut palm. The best results were obtained using 2.0 g of stem, 1.6 g of Florisil as sorbent and cyclohexane:acetone mixture (4:1). The method was validated using stem samples spiked with pesticides at four concentration levels (0.05-2.0 ?g/g). Average recoveries ranged from 70 % to 114.3 %, with relative standard deviations between 1.2 % and 19.2 %. Detection and quantification limits were in the ranges 0.02-0.03 and 0.05-0.1 ?g/g, respectively. PMID:23722654

Ferreira, Jordana Alves; Santos, Luís Fabrício Santana; Souza, Nicaellen Roberta da Silva; Navickiene, Sandro; de Oliveira, Frederico Alberto; Talamini, Viviane

2013-05-31

107

Ability of NIRS technology to determine pesticides in liquid samples at maximum residue levels.  

UK PubMed Central (United Kingdom)

BACKGROUND: Pesticide residues remaining on food represent a potential risk to consumer's health. Determination of these pesticide residues involves tedious procedures of analysis with regard to time and laboratory work. Near-infrared spectroscopy (NIRS) is a possible alternative to these methods. The aim of this research was to evaluate the ability of NIRS to classify two pesticides used for controlling apple fruit pests according to their concentration. Different solutions were prepared, based on the dose recommended by the pesticide producers for apple pest treatments. Spectra were acquired on a spectrophotometer from liquid samples belonging to these solutions. RESULTS: Calibration models were developed from liquid samples, following the soft independent modelling of class analogy (SIMCA) analysis method. These models classified between 99 and 100% of the validation samples belonging to different pesticide concentration solutions even at the maximum residue limit level of these products in apple fruit. CONCLUSIONS: NIRS technology shows a high potential for identifying pesticides in liquid samples, according to their concentration, at the levels required by the legislation.

Arias N; Arazuri S; Jarén C

2013-04-01

108

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

DEFF Research Database (Denmark)

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

Hjorth, Karen; Johansen, K.

2011-01-01

109

APPARATUS FOR TREATMENT OF PESTICIDE RESIDUES BY UTILIZING OZONE AND ULTRASONIC WAVES WHILE REMOVING PESTICIDE RESIDUES AT SAME TIME  

UK PubMed Central (United Kingdom)

PURPOSE: An apparatus for treatment of pesticide residues by sterilizing an object of treatment in which pesticides remain on the surface by utilizing ozone and ultrasonic waves while removing pesticide residues, in particular removing ozone remaining in the air after the treatment using an ozone treatment catalyst is provided. It enables the opening of the lid as soon as the sterilizing and pesticide residues-removing treatment of the object of treatment is completed. CONSTITUTION: The apparatus for treatment of pesticide residues consists of: a packing(2), an ozone sensor(29) for detecting the ozone concentration and a circulating fan(28) installed at the upper part of a box type container for receiving water an ozone inlet(22) installed at the lower part of the container through the intervention of an ozone tube(21) which is in communication with an ozone generator(20) an ultrasonic wave generator(25) installed at the lower part of the container, a vibrating plate(26) connected to the ultrasonic wave generator an ozone treatment catalyst(4) at the lower part of a lid part(3).

KIM DO WOAN; LEE DONG KYU; MAENG JU SUK; MOON YOUNG HWAN; PARK JIN SEONG

110

Organochlorine Pesticide Residues in Human Adipose Tissue.  

Science.gov (United States)

The article presents findings of selected organochlorine residues for surveys conducted on human adipose tissue during fiscal years 1970, 1971, and 1972. The residues selected for presentation in this paper were beta-benzene hexachloride, total DDT equiva...

F. W. Kutz A. R. Yobs S. C. Strassman

1976-01-01

111

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

Science.gov (United States)

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

Swarnam, T P; Velmurugan, A

2012-12-04

112

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

UK PubMed Central (United Kingdom)

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

Swarnam TP; Velmurugan A

2013-07-01

113

Reduction of pesticide residues in tomatoes and other produce.  

UK PubMed Central (United Kingdom)

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

Al-Taher F; Chen Y; Wylie P; Cappozzo J

2013-03-01

114

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

Scientific Electronic Library Online (English)

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

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

2001-08-01

115

Evaluation of cost-effective methods in the pesticide residue analysis of non-fatty baby foods  

UK PubMed Central (United Kingdom)

Three non-fatty ready-to-eat baby food matrices (fruits: juice, purée and cocktail plus rice flour/starch and sugar) were fortified with 0.01, 0.05, 0.1 and 0.2mg/kg of dimethoate, chlorpyrifos, methidathion, phosalone and diazinon. Simple methods including extraction by ethyl acetate [EtAc] and acetone partition and determination by gas chromatography with Nitrogen-Phosphorus Detector (GC-NPD) were used. Acceptable pesticides recoveries (70-110%), low detection and quantification limits (0.001 to >0.1mg/kg and 0.005 to 0.04mg/kg, respectively) and repeatabilities (%RSDs), in 0.01mg/kg, within 2.9-13.9% were observed. However, analytes recoveries were affected (p <0.05) by both the baby food formulation and the extraction method used. Specifically, fruits purée and cocktail EtAc extracts gave excessively over-(dimethoate recoveries of 119.7-153.5%) or underestimation (phosalone and especially diazinon recoveries of 19.3-79.2%) in contrast to fruits juice (e.g., 61.3-87.9%). Also, EtAc extracts showed higher amount of lipophilic compounds and provided lower recoveries for non-polar analytes than those of acetone partition. Consequently, the examined methods may be successfully applied in non-fatty baby foods with the matrix-matched standards determination, following improvements of certain parameters in relation to the clean-up of samples.

Georgakopoulos Panagiotis; Mylona Aggeliki; Athanasopoulos Panagiotis; Drosinos EleftheriosH; Skandamis PanagiotisN

2009-08-01

116

Pesticide residues in the soil of the Central Jordan Valley  

International Nuclear Information System (INIS)

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

1997-01-01

117

Organochlorine Pesticide Residues in Fish Samples from Lagos Lagoon, Nigeria  

Directory of Open Access Journals (Sweden)

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

David Adeyemi; Grace Ukpo; Chimezie Anyakora; JohnPaul Unyimadu

2008-01-01

118

Removal of residual pesticides in vegetables using ozone microbubbles.  

UK PubMed Central (United Kingdom)

The removal of fenitrothion (FT) pesticide residues from vegetables by immersion in ozone-microbubbled solution was demonstrated. FT-treated lettuce, cherry tomatoes, and strawberries were immersed in ozone-microbubbled, ozone-millibubbled, and dechlorinated water. After that the percentage of residual FT in the vegetables was determined. Residual FT was efficiently removed from lettuce by immersing it in ozone-microbubbled solution containing more than 1.0 ppm dissolved ozone, or continuously generated ozone-microbubbled solution containing 2.0 ppm dissolved ozone. Similarly, for cherry tomatoes and strawberries, the continuously generated ozone-microbubbled solution containing 2.0 ppm dissolved ozone was highly effective. These results showed that ozone microbubbles effectively removed residual pesticides not only from leafy vegetables but also from fruity vegetables.

Ikeura H; Kobayashi F; Tamaki M

2011-02-01

119

Removal of residual pesticides in vegetables using ozone microbubbles.  

Science.gov (United States)

The removal of fenitrothion (FT) pesticide residues from vegetables by immersion in ozone-microbubbled solution was demonstrated. FT-treated lettuce, cherry tomatoes, and strawberries were immersed in ozone-microbubbled, ozone-millibubbled, and dechlorinated water. After that the percentage of residual FT in the vegetables was determined. Residual FT was efficiently removed from lettuce by immersing it in ozone-microbubbled solution containing more than 1.0 ppm dissolved ozone, or continuously generated ozone-microbubbled solution containing 2.0 ppm dissolved ozone. Similarly, for cherry tomatoes and strawberries, the continuously generated ozone-microbubbled solution containing 2.0 ppm dissolved ozone was highly effective. These results showed that ozone microbubbles effectively removed residual pesticides not only from leafy vegetables but also from fruity vegetables. PMID:21168959

Ikeura, H; Kobayashi, F; Tamaki, M

2010-11-27

120

A review of organochlorine pesticide residues in Swainson's hawk eggs  

Science.gov (United States)

U. s. Fish and Wildlife Service research projects during the last 10 years in the Pacific Northwest resulted in the collecting of a sample egg from 35 Swainson's Hawk nests (Henny and Kaiser, 1979. Murrelet 60:2-5; Henny et al. 1984. Raptor Research 18:41-48). Pesticide residues, eggshell thickness, and reproductive success from these nests will be reviewed. In addition, egg residues from other published studies in the Pacific Northwest and elsewhere will be discussed.

Henny, C. J.

1985-01-01

 
 
 
 
121

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

UK PubMed Central (United Kingdom)

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.

Yang L; Li H; Miao H; Zeng F; Li R; Chen H; Zhao Y; Wu Y

2011-10-01

122

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

Directory of Open Access Journals (Sweden)

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

Mohd Aslam; Sumbul Rais; Masood Alam

2013-01-01

123

[Determination of organophosphorus pesticide residues in vegetables by gas chromatography using back-flush technique].  

UK PubMed Central (United Kingdom)

The back-flush technique was used in the determination of organophosphorus pesticide residues in vegetables by gas chromatography. The pesticide residues were extracted with acetonitrile and sodium chloride under mechanical shaking, and separated by centrifuging and partitioning. The extract was analyzed by gas chromatograph equipped with a flame photometric detector and a micro fluidic device with back-flush function. The results showed that the 16 organophosphorus pesticides have good linearity within the concentration range of 0.040 -3.20 mg/L. The recoveries varied from 75.2% to 111.5%, with the relative standard deviations (RSDs) in the range of 2.8% - 10.4%. The detection limits of these target compounds were from 0.003 to 0.01 mg/kg. The application of back-flush technique in this method significantly reduced the cycle time and matrix effect and improved the analysis efficiency.

Li L; Wu C; Chen J; Zhang S; Ye Y

2010-07-01

124

The Organochlorine Pesticides Residue Levels in Karun River Water  

Directory of Open Access Journals (Sweden)

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

Behrooz Jannat; Abdolazim Behfar; Zahra Nazari; Mohammad Hassan Rabiee; Gholamreza Raeesi; Mohammad Reza Oveisi; Nafiseh Sadeghi

2013-01-01

125

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

Directory of Open Access Journals (Sweden)

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

B. ?ozowicka; P. Kaczy?ski; E. Rutkowska; M. Jankowska; I. Hrynko

2013-01-01

126

Acetylcholinesterase Based Detection of Residual Pesticides on Cotton  

Directory of Open Access Journals (Sweden)

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

Syed Zameer Ul Hassan; Jiri Militky

2012-01-01

127

Detoxicating and cleaning agent for residual pesticide of garden stuff  

UK PubMed Central (United Kingdom)

The invention relates to a detoxification and cleaning agent of residual pesticides in fruits and vegetables, and the detoxification and cleaning agent is prepared by adopting pure natural plants and formed by mixing emulsifier, fruit acid, citric acid, biological enzyme, stabilizer, defoamer, thickener, fragrance and distilled water according to certain proportion. The decomposition and removal rate of the detoxification and cleaning agent on the residual pesticides in the fruits and the vegetables can be more than 90-98 percent, and the detoxification and cleaning agent has no secondary pollution by being used for cleaning the fruits and the vegetables. The detoxification and cleaning agent is characterized by convenient use, safety, reliability, no toxicity or stimulus to human body, etc.

YI ZHANG

128

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

Directory of Open Access Journals (Sweden)

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

Sh. Najafpour; S.M.V. Farabi; M. Yousefian; F.M. Abbas Alkarkhi; Ganjian Khenary

2010-01-01

129

Evaluation of two sample treatment methodologies for large-scale pesticide residue analysis in olive oil by fast liquid chromatography-electrospray mass spectrometry.  

UK PubMed Central (United Kingdom)

In this study, a comprehensive evaluation of two simple sample treatment methodologies has been carried out for the development of large-scale multi-residue methods for pesticide testing in olive oil. The proposed methodologies are based on (a) liquid-liquid partitioning with acetonitrile followed by dispersive solid-phase extraction clean-up using graphitized carbon black, primary-secondary amine and C(18) sorbents; (b) liquid partitioning with acetonitrile saturated with petroleum ether followed by matrix solid-phase dispersion (MSPD) using aminopropyl as sorbent material and a Florisil cartridge for final clean-up in the elution step. To evaluate the proposed sample treatment methodologies, 105 representative multi-class pesticides were studied using fast liquid chromatography-electrospray time-of-flight mass spectrometry (LC-TOFMS). For validation purposes, recoveries studies were carried out at 10 and 100microgkg(-1) levels, yielding recovery rates in the range 70-130% for 72% of analytes using liquid-liquid procedure and for 57% analytes using MSPD procedure. The LC-MS method provided good linearity, precision and accuracy. The limits of detection obtained were lower than 10microgkg(-1) for more than 85% analytes using both sample treatment methodologies. In addition, minor matrix effects (i.e. signal suppression or enhancement < or =20%) were observed in ca. 70% of the studied compounds. Data obtained shows that both sample treatment methodologies proposed can be successfully applied for large-scale pesticide testing in olive oil samples, showing the ability to quickly detect trace amount of over one hundred target species with different physicochemical properties, without requiring expensive instrumentation for sample treatment step and involving relatively low amounts of solvent consumption and waste generation.

Gilbert-López B; García-Reyes JF; Fernández-Alba AR; Molina-Díaz A

2010-06-01

130

Organochlorine pesticide residues in biological compartments of healthy mothers.  

UK PubMed Central (United Kingdom)

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

Elserougy S; Beshir S; Saad-Hussein A; Abouarab A

2013-06-01

131

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

Science.gov (United States)

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

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

2008-01-01

132

Fast, low-pressure gas chromatography triple quadrupole tandem mass spectrometry for analysis of 150 pesticide residues in fruits and vegetables.  

UK PubMed Central (United Kingdom)

We developed and evaluated a new method of low-pressure gas chromatography-tandem mass spectrometry (LP-GC/MS-MS) using a triple quadrupole instrument for fast analysis of 150 relevant pesticides in four representative fruits and vegetables. This LP-GC (vacuum outlet) approach entails coupling a 10 m, 0.53 mm i.d., 1 ?m film analytical column between the MS transfer line and a 3 m, 0.15 mm i.d. capillary at the inlet. The MS creates a vacuum in the 10 m analytical column, which reduces the viscosity of the He carrier gas and thereby shifts the optimal flow rate to greater velocity. By taking advantage of the H(2)-like properties of He under vacuum, the short analytical column, a rapid oven temperature ramp rate, and the high selectivity and sensitivity of MS/MS, 150 pesticides were separated in <6.5 min. The 2.5 ms dwell time and 1 ms interscan delay of the MS/MS instrument were critical for achieving >8 data points across the 2-3 s wide peaks. To keep dwell and cycle times constant across all peaks, each segment consisted of 30 analytes (60 transitions). For assessment, we injected extracts of spiked broccoli, cantaloupe, lemon, and sweet potato from the updated QuEChERS sample preparation method. Average recoveries (n=72) were 70-120% for 144 of the pesticides, and reproducibilities were <20% RSD for all but 4 analytes. Also, detection limits were <5 ng/g for all but a few pesticides, depending on the matrix. In addition to high quality performance, the method gave excellent reliability and high sample throughput, including easy peak integration to obtain rapid results.

Koesukwiwat U; Lehotay SJ; Leepipatpiboon N

2011-09-01

133

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

UK PubMed Central (United Kingdom)

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

Gutierrez R; Ortiz R; Vega S; Schettino B; Ramirez ML; Perez JJ

2013-01-01

134

Potential and real residues of pesticides in sugar beet  

Directory of Open Access Journals (Sweden)

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

Šovljanski Radmila A.; Lazi? Sanja D.; Vukovi? Slavica

2006-01-01

135

Organochlorine pesticide residues in fish from southern Italian rivers  

Energy Technology Data Exchange (ETDEWEB)

Extensive use of pesticides in agricultural and municipal fields contributed all over the world to an effective increase of production and to a limitation of the vector injuries to health. However the large quantities of synthetic chemical products employed to achieve these purposes have resulted in an extended environmental pollution, especially worrying about the organochlorine insecticides that are very persistent and suspected of carcinogenicity. For these reasons, this group of pesticides has been banned or strongly restricted in many countries including Italy, where just Lindane and Endosulfan are now allowed in agriculture, representing only 7% of the annual use of synthetic pesticides. In order to control the amount of contamination of surface water from organochlorine pesticides, some surveys were carried out in northern and central Italy, but information regarding situation in southern Italy is not available. The purpose of this study was to evaluate the occurrence and the magnitude of chlorinated pesticide aquatic pollution in southern Italy by the analysis of some permanent freshwater fish species.

Amodio-Cocchieri, R.; Arnese, A.

1988-02-01

136

Method for detecting chlorothalonil pesticide residue and detection kit therefor  

UK PubMed Central (United Kingdom)

The invention relates to a method for detecting ELISA remained in chlorothalonil pesticide and a reagent kit thereof. Glycol is utilized to substitute chloride atoms on 6 position carbon atoms of chlorothalonil molecules to synthesize a semiantigen then an imidazolone method is adopted to link the semiantigen to a carrier, namely bovine serum albumin molecules to form an artificial complete antigen an antigen-immunized rabbit is used to prepare a polyclonal antibody which is assembled with related reagents into an ELISA reagent kit and an ELISA indirect method of antigen-primary antibody-ELIAS secondary antibody is used to detect residues of the chlorothalonil pesticide. The method has the advantages of low cost, high efficiency, and low detection limit the detection of 96 samples at one time can be finished within four hours, and the lowest limit of the detection is 0.016mg.kg<-1>.

