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Sample records for aged pesticide residues

  1. Pesticide adsorptivity of aged particulate matter arising from crop residue burns.

    PubMed

    Yang, Yaning; Sheng, Guangyao

    2003-08-13

    Particulates (ashes) arising from the burning of crop residues are potentially effective adsorbents for pesticides in agricultural soils. To determine the long-term adsorptive sustainability of ashes, a wheat (Triticum aestivum L.) ash was aged under environmentally relevant conditions (in CaCl(2) solution at room temperature and pH 7) in soil extract for 1 month and in a soil (1% ash) for a period of up to 12 months. The aged ash and ash-amended soil were used to sorb diuron from water. The diuron sorption was also measured in the presence of atrazine as a competing pesticide. There was no observed microbial impact on the stability of the wheat ash in soil. All isotherms with the ash were nonlinear type-I curves, suggestive of the surface adsorption. On a unit mass basis, the ash in soil extract was 600-10000 times more effective than the soil in sorbing diuron. Adsorption of dissolved soil organic matter (DOM) during aging on the ash surfaces reduced the diuron adsorption by 50-60%. Surface competition from the atrazine adsorption also reduced the ash adsorption of diuron by 10-30%. A total of 55-67% reduction in diuron sorption by the ash-amended soil was observed. Due to its high initial adsorptivity, the ash fraction of the aged ash-amended soil contributed >50% to the total diuron sorption. Thus, the wheat ash aged in the soil remained highly effective in adsorbing diuron. As crop residues are frequently burned in the field, pesticides in agricultural soils may be highly immobilized due to the presence of ashes. PMID:12903968

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

    NASA Astrophysics Data System (ADS)

    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

    , 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 (-0.73<ρ<-0.89, p<0.001) and positively with the lignin fraction of the residue in decomposition (0.54<ρ<0.85, p<0.05). The correlation between adsorption and wettability was slight and not significant, except for glyphosate on oat and turnip rape (ρ=-0.99 and ρ=-0.62, p<0.05 respectively), leading to the assumption of the contribution of other factors than biochemical composition in wettability. This study highlighted that the nature and level of decomposition of cover crop at the soil surface influenced the mobility of pesticides as it was observed in decomposing mulch of crop residues (Aslam et al., 2013). As a result, the type of cover crop and the changes of cover crop residues composition during decomposition in field may control differently the movement of non-ionic pesticides compared to ionic compounds such as glyphosate, largely used in conservation agriculture practices. Keywords : Cover crops ; Glyphosate ; S-metolachlor ; Epoxiconazole ; Mulch; Sorption ; Biochemical composition References Alletto L., Benoit P., Justes E., Coquet Y. 2012. Effects of tillage and fallow period management on the fate of the herbicide isoxaflutole in an irrigated continuous-maize field. Agriculture, Ecosystems Environment, 153, 40- 49. http://dx.doi:10.1016/j.agee.2012.03.002 Alletto L., Benoit P., Coufignal M., Bergheaud V., Dumény V., Longueval D., Barriuso E. 2013. Sorption and mineralization of S-metolachlor in 51 fields cultivated with conservation tillage. Soil Tillage Research 128, 97-103. http://dx.doi.org/10.1016/j.still.2012

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

    NASA Astrophysics Data System (ADS)

    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

    , 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 (-0.73<ρ<-0.89, p<0.001) and positively with the lignin fraction of the residue in decomposition (0.54<ρ<0.85, p<0.05). The correlation between adsorption and wettability was slight and not significant, except for glyphosate on oat and turnip rape (ρ=-0.99 and ρ=-0.62, p<0.05 respectively), leading to the assumption of the contribution of other factors than biochemical composition in wettability. This study highlighted that the nature and level of decomposition of cover crop at the soil surface influenced the mobility of pesticides as it was observed in decomposing mulch of crop residues (Aslam et al., 2013). As a result, the type of cover crop and the changes of cover crop residues composition during decomposition in field may control differently the movement of non-ionic pesticides compared to ionic compounds such as glyphosate, largely used in conservation agriculture practices. Keywords : Cover crops ; Glyphosate ; S-metolachlor ; Epoxiconazole ; Mulch; Sorption ; Biochemical composition References Alletto L., Benoit P., Justes E., Coquet Y. 2012. Effects of tillage and fallow period management on the fate of the herbicide isoxaflutole in an irrigated continuous-maize field. Agriculture, Ecosystems Environment, 153, 40- 49. http://dx.doi:10.1016/j.agee.2012.03.002 Alletto L., Benoit P., Coufignal M., Bergheaud V., Dumény V., Longueval D., Barriuso E. 2013. Sorption and mineralization of S-metolachlor in 51 fields cultivated with conservation tillage. Soil Tillage Research 128, 97-103. http://dx.doi.org/10.1016/j.still.2012

  4. High-Throughput Analytical Techniques for Determination of Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea, Part VI: Study of the Degradation of 271 Pesticide Residues in Aged Oolong Tea by Gas Chromatography-Tandem Mass Spectrometry and Its Application in Predicting the Residue Concentrations of Target Pesticides.

    PubMed

    Chang, Qiao-Ying; Pang, Guo-Fang; Fan, Chun-Lin; Chen, Hui; Wang, Zhi-Bin

    2016-07-01

    The degradation rate of 271 pesticide residues in aged Oolong tea at two spray concentrations, named a and b (a < b), were monitored for 120 days using GC-tandem MS (GC-MS/MS). To research the degradation trends and establish regression equations, determination days were plotted as horizontal ordinates and the residue concentrations of pesticide were plotted as vertical ordinates. Here, we consider the degradation equations of 271 pesticides over 40 and 120 days, summarize the degradation rates in six aspects (A-F), and discuss the degradation trends of the 271 pesticides in aged Oolong tea in detail. The results indicate that >70% of the determined pesticides coincide with the degradation regularity of trends A, B, and E, i.e., the concentration of pesticide will decrease within 4 months. Next, 20 representative pesticides were selected for further study at higher spray concentrations, named c and d (d > c > b > a), in aged Oolong tea over another 90 days. The determination days were plotted on the x-axis, and the differences between each determined result and first-time-determined value of target pesticides were plotted on the y-axis. The logarithmic function was obtained by fitting the 90-day determination results, allowing the degradation value of a target pesticide on a specific day to be calculated. These logarithmic functions at d concentration were applied to predict the residue concentrations of pesticides at c concentration. Results revealed that 70% of the 20 pesticides had the lower deviation ratios of predicted and measured results. PMID:27151741

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

    EPA Science Inventory

    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...

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

    NASA Astrophysics Data System (ADS)

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

    2012-04-01

    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 μm) 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 μg kg-1 soil (dry/wet) and 10.7 μg kg-1 soil (wet/wet), accounting for 3.45 and 1.35% of total parent compound

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

    NASA Astrophysics Data System (ADS)

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

    2012-04-01

    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 μm) 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 μg kg-1 soil (dry/wet) and 10.7 μg kg-1 soil (wet/wet), accounting for 3.45 and 1.35% of total parent compound

  8. Pesticide Residues in Food: Your Daily Dose.

    ERIC Educational Resources Information Center

    Mott, Lawrie

    1985-01-01

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

  9. PESTICIDE RESIDUE RECOVERIES FROM SURFACE WIPES

    EPA Science Inventory

    Human exposure is a consequence of pesticide use indoors with a primary source resulting from residue deposition on household surfaces. Accurate measurements of surface residues is essential for estimating exposure from different routes. Various procedures have been developed ...

  10. Organochlorine pesticides residue in breast milk: a systematic review

    PubMed Central

    Pirsaheb, Meghdad; Limoee, Mojtaba; Namdari, Farideh; Khamutian, Razieh

    2015-01-01

    Background: Chlorinated pesticides have been used in pest control for several decades in the world. These compounds are still applied in many regions, and their continuous usage has resulted in their bioaccumulation and residue in the food chain. These residues could transfer to food products and accumulate in fat tissues. Undoubtedly, the breast milk could be a significant biomarker for estimation of these residues in the human body. This study was conducted to review and compile the results of the studies undertaken in the world which surveyed the organochlorine pesticides residue in breast milk. Methods: A total of 710 national and international articles and texts related to the focused subject were extracted from the virtual databases using the following key words: Chlorinated pesticides, residue and breast milk. Thirty articles published between 1980 and 2013 were selected and reviewed. Results: The majority of the reviewed articles indicated the presence of two or more organochlorine pesticides in the collected samples of breast milk. Based on the reviewed studies, dichlorodiphenyltrichloroethane (DDT) had the highest level of concentration in the collected samples of breast milk. Moreover, there was a statistically significant positive correlation between mother’s age, her multiparty and concentration of chlorinated pesticides in breast milk. Conclusion: The organochlorine pesticides are still applied in some developing countries including some regions of Iran. Thus, it seems essential to inform the community about the adverse effects of this class of pesticides; and most importantly the governments should also ban the use of such compounds. PMID:26478886

  11. Determination of pesticide residues in cannabis smoke.

    PubMed

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

    2013-01-01

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

  12. Monitoring of pesticide residues in vegetarian diet.

    PubMed

    Kumari, Beena; Kathpal, T S

    2009-04-01

    Samples (28) of complete vegetarian diet consumed from morning till night i.e. tea, milk, breakfast, lunch, snacks, dinner, sweet dish etc. were collected from homes, hostels and hotels periodically from Hisar and analysed for detecting the residues of organochlorine, synthetic pyrethriod, organophosphate and carbamate insecticides. The estimation was carried out by using multi-residue analytical technique employing gas chromatograph (GC)-electron capture detector and GC-nitrogen phosphorous detector systems equipped with capillary columns. The whole diet sample was macerated in a mixer grinder and a representative sample in duplicate was analyzed for residues keeping the average daily diet of an adult to be 1,300 g. On comparing the data, it was found that actual daily intake (microgram/person/day) of lindane in two and endosulfan in four samples exceeded the acceptable daily intake. Residues of other pesticides in all the diet samples were lower than the acceptable daily intake (ADI) of the respective pesticides. The study concluded that although all the diet samples were found contaminated with one or the other pesticide, the actual daily intake of only a few pesticides was higher than their respective ADI. More extensive study covering other localities of Haryana has been suggested to know the overall scenario of contamination of vegetarian diet. PMID:18386151

  13. 7 CFR 29.427 - Pesticide residue standards.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... 7 Agriculture 2 2014-01-01 2014-01-01 false Pesticide residue standards. 29.427 Section 29.427... REGULATIONS TOBACCO INSPECTION Regulations Miscellaneous § 29.427 Pesticide residue standards. The maximum concentration of residues of the following pesticides allowed in flue-cured or burley tobacco, expressed...

  14. 7 CFR 29.427 - Pesticide residue standards.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 7 Agriculture 2 2013-01-01 2013-01-01 false Pesticide residue standards. 29.427 Section 29.427... REGULATIONS TOBACCO INSPECTION Regulations Miscellaneous § 29.427 Pesticide residue standards. The maximum concentration of residues of the following pesticides allowed in flue-cured or burley tobacco, expressed...

  15. 7 CFR 29.427 - Pesticide residue standards.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 7 Agriculture 2 2011-01-01 2011-01-01 false Pesticide residue standards. 29.427 Section 29.427... REGULATIONS TOBACCO INSPECTION Regulations Miscellaneous § 29.427 Pesticide residue standards. The maximum concentration of residues of the following pesticides allowed in flue-cured or burley tobacco, expressed...

  16. 7 CFR 29.427 - Pesticide residue standards.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... 7 Agriculture 2 2012-01-01 2012-01-01 false Pesticide residue standards. 29.427 Section 29.427... REGULATIONS TOBACCO INSPECTION Regulations Miscellaneous § 29.427 Pesticide residue standards. The maximum concentration of residues of the following pesticides allowed in flue-cured or burley tobacco, expressed...

  17. 7 CFR 29.427 - Pesticide residue standards.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 7 Agriculture 2 2010-01-01 2010-01-01 false Pesticide residue standards. 29.427 Section 29.427... REGULATIONS TOBACCO INSPECTION Regulations Miscellaneous § 29.427 Pesticide residue standards. The maximum concentration of residues of the following pesticides allowed in flue-cured or burley tobacco, expressed...

  18. Persistent organochlorine pesticide residues in animal feed.

    PubMed

    Nag, Subir Kumar; Raikwar, Mukesh K

    2011-03-01

    Animal products like milk and meat are often found to be contaminated with residues of persistent pesticides and other toxic substances. The major source of entry of these compounds to animal body is the contaminated feed and fodder. So, unless the residues are managed at this stage, it is very difficult to prevent contamination in milk and meat. Therefore, the status of residue level of most persistent organochlorinated pesticides (OCP) in feed and fodder should be monitored regularly. The frequency of occurrence and contamination levels of OCP residues in different kinds of animal concentrate feed and straw samples collected from Bundelkhand region of India were determined. Out of 533 total samples, 301 i.e. 56.47% samples were positive containing residues of different OCPs like hexachlorocyclohexane (HCH) isomers, dichlorodiphenyltrichloroethane (DDT) complex, endosulfan and dicofol. Among different HCH isomers, the mean concentration of β-HCH was highest, and total HCH varied from 0.01 to 0.306 mg kg(-1). In case of DDT complex, i.e. DDD, DDE and DDT, the concentration ranged between 0.016 and 0.118 mg kg(-1) and the pp(|) isomers were more frequently encountered than their op(|) counterparts. Endosulfan was also found in some samples in concentration ranging from 0.009 to 0.237 mg/kg, but dicofol could be recorded in very few samples. Although feed samples were found to contain OC residues, after comparing their levels in positive samples with the limiting values of respective pesticides, only very few were found to exceed the threshold level. Otherwise, they were mostly within safe limits. PMID:20443138

  19. Pesticides.

    ERIC Educational Resources Information Center

    Sherma, Joseph

    1989-01-01

    This review is devoted to methods for the determination of residues of pesticides and some related industrial chemicals. Topics include: residue methods, sampling, chromatography, organochlorine pesticides, organophosphorus pesticides, carbamate insecticides, herbicides, fungicides, pyrethrins, fumigants, and related chemicals. (MVL)

  20. Research of pesticide residues on fruit by terahertz spectroscopy technology

    NASA Astrophysics Data System (ADS)

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

    2011-11-01

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

  1. Pesticide residues in imported, organic, and "suspect" fruits and vegetables.

    PubMed

    Winter, Carl K

    2012-05-01

    Consumers are frequently urged to avoid imported foods as well as specific fruits and vegetables due to health concerns from pesticide residues and are often encouraged to choose organic fruits and vegetables rather than conventional forms. Studies have demonstrated that while organic fruits and vegetables have lower levels of pesticide residues than do conventional fruits and vegetables, pesticide residues are still frequently detected on organic fruits and vegetables; typical dietary consumer exposure to pesticide residues from conventional fruits and vegetables does not appear to be of health significance. Similarly, research does not demonstrate that imported fruits and vegetables pose greater risks from pesticide residues than do domestic fruits and vegetables or that specific fruits and vegetables singled out as being the most highly contaminated by pesticides should be avoided in their conventional forms. PMID:22335627

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

    PubMed

    Choudhary, Amit; Sharma, Duni C

    2008-05-01

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

  3. [Organochlorine pesticide residues in human adipose tissue in Costa Rica].

    PubMed

    Barquero, M; Constenla, M A

    1986-06-01

    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. PMID:2445007

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

    PubMed

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

    2004-04-01

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

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

    NASA Astrophysics Data System (ADS)

    Andreou, Kostas; Semple, Kirk; Jones, Kevin

    2010-05-01

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

  6. Pesticides

    MedlinePlus

    ... are applied during farming and how much pesticide residue can remain in foods sold in stores. Exposure ... to pesticides at work should carefully clean any residue from their skin and remove their clothes and ...

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Performance of compost and biochar amendments for in situ risk mitigation of aged DDT, DDE and dieldrin residues in an old orchard soil was examined. The change in bioavailability of pesticide residues relative to an unamended control soil was assessed using Lumbricus terrestris in 4-L soil microcos...

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

    PubMed

    Sadło, Stanisław; Szpyrka, Ewa; Rogozińska, Krystyna; Rupar, Julian; Kuźmenko, Arletta

    2007-01-01

    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

  9. FOR HEALTHY KIDS: REDUCTION OF HOME PESTICIDE RESIDUE EXPOSURES

    EPA Science Inventory

    For Healthy Kids focuses on preventing children's exposure to pesticides by educating agricultural workers on preventing "the take home pathway" for pesticide residue. A baseline survey encompassing over 570 households in the Yakima valley was conducted in the summer of 1999. Ho...

  10. Laundering as decontamination of apparel fabrics: residues of pesticides from six chemical classes.

    PubMed

    Nelson, C; Laughlin, J; Kim, C; Rigakis, K; Raheel, M; Scholten, L

    1992-07-01

    Research on reducing the level of pesticide residue on a textile substrate has examined many variables under many different conditions. This study controlled fiber type and the use of prewash product in an examination of residue levels for a number of pesticides in different pesticide classes. For all pesticides examined, the use of prewash lowered pesticide residues regardless of fiber type. Differences in pesticide residue level attributable to fiber type were not consistent. PMID:1637202

  11. The 47th annual Florida pesticide residue workshop

    Technology Transfer Automated Retrieval System (TEKTRAN)

    This is an introductory article to a special section of the Journal of Agricultural and Food Chemistry consisting of publications from the 47th Annual Florida Pesticide Residue Workshop held in St. Pete Beach, FL in July of 2010....

  12. Pesticide residue quantification analysis by hyperspectral imaging sensors

    NASA Astrophysics Data System (ADS)

    Liao, Yuan-Hsun; Lo, Wei-Sheng; Guo, Horng-Yuh; Kao, Ching-Hua; Chou, Tau-Meu; Chen, Junne-Jih; Wen, Chia-Hsien; Lin, Chinsu; Chen, Hsian-Min; Ouyang, Yen-Chieh; Wu, Chao-Cheng; Chen, Shih-Yu; Chang, Chein-I.

    2015-05-01

    Pesticide residue detection in agriculture crops is a challenging issue and is even more difficult to quantify pesticide residue resident in agriculture produces and fruits. This paper conducts a series of base-line experiments which are particularly designed for three specific pesticides commonly used in Taiwan. The materials used for experiments are single leaves of vegetable produces which are being contaminated by various amount of concentration of pesticides. Two sensors are used to collected data. One is Fourier Transform Infrared (FTIR) spectroscopy. The other is a hyperspectral sensor, called Geophysical and Environmental Research (GER) 2600 spectroradiometer which is a batteryoperated field portable spectroradiometer with full real-time data acquisition from 350 nm to 2500 nm. In order to quantify data with different levels of pesticide residue concentration, several measures for spectral discrimination are developed. Mores specifically, new measures for calculating relative power between two sensors are particularly designed to be able to evaluate effectiveness of each of sensors in quantifying the used pesticide residues. The experimental results show that the GER is a better sensor than FTIR in the sense of pesticide residue quantification.

  13. Pesticide residues in rain water from Hisar, India.

    PubMed

    Kumari, Beena; Madan, V K; Kathpal, T S

    2007-10-01

    Presence of pesticide residues was studied in rain water during 2002 employing multi residue analysis method by gas liquid chromatography equipped with ECD and NPD detectors and capillary columns. The presence of pesticide residues in surface aquatic system triggered the investigation of the presence of pesticides in rain water. A total of 13 pesticides were detected in rain water samples. Among the different groups of pesticides, organochlorines were present in the range of 0.041-7.060 ppb with maximum concentration of p,p'-DDT up to 7.060 microg l(-1). Synthetic pyrethroids were present ranging from 0.100 to 1.000 microg l(-1) and organophosphates in the range of 0.050-4.000 microg l(-1) showing maximum contamination with cypermethrin (1.000 microg l(-1)) and monocrotophos (4.000 microg l(-1)) of the respective groups. Almost 80% samples showed the residues above MRL of 0.5 ppb fixed for multi residues and on the basis of single pesticide, 16-50% samples contained residues above the MRL value of 0.1 ppb. PMID:17268917

  14. Organochlorine pesticide residues in wheat from Konya region, Turkey.

    PubMed

    Guler, G O; Cakmak, Y S; Dagli, Z; Aktumsek, A; Ozparlak, H

    2010-05-01

    The present study has been carried out to evaluate the organochlorine pesticide contamination in wheat from Konya region. This region is the largest area of cereal production in Turkey. The contamination level has been determined according to the European Community Directives. Different wheat samples (36) were obtained from local farmers and wheat factories in this region. All the wheat samples examined were found to be contaminated by organochlorine pesticide residues of cis-Chlordane and methoxychlor. Chlordane isomers, methoxychlor, DDT and its metabolites, aldrin, beta HCH, heptachlor and lindane have been found to be the highest organochlorine pesticide residues. In some of these samples, various organochlorine pesticide residues have been determined to be higher than European Community maximum residual limits. The residues of aldrin in one sample, trans-Chlordane in one sample, oxy-chlordane in eight samples and methoxychlor in one sample were found to be in excess of EC MRLs. Since most of the samples have been found to be contaminated with residues and some residues exceed EC MRLs, a control of organochlorine pesticide residues in wheat is necessary. PMID:20156519

  15. Leaf surfaces and the bioavailability of pesticide residues.

    PubMed

    Chowdhury, A B; Jepson, P C; Howse, P E; Ford, M G

    2001-05-01

    Laboratory bioassays were carried out to determine the toxicity to Folsomia candida Willem (Collembola: Isotomidae) of residues of a pyrethroid insecticide, deltamethrin, and an organophosphorus insecticide, dimethoate, on different leaf surfaces. The test leaves included a range of species and leaves of different ages. Dose-response relationships were estimated for F candida walking over the various treated leaf substrates. Probit analysis was used to estimate the means and standard deviations of the associated tolerance distributions expressed as gAIha-1. Parallelism tests were undertaken to compare the susceptibilities of F candida to the two compounds applied to the different leaf surfaces. On deltamethrin-treated leaf surfaces, the LD50 values for F candida varied from 6.36 to 77.14 gAIha-1. F candida was least susceptible to deltamethrin residues when applied to leaves of dwarf bean (Phaseolus vulgarus L) and the highest susceptibility was observed following application to leaves of seedlings of barley (Hordeum vulgare L). In contrast, the LD50 values observed for dimethoate treatments did not differ significantly between leaf types, ranging from 1.35 to 8.69 gAIha-1. The laboratory data on susceptibility of F candida on different leaf types for different pesticides can be used to investigate the role of leaf surface properties in modifying the toxicity of applied pesticides to exposed invertebrates. PMID:11374156

  16. 78 FR 70906 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-11-27

    ... AGENCY 40 CFR Part 180 Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on... residues of pesticide chemicals in or on various commodities. DATES: Comments must be received on or before...), requesting the establishment or modification of regulations in 40 CFR part 180 for residues of...