LILI ZHANG; HONGJIN BAI; YANQIN WANG; CHUANXING WAN; WENJIE LIU; WEI CHEN; XIAOLIANG ZHAO; BO JING

137

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

International Nuclear Information System (INIS)

Cocoa is a major cash crop and contributes significantly to Ghana's economy. Majority of this contribution is as a result of foreign earnings in foreign trade partnership. Cocoa products are consumed locally aside it generating foreign income for the country. Pesticide residues above allowable limits in cocoa beans have potential detrimental effects on human health, depending on the frequency of exposure and/or the potency or toxicity of the pesticide. Pesticide residues on cocoa also attract trade sanctions from international trading partners. The approved pesticides, which are used to control pests in the growing cocoa in Ghana, are: Diazinon, Cypermethrin, Deltamethrin, Acetamiprid, Imidicloprid and Pyrethrums; nevertheless some unapproved pesticides on cocoa such as Pirimiphos-methyl, Chlorpyrifos, Endosulfan, Fenitrotion, Fenvalerate, Permethrin and others find their way for use on cocoa in Ghana. The main objective of this study was to determine the levels of pesticide residues in fermented dried cocoa beans produced and ready for export in Ghana, using gas chromatography mass spectrometry. It also seeks to provide the baseline information on contamination levels of pesticide residues in semi-finished and selected finished fermented dried cocoa beans products. Fermented dried cocoa beans were sampled at random in the two main COCOBOD warehouses located in Tema and Takoradi. Semi-finished and finished cocoa products were obtained from processing industries in Tema. Two extraction methods were used. The second extraction method was as by the QuEChERS method for vegetable oils which was used for the cocoa butter samples only, after being liquefied in water bath at 40 degrees celsius. The investigated pesticides consisted of fifteen organochlorine pesticides, thirteen organophosphorous pesticides and nine synthetic pyrethroids pesticides. Percentage recoveries ranged from 70-110 percent, with instrumental detection limits of 0.3ug/kg, 0.15ug/g and 0.15ug/g for the organochlorine, organophosphorous and synthetic pyrethroids pesticides respectively. Multivariate analysis on the residue data obtained from fermented dried cocoa beans in R-mode and Q-mode grouped the detected pesticides into currently used, previously used and drift from neighbouring crops pesticides applications. It also grouped sampled cocoa beans into four major clusters based on similarities in crop storage and farm practices. Beta-HCH (18.7 ?g/kg), Gamma-chlordane (152.0 ?g/kg), Methamidophos (18.5 ?g/kg), Profenofos (31.8 ?g/kg), Allethrin (10.5 ?g/kg), Cypermethrin (32.0 ?g/kg) and Fenvalerate (14.6 ?g/kg) were the average residues concentrations of pesticides that exceeded the Japanese maximum residue levels (MRLs). However, all the detected pesticides with exception of Allethrin were below the MRLs for European Union. From results recorded in semi-finished and finished cocoa beans products produced in Ghana, de-shelling and roasting temperatures drastically reduced the residue levels in the cocoa products, but these were not enough solution for pesticide residues in cocoa beans. And thus raises concern about the health implication of these chemicals for domestic consumption of these products. It is highly recommended that a national quality control laboratory be established to continually monitor pesticides efficacy in order to avoid overdose of pesticides application.[au

2011-01-01

138

Pesticide Residues, Results from the period 2004-2011  

DEFF Research Database (Denmark)

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

Petersen, Annette; Jensen, Bodil Hamborg

2013-01-01

139

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

International Nuclear Information System (INIS)

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

2001-01-01

140

Analysis of pesticide residues in matrices with high lipid contents by membrane separation coupled on-line to a high-performance liquid chromatography system.  

Science.gov (United States)

Separation through membranes coupled to an HPLC system was used as a technique for the analysis of pesticide multiresidues in samples with high lipid contents. As well as the usual procedure, in the proposed system it is possible to recirculate the sample through the membrane cell, which permits the extraction system to be applied to cases in which only a very small volume of sample is available. A procedure for pesticide multiresidue analysis in egg samples was developed as a representative example of the applicability of the proposed method. To accomplish this, the analytes (dichlorvos, dimethoate, propoxur, paraoxon, pirimicarb, atrazine, ametryne, terbutryne, azinphos-methyl, folpet) were subjected to prior extraction in a Soxhlet system, after which the extract was introduced into the membrane separation device coupled to the HPLC system. This procedure afforded clean chromatograms, hence considerably facilitating determination, and at the same time was efficient in removing macromolecular compounds. For egg samples, spiked at a concentration level of 0.750 mg/kg, recoveries ranged from 60 to 98%. The detection limits varied from 0.018 mg/kg for dichlorvos to 0.002 mg/kg for atrazine. PMID:10720256

Carabias-Martínez, R; Rodríguez-Gonzalo, E; Paniagua-Marcos, P H; Hernández-Méndez, J

2000-02-11

 
 
 
 
141

Analysis of pesticide residues in matrices with high lipid contents by membrane separation coupled on-line to a high-performance liquid chromatography system.  

UK PubMed Central (United Kingdom)

Separation through membranes coupled to an HPLC system was used as a technique for the analysis of pesticide multiresidues in samples with high lipid contents. As well as the usual procedure, in the proposed system it is possible to recirculate the sample through the membrane cell, which permits the extraction system to be applied to cases in which only a very small volume of sample is available. A procedure for pesticide multiresidue analysis in egg samples was developed as a representative example of the applicability of the proposed method. To accomplish this, the analytes (dichlorvos, dimethoate, propoxur, paraoxon, pirimicarb, atrazine, ametryne, terbutryne, azinphos-methyl, folpet) were subjected to prior extraction in a Soxhlet system, after which the extract was introduced into the membrane separation device coupled to the HPLC system. This procedure afforded clean chromatograms, hence considerably facilitating determination, and at the same time was efficient in removing macromolecular compounds. For egg samples, spiked at a concentration level of 0.750 mg/kg, recoveries ranged from 60 to 98%. The detection limits varied from 0.018 mg/kg for dichlorvos to 0.002 mg/kg for atrazine.

Carabias-Martínez R; Rodríguez-Gonzalo E; Paniagua-Marcos PH; Hernández-Méndez J

2000-02-01

142

Multi-analyst, multi-matrix performance of the QuEChERS approach for pesticide residues in foods and feeds using HPLC/MS/MS analysis with different calibration techniques.  

UK PubMed Central (United Kingdom)

Three different calibration approaches were applied in HPLC/MS/MS using electrospray ionization for the determination of 14 diverse pesticide residues at different levels in a variety of food matrixes. This study was conducted as part of a 4 day training course for 17 chemists to learn the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) approach to pesticide residue analysis in foods. The analysts were divided into four different teams for the analysis of 12 different matrixes (strawberries, plums, carrots, green peppers, milk, molasses, alfalfa oats, corn silage, dry pet food, soybean, almonds, and foliage). The acetate-buffered QuEChERS protocol gave excellent results in the spiked samples for all matrixes tested. The HPLC/MS/MS calibration techniques consisted of external standardization in solvent solutions, matrix-matching, and the echo-peak technique. Peak areas were normalized to an internal standard in all three approaches. Matrix effects were observed with the corn silage, carrot, and foliage extracts, but they were minimal or nonexistent in the other matrixes. Matrix-matching best compensated for matrix effects, but has logistical difficulties in real-world application and required extra sample preparation compared to the other approaches. The echo-peak technique reduced matrix effects but did not eliminate them.

Lehotay SJ; Mastovska K; Lightfield AR; Gates RA

2010-03-01

143

Pesticide residues in conventional, integrated pest management (IPM)-grown and organic foods: insights from three US data sets.  

UK PubMed Central (United Kingdom)

An analysis of pesticide residue data was performed to describe and quantify differences between organically grown and non-organic fresh fruits and vegetables. Data on residues in foods from three different market categories (conventionally grown, integrated pest management (IPM)-grown/no detectable residues (NDR), and organically grown) were compared using data from three test programmes: The Pesticide Data Program of the US Department of Agriculture; the Marketplace Surveillance Program of the California Department of Pesticide Regulation; and private tests by the Consumers Union, an independent testing organization. Organically grown foods consistently had about one-third as many residues as conventionally grown foods, and about one-half as many residues as found in IPM/NDR samples. Conventionally grown and IPM/NDR samples were also far more likely to contain multiple pesticide residues than were organically grown samples. Comparison of specific residues on specific crops found that residue concentrations in organic samples were consistently lower than in the other two categories, across all three data sets. The IPM/NDR category, based on data from two of the test programmes, had residues higher than those in organic samples but lower than those in conventionally grown foods.

Baker BP; Benbrook CM; Groth E 3rd; Lutz Benbrook K

2002-05-01

144

Pesticide residues in conventional, integrated pest management (IPM)-grown and organic foods: insights from three US data sets.  

Science.gov (United States)

An analysis of pesticide residue data was performed to describe and quantify differences between organically grown and non-organic fresh fruits and vegetables. Data on residues in foods from three different market categories (conventionally grown, integrated pest management (IPM)-grown/no detectable residues (NDR), and organically grown) were compared using data from three test programmes: The Pesticide Data Program of the US Department of Agriculture; the Marketplace Surveillance Program of the California Department of Pesticide Regulation; and private tests by the Consumers Union, an independent testing organization. Organically grown foods consistently had about one-third as many residues as conventionally grown foods, and about one-half as many residues as found in IPM/NDR samples. Conventionally grown and IPM/NDR samples were also far more likely to contain multiple pesticide residues than were organically grown samples. Comparison of specific residues on specific crops found that residue concentrations in organic samples were consistently lower than in the other two categories, across all three data sets. The IPM/NDR category, based on data from two of the test programmes, had residues higher than those in organic samples but lower than those in conventionally grown foods. PMID:12028642

Baker, B P; Benbrook, C M; Groth, E; Lutz Benbrook, K

2002-05-01

145

Organochlorine Pesticides Residues in Mussels of Greek Island Evia  

Directory of Open Access Journals (Sweden)

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

Konstantinos M. Kasiotis

2009-01-01

146

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

International Nuclear Information System (INIS)

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

2009-01-01

147

[Determination of 29 pesticide residues in tobacco by gas chromatography-electron impact ionization mass spectrometry].  

UK PubMed Central (United Kingdom)

A method was developed for rapid determination of 29 pesticide residues in tobacco based on gas chromatography coupled with electron impact ionization mass spectrometric detection (GC-EI/MS). After the optimization of different parameters, such as the extraction solvent, elution solvent, purificant, pesticides were extracted from tobacco with hexaneacetone (1: 1, v/v) in an ultrasonic bath, cleaned-up on a column, packed with Florisil and neutral alumina, eluted with dichloromethane-hexane (95:5, v/v), and then determined by GC-EI/MS in the selected ion monitoring mode (SIM) with triphenyl phosphate (TPP) as internal standard. The recoveries were performed at 20, 50 and 100 microg/kg fortification levels for each pesticide, and the recoveries ranged from 70% to 110% with the relative standard deviations between 2% and 8%. The detection limits were less than 0.8 microg/kg for 26 pesticides except for the fenpropathrin, deltamethrin and permethrin. The method was linear over the range of 5.0-500.0 microg/kg with the correlation coefficients between 0.9994 to 0.9999. The method was successfully applied to the analysis of these pesticides in tobacco.

Zou X; Lin Z; Peng S; Chen Z

2009-03-01

148

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

UK PubMed Central (United Kingdom)

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

Watanabe E; Kobara Y; Baba K; Eun H

2013-05-01

149

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

Science.gov (United States)

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

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

2013-05-13

150

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

Science.gov (United States)

The use and application of pesticides in vineyard is a common practice, which is important to prevent pest and diseases and improve the crop health and production, but on the other hand it could involve a potential risk for humans and the environment. For this reason, it is important to develop and validate a simple and fast multiresidue method to determine the presence of these compounds in soils. La Rioja region (Spain) is one of the most important wine-growing regions in Spain, which also entails that could be an important area of pesticide pollution. The objective of this work is to assess the temporal distribution of the possible pesticide pollution in soils from different areas of La Rioja (Spain). The pesticides selected in this study included fungicides (metalaxyl, and its metabolite CGA62826, pyrimethanil, tebuconazole, myclobutanil, kresoxim-methyl, triadimenol and flutriafol); herbicides (fluometuron, terbuthylazine and its metabolites desethylterbuthylazine and hydroxyterbuthylazine, lenacil, ethofumesate and acetochlor) and insecticides (methoxyfenozide and pirimicarb). The pesticide residues were evaluated by two analytical techniques, gas chromatography and liquid chromatography (GC-MS and LC-MS). The extraction procedure of pesticides from soils was optimized using two soil samples (blank soils) with different texture and characteristics collected from areas without pesticide application. Recoveries were studied in soil samples fortified with all pesticides at two levels of concentrations (the agronomic dose, 0.1 mg kg-1, and ten times this dose, 1 mg kg-1). Different extraction solvents were tested. The best results were obtained with methanol:acetone (50:50) mixture or methanol:CaCl2 0.01 M (50:50) mixture for hydroxyterbuthylazine and CGA62826. The accuracy (average recovery) and precision (reproducibility and repeatability) of the method were assessed using six replicates and the limits of detection (LODs) and quantification (LOQs) were estimated. Recoveries were above 70% for all pesticides. Good linear relationships of the calibration curves (0.01-1 ?g mL-1) were obtained for all the compounds by the two analytical methods with regression coefficients (r2) higher than 0.99 in the range of concentrations studied. Detection limits were < 2 ng g-1 for pesticides studied. After the development and validation of an analytical method, the study of the temporal variability of the pesticide pollution in different periods of time (September 2011, and March, June and October 2012) were performed. Herbicide residues were found in most of the soils and an increment in concentrations of these compounds and in the number of positive samples were detected in samples collected in March 2012 in relation to those collected in September 2011. This increase in the number of positive samples was of 30 % for terbuthylazine. Fungicide residues were detected in greater concentrations in samples collected in September. Both behaviours may be related with the time of application of both types of compounds. Herbicides are commonly applied in March-April and fungicides are usually applied in summer, when different grapevine diseases like botrytis or mildiu commonly appear. Moreover, new pesticide residues were detected in March 2012, which were not detected in September 2011 in any soil sample. Further analysis of results is in course.

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

2013-04-01

151

A Survey of Determination for Organophosphorus Pesticide Residue in Agricultural Products  

Directory of Open Access Journals (Sweden)

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

Wen Li; Ming Sun; Minzan Li

2013-01-01

152

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

UK PubMed Central (United Kingdom)

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

Kusvuran E; Yildirim D; Mavruk F; Ceyhan M

2012-11-01

153

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

Science.gov (United States)

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

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

2012-09-26

154

Multiresidue pesticide analysis of the medicinal plant Origanum syriacum.  

Science.gov (United States)

Origanum syriacum is a medicinal plant widely used in Jordan both as a folk remedy and in the food and beverage industry. As the plant can be treated with pesticides during commercial production, three different methods for pesticide multiresidue analysis of this plant have been evaluated. One method based on soxhlet extraction followed by acetonitrile/petroleum ether (PE) partitioning was found to be particularly suitable. Extracts were cleaned-up using a Florisil column. Mean recoveries of pesticides from spiked herbal samples were 74-119%, with coefficients of variation between 1.0 and 23.6%. The limits of detection were in the range 0.0008-0.5 mg kg(-1). The method was used for the determination of pesticide residues in O. syriacum samples purchased from the local market. Seven out of eight samples contained detectable levels of dichlorodiphenyltrichloroethane (DDT), folpet, dicofol, hexachlorobenzene (HCB), hecachlorocyclohexane (HCH), quintozene, transchlordane and vinclozolin. PMID:17364929

Hajjo, R M; Afifi, F U; Battah, A H

2007-03-01

155

Multiresidue pesticide analysis of the medicinal plant Origanum syriacum.  

UK PubMed Central (United Kingdom)

Origanum syriacum is a medicinal plant widely used in Jordan both as a folk remedy and in the food and beverage industry. As the plant can be treated with pesticides during commercial production, three different methods for pesticide multiresidue analysis of this plant have been evaluated. One method based on soxhlet extraction followed by acetonitrile/petroleum ether (PE) partitioning was found to be particularly suitable. Extracts were cleaned-up using a Florisil column. Mean recoveries of pesticides from spiked herbal samples were 74-119%, with coefficients of variation between 1.0 and 23.6%. The limits of detection were in the range 0.0008-0.5 mg kg(-1). The method was used for the determination of pesticide residues in O. syriacum samples purchased from the local market. Seven out of eight samples contained detectable levels of dichlorodiphenyltrichloroethane (DDT), folpet, dicofol, hexachlorobenzene (HCB), hecachlorocyclohexane (HCH), quintozene, transchlordane and vinclozolin.

Hajjo RM; Afifi FU; Battah AH

2007-03-01

156

[Determination of 88 pesticide residues in cranberry plant extract by gas chromatography-triple quadrupole tandem mass spectrometry].  

Science.gov (United States)

A method by using a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) and gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS) was established to analyze 88 pesticide residues in cranberry plant extract. The sample was extracted with acetone-hexane (1: 1, v/v) containing 1% acetic acid, then cleaned-up by ethylenediamine-N-propyl silyl (PSA) and graphite carbon (GCB). The extract was determined by GC-MS/MS in multi-reaction monitoring (MRM) mode, and external standard method was applied to quantified the pesticides. All the 88 pesticides showed good linearity in the range of 0. 001 - 0. 2 mg/L, and the limits of quantification (LOQs, S/N > or = 10) were all less than 31. 5 microg/kg. The average recoveries of all the pesticides were in the range of 71. 4% to 116. 6% at three spiked levels of 5, 25 and 50 microg/kg in cranberry plant extract, with the relative standard deviations (RSDs) of 2. 4% - 16. 9%. The results demonstrated that this method is simple, rapid and suitable for the determination of 88 pesticide residues in cranberry plant extract. The analytical sensitivity and accuracy can meet the requirements of multiple pesticide residue analysis. PMID:22268353

Huang, Jiangrui; Kong, Xianghong; Yao, Binghua; He, Qiang; Hao, Kaituo

2011-10-01

157

[Determination of 88 pesticide residues in cranberry plant extract by gas chromatography-triple quadrupole tandem mass spectrometry].  

UK PubMed Central (United Kingdom)

A method by using a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) and gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS) was established to analyze 88 pesticide residues in cranberry plant extract. The sample was extracted with acetone-hexane (1: 1, v/v) containing 1% acetic acid, then cleaned-up by ethylenediamine-N-propyl silyl (PSA) and graphite carbon (GCB). The extract was determined by GC-MS/MS in multi-reaction monitoring (MRM) mode, and external standard method was applied to quantified the pesticides. All the 88 pesticides showed good linearity in the range of 0. 001 - 0. 2 mg/L, and the limits of quantification (LOQs, S/N > or = 10) were all less than 31. 5 microg/kg. The average recoveries of all the pesticides were in the range of 71. 4% to 116. 6% at three spiked levels of 5, 25 and 50 microg/kg in cranberry plant extract, with the relative standard deviations (RSDs) of 2. 4% - 16. 9%. The results demonstrated that this method is simple, rapid and suitable for the determination of 88 pesticide residues in cranberry plant extract. The analytical sensitivity and accuracy can meet the requirements of multiple pesticide residue analysis.

Huang J; Kong X; Yao B; He Q; Hao K

2011-10-01

158

Pesticide residues in sediments and aquatic species in Lake Nokoue and Cotonou Lagoon in the Republic of Benin.  

UK PubMed Central (United Kingdom)

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

Yehouenou A Pazou E; Aléodjrodo PE; Azehoun JP; van Straalen NM; van Hattum B; Swart K; van Gestel CA

2013-08-01

159

[Survey of pesticide residues in imported tea (1992.4-2010.3)].  

UK PubMed Central (United Kingdom)

A survey of pesticide residues in 116 imported tea samples on the Tokyo market from April 1992 to March 2010 was carried out. Twenty-two kinds of pesticides, including organophosphorus, organochlorine, pyrethroid and others, were detected at levels between trace (below 0.01 ppm) and 4.0 ppm in 76 samples. The rate of detection was 90% in non-fermented tea, 89% in semi-fermented tea, and 49% in fermented tea. Organophosphorus pesticide was not detected in puer tea, which is fermented with bacteria. The pesticide residues tended to be decreased by a fermentation process. However, organochlorine and pyrethroid pesticides appeared to be chemically stable, so they were still detected in fermented teas. Residue levels of these pesticides were calculated as less than 1% of ADI, except for ethion (45% of ADI) based on the daily intake of tea. Therefore, these teas should be safe when drunk in customary amounts.

Kobayash M; Ohtsuka K; Tamura Y; Tomizawa S; Kinoshita T; Kamijo K; Iwakoshi K; Sato C; Nagayama T; Takano I

2013-01-01

160

[Simultaneous determination of pesticide residues in agricultural products by LC-MS/MS].  

UK PubMed Central (United Kingdom)

A method for the simultaneous determination of multiple pesticide residues in agricultural products was developed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). The sample was extracted with acetonitrile. Co-extractives were removed by GPC/graphitized carbon column SPE, and silica gel/PSA cartridge column SPE. Pesticides in the test solution were determined by LC-MS/MS using scheduled MRM. Recoveries of 124 pesticides from spinach, brown rice, soybean, orange and tomato were tested at the level of 0.1 µg/g, and those of 121 pesticides ranged from 70 to 120% (RSD?15%). Pesticide residues in 239 agricultural products were investigated by this method, and residues of 49 pesticides were detected in 98 agricultural products.

Watanabe M; Ueno E; Inoue T; Ohno H; Ikai Y; Morishita T; Oshima H; Hayashi R

2013-01-01

 
 
 
 
161

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

International Nuclear Information System (INIS)

The Densu River Basin is one of the largest agricultural areas in Ghana. About 80% of people living in this area rely on agricultural activities for subsistence. The practice of using pesticides such as organochlorines, organophosphates, carbamates, pyrethroids and several others in agriculture and public health programs have raised concerns about potentially adverse effects on human health and the environment. Assessment of human health implications of non-point sources within a river basin include pesticide residues analysis of water, sediment and fish and monitoring of physico-chemical parameters in waters that serve as source of drinking water for the entire community within the basin. In this study, a field survey was conducted to assess farmers' knowledge of safe handling and use of pesticides. Nutrient chemistry and surface water characteristics of the Densu River and its tributaries, type and levels of pesticide residues and their trends in water, sediment and fish in the basin were also evaluated. The study also assessed the health risk associated with pesticide contamination of fish from the Basin as well as the relationship between land use and groundwater contamination. Generally surface and ground water bodies in the Densu River basin were found to be polluted with respect to nutrients and pesticides. Waters from the basin were found to be fresh, slightly acidic, and weakly mineralized with low chemical constituents. Nitrate (NO3-N) levels in surface water ranged between 0.12 - 31.07 mgL-1 while ammonia was between 0.01 - 2.10 mgL-1 and that of phosphate was 0.012 - 2.45 mgL-1. Pesticide residues and metabolites detected in water, sediment and fish samples from the Densu River Basin were organochlorines. In an average 96% of fish samples, 13.69% of sediment and 3.30% of water samples, at least one pesticide residue was detected per sample. Of the numerous pesticides evaluated, ? -HCH, DDT, aldrin, dieldrin, DDE, endosulfan sulphate, ?-chlordane, endrin and ?-HCH were detected in fish, water and sediment samples. Aldrin and dieldrin levels detected were above the recommended limit of 0.03 ?L-1 with endosulfan, endrin and chlordane registering levels above their recommended limits of 20.0?L-1 and 0.2 ?L-1 respectively for drinking water. Pesticide residues in fish samples varied between 0.10 ?gKg-1 to 30.90 ?gKg-1. The highest level was detected in Hepsetus odoe (HO-N). Contamination pattern of pesticide residues in fish samples was generally in the order of p'p'-DDE > heptachlor > ?- HCH > p'p'-DDT > endosulfan Sulphate > ?-endosulfan > ?- HCH > ?-chlordane > dieldrin > endrin ketone > methoxychlor > endrin > aldrin > endrin aldehyde. Data obtained from the field survey regarding safe use of pesticides, toxicity awareness and symptoms among farmers indicated that a very high proportion of farmers were at high risk of pesticide poisoning from occupational exposure. More than 90% of farm workers did not practice safety precaution during pesticide formulation and application leading to considerable prevalence of pesticide related illness in this agricultural community. The presence of pesticide residues in fish was of further concern because fish is the main protein diet for humans in the basin. The estimated dose for aldrin, methoxychlor, ?-chlordane, endrin aldehyde, endrin ketone, endrin, p'p'-DDT and ?-HCH do not pose a direct hazard to human health, although present in fish samples since the values registered were lower than the reference doses. However, ?- HCH, heptachlor, ?-endosulfan, endosulfan sulphate, p'p'-DDE and dieldrin levels exceeded the reference dose, indicating a great potential for systemic toxicity in children who are considered to be the most vulnerable population subgroup. In children, between the ages of 0 - 1year, the hazard indices of 2.64, 1.720, 1.736 and 0.792 were computed for ?-endosulfan, heptachlor, endosulfan sulphate and dieldrin respectively while for children between the ages 1 -11years, hazard indices for heptachlor, ?-endosulfan and endosulfan were 0.573,

2010-01-01

162

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

Science.gov (United States)

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

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

2011-08-09

163

[Assessment of pesticide residues in food of plant origin in Milan (Italy), 2008-2011].  

UK PubMed Central (United Kingdom)

Objectives: To monitor the presence of pesticide residues in food of plant origin in Milan from 1 July 2008 to 31 December 2011. Materials and methods: Food of plant origin found in fruit and vegetable markets and in supermarkets was analysed, to evaluate whether it was contaminated by any seventy active principles of pesticides. Results: Two hundred seventy-seven samples of fruits and vegetables were analysed. No pesticide residues were found in 61.7% of the samples, 37.9% had residues below the maximum threshold and 0.4% had residues above the threshold. Conclusions: Results are satisfactory and in agreement with national and international data.

Tesauro M; Cesaria MC; Fracchia S; Benzoni M; Bollani M; Consonni M; Bianchi A

2013-05-01

164

Detoxification machine of residual pesticide on fruit and vegetable  

UK PubMed Central (United Kingdom)

The present utility model relates to a fruit and vegetable pesticide residue detoxifying device, comprising an aeration tank, an ozonizer, ablending pump and a plurality of pipelines which are connected to them. The water inlet of blending pump is connected to ozone outlet of ozonizer and water return inlet in the aeration tank the water discharging pipe of blending pump is connected to the outlet of aeration tank, whose water return inlet is equipped with filtering layer and one side of bottom with feculency collecting slot. The present utility model is characterized by solving the problems that current home detoxifying device can not utilize the washing water circularly and aeration head is used to input the ozone into the water directly with uneven mixture, low utilization rate of ozone, bad sterilization effect and so on.

DI WEI ZHANG

165

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

UK PubMed Central (United Kingdom)

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 <15% in the concentration range of 0.005-0.250 mg/kg. The limit of detection (LOD) for all compounds met maximum 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 ?-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.

Fernandes VC; Domingues VF; Mateus N; Delerue-Matos C

2011-07-01

166

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

International Nuclear Information System (INIS)

[en] There is a basic lack of information about the presence of pesticide residues in the environment in Central America. Over the period of February 1995 to June 1997, river, well, lagoon and spring water samples, as well as soil, fish tissue, lagoon bed sediments and some foodstuffs were taken from the greater Cholutecan River Basin of Honduras and analyzed for pesticide residues. These were collected at three separate sites (La Lima, Zamorano and Choluteca), each characterized by differing agricultural production systems. The main pesticide residues found in soil samples were dieldrin and p,p'-DDT, while river water samples were found to have detectable levels of heptachlor, endosulfan and chlorpyrifos, with lagoon and well water also being shown to contain heptachlor. These pesticides detected were in more than 20% of the samples assessed. In river water samples more pesticide residues at higher concentrations were found to be associated with areas of more intensive agricultural production. The fewest pesticides with lowest concentrations were found in the small subwatershed associated with traditional agricultural production. Although the pesticides found in the soils at the three sites were generally similar they tended to be higher in the southern part of the Cholutecan watershed, followed by the central zone, with the lowest concentrations being found in the more traditional production zone. In lagoon and well water samples more pesticides, but mostly in lower concentrations were detected at the traditional production site than at the others. Ten pesticide compounds were detected in fish tissue, mainly organochlorines, some of which were also found in lagoon sediments. In terms of food products, almost no pesticides were detected in vegetables, but the kidney adipose tissue taken from slaughtered cows was shown to have a tendency to contain some organochlorines. Spring water in the traditional agricultural production zone contained three organochlorine compounds as well as chlorpyrifos, but these were detected only in the rainy season. This study indicates that pesticide residues are present and strongly associated with areas of intensive agriculture, although even in the areas practicing more traditional agriculture, pesticide residues were not absent. Further pesticide monitoring is necessary to obtain a more complete picture of the situation and based on this data an effective policy framework to assist in minimizing pesticide residue accumulation may be developed to reduce the adverse impact these compounds are known to have on the environment and human health. This snapshot of the pesticide distribution in three agriculturally distinct regions within the Choluteca watershed indicates that the situation is stable, but should be monitored to determine if pesticides residues will pose a health hazard in the future. (author)

1999-01-01

167

Influences of sampling methodologies on pesticide-residue detection in stream water.  

UK PubMed Central (United Kingdom)

Traditional grab sampling (GS) used widely in the study of water quality has been found lacking in spatial and temporal resolution for pesticide residue monitoring in stream water. The objectives of this article are to present a hydrograph-based sampling approach and compare it with traditional GS according to sensitivity at temporal and spatial scales and maximum concentrations of pesticide residues detected in-stream. Data collected from streams receiving water from three nested watersheds located in northwestern New Brunswick, Canada, were used in this study. The results showed that the hydrograph-based sampling method detected 20 to 30 % more pesticide cases than GS for rainfall events causing runoff. Grab sampling significantly underestimated average concentrations of pesticide residues by 50 % and maximum concentrations by 1 to 3 orders of magnitude. Using a modified sampler design, the spatial and temporal variability of pesticide residues was more accurately captured by hydrograph-based sampling, and therefore its use in monitoring programs is recommended.

Xing Z; Chow L; Rees H; Meng F; Li S; Ernst B; Benoy G; Zha T; Hewitt LM

2013-02-01

168

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

Science.gov (United States)

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

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

2002-01-01

169

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

International Nuclear Information System (INIS)

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

2009-01-01

170

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

UK PubMed Central (United Kingdom)

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

Seebunrueng K; Santaladchaiyakit Y; Soisungnoen P; Srijaranai S

2011-09-01

171

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

Science.gov (United States)

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

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

2011-07-10

172

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

UK PubMed Central (United Kingdom)

A multi-class, multi-residue method for the analysis of 13 novel flame retardants, 18 representative pesticides, 14 polychlorinated biphenyl (PCB) congeners, 16 polycyclic aromatic hydrocarbons (PAHs), and 7 polybrominated diphenyl ether (PBDE) congeners in catfish muscle was developed and evaluated using fast low pressure gas chromatography triple quadrupole tandem mass spectrometry (LP-GC/MS-MS). The method was based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction with acetonitrile and dispersive solid-phase extraction (d-SPE) clean-up with zirconium-based sorbent prior to LP-GC/MS-MS analysis. The developed method was evaluated at 4 spiking levels and further validated by analysis of NIST Standard Reference Materials (SRMs) 1974B and 1947. Sample preparation for a batch of 10 homogenized samples took about 1h/analyst, and LP-GC/MS-MS analysis provided fast separation of multiple analytes within 9min achieving high throughput. With the use of isotopically labeled internal standards, recoveries of all but one analyte were between 70 and 120% with relative standard deviations less than 20% (n=5). The measured values for both SRMs agreed with certified/reference values (72-119% accuracy) for the majority of analytes. The detection limits were 0.1-0.5ng g(-1) for PCBs, 0.5-10ng g(-1) for PBDEs, 0.5-5ng g(-1) for select pesticides and PAHs and 1-10ng g(-1) for flame retardants. The developed method was successfully applied for analysis of catfish samples from the market.

Sapozhnikova Y; Lehotay SJ

2013-01-01

173

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

Energy Technology Data Exchange (ETDEWEB)

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

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

1996-12-31

174

Pesticide residue legal standards for beverages: risk regulation and public perception  

DEFF Research Database (Denmark)

Exposure to pesticide residues in dietary sources is a major concern of Europeans. Meanwhile, drinking water and food safety authorities establish and implement maximum residue levels (MRLs) for pesticides in drinking water and food. This study compares MRLs between EU, US and Codex authorities for both drinking water and other beverages, i.e. milk, juice and wine, investigating differences between authorites as well as between beverage types. These results were confronted with public perceptions towards pesticide residues in beverages, based on a consumer survey conducted in Copenhagen, Denmark. Seven frequently-occurring pesticides were selected for this study. Results show that since no specific MRLs for juice and wine exist, MRLs for the raw products were used instead. Furthermore, established MRLs are significantly greater for pesticides in beverages when compared to legal standards for drinking water. Maximum levels in drinking water, if available, are generally low (0.0001 mg/L in the EU), while MRLs for pesticides in milk, juice and wine range from 0.05 to 60 mg/L. At the same time, questionnaire participants were equally concerned about their exposure to pesticide residues in drinking water and other beverage types. These findings reveal some inconsistencies in setting legal maximum concentrations for pesticide residues in different dietary sources as well as between different drinking water and food safety authorities.

Grieger, Khara Deanne; Trapp, Stefan

2007-01-01

175

Multi pesticide and PCB residues in Nile tilapia and catfish in Assiut city, Egypt.  

UK PubMed Central (United Kingdom)

The current study investigated the levels of multi pesticide residues in the highly consumed types of Nile fish in Egypt: tilapia and cat fish. A total of 50 Nile tilapia (Oreochromis niloticus) and 50 African catfish (Clarias gariepinus) were collected from two areas in Assiut city, where most industries are situated and where agricultural activities and raising of farm animals are the main activities. In the first area, Elwasta, there is an electrical power station, and the second area, Mankbad, there is a cement factory. Fish samples were analyzed by High Resolution Gas Chromatography/Mass Spectrometry. Average pesticide residue concentrations±SE in muscle of tilapia and catfish (n=10 pooled samples with five fish each) were determined. The results indicated the presence of different types of organophosphorous (OPs), organochlorine (OC), polychlorinated biphenyles (PCBs), hexachlorobenzene (HCB) and trifluralin pesticides in Elwasta and Mankbad in varying degrees. Diazenon was the only OP pesticide which exceeded the permissible limit in both investigated areas with the two types of fish. On the other hand, OCs, PCBs, HCB and trifluralin pesticide residue levels have not exceeded the maximum allowable concentration limit. In general, a higher pesticide residue level was obtained in Mankbad than Elwasta. In addition, higher values are realized for the detected pesticide residues in cat fish than tilapia. The results of the study have shown the extensive and recent use of these types of pesticides in the present time in Egypt.