  17. EXPOSURE TO CHILDREN FROM PESTICIDE RESIDUES

    EPA Science Inventory

    Children's aggregate exposure to pesticides will be characterized using pesticide exposure data from Brownsville, TX. The aggregate exposure methodology developed in this phase of the project will be tested with a larger data set from Arizona using data from US-Mexico border are...

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

    PubMed

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

    2010-11-01

    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

  19. 40 CFR 158.2130 - Microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 25 2012-07-01 2012-07-01 false Microbial pesticides residue data... (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Microbial Pesticides § 158.2130 Microbial pesticides residue data requirements table. (a) General. Sections 158.100 through 158.130 describe how to...

  20. 40 CFR 158.2172 - Experimental use permit microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

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

  1. 40 CFR 158.2172 - Experimental use permit microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

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

  2. 40 CFR 158.2130 - Microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 24 2014-07-01 2014-07-01 false Microbial pesticides residue data... (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Microbial Pesticides § 158.2130 Microbial pesticides residue data requirements table. (a) General. Sections 158.100 through 158.130 describe how to...

  3. 40 CFR 158.2172 - Experimental use permit microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

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

  4. 40 CFR 158.2130 - Microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 25 2013-07-01 2013-07-01 false Microbial pesticides residue data... (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Microbial Pesticides § 158.2130 Microbial pesticides residue data requirements table. (a) General. Sections 158.100 through 158.130 describe how to...

  5. 40 CFR 158.2172 - Experimental use permit microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

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

  6. 40 CFR 158.2130 - Microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 24 2011-07-01 2011-07-01 false Microbial pesticides residue data... (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Microbial Pesticides § 158.2130 Microbial pesticides residue data requirements table. (a) General. Sections 158.100 through 158.130 describe how to...

  7. 40 CFR 158.2172 - Experimental use permit microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

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

  8. 40 CFR 158.2130 - Microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

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

  9. Airborne pesticide residues along the Mississippi River

    USGS Publications Warehouse

    Majewski, M.S.; Foreman, W.T.; Goolsbys, D.A.; Nakagaki, N.

    1998-01-01

    The occurrence, concentration, and geographical distribution of agricultural pesticides were determined in air over the Mississippi River from New Orleans, LA, to St. Paul, MN, during the first 10 days of June 1994. Air samples were collected from a research vessel by pulling air through polyurethane foam plugs at about 100 L/min for up to 24 h. Each sample was analyzed for 42 pesticides and 3 pesticide transformation products. Twenty- five compounds-15 herbicides, 7 insecticides, and 3 pesticide transformation products-were detected in one or more samples with concentrations ranging from 0.05 to 80 ng/m3. Alachlor, chlorpyrifos, diazinon, fonofos, malathion, methyl parathion, metolachlor, metribuzin, pendimethalin, and trifluralin were detected in 80% or more of the samples. The highest concentrations for chlorpyrifos (1.6 ng/m3), diazinon (0.36 ng/m3), and malathion (4.6 ng/m3) all occurred near major metropolitan areas. These samples represent a 'snapshot in time', a spatial and temporal integration of which pesticides were present in the air during each sampling period. The occurrence and atmospheric concentrations of the observed pesticides were most closely related to their use on cropland within 40 km of the river.The occurrence, concentration, and geographical distribution of agricultural pesticides were determined in air over the Mississippi River from New Orleans, LA, to St. Paul, MN, during the first 10 days of June 1994. Air samples were collected from a research vessel by pulling air through polyurethane foam plugs at about 100 L/min for up to 24 h. Each sample was analyzed for 42 pesticides and 3 pesticide transformation products. Twenty-five compounds-15 herbicides, 7 insecticides, and 3 pesticide transformation products-were detected in one or more samples with concentrations ranging from 0.05 to 80 ng/m3. Alachlor, chlorpyrifos, diazinon, fonofos, malathion, methyl parathion, metolachlor, metribuzin, pendimethalin, and trifluralin were detected in

  10. A review of organochlorine pesticide residues in ferruginous hawk eggs

    USGS Publications Warehouse

    Henny, C.J.

    1985-01-01

    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.

  11. Pesticides

    MedlinePlus

    ... and rats. Because of the widespread use of agricultural chemicals in food production, people are exposed to ... effects of these pesticide residues. Results from the Agricultural Health Study, an ongoing study of pesticide exposures ...

  12. Glove accumulation of pesticide residues for strawberry harvester exposure assessment.

    PubMed

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

    2011-06-01

    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

  13. Global Harmonization of Maximum Residue Limits for Pesticides.

    PubMed

    Ambrus, Árpád; Yang, Yong Zhen

    2016-01-13

    International trade plays an important role in national economics. The Codex Alimentarius Commission develops harmonized international food standards, guidelines, and codes of practice to protect the health of consumers and to ensure fair practices in the food trade. The Codex maximum residue limits (MRLs) elaborated by the Codex Committee on Pesticide Residues are based on the recommendations of the FAO/WHO Joint Meeting on Pesticides (JMPR). The basic principles applied currently by the JMPR for the evaluation of experimental data and related information are described together with some of the areas in which further developments are needed. PMID:25603277

  14. 78 FR 33785 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-06-05

    ...This document announces the Agency's receipt of several initial filings of pesticide petitions requesting the establishment or modification of regulations for residues of pesticide chemicals in or on various...

  15. 75 FR 65321 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-10-22

    ...This notice announces the Agency's receipt of several initial filings of pesticide petitions proposing the establishment or modification of regulations for residues of pesticide chemicals in or on various...

  16. 77 FR 25954 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-05-02

    ...This document announces the Agency's receipt of several initial filings of pesticide petitions requesting the establishment or modification of regulations for residues of pesticide chemicals in or on various...

  17. 78 FR 56185 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-09-12

    ...This document announces the Agency's receipt of several initial filings of pesticide petitions requesting the establishment or modification of regulations for residues of pesticide chemicals in or on various...

  18. 78 FR 11126 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-02-15

    ...This document announces the Agency's receipt of several initial filings of pesticide petitions requesting the establishment or modification of regulations for residues of pesticide chemicals in or on various...

  19. 76 FR 61647 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-10-05

    ...This document announces the Agency's receipt of several initial filings of pesticide petitions requesting the establishment or modification of regulations for residues of pesticide chemicals in or on various...

  20. 77 FR 43562 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-07-25

    ...This document announces the Agency's receipt of several initial filings of pesticide petitions requesting the establishment or modification of regulations for residues of pesticide chemicals in or on various...

  1. 76 FR 39358 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-07-06

    ...This document announces the Agency's receipt of several initial filings of pesticide petitions requesting the establishment or modification of regulations for residues of pesticide chemicals in or on various...

  2. 76 FR 82238 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-12-30

    ...This document announces the Agency's receipt of several initial filings of pesticide petitions requesting the establishment or modification of regulations for residues of pesticide chemicals in or on various...

  3. 76 FR 49396 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-08-10

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

  4. 77 FR 59578 - Notice of Filing of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-09-28

    ...This document announces the Agency's receipt of several initial filings of pesticide petitions requesting the establishment or modification of regulations for residues of pesticide chemicals in or on various...

  5. 76 FR 53372 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-08-26

    ...This document announces the Agency's receipt of several initial filings of pesticide petitions requesting the establishment or modification of regulations for residues of pesticide chemicals in or on various...

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

    PubMed

    Swarnam, T P; Velmurugan, A

    2013-07-01

    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, α-endosulfan, β-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 α-cypermethrin, fenvalerate I, fluvalinate I, deltamethrin, and λ-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

  7. Sampling and sample processing in pesticide residue analysis.

    PubMed

    Lehotay, Steven J; Cook, Jo Marie

    2015-05-13

    Proper sampling and sample processing in pesticide residue analysis of food and soil have always been essential to obtain accurate results, but the subject is becoming a greater concern as approximately 100 mg test portions are being analyzed with automated high-throughput analytical methods by agrochemical industry and contract laboratories. As global food trade and the importance of monitoring increase, the food industry and regulatory laboratories are also considering miniaturized high-throughput methods. In conjunction with a summary of the symposium "Residues in Food and Feed - Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods" held at the 13th IUPAC International Congress of Pesticide Chemistry, this is an opportune time to review sampling theory and sample processing for pesticide residue analysis. If collected samples and test portions do not adequately represent the actual lot from which they came and provide meaningful results, then all costs, time, and efforts involved in implementing programs using sophisticated analytical instruments and techniques are wasted and can actually yield misleading results. This paper is designed to briefly review the often-neglected but crucial topic of sample collection and processing and put the issue into perspective for the future of pesticide residue analysis. It also emphasizes that analysts should demonstrate the validity of their sample processing approaches for the analytes/matrices of interest and encourages further studies on sampling and sample mass reduction to produce a test portion. PMID:25677085

  8. Pesticide residues in agricultural drains, southeastern desert area, California

    USGS Publications Warehouse

    Eccles, Lawrence A.

    1979-01-01

    A study is being made to determine the occurrence and distribution of pesticides in the agricultural drains for approximately 3/4 million irrigated acres in the southeastern desert area of California. This report describes the results of the first year of sampling and analyzing (1) water in the drains , (2) bed material in the drains, (3) water from field tile-drainage lines, and (4) irrigation tailwater and water in the drains directly exposed to drift from aerial application of pesticides. Residues of almost all the pesticides selected for monitoring were found in water in the drains. Examination of the data to determine the probable source of pesticides indicated generally slight concentrations from bed material in the drains, usually no detectable concentrations from field tile-drainage lines, and apparently large concentrations from irrigation tailwater and drift from aerial application. (Woodard-USGS)

  9. Evaluation of pesticide residues in human blood samples from Punjab (India)

    PubMed Central

    Bedi, Jasbir Singh; Gill, J. P. S.; Kaur, P.; Sharma, A.; Aulakh, R. S.

    2015-01-01

    Aim: The present study was undertaken to estimate the current status of residues of organochlorine pesticides (OCPs), organophosphates (OPs) and synthetic pyrethroids (SPs) pesticides in human blood. Materials and Methods: Human blood samples were analyzed by gas chromatography and confirmed by gas chromatography-mass spectrometry in selective ion monitoring mode. Results: The gas chromatographic analysis of human blood samples collected from Punjab revealed the presence of p,p’-dichlorodiphenyl dichloroethylene (DDE), p,p’ dichlorodiphenyl dichloroethane (DDD), o,p’ DDE and β-endosulfan at mean levels of 15.26, 2.71, 5.62 and 4.02 ng/ml, respectively. p,p’ DDE residue was observed in 18.0% blood samples, and it contributes 55% of the total pesticide burden in human blood. The difference of total dichlorordiphenyl trichloroethane (DDT) between different age groups of humans was found to be statistically significant (p<0.05). The difference of DDT and endosulfan between dietary habits, gender and spraying of pesticides was found statistically non-significant, however endosulfan residues were observed only in pesticide sprayer’s population. Conclusion: Occurrence of p,p’ DDE, p,p’ DDD, o,p’ DDE in human blood indicated restricted use of DDT. However, presence of endosulfan residues in occupationally exposed population is a matter of public health concern. PMID:27046999

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

    USGS Publications Warehouse

    Henny, C.J.

    1985-01-01

    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.

  11. International Harmonization of Food Safety Assessment of Pesticide Residues.

    PubMed

    Ambrus, Árpád

    2016-01-13

    This paper summarizes the development of principles and methods applied within the program of the FAO/WHO Codex Alimentarius during the past 50 years for the safety assessment of pesticide residues in food and feed and establishing maximum residue limits (MRLs) to promote free international trade and assure the safety of consumers. The role of major international organizations in this process, the FAO capacity building activities, and some problematic areas that require special attention are briefly described. PMID:25660755

  12. CHARACTERIZING PESTICIDE RESIDUE TRANSFER EFFICIENCIES USING FLUORESCENT TRACER IMAGING TECHNIQUES

    EPA Science Inventory

    To reduce the uncertainty associated with current estimates of children's exposure to pesticides by dermal contact and non-dietary ingestion, residue transfer data are required. Prior to conducting exhaustive studies, a screening study was conducted to identify the important pa...

  13. Sampling and sample processing in pesticide residue analysis

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Proper sampling and sample processing in pesticide residue analysis of food and soil has always been essential to obtain accurate results, but the subject is becoming a greater concern as approximately 100 mg test portions are being analyzed with automated high-throughput analytical methods by agroc...

  14. PESTICIDE SURFACE RESIDUE MEASUREMENTS BY A PRESS SAMPLER

    EPA Science Inventory

    Pesticides on household surfaces are a source of exposure to children. Accurate measurements of residues on surfaces are needed to determine amounts available for transfer to foods and other objects handled or eaten by a child. Wiping the surface with a solvent has been the acc...

  15. 5th Latin American pesticide residue workshop (LAPRW 2015)

    Technology Transfer Automated Retrieval System (TEKTRAN)

    This invited editorial proceedings article introduces the 6 research papers published in the special topical collection for the 5th Latin American Pesticide Residue Workshop held in Santiago, Chile, May 10-13, 2015. The meeting was a great success with more than 50 talks, 140 posters, 21 vendors, a...

  16. 9 CFR 318.16 - Pesticide chemicals and other residues in products.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... 9 Animals and Animal Products 2 2014-01-01 2014-01-01 false Pesticide chemicals and other residues... PREPARATION OF PRODUCTS General § 318.16 Pesticide chemicals and other residues in products. (a) Nonmeat ingredients. Residues of pesticide chemicals, food additives and color additives or other substances in or...

  17. 9 CFR 318.16 - Pesticide chemicals and other residues in products.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 9 Animals and Animal Products 2 2011-01-01 2011-01-01 false Pesticide chemicals and other residues... PREPARATION OF PRODUCTS General § 318.16 Pesticide chemicals and other residues in products. (a) Nonmeat ingredients. Residues of pesticide chemicals, food additives and color additives or other substances in or...

  18. 9 CFR 318.16 - Pesticide chemicals and other residues in products.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 9 Animals and Animal Products 2 2013-01-01 2013-01-01 false Pesticide chemicals and other residues... PREPARATION OF PRODUCTS General § 318.16 Pesticide chemicals and other residues in products. (a) Nonmeat ingredients. Residues of pesticide chemicals, food additives and color additives or other substances in or...

  19. 9 CFR 318.16 - Pesticide chemicals and other residues in products.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... 9 Animals and Animal Products 2 2012-01-01 2012-01-01 false Pesticide chemicals and other residues... PREPARATION OF PRODUCTS General § 318.16 Pesticide chemicals and other residues in products. (a) Nonmeat ingredients. Residues of pesticide chemicals, food additives and color additives or other substances in or...

  20. 9 CFR 318.16 - Pesticide chemicals and other residues in products.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 9 Animals and Animal Products 2 2010-01-01 2010-01-01 false Pesticide chemicals and other residues... PREPARATION OF PRODUCTS General § 318.16 Pesticide chemicals and other residues in products. (a) Nonmeat ingredients. Residues of pesticide chemicals, food additives and color additives or other substances in or...

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

    NASA Astrophysics Data System (ADS)

    Mukherjee, Santanu

    2016-04-01

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

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

    PubMed

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

    1997-12-01

    This monitoring study of 355 samples of cow's milk collected from the central region of Veracruz state and 448 samples of national butter brands was conducted to determine the contamination levels of organochlorine pesticides. The results obtained for mean HCH levels were 0.094 and 0.093 mg/kg on fat basis in cow's milk and butter samples, respectively. The mean DDT levels were 0.159 and 0.049 mg/kg, respectively. In relation to cow's milk, the total HCH levels in Veracruz state were higher but total DDT levels were comparable to those reported in other countries. On the other hand, organochlorine levels detected in national brand butter samples were lower than those found in other countries, where these pesticides are still used in sanitary actions. These results confirmed that dairy products in Mexico presented organochlorine pesticide residues (owing to their use in sanitary actions) indicating a human exposure through these food products. PMID:9496657

  3. Proficiency test on the determination of pesticide residues in grapes with multi-residue methods.

    PubMed

    Dehouck, Pieter; Grimalt, Susana; Dabrio, Marta; Cordeiro, Fernando; Fiamegos, Yiannis; Robouch, Piotr; Fernández-Alba, Amadeo R; de la Calle, Beatriz

    2015-05-22

    This manuscript presents the results of the International Measurement Evaluation Programme 37 (IMEP-37) study, a proficiency test (PT) which was organised to assess the world-wide performance of food control laboratories on the determination of pesticide residues in grapes. This PT supports the implementation of Regulation (EC) No 396/2005 on maximum residue levels of pesticides in or on food and feed of plant and animal origin. Eighty-one participants reported results, forty from EU Member States and forty-one from outside the EU. The test item was a grape sample spiked with 20 selected pesticides. The results of the participants were rated with z- and zeta (ζ-) scores in accordance with ISO 13528 and ISO 17043. The standard deviation for the proficiency assessment, σˆ, of this PT was set at 25% for the 20 measured pesticides based on previous experience with similar measurands. The results reported to IMEP-37 showed that the participants performed satisfactorily, ranging from 81% (carbendazim) to 97% (azoxystrobin, penconazole, pyrimethanil) of the participating laboratories. However, only 30% of the participants managed to analyze all pesticides satisfactorily. Overall, the performance of the participants in this PT was good but there is room for improvement in the development of multi-residue methods for the simultaneous analysis of a large number of pesticides with an increased accuracy. PMID:25888097

  4. Fast gas chromatography for pesticide residues analysis using analyte protectants.

    PubMed

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

    2008-04-01

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

  5. Pesticide residue in water--a challenging task in India.

    PubMed

    Agarwal, Akriti; Prajapati, Rajmani; Singh, Om Pal; Raza, S K; Thakur, L K

    2015-02-01

    Modern agriculture practices reveal an increase in use of pesticides to meet the food demand of increasing population which results in contamination of the environment. In India, crop production increased to 100 %, but the cropping area has increased marginally by 20 %. Pesticides have played a major role in achieving the maximum crop production but maximum usage and accumulation of pesticide residues is highly detrimental to aquatic and other ecosystem. Pesticide residues in drinking water have become a major challenge over the last few years. It has been monitored in public water supply resources in National capital territory, i.e., Delhi. Organochlorine pesticides (OCPs), mainly isomers of hexachlorohexane (HCH), dichloro-diphenyl-trichloroethane (DDT), endosulphan, endrin, aldrin, dieldrin, and heptachlore, were identified from potable water samples. Results suggested that continuous consumption of contaminated water can pose severe health threats to local residents of this area. Central Pollution Control Board (CPCB), Delhi, had found α and β isomers of endosulphan residues in the Yamuna river. High concentrations of γ-HCH (0.259 μg/l) and malathion (2.618 μg/l) were detected in the surface water samples collected from the river Ganga in Kanpur, Uttar Pradesh (UP). High concentration of methyl parathion, endosulfan, and DDT were observed in water samples collected from the river at Bhagalpur, Bihar. The Industrial Toxicology Research Centre (ITRC), Lucknow (UP) study also found 0.5671 ppb concentrations of endosulfan in the river at Allahabad, UP. Similar results were found in other water samples in India. PMID:25638058

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

    PubMed

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

    2016-03-01

    Performance of compost and biochar amendments for in situ risk mitigation of aged DDT, DDE and dieldrin residues in an old orchard soil was examined. The change in bioavailability of pesticide residues to Lumbricus terrestris L. relative to the unamended control soil was assessed using 4-L soil microcosms with and without plant cover in a 48-day experiment. The use of aged dairy manure compost and biosolids compost was found to be effective, especially in the planted treatments, at lowering the bioavailability factor (BAF) by 18-39%; however, BAF results for DDT in the unplanted soil treatments were unaffected or increased. The pine chip biochar utilized in this experiment was ineffective at lower the BAF of pesticides in the soil. The US EPA Soil Screening Level approach was used with our measured values. Addition of 10% of the aged dairy manure compost reduced the average hazard quotient values to below 1.0 for DDT + DDE and dieldrin. Results indicate this sustainable approach is appropriate to minimize risks to wildlife in areas of marginal organochlorine pesticide contamination. Application of this remediation approach has potential for use internationally in areas where historical pesticide contamination of soils remains a threat to wildlife populations. PMID:26716732

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

    USGS Publications Warehouse

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

    2015-01-01

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

  8. Pesticide Residues and Bees – A Risk Assessment

    PubMed Central

    Sanchez-Bayo, Francisco; Goka, Koichi

    2014-01-01

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

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

    PubMed

    Sanchez-Bayo, Francisco; Goka, Koichi

    2014-01-01

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

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

    PubMed

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

    2016-01-01

    Pesticide residues in fruits and vegetables are among the primary sources of pesticide exposure through diet, but the lack of adequate measurements hinder the research on health effects of pesticide residues. Pesticide Residue Burden Score (PRBS) for estimating overall dietary pesticide intake, organochlorine pesticide score (OC-PRBS) and organophosphate pesticide score (OP-PRBS) for estimating organochlorine and organophosphate pesticides-specific intake, respectively, were derived using U.S. Department of Agriculture Pesticide Data Program data and National Health and Nutrition Examination Survey (NHANES) food frequency questionnaire data. We evaluated the performance of these scores by validating the scores against pesticide metabolites measured in urine or serum among 3,679 participants in NHANES using generalized linear regression. The PRBS was positively associated with a score summarizing the ranks of all pesticide metabolites in a linear fashion (p for linear trend <0.001). Furthermore, individuals in the top quintile of this score had urinary pesticide metabolite levels 13.0% (95% CI 8.3%-17.7%) higher than individuals in the lowest quintile. Similarly, we observed significant associations of the OC-PRBS and OP-PRBS with the levels of lipid-adjusted total serum organochlorine pesticides and urinary creatinine-adjusted organophosphate pesticides, respectively. The relative difference (RD) in average pesticide metabolite rank between extreme quintiles was 17.8% (95% CI: 11.1%-24.4%, p for trend <0.001) for the OP-PRBS, whereas the RD was marginally significant at 7.0% (95% CI: -0.5%-14.4%, p for trend 0.07) for the OC-PRBS. The PRBS and OP-PRBS had similar performance when they were derived from fruits and vegetables with high vs. low pesticide residues, respectively (p for trend <0.001 for all associations). The OP-PRBS was associated with all measured organophosphate pesticides, whereas the positive association between OC-PRBS and averaged measured

  11. Organochlorine pesticide residues in chicken eggs: a survey.

    PubMed

    Kahunyo, J M; Froslie, A; Maitai, C K

    1988-01-01

    One hundred and five chicken egg samples were taken from seven geographical locations in Kenya and analyzed for organochlorine pesticide residues using gas-liquid chromatography. Nine organochlorine compounds were detected: alpha- and gamma-HCH/BHC (hexachlorocyclohexane/benzene hexachloride), aldrin, dieldrin, p,p'-DDE [1,1-dichloro-2,2-bis(p-chlorophenyl)ethylene], p,p'-DDD (TDE) [2,2-bis(p-chlorophenyl)-1,1-dichloroethane] (tetrachlorodiphenylethane), o,p'-DDD [2-(o-chlorophenyl)-2-(p-chlorophenyl)-1,1-dichloroethane], o,p'-DDT [2-(o-chlorophenyl)-2-(p-chlorophenyl)-1,1,1-trichloroethane], and p,p'-DDT. Eighteen of the samples contained DDT levels exceeding the practical residue limit (0.5 ppm). The mean DDT residue content was 0.68 ppm, a result influenced greatly by the high contamination in the 18 samples. Both individual and mean residue levels for other organochlorine pesticides detected were well within the respective practical residue limits. PMID:3411637

  12. Pesticide residues in food--acute dietary exposure.

    PubMed

    Hamilton, Denis; Ambrus, Arpád; Dieterle, Roland; Felsot, Allan; Harris, Caroline; Petersen, Barbara; Racke, Ken; Wong, Sue-Sun; Gonzalez, Roberto; Tanaka, Keiji; Earl, Mike; Roberts, Graham; Bhula, Raj

    2004-04-01

    Consumer risk assessment is a crucial step in the regulatory approval of pesticide use on food crops. Recently, an additional hurdle has been added to the formal consumer risk assessment process with the introduction of short-term intake or exposure assessment and a comparable short-term toxicity reference, the acute reference dose. Exposure to residues during one meal or over one day is important for short-term or acute intake. Exposure in the short term can be substantially higher than average because the consumption of a food on a single occasion can be very large compared with typical long-term or mean consumption and the food may have a much larger residue than average. Furthermore, the residue level in a single unit of a fruit or vegetable may be higher by a factor (defined as the variability factor, which we have shown to be typically x3 for the 97.5th percentile unit) than the average residue in the lot. Available marketplace data and supervised residue trial data are examined in an investigation of the variability of residues in units of fruit and vegetables. A method is described for estimating the 97.5th percentile value from sets of unit residue data. Variability appears to be generally independent of the pesticide, the crop, crop unit size and the residue level. The deposition of pesticide on the individual unit during application is probably the most significant factor. The diets used in the calculations ideally come from individual and household surveys with enough consumers of each specific food to determine large portion sizes. The diets should distinguish the different forms of a food consumed, eg canned, frozen or fresh, because the residue levels associated with the different forms may be quite different. Dietary intakes may be calculated by a deterministic method or a probabilistic method. In the deterministic method the intake is estimated with the assumptions of large portion consumption of a 'high residue' food (high residue in the sense

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

    EPA Science Inventory

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

  14. Level of organochlorine pesticide residues in dry fruit nuts.

    PubMed

    Pandey, Pragya; Raizada, R B; Srivastava, L P

    2010-09-01

    The use of pesticides on cash crops and exportable food commodities had always been a serious concern. Fruits form one of the important constituents of human diet, in that they give one third of the requirement of calories, vitamins, and minerals. This study has been carried out to determine the level of organochlorine pesticides namely HCH, DDT and Endosulfan in raw fruit nuts. Nuts have proteins and high level of fat content. These properties of nuts attract organochlorine pesticides to accumulate. The analysis of organochlorine pesticide residues in commonly used dry fruits like Cashewnut, Walnut, Coconut, Chilgoza, Chironji, Makhana, Resins, Apricot, Almonds, Date palm, Pistachio nut collected from local market of Lucknow India has indicated presence of very low level of HCH (0.007-1.328 mg kg(-1)), DDT(ND-0.140 mg kg(-1)) and Endosulfan (ND-0.091 mg kg(-1)). There are no MRL values established for nuts in the country. This finding is based on a smaller number of samples, which however suggest that the presence of low level of DDT, HCH and Endosulfan might be due to environmental rather than direct exposure. PMID:21387926

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

    PubMed

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

    2008-12-01

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

  16. Pesticide residue determination in vegetables from western China applying gas chromatography with mass spectrometry.

    PubMed

    Qin, Guofu; Zou, Keting; Li, Yongbo; Chen, Yan; He, Fengrui; Ding, Guirong

    2016-09-01

    In this study,an effort has been made to evaluate the pesticide residues in vegetables from western China. Fifty-one pesticides, including organophosphorus, organochlorine, carbamate and pyrethroid, were detected in 369 commonly used vegetables by GC-MS. Concentrations of organophosphorus pesticides were detected ranging from 0.0008 to 18.8200 mg/kg, among which organophosphorus pesticide concentrations exceeded their maximum residue levels (MRLs) in five samples. Carbamate and organochlorine pesticides were determined to have concentrations in the range of 0.0012-0.7928 mg/kg. The residual concentrations of carbamate pesticides in six samples and organochlorine pesticides in four samples exceeded their MRLs. The residual concentrations of five pyrethroid pesticides were within the range of 0.0016-6.0827 mg/kg and the pyrethroid residues in two samples exceeded their MRLs. The results revealed that pesticide residues in 70.73% of the vegetables samples were not detected, while in the rest of vegetables there were one or more pesticide residues and some even exceeded their MRLs, which would threaten the health of consumers. Our work provides significant information for the food safety regulations to control the excessive use of some pesticides on those kinds of vegetables from western China. Copyright © 2016 John Wiley & Sons, Ltd. PMID:26864471

  17. 77 FR 8755 - Receipt of a Pesticide Petition Filed for Temporary Tolerance Exemption for Residues of...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-02-15

    ... Residues of Prohydrojasmon in or on Various Commodities AGENCY: Environmental Protection Agency (EPA... residues of pesticide chemicals in or on various commodities. DATES: Comments must be received on or before... modification of a regulation in 40 CFR part 180 for residues of pesticide chemicals in or on various...

  18. Some organochlorine pesticide residues in fish species in Konya, Turkey.

    PubMed

    Kalyoncu, Leyla; Agca, Ihsan; Aktumsek, Abdurrahman

    2009-02-01

    The levels of organochlorine pesticides were measured in 18 fish species from Konya markets, Turkey. These species were selected on the basis of their importance to local human fish consumption. The extracted residues were analyzed on a micro capillary gas chromatograph equipped with an electron capture detector. Total 14 different organochlorine pesticides were determined. These residues were detected in all fish species, except in trout, horse mackerel and bonito. DDT and its metabolites and HCH were the predominant contaminants in fish muscles. The mean concentrations of summation operator DDT were in the range between 0.0008 and 0.0828 microg g(-1). DDT was the predominant residue in Sparus aurata. Detectable levels of HCH, aldrin, and heptachlor were found in most samples. However, dieldrin, endrin, beta endosulfan, p-p' DDT, and p-p' DDD were not found in Salmo trutta. The mean of endrin ranged from 0.0040 microg g(-1) (Triglia lineate) to 0.0326 microg g(-1) (Trachurus trachurus). These results give no indication of important health risks associated with the consumption of these fishes in Konya markets. PMID:19103455

  19. Monitoring of organochlorine pesticides residues in green mussels (Perna viridis) from the coastal area of Thailand.

    PubMed

    Boonyatumanond, Ruchaya; Jaksakul, Areerat; Puncharoen, Pornthip; Tabucanon, Monthip Sriratana

    2002-01-01

    The utilization of organochlorine pesticides for pest control chemical has been of great interest on residue contamination from biological organisms in the environment. Green mussel (Perna viridis) samples were monitored as bioindicators for assessment of the water quality in coastal waters along the Gulf of Thailand. Thirty-six samples were collected from 12 stations during 1997-1999 and analysed for 26 organochlorine pesticide compounds. This paper focuses on the contamination of organochlorine pesticide residues in green mussel (P. viridis) during 1997-1999. The limit of detection of all organochlorine pesticides compounds was at the range of 0.1-8.3 ng g(-1) wet weight and recovery 75-95%. The concentration of organochlorine pesticides residues in green mussel was lower than the maximum residue limit for aquatic animals as recommended by the Ministry of Public Health of Thailand. The trend of organochlorine pesticide residue contamination in this area decreased from 1989 to 1999. PMID:12152831

  20. 7 CFR 29.429 - Disposition of imported tobacco exceeding pesticide residue standards.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... 7 Agriculture 2 2012-01-01 2012-01-01 false Disposition of imported tobacco exceeding pesticide... Disposition of imported tobacco exceeding pesticide residue standards. Within 10 days of the receipt of test results from pesticide test samples, the Director shall notify the importer or entity responsible for...

  1. 7 CFR 29.429 - Disposition of imported tobacco exceeding pesticide residue standards.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 7 Agriculture 2 2011-01-01 2011-01-01 false Disposition of imported tobacco exceeding pesticide... Disposition of imported tobacco exceeding pesticide residue standards. Within 10 days of the receipt of test results from pesticide test samples, the Director shall notify the importer or entity responsible for...

  2. 7 CFR 29.429 - Disposition of imported tobacco exceeding pesticide residue standards.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... 7 Agriculture 2 2014-01-01 2014-01-01 false Disposition of imported tobacco exceeding pesticide... Disposition of imported tobacco exceeding pesticide residue standards. Within 10 days of the receipt of test results from pesticide test samples, the Director shall notify the importer or entity responsible for...

  3. 7 CFR 29.429 - Disposition of imported tobacco exceeding pesticide residue standards.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 7 Agriculture 2 2013-01-01 2013-01-01 false Disposition of imported tobacco exceeding pesticide... Disposition of imported tobacco exceeding pesticide residue standards. Within 10 days of the receipt of test results from pesticide test samples, the Director shall notify the importer or entity responsible for...

  4. 7 CFR 29.429 - Disposition of imported tobacco exceeding pesticide residue standards.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 7 Agriculture 2 2010-01-01 2010-01-01 false Disposition of imported tobacco exceeding pesticide... Disposition of imported tobacco exceeding pesticide residue standards. Within 10 days of the receipt of test results from pesticide test samples, the Director shall notify the importer or entity responsible for...

  5. Organochlorine pesticide residues in human fat in the United Kingdom 1976-7.

    PubMed Central

    Abbott, D C; Collins, G B; Goulding, R; Hoodless, R A

    1981-01-01

    Between May 1976 and August 1977 samples of human body fat were taken during routine necropsies in the United Kingdom on 236 subjects aged over 5 years and four infants aged under 4 months. Comparison with results from earlier studies showed a further decline in residues of pp'-dichlorodiphenyltrichloroethane (pp'-DDT) and dieldrin (HEOD) and increased amounts of hexachlorobenzene residues; concentrations of other compounds were similar to those observed in the studies carried out in 1963-4, 1965-7, and 1969-71. Comparison of the data with those from other countries, showed that the concentrations of organochlorine pesticide residues and polychlorobiphenyls in human fat samples from residents of the United Kingdom remain among the lowest in Europe and, indeed, the world. PMID:6797569

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

    PubMed Central

    Centner, Terence; Eberhart, Nicholas

    2014-01-01

    Agricultural producers and public health authorities apply pesticides to control pests that damage crops and carry diseases. Due to the toxic nature of most pesticides, they are regulated by governments. Regulatory provisions require pesticides to be registered and restrictions operate to safeguard human health and the environment. Yet pesticides used near surface waters pose dangers to non-target species and drinking water supplies leading some governments to regulate discharges of pesticides under pollution discharge permits. The dual registration and discharge permitting provisions are burdensome. In the United States, agricultural interest groups are advancing new legislation that would exempt pesticide residues from water permitting requirements. An analysis of the dangers posed by pesticide residues in drinking water leads to a conclusion that both pesticide registration and pollutant discharge permitting provisions are needed to protect human health and aquatic species. PMID:24814945

  7. Requiring pollutant discharge permits for pesticide applications that deposit residues in surface waters.

    PubMed

    Centner, Terence; Eberhart, Nicholas

    2014-05-01

    Agricultural producers and public health authorities apply pesticides to control pests that damage crops and carry diseases. Due to the toxic nature of most pesticides, they are regulated by governments. Regulatory provisions require pesticides to be registered and restrictions operate to safeguard human health and the environment. Yet pesticides used near surface waters pose dangers to non-target species and drinking water supplies leading some governments to regulate discharges of pesticides under pollution discharge permits. The dual registration and discharge permitting provisions are burdensome. In the United States, agricultural interest groups are advancing new legislation that would exempt pesticide residues from water permitting requirements. An analysis of the dangers posed by pesticide residues in drinking water leads to a conclusion that both pesticide registration and pollutant discharge permitting provisions are needed to protect human health and aquatic species. PMID:24814945

  8. Organochlorine and organophosphorus pesticide residues in raw buffalo milk from agroindustrial areas in Assiut, Egypt.

    PubMed

    Shaker, Eman M; Elsharkawy, Eman E

    2015-01-01

    Raw buffalo milk samples from the agroindustrial zone in upper Egypt were analyzed for the presence of organochlorine and organophosphorus pesticides using gas chromatography-mass spectroscopy. Five organochlorine pesticides namely, alachlor, dieldrin, hexachlorobenzene, lindane and methoxychlor and three organophosphorus pesticides chlorpyrifos, malathion, and parathion-methyl were detected in the milk samples. In 44% of the samples, the concentrations of lindane and malathion residues exceeded tolerance levels set by the European Commission (EC) in 2008. In addition, the concentrations of chlorpyrifos, methoxychlor, and hexachlorobenzene residues exceeded the 2008 EC maximum residual limits (MRLs) by 33, 66, and 88% of the examined samples, respectively. However, the levels of alachlor, dieldrin, and parathion-methyl residues were below EC MRLs. The results of this study confirm the risks of pesticide residues exposure that threaten consumer health in Egypt. Thus, we recommend that pesticide residue monitoring programs be instituted in all the developing countries. PMID:25575291

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

    PubMed

    Bajwa, Usha; Sandhu, Kulwant Singh

    2014-02-01

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

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

    PubMed

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

    2009-06-01

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

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

    PubMed

    Angioni, Alberto; Dedola, Fabrizio

    2013-05-01

    This paper reports the results of a pesticide monitoring survey on wine grapes from the 2008-2010 vintage from vineyards grown according to integrated pest management strategies. A multi-residue gas chromatography-mass spectrometry method in electron ionization and chemical ionization mode has been used for the determination of 30 pesticides in wine samples. The analytical method showed good recoveries and allowed a good separation of the selected pesticides. Repeatability and intermediate precision showed good results with CV < 20 %. The instrumental method limits of determination (LOD) and of quantification (LOQ) were below the maximum residue levels set in wine. The analysis of the wines showed that pesticide residues were below the instrumental LOQ, and most of them were undetectable (pesticide applied has been detected in at least one cultivar. Metalaxil, myclobutanil, and penconazole were the pesticides most frequently found, while carignano and vermentino were the cultivars with the higher number of residues. PMID:22976121

  12. Health risk for children and adults consuming apples with pesticide residue.

    PubMed

    Lozowicka, Bozena

    2015-01-01

    The presence of pesticide residues in apples raises serious health concerns, especially when the fresh fruits are consumed by children, particularly vulnerable to the pesticide hazards. This study demonstrates the results from nine years of investigation (2005-2013) of 696 samples of Polish apples for 182 pesticides using gas and liquid chromatography and spectrophotometric techniques. Only 33.5% of the samples did not contain residues above the limit of detection. In 66.5% of the samples, 34 pesticides were detected, of which maximum residue level (MRL) was exceeded in 3%. Multiple residues were present in 35% of the samples with two to six pesticides, and one sample contained seven compounds. A study of the health risk for children, adults and the general population consuming apples with these pesticides was performed. The pesticide residue data have been combined with the consumption of apples in the 97.5 percentile and the mean diet. A deterministic model was used to assess the chronic and acute exposures that are based on the average and high concentrations of residues. Additionally, the "worst-case scenario" and "optimistic case scenario" were used to assess the chronic risk. In certain cases, the total dietary pesticide intake calculated from the residue levels observed in apples exceeds the toxicological criteria. Children were the group most exposed to the pesticides, and the greatest short-term hazard stemmed from flusilazole at 624%, dimethoate at 312%, tebuconazole at 173%, and chlorpyrifos methyl and captan with 104% Acute Reference Dose (ARfD) each. In the cumulative chronic exposure, among the 17 groups of compounds studied, organophosphate insecticides constituted 99% acceptable daily intake (ADI). The results indicate that the occurrence of pesticide residues in apples could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring and tighter regulation of pesticide residues is recommended. PMID

  13. Distribution of pesticide residues within homes in central New York State.

    PubMed

    Obendorf, S K; Lemley, A T; Hedge, A; Kline, A A; Tan, K; Dokuchayeva, T

    2006-01-01

    Residues for 17 pesticides were analyzed in 41 households in central New York State that represented farm, rural, and urban houses. Samples were taken in both summer and winter of 2000-2001 from the same households from four locations; family room carpet; adjacent smooth floor; flat tabletop surface; and settled dust collected in a Petri dish on a tabletop. Pesticide residues were analyzed to identity factors that influence both the transport into and the redistribution of pesticides in the indoor environment. Differences were observed between the various pesticides and pesticide classifications relative to location within and between households as well as by season. Variations in the pesticide residues were related to a number of factors. Higher residues were observed in the farm households, particularly in summer, with the highest amount observed for chloropyrifos in carpet (33 microg/m2). For many pesticides, the frequency of detection and the amount of residues were higher in summer, which relates to usage patterns in agriculture and horticulture; however, larger amounts of insecticides such as mecoprop, resmethrin, and tetramethrin were found on flat surfaces in winter, indicating household use and possible redistribution within the home. Distribution patterns suggest that routines within a household may cause high variation in residues; these practices include indoor pets and treatment for fleas and ticks, use of termiticides, and fastidiousness of occupants. Frequency of pesticide detection was highest in carpet for both summer and winter for all households, indicating that carpets hold pesticides over time. Adsorbent fibrous materials such as textiles hold pesticides by macro- and micro-occlusion in their complex structures. Amounts of pesticide residue were higher in carpets than on smooth floors, particularly for rural farm households where the farmer was a certified pesticide applicator. The maximum amount of pesticide residue on a smooth floor surface

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

    PubMed

    Sungur, Sana; Tunur, Cetin

    2012-01-01

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

  15. Pesticides

    MedlinePlus

    ... ACMT Recognition Awards Annual Scientific Meeting Travel Scholarships Pesticides Public Health > Public > Toxicology FAQ's > Pesticides Pesticides What are pesticides ? How do pesticides work ? How ...

  16. Acute intake assessment: evolution within the Codex Committee on Pesticide Residues. WHO Joint Secretary of the Joint FAO/WHO meeting on pesticide residues JMPR.

    PubMed

    Herrman, J L

    2000-07-01

    The Codex Committee on Pesticide Residues (CCPR), in its development of international standards, has been considering during the last few years the implications of residues of acutely toxic pesticides in food commodities. CCPR has asked its scientific advisory body, the Joint FAO/WHO Meeting on Pesticide Residues (JMPR), for advice on the safety of the standards that are being developed. This work began in 1993. The 1994 JMPR first decided to use the 'acute reference dose' as a toxicological benchmark for a 'short-term ADI'. A number of acute reference doses have been allocated at subsequent meetings. The 1998 JMPR decided to consider the allocation of an acute reference dose whenever a full evaluation of a pesticide is undertaken. General guidance for the allocation of an acute reference dose was provided by the 1998 JMPR, which is discussed in this paper. PMID:10983577

  17. A survey of organochlorine pesticide residues in cheese samples from three Mexican regions.

    PubMed

    Albert, L A; Alpuche, L; Bárcenas, C; Rendón, J

    1990-01-01

    Organochlorine pesticide residues were determined in cheese samples from three Mexican regions. All samples were found to be contaminated by these residues: p,p'-DDE was present in 100% of the samples. Other pesticides found with high frequencies were HCB, three of the BHC isomers, as well as heptachlor and its epoxide. Also found, although less frequently, were residues of p,p'-DDD, p,p'-DDT, aldrin, dieldrin and endrin. Samples from the region known as Comarca Lagunera had the highest number of pesticides per sample. The highest concentrations of residues were found in cheese samples from the Soconusco and the Comarca Lagunera regions. PMID:15092270

  18. 7 CFR 29.425 - Submission and disposition of pesticide residues and end user(s) certification.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 7 Agriculture 2 2011-01-01 2011-01-01 false Submission and disposition of pesticide residues and... Miscellaneous § 29.425 Submission and disposition of pesticide residues and end user(s) certification. (a) Completion of certification: The importer shall complete a pesticide residue and end user(s) certification...

  19. 7 CFR 29.425 - Submission and disposition of pesticide residues and end user(s) certification.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... 7 Agriculture 2 2014-01-01 2014-01-01 false Submission and disposition of pesticide residues and... Miscellaneous § 29.425 Submission and disposition of pesticide residues and end user(s) certification. (a) Completion of certification: The importer shall complete a pesticide residue and end user(s) certification...

  20. 7 CFR 29.425 - Submission and disposition of pesticide residues and end user(s) certification.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... 7 Agriculture 2 2012-01-01 2012-01-01 false Submission and disposition of pesticide residues and... Miscellaneous § 29.425 Submission and disposition of pesticide residues and end user(s) certification. (a) Completion of certification: The importer shall complete a pesticide residue and end user(s) certification...

  1. 7 CFR 29.425 - Submission and disposition of pesticide residues and end user(s) certification.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 7 Agriculture 2 2013-01-01 2013-01-01 false Submission and disposition of pesticide residues and... Miscellaneous § 29.425 Submission and disposition of pesticide residues and end user(s) certification. (a) Completion of certification: The importer shall complete a pesticide residue and end user(s) certification...

  2. 7 CFR 29.425 - Submission and disposition of pesticide residues and end user(s) certification.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 7 Agriculture 2 2010-01-01 2010-01-01 false Submission and disposition of pesticide residues and... Miscellaneous § 29.425 Submission and disposition of pesticide residues and end user(s) certification. (a) Completion of certification: The importer shall complete a pesticide residue and end user(s) certification...