Yahia D; Elsharkawy EE

2013-07-01

176

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

UK PubMed Central (United Kingdom)

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

Toan PV; Sebesvari Z; Bläsing M; Rosendahl I; Renaud FG

2013-05-01

177

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

Science.gov (United States)

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

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

2013-03-15

178

Pesticide residues in fruits at the market level in Accra Metropolis, Ghana, a preliminary study.  

UK PubMed Central (United Kingdom)

A number of pesticide residues in fruits were monitored at five markets in the Accra Metropolis for almost a year. Locally produced fruits (pawpaw and tomato) and imported apple were purchased from these selected markets in the metropolis and analyzed for pesticide residues by gas chromatography equipped with electron capture detector. In all, 320 sampled fruits were extracted and analyzed for pesticide residues, mainly organochlorines (?-HCH, ?-HCH, aldrin, heptachlor, ?-chlordane, heptachlor epoxide, ?-endosulfan, p,p'-DDE, endrin, ?-endosulfan, o,p'-DDT, endrin aldehyde, p,p'- DDT, endrin ketone, and methoxychlor). The data revealed that 32.8% of the fruit samples analyzed contained residues of the monitored insecticides above the accepted maximum residue limit (MRL) whereas 48.7% were below the MRL. Nonetheless, the continuous consumption of such fruits with modest pesticide levels can accumulate and could result in deadly chronic effects.

Bempah CK; Donkor AK

2011-04-01

179

Pesticide residues in fruits at the market level in Accra Metropolis, Ghana, a preliminary study.  

Science.gov (United States)

A number of pesticide residues in fruits were monitored at five markets in the Accra Metropolis for almost a year. Locally produced fruits (pawpaw and tomato) and imported apple were purchased from these selected markets in the metropolis and analyzed for pesticide residues by gas chromatography equipped with electron capture detector. In all, 320 sampled fruits were extracted and analyzed for pesticide residues, mainly organochlorines (?-HCH, ?-HCH, aldrin, heptachlor, ?-chlordane, heptachlor epoxide, ?-endosulfan, p,p'-DDE, endrin, ?-endosulfan, o,p'-DDT, endrin aldehyde, p,p'- DDT, endrin ketone, and methoxychlor). The data revealed that 32.8% of the fruit samples analyzed contained residues of the monitored insecticides above the accepted maximum residue limit (MRL) whereas 48.7% were below the MRL. Nonetheless, the continuous consumption of such fruits with modest pesticide levels can accumulate and could result in deadly chronic effects. PMID:20559713

Bempah, Crentsil Kofi; Donkor, Augustine Kwame

2010-06-18

180

Pesticide residue levels in maize samples from markets in Lagos State, Nigeria.  

UK PubMed Central (United Kingdom)

BACKGROUND: Pesticides are used widely in agriculture to control destructive pests and hence increase food supply. Their use inadvertently leads to residues in food crops and the environment. Pesticides, by nature are poisonous and exposure of humans to their residues may cause health hazards which include neurotoxicity and carcinogenicity among others. Evaluation of pesticide residues in food is therefore of public health importance and would help to ensure that levels are kept within safety limits. OBJECTIVE: The aim of this study was to determine the incidence and quantity of organochlorine pesticide residues in maize samples collected from various markets in Lagos State and compare values obtained with established safety values in order to highlight possible health hazards. METHODS: In this study, samples of white maize (Zea mays L.) purchased from different markets in Lagos State were analyzed for residues of organochlorine pesticides using gas chromatograph with mass spectrometric detector (GC-MS) after careful extraction and cleanup. RESULTS: The results showed that 96% of the maize samples contained residues of one or more organochlorine pesticides. Mean concentrations ranged from 7.9-52.0 microg/kg and maximum residue limits (MRLs) of some pesticides were exceeded in up to 7% of samples. The estimated total diet intakes (ETDIs) for aldrin and dieldrin exceeded their maximum permissible intakes. CONCLUSION: It is concluded that residues of organochlorine pesticides are present in maize in Lagos markets. Some exceed safety levels with possible adverse effects on human health. There is therefore a need for more stringent monitoring of the use of pesticides in agriculture and food storage in Nigeria.

Ogah CO; Coker HA; Adepoju-Bello AA

2011-04-01

 
 
 
 
181

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

Several insecticides, germicides and herbicides which, are now prohibited, are still used in Chinese common tea gardens. Applied amounts of the pesticides with high toxicity and long time residues, such as methomyl, cannot bypass certain limits in A-grade green food tea gardens. Pesticides are forbi...

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

182

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

UK PubMed Central (United Kingdom)

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

Tascone O; Roy C; Filippi JJ; Meierhenrich UJ

2013-06-01

183

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

UK PubMed Central (United Kingdom)

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

Kamijo K; Kobayashi M; Otsuka K; Tamura Y; Tomizawa S; Sakai N; Kageyama Y; Takano I; Nagayama T

2009-06-01

184

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

UK PubMed Central (United Kingdom)

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

Tsiropoulos NG; Amvrazi EG

2011-03-01

185

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

UK PubMed Central (United Kingdom)

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

Bedi JS; Gill JP; Aulakh RS; Kaur P; Sharma A; Pooni PA

2013-10-01

186

Monitoring of Some Pesticides Residue in Consumed tea in Tehran Market  

Directory of Open Access Journals (Sweden)

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

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

2013-01-01

187

Monitoring of some pesticides residue in consumed tea in Tehran market  

Directory of Open Access Journals (Sweden)

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

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

2013-01-01

188

Monitoring of some pesticides residue in consumed tea in Tehran market  

Science.gov (United States)

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

2013-01-01

189

The Concept of Withholding Period and Pesticide Residue in Grain Storage  

Directory of Open Access Journals (Sweden)

Full Text Available This review focuses on pesticides, their unquantifiable benefits to agriculture, pesticide residue, maximum pesticide residue limit, and withholding period in grain storage. It delved into the origin of synthetic pesticide and its introduction to Nigeria in the 1950s, it maintained that pesticide have posed major health and social challenges, and have had negative, unintended, catastrophic, fatal consequences to man, animals, and even the environment especially when instructions on their labels are not adhered to. Again, it maintained that withholding periods are often stipulated on the labels of genuine pesticides, it reiterated that not adhering to the stipulated withholding period can have catastrophic consequences on consumers of grain and grain products. Furthermore, it dwelt on the activities of Nigerian stored Products Research Institute (NSPRI) and National Food Drug Administration and Control (NAFDAC), their mandates and quest to nip pesticide poisoning in the bud. Finally, recommendations were put forward to check the seeming ignorance and dearth of information about pesticide residue limit and withholding period, and dangers that are concomitants of not adhering to these.

Adegbola, J. A.; Anugwom, U. D.; Awagu, F.; Adu, E. A.

2012-01-01

190

Residual pesticide concentrations in tea after processing to various types of tea and in tea infusions.  

UK PubMed Central (United Kingdom)

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

Kondo T; Watanabe A; Shitara H; Kaburagi Y; Shibata M; Kanda N; Kurokawa C; Inoue Y; Miyazaki M; Togawa M; Ozawa A; Uchiyama T; Koizumi Y; Nakamura Y; Masuda S; Maitani T

2013-01-01

191

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

Directory of Open Access Journals (Sweden)

Full Text Available "n "nBackgrounds and Objectives: Water contamination by pesticides is considered as an environmentalproblem today. In terms of agricultural development and diversity of plant pests, the use of pesticides has been increasing. Hamedan province has a suitable agricultural condition, it has enjoyed significant development in this respect. Among all the cities of Hamedan province, Hamedan city has the highest rank in tiller crops. Therefore, yearly use of pesticides is increasing in this area; which could be a serious threat to water resources of the city. The aim of this survey was determinaton of Organophosphorous and Carbamat pesticides residue in drinking water resources of Hamadan in 2007."nMaterials and Methods: In this survey, 126 water samples were collected from 7 drinking water resources of Hamedan during 12 consecutive months in 2007. for determination of these pesticides,two methods (solid- phase extraction and Liquid-Liquid extraction) were adopted .and samples were analyzed by means of HPLC and GC/MS applying standard methods."nResults: Final results showed that the most concentration of Chlorpyrifos and Carbaryl pesticides were found to be about 3.85 ppb (part per billion) and 1.8 ppb in spring and June respectively; the maximum concentration of Diazinon was about 36.5ppb in October (autumn).The minimum concentration of the three pesticides was detected in winter. According to the statistical test Two - Way ANOWA there were significant differences among pesticides concentrations in the water samples in different seasons (p0.05). "nConclusion: Different studies have shown that pesticides residue concentration in water samples have a relationship with the amount of pesticides used in an area, physical and chemical refractory properties of pesticides; and environmental conditions. Thus, using resistant pollutants such as pesticides will be a serious threat to health of water consumers if they are not properly controlled.

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

2010-01-01

192

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

Directory of Open Access Journals (Sweden)

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

Fatemeh Nasehi; Mohammad Zaeefi Zadeh; Hossein Shahbazi; Ghadir Noori Ghonbalani

2007-01-01

193

Determination of pesticide residue in selected fruits and vegetable  

International Nuclear Information System (INIS)

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

2005-01-01

194

[Determination of twenty pesticide residues in Viscum coloratum by gas chromatography using cloud-point extraction].  

UK PubMed Central (United Kingdom)

OBJECTIVE: To establish a gas chromatography method for simultaneous determination of organochlorine and pyrethroid pesticide residues in Viscum coloratum by cloud-point extraction (CPE). METHOD: Pesticides were extracted with the non-ionic surfactant Triton X-100. The apparatus was gas chromatography with electron capture detector and the separation was performed on an Hp-5 column. The pesticide residues were calculated by external standard method. RESULT: Good linear relation was obtained over the range of 5-500 microg L(-1) for organochlorine and 10-1,000 microg L(-1) for pyrethroid. The limits of detection was 1.5-7.5 microg kg(-1). The average recoveries of organochlorine and pyrethroid were 74.15% -111.6% with corresponding RSD of 4.0% -9.1%. CONCLUSION: The sample and rapid method was applied to pesticide residues determination.

Zhang S; Chen X; Yu Z; Shen X; Gou M; Bi K

2009-10-01

195

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

UK PubMed Central (United Kingdom)

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

Kobayashi M; Ohtsuka K; Tamura Y; Tomizawa S; Kinoshita T; Kamijo K; Iwakoshi K; Sato C; Nagayama T; Takano I

2013-01-01

196

[Determination of organochlorine pesticide residues in the roots of Zanthoxylum nitidum by GC-MS].  

UK PubMed Central (United Kingdom)

OBJECTIVE: To determine the contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum and provide scientific foundation for the quality control and standard establishment. METHODS: GC-MS method with selected ion monitoring (SIM) mode was used to analyze the contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum. The samples were extracted with acetone and ultrasonic vibrations, and the analytical samples were purified by anhydrous sodium sulfate-anhydrous magnesium sulfate -PSA -C18-PestiCarb -phase extraction (SPE) cartridge. RESULTS: Eight kinds of organochlorine pesticide were detected simultanously. Small amounts of OP-DDT were detected in samples 1, 4, 5, 6, 11 and 12, no organochlorine pesticide residue was detected in other samples. The RSD of precision ranged from 0.89% to 2.21%, and the average recovery ranged from 85.33% to 103.70%, with the RSD less than 4%. CONCLUSION: The contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum are less than 0.2 ppm. This method is sensitive, good purifying, and suitable for analyzing organochlorine pesticide residues in the roots of Zanthoxylum nitidum.

Jiao AJ; Feng J; Lai MX

2013-04-01

197

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

UK PubMed Central (United Kingdom)

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

Essumang DK; Asare EA; Dodoo DK

2013-09-01

198

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

UK PubMed Central (United Kingdom)

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

Young SJ; Kamps LR

1982-07-01

199

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

Science.gov (United States)

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

Young, S J; Kamps, L R

1982-07-01

200

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

Science.gov (United States)

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

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

2008-04-01

 
 
 
 
201

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

Directory of Open Access Journals (Sweden)

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

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

2012-01-01

202

Organochlorine Pesticide Residues in the Major Rivers of Southern Thailand  

Directory of Open Access Journals (Sweden)

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

Abd Naser Haji Samoh

2009-01-01

203

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

Directory of Open Access Journals (Sweden)

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

D.K. Essumang; G.K. Togoh; L. Chokky

2009-01-01

204

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

Science.gov (United States)

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

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

2013-01-23

205

Results of the monitoring program of pesticide residues in organic food of plant origin in Lombardy (Italy).  

UK PubMed Central (United Kingdom)

Organic agriculture, with its restrictions on the use of synthetic chemical inputs, seems to offer a low-residue alternative to conventional methods. In Europe, the Council Regulation n. 2092/91/EEC regulates the production and trade of organic products and foodstuffs; national and regional legislation in Italy gives specific guidance on the surveillance of organic agriculture. However, monitoring of specific chemical residues in organic foodstuffs is part of the regular controls on food, aiming to safeguard consumer's health. Monitoring programs are coordinated at the national level by the Ministry of Health and at local level by Regional authorities. In Lombardy, in accordance with the provisions of the General Directorate of Health of the Region and under the supervision of the 15 Local Health Units, a monitoring program of pesticide residues in food of plant origin is undertaken every year. The International Centre for Pesticides and Health Risk Prevention (ICPS), on behalf of the General Directorate of Health of the Region of Lombardy, has been collecting and elaborating the data resulting from the analysis of food samples, carried out by the local laboratories. During the period 2002-2005, a total of 3508 samples food of plant origin were analyzed for pesticide residues, among which were 266 samples of organic farming products. Commodities were classified into groups (citrus fruits, legumes, vegetables, potatoes, processed products, cereals, and fruit other than citrus) and the outcomes of the analyses were reported by year, origin of the sample and presence/absence of pesticide residues. Results showed that the vast majority of organic farming products were in conformity with the relevant legislation and did not contain detectable pesticide residues. A limited amount of samples had residues at concentration below the Maximum Residue Limit (MRL). Only in one sample the residue level was above the MRL, however it did not pose a concern for public health, as demonstrated by the outcomes of dietary risk assessment. Organic fruits and vegetables can be expected to contain fewer agrochemical residues than conventionally grown alternatives. There is a widespread belief that organic agriculture products are safer and healthier than conventional foods. It is difficult to come to conclusions, but what should be made clear to the consumer is that "organic" does not automatically equal "safe". In the absence of adequate comparative data, additional studies in this area of research are required.

Tasiopoulou S; Chiodini AM; Vellere F; Visentin S

2007-09-01

206

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

International Nuclear Information System (INIS)

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

2011-01-01

207

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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

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

208

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

Directory of Open Access Journals (Sweden)

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

Tong Dewen; Hesheng Yang; Wang Jinyi

2007-01-01

209

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

Science.gov (United States)

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

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

2011-01-01

210

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

UK PubMed Central (United Kingdom)

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

Kobayashi M; Ohtsuka K; Tamura Y; Tomizawa S; Kamijo K; Iwakoshi K; Kageyama Y; Nagayama T; Takano I

2011-01-01

211

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

International Nuclear Information System (INIS)

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

1999-01-01

212

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

Directory of Open Access Journals (Sweden)

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

Mohammed A. Al-Doghairi; Suloiman AL-Rehiayani; Khaled A. Osman; Eltayeb A. Elhag

2004-01-01

213

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

International Nuclear Information System (INIS)

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

2005-01-01

214

Residues of chlormequat and mepiquat in grain--results from the Danish National Pesticide Survey.  

UK PubMed Central (United Kingdom)

The objective of the present work was to establish information on chlormequat and mepiquat residues in grain for human consumption. Chlormequat (2-chloro-N,N,N-trimethylethylammonium, CAS RN 7003-89-6) and mepiquat (1,1-dimethylpiperidinium, CAS RN 15302-91-7) are plant growth regulators used to stabilize stalks in cereals. The study was part of the Danish National Pesticide Survey, managed by the Danish Veterinary and Food Administration. Samples were collected in autumn 1997. Residue contents were determined with a newly developed liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method for chlormequat analysis. The method was extended to include mepiquat in the present study. Quantitation was done by the internal standards method, using mass chromatograms of the most intense daughter ions of mepiquat (m/z 98), chlormequat (m/z 58), and [13C]-chlormequat (m/z 61, internal standard). For chlormequat, the overall limit of detection (LD) was 6 micrograms/kg and the limit of determination (LOD) was 10 micrograms/kg. For mepiquat, LD was 2 micrograms/kg and LOD was 3 micrograms/kg. Of 77 samples analyzed, 51 contained chlormequat and 11 contained mepiquat. The highest levels of chlormequat were found in samples of oatmeal (3.76 mg/kg) and rye (1.08 mg/kg). In 9 rye grain samples containing chlormequat, 5 also contained mepiquat. However, in all samples analyzed, the residues of chlormequat and mepiquat were below maximum residue limits.

Juhler RK; Vahl M

1999-03-01

215

Residues of chlormequat and mepiquat in grain--results from the Danish National Pesticide Survey.  

Science.gov (United States)

The objective of the present work was to establish information on chlormequat and mepiquat residues in grain for human consumption. Chlormequat (2-chloro-N,N,N-trimethylethylammonium, CAS RN 7003-89-6) and mepiquat (1,1-dimethylpiperidinium, CAS RN 15302-91-7) are plant growth regulators used to stabilize stalks in cereals. The study was part of the Danish National Pesticide Survey, managed by the Danish Veterinary and Food Administration. Samples were collected in autumn 1997. Residue contents were determined with a newly developed liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method for chlormequat analysis. The method was extended to include mepiquat in the present study. Quantitation was done by the internal standards method, using mass chromatograms of the most intense daughter ions of mepiquat (m/z 98), chlormequat (m/z 58), and [13C]-chlormequat (m/z 61, internal standard). For chlormequat, the overall limit of detection (LD) was 6 micrograms/kg and the limit of determination (LOD) was 10 micrograms/kg. For mepiquat, LD was 2 micrograms/kg and LOD was 3 micrograms/kg. Of 77 samples analyzed, 51 contained chlormequat and 11 contained mepiquat. The highest levels of chlormequat were found in samples of oatmeal (3.76 mg/kg) and rye (1.08 mg/kg). In 9 rye grain samples containing chlormequat, 5 also contained mepiquat. However, in all samples analyzed, the residues of chlormequat and mepiquat were below maximum residue limits. PMID:10191539

Juhler, R K; Vahl, M

216

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

UK PubMed Central (United Kingdom)

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

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

2012-01-01

217

Fast screening of pesticide residues in fruit juice by solid-phase microextraction and gas chromatography-mass spectrometry  

UK PubMed Central (United Kingdom)

A new vanguard-rearguard analytical method for determining 54 pesticide residues in different fruit juices (natural and commercial orange, peach and pineapple juices were tested) is proposed. For that, in a first step, a fast screening (vanguard) method is applied for detecting those samples containing pesticides at concentrations above a pre-established cut-off value. In a second step, those samples are re-analyzed by a conventional pesticide residue (rearguard) method that confirms the presence of the pesticides and quantifies them. The sample process is very simple, fast and semiautomatic and therefore, it reduces significantly the average time required per sample, increases precision and minimizing human mistakes. Only 1 mL of juice sample is required for analysis. Pesticides are quickly extracted with ethyl acetate in a test tube, transferred to a mixture water:acetone 9:1 (v/v), and isolated by solid-phase microextraction (SPME). The SPME screening method only requires 10 min of SPME extraction. The SPME confirming/quantifying method requires 55 min of SPME extraction. The instrumental determination is carried out by gas chromatography-mass spectrometry (GC-MS) using a full scan acquisition mode for the screening method (less than 17 min of chromatographic run) and a tandem mass spectrometry (MS/MS) acquisition mode for the quantifying/confirming method (less than 70 min of chromatographic run). The use of full scan MS and tandem MS for the detection increase significantly the certainty of the results. Also, the combination of a solvent and SPME extractions and GC-MS/MS offers a significant selectivity and sensitivity with a proven reduction of false positive and negative cases. The use of a vanguard-rearguard strategy can reduce the 50% of the total time required for determining routinely juices in a laboratory by a traditional strategy (identification, confirmation and quantitation of the pesticides in the samples by a conventional analytical method).

Corte?s-Aguado S; Sa?nchez-Morito N; Arrebola FJ; Garrido Frenich A; Marti?nez Vidal JL

2008-04-01

218

Determination of pesticide residues in fruits and vegetables in Islamabad market.  

Science.gov (United States)

Pesticide residues in fruits and vegetable from Islamabad market, Pakistan were determined by GLC using Perkin Elmer Autosystem equipped with 63NECD and capillary column. Dimethoate was determined in the quantity of 0.032 mg kg-1 in apple, 0.110 mg kg-1 in banana, 0.004 mg kg-1 in brinjal, 1.80 mg kg-1 in cauliflower and 0.13 mg kg-1 in arvi, fenvalerate 0.010 mg kg-1 in apple and chlorpyrifos 0.004 mg kg-1 in brinjal. The importance of these pesticide residues with reference to human health is also briefly discussed. PMID:11480355

Tahir, S; Anwar, T; Ahmad, I; Aziz, S; Mohammad, A; Ahad, K

2001-01-01

219

Determination of pesticide residues in fruits and vegetables in Islamabad market.  

UK PubMed Central (United Kingdom)

Pesticide residues in fruits and vegetable from Islamabad market, Pakistan were determined by GLC using Perkin Elmer Autosystem equipped with 63NECD and capillary column. Dimethoate was determined in the quantity of 0.032 mg kg-1 in apple, 0.110 mg kg-1 in banana, 0.004 mg kg-1 in brinjal, 1.80 mg kg-1 in cauliflower and 0.13 mg kg-1 in arvi, fenvalerate 0.010 mg kg-1 in apple and chlorpyrifos 0.004 mg kg-1 in brinjal. The importance of these pesticide residues with reference to human health is also briefly discussed.

Tahir S; Anwar T; Ahmad I; Aziz S; Mohammad A; Ahad K

2001-01-01

220

[Study on experiment of fluorescence spectra detection of pesticide residue of imidacloprid in apple juices].  

UK PubMed Central (United Kingdom)

The fluorescence properties of imidacloprid was studied based on the basic theory that organic molecules can emit fluorescence as they are excited by rays. The fluorescence spectra were obtained under the condition of different content of imidacloprid in apple juices and pure apple juices respectively through fluorescence spectrometer, and the relation between their fluorescence intensity and content of imidacloprid was analyzed. The experiment results show that the most intensive fluorescence (373 nm) was found in the spectrum of imidacloprid, while the fluorescence was not found in the pure apple juices with 234 nm as the excitation wavelength. Then the imidacloprid solution was added to the fruit juices increasingly. The best prediction model was obtained for the contend of imidacloprid in the apple juices, the coefficient of determination is 0.99674, and the accuracy is higher than 90%. As a result, it is fast and feasible to carry out the detection and analysis of the pesticide residue of imidacloprid in the apple juices.

Ji RD; Zhao ZM; Zhang L; Ji L; Zhang JH; Shen LB; Lan XF

2013-03-01

 
 
 
 
221

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

Science.gov (United States)

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

Stoner, Kimberly A.; Eitzer, Brian D.

2013-01-01

222

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

Science.gov (United States)

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

Stoner, Kimberly A; Eitzer, Brian D

2013-10-15

223

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

Science.gov (United States)

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

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

2012-07-03

224

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

UK PubMed Central (United Kingdom)

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

S?owik-Borowiec M; Szpyrka E; Walorczyk S

2012-09-01

225

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

Directory of Open Access Journals (Sweden)

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

Crentsil Kofi Bempah; Jacob Asomaning; Juliana Boateng

2012-01-01

226

[Assessment of the chronic risk for ingestion of pesticide residues in the Brazilian diet  

UK PubMed Central (United Kingdom)

OBJECTIVE: To conduct a chronic dietary risk assessment of the pesticides registered in Brazil up until 1999. METHODS: The Theoretical Maximum Daily Intake (TMDI) for each pesticide was calculated using the Brazilian maximum residue limits and food consumption data from IBGE, the Brazilian Statistical Institute. The risk characterization was done comparing the TMDI with the acceptable daily intakes (ADI) from other countries and from the Codex Alimentarius. RESULTS: The TMDI was higher than the ADI (%ADI>100) at least in one Brazilian metropolitan region for 23 pesticides. Sixteen compounds are organophosphate insecticides, with methyl parathion having the TMDI exceeding the most toxicological parameter (%ADI N=9,300). Rice, beans, citrus and tomato were the commodities which most contributed to the ingestion. From the compounds under higher risk, only 6 were registered according to the Law 98.816/90, which concerns the use of pesticides in the country. CONCLUSIONS: The compounds identified in the study as presenting a potential health concern to the Brazilian consumers, and the commodities which most contributed to the ingestion, should be prioritized by the government in pesticide residue monitoring programs and in the re-registration process. In addition, residue data in food as consumed, processing factors and appropriate consumption data should be generated to allow further studies.

Caldas ED; de Souza LC

2000-10-01

227

Optical instrument development for detection of pesticide residue in apple surface  

Science.gov (United States)

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

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

2013-05-01

228

Simultaneous and rapid detection of multiple pesticide and veterinary drug residues by suspension array technology.  

UK PubMed Central (United Kingdom)

Suspension array technology is proposed for the simultaneous quantitative determination of seven kinds of pesticide and veterinary drug residues, namely, atrazine, chloramphenicol, carbaryl, clenbuterol, 17-?-estradiol, imidacloprid, and tylosin. The assay is simple and can be accomplished within 2h without repeated pumping and washing steps unlike conventional suspension arrays. The hapten-protein conjugate-coated beads bind to their complementary biotinylated antibodies using a competitive immunoassay format. The coefficients of determination R(2) for six targets were greater than 0.992, whereas that for atrazine was 0.961, which indicate good logistic correlations. The dynamic ranges for the seven targets in the 7-plex assay ranged from 2 log units to 4 log units(1.60×10(0)-1.64×10(3), 5.12×10(-2)-1.60×10(2), 1.00×10(0)-3.13×10(3), 4.00×10(-1)-4.10×10(2), 4.00×10(-1)-4.10×10(2), 5.12×10(-2)-1.60×10(2), and 2.00×10(0)-4.00×10(2)ngmL(-1)). The minimum detection concentrations of chloramphenicol, carbaryl, clenbuterol and 17-?-estradiol in the suspension array (0.05, 1.00, 0.40 and 0.40 ng mL(-1)) were lower than the corresponding limits of detection (0.25, 6.60, 24.23 and 13.96 ng mL(-1)) of using an indirect competitive enzyme-linked immunosorbent assay. Environmental scanning electron microscope was employed to characterize the bead surface, which directly confirmed the reactions on the beads. The suspension array is more flexible and feasible than ELISA for the fast quantitative analysis of pesticide and veterinary drug residues.

Liu N; Gao Z; Ma H; Su P; Ma X; Li X; Ou G

2013-03-01

229

Health risks associated with pesticide residues in sediments, fish, and plants from the Oueme Valley in the Republic of Benin.  

UK PubMed Central (United Kingdom)

To determine possible human and environmental health risks, organochlorine pesticide residues were determined in vegetables grown in floodplains along the Ouémé River near Lowé in Bénin. Testing of vegetables found 13 pesticides with ?DDT, ?-endosulfan, ?drin, and lindane being most important. The same pesticides were also detected in plants eaten by bovine cattle, sheep, and herbivorous fish. Human pesticide intake by vegetable consumption was compared with tolerable daily intake (TDI) values reported by the World Health Organization. Pesticide intake by fish consumption was estimated from residue levels in whole fish collected from the Ouémé River in 2004 and reported earlier. Fish consumption does not pose a risk for human health, but consuming vegetables that contain pesticide residues may lead to exceedance of TDI values. Based on these findings, concerns are warranted, and more work is needed to understand the full exposure profile for the local population.

Yehouenou A Pazou E; Azehoun JP; Aléodjrodo PE; van Straalen NM; van Hattum B; van Gestel CA

2013-08-01

230

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

UK PubMed Central (United Kingdom)

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.

Muhammad F; Awais MM; Akhtar M; Anwar MI

2013-01-01

231

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

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 in...

Uthuppu, Basil; Kostesha, Natalie; Jakobsen, Mogens Havsteen; Kiersgaard, S M; Aamand, J; Jorgensen, C

232

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

A study was conducted to investigate the organochlorine, organophosphorus and synthetic pyrethroid pesticide residues in fruits and vegetables from markets in Ghana. For this purpose, a total of 309 fruits and vegetable samples, were collected and analyzed by gas chromatography with electron captur...

Crentsil Kofi Bempah; Jacob Asomaning; Juliana Boateng

233

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

Abstract Two varieties of melons (Cucumis melo) were treated by two fungicides (carbendazim and maneb) and four insecticides (acetamiprid, cyromazin, imazalil and thiamethoxam) to quantify the effect of household processing on the pesticide residues. To ensure sufficiently high levels of re...

234

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

Science.gov (United States)

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

Lorenzin, Michele

235

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

UK PubMed Central (United Kingdom)

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

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

2012-08-01

236

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

UK PubMed Central (United Kingdom)

Monitoring pesticide residues in tropical fruits is of great interest for many countries, e.g., from South America, that base an important part of their economy on the exportation of these products. In this work, a LC-MS/MS multi-residue method using a triple quadrupole analyzer has been developed for around 30 pesticides in seven Colombian tropical fruits of high commercial value for domestic and international markets (uchuva, tamarillo, granadilla, gulupa, maracuya, papaya, and pithaya). After sample extraction with acetonitrile, an aliquot of the extract was diluted with water and directly injected into the HPLC-MS/MS system (electrospray interface) without any cleanup step. The formation of sodium adducts-of poor fragmentation-was minimized using 0.1% formic acid in the mobile phase, which favored the formation of the protonated molecule. However, the addition of ammonium acetate made the formation of the ammonium adducts in some particular cases possible, avoiding the presence of the sodium adducts. The highest sensitivity was observed in positive electrospray ionization for the wide majority of pesticides, with a few exceptions for acidic compounds that gave better response in the negative mode (e.g., 2,4-D, fluazinan). Thus, simultaneous acquisition on the positive/negative mode was applied. Two MS/MS transitions were acquired for each compound to ensure a reliable quantification and identification of the compounds detected in samples, although for malathion a third transition was acquired due to the presence of interfering isobaric compounds in the sample extracts. A detailed study of matrix effects was made by a comparison of standards in solvent and in matrix. Both ionization suppression and ionization enhancement were observed depending on the analyte/matrix combination tested. Correction of matrix effects was made by the application of calibration in matrix. Three matrices were selected (uchuva, maracuya, gulupa) to perform matrix calibration in the analysis of all seven fruit varieties studied. The method was validated by recovery experiments in samples spiked at two levels (0.05 and 0.5 mg/kg). The data were satisfactory for the wide majority of analyte/matrix combinations, with most recoveries between 70% and 110% and the RSD below 15%. Several samples collected from the market were finally analyzed. Positive findings were confirmed by evaluating the experimental Q/q ratios and retention times, and comparing them with those of reference standards.

Botero-Coy AM; Marín JM; Ibáñez M; Sancho JV; Hernández F

2012-03-01

237

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

Science.gov (United States)

Monitoring pesticide residues in tropical fruits is of great interest for many countries, e.g., from South America, that base an important part of their economy on the exportation of these products. In this work, a LC-MS/MS multi-residue method using a triple quadrupole analyzer has been developed for around 30 pesticides in seven Colombian tropical fruits of high commercial value for domestic and international markets (uchuva, tamarillo, granadilla, gulupa, maracuya, papaya, and pithaya). After sample extraction with acetonitrile, an aliquot of the extract was diluted with water and directly injected into the HPLC-MS/MS system (electrospray interface) without any cleanup step. The formation of sodium adducts-of poor fragmentation-was minimized using 0.1% formic acid in the mobile phase, which favored the formation of the protonated molecule. However, the addition of ammonium acetate made the formation of the ammonium adducts in some particular cases possible, avoiding the presence of the sodium adducts. The highest sensitivity was observed in positive electrospray ionization for the wide majority of pesticides, with a few exceptions for acidic compounds that gave better response in the negative mode (e.g., 2,4-D, fluazinan). Thus, simultaneous acquisition on the positive/negative mode was applied. Two MS/MS transitions were acquired for each compound to ensure a reliable quantification and identification of the compounds detected in samples, although for malathion a third transition was acquired due to the presence of interfering isobaric compounds in the sample extracts. A detailed study of matrix effects was made by a comparison of standards in solvent and in matrix. Both ionization suppression and ionization enhancement were observed depending on the analyte/matrix combination tested. Correction of matrix effects was made by the application of calibration in matrix. Three matrices were selected (uchuva, maracuya, gulupa) to perform matrix calibration in the analysis of all seven fruit varieties studied. The method was validated by recovery experiments in samples spiked at two levels (0.05 and 0.5 mg/kg). The data were satisfactory for the wide majority of analyte/matrix combinations, with most recoveries between 70% and 110% and the RSD below 15%. Several samples collected from the market were finally analyzed. Positive findings were confirmed by evaluating the experimental Q/q ratios and retention times, and comparing them with those of reference standards. PMID:21983979

Botero-Coy, A M; Marín, J M; Ibáñez, M; Sancho, J V; Hernández, F

2011-10-08

238

De-contamination of pesticide residues in food by ionizing radiation  

International Nuclear Information System (INIS)

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

1144-01-00

239

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

Directory of Open Access Journals (Sweden)

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

Puneeta Pandey; P.S. Khillare; Krishan Kumar

2011-01-01

240

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

DEFF Research Database (Denmark)

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

Poulsen, Mette E.; Wenneker, Marcel

2012-01-01

 
 
 
 
241

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

UK PubMed Central (United Kingdom)

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

Poulsen ME; Wenneker M; Withagen J; Christensen HB

2012-05-01

242

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

Science.gov (United States)

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

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

2012-10-11

243

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

UK PubMed Central (United Kingdom)

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

Gebremichael S; Birhanu T; Tessema DA

2013-02-01

244

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

Directory of Open Access Journals (Sweden)

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

Botwe, B. O.; Ntow, W. J.; Kelderman, P.; Drechsel, P.; Professor Derick Carboo; Professor Vincent K. Nartey; Gijzen, H. J.

2011-01-01

245

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

Directory of Open Access Journals (Sweden)

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

M Shokerzadeh; H Vahedi; B Shabankhani

2006-01-01

246

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

International Nuclear Information System (INIS)

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

2008-01-01

247

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

UK PubMed Central (United Kingdom)

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

Ikeura H; Hamasaki S; Tamaki M

2013-05-01

248

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

Science.gov (United States)

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

Ikeura, Hiromi; Hamasaki, Sadahiro; Tamaki, Masahiko

2012-11-10

249

What we know, don't know, and need to know about pesticide residues in food.  