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

    PubMed

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

    2003-11-01

    The effects of washing, storing, boiling, peeling, coring and juicing on pesticide residue were investigated for field-sprayed Discovery and Jonagold apples. Residues of chlorpyrifos, cypermethrin, deltamethrin, diazinon, endosulfan, endosulfan sulfate, fenitrothion, fenpropathrin, iprodione, kresoxim-methyl, lambda-cyhalothrin, quinalphos, tolylfluanid and vinclozolin in the processed apples were analysed by gas chromatography. Statistical analysis showed that reductions of 18-38% were required to obtain significant effects of processing practices, depending on pesticide and apple variety. Juicing and peeling the apples significantly reduced all pesticide residues. In the case of detectable pesticide residues, 1-24% were distributed in the juice and in the peeled apple. None of the pesticide residues was significantly reduced when the apples were subject to simple washing or coring. Storing significantly reduced five of the pesticide residues: diazinon, chlorpyrifos, fenitrothion, kresoxim-methyl and tolylfluanid, by 25-69%. Residues of the metabolite endosulfan sulfate were increased by 34% during storage. Boiling significantly reduced residues of fenitrothion and tolylfluanid by 32 and 81%, respectively. Only a few of the observed effects of processing could be explained by the physical or chemical characteristics of the pesticides. No differences in effect of processing due to apple variety were identified. PMID:14668155

  4. Monitoring of pesticide residues in human breast milk from Punjab, India and its correlation with health associated parameters.

    PubMed

    Sharma, Anupama; Gill, J P S; Bedi, J S; Pooni, P A

    2014-10-01

    This study was undertaken to determine the present status of pesticide residues in breast milk from Punjab. A total of 127 breast milk samples were analyzed and pesticide residues were detected in 25 % of the milk samples. Residues of cyfluthrin, fenvalerate, cypermethrin, profenophos, γ-HCH, β-HCH, chlorpyriphos, monocrotophos, p,p' DDE and phosalone were detected with mean levels of 63.04, 11.69, 3.63, 2.66, 2.64, 2.29, 1.91, 1.63, 0.56 and 0.29 ng g(-1), respectively. Cyfluthrin was leading pesticide detected in breast milk contributing 31.28 % to the total residue load. It was observed that the residue levels were decreasing with increase in parity and age of mother and cyfluthrin had highest mean concentration of 90.63 ng g(-1) in the first parity and 21.11 ng g(-1) in youngest age group. Residue levels were higher in urban population than the rural population although, statistically non-significant difference was found between the two (p > 0.05). PMID:25011502

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

    PubMed

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

    2014-10-01

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

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

    SciTech Connect

    Armour, M.A.; Nelson, C.; Sather, P. Briker, Y.

    1996-12-31

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

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

    PubMed

    Yahia, Doha; Elsharkawy, Eman E

    2014-01-01

    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. PMID:23911921

  8. Determination of some organochlorine pesticide residues in honeys from Konya, Turkey.

    PubMed

    Yavuz, Halil; Guler, Gokalp O; Aktumsek, Abdurrahman; Cakmak, Yavuz S; Ozparlak, Haluk

    2010-09-01

    In this study, 24 organochlorine pesticide residues in 109 different honey samples collected from stores and open markets in Konya, Turkey were analyzed by gas chromatography-electron capture detection. Aldrin, cis-chlordane, trans-chlordane, oxy-chlordane, 2,4(')-DDE, and 4,4(')-DDE were found in all honey samples. The mean value was 0.0540 microg g(-1) for oxy-chlordane. In the 55 samples of 109, levels of organochlorine pesticide residues of oxy-chlordane were determined as higher than those of Turkish Alimentarius Codex maximum residual limits (MRLs). Other organochlorine pesticide residues also exceeded MRLs except for cis-heptachlor epoxide and alpha-hexachlorocyclohexane. Since all of the honey samples are found contaminated and most of these samples exceeded MRLs, a control of organochlorine pesticide residues in honey is necessary for consumer health. PMID:19685151

  9. Pesticide residues in market foods in Shaanxi Province of China in 2010.

    PubMed

    Wang, Shumei; Wang, Zhilun; Zhang, Yibei; Wang, Jiang; Guo, Rong

    2013-06-01

    The aim of this study was to investigate the pesticide residues in market vegetables in Shaanxi Province of China. The concentrations of 33 pesticides were determined by gas chromatography (GC) in 285 samples. Ten organophosphorus pesticides (OPs) were found in concentrations ranging from 0.004 to 0.257 mg/kg. The mean levels of omethoate, phorate, chlorpyrifos, methidathion, ethoprophos in vegetables exceeded the maximum residue limits (MRLs) allowed by the Ministry of Health, of China. Other detectable OP pesticide residues levels were below their MRLs. Dicofol were detectable in green pepper and chives samples. Five pyrethroid pesticides (PYRs) were detectable in vegetable samples respectively. The results provide useful information on the current contamination status of a key agricultural area in China, and point to the need for urgent action to control the excessive use of some chemicals. PMID:23411338

  10. Adverse effects of pesticides residues on biochemical markers in pakistani tobacco farmers.

    PubMed

    Khan, Dilshad A; Bhatti, Mahwish M; Khan, Farooq A; Naqvi, Syed T; Karam, A

    2008-01-01

    Tobacco is an important cash crop of Pakistan and tremendous amount of irrational pesticides are being used to control insect growth. The frequency of plasma pesticide residues above acceptable daily intake (ADI) and its correlation with biochemical markers for assessment of adverse health effects in the tobacco farmers at district Sawabi, Pakistan was determined. Total 109 adult males consisting of 55 tobacco farmers exposed to pesticides and 54 controls were included. Pesticides residues in blood were analyzed on HPLC and GC-NPD. Plasma butyrylcholinesterase (BChE) was analyzed by Ellman's method. Biochemical markers including serum calcium, phosphorus, urea, creatinine, bilirubin and liver enzymes were measured on Selectra-E auto analyzer. The tobacco farmers had multiple pesticides residues above ADI in their blood consisting of 35 (63%) methomyl; 31 (56%) thiodicarb; 34(62%) cypermethrin; 27 (49%) Imidacloprid; 18 (32%) Methamidophos and 15 (27%) endosulfan. BChE activity was significantly decreased in the pesticides exposed farmers as compared to controls (P<0.001). Plasma biochemical markers including ALT, AST, CK, LDH and phosphate were significantly raised in the pesticides exposed farmers as compared to control group (P<0.001). Total pesticides residues revealed a significant positive correlation with AST (r=0.42), LDH(r= 0.47), ALT (r=0.20) and phosphorus (r=0.51). Excessive exposure to pesticide caused cytotoxic changes in the hepatic and renal biochemical markers which were positively correlated with pesticide residue. Hence these biomarkers might be used in addition to BChE activity for monitoring of adverse effects of pesticides on the health of farm workers. PMID:19079663

  11. Adverse Effects of Pesticides Residues on Biochemical Markers in Pakistani Tobacco Farmers

    PubMed Central

    Khan, Dilshad A; Bhatti, Mahwish M; Khan, Farooq A; Naqvi, Syed T; Karam, A

    2008-01-01

    Tobacco is an important cash crop of Pakistan and tremendous amount of irrational pesticides are being used to control insect growth. The frequency of plasma pesticide residues above acceptable daily intake (ADI) and its correlation with biochemical markers for assessment of adverse health effects in the tobacco farmers at district Sawabi, Pakistan was determined. Total 109 adult males consisting of 55 tobacco farmers exposed to pesticides and 54 controls were included. Pesticides residues in blood were analyzed on HPLC and GC-NPD. Plasma butyrylcholinesterase (BChE) was analyzed by Ellman's method. Biochemical markers including serum calcium, phosphorus, urea, creatinine, bilirubin and liver enzymes were measured on Selectra-E auto analyzer. The tobacco farmers had multiple pesticides residues above ADI in their blood consisting of 35 (63%) methomyl; 31 (56%) thiodicarb; 34(62%) cypermethrin; 27 (49%) Imidacloprid; 18 (32%) Methamidophos and 15 (27%) endosulfan. BChE activity was significantly decreased in the pesticides exposed farmers as compared to controls (P<0.001). Plasma biochemical markers including ALT, AST, CK, LDH and phosphate were significantly raised in the pesticides exposed farmers as compared to control group (P<0.001). Total pesticides residues revealed a significant positive correlation with AST (r=0.42), LDH(r= 0.47), ALT (r=0.20) and phosphorus (r=0.51). Excessive exposure to pesticide caused cytotoxic changes in the hepatic and renal biochemical markers which were positively correlated with pesticide residue. Hence these biomarkers might be used in addition to BChE activity for monitoring of adverse effects of pesticides on the health of farm workers. PMID:19079663

  12. Environmental impact and remediation of residual lead and arsenic pesticides in soil

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Lead arsenate (PbHAsO4) was used as a pesticide for over 50 years in orchards throughout the world, and residual lead and arsenic have been found in high concentrations in these orchard soils long after the pesticide use ended. These high concentrations of lead and arsenic may create a potential ri...

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  15. MONITORING THE TRANSFER OF PESTICIDE RESIDUES FROM SOFT SURFACES TO FOODS

    EPA Science Inventory

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

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

    PubMed Central

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

    2010-01-01

    Background The data presented here are a response to calls for more direct measurements of pesticide residues in foods consumed by children and provide an opportunity to compare direct measures of pesticide residues in foods representing actual consumption with those reported by the U.S. Department of Agriculture Pesticide Data Program. Objective We measured pesticide residues in 24-hr duplicate food samples collected from a group of 46 young children participating in the Children’s Pesticide Exposure Study (CPES). Methods Parents were instructed to collect 24-hr duplicate food samples of all conventional fruits, vegetables, and fruit juices equal to the quantity consumed by their children, similarly prewashed/prepared, and from the same source or batch. Individual or composite food items were analyzed for organophosphate (OP) and pyrethroid insecticide residues. Results We collected a total of 239 24-hr duplicate food samples collected from the 46 CPES children. We found 14% or 5% of those food samples contained at least one OP or pyrethroid insecticide, respectively. We measured a total of 11 OP insecticides, at levels ranging from 1 to 387 ng/g, and three pyrethroid insecticides, at levels ranging from 2 to 1,133 ng/g, in children’s food samples. We found that many of the food items consumed by the CPES children were also on the list of the most contaminated food commodities reported by the Environmental Working Group. Conclusions The frequent consumption of food commodities with episodic presence of pesticide residues that are suspected to cause developmental and neurological effects in young children supports the need for further mitigation. PMID:20639183

  17. STUDY TO IDENTIFY IMPORTANT PARAMETERS FOR CHARACTERIZING PESTICIDE RESIDUE TRANSFER EFFICIENCIES

    EPA Science Inventory

    To reduce the uncertainty associated with current estimates of children's exposure to pesticides by dermal contact and non-dietary ingestion, residue transfer data are required. Prior to conducting exhaustive studies, a screening study to identify the important parameters for...

  18. 40 CFR 180.7 - Petitions proposing tolerances or exemptions for pesticide residues in or on raw agricultural...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... exemptions for pesticide residues in or on raw agricultural commodities or processed foods. 180.7 Section 180.7 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS TOLERANCES AND EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Procedural Regulations § 180.7...

  19. 40 CFR 180.7 - Petitions proposing tolerances or exemptions for pesticide residues in or on raw agricultural...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... exemptions for pesticide residues in or on raw agricultural commodities or processed foods. 180.7 Section 180.7 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS TOLERANCES AND EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Procedural Regulations § 180.7...

  20. 40 CFR 180.7 - Petitions proposing tolerances or exemptions for pesticide residues in or on raw agricultural...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... exemptions for pesticide residues in or on raw agricultural commodities or processed foods. 180.7 Section 180.7 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS TOLERANCES AND EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Procedural Regulations § 180.7...

  1. 40 CFR 180.7 - Petitions proposing tolerances or exemptions for pesticide residues in or on raw agricultural...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... exemptions for pesticide residues in or on raw agricultural commodities or processed foods. 180.7 Section 180.7 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS TOLERANCES AND EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Procedural Regulations § 180.7...

  2. 40 CFR 180.7 - Petitions proposing tolerances or exemptions for pesticide residues in or on raw agricultural...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... exemptions for pesticide residues in or on raw agricultural commodities or processed foods. 180.7 Section 180.7 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS TOLERANCES AND EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Procedural Regulations § 180.7...

  3. Pesticide residue dynamics in passion fruits: comparing field trial and modelling results.

    PubMed

    Juraske, Ronnie; Fantke, Peter; Ramírez, Ana Cecilia Romero; González, Alonso

    2012-10-01

    We evaluated the exposure to pesticides from the consumption of passion fruits and subsequent human health risks by combining several methods: (i) experimental field studies including the determination of pesticide residues in/on passion fruits, (ii) dynamic plant uptake modelling, and (iii) human health risk assessment concepts. Eight commonly used pesticides were applied onto passion fruits cultivated in Colombia. Pesticide concentrations were measured periodically (between application and harvest) in whole fruits and fruit pulp. Measured concentrations were compared with predicted residues calculated with a dynamic and crop-specific pesticide uptake model, namely dynamiCROP. The model accounts for the time between pesticide application and harvest, the time between harvest and consumption, the amount of spray deposition on plant surfaces, uptake processes, dilution due to crop growth, degradation in plant components, and reduction due to food processing (peeling). Measured and modelled residues correspond well (r(2)=0.88-0.99), with all predictions falling within the 90% confidence interval of the measured values. A mean error of 43% over all studied pesticides was observed between model estimates and measurements. The fraction of pesticide applied during cultivation that is eventually ingested by humans is on average 10(-4)-10(-6), depending on the time period between application and ingestion and the processing step considered. Model calculations and intake fractions via fruit consumption based on experimental data corresponded well for all pesticides with a deviation of less than a factor of 2. Pesticide residues in fruits measured at recommended harvest dates were all below European Maximum Residue Limits (MRLs) and therefore do not indicate any violation of international regulatory thresholds. PMID:22673401

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

    PubMed Central

    2013-01-01

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

  5. Studies of pesticide residues in tomatoes and cucumbers from Kazakhstan and the associated health risks.

    PubMed

    Lozowicka, Bozena; Abzeitova, Elmira; Sagitov, Abai; Kaczynski, Piotr; Toleubayev, Kazbek; Li, Alina

    2015-10-01

    The aim of the present study was to assess the level of pesticide residues in vegetables in the Almaty Region of Kazakhstan and to determine the potential health risks associated with the exposures to these pesticides. A total of 82 samples of cucumbers and tomatoes from top agro-based market and greenhouses were analysed using a gas chromatography-micro electron capture detector/nitrogen-phosphorous detector (GC-μECD/NPD), a multiresidue method to analyse 184 different pesticide types. The results indicated that more than half of samples (59 %) contained 29 pesticides, in which 10 are not registered in Kazakhstan, ranging from 0.01 to 0.88 mg kg(-1), and 28 % contained pesticide residues above maximum residue levels (MRLs). The estimated daily intakes (EDIs) ranged from 0.01 % of the acceptable daily intake (ADI) for pyrimethanil to 12.05 % of the ADI for lambda-cyhalothrin. The most critical commodity is triazophos and flusilazole in tomatoes, contributing 70.8 and 42.5 % to the acute hazard index (aHI). The results provided important information on the current pesticide contamination status of two commonly consumed vegetables and pointed an urgent need to control the use of plant protection products applied, especially potentially persistent pesticides, such as endosulfan and dicofol. These results also show that the detected pesticides may be considered a public health problem. PMID:26337756

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

    PubMed

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

    2013-01-01

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

  7. Rapid detection of pesticide residue in apple based on Raman spectroscopy

    NASA Astrophysics Data System (ADS)

    Li, Yongyu; Sun, Yunyun; Peng, Yankun; Dhakal, Sagar; Chao, Kuanglin; Liu, Qiaoqiao

    2012-05-01

    The potential of Raman spectroscopy in the analysis of low concentration organic contaminants on apples' surface was evidenced in this study. Chlorpyrifos, an organophosphorus pesticide, was used as a probe for this purpose. The characteristic peaks of fingerprints of pesticide on an aluminum substrate and apple fruit cuticle without pesticide residue were acquired first. Then a concentration range of chlorpyrifos (commercial products at 40%) solutions were made using deionised and distilled water. Single 100 μL droplets of the chlorpyrifos solutions were placed gently on apple fruit cuticles and left to dry before analysis. Through comparative analysis of the Raman spectra data collected, 341, 632 and 1237cm-1 were identified to detect the chlorpyrifos pesticide residue on apple surface. Based on the relationship between the Raman intensity of the most prominent peak at around 632cm-1 and the pesticide concentrations, the limit of detection of ordinary Raman spectrum for chlorpyrifos was estimated to be 48ppm.

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

    NASA Astrophysics Data System (ADS)

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

    2009-04-01

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

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

    PubMed

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

    2013-01-01

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

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

    PubMed

    Łozowicka, B; Kaczyński, P; Jankowska, M; Rutkowska, E; Hrynko, I

    2012-01-01

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

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

    PubMed

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

    2014-01-01

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

  12. Risk assessment of the cumulative acute exposure of Hungarian population to organophosphorus pesticide residues with regard to consumers of plant based foods.

    PubMed

    Zentai, Andrea; Szabó, István J; Kerekes, Kata; Ambrus, Árpád

    2016-03-01

    Based on the Hungarian pesticide residues monitoring data of the last five years and the consumption data collected within a 3-day dietary record survey in 2009 (more than 2 million pesticide residue results and almost 5000, 0-101-year-old consumers 3 non-consecutive-day personal fruit and vegetable consumption data), the cumulative acute exposure of organophosphorus pesticide residues was evaluated. The relative potency factor approach was applied, with acephate chosen as index compound. According to our conservative calculation method, applying the measured residues only, the 99.95% of the 99th percentiles of calculated daily intakes was at or below 87 μg/kgbwday, indicating that the cumulative acute exposure of the whole Hungarian population (including all age classes) to organophosphorus compounds was not a health concern. PMID:26807885

  13. GC/MIP/AED method for pesticide residue determination in fruits and vegetables.

    PubMed

    Ting, K C; Kho, P

    1991-01-01

    This research describes the results of a gas chromatography/microwave induced plasma/atomic emission detection (GC/MIP/AED) method performed on a Hewlett-Packard 5921A system for pesticide residue analysis in fruits and vegetables. A total of 6 experiments were conducted: (1) sensitivity and linearity studies for elements S, P, Cl, and N by analyzing dursban; (2) a study of instrument response to Cl concentration in pesticide molecules; (3) organochlorinated pesticide recoveries; (4) organophosphate pesticide recoveries; (5) carbamate pesticide recoveries; and (6) investigation of metallic pesticides with plictran and vendex as standards. The rank according to sensitivity and linearity was found to be as follows: S-181 greater than P-178 greater than Cl-479 greater than N-174. Instrument response to the concentration of chlorine atoms in the pesticide molecule was linear, with a correlation coefficient of 0.89. Recoveries of organochlorinated pesticides were 91.7-109.3%, with the exception of citrus, whose recovery was affected by coeluting interferences. Organophosphate recoveries were 73.2% or higher, except for the cygon oxygen analog, which degraded in the GC system under all circumstances. Carbamate recoveries were inconsistent quantitatively; however, the information generated from elements N and S were useful for qualitative confirmation of other methods, such as LC postcolumn derivatization analysis. Overall, the GC/MIP/AED method is powerful for qualitative confirmation in pesticide residue analysis. The instrument's capability of acquiring multi-elements (Cl and P) selectively and accurately is an alternative method for organochlorinated and organophosphate pesticide residue analyses. In addition, the GC/MIP/AED system is easy to use, simple to maintain, and its chromatograms can be interpreted by any chromatography analyst without much prior training. PMID:1757425

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

    NASA Astrophysics Data System (ADS)

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

    2004-03-01

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

  15. Pesticides residues in milks and feedstuff of farm animals drawn from Greece.

    PubMed

    Tsiplakou, E; Anagnostopoulos, C J; Liapis, K; Haroutounian, S A; Zervas, G

    2010-07-01

    The objective of this study was to investigate if milk from dairy sheep and goats, fed mainly with supplementary feed during the winter months, was contaminated with pesticides residues. Tauwo hundred milk samples from sheep and goats were collected from 10 farms of each animals. The sheep and goats farms were selected from those which represent common conventional production and feeding systems in Greece. Milk and feed samples (alfalfa hay, wheat straw, shrubs, pasture and concentrates) were taken from each farm to analyze for pesticides residues. The results showed that the summation operatorendosulfan was the main pesticide residue which was detected in all the concentrates samples at a mean concentration of 5.36 mgkg(-1), which is much higher from the maximum residue level (MRL). In addition, the summation operatorendosulfan was also detected in all the alfalfa hay samples but at a mean concentration of 0.10 mgkg(-1) which is lower than the MRL. The mean concentrations of endosulfan alpha and beta were 2.82 and 2.39 mgkg(-1) in the concentrates samples and 0.08 and 0.02 mgkg(-1) respectively in alfalfa hay samples. In the wheat straw, shrubs and pasture samples no pesticides residues were detected. No pesticide residues were also detected in milk samples of sheep and goats. Thus, this milk from the farms sampled presents no human health risks as far as the contaminants analyzed concerned. PMID:20537679

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

    PubMed Central

    2012-01-01

    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. PMID:22293037

  17. Plant uptake of pesticides and human health: dynamic modeling of residues in wheat and ingestion intake.

    PubMed

    Fantke, Peter; Charles, Raphaël; de Alencastro, Luiz Felippe; Friedrich, Rainer; Jolliet, Olivier

    2011-11-01

    Human intake of pesticide residues from consumption of processed food plays an important role for evaluating current agricultural practice. We take advantage of latest developments in crop-specific plant uptake modeling and propose an innovative dynamic model to estimate pesticide residues in the wheat-environment system, dynamiCROP. We used this model to analyze uptake and translocation of pesticides in wheat after foliar spray application and subsequent intake fractions by humans. Based on the evolution of residues in edible parts of harvested wheat we predict that between 22 mg and 2.1 g per kg applied pesticide are taken in by humans via consumption of processed wheat products. Model results were compared with experimentally derived concentrations in wheat ears and with estimated intake via inhalation and ingestion caused by indirect emissions, i.e. the amount lost to the environment during pesticide application. Modeled and measured concentrations in wheat fitted very well and deviate from less than a factor 1.5 for chlorothalonil to a maximum factor 3 for tebuconazole. Main aspects influencing pesticide fate behavior are degradation half-life in plant and time between pesticide application and crop harvest, leading to variations in harvest fraction of at least three orders of magnitude. Food processing may further reduce residues by approximately 63%. Intake fractions from residues in sprayed wheat were up to four orders of magnitude higher than intake fractions estimated from indirect emissions, thereby demonstrating the importance of exposure from consumption of food crops after direct pesticide treatment. PMID:21955352

  18. Codex Committee on Pesticide Residues--a plan for improved participation by governments.

    PubMed

    Wessel, J R

    1992-10-01

    The Codex Committee on Pesticide Residues (CCPR), which is responsible for establishing maximum residue limits (MRLs) for pesticides on food, has a vital role in protecting the public health and facilitating international trade. Codex MRLs are based on scientific evaluations by expert panels that constitute the Joint FAO/WHO Meeting on Pesticide Residues (JMPR). These panelists estimate an acceptable daily intake for a pesticide and expected level of residue remaining in food when the pesticide is used according to good agricultural practice. The goals of the CCPR are not being fully achieved. Governments are generally not accepting Codex MRLs; instead, technical and procedural aspects of the JMPR and CCPR process are being criticized. The CCPR is responding to valid criticisms of the process; however, governments may still lack the will to seek harmonization of pesticide limits for food in international trade. Overcoming this problem will be difficult, but not impossible. A plan of action is proposed that allows countries to selectively accept Codex MRLs, increase the number of chemicals in the JMPR/CCPR system for evaluation, and be responsive to both their consumers and their food producers without compromising national health and safety standards and competitive trade advantages. PMID:1438994

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

    PubMed

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

    2015-01-01

    Crops grown under plastic-clad structures or in greenhouses may be prone to an increased frequency of pesticide residue detections and higher concentrations of pesticides relative to equivalent crops grown in the open field. To test this we examined pesticide data for crops selected from the quarterly reports (2004-2009) of the UK's Pesticide Residue Committee. Five comparison crop pairs were identified whereby one crop of each pair was assumed to have been grown primarily under some form of physical protection ('protected') and the other grown primarily in open field conditions ('open'). For each pair, the number of detectable pesticide residues and the proportion of crop samples containing pesticides were statistically compared (n=100 s samples for each crop). The mean concentrations of selected photolabile pesticides were also compared. For the crop pairings of cabbage ('open') vs. lettuce ('protected') and 'berries' ('open') vs. strawberries ('protected') there was a significantly higher number of pesticides and proportion of samples with multiple residues for the protected crops. Statistically higher concentrations of pesticides, including cypermethrin, cyprodinil, fenhexamid, boscalid and iprodione were also found in the protected crops compared to the open crops. The evidence here demonstrates that, in general, the protected crops possess a higher number of detectable pesticides compared to analogous crops grown in the open. This may be due to different pesticide-use regimes, but also due to slower rates of pesticide removal in protected systems. The findings of this study raise implications for pesticide management in protected-crop systems. PMID:25465948

  20. Specific antibody for pesticide residue determination produced by antibody-pesticide complex

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A new method for specific antibody production was developed using antibody (Ab)-pesticide complex as a unique immunogen. Parathion (PA) was the targeted pesticide, and rabbit polyclonal antibody (Pab) and mouse monoclonal antibody (Mab) were used as carrier proteins. The Ab-PA complexes were genera...

  1. Potential Transport and Degradation of “Aged” Pesticide Residues in Soil

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Increased pesticide residence time in soil, or “aging”, has been shown to affect the sorption-desorption of pesticides in the soil, which in turn can control transport and degradation processes. Aging effects have been characterized by batch sequential extraction methods, in which sorption coefficie...

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

    PubMed

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

    2013-07-01

    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

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

    PubMed

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

    2011-01-01

    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

  4. Method for determination of organohalogen pesticide residues in vegetable oil refinery by-products.

    PubMed

    Young, S; Clower, M; Roach, J A

    1984-01-01

    A method using gel permeation and Florisil column chromatographic cleanup techniques is described for determination of residues of nonpolar organohalogen pesticides and pesticide alteration products in vegetable oils and their refinery by-products. Supplemental Florisil separation and alkali cleanup techniques are used to facilitate determinations. Residues are determined with a 63Ni electron capture gas chromatographic detection system used in conjunction with 3 different gas chromatographic columns. Residue identities are confirmed by gas chromatography-mass spectrometry. Recoveries of 7 organohalogen pesticides, ranging from 90 to 103%, were determined by the supplemental Florisil separation technique to augment previously reported recovery data determined for initial GPC and Florisil cleanup steps. Soybean, peanut, and cottonseed deodorizer distillates and crude and refined oil, as well as additional refinery by-products, were analyzed. Nine to 13 organohalogen residues ranging from 0.5 to 6.3 ppm were determined in the 2 soybean deodorizer distillate samples used to develop and test the method. Identities of residues present at greater than or equal to 0.3 ppm were confirmed by gas chromatography-mass spectrometry. An intralaboratory trial of the method provided additional recovery and residue determination data as follows: Recoveries ranging from 102 to 116% were obtained for 4 pesticides added to peanut oil deodorizer distillate. Residues determined in 1 soybean deodorizer distillate sample supported previously obtained data for this sample. PMID:6698936

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

    PubMed

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

    2015-11-01

    There is increasing public concern over human health risks associated with extensive use of pesticides in agriculture. Regulation of pesticide maximum residue limits (MRLs) in food commodities is established in many developed countries. For Thailand, this regulation exists in law but is not fully enforced. Therefore, pesticide residues in vegetables and fruits have not been well monitored. This study investigated the pesticide residues in Chinese kale, a commonly eaten vegetable among Asians. The Chinese kale samples (N = 117) were purchased from markets in Nakhon Pathom Province, Thailand, and analyzed for the content of 28 pesticides. Analysis was performed by the multiresidual extraction followed by GC-MS/MS. Of pesticides investigated, 12 pesticides were detected in 85% of the Chinese kale samples. Although carbaryl, deltamethrin, diazinon, fenvalerate and malathion were found in some samples, their levels were lower than their MRLs. However, in 34 samples tested, either carbofuran, chlorpyrifos, chlorothalonil, cypermethrin, dimethoate, metalaxyl or profenofos was detected exceeding their MRLs. This represents a 29% rate of pesticide detection above the MRL; a rate much higher than in developed countries. Washing vegetables under running water significantly reduced (p < 0.05) profenofos residues by 55%. The running water method did not significantly decrease cypermethrin residues in the samples but washing with vinegar did. Our research suggests that routine monitoring of pesticide residues is necessary to reduce the public health risks associated with eating contaminated vegetables. Washing vegetables before consumption is advisable as this helps to reduce the level of pesticide residues in our daily intake. PMID:26093223

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

    PubMed

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

    1999-01-01

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

  7. A review on the fermentation of foods and the residues of pesticides-biotransformation of pesticides and effects on fermentation and food quality.

    PubMed

    Regueiro, Jorge; López-Fernández, Olalla; Rial-Otero, Raquel; Cancho-Grande, Beatriz; Simal-Gándara, Jesús

    2015-01-01

    Residues of pesticides in food are influenced by processing such as fermentation. Reviewing the extensive literature showed that in most cases, this step leads to large reductions in original residue levels in the fermented food, with the formation of new pesticide by-products. The behavior of residues in fermentation can be rationalized in terms of the physical-chemical properties of the pesticide and the nature of the process. In addition, the presence of pesticides decrease the growth rate of fermentative microbiota (yeasts and bacterias), which provokes stuck and sluggish fermentations. These changes have in consequence repercussions on several aspects of food sensory quality (physical-chemical properties, polyphenolic content, and aromatic profile) of fermented food. The main aim of this review is to deal with all these topics to propose challenging needs in science-based quality management of pesticides residues in food. PMID:24915365

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

    PubMed

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

    2009-02-01

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

  9. Pesticides Residue in Drinking Groundwater Resources of Rural Areas in the Northwest of Iran

    PubMed Central

    Shakerkhatibi, Mohammad; Mosaferi, Mohammad; Asghari Jafarabadi, Mohammad; Lotfi, Ehtesham; Belvasi, Mehdi

    2014-01-01

    Background:The majority of rural population in Iran depends on groundwater resources for drinking purposes. In recent years, pesticide contamination of limited water resources has become a serious challenge worldwide. This study quantified the pesticides residue in rural groundwater resources in the northwest of Iran. Methods: A total of 78 groundwater samples were collected in June and Sep-tember 2011 from all 39 drinking water wells. Liquid-liquid extraction (LLE) followed by Gas Chroma9tography/Mass Spectrometry (GC/MS) was used to determine the selected pesticides. Results: Detection frequencies of profenofos, malathion, diazinon, endosulfan, trifluralin, deltamethrin, methyl parathion, and fenitrothion were determined with the concentrations exceeded 0.1 μg/L in 2.6, 17.9, 15.4, 10.3, 2.6, 2.6, 7.7, and 44.9% of the samples, respectively. Total pesticides residue was also ob-served in 26.9% of the samples with concentrations exceeded 0.5 μg/L. Among them, profenofos, malathion and diazinon were detected as the most frequently observed pesticides with the maximum concentrations of 0.542, 0.456 and 0.614 μg/L, respectively. Conclusion: Higher pesticides residue than European Economic Commission (EEC) guidelines occurred in a number of monitored resources. PMID:25648583

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

    PubMed Central

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

    2008-01-01

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

  11. Chlorinated pesticide residues in sediments from the Arabian Sea along the central west coast of India

    SciTech Connect

    Sarkar, A.; Gupta, R.S.

    1987-12-01

    The problem of environmental contamination by persistent chlorinated pesticides still evokes major concern due to the presence of their residues in the environment and in human tissues. In developing countries like India organochlorine insecticides, especially DDT are extensively being used in agriculture and vector control programs. Few data are available on their levels of concentration from the seas around India. Persistent pesticides residues can be expected to accumulate in marine sediments. However, very little data on this are available along the Indian coast. An attempt has been made in the present communication to identify and quantify some of the chlorinated pesticides residues in the marine sediments collected from different region along the central west coast of India. This is a part of our ongoing project to monitor and map pollutants within the exclusive economic zone of India.

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

    NASA Astrophysics Data System (ADS)

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

    2015-06-01

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

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

    PubMed

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

    2016-05-01

    More than 90% of the pesticides residues in apples are located in the peel. We developed a gas chromatography/ion trap tandem mass spectrometry method for investigating all detectable residues in the peel of 3 apple varieties. Sample preparation is based on the use of the Quick Easy Cheap Effective Rugged and Safe method on the whole fruit, the flesh, and the peel. Pesticide residues were quantified with solvent-matched and matrix-matched standards, by spiking apple sample extracts. Matrix effects dependent on the type of extract (fruit, flesh, or peel) and the apple variety were detected. The best data processing methods involved normalizing matrix effect rates by matrix-matched internal/external calibration. Boscalid, captan, chlorpyrifos, fludioxonil, and pyraclostrobin were the most frequently detected pesticides. However, their concentrations in the whole fruit were below European maximum residue levels. Despite negative matrix effects, the residues in peel were detected at concentrations up to 10 times higher than those in whole fruits. Consequently, other pesticide residues present at concentrations below the limit of quantification in the whole fruit were detected in the peel. PMID:27095394

  14. Determination of pesticide residues in IPM and non-IPM samples of mango (Mangifera indica).

    PubMed

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

    2008-05-01

    Studies were conducted to analyze the residue of commonly used pesticides viz. methyl parathion, chloropyrifos, endosulfan, cypermethrin, fenvalerate, carbendazim, imidacloprid and carbaryl in mango, Dashehari variety, integrated pest management (IPM) and non-IPM samples were collected from the IPM and non-IPM orchards, Lucknow, India. We also present a method for the simultaneous determination of these pesticides in mango samples. Residues of methyl parathion, chloropyriphos, endosulfan, cypermethrin, fenvalerate were extracted from the samples with acetone: cyclohexane: ethyl acetate in the ratio 2:1:1 followed by cleanup using neutral alumina. Analysis was performed by gas chromatography-electron capture detector (GC-ECD) with a megabore column (OV-1). Residues of carbendazim, imidacloprid and carbaryl were extracted with acetone and after cleanup, analysis was performed by high performance liquid chromatography (HPLC) using photo diode array (PDA) detector. Recoveries of all the pesticides ranged between 72.7-110.6%, at 0.1 and 1.0 microg g(-1) level of fortification. The residues detected in non-IPM samples of mango were found to be below the prescribed limits of maximum residue limit (MRL) while IPM samples were free from pesticide residues. PMID:18437617

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

    PubMed

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

    2008-04-01

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

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

    PubMed

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

    2012-01-01

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

  17. Monitoring and risk assessment of 74 pesticide residues in Pu-erh tea produced in Yunnan, China.

    PubMed

    Chen, Hongping; Wang, Qinghua; Jiang, Ying; Wang, Chuanpi; Yin, Peng; Liu, Xin; Lu, Chengyin

    2015-01-01

    A number of 100 Pu-erh tea samples from the 2013 harvest in Yunnan Province (China) were analysed for 74 pesticides. A total of 11 pesticides were detected. At least one pesticide was detected in 56% of the samples. None of these samples contained the 74 monitored pesticides at concentrations above the Chinese maximum residual levels. Imidacloprid, bifenthrin and acetamiprid were most frequently found, with percentages of 53%, 46% and 31%, respectively. These were also the top three pesticides with maximum concentrations of 140, 246 and 672 μg kg⁻¹, respectively. Residual levels of the monitored pesticides showed no significant correlation with the production time or area of Pu-erh tea. Whereas a high incidence of pesticide residues was detected in Pu-erh tea, the contamination levels observed do not pose any serious health risks. PMID:25308103

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

    PubMed

    Mekonen, Seblework; Ambelu, Argaw; Spanoghe, Pieter

    2015-09-30

    Coffee is a highly consumed and popular beverage all over the world; however, coffee beans used for daily consumption may contain pesticide residues that may cause adverse health effects to consumers. In this monitoring study, the effect of household coffee processing on pesticide residues in coffee beans was investigated. Twelve pesticides, including metabolites and isomers (endosulfan α, endosulfan β, cypermethrin, permethrin, deltamethrin, chlorpyrifos ethyl, heptachlor epoxide, hexachlorobenzene, p'p-DDE, p'p-DDD, o'p-DDT, and p'p-DDT) were spiked in coffee beans collected from a local market in southwestern Ethiopia. The subsequent household coffee processing conditions (washing, roasting, and brewing) were established as closely as possible to the traditional household coffee processing in Ethiopia. Washing of coffee beans showed 14.63-57.69 percent reduction, while the roasting process reduced up to 99.8 percent. Chlorpyrifos ethyl, permethrin, cypermethrin, endosulfan α and β in roasting and all of the 12 pesticides in the coffee brewing processes were not detected. Kruskal-Wallis analysis indicated that the reduction of pesticide residues by washing is significantly different from roasting and brewing (P < 0.0001). However, there was no significant difference between coffee roasting and brewing (P > 0.05). The processing factor (PF) was less than one (PF < 1), which indicates reduction of pesticides under study during processing of the coffee beans. The cumulative effect of the three processing methods has a paramount importance in evaluating the risks associated with ingestion of pesticide residues, particularly in coffee beans. PMID:26344013

  19. Effect of Cooking Process on the Residues of Three Carbamate Pesticides in Rice

    PubMed Central

    Shoeibi, Shahram; Amirahmadi, Maryam; Yazdanpanah, Hassan; Pirali-Hamedani, Morteza; Pakzad, Saied Reza; Kobarfard, Farzad

    2011-01-01

    A gas chromatography mass spectrometry with spike calibration curve method was used to quantify three carbamate pesticides residue in cooked white rice and to estimate the reduction percentage of the cooking process duration. The selected pesticides are three carbamate pesticides including carbaryl and pirimicarb that their MRL is issued by “The Institute of Standards of Iran” and propoxur which is used as a widely consumed pesticide in rice. The analytical method entailed the following steps: 1- Blending 15 g cooked sample with 120 mL acetonitrile for 1 min in solvent proof blender, 2- Adding 6 g NaCl and blending for 1 min, 3- Filtering upper layer through 25 g anhydrous Na2SO4, 4- Cleaning up with PSA and MgSO4, 5- Centrifuging for 7 min, 6- Evaporating about 0.3 mL and reconstituting in toluene till 1 mL, 7- Injecting 2 μL extract into GC/MS and analyzing by single quadruple selected ion monitoring GC/MS-SQ-SIM. The concentration of pesticides and the percentage of pesticides amounts after the cooking were determined by gas chromatography mass-spectrometry (GC/MS) using with interpolation of the relative peak areas for each pesticide to internal standard peak area in the sample on the spiked calibration curve. Calibration curve was linear over the range of 25 to 1000 ng/g, and LOQ was 25 ng/g for all three pesticides. The percent of loss for the three pesticides were 78%, 55% and 35% for carbaryl, propoxur and pirimicarb respectively. Different parameters such as vapor pressure, boiling point, and suspect ability of the compound to hydrolysis, could be responsible for the losing of pesticides during the cooking process. PMID:24363690

  20. Determination of organochlorine pesticide residue in sediment and water from the Densu river basin, Ghana.

    PubMed

    Kuranchie-Mensah, Harriet; Atiemo, Sampson Manukure; Palm, Linda Maud Naa-Dedei; Blankson-Arthur, Sarah; Tutu, Anita Osei; Fosu, Paul

    2012-01-01

    The distribution of organochlorine pesticides in the aquatic ecosystem from the Densu river revealed varying levels of concentration in water and the sediment samples. Three locations were sampled along the river to evaluate the levels of organochlorine pesticide residue in the river. Sediment and surface water samples were extracted by soxhlet and liquid-liquid extraction respectively and analyzed using Gas Chromatograph coupled with electron capture detector. The detectable organochlorine pesticides were gamma-hexachlorocyclohexane (HCH), delta-hexachlorocyclohexane, heptachlor, aldrin and dieldrin. The other pesticides that were investigated are gamma-chlordane, alpha endosulfan, endosulfan sulfate, p,p'-DDT and its metabolite p,p'-DDE, methoxychlor, endrin and its metabolite endrin aldehyde and endrin ketone. The order of increasing frequency of detection of samples was higher in sediment than water. In sediment, the mean concentration ranged from 0.030 μg kg(-1) dry weight (endrin) to 10.98 μg kg(-1) dry weight (aldrin). The highest detected concentration of organochlorine in water was endosulfan sulfate with mean concentration of 0.185 μg L(-1). Analysis of variance indicated significant differences for most organochlorine pesticide residue in the sediment sampled from the various locations. Some of the levels of organochlorine pesticides detected in water were relatively high compared to guideline values set by World Health Organization and Australia and thus could be harmful if the trend is not checked. PMID:22123529

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

    PubMed

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

    2016-02-01

    The pesticide residue levels of three nuts (chestnut, walnut, pinenut) collected from seven main producing areas of China were investigated. Twenty-nine pesticides, including organophosphates (OPs), organochlorines (OCs), pyrethroids (PYs) and two fungicides (triadimefon and buprofezin) were analyzed by gas chromatography (GC). Four OPs (acephate, dimethoate, chlorpyrifos and parathion-methyl) were found in 11.4% samples, with the concentrations of 19.0 µg kg(-1) to 74.0 µg kg(-1). Six OCs (DDT, HCH, endosulfan, quintozene, aldrin and dieldrin) were found in 18.2% samples, with the concentrations of 2.0 µg kg(-1) to 65.7 µg kg(-1). Among OCs, p,p-DDE and α-HCH were the dominant isomer for DDT and HCH. Five PYs (fenpropathrin, fenvalerate, cypermethrin, bifenthrin and cyhalothrin) were found in 15.9% samples, with the concentrations of 2.5 µg kg(-1) to 433.0 µg kg(-1). Fenpropathrin was the most frequently detected pesticide. In addition, triadimefon and buprofezin were detected only in two samples. For the tested nuts, 25.0% samples with multiple residues (containing more than two pesticides) were noted, even up to 9.1% samples with five pesticide residues. The residue of 15.9% samples was higher than the maximum residue limits (MRLs) of China. The short-term risks for the tested nuts were below 1.2%, and the highest long-term risk was 12.58%. The cumulative risk (cHI) for the tested pesticides were 8.43% (OPs), 0.42% (OCs), 12.82% (PYs) and 0.15% (fungicides), respectively. The total cHI was 21.82%. There was no significant health risk for consumers via nuts consumption. PMID:26408971

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

    PubMed Central

    Kotinagu, Korrapati; Krishnaiah, Nelapati

    2015-01-01

    Aim: The present study was conducted to find the organochlorine pesticide (OCP) and organophosphorus pesticide (OPP) residues in fodder and milk samples along Musi river belt, India. Materials and Methods: Fodder and milk samples collected from the six zones of Musi river belt, Hyderabad India were analyzed by gas chromatography with electron capture detector for OCP residues and pulsated flame photometric detector for the presence of OPP residues. Results: The gas chromatographic analysis of fodder samples of Zone 5 of Musi river showed the residues of dicofol at concentration of 0.07±0.0007 (0.071-0.077). Among organophosphorus compounds, dimetheoate was present in milk samples collected from Zone 6 at a level of 0.13±0.006 (0.111-0.167). The residues of OCPs, OPPs and cyclodies were below the detection limit in the remaining fodder and milk samples collected from Musi river belt in the present study. Conclusion: The results indicate that the pesticide residues in fodder and milk samples were well below the maximum residue level (MRL) values, whereas dicofol in fodder and dimethoate in milk were slightly above the MRL values specified by EU and CODEX. PMID:27047132

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

    PubMed

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

    2013-11-01

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

  4. Residual pesticide detection on food with particle-enhanced Raman scattering

    NASA Astrophysics Data System (ADS)

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

    2014-08-01

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

  5. Pesticide residue transfer in Thai farmer families: using structural equation modeling to determine exposure pathways.

    PubMed

    Liu, Hanhua; Hanchenlaksh, Chalalai; Povey, Andrew C; de Vocht, Frank

    2015-01-01

    Use of pesticides in agriculture may lead to downstream exposure of farmers' families to pesticide residues inadvertently taken home. Identification of the independent contribution of different exposure pathways from the farmer to their children can provide clear targets to reduce exposure of farmers' children. Individual contributions of different pesticide transfer exposure pathways were investigated using structural equation modeling methods, and the benefits of these methods compared to standard multiple regression are described. A total of 72 Thai families, consisting of a farmer, a spouse, and a child, participated in this study. Family members completed a questionnaire and self-collected three spot morning urine samples in the spraying season. Urine samples were analyzed for diethyl phosphate, diethyl thiophosphate, diethyl dithiophosphate, dimethyl phosphate, dimethyl thiophosphate, and dimethyl dithiophosphate. A path model was developed based on an a priori hypothesized framework to examine the individual contributions of different exposure pathways that may directly or indirectly affect transfer of pesticide residues from farmers to their children. Transfer from the farmer to the child occurs indirectly, primarily through transfer to the spouse in the first instance, but also through contamination of the home environment. Clear targets for interventions are directly the reduction of farmers' take-home exposures and indirectly frequent cleaning of the home to avoid buildup of pesticide residues. PMID:25407029

  6. Optical instrument development for detection of pesticide residue in apple surface

    NASA Astrophysics Data System (ADS)

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

    2013-05-01

    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.