UK PubMed Central (United Kingdom)

Factors contributing to growing public concern about pesticide residues are assessed, with special focus on the need for more accurate and credible exposure assessments. Current knowledge about residues is examined, and found incomplete. The critical need for a resolution of uncertainty over the risk standard governing the setting of "safe" tolerances is highlighted, along with a number of technical issues and assumptions in the risk assessment process. Criteria for the targeting of residue monitoring activities are suggested as one viable option to more effectively protect the public's health.

Benbrook CM

1991-01-01

250

Organochlorine pesticide residues in animals of Tasmania, Australia-1975-77.  

UK PubMed Central (United Kingdom)

Animals taken in Tasmania including duck (Anas superciliosa), eel (Anguilla australis), English perch (Perca fluviatilis), white-faced heron (Ardea pacifica), brown trout (Salmo trutta), European starling (Strunus vulgaris), cat (Felis cattus), cormorant (Phalacrocorax sp.), mutton bird (Puffinus tenuirostris), Tasmanian devil (Sarcophilus harrisii), rainbow trout (Salmo gairdnerii), Tasmanian raven (Corvus mellori), tench (Tinca tinca), and quail (Coturnix sp.) were sampled for p,p'-DDE, pp,p'-TDE, p,p'-DDT, lindane, dieldrin, and hexachlorobenzene. Pesticide residue levels exceeded 0.1 ppm in at least one animal from each area and in the majority of animals sampled from all areas. Pesticide sources could not be determined, partly because migratory species such as ducks, mutton birds, cormorants, and eels may have ingested pesticides outside of Tasmania.

Bloom H; Taylor W; Bloom WR; Ayling GM

1979-12-01

251

Organochlorine pesticide residues in animals of Tasmania, Australia-1975-77.  

Science.gov (United States)

Animals taken in Tasmania including duck (Anas superciliosa), eel (Anguilla australis), English perch (Perca fluviatilis), white-faced heron (Ardea pacifica), brown trout (Salmo trutta), European starling (Strunus vulgaris), cat (Felis cattus), cormorant (Phalacrocorax sp.), mutton bird (Puffinus tenuirostris), Tasmanian devil (Sarcophilus harrisii), rainbow trout (Salmo gairdnerii), Tasmanian raven (Corvus mellori), tench (Tinca tinca), and quail (Coturnix sp.) were sampled for p,p'-DDE, pp,p'-TDE, p,p'-DDT, lindane, dieldrin, and hexachlorobenzene. Pesticide residue levels exceeded 0.1 ppm in at least one animal from each area and in the majority of animals sampled from all areas. Pesticide sources could not be determined, partly because migratory species such as ducks, mutton birds, cormorants, and eels may have ingested pesticides outside of Tasmania. PMID:537866

Bloom, H; Taylor, W; Bloom, W R; Ayling, G M

1979-12-01

252

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

International Nuclear Information System (INIS)

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

1999-01-01

253

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

UK PubMed Central (United Kingdom)

Pesticides are among the most widely used chemicals in the world. Because of the widespread use of agricultural chemicals in food production, people are exposed to low levels of pesticide residues through their diets. Scientists do not yet have a total understanding of the health effects of these pesticide residues. This work aims to determine differences in terms of pesticide residue content in Portuguese strawberries grown using different agriculture practices. The Quick, Easy, Cheap, Effective, Rugged, and Safe sample preparation method was conducted and shown to have good performance for multiclass pesticides extraction in strawberries. The screening of 25 pesticides residue was performed by gas chromatography-tandem mass spectrometry. In quantitative validation, acceptable performances were achieved with recoveries of 70-120 and <12 % residual standard deviation for 25 pesticides. Good linearity was obtained for all the target compounds, with highly satisfactory repeatability. The limits of detection were in the range of 0.1-28 ?g/kg. The method was applied to analyze strawberry samples from organic and integrated pest management (IPM) practices harvested in 2009-2010. The results showed the presence of fludioxonil, bifenthrin, mepanipyrim, tolylfluanid, cyprodinil, tetraconazole, and malathion when using IPM below the maximum residue levels.

Fernandes VC; Domingues VF; Mateus N; Delerue-Matos C

2012-11-01

254

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

UK PubMed Central (United Kingdom)

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

Watanabe E; Kobara Y; Yogo Y

2012-09-01

255

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

Science.gov (United States)

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

Watanabe, Eiki; Kobara, Yuso; Yogo, Yasuhiro

2012-09-04

256

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

Science.gov (United States)

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

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

2013-04-01

257

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

Directory of Open Access Journals (Sweden)

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

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

2009-01-01

258

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

Scientific Electronic Library Online (English)

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

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

2009-01-01

259

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

UK PubMed Central (United Kingdom)

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

Lazartigues A; Thomas M; Cren-Olivé C; Brun-Bellut J; Le Roux Y; Banas D; Feidt C

2013-01-01

260

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

Science.gov (United States)

Residues of pesticides in fish farming productions from barrage ponds are seldom studied in spite of increasing health questionings and environmental concerns. The purpose of this study is to establish the pesticide contamination profiles of sediments and edible fish from five ponds in Northeastern France. Multi-residues method and liquid chromatography-tandem mass spectrometry analysis were used to quantify 13 pesticides (azoxystrobin, carbendazim, clomazone, diflufenican, dimethachlor, fluroxypyr, iprodion, isoproturon, mesosulfuron-methyl, metazachlor, napropamid, quizalofop and thifensulfuron-methyl). Ten sediments and 143 muscles samples were analysed, corresponding to two successive fishing campaigns (first fishing date and second fishing date (P2), about 1 year later) on five sites (noted C-0, C-25, C-45, C-75 and C-85 to express the increasing gradient of crop area). Isoproturon was present in all sediments samples (1.8-56.4 ?g/kg dry weight). During P2 period, carbendazim was quantified in the fish of site C-0 (0.09 ± 0.02, 0.2 ± 0.1 and 0.17 ± 0.06 ?g/kg wet weight (ww) for roach, carp and perch, respectively). Metazachlor was only quantified in perch of the site C-25 (0.13 ± 0.02 ?g/kg ww). Concentrations of isoproturon were similar for the sites C-45 and C-75 with 0.4 ± 0.1 and 0.75 ± 0.06 ?g/kg ww for carp and perch, respectively. Contamination of fish reflected generally concentrations in surroundings. Isoproturon was the most concentrated and its main source was water for perch while carp was exposed through both water and sediments, highlighting their life strategies in pond. PMID:22961490

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

2012-09-08

 
 
 
 
261

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

Directory of Open Access Journals (Sweden)

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

Ademola F. Aiyesanmi; Gideon A. Idowu

2012-01-01

262

Further studies on the bound pesticide residues in soil and plants  

International Nuclear Information System (INIS)

[en] The data presented in this paper demonstrate that the various physiological groups of microbes used in this study have the enzymatic and/or biological potential to release bound pesticide residues from soil. The release was not influenced by the nature of the microbial population present, thereby indicating that the process involved cometabolism or that the residues are bound in various matrices, or both. Our studies also indicate that the in vitro incubation of chicken liver homogenate with plant tissues containing bound 14C residues released and metabolized some of these residues. However, no apparent release of 14C residues was observed when the incubation involved rumen liquor. It appears that in the liver homogenate incubation system, bound 2-chloro dealkylated metabolites in the plant tissues were released and subsequently metabolized to 2-hydroxy analogues

1984-01-01

263

Pesticide residues in food-based proficiency test materials, spiking values versus consensus assigned values.  

Science.gov (United States)

We examine the differences among the three estimates of the true value of the measurand derived from routine proficiency testing of laboratories analyzing foodstuffs for pesticide residues. The three values are (i) the spike level (Sp), (ii) the mean result found by the laboratory conducting the test for sufficient homogeneity (Ho), and (iii) the consensus of the participants' results used as the assigned value (AV) in converting results into z scores. Data amounting to 205 examples were collected from successive rounds of three series of proficiency tests from the Food Analysis Performance Assessment Scheme (FAPAS): namely, series 05 (fats, oils, and animal products), series 09 (cereals and their products), and series 19 (fruits, vegetables, and their products). Irrespective of the class of test material, we found that the means of AV and Ho were almost identical, while the value of Sp was systematically higher than AV by a factor of 1.22. The dispersion of the individual values of both ratios, Ho/AV and Sp/AV, was examined by analysis of variance. A small part of the variance was attributed to the series, but a greater part, about 40%, was attributed to individual rounds within series. We discovered no connection between the ratios and the chemistry of the analyte. PMID:23631620

Sykes, Mark; Thompson, Michael; Reynolds, Stewart

2013-04-30

264

Analysis of 118 Pesticides in Tobacco after Extraction With the Modified QuEChRS Method by LC-MS-MS.  

UK PubMed Central (United Kingdom)

A liquid chromatography-tandem quadrupole mass spectrometry (LC-MS-MS) multi-residue method for the simultaneous target analysis of a wide range of pesticides in tobacco has been developed. Gradient elution has been used in conjunction with positive mode electrospray ionization tandem mass spectrometry to detect up to 118 pesticides in tobacco. The recoveries obtained for each pesticide ranged between 70 and 118% at two spiked concentration levels. Good linear relationships were observed with correlation coefficients r(2) > 0.992 for all analytes. The established method was successfully applied to the determination of pesticide residues in real tobacco samples in order to validate the suitability for routine analysis.

Yang F; Bian Z; Chen X; Liu S; Liu Y; Tang G

2013-07-01

265

Potassium-boron-selenium fertilizer capable of promoting growth of fruit trees and degrading residual pesticide  

UK PubMed Central (United Kingdom)

The invention discloses a potassium-boron-selenium fertilizer capable of promoting the growth of fruit trees and degrading residual pesticide. Seleninic acid is neutralized by potassium hydroxide, so that potassium selenite is obtained diboron trioxide is dissolved in water, and is mixed with the potassium selenite, and thereby potassium-boron-selenium reagent with the PH value between 7.0 and 8.8 is prepared. The potassium-boron-selenium fertilizer has the multiple fertilizer effects of selenium fertilizer and conventional potash fertilizer and boron fertilizer, and when the potassium-boron-selenium fertilizer is sprayed on the surfaces of the leaves of fruit trees, not only can the fruit-setting rate be increased, but also residual pesticide can be degraded and the selenium content of fruits can be increased.

BAITAO YU

266

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

UK PubMed Central (United Kingdom)

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

Gutiérrez R; Ruíz JL; Ortiz R; Vega S; Schettino B; Yamazaki A; de Lourdes Ramírez M

2012-10-01

267

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

Science.gov (United States)

Thirty six samples of bovine milk were collected from Chiapas State, Mexico between January 2011 and December 2011 with the intention of identifying and quantifying organochlorine pesticide residues in organic farms. The analyses were done using gas chromatography with an electron capture detector (Ni(63)). In general the values found in raw milk were lower than the permissible limit proposed by FAO/WHO/Codex Alimentarius 2006. Average concentrations for alpha + beta HCH were 3.62 ng/g, gamma HCH 0.34 ng/g, heptachlor + epoxide 0.67 ng/g, DDT and isomers 1.53 ng/g, aldrin + dieldrin 0.77 ng/g, and endrin 0.66 ng/g (only present in samples from farm 2). The organic milk from Chiapas has shown low concentrations of pesticide residues in recent years and satisfies international and national regulations for commercialization. PMID:22864634

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

2012-08-05

268

Extraction and detection of pesticide residues from air filter inserts using supercritical carbon dioxide  

Energy Technology Data Exchange (ETDEWEB)

Trace quantities of airborne herbicide residues were collected on adsorbent bed cartridges and were subsequently extracted from the adsorbent using supercritical carbon dioxide. An apparatus was constructed to facilitate the extraction and recovery of the desired analytes. The resulting extracts were analyzed using gas chromatography/mass spectrometry (GC/MS) or high performance liquid chromatography (HPLC) techniques. Results are presented for a series of analytes representative of common commercial pesticides or herbicides.

Zemanian, T.S.; Robins, W.H.; Lee, R.N.; Wright, B.W.

1994-10-01

269

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

UK PubMed Central (United Kingdom)

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

Takatori S; Yamamoto H; Fukui N; Yamaguchi S; Kitagawa Y; Kakimoto Y; Osakada M; Okihashi M; Kajimura K; Obana H

2013-01-01

270

Degradation bacteria for removing fomesafen pesticide residue and microbial inoculum prepared by same  

UK PubMed Central (United Kingdom)

The invention provides a degradation microbial inoculum for removing fomesafen pesticide residue, which belongs to the high-technical field of biology. Gram-positive bacteria ZB-1 are used as a bacterial strain which is a bacillus (Bacillus sp.) by identification. The bacillus has the main biological characteristic of G<+>, a thalli is in the shape of a brevibacterium, and the size of the thalli is 0.5-1.0*1.5-5.0 microns, the gonite is round, and the bacillus is positive by catalase reaction, gelatin hydrolization and phenylalanine deaminase the bacillus is negative by V-P reaction, M.R reaction, nitrate reaction, starch hydrolization and tyrosine hydrolization. The culture fluid which is obtained after the ZB-1 strain is fermented is the microbial inoculum. By using the degradation bacteria product, the pesticide residue of fomesafen in the earth is reduced by more than 67 percent, and the overproof problem of the fomesafen pesticide residue can be solved in agricultural production.

SHUNPENG LI; BO LIANG; XING HUANG; ZHAOZHONG FENG; JIQUAN SUN

271

Evaluation of pesticide residues in farmgate samples of vegetables in Karnataka, India.  

UK PubMed Central (United Kingdom)

Fifty Vegetable samples (Beans, Brinjal, Cabbage and Carrot) grown in Kolar district of Karnataka, India were analysed for 20 pesticide residues by gas liquid chromatography equipped with ECD and FTD. Recovery studies were performed at 0.1, 0.5 and 1.0 mg kg(-1) fortification levels of each compound and the recoveries obtained ranged from 73.0% to 96.6% with relative standard deviations lower than 7.5%. The method showed good linearity over the range assessed 0.01-1.0 mg Kg(-1) with correlation coefficient >0.998 and the detection and quantification limits for the pesticides studied varied from 0.0001 to 0.002 mg Kg(-1) and 0.0001-0.001 mg Kg(-1), respectively. All the samples were found to be contaminated, the organo chlorines (97%) dominated followed by organophosphates (83%) and pyrethroids (60%). However, 58% of the samples were found to contain the residues of these insecticides above their respective maximum residue limits (MRL). It is therefore proposed to perform extensive monitoring studies covering all the vegetable crops from different agro-climatic regions of the Karnataka to know the exact status of pesticide contamination.

Ananda Gowda SR; Somashekar RK

2012-09-01

272

Evaluation of pesticide residues in farmgate samples of vegetables in Karnataka, India.  

Science.gov (United States)

Fifty Vegetable samples (Beans, Brinjal, Cabbage and Carrot) grown in Kolar district of Karnataka, India were analysed for 20 pesticide residues by gas liquid chromatography equipped with ECD and FTD. Recovery studies were performed at 0.1, 0.5 and 1.0 mg kg(-1) fortification levels of each compound and the recoveries obtained ranged from 73.0% to 96.6% with relative standard deviations lower than 7.5%. The method showed good linearity over the range assessed 0.01-1.0 mg Kg(-1) with correlation coefficient >0.998 and the detection and quantification limits for the pesticides studied varied from 0.0001 to 0.002 mg Kg(-1) and 0.0001-0.001 mg Kg(-1), respectively. All the samples were found to be contaminated, the organo chlorines (97%) dominated followed by organophosphates (83%) and pyrethroids (60%). However, 58% of the samples were found to contain the residues of these insecticides above their respective maximum residue limits (MRL). It is therefore proposed to perform extensive monitoring studies covering all the vegetable crops from different agro-climatic regions of the Karnataka to know the exact status of pesticide contamination. PMID:22825007

Ananda Gowda, S R; Somashekar, R K

2012-07-24

273

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

International Nuclear Information System (INIS)

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

2011-01-01

274

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

Science.gov (United States)

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

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

2009-12-01

275

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

UK PubMed Central (United Kingdom)

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

Singh SB; Mukherjee I; Maisnam J; Kumar P; Gopal M; Kulshrestha G

2009-12-01

276

Prediction of the processing factor for pesticides in apple juice by principal component analysis and multiple linear regression.  

UK PubMed Central (United Kingdom)

The main objective of this work was to establish a mathematical function that correlates pesticide residue levels in apple juice with the levels of the pesticides applied on the raw fruit, taking into account some of their physicochemical properties such as water solubility, the octanol/water partition coefficient, the organic carbon partition coefficient, vapour pressure and density. A mixture of 12 pesticides was applied to an apple tree; apples were collected after 10 days of application. After harvest, apples were treated with a mixture of three post-harvest pesticides and the fruits were then processed in order to obtain apple juice following a routine industrial process. The pesticide residue levels in the apple samples were analysed using two multi-residue methods based on LC-MS/MS and GC-MS/MS. The concentration of pesticides was determined in samples derived from the different steps of processing. The processing factors (the coefficient between residue level in the processed commodity and the residue level in the commodity to be processed) obtained for the full juicing process were found to vary among the different pesticides studied. In order to investigate the relationships between the levels of pesticide residue found in apple juice samples and their physicochemical properties, principal component analysis (PCA) was performed using two sets of samples (one of them using experimental data obtained in this work and the other including the data taken from the literature). In both cases the correlation was found between processing factors of pesticides in the apple juice and the negative logarithms (base 10) of the water solubility, octanol/water partition coefficient and organic carbon partition coefficient. The linear correlation between these physicochemical properties and the processing factor were established using a multiple linear regression technique.