  7. Monitoring of some organochlorine pesticide residues of butter in Konya, Turkey.

    PubMed

    Nizamlioglu, Ferhan; Aktumsek, Abdurrahman; Kara, Huseyin; Dinc, Iffet

    2005-06-01

    Some organochlorine pesticide residues were investigated in the samples of all local commercial butter brands sold in the supermarket in Konya (Turkey). Some of the samples were found to have the DDT complex (DDT, DDD, DDE and isomers), total HCH complex (alpha-HCH, beta-HCH, gamma-HCH), aldrin, dieldrin and endosulfan (I and II). Nearly 94% of the butter samples were found to be contaminated. Endrin and heptachlorine were detected in three and two samples, respectively, while 87% of samples were contaminated by one or more HCH isomers. 78% of the organochlorine pesticide was DDT and/or its metabolites. These results confirmed that butters sold in Konya presented organochlorine pesticide residues indicating a human exposure. PMID:16334269

  8. Sub-Lethal Effects of Pesticide Residues in Brood Comb on Worker Honey Bee (Apis mellifera) Development and Longevity

    PubMed Central

    Wu, Judy Y.; Anelli, Carol M.; Sheppard, Walter S.

    2011-01-01

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

  9. Organochlorine pesticide residues in woodcock, soils and earthworms in Louisiana, 1965

    USGS Publications Warehouse

    McLane, M.A.R.; Stickel, L.F.; Newsom, J.D.

    1971-01-01

    Woodcock (Philohela minor), earthworms, and soil samples were collected from January-March 1965, from fields in southeastern Louisiana approximately 3 years after discontinuance of areal treatments with heptachlor in this region. Heptachlor epoxide residues in woodcock averaged 0.42 ppm (dry weight), conspicuously lower than in 1961 and 1962. Residues of DDE in woodcock averaged 3.62 pprn, higher than in birds taken in the same area in 1961-62. Earthworms and soils contained traces of several organochlorine pesticides.

  10. Dissipation behavior of organophosphorus pesticides during the cabbage pickling process: residue changes with salt and vinegar content of pickling solution.

    PubMed

    Lu, Yuele; Yang, Zhonghua; Shen, Luyao; Liu, Zhenmin; Zhou, Zhiqiang; Diao, Jinling

    2013-03-01

    In this experiment, the behavior of 10 pesticides in three different cabbage pickling treatments has been studied. The brine used for pickling was made up with different salt and vinegar contents to determine the influence of different pickling solutions on pesticide dissipation and distribution. A modified QuECHERS and SPE method was established for the analysis of the pesticides in the cabbage and brine. It was found that different pesticides showed different dissipation patterns and finally represented dissimilar residue levels in the cabbage and brine. Statistical analysis was performed to compare the distinctions of these pesticides between each treatment and proved that salt content and pH value had certain influence on the dissipation and distribution of these pesticides during the pickling process. The data from this experiment would help to control pesticide residues in pickled cabbage and prevent potential risk to human health and environmental safety. PMID:23402557

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

    NASA Astrophysics Data System (ADS)

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

    1993-09-01

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

  12. Sample treatment and determination of pesticide residues in fatty vegetable matrices: a review.

    PubMed

    Gilbert-López, Bienvenida; García-Reyes, Juan F; Molina-Díaz, Antonio

    2009-07-15

    A demanding task in pesticide residue analysis is yet the development of multi-residue methods for the determination of pesticides in vegetables with relatively high fat content (i.e. edible oils and fatty vegetables). The separation of pesticides and other chemical contaminants from high-fat food samples prior to subsequent steps in the analytical process is yet a challenging issue to which much effort in method development has being applied. This review addresses the main sample treatment methodologies for pesticide residue analysis in fatty vegetable matrices. Even with the advent of advanced hyphenated techniques based on mass spectrometry these complex fatty matrices usually require extensive sample extraction and purification. Current methods involve the use of one or the combination of some of the following techniques for both the sample extraction and clean-up steps: liquid-liquid partitioning, solid-phase extraction (SPE), gel-permeation chromatography (GPC), matrix solid-phase dispersion (MSPD), etc. An overview of methods developed for these contaminants in fatty vegetables matrices is presented. Sample extraction and purification techniques are discussed and their most recent applications are highlighted. This review emphasizes that sample preparation is a critical step, but also the determination method is, and cannot be treated separately from sample treatment. In recent years, the appearance and use of new, more polar pesticides has fostered the development of liquid chromatography/mass spectrometry (LC-MS) besides gas chromatography. The main features of LC-MS for the analysis of multi-class pesticides in fatty vegetable samples will be also underlined, with an emphasis on the multi-class, multi-residue strategy and the difficulties associated. PMID:19559852

  13. MACRO AND MICRO APPROACHES TO THE DETERMINATION OF PESTICIDE RESIDUES IN HUMAN AND ANIMAL TISSUES

    EPA Science Inventory

    Analytical approaches to the determination of pesticides and metabolites in human and animal tissues will take many forms. Several factors must be considered in choosing an analytical scheme if the results are to be meaningful. Whenever possible the residue chemist will use stand...

  14. QuEChERS sample preparation approach for mass spectrometric analysis of pesticide residues in foods

    Technology Transfer Automated Retrieval System (TEKTRAN)

    This chapter describes an easy, rapid, and low-cost sample preparation approach for the determination of pesticide residues in foods using gas and/or liquid chromatographic (GC and/or LC) analytical separation and mass spectrometric (MS) detection. The approach is known as QuEChERS, which stands fo...

  15. Pesticide and PCB residues in the Neuse River waterdog, Necturus lewisi

    USGS Publications Warehouse

    Hall, R.J.; Prouty, R.M.; Ashton, R.E.

    1985-01-01

    Residues of 6 organochlorine contaminants were found in N. lewisi from 6 sites in the Tar and Neuse river systems. Concentrations of pesticides were low and apparently related to geographic patterns of use. Levels of PCB were higher and did not seem to vary geographically.

  16. Determination of Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate: Collaborative Study

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A collaborative study was conducted to determine multiple pesticide residues in fruits and vegetables using a quick, simple, inexpensive, and effective sample preparation method followed by concurrent analysis with gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass sp...

  17. Comparison of Wipe Materials and Wetting Agents for Pesticide Residue Collection from Hard Surfaces

    EPA Science Inventory

    Different wipe materials and wetting agents have been used to collect pesticide residues from surfaces, but little is known about their comparability. To inform the selection of a wipe for the National Children's Study, the analytical feasibility, collection efficiency, and preci...

  18. Monitoring of pesticide residues in Egyptian fruits and vegetables during 1997.

    PubMed

    Dogheim, S M; El-Marsafy, A M; Salama, E Y; Gadalla, S A; Nabil, Y M

    2002-11-01

    A total of 2318 domestic samples of different types of fruits and vegetables were collected from eight Egyptian local markets in six different regions of the country. All samples were examined for residues of 54 pesticides, including organophosphorus, organonitrogen, organohalogen and certain pyrethroides. However, dithiocarbamates were analysed in only 318 samples. Overall, 81.5% of the samples had no detectable pesticide residues. Of the contaminated samples, 18.5% contained detectable residues and 1.9% exceeded their maximum residue limits (MRLs). Root and leafy vegetables showed the lowest contamination rates (1.9 and 4.7%, respectively), slightly exceeding the MRLs in leafy vegetables. However, fruit samples showed a slightly higher proportion of contamination than vegetables (29 and 14.3%, respectively). Fruit also exhibited a higher level of violation than vegetables (2.3 and 1.9%, respectively). The contamination and violation rates were lower than the percentages recorded in previous years' monitoring studies. Dicofol and dimethoate were the most frequently occurring pesticide residues at 5.1 and 5.0%, respectively. Dimethoate showed higher violation levels (0.69%). However, dicofol showed a slight violation rate (0.09%) which indicates good agricultural practices for dicofol use. Dithiocarbamates residues were found in 21 of the 318 samples analysed, which when expressed as a percentage contamination was 6.6%, and only one sample exceeded the MRL. PMID:12456272

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

    PubMed

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

    2012-08-01

    The effect of home processing (washing, peeling, coring and juicing) on residue levels of chlorpyrifos, β-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, β-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, β-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 β-cypermethrin during peeling and coring process. The removal effect of apple juicing was found to be the most pronounced on β-cypermethrin residue, which was reduced in the range of 81-84%, and the reductions of chlorpyrifos, tebuconazole, acetamiprid and carbendazim upon apple juicing were in the range of 15-36%. PMID:22738391

  20. Multi-residue detection of pesticides using a sensitive immunochip assay based on nanogold enhancement.

    PubMed

    Lan, Meijing; Guo, Yirong; Zhao, Ying; Liu, Yihua; Gui, Wenjun; Zhu, Guonian

    2016-09-28

    This paper describes the development of a new multiplex immunoassay for simultaneous detection of seven pesticides (triazophos, methyl-parathion, fenpropathrin, carbofuran, thiacloprid, chlorothalonil, and carbendazim). Sixteen pairs of pesticide antibodies and antigens were screened for reactivity and cross-reaction. A microarray chip consisting of seven antigens immobilized on a nitrocellulose membrane was then constructed. Nanogold was employed for labeling and signal amplification to obtain a sensitive colorimetric immunoassay. The direct and indirect detection formats were further compared using primary antibody-gold and secondary antibody-gold conjugates as tracers. An integrated 7-plex immunochip assay based on the indirect model was established and optimized. The detection limits for the pesticides were 0.02-6.45 ng mL(-1), which meets detection requirements for pesticide residues. Naked-eye assessment showed the visual detection limits of the assay ranged from 1 to 100 ng mL(-1). Spiked recovery results demonstrated that the immunochip assay had potential for multi-analysis of pesticide residues in vegetables and fruits. The proposed microarray methodology is a flexible and versatile tool, which can be applied to other competitive multiplex immunoassays for small molecular compounds. PMID:27619097

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

    PubMed

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

    2016-11-01

    Access to safe and reliable drinking water is vital for a healthy population. However, surface water may be contaminated with pesticides because of the nearby agricultural areas as well as from household application. Water samples were collected from water sources in Jimma zone and Addis Ababa, Ethiopia. The extraction and clean up of the samples were undertaken using liquid-solid and liquid-liquid methods. Human exposure was assessed by calculating the estimated daily intake (EDI) of pesticides in water and compared with the acceptable daily intake (ADI) and the acute reference dose (ARfD). The mean concentrations of 2,4-D, malathion, diazinon and fenpropimorph were 1.59-13.90 μg/l and 0.11-138 µg/l in Jimma and Addis Ababa water sources, respectively. The residue level of some of the pesticides were above the European drinking water guide line values, which is an indication of an illegal use of pesticides in the study areas. Concerning human health risk estimation, there was no acute risk (EDI < ARfD). However, chronic risks to human health were observed from exposure to diazinon and fenpropimorph (EDI > ADI) for Jimma and Addis Ababa populations, respectively. A comprehensive monitoring is required to reduce the level of pesticide residues in the water and to minimize particularly the long term human health risks. PMID:27501312

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

    PubMed

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

    2013-01-01

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

  3. Assessment of organochlorine pesticide residues in soils and drinking water sources from cocoa farms in Ghana.

    PubMed

    Fosu-Mensah, Benedicta Y; Okoffo, Elvis D; Darko, Godfred; Gordon, Christopher

    2016-01-01

    Residues of organochlorine pesticides were determined in soils and drinking water sources in cocoa growing areas in Ghana. Soil samples analysed showed the presence of four organochlorine pesticide residues namely lindane (0.005-0.05 mg/kg), beta-HCH (<0.01-0.05 mg/kg), dieldrin (0.005-0.02 mg/kg), and p,p'-DDT (0.005-0.04 mg/kg), with dieldrin occurring most frequently. Similarly, organochlorine pesticide residues detected in the water samples were lindane (0.01-0.03 µg/l), alpha-endosulfan (0.01-0.03 µg/l), endosulfan-sulphate (0.01-0.04 µg/l), dieldrin (0.01-0.03 µg/l) and p,p'-DDT (0.01-0.04 µg/l), with heptachlor occurring most frequently. The concentrations of the detected organochlorine residues in the soil samples were below their respective US maximum residues limits (MRLs) for agricultural soils, except for lindane recorded at Kwakuanya (S4) and beta-HCH recorded at Krakrom (S3) and Kwakuanya (S4). Similarly, the organochlorine pesticide residues recorded in the water samples were below and within their respective WHO MRLs for drinking water except for alpha-endosulfan at Diabaa (S2) and Kwakuanya (S4) at distance 0-15 m and Kwakuanya (S4) at distance 16-30 m, endosulfan-sulfate at Nkrankwanta (S1) and Diabaa (S2) at distance 0-15 m and heptachlor at Krakrom (S3) at distance 16-30 m which were above their WHO MRLs. The presence of the banned organochlorine pesticide residues in soil and water samples from the study area indicates that these chemicals are still being used, illegally, on some cocoa farms. Routine monitoring of pesticide residues in the study area is necessary for the prevention, control and reduction of environmental pollution to minimize health risks. PMID:27386318

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

    PubMed

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

    2014-09-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-05-01

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

  6. Dietary exposure to pesticide residues from foods of plant origin and drinks in Lebanon.

    PubMed

    Nasreddine, Lara; Rehaime, Maria; Kassaify, Zeina; Rechmany, Roula; Jaber, Farouk

    2016-08-01

    This study assesses the dietary exposure of Lebanese adults to 47 pesticide residues from both foods of plant origin and drinks. The study was conducted using the Total Diet Study protocol in two different areas of Lebanon: Greater Beirut (urban) and Keserwan (semi-rural). A total of 1860 individual foods were collected, prepared, and cooked prior to analysis. Composite samples of similar foods were analyzed, following the QuEChERS Multiresidue method. Eighteen residues were detected/quantified on at least one composite sample, with 66.7 % of the results being quantifiable and 33.3 % detectable. Quantifiable levels ranged between 10.3 and 208 μg/kg. For the composite samples where residues were detected, 55 % had one residue, while 45 % had 2-4 residues. The most frequently detected/quantified pesticide residues included Chlorpyrifos, Procymidone, Primiphos methyl, Dimethoate, and Dieldrin. The dietary exposure assessment was conducted using the deterministic approach with two scenarios: (1) the lower bound (LB) approach and (2) the upper bound (UB) approach. Using the LB approach, mean estimated daily exposures were far below the acceptable daily intakes (ADIs) for all investigated residues. Using the UB approach, which tends to overestimate exposure, mean estimated daily exposures were below the ADIs for all residues except for Dieldrin (semi-rural: 128.7 % ADI; urban: 100.7 % ADI). Estimates of mean exposure to Diazinon reached 50.3 % of ADI in the urban diet and 61.9 % in the semi-rural diet. Findings of this study identify specific pesticide residues as monitoring priorities for which more comprehensive and sensitive analyses are needed in order to refine exposure assessment. PMID:27461424

  7. Pesticide Residues in Bovine Milk in Punjab, India: Spatial Variation and Risk Assessment to Human Health.

    PubMed

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

    2015-08-01

    In the present study, gas chromatographic analysis of pesticide residues in bovine milk (n = 312) from Punjab, India, showed chlorpyrifos, DDT, and γ-HCH as the predominant contaminants. In addition, the presence of β-endosulfan, endosulfan suphate, cypermethrin, cyhalothrin, fenvalerate, deltamethrin, malathion, profenofos, and ethion was reported in milk samples. In this study, it was observed that 12 milk samples exceeded the maximum residue limits (MRLs) for γ-HCH (lindane), 18 for DDT and chlorpyrifos, and 1 sample each for endosulfan, cypermethrin, and profenophos. In India, DDT is still permitted for a malaria control program, which may be the plausible reason for its occurrence in milk samples. The spatial variation for presence of pesticide residues in milk indicated greater levels in cotton-growing areas of Punjab. At current levels of pesticide residues in bovine milk, the human health risk assessment in terms of noncancer and cancer hazard was calculated based on both lower-bound [LB (mean residue levels)] and upper-bound [UP (95th percentile level)] limits. It was noticed that cancer and noncancer risk were within United States Environmental Protection Agency prescribed limits for both adults and children at the LB, but children were being exposed to greater risk for DDT and HCH at the 95th-percentile UB level. PMID:26008642

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

    PubMed

    Loch, J P; Verdam, B

    1989-01-01

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

  9. A perspective of pesticide residue variability and acute dietary risk assessment.

    PubMed

    Walsh, M

    2000-07-01

    The question of the variability of pesticide residues and acute risk assessment has arisen in the context of the work of the European Commission's Scientific Committee for Plants (SCP). A brief outline is presented of European Community legislation on pesticide residues and the authorization of plant protection products. It is stated that although chronic risk assessment is systematically carried out in connection with the fixing of Community MRLs, the same has not applied for acute risk assessment. The reasons for this situation have been the absence of an agreed methodology, acute reference dose (RfD) and adequate dietary and residue data. It is stated that in the opinion of the Scientific Committee for Plants an acute risk assessment should be considered on a routine basis and that steps should be taken to ensure the availability of the necessary data. Possible implications for risk communication and the authorization of plant protection products in the EC are also discussed. PMID:10983589

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

    NASA Astrophysics Data System (ADS)

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

    2014-07-01

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

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

    PubMed Central

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

    2014-01-01

    Here we reported a residue-free green nanotechnology which synergistically enhance the pesticides efficiency and successively eliminate its residue. We built up a composite antifungal system by a simple pre-treating and assembling procedure for investigating synergy. Investigations showed 0.25 g/L ZnO nanoparticles (NPs) with 0.01 g/L thiram could inhibit the fungal growth in a synergistic mode. More importantly, the 0.25 g/L ZnO NPs completely degraded 0.01 g/L thiram under simulated sunlight irradiation within 6 hours. It was demonstrated that the formation of ZnO-thiram antifungal system, electrostatic adsorption of ZnO NPs to fungi cells and the cellular internalization of ZnO-thiram composites played important roles in synergy. Oxidative stress test indicated ZnO-induced oxidative damage was enhanced by thiram that finally result in synergistic antifungal effect. By reducing the pesticides usage, this nanotechnology could control the plant disease economically, more significantly, the following photocatalytic degradation of pesticide greatly benefit the human social by avoiding negative influence of pesticide residue on public health and environment. PMID:25023938

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

    PubMed

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

    2016-07-01

    This paper presents the results of official control of pesticide residues in minor crops collected in southeastern Poland in 2013-2014. Compliance of used pesticides with applicable law was also verified, and determined residues were compared to maximum residue levels (MRLs) provided for in Regulation (EC) No. 395/2005. A total of 583 samples of 25 different types of fresh fruit and vegetables were analyzed for pesticide residues. Pesticide residues were detected in 158 samples (27.1 % of the analyzed samples). According to the European Commission Health & Consumer Protection Directorate-General (SANCO) guidelines document, MRL violations were understood as cases where a residue level exceeded the MRL after the uncertainty of the method (50 %) was considered. MRL violations were found in four samples. The usage of unauthorized pesticides was detected in 5.8 % of analyzed samples. Substances banned in Poland were found in two samples. Fungicides were the most frequently detected group of pesticides. Pesticide residues were most commonly found in fruit samples (19.4 % of all analyzed samples), mainly in gooseberry, redcurrant, and huckleberry. The majority of samples were compliant with MRLs, which means that they were suitable for trade. PMID:27251221

  13. Residues of organochlorine pesticides and polychlorinated biphenyls and autopsy data for bald eagles, 1973-74

    USGS Publications Warehouse

    Prouty, R.M.; Reichel, W.L.; Locke, L.N.; Belisle, A.A.; Cromartie, E.; Kaiser, T.E.; Lamont, T.G.; Mulhern, B.M.; Swineford, D.M.

    1977-01-01

    Thirty-nine bald eagles found sick or dead in 13 States during 1969 and 1970 were analyzed for pesticide residues. Residues of DDE, dieldrin, polychlorinated biphenyls (PCB's), and mercury were detected in all bald eagle carcasses; DDD residues were detected in 38; DDT, heptachlor epoxide, and dichlorobenzophenone (DCBP) were detected less frequently. Six eagles contained possible lethal levels of dieldrin in the brain, and one contained a lethal concentration of DDE (385 ppm) in the brain together with 235 ppm of PCB's. Autopsy revealed that 18 bald eagles were illegally shot; other causes of death were impact injuries, electrocution, emaciation, and infectious diseases.

  14. Nationwide residues of organochlorine pesticides in wings of mallards and black ducks

    USGS Publications Warehouse

    Heath, R.G.

    1969-01-01

    Nationwide monitoring of organochlorine pesticides in wings of more than 24,000 mallards and black ducks bagged during the1965 and 1966 hunting seasons showed DDE to be the predominant residue, followed in order by DDT, DDD, dieldrin, and heptachlor epoxide. Residues were generally highest in wings from the Atlantic and Pacific Flyways, and lowest in the Central Flyway. DDE was reported for every State and was notably high in wings from New Jersey, Massachusetts, Connecticut, Rhode Island, New York, Pennsylvania, Alabama, California, and Utah. Dieldrin residues were prevalent in wings from Arkansas, Texas, Utah, California, and several Stales in the Atlantic Flyway.

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

    PubMed

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

    2007-05-01

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

  16. Pesticides

    MedlinePlus

    ... or cause harm to crops, people, or animals. Pesticides can help get rid of them. Pesticides are not just insect killers. They also include ... mildew, germs, and more. Many household products contain pesticides. Pesticides can protect your health by killing germs, ...

  17. Evaluating spray adjuvants to extend residual activity of microbiol pesticides`

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Based on requests to improve the residual efficacy of baculovirus applications, a commercial adjuvant (Nu-Film 17(R) and an experimental lignin adjuvant were evaluated for resistance to environmental degradation. Nu-Film is a commercial product derived from pine resin; and lignin is a by-product of...

  18. Extraction and clean-up procedure for analysis of organochlorine pesticide residues in ethoxylated lanolin.

    PubMed

    Polese, L; Sannomiya, M; de Olivera Sader, A P; Lúcia Ribeiro, M

    2000-01-01

    In the present study an evaluation was made of a method for the determination of organochlorine pesticide residues in ethoxylated lanolin. Samples were homogenized with Celite, transferred to chromatographic columns, prepacked with silica gel deactivated to 10%. The pesticide elution was processed with n-hexane-dichloromethane and the concentrated eluate was analyzed using gas-liquid chromatography (GC) with electron capture detection (ECD). The composition of the elution solvent was a significant factor for the recovery of the pesticides. Mean recoveries obtained for fortified samples ranged from 87 to 94% for p,p'-DDE, dieldrin, endrin, p,p'-DDD and p,p'-DDT. Optimization of the experimental conditions resulted in a small-scale method that combines extraction and cleanup in a single step. PMID:11152246

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

    NASA Astrophysics Data System (ADS)

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

    2013-04-01

    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

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

    PubMed

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

    2012-02-15

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

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

    PubMed

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

    2012-08-01

    There is a current trend for many laboratories to develop and use qualitative gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS) based multi-residue methods (MRMs) in order to greatly increase the number of pesticides that they can target. Before these qualitative MRMs can be used for the monitoring of pesticide residues in food, their fitness-for-purpose needs to be established by initial method validation. This paper sets out to assess the performances of two such qualitative MRMs against a set of parameters and criteria that might be suitable for their effective validation. As expected, the ease of detection was often dependent on the particular pesticide/commodity combinations that were targeted, especially at the lowest concentrations tested (0.01 mg/kg). The two examples also clearly demonstrated that the percentage of pesticides detected was dependent on many factors, but particularly on the capabilities of the automated software/library packages and the parameters and threshold settings selected for operation. Another very important consideration was the condition of chromatographic system and detector at the time of analysis. If the system was relatively clean, then the detection rate was much higher than if it had become contaminated over time from previous injections of sample extracts. The parameters and criteria suggested for method validation of qualitative MRMs are aimed at achieving a 95% confidence level of pesticide detection. However, the presence of any pesticide that is 'detected' will need subsequent analysis for quantification and, depending on the qualitative method used, further evidence of identity. PMID:22851355

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

    PubMed

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

    2005-01-01

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

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

    PubMed

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

    2012-01-01

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

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

    PubMed

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

    2012-05-01

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

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

    PubMed

    Esturk, Okan; Yakar, Yasin; Ayhan, Zehra

    2014-03-01

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

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

    EPA Science Inventory

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

  7. 75 FR 53690 - Notice of Receipt of Pesticide Petition Filed for Residues of Potassium Peroxymonosulfate in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-09-01

    ... AGENCY Notice of Receipt of Pesticide Petition Filed for Residues of Potassium Peroxymonosulfate in or on... regulations for residues of potassium peroxymonosulfate in or on various commodities. DATES: Comments must be... the requirement of a tolerance for residues of the antimicrobial, potassium peroxymonosulfate, in...

  8. Pesticide residues in tobacco leaves from the Kushtia district in Bangladesh.

    PubMed

    Rahman, Mohammad Abdur; Chowdhury, Alamgir Zaman; Moniruzzaman, Mohammed; Gan, Siew Hua; Islam, Mohammad Nazrul; Fardous, Zeenath; Alam, Mohammad Khorshed

    2012-09-01

    In this study, tobacco leaf samples (n = 26) were collected from different areas in Kushtia to determine the presence of residues of cypermethrin, diazinon, heptachlor, methoxychlor dichlorodiphenyltrichloroethane (DDT), dichlorodiphenyldichloroethan (DDD) and dichlorodiphenyldichloroethylene (DDE). The analysis was conducted by a High Performance Liquid Chromatography (HPLC) system that was equipped with a photodiode array detector. Both cypermethrin and diazinon were detected in tobacco samples from six districts, namely, Mirzapur, Shahebnagar, Kodalipara, Pragpur, Farakpur and Taragunia. The highest concentration of cypermethrin was found in Kodalipara (2.00 ppm) while the highest concentration of diazinon was detected in a sample from Pragpur (0.15 ppm). The pesticide DDT was only detected in the sample from Pragpur at 4.00 ppm. This is the first study in Bangladesh that reports pesticide residue concentrations in tobacco leaf samples. PMID:22782359

  9. SELECTED PESTICIDE RESIDUES AND METABOLITES IN URINE FROM A SURVEY OF THE U.S. GENERAL POPULATION

    EPA Science Inventory

    Residues of toxic chemicals in human tissues and fluids can be important indicators of exposure. Urine collected from a subsample of the second National Health and Nutrition Examination Survey was analyzed for organochlorine, organophosphorus, and chlorophenoxy pesticides or the...

  10. 75 FR 1773 - Notice of Receipt of a Pesticide Petition Filed for Residues of Polymeric Polyhydroxy Acid in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-01-13

    ...This notice announces the Agency's receipt of an initial filing of a pesticide petition proposing the establishment of a regulation for residues of the plant growth regulator, polymeric polyhydroxy acid, in or on all food...

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

    SciTech Connect

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

    1994-10-01

    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.

  12. Children, Pesticides and Cancer.

    ERIC Educational Resources Information Center

    White, Alison

    1998-01-01

    Young children receive higher doses of pesticides than any other age group. The younger a child is the more difficulty the body will have in coping with toxins in general. Maximum Residue Limits (MRL) do not adequately protect children. Evidence of harm from a pesticide often has to be overwhelmingly strong before anything is done about it.…

  13. Persistent organochlorine pesticide residues in fish, sediments and water from Lake Bosomtwi, Ghana.

    PubMed

    Darko, Godfred; Akoto, Osei; Oppong, Caleb

    2008-05-01

    Some organochlorine pesticide residues in tilapia fish (Tilapiazilli), sediment and water samples from Lake Bosomtwi (the largest natural lake in Ghana) were determined to find out the extent of pesticide contamination and accumulation in the lake. The extracted residues were analyzed on a micro-capillary gas chromatograph equipped with electron capture detector. DDE (p,p'-1,1-dichloro-2,2-bis-(4-chlorophenyl)ethylene) was the predominant residue in all the samples analyzed; detected in 82% of water samples, 98% of sediment samples and 58% of fish samples at concentrations of 0.061+/-0.03 ng g(-1), 8.342+/-2.96 ng g(-1) and 5.232+/-1.30 ng g(-1), respectively. DDT (p,p'-1,1,1-trichloro-2,2-bis-(4-chlorophenyl)ethane) was detected in 78% at a mean concentration 0.012+/-0.62 ng g(-1) of water samples analyzed. The mean concentrations of DDT in sediments and fish were 4.41+/-1.54 ng g(-1) and 3.645+/-1.81 ng g(-1), respectively. The detection of lower levels of DDT than its metabolite, DDE, in the samples implies that the presence of these contaminants in the lake is as result of past usage of the pesticides. PMID:18397799

  14. Organophosphorus pesticide residues in raw milk and infant formulas from Spanish northwest.

    PubMed

    Melgar, M J; Santaeufemia, M; Garcia, M A

    2010-10-01

    Residue levels of seven organophosphorus pesticides (OPPs), widely used as dairy cattle ectoparasiticides or in crops used for animal feed, were determined in raw milk and infant formulas. A total of 312 samples were collected (70 from infant formulas and 242 from raw milk) biweekly during a 24-month period. Pesticides were extracted by means of a solid phase system into acetone. An extract aliquot of acetone was injected into a gas chromatograph (GC) with a nitrogen-phosphorus detector. Recoveries of pesticides spiked in milk samples were 62.2 - 97.2 %. The frequency of total samples containing detectable levels of OPP residues was 6.73 % in total milk and 8.67 % in raw milk. The highest percentage incidence measured was for dichlorvos (5.78 %), followed by coumaphos (2.06 %), and parathion methyl (0.83 %). The range of positive results was calculated to be between 0.005 and 0.220 mg kg(- 1). No residue was detected in the final product (infant formulas), so any risk to consumer health, especially to children's health, would be limited. PMID:20803361

  15. The effect of pesticide residue on caged mosquito bioassays.

    PubMed

    Barber, J A S; Greer, Mike; Coughlin, Jamie

    2006-09-01

    Wind tunnel experiments showed that secondary pickup of insecticide residue by mosquitoes in cage bioassays had a significant effect on mortality. Cage bioassays using adult Ochlerotatus taeniorhynchus (Wiedemann) investigated the effect of exposure time to a contaminated surface. Cages were dosed in a wind tunnel using the LC50 for naled (0.124 mg a.i./ml) and an LC25 (0.0772 mg a.i./ml) for naled. Half of the bioassay mosquitoes were moved directly into clean cages with the other half remaining in the sprayed, hence contaminated, cage. Treatment mortality was assessed at 8, 15, 30, 60, 120, 240, and 1,440 min postapplication. Cage contamination had a significant effect on mosquito mortality for both the LC25 and LC50 between 15 and 30 min postapplication. PMID:17067048

  16. Potential transport and degradation of “Aged” pesticide residues in soil

    Technology Transfer Automated Retrieval System (TEKTRAN)

    “Aging” has been shown to affect the sorption-desorption of pesticides in the soil, which in turn can control transport and degradation processes. Aging effects have been characterized by batch sequential extraction methods, in which sorption coefficients (i.e. Kd) are determined for the chemical re...

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

    PubMed

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

    2007-06-01

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

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

    PubMed

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

    2009-12-01

    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

  19. Residues of organochlorine pesticides and polycyclic aromatic hydrocarbons in drinking water of Ahmedabad City, India

    SciTech Connect

    Jani, J.P.; Mistry, J.S. ); Raiyani, C.V.; Patel, J.S.; Desai, N.M.; Kashyap, S.K. )

    1991-09-01

    The ubiquitous environmental pollutants organochlorine pesticides (OCP) and polycyclic aromatic hydrocarbons (PAH) have been extensively studied for their toxicity. Monitoring of OCP and PAH residues has always been considered important for controlling human exposure. As compared to several other countries, the higher body burden of OCP in Indian general population is indicative of higher exposure to these chemicals. Recent studies have shown higher residues of OCP in food commodities including human mother's milk. The levels of OCP in drinking water is still a matter of concern and practically nothing is known about the residues of PAH in drinking water in India. This is the first report of its kind regarding the residues of OCP and PAH in drinking water of Ahmedabad City, the sixth largest city of India with a population of more than 2.5 million.

  20. Concentrations of pesticide residues in tissues of fish from Kolleru Lake in India.

    PubMed

    Amaraneni, S R; Pillala, R R

    2001-01-01

    Kolleru Lake is the largest natural freshwater lake of Andhra Pradesh in India. It is situated between latitudes 16 degrees 32' and 16 degrees 47'N and longitudes 81 degrees 05' and 81 degrees 27'E. The use of pesticides for agricultural purposes is widespread in the Kolleru Lake region. The biological indicators like fish help in the studies of aquatic pollution by pesticides. Fish species Channa striata and Catla catla and water samples were collected from Kolleru Lake in each of three seasons over a period of three years. Fish samples were analyzed according to a modified method which is proposed for the gas chromatographic determination for the pesticides viz., alpha-BHC, gamma-BHC, malathion, chloirpyrifos, isodrin, endosulfan, dieldrin, and p,p-DDT. Water samples were analyzed for selected physico-chemical parameters. The extraction efficiency for the selected pesticides is between 82.8% and 91.2%. The maximum concentrations of pesticide residues in Kolleru Lake fish on wet weight basis are 123.8 micrograms/g for alpha-BHC, 98.7 micrograms/g for gamma-BHC, 2.5 micrograms/g for malathion, 88.6 micrograms/g for chlorpyrifos, 0.91 microgram/g for isodrin, 76.5 micrograms/g for endosulfan, 1.98 micrograms/g for dieldrin, and 157.4 micrograms/g for p,p'-DDT. These analyses were used to evaluate the baseline data and the pesticide pollution in the lake's ecosystem. PMID:11769254

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

    PubMed

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

    2016-06-01

    Twenty-two commonly used pesticides were monitored during autumn, winter, and summer of 2004-2005 in 27 water samples from three sites along the White Nile in Sudan (former Sudan). Sites were selected to reflect pesticides gathered from drainage canals in central Sudan and from upstream sources. Collected samples were extracted and subjected to gas chromatographic analysis. Pesticides levels were measured in nanograms per liter. Pesticides residues were detected in 96 % of the samples with a total residue burden of 4132.6 ng L(-1), and an overall mean concentration and range of 50.99 and not detected-1570 ng L(-1), respectively. Ororganochlorines were the most frequently detected contaminants, which were found in 70 % of the samples, causing a total burden of 2852.8 ng L(-1), followed by pyrethroids 15 % of the samples, with a total burden of 926.5 ng L(-1). The tested herbicides were detected in ˂4 % of the samples with a total burden of 353.3 ng L(-1), while organophosphorus levels were below the detection limit. The most frequent contaminants were the following: heptachlor and its epoxide (52 % of samples), followed by DDTs (dichlorodiphenyltrichloroethanes) (DDT and DDE, in 19 % of the samples), cypermethrin and fenvalerate (in 11 % of the samples), and pendimethalin (in <4 % of the samples). Residues of hexachlorocyclohexane (HCH) isomers (α, β, γ and δ), endosulfan (α and β), p, p-DDD, λ cyhalothrin, deltamethrin, and oxyfluorfen were not detected in the analyzed samples. Generally, levels were least in autumn, and followed by summer and winter. Sources of contamination might include agricultural lands in central Sudan and upstream sources. Both recent and old contaminations were indicated. PMID:27230426

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

    PubMed

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

    2015-03-01

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

  3. Dietary exposure of Hong Kong adults to pesticide residues: results of the first Hong Kong Total Diet Study.

    PubMed

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

    2014-01-01

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

  4. A smartphone-readable barcode assay for the detection and quantitation of pesticide residues.

    PubMed

    Guo, Juan; Wong, Jessica X H; Cui, Caie; Li, Xiaochun; Yu, Hua-Zhong

    2015-08-21

    In this paper, we present a smartphone-readable barcode assay for the qualitative detection of methyl parathion residues, a toxic organophosphorus pesticide that is popularly used in agriculture worldwide. The detection principle is based on the irreversible inhibition of the enzymatic activity of acetylcholinesterase (AchE) by methyl parathion; AchE catalytically hydrolyzes acetylthiocholine iodine to thiocholine that in turn dissociates dithiobis-nitrobenzoate to produce a yellow product (deprotonated thio-nitrobenzoate). The yellow intensity of the product was confirmed to be inversely dependent on the concentration of the pesticide. We have designed a barcode-formatted assay chip by using a PDMS (polydimethylsiloxane) channel plate (as the reaction reservoir), situated under a printed partial barcode, to complete the whole barcode such that it can be directly read by a barcode scanning app installed on a smartphone. The app is able to qualitatively present the result of the pesticide test; the absence or a low concentration of methyl parathion results in the barcode reading as "-", identifying the test as negative for pesticides. Upon obtaining a positive result (the app reads a "+" character), the captured image can be further analyzed to quantitate the methyl parathion concentration in the sample. Besides the portability and simplicity, this mobile-app based colorimetric barcode assay compares favorably with the standard spectrophotometric method. PMID:26087169

  5. Selective, solid-matrix dispersion extraction of organophosphate pesticide residues from milk.

    PubMed

    Di Muccio, A; Pelosi, P; Camoni, I; Attard Barbini, D; Dommarco, R; Generali, T; Ausili, A

    1996-11-22

    A rapid procedure has been developed that allows a single-step, selective extraction and cleanup of organophosphate (OP) pesticide residues from milk dispersed on solid-matrix diatomaceous material filled into disposable cartridges by means of light petroleum saturated with acetonitrile and ethanol. Recovery experiments were carried out on homogenized commercial milk (3.6% fat content) spiked with ethanolic solutions of 24 OP pesticides, viz., ethoprophos, diazinon, dimethoate, chlorpyrifos-methyl, parathion-methyl, chlorpyrifos-ethyl, malathion, isofenphos, quinalphos, ethion, pyrazophos, azinphosethyl, heptenophos, omethoate, fonofos, pirimiphos-methyl, fenitrothion, parathion, chlorfenvinphos, phenthoate, methidathion, triazophos, phosalone, azinphos-methyl, at levels ranging for the different OP pesticides from 0.02 mg/kg to 1.11 mg/kg. Average recoveries of four replicates were in the range 72-109% for the different OP pesticides, with relative standard deviations (R.S.D.) from ca. 1 to 19%, while dimethoate and omethoate were not recovered. Coextracted fatty material amounted to an average of about 4.0 mg/ml of milk. The extraction procedure requires about 30 min. The main advantages are that extraction and cleanup are carried out in a single step, emulsions do not occur, several samples can be run in parallel by a single operator, reusable glassware is not needed and simple operations are required. PMID:8997741

  6. De-contamination of pesticide residues in food by ionizing radiation

    NASA Astrophysics Data System (ADS)

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

    2012-04-01

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

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

    PubMed

    Malinowska, Elżbieta; Jankowski, Kazimierz

    2015-12-01

    The aim of this paper was to assess residue content of plant protection products in selected herbs: Achillea millefolium L., Cichorium intybus L., Equisetum arvense L., Polygonum persicaria L., Plantago lanceolata L., and Plantago major L. The study comprises herbs growing in their natural habitat, 1 and 10 m away from crop fields. The herbs, 30 plants of each species, were sampled during the flowering stage between 1 and 20 July 2014. Pesticide residue content was measured with the QuECHERS method in the dry matter of leaves, stalks, and inflorescence, all mixed together. Out of six herb species growing close to wheat and maize fields, pesticide residues were found in three species: A. millefolium L., E. arvense L., and P. lanceolata L. Most plants containing the residues grew 1 m away from the wheat field. Two active substances of fungicides were found: diphenylamine and tebuconazole, and one active substance of insecticides: chlorpyrifos-ethyl. Those substances are illegal to use on herbal plants. Samples of E. arvense L. and P. lanceolata L. contained two active substances each, which constituted 10% of all samples, while A. millefolium L. contained one substance, which is 6.6% of all samples. PMID:26612566

  8. Contributions of pesticide residue chemistry to improving food and environmental safety: past and present accomplishments and future challenges.

    PubMed

    Seiber, James N; Kleinschmidt, Loreen A

    2011-07-27

    The principles of modern pesticide residue chemistry were articulated in the 1950s. Early authors pointed out the advantages of systematizing and standardizing analytical methods for pesticides so that they could be widely practiced and the results could be reproduced from one laboratory to the next. The availability of improved methods has led to a much more complete understanding of pesticide behavior and fate in foods and the environment. Using methods based largely upon gas chromatography (GC) and high-performance liquid chromatography (HPLC) coupled increasingly with mass spectrometry (MS) and MS(n) as the detection tool, residues can be measured at parts per billion levels and below in a variety of food and environmental matrices. Development of efficient extraction and cleanup methods, techniques such as ELISA, efficient sample preparation techniques such as QuEChERS, and automated laboratory and field instrumentation has also contributed to the tools available for use in modern pesticide residue analysis. As a result, great strides have been made in improving food and worker safety and in understanding environmental behavior and fate of pesticides. There are many challenges remaining in the field of pesticide residue chemistry that will continue to stimulate analytical chemists. New chemistries are emerging, often patterned on complex natural products. Analyzing for the parent chemicals and potentially multiple breakdown products will require analytical ingenuity. The development of more sensitive bioassays and knowledge of unintended side effects will challenge residue chemistry as well, as in the case of following the fate of environmental endocrine disruptors associated with some pesticides as well as nonpesticide contaminants from packaging materials and other familiar articles. Continued funding and other resources to ensure better training, international cooperation, and accelerated research and development activities will be a constant need in

  9. Release of aged 14C-atrazine residues from soil facilitated by dry-wet cycles

    NASA Astrophysics Data System (ADS)

    Jablonowski, N. D.; Yu, K.; Koeppchen, S.; Burauel, P.

    2012-04-01

    Intermittent dry-wet cycles may have an important effect on soil structure and aged pesticide residues release (1). A laboratory study was conducted to assess the maximum potential of water extractable aged atrazine residues influenced by soil drying and wetting. The used soil was obtained from an outdoor lysimeter (gleyic cambisol; Corg: 1.45%), containing environmentally aged (22 years) 14C-atrazine residues. For the experiment, soil from 0-10 cm depth was used since most residual 14C activity was previously found in this layer (2,3). Triplicate soil samples with a residual water content of approx. 8% were either dried (45° C) prior water addition or directly mixed with distilled water (soil+water: 1+2, w:w). The samples were shaken (150 rmp, 60 min, at 21° C), centrifuged (approx. 2000 g), and the supernatants were filtered. Water-extracted residual 14C activity was detected via liquid scintillation counter. The total water-extracted 14C activity (the amount of residual 14C activity in a sample equals 100%) was significantly higher (p

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

    PubMed

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

    2011-11-01

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

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

    PubMed

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

    2012-04-01

    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 (γ-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 μg/L prescribed for HCH under the prevention of food adulteration act. Therefore, the present study recommends continuous monitoring with larger sample size. PMID:22323047

  12. ANALYSIS OF PESTICIDE RESIDUES IN HUMAN AND ENVIRONMENTAL SAMPLES: A COMPILATION OF METHODS SELECTED FOR USE IN PESTICIDE MONITORING PROGRAMS

    EPA Science Inventory

    This manual provides the pesticide chemist with methodology useful in determining human exposure to pesticides and related industrial chemicals. Methods are also presented for measuring the extent of environmental contamination with these compounds. This manual has been compiled ...