Martin L; Mezcua M; Ferrer C; Gil Garcia MD; Malato O; Fernandez-Alba AR

2013-01-01

277

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

International Nuclear Information System (INIS)

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

2005-01-01

278

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

Science.gov (United States)

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

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

2007-06-01

279

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

UK PubMed Central (United Kingdom)

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.

Ticha J; Hajslova J; Kovalczuk T; Jech M; Honzicek J; Kocourek V; Lansky M; Kloutvorova J; Falta V

2007-06-01

280

Analysis of Coupling the Pesticide Use Reduction with Environmental Policy for Agricultural Sustainability in Taiwan  

Directory of Open Access Journals (Sweden)

Full Text Available As Taiwan has a dense population and only limited natural resources, the government began actively establishing a Taiwan’s sustainable development indicators (TSDI) system in 2003 to evaluate the progress towards sustainability. Commonly used pesticides could pose a risk of causing adverse effects to food sanitation, human health and the environment. Thus, the pesticide usage rate per hectare of farmland and the area of organic cultivation have been selected as agricultural sustainability indicators. The objective of this paper was to describe an analysis of current status of pesticide use and regulatory policy for environmental sustainability in Taiwan. Furthermore, it can be connected with the regulatory infrastructure, which has been established by the joint-venture of the central competent authorities (i.e., Council of Agriculture, Environmental Protection Administration, Department of Health, Ministry of Economic Affairs, and Council of Labor Affairs) for controlling and/or preventing pesticide distribution in the environment. The significant progress is that the residual pesticides have notably declined in the past decade, which was in parallel with the pesticide usage rate decreased and organic farming area increased. For example, total area of organically certified cropping in Taiwan has been increased from 900 hectares (ha) in 2001 to about 4,500 ha in 2010. Finally, some recommendations for the pollution prevention and toxicity reduction of pesticide use were also addressed to progress towards a sustainable agriculture in Taiwan.

Wen-Tien Tsai

2013-01-01

 
 
 
 
281

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

UK PubMed Central (United Kingdom)

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 approximately 3.0 and approximately 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 approximately 7.0 than at pH approximately 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 approximately 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 approximately 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 approximately 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.

Sheng G; Yang Y; Huang M; Yang K

2005-04-01

282

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

Science.gov (United States)

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 approximately 3.0 and approximately 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 approximately 7.0 than at pH approximately 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 approximately 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 approximately 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 approximately 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. PMID:15620591

Sheng, Guangyao; Yang, Yaning; Huang, Minsheng; Yang, Kai

2005-04-01

283

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

Science.gov (United States)

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

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

2011-12-01

284

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

Energy Technology Data Exchange (ETDEWEB)

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.

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

285

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

International Nuclear Information System (INIS)

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

1982-01-01

286

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

International Nuclear Information System (INIS)

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

2002-01-01

287

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

Energy Technology Data Exchange (ETDEWEB)

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

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

2002-12-01

288

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

International Nuclear Information System (INIS)

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

1994-02-04

289

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

Directory of Open Access Journals (Sweden)

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

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

2009-01-01

290

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

Science.gov (United States)

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

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

2009-09-16

291

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

UK PubMed Central (United Kingdom)

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

Nishina T; Kien CN; Noi NV; Ngoc HM; Kim CS; Tanaka S; Iwasaki K

2010-10-01

292

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

UK PubMed Central (United Kingdom)

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

Deng X; Guo Q; Chen X; Xue T; Wang H; Yao P

2014-02-01

293

Organochlorine pesticide residues in blood samples of agriculture and sheep wool workers in Bangalore (rural), India.  

Science.gov (United States)

To describe exposure level of organochlorine pesticides (OCP) among workers occupationally engaged in agriculture and sheep wool associated jobs, the present study was carried out in rural neighborhood of Bangalore city, India. Thirty participants were interviewed and obtained informed consent before blood sample collection. The maximum concentrations of OCP were detected in blood samples of agriculture workers than sheep wool workers. Among the metabolites of HCH and DDT, lindane (?-HCH) and p,p'-DDE were the most contributed to the total OCP. There were no differences in pesticide residues found between sex and work groups. It was observed that about 30% of samples exceeded the tolerance limits of 10 ?g/L prescribed for HCH under the prevention of food adulteration act. Therefore, the present study recommends continuous monitoring with larger sample size. PMID:22323047

Dhananjayan, V; Ravichandran, B; Rajmohan, H R

2012-02-10

294

Organochlorine pesticide residues in blood samples of agriculture and sheep wool workers in Bangalore (rural), India.  

UK PubMed Central (United Kingdom)

To describe exposure level of organochlorine pesticides (OCP) among workers occupationally engaged in agriculture and sheep wool associated jobs, the present study was carried out in rural neighborhood of Bangalore city, India. Thirty participants were interviewed and obtained informed consent before blood sample collection. The maximum concentrations of OCP were detected in blood samples of agriculture workers than sheep wool workers. Among the metabolites of HCH and DDT, lindane (?-HCH) and p,p'-DDE were the most contributed to the total OCP. There were no differences in pesticide residues found between sex and work groups. It was observed that about 30% of samples exceeded the tolerance limits of 10 ?g/L prescribed for HCH under the prevention of food adulteration act. Therefore, the present study recommends continuous monitoring with larger sample size.

Dhananjayan V; Ravichandran B; Rajmohan HR

2012-04-01

295

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

DEFF Research Database (Denmark)

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

Bache, Michael; Taboryski, Rafael Jozef

2011-01-01

296

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

Directory of Open Access Journals (Sweden)

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

Bache Michael; Taboryski Rafael; Schmid Silvan; Aamand Jens; Jakobsen Mogens

2011-01-01

297

Residual gas analysis device  

Energy Technology Data Exchange (ETDEWEB)

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

Thornberg, Steven M. (Peralta, NM)

2012-07-31

298

Potential of ozone utilization for reduction of pesticide residue in food of plant origin. A review.  

UK PubMed Central (United Kingdom)

Residues of plant protection products can be nowadays found in almost all samples of fruits as even if their application was carried out with respect to standards of Good Agricultural Practice. The intake of these compounds with food of plant origin may result in various disorders and diseases. Since the use of plant protection agents seems unavoidable, it is necessary to treat contaminated food material to eliminate or reduce residues content within food products. Ozone is utilized for elimination of biological and chemical contaminants in various environmental matrixes. Since its utilization in food industry has been permitted many experiments were conducted in order to determine its efficiency and side effects on food quality. The goal of this paper is to contribute to a discussion on the ozonization as a process leading to reduction of pesticide residues on plant surface.

Balawejder M; Antos P; Sad?o S

2013-01-01

299

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

Science.gov (United States)

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

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

2013-03-21

300

Multiresidue analysis of pesticides with hydrolyzable functionality in cooked vegetables by liquid chromatography tandem mass spectrometry.  

Science.gov (United States)

It would be preferable for pesticide residues substituted by hydrolyzable functionality to be analyzed after cooking because their structures are apt to degrade during boiling and/or heating. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantitative determination of 44 pesticide residues with hydrolyzable functional group in five typical vegetable widely consumed in Republic of Korea is described. The sample clean-up was carried out according to the method of Food Code No. 83 established by the Korea Food and Drug Administration (KFDA). Zorbox XDB-C(18) column was selected for the analysis because of the best peak separation. The LC mobile phase consisted of water and 5 mm methanolic ammonium formate, which resulted in a peak shape with good symmetry at each run. Tandem mass spectroscopic (MS/MS) experiments were performed in ESI positive mode and the multiple reaction monitoring modes. A conventional matrix effect was modified to more comprehensive form 100gamma(ij) (%). A high matrix effect (thiacloprid, pirimicarb and methabenzthiazuron. The limits of detection were in the range of 0.1-8.1 microg/kg, indicating a good sensitivity. Most of the recoveries ranged from 70 to 131% with RSDs pesticide levels in the cooked vegetable samples. Of the screened pesticide residues, only fluquinconazole and dimethomorph below the maximum residue levels established by the KFDA were detected in onion and cucumber samples. PMID:19360753

Lee, Sung Joong; Park, Semin; Choi, Jin Young; Shim, Jae-Han; Shin, Eun-Ho; Choi, Jeong-Heui; Kim, Soo Taek; Abd El-Aty, A M; Jin, Jong Sung; Bae, Dong Won; Shin, Sung Chul

2009-07-01

 
 
 
 
301

Comparison of solvent extraction and solid-phase extraction for the determination of organochlorine pesticide residues in water.  

UK PubMed Central (United Kingdom)

Solid-phase extraction (SPE) of organochlorine pesticide residues from environmental water samples was evaluated using octadecyl (C18)-bonded porous silica. The efficiency of SPE of these pesticide residues from reagent water samples at 1-5 micrograms dm-3 levels was compared with those obtained by solvent extraction with hexane and Freon TF (trichlorotrifluoroethane). Average recoveries exceeding 80% for these organochlorine pesticides were obtained via the SPE method using small cartridges containing 100 mg of 40 microns C18-bonded porous silica. The average recovery by solvent extraction with hexane and Freon TF exceeded 90% in both instances. It was concluded that the recoveries and precision for the SPE of organochlorine pesticides were poorer than those for the solvent extraction method. Organochlorine pesticide residue levels in environmental water samples from two major rivers flowing through predominantly rice-growing areas were monitored by gas chromatography using the solvent extraction method with hexane. Exceptionally high levels of organochlorine pesticide residues such as BHC, DDT, heptachlor, endosulfan and dieldrin were found in these water samples.

Tan GH

1992-07-01

302

Results from the monitoring of pesticide residues in fruits and vegetables marketed in Piedmont (Italy), 2000-2008.  

UK PubMed Central (United Kingdom)

The Regional Agency for Public Health in Piedmont (Italy) analyzed pesticide residue levels (more than 190 pesticides) from 2000 to 2008 in 4.078 fruit samples, 2.869 vegetable samples from conventional agriculture, and 428 fruit and vegetable samples (2004-2007) from organic agriculture. Residues above the maximum residue levels were found in 4% of the fruit samples, in 2% of the vegetable samples, and in 2% of samples from organic farming. The main purpose of the present work was to evaluate the opportunity to start specific procedures of risk management and prevention strategies along the production chain and the official control.

Zicari G; Soardo V; Cerrato E; Rivetti D

2011-03-01

303

Hair as a marker for pesticides exposure.  

UK PubMed Central (United Kingdom)

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

Smith-Baker C; Saleh MA

2011-01-01

304

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

UK PubMed Central (United Kingdom)

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

Das B; Khan YS; Das P; Shaheen SM

2002-01-01

305

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

Science.gov (United States)

Organochlorine pesticides (p,p'-DDT, p,p'-DDD, p,p'-DDE, aldrin, lindane, and heptachlor) were measured in muscle tissue of catfish (Tachysurus thalassinus) during the dry and wet season. Catfish were collected from the South Patches of the Bay of Bengal during October-December 1997 and May-July 1998. Tissue residues were analyzed by using gas-chromatography (GC) in electron capture detector (ECD) mode and were verified by thin layer chromatography (TLC). The pesticide residues levels were found in order of sigma DDT > Heptachlor > Lindane > Aldrin. Higher levels of pesticide residues were found in all samples during dry season, as compared with the wet season, primarily due to elevated lipid content in fishes. A positive correlation and linear relationship was observed between the pesticide residues (sigmaDDT and sigmaOCs) and lipid content of fishes. However, the concentrations of pesticide residues in the muscle were found to be lower than the FAO/WHO [(1993) Food standards programme. Codex Alimentarius Commission. vol. 9 (4) pp. 149-158] recommended permissible limit for human consumption. PMID:12395837

Das, Biplob; Khan, Yusuf Sharif Ahmed; Das, Pranab; Shaheen, S M

2002-01-01

306

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

Science.gov (United States)

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

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

2010-07-16

307

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

UK PubMed Central (United Kingdom)

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

Srivastava AK; Trivedi P; Srivastava MK; Lohani M; Srivastava LP

2011-05-01

308

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

Scientific Electronic Library Online (English)

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

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

2012-01-01

309

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

UK PubMed Central (United Kingdom)

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

Turgut C; Ornek H; Cutright TJ

2011-02-01

310

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

Directory of Open Access Journals (Sweden)

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

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

2012-01-01

311

Monitoring the Residue Level of Three Selected Pesticides in Red Amaranth  

Directory of Open Access Journals (Sweden)

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

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

2004-01-01

312

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

UK PubMed Central (United Kingdom)

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).

Camino-Sánchez FJ; Zafra-Gómez A; Oliver-Rodríguez B; Ballesteros O; Navalón A; Crovetto G; Vílchez JL

2010-11-01

313

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

Science.gov (United States)

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

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

2010-11-01

314

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

UK PubMed Central (United Kingdom)

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

Witczak A; Abdel-Gawad H

2012-01-01

315

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

Directory of Open Access Journals (Sweden)

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

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

2006-01-01

316

Determination of organochlorine pesticide residues in freshwater fish species in Punjab, India.  

UK PubMed Central (United Kingdom)

The levels of organochlorine pesticides residues were determined in five freshwater fish species in Punjab State, India. These species were selected in view of their importance to local human fish consumer. DDTs were the predominant organochlorine contaminants in all species with pp DDT and pp DDE as the main pollutants. Other organochlorines, such as HCH isomers and dieldrin were also found at lower levels in fish species. The alpha-HCH was the dominant isomer of HCH in all fish species followed by gamma-, beta- and delta-HCH. The residues of aldrin, chlordane, heptachlor and endosulphan were not detected in any fish sample. The levels of organochlorines detected in present study were below the tolerance limits recommended at National and International standards.

Kaur M; Sharma JK; Gill JP; Aulakh RS; Bedi JS; Joia BS

2008-02-01

317

Removal of residual pesticide, fenitrothion, in vegetables by using ozone microbubbles generated by different methods  

UK PubMed Central (United Kingdom)

The effects of ozone microbubbles (OMB) generated by different methods on removal of residual fenitrothion (FT) in three kinds of vegetables were examined. FT-infiltrated lettuce, cherry tomatoes and strawberries were immersed in solutions containing OMB generated by using a microbubble generator of a decompression-type or a gas-water circulating-type combined with an ozone generator at an initial OMB concentration of 2.0ppm for 0, 5 or 10min. Residual FT in each vegetable was removed more efficiently by the OMB treatments with the decompression type than with the gas-water circulation type, showing that the pesticide-removing effect of OMB varies with the method of OMB generation.

Ikeura H; Kobayashi F; Tamaki M

2011-04-01

318

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

Science.gov (United States)

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

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

2012-04-19

319

Application of low-pressure gas chromatography/tandem mass spectrometry to the determination of pesticide residues in tropical fruits.  

Science.gov (United States)

A multiresidue method has been developed for determining pesticide residues in the tropical fruits kiwi, custard apple, and mango. The intended purpose of the method is for regulatory analyses of commodities for pesticides that have established maximum residue limits. A fast and simple extraction method with cyclohexane-ethyl acetate (1 + 1, v/v) and a high-speed homogenizer was optimized. Pressurized liquid extraction was evaluated as an alternative automated extraction technique. The pesticide residues were determined by using low-pressure gas chromatography coupled to tandem mass spectrometry. The proposed methodology was validated for each matrix. Pesticide recoveries ranged from 70 to 110%, with repeatability relative standard deviations of < or = 18% at spiking levels of 12 and 50 microg/kg. The limits of quantitation were in the range of 0.03-6.17 microg/kg, and the limits of detection were between 0.01 and 3.75 microg/kg. Mango can be selected as a representative matrix for calibration on the basis of the results of a potential matrix effect study. The method was successfully applied to the determination of pesticide residues in real samples in Spain. PMID:17760354

Martínez Vidal, José Luis; Fernández Moreno, José Luis; Arrebola Liébanas, Francisco Javier; Garrido Frenich, Antonia

320

Application of low-pressure gas chromatography/tandem mass spectrometry to the determination of pesticide residues in tropical fruits.  

UK PubMed Central (United Kingdom)

A multiresidue method has been developed for determining pesticide residues in the tropical fruits kiwi, custard apple, and mango. The intended purpose of the method is for regulatory analyses of commodities for pesticides that have established maximum residue limits. A fast and simple extraction method with cyclohexane-ethyl acetate (1 + 1, v/v) and a high-speed homogenizer was optimized. Pressurized liquid extraction was evaluated as an alternative automated extraction technique. The pesticide residues were determined by using low-pressure gas chromatography coupled to tandem mass spectrometry. The proposed methodology was validated for each matrix. Pesticide recoveries ranged from 70 to 110%, with repeatability relative standard deviations of < or = 18% at spiking levels of 12 and 50 microg/kg. The limits of quantitation were in the range of 0.03-6.17 microg/kg, and the limits of detection were between 0.01 and 3.75 microg/kg. Mango can be selected as a representative matrix for calibration on the basis of the results of a potential matrix effect study. The method was successfully applied to the determination of pesticide residues in real samples in Spain.

Martínez Vidal JL; Fernández Moreno JL; Arrebola Liébanas FJ; Garrido Frenich A

2007-07-01

 
 
 
 
321

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

UK PubMed Central (United Kingdom)

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

Pareja L; Colazzo M; Pérez-Parada A; Besil N; Heinzen H; Böcking B; Cesio V; Fernández-Alba AR

2012-05-01

322

Pesticide residues in coastal waters affected by rice paddy effluents temporarily stored in a wastewater reservoir in southern Japan.  

UK PubMed Central (United Kingdom)

This paper presents the occurrence, distribution, and environmental impact of pesticide residues in coastal water in southern Japan that receives effluents from a wastewater reservoir temporarily storing surface runoffs of rice paddy fields located near the coastline during the 2005 rice planting season. Concentrations of 14 target pesticides were measured by GC-MS and the hazards posed by the most important pesticides detected were evaluated by acute toxicity tests using a marine diatom, Chaetoceros sp., and a marine amphipod, Hyale barbicornis. Six pesticides (fenobucarb, flutolanil, iprobenfos, mefenacet, phthalide, pyriproxyfen) were detected in the coastal water, with three pesticides (fenobucarb, iprobenfos, and mefenacet) having 100% frequencies of detection. The maximum concentration of mefenacet, at 4.22 microg/L, was at least one magnitude higher than that of fenobucarb and iprobenfos, at 0.27 and 0.19 microg/L, respectively, while the three remaining pesticides had concentrations just around the detection limit of 0.01 microg/L. Consequently, detected concentrations of mefenacet were highly correlated with salinity levels, confirming that the wastewater reservoir is a major source of rice pesticide residues in this particular coastal environment. Hence, the spatial distribution of mefenacet was simulated using their relationship and the results indicate that mefenacet has a tendency to enter and spread to a relatively wide portion of the coastal area during the rice planting season. There is also a possibility that the other pesticides used in rice farming such as fenobucarb and iprobenfos may show similar distribution patterns in coastal waters when they are present in the wastewater reservoir at higher concentrations. These pesticides, however, manifested low acute toxicities to both Chaetoceros sp. and H. barbicornis, suggesting little impact to marine organisms.

Añasco NC; Koyama J; Uno S

2010-02-01

323

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

Scientific Electronic Library Online (English)

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

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

2004-11-01

324

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

Directory of Open Access Journals (Sweden)

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

Wanpen Mesomya

2012-01-01

325

Validation of pestice multi residue analysis method on cucumber  

International Nuclear Information System (INIS)

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

2011-01-01

326

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

Science.gov (United States)

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

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

2012-04-01

327

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

International Nuclear Information System (INIS)

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

2007-01-01

328

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

UK PubMed Central (United Kingdom)

The capabilities of a recently launched atmospheric pressure chemical ionization (APCI) source for mass spectrometry (MS) coupled to gas chromatography (GC) have been tested in order to evaluate its potential in pesticide residue analysis in fruits and vegetables. Twenty-five pesticides were selected due to their high fragmentation under electron ionization (EI), making that the molecular ion (M+) is practically absent in their spectra. The fragmentation of these pesticides under APCI conditions was studied, with the result that M+ was not only present but also highly abundant for most compounds, with noticeable differences in the fragmentation patterns in comparison with EI. Moreover, the addition of water as modifier was tested to promote the formation of protonated molecules ([M+H]+). Under these conditions, [M+H]+ became the base peak of the spectrum for the majority of compounds, thus leading to an increase of sensitivity in the subsequent GC-MS/MS method developed using triple quadrupole analyzer (QqQ). Highly satisfactory sensitivity and precision, in terms of repeatability, were reached and linearity was satisfactory in the range 0.01-100 ng/mL. The developed methodology was applied to apple, orange, tomato and carrot QuEChERS fortified extracts in order to evaluate the matrix effects. In summary, the soft and reproducible ionization in the APCI source has greatly favored the formation of [M+H]+ oppositely to EI where abundant fragmentation occurs and where the molecular ions have low abundance or are even absent in the mass spectrum. In this way, the use of APCI has facilitated the development of tandem MS methods based on the selection of abundant [M+H]+ as precursor ion.

Portolés T; Cherta L; Beltran J; Hernández F

2012-10-01

329

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

UK PubMed Central (United Kingdom)

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

Lavagnini I; Urbani A; Magno F

2011-02-01

330

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

Science.gov (United States)

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

Lavagnini, Irma; Urbani, Alessandro; Magno, Franco

2010-12-13

331

Multiresidue analysis of pesticides with hydrolyzable functionality in cooked vegetables by liquid chromatography tandem mass spectrometry.  

UK PubMed Central (United Kingdom)

It would be preferable for pesticide residues substituted by hydrolyzable functionality to be analyzed after cooking because their structures are apt to degrade during boiling and/or heating. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantitative determination of 44 pesticide residues with hydrolyzable functional group in five typical vegetable widely consumed in Republic of Korea is described. The sample clean-up was carried out according to the method of Food Code No. 83 established by the Korea Food and Drug Administration (KFDA). Zorbox XDB-C(18) column was selected for the analysis because of the best peak separation. The LC mobile phase consisted of water and 5 mm methanolic ammonium formate, which resulted in a peak shape with good symmetry at each run. Tandem mass spectroscopic (MS/MS) experiments were performed in ESI positive mode and the multiple reaction monitoring modes. A conventional matrix effect was modified to more comprehensive form 100gamma(ij) (%). A high matrix effect (<-30%) was detected for the seven polar pesticides, namely thiamethoxam, clothianidin, acetamiprid, aldicarb, thiacloprid, pirimicarb and methabenzthiazuron. The limits of detection were in the range of 0.1-8.1 microg/kg, indicating a good sensitivity. Most of the recoveries ranged from 70 to 131% with RSDs pesticide levels in the cooked vegetable samples. Of the screened pesticide residues, only fluquinconazole and dimethomorph below the maximum residue levels established by the KFDA were detected in onion and cucumber samples.

Lee SJ; Park S; Choi JY; Shim JH; Shin EH; Choi JH; Kim ST; Abd El-Aty AM; Jin JS; Bae DW; Shin SC

2009-07-01

332

Decontamination of organochlorine pesticides residue and heavy metal in Rehmannia glutinosa Libosch by SFE.  

UK PubMed Central (United Kingdom)

A method involving the simultaneous extraction and decontamination of 12 organochlorine pesticides (OCPs) and seven heavy metals (HM) from Rehmannia glutinosa Libosch was established using supercritical fluid extraction (SFE). A gas chromatography (GC) method with electron capture detection was employed for the determination of the OCPs. The quantitative determination of active constituents (iridoid glycoside and catalpol) in Rehmannia glutinosa Libosch was detected by high-performance liquid chromatography (HPLC). An atomic absorption spectrometry (AAS) was designed for the determination of seven HM, including lead (Pb), cadmium (Cd), copper (Cu), iron (Fe), zinc (Zn), arsenic (As), and mercury (Hg) in Rehmannia glutinosa Libosch. Recovery of the determination of the 12 organochlorine pesticides in Rehmannia glutinosa Libosch sample was 85.9%-101.4% by GC, and relative standard deviation (RSD) was 1.9%-6.0%. Catalpol determination with HPLC in a Rehmannia glutinosa Libosch sample was 0.2486 and 0.2559 mg/mL before and after decontaminating OCPs by SFE, respectively. Those were 0.2486 and 0.2632 mg/mL before and after decontaminating HM by SFE, respectively. After a series of experiments to optimize the final SFE, the following conditions were used to determine the OCPs: pure CO(2), extraction pressure of 15 Mpa, extraction temperature of 60 degrees C, extraction time of 30 min, flow rate at 35 kg/h, and the final SFE conditions of HM was pure CO(2), extraction pressure of 18 Mpa, extraction temperature of 50 degrees C, extraction time of 20 min, modifier at 2.5 mL/50 g. The SFE was used to remove the 12 OCP residues and seven HM residues from Rehmannia glutinosa Libosch with less residue left and negligible loss of the active constituent catalpol.

Zhao C; Bai L; Ou Y; Li D; Xin C

2009-11-01

333

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

International Nuclear Information System (INIS)

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

2006-02-03

334

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

Energy Technology Data Exchange (ETDEWEB)

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

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

2006-02-03

335

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

UK PubMed Central (United Kingdom)

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

Coscollà C; Yusà V; Beser MI; Pastor A

2009-12-01

336

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

Science.gov (United States)

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

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

2009-10-28

337

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

Scientific Electronic Library Online (English)

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

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

2007-12-01

338

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

UK PubMed Central (United Kingdom)

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

Loos M; Krauss M; Fenner K

2012-09-01

339

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

UK PubMed Central (United Kingdom)

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.

Grimalt S; Pozo OJ; Sancho JV; Hernández F

2007-04-01

340

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

Science.gov (United States)

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

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

2007-02-20

 
 
 
 
341

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

Scientific Electronic Library Online (English)

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

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

2004-12-01

342

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

Digital Repository Infrastructure Vision for European Research (DRIVER)

This monitoring study of 40 samples of cow`s milk collected from different locations at Gharbia Governorate during the four different seasons of the years 2005-2006, was conducted to determine the contamination levels of seven pesticide residues including four organophosphorus (chlorpyrifos, diazino...

I.N. Nasr; A.A.A. Sallam; A.A. Abd El-Khair

343

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

Science.gov (United States)

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

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

2008-03-02

344

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

International Nuclear Information System (INIS)

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

1975-01-01

345

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

Directory of Open Access Journals (Sweden)

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

Afshar M; Tahery E; Alasty D

1997-01-01

346

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

International Nuclear Information System (INIS)

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

2007-01-01

347

Organochlorine pesticide residues in sediments and biota from the coastal area of Dar es Salaam city, Tanzania.  

UK PubMed Central (United Kingdom)

Sediment and biota samples were collected from Msimbazi and Kizinga rivers and from the coastal marine environment of Dar es Salaam during both dry and wet seasons. The samples were analyzed for various organochlorine pesticide residues using GC-ECD and GC-MS. Dieldrin, p,p'-DDT, p,p'-DDE, p,p'-DDD, o,p'-DDT and y-HCH were detected at significantly greater concentrations above the method detection limits. Recoveries of pesticide residues ranged 86.5-120% in sediments and 62-102% in biota. The average concentrations of total DDT in sediments for the two seasons were almost the same. Biota samples showed significant difference in levels of residues depending on mode of feeding and age of analyzed biota. p,p'-DDT to total DDT ratios in all matrices indicated recent use of DDT. The levels of residues in sediments suggest possible adverse effects to humans consuming biota that are directly exposed to the sediments. This effect, which is associated with bio-concentration of residues in the tissues of edible aquatic biota, should not affect wildlife. In spite of concern on the adverse effect to humans posed by pesticide residues in sediments, edible biota from the examined water bodies were found to be safe for human consumption.

Mwevura H; Othman OC; Mhehe GL

2002-01-01

348

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

Science.gov (United States)

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. PMID:15274579

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

2004-08-01

349

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

UK PubMed Central (United Kingdom)

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.

Yang Y; Chun Y; Sheng G; Huang M

2004-08-01

350

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

DEFF Research Database (Denmark)

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

Uthuppu, Basil; Kostesha, Natalie

2011-01-01

351

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

UK PubMed Central (United Kingdom)

BACKGROUND: 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. OBJECTIVE: To determine the incidence of pesticide residues in berries harvested from South-Eastern Poland in 2009-2011. MATERIAL AND METHODS: . 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). CONCLUSIONS: Most pesticides were present in raspberries, redcurrants, gooseberries and grapes of which fungicides were the most frequently detected. These results are in keeping with other similar studies.

Matyaszek A; Szpyrka E; Podbielska M; S?owik-Borowiec M; Kurdziel A

2013-01-01

352

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

Science.gov (United States)

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

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

353

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

Science.gov (United States)

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

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

2012-05-15

354

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

UK PubMed Central (United Kingdom)

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

Nougadère A; Sirot V; Kadar A; Fastier A; Truchot E; Vergnet C; Hommet F; Baylé J; Gros P; Leblanc JC

2012-09-01

355

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

Science.gov (United States)

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

2012-07-25

356

Use of simultaneous dual-probe microdialysis for the determination of pesticide residues in a jade plant (Crassula ovata).  

Science.gov (United States)

A microdialysis application for the sampling of plant pesticide residues has been developed utilizing two probes with differing perfusate rates simultaneously inserted into symmetric components of a sampling system. A simple empirical equation is proposed to calculate analyte concentrations in a semi-solid matrix using two different dialysate concentrations. In vitro application yielded excellent correlations between the calculated and spiked concentrations. Subsequent in vivo application of this technique for the determination of pesticide distributions in leaves of a jade plant (Crassula ovata) indicated the utility of this approach in complex living matrices. PMID:19305926

Zhou, Simon Ningsun; Oakes, Ken D; Servos, Mark R; Pawliszyn, Janusz

2009-01-27

357

Use of simultaneous dual-probe microdialysis for the determination of pesticide residues in a jade plant (Crassula ovata).  

UK PubMed Central (United Kingdom)

A microdialysis application for the sampling of plant pesticide residues has been developed utilizing two probes with differing perfusate rates simultaneously inserted into symmetric components of a sampling system. A simple empirical equation is proposed to calculate analyte concentrations in a semi-solid matrix using two different dialysate concentrations. In vitro application yielded excellent correlations between the calculated and spiked concentrations. Subsequent in vivo application of this technique for the determination of pesticide distributions in leaves of a jade plant (Crassula ovata) indicated the utility of this approach in complex living matrices.

Zhou SN; Oakes KD; Servos MR; Pawliszyn J

2009-04-01

358

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

Directory of Open Access Journals (Sweden)

Full Text Available Esta investigación tuvo como objetivos identificar y cuantificar residuos de los plaguicidas organoclorados (POC) hexaclorobenceno (HCB), lindano, cis-clordano, heptacloro, aldrín, dieldrín, endrín y o,p’-diclorodifeniltricloroetano (o,p’-DDT) en aceites de maíz, soya, girasol y mezclas de aceites, que se expenden en la ciudad de Maracaibo, Venezuela. Se analizaron 30 muestras de 4 tipos de aceites de 10 marcas comerciales. La extracción de residuos de POC se realizó según la técnica de la AOAC. Para la identificación y cuantificación se utilizó un cromatógrafo de gases con detector de captura electrónica (GC-ECD), y para la confirmación, un cromatógrafo de gases acoplado a un espectrómetro de masas (GCMS). Todos los residuos de POC investigados fueron detectados en las muestras analizadas. Se detectaron en mayor concentración (mg/ g) aldrín (0,0088), lindano (0,0054) y o,p’-DDT (0,0035). El análisis estadístico demostró diferencias significativas (PThe present study had as objectives to identify and to quantify organochlorine pesticide residues (OCP) hexachlorobenzene (HCB), lindane, cis-chlordane, heptachlor, aldrín, dieldrín, endrín and o,p’-DDT in vegetable oils of corn, soybean, sunflower and mixtures of oils, sold in the city of Maracaibo, Venezuela. 30 samples of 4 types of vegetable oils of 10 commercial brands were analyzed. The extraction of OCP residues was done according to the Official Method of AOAC. A gas chromatograph with an electronic capture detector (GC-ECD) was used for identification and quantification of OCP residues and confirmation was done with a gas chromatograph coupled with a mass spectrometer (GC-MS). All the OCP residues investigated were detected in the analyzed samples. Aldrin (0.0088), lindane (0.0054) and o,p’-DDT (0.0035) were the OCP residues detected in higher concentrations (mg/g). The statistical analysis showed significant differences (P<0.05) for the concentration of OCP in the different types and commercial brands of vegetable oils. Lindane concentration in the corn oil (0.0125 mg/g), as well as cischlordane (0.0091mg/g) and aldrín (0.0287 mg/g) in the soybean oil exceeded maximal residual limits (MRL) established by Food and Agriculture Organization of the United Nations/World Health Organization (FAO/WHO). In conclusion, it was detected a high incidence of OCP residues in vegetable oils analyzed.

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

2007-01-01

359

[Dietary risk assessment for pesticide residues in food of plant origin during the plant protection product's registration process].  

Science.gov (United States)

One of the main goals of risk assessment during registration of plant protection product is to approve (or not) the proposed Maximum Residue Levels (MRLs) derived from the field trials conducted under Good Agricultural Practice (GAP). Generally, risk assessment at this stage is based on comparison of potential long- and short-term dietary intake of given pesticide with two earlier established outputs of hazard characterisation, i.e. Acceptable Daily Intake - ADI and Acute Reference Dose--ARfD. The first estimate of long-term hazard, which overestimates the risk, is comparing the Theoretical Maximum Daily Intake (TMDI) to the ADI of the pesticide. TMDI is based on assumption that all food products consumed over the lifetime of the consumer contain residues at level of MRL. Afterwards, the ADI is compared against International/National Estimated Daily Intake (IEDI/NEDI). I(N)EDI values provide a "best estimate" of dietary intake as they take into account residues in edible portions at level of median residue values from supervised trials. In case of short-term dietary exposure to acute toxic pesticides, the intake is compared to ARfD. The calculation of International/National Estimated Short-Term Intake IESTI/NESTI) requires single-day consumption data for the 97.5th percentile for each subgroups of consumers (so called "large portions") together with typical unit weight, and percentage of edible portion for each commodity as well as high, and median residue levels derived from the field trials. Additionally, in intake calculations for commodities with unit weight over 25 g, the variability factor (from 3 to 10) has been introduced, which reflects the possible high deposition of a pesticide on the individual unit, even when the quantified residue level in composite sample is relatively low. PMID:17713193

Struci?ski, Pawe?; Góralczyk, Katarzyna; Czaja, Katarzyna; Hernik, Agnieszka; Korcz, Wojciech; Ludwicki, Jan K

2006-01-01

360

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

Directory of Open Access Journals (Sweden)

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

Samuel Afful; A.K. Anim and Y. Serfor-Armah

2010-01-01