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

    PubMed Central

    2010-01-01

    Background Organophosphorous pesticides are the most popular pesticides used in agriculture. As acetylcholinesterase inhibitors, organophosphorous pesticides are toxic organic chemicals. The control and detection of organophosphorous pesticide residue in food, water, and environment therefore plays a very important role in maintaining physical health. A sensitive, rapid, simple chemiluminescence(CL) method has been developed for the determination of quinalphos based on the reaction of quinalphos with luminol-H2O2 in an alkaline medium. The method has been applied to detection of quinalphos in vegetable samples with satisfactory results. Results The CL method for the determination of organophosphorous pesticide quinalphos is based on the phenomenon that quinalphos can apparently enhance the CL intensity of the luminol-H2O2 system. The optimal conditions were: luminol concentration 5.0 × 10-4 mol/L, H2O2 concentration 0.05 mol/L.pH value 13. In order to restrain the interference from metal ions, 1.0 × 10-3 mol/L of EDTA was added to the luminol solution. The possible mechanism was proposed. Conclusion Under the optimum reaction conditions, CL was linear with the concentration of quinalphos in the range of 0.02 μg/mL -1.0 μg/mL and the detection limit was 0.0055 μg/mL (3σ). This method has been successfully applied to the detection of quinalphos in vegetable samples. According to the experimental data, the average recoveries for quinalphos in cherry tomato and green pepper 97.20% and 90.13%. Meanwhile, the possible mechanism was proposed. PMID:20576096

  14. Realistic approach of pesticide residues and French consumer exposure within fruit & vegetable intake.

    PubMed

    Drouillet-Pinard, Peggy; Boisset, Michel; Periquet, Alain; Lecerf, Jean-Michel; Casse, Francine; Catteau, Michel; Barnat, Saida

    2011-01-01

    The increase of fruit and vegetable (F&V) intake contributes to the prevention of chronic diseases, but could also significantly increase pesticide exposure and may thus be of health concern. Following a previous pesticide exposure assessment study, the present study was carried out to determine actual levels of pesticides within 400 g of F&V intake and to evaluate consumer risk. Forty-three Active Substances (AS) exceeding 10 % of the Acceptable Daily Intake (ADI) in balanced menus established for our previous theoretical study were considered. Fifty-six pooled food samples were analyzed: 28 fruit samples and 28 vegetable samples. Pesticide values were compared to Maximum Residue Levels (MRL) and to the "toxicological credit" derived from ADI. It was observed that 23 out of the 43 retained AS were never detected, 5 were detected both in F&V samples, 12 only in fruits and 3 only in vegetables. The most frequently detected AS were carbendazim, iprodione and dithiocarbamates. When detected, AS were more frequently found in fruit samples (74 %) than in vegetable samples (26 %). A maximum of 3 AS were detected at once in a given sample. Overall, we observed 8 and 14 overruns of the MRL in 1204 measures in pooled vegetable and fruit samples, respectively (0.7 % and 1.2 % of cases, respectively). Chronic exposure for adults was the highest for dithiocarbamates but did not exceed 23.7 % of the ADI in F&V. It was concluded that raising both F&V consumption up to 400 g/day (~5 F&V/day) according to recommendations of the national health and nutrition plan, does not induce pesticide overexposure and should not represent a risk for the consumer. PMID:21191868

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

    PubMed

    Masci, Maurizio; Orban, Elena; Nevigato, Teresina

    2014-01-01

    A sampling campaign from 21 sites in Italy was carried out to investigate the presence of organochlorine pesticide residues in different fish species. Samples came from marine fishery and either from sea- or freshwater aquaculture. Fish feed used in some fish farms were also analyzed. Pesticides studied belong to Persistent Organic Pollutants widely used in the past such as DDT, chlordane, heptachlor, and others. To ensure good quality results and proper data validation the main existing guidelines in the field were applied. The instrumental technique was a Dual column-Dual detector Gas Chromatography (GC-ECD and Ion Trap GC-MS) which allowed that complementary data on the same sample were acquired. Results for fishery showed a wide range of concentrations depending from the area and species examined. DDT, the major OC pesticide detected, varied from 0.02 to 130.03 ng g(-1) edible portion. As regards the products of aquaculture we observed slightly lower average levels of pollutants in a more narrow range of concentration: this is probably due to fish feed used as shown by some measures performed in the present study. Organochlorine pesticide residues were detected in all samples examined but they were generally well below the existing tolerance or action levels. Also the estimated daily intakes are well below than those recommended by WHO. This is a good indication about OCPs in the areas investigated but some further considerations on fish safety must be taken into account. An example on how fishes may act as bioindicators is reported. PMID:24184045

  16. Removal of 16 pesticide residues from strawberries by washing with tap and ozone water, ultrasonic cleaning and boiling.

    PubMed

    Lozowicka, Bozena; Jankowska, Magdalena; Hrynko, Izabela; Kaczynski, Piotr

    2016-01-01

    The effects of washing with tap and ozone water, ultrasonic cleaning and boiling on 16 pesticide (ten fungicides and six insecticides) residue levels in raw strawberries were investigated at different processing times (1, 2 and 5 min). An analysis of these pesticides was conducted using gas chromatography with nitrogen-phosphorous and electron capture detection (GC-NPD/ECD). The processing factor (PF) for each pesticide in each processing technique was determined. Washing with ozonated water was demonstrated to be more effective (reduction from 36.1 to 75.1 %) than washing with tap water (reduction from 19.8 to 68.1 %). Boiling decreased the residues of the most compounds, with reductions ranging from 42.8 to 92.9 %. Ultrasonic cleaning lowered residues for all analysed pesticides with removal of up to 91.2 %. The data indicated that ultrasonic cleaning and boiling were the most effective treatments for the reduction of 16 pesticide residues in raw strawberries, resulting in a lower health risk exposure. Calculated PFs for alpha-cypermethrin were used to perform an acute risk assessment of dietary exposure. To investigate the relationship between the levels of 16 pesticides in strawberry samples and their physicochemical properties, a principal component analysis (PCA) was performed. Graphical abstract ᅟ. PMID:26694708

  17. Investigation into the validity of extrapolation in setting maximum residue levels for pesticides in crops of similar morphology.

    PubMed

    Reynolds, S L; Fussell, R J; MacArthur, R

    2005-01-01

    Field trials were initiated to investigate if extrapolation procedures, which were adopted to limit costs of pesticide registration for minor crops, are valid. Three pairs of crops of similar morphology; carrots/swedes, cauliflower/calabrese (broccoli) and French beans/edible-podded peas; were grown in parallel at four different geographical locations within the UK. The crops were treated with both systemic and non-systemic pesticides under maximum registered use conditions, i.e. the maximum permitted application rates and the minimum harvest intervals. Once mature, the crops were harvested and analysed for residues of the applied pesticides. The limits of quantification were in the range 0.005-0.02 mg kg(-1). Analysis of variance and bootstrap estimates showed that in general, the mean residue concentrations for the individual pesticides were significantly different between crop pairs grown on each site. Similarly, the mean residue concentrations of most of the pesticides in each crop across sites were significantly different. These findings demonstrate that the extrapolations of residue levels for most of the selected pesticide/crop combinations investigated; chlorfenvinphos and iprodione from carrots to swedes; carbendazim, chlorpyrifos, diflubenzuron and dimethoate from cauliflower to calabrese; and malathion, metalaxyl and pirimicarb from French beans to edible-podded peas; appear invalid. PMID:15895609

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

    PubMed

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

    2013-10-01

    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 β-, γ-HCH, p,p' DDD, p,p' DDE, p,p' DDT and endrin with mean concentration of 97.9, 101.7, 239.8, 1574.1, 100.3 and 90.7 ng g(-1) lipid wt., respectively. In addition, occurrence of β-endosulfan, endosulfan sulphate, cypermethrin and chlorpyrifos in this study have also been reported for the first time in human breast milk in Punjab, India. With increase in parity, HCH and DDT residue burden in donor's milk decreased. Although levels of HCH and DDT residues in breast milk samples have decreased significantly, yet estimated daily intake values for DDT are higher than the FAO/WHO permissible tolerable daily intake values for few infants. PMID:23850662

  19. [Validation of ELISA Kits for Pesticide Residue Analysis in Vegetables and Fruits].

    PubMed

    Yamasaki, Tomomi; Inoue, Tomomi; Hirakawa, Yuki; Miyake, Shiro; Ueno, Eiji; Saito, Isao

    2015-01-01

    Five kinds of commercially available ELISA kits (acetamiprid, azoxystrobin, chlorothalonil, fenitrothion and imidacloprid) were validated for determination of pesticide residues in vegetables and fruits. The reaction characteristics were also examined to evaluate their influence on the determinations. The trueness value was 91-162%, the repeatability was 2.1-16.2%, and the reproducibility was 4.0-20.3%. The desired values were achieved for 18 among 30 combinations (60%) of the ELISA kits and the agricultural products examined. A standard curve was necessary for each of the ELISA examinations. The matrix of the agricultural products and pipetting skill of the lab technician both influenced the measurment results. PMID:26699271

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

    PubMed

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

    2013-05-22

    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

  1. Development, validation and determination of multiclass pesticide residues in cocoa beans using gas chromatography and liquid chromatography tandem mass spectrometry.

    PubMed

    Zainudin, Badrul Hisyam; Salleh, Salsazali; Mohamed, Rahmat; Yap, Ken Choy; Muhamad, Halimah

    2015-04-01

    An efficient and rapid method for the analysis of pesticide residues in cocoa beans using gas and liquid chromatography-tandem mass spectrometry was developed, validated and applied to imported and domestic cocoa beans samples collected over 2 years from smallholders and Malaysian ports. The method was based on solvent extraction method and covers 26 pesticides (insecticides, fungicides, and herbicides) of different chemical classes. The recoveries for all pesticides at 10 and 50 μg/kg were in the range of 70-120% with relative standard deviations of less than 20%. Good selectivity and sensitivity were obtained with method limit of quantification of 10 μg/kg. The expanded uncertainty measurements were in the range of 4-25%. Finally, the proposed method was successfully applied for the routine analysis of pesticide residues in cocoa beans via a monitoring study where 10% of them was found positive for chlorpyrifos, ametryn and metalaxyl. PMID:25442595

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

    PubMed

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

    2015-09-01

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

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

    PubMed Central

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

    2014-01-01

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

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

    NASA Astrophysics Data System (ADS)

    Mukherjee, S.

    2015-12-01

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

  5. Occurrence of organochlorine pesticide residues in eggs, chicken and meat in Jordan.

    PubMed

    Ahmad, Rafat; Salem, Nida' M; Estaitieh, Hussein

    2010-02-01

    Organochlorine pesticide (OCP) residues in 519 samples; comprising eggs, chicken and meat (lamb and beef), collected from Jordan were determined. All samples were analyzed for their residual contents of aldrin, dichlorodiphenyltrichloroethane and metabolites (DDTs), dieldrin, endosulfan isomers, endrin, hexachlorocyclohexane isomers (HCHs), heptachlor, heptachlor epoxide and hexachlorobenzene (HCB). The samples were Soxhlet extracted for 8h in 250mL petroleum ether. The cleanup of the samples was performed by Florisil column chromatography and analysis was done on a gas chromatography equipped with an electron capture detector (GC-ECD). The results indicated that 28% (38/134), 20% (23/115) and 49% (131/270) of the examined eggs, chicken and meat samples, respectively, were contaminated with OCP residues. HCHs and DDTs are the most prominently noticed compounds, as they were detected at a high incidence. On the other hand, heptachlor, heptachlor epoxide, HCB, aldrin and endrin compounds were only present in less than 7% of the analyzed samples. These residues are present despite complete ban on the use of OCPs for agricultural purposes in Jordan. No residues of op'-DDD, op'-DDT, dieldrin, alpha-endosulfan and beta-endosulfan were detected. PMID:20042222

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

    PubMed

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

    2016-05-01

    Most countries have clearly defined regulations governing the use of pesticides in agricultural activity. The application of pesticides in agriculture usually leads to a residual amount of these pesticides on food products such as fruit and vegetables. The presence of pesticide residues on these foods destined for human consumption may pose food safety risks to consumers. To protect consumers, national authorities have established maximum limits for pesticide residues in foods. These limits can only be enforced if there are methods available to detect and monitor their concentrations in the applicable food products. To support the enforcement of this legislation, we have developed a multi-residue liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the analysis of 120 pesticide residues in apples and cucumbers which has been validated and implemented in the routine monitoring and surveillance programme for these pesticides. In this method, apple and cucumber samples are extracted using the QuEChERS method (quick, easy, cheap, effective, rugged, and safe) and the extracts were analyzed directly by LC-MS/MS. The mean recoveries at three different concentrations of 0.01 µg/g , 0.05 µg/g, and 0.1 µg/g over the analytical range varied between 70 and 120%. The repeatability of the method expressed as %RSD was less than 20%. The limit of detection (LOD) of the method ranged between 0.0014 and 0.0110 µg/g for apples and between 0.0012 and 0.0075 µg/g for cucumbers. The limit of quantification (LOQ) of the method was 0.01 µg/g for apples and cucumbers. The method has been used for the analysis of over 600 apple and 550 cucumber samples over the past two years. Copyright © 2016 John Wiley & Sons, Ltd. PMID:27443204

  7. Pesticide residues in vineyard soils from Spain: Spatial and temporal distributions.

    PubMed

    Pose-Juan, Eva; Sánchez-Martín, María J; Andrades, M Soledad; Rodríguez-Cruz, M Sonia; Herrero-Hernández, Eliseo

    2015-05-01

    Spatial and temporal evaluations of seventeen pesticides and some of their degradation products were carried out in seventeen vineyard soils from La Rioja region (Spain). The soils were sampled in March, June and October 2012, and the pesticides were selected among those previously detected in surface and ground waters from the same area. All pesticides were detected in some of the soils in the three different areas of La Rioja at the different sampling times, with only the metalaxyl metabolite, CGA-62826, not being detected in any of the soils sampled in October. The highest concentrations were determined for the fungicides metalaxyl (11.5 μg kg(-1)) and triadimenol (26.1 μg kg(-1)), the herbicides fluometuron (174.6 μg kg(-1)) and terbuthylazine (403.3 μg kg(-1)), and the insecticide methoxyfenozide (4.61 μg kg(-1)). While the highest total concentration of pesticides was detected in March, the highest number of positive detections was recorded in June (46), as opposed to 26 and 19 in March and October, respectively. Significant differences were detected in the concentrations of herbicides in soils from the three areas in La Rioja, but this was not the case for the fungicides and the insecticides. The study revealed a more intensive use of herbicides in March, while the use of insecticides and fungicides probably depended on the specific needs of crops and/or the onset of diseases. The results are consistent with the residues found in waters in the region, and highlight the need to implement strategies for more efficient application of these compounds to avoid risk of water contamination. PMID:25679815

  8. Pesticide residues in eggs of wild birds: Adjustment for loss of moisture and lipid

    USGS Publications Warehouse

    Stickel, L.F.; Wiemeyer, Stanley N.; Blus, L.J.

    1973-01-01

    Eggs of wild birds collected for the purpose of measuring concentrations of pesticides or other pollutants vary from nearly fresh to nearly dry so that objective comparisons cannot be made on the basis of weight of the contents at the time of collection. Residue concentrations in the nearly dry eggs can be greatly exaggerated by this artifact. Valid interpretation of residue data depends upon compensation for these losses. A method is presented for making adjustments on the basis of volume of the egg, and formulas are derived for estimating the volume of eggs of eagles, ospreys, and pelicans from egg measurements. The possibility of adjustments on the basis of percentage of moisture, solids, or fat in fresh eggs is discussed also.

  9. Organochlorine pesticide residues in moths from the Baltimore, MD-Washington, DC area

    USGS Publications Warehouse

    Beyer, W.N.; Kaiser, T.E.

    1984-01-01

    Moths were collected with a light trap from 15 sites in the Baltimore, Maryland - Washington, D.C. area and analyzed for organochlorine pesticide residues. On the average, the species sampled contained 0.33 ppm heptachlor-chlordane compounds, 0.25 ppm DDE, and 0.11 ppm dieldrin. There were large differences in the concentrations detected in different species. Concentrations were especially high in moths whose larvae were cutworms, and were virtually absent from moths whose larvae fed on tree leaves. It was concluded that at least some species sampled could be an important source of insecticides to insectivorous wildlife. In some instances moths may be useful indicators of environmental contamination, especially when insectivorous wildlife species cannot be collected. However, the differences in residues observed among species means that only similar species should be compared, and this limits their potential for monitoring.

  10. Analysis of pesticide multi-residues in leafy vegetables by ultrasonic solvent extraction and liquid chromatography-tandem mass spectrometry.

    PubMed

    Pan, Jian; Xia, Xiao-Xiao; Liang, Juan

    2008-01-01

    Ultrasonic solvent extraction (USE) of pesticide multi-residues including monocrotophos, dimethoate, imidacloprid, carbendazim, carbaryl and simazine from leafy vegetables is presented. The extraction procedure was optimized with regard to the solvent type and amount, sonication time and number of extraction steps. The extract did not need clean-up before injected into liquid chromatography-tandem mass spectrometry (LC-MS-MS) which was employed together with electron microscope to verify the effect of USE method. The proposed procedure allows the extraction of six pesticide residues in a single step with 40 ml of ethyl acetate for 35 min sonication, providing recovery over 83% and LOQ less than 1.4 microg/kg. The optimized USE method is a simple, low cost and an effective preparation method for determination of pesticide multi-residues at trace levels in leafy vegetables in comparison with homogenized extraction method. PMID:17664080

  11. Contribution of Sample Processing to Variability and Accuracy of the Results of Pesticide Residue Analysis in Plant Commodities.

    PubMed

    Ambrus, Árpád; Buczkó, Judit; Hamow, Kamirán Á; Juhász, Viktor; Solymosné Majzik, Etelka; Szemánné Dobrik, Henriett; Szitás, Róbert

    2016-08-10

    Significant reduction of concentration of some pesticide residues and substantial increase of the uncertainty of the results derived from the homogenization of sample materials have been reported in scientific papers long ago. Nevertheless, performance of methods is frequently evaluated on the basis of only recovery tests, which exclude sample processing. We studied the effect of sample processing on accuracy and uncertainty of the measured residue values with lettuce, tomato, and maize grain samples applying mixtures of selected pesticides. The results indicate that the method is simple and robust and applicable in any pesticide residue laboratory. The analytes remaining in the final extract are influenced by their physical-chemical properties, the nature of the sample material, the temperature of comminution of sample, and the mass of test portion extracted. Consequently, validation protocols should include testing the effect of sample processing, and the performance of the complete method should be regularly checked within internal quality control. PMID:26755282

  12. Flexible and Adhesive Surface Enhance Raman Scattering Active Tape for Rapid Detection of Pesticide Residues in Fruits and Vegetables.

    PubMed

    Chen, Jiaming; Huang, Youju; Kannan, Palanisamy; Zhang, Lei; Lin, Zhenyu; Zhang, Jiawei; Chen, Tao; Guo, Longhua

    2016-02-16

    The efficient extraction of targets from complex surfaces is vital for technological applications ranging from environmental pollutant monitoring to analysis of explosive traces and pesticide residues. In our present study, we proposed a proof-of-concept surface enhance Raman scattering (SERS) active substrate serving directly to the rapid extraction and detection of target molecules. The novel substrate was constructed by decorating the commercial tape with colloidal gold nanoparticles (Au NPs), which simultaneously provides SERS activity and "sticky" of adhesive. The utility of SERS tape was demonstrated by directly extracting pesticide residues in fruits and vegetables via a simple and viable "paste and peel off" approach. The obtained strong and easily distinguishable SERS signals allow us to detect various pesticide residues such as parathion-methyl, thiram, and chlorpyrifos in the real samples with complex surfaces including green vegetable, cucumber, orange, and apple. PMID:26810698

  13. Pesticide residues in river Yamuna and its canals in Haryana and Delhi, India.

    PubMed

    Kaushik, C P; Sharma, H R; Jain, S; Dawra, J; Kaushik, A

    2008-09-01

    Yamuna, a prominent river of India covers an extensive area of 345,843 km(2) from Yamunotri glacier through six Indian states. Residues of organochlorine pesticides (OCPs) namely, isomers of HCH and endosulfan, DDT and its metabolites, aldrin, dieldrin, were analysed in water of river Yamuna along its 346 km stretch passing through Haryana-Delhi-Haryana and the canals originating from it. beta-HCH, p.p'-DDT, p.p'-DDE and p.p'-DDD had maximum traceability in test samples (95-100%) followed by gamma-HCH, alpha-HCH and o.p'-DDD (60-84%) and o.p'-DDT, delta-HCH and o.p'-DDE (7-30%) while aldrin, dieldrin, alpha and beta endosulfan remained below detection limits (BDL). The concentration of SigmaHCH and SigmaDDT at different sites of the river ranged between 12.76-593.49 ng/l (with a mean of 310.25 ng/l) and 66.17-722.94 ng/l (with a mean of 387.9 ng/l), respectively. In canals the values were found between 12.38-571.98 ng/l and 109.12-1572.22 ng/l for SigmaHCH and SigmaDDT, respectively. Water of Gurgaon canal and Western Yamuna canal contained maximum and minimum concentration, respectively both of SigmaHCH and SigmaDDT residues. Sources of these pesticides and suggested measures to check pesticide pollution of this major Indian river, keeping in view its vital link with life, are discussed in this paper. PMID:18044005

  14. Distribution of aged atrazine related 14C-residues in natural soil following incubation with the earthworm Apporectodea caliginosa.

    NASA Astrophysics Data System (ADS)

    Andreou, K.; Jablonowski, N.; Jones, K.; Burauel, P.; Semple, K.

    2009-04-01

    The distribution and localisation of atrazine related 14C-residues into the different physical fractions of soil may reveal information on processes taking place in soil. Soils amended with 14C-atrazine, were aged for 22 years under environmental conditions in a lysimeter in Germany. The soil was sampled and subjected to physical and chemical fractionation before and after incubation for 7 days with the earthworm Apporectodea caliginosa. No significant change in the soil physical and chemical fractionation of the atrazine related 14C-residues and organic carbon was observed in this study due to the activity of the A. caliginosa. The smaller size soil fractions (Microaggregates and Colloids) were highly enriched with aged atrazine 14C-residues equivalents and organic carbon. Also the humic acid extracted using a simple alkaline extraction have were also enriched with aged atrazine 14C-residues equivalents. The low organic carbon content of the soil, the absence of relatively fresh organic matter and the long ageing time might explain the limited bioavailability of the atrazine related 14C-residues to the earthworm. This finding is of particular importance given that the soil used here was aged under natural environmental conditions compared to laboratory studies. Earthworms are important species in soil ecology and thus, the question of the bioavailability of aged pesticide residues to such organism is critical. The bioavalability of the atrazine 14C-residues equivalent was absent in the current study illustrating that those aged residues posed minimal risk to earthworms.

  15. Distribution of aged atrazine related 14C-residues in natural soil following incubation with the earthworm Apporectodea caliginosa

    NASA Astrophysics Data System (ADS)

    Andreou, Kostas; Semple, Kirk; Jones, Kevin

    2010-05-01

    The distribution and localisation of atrazine related 14C-residues into the different physical fractions of soil may reveal information on processes taking place in soil. Soils amended with 14C-atrazine, were aged for 22 years under environmental conditions in a lysimeter in Germany. The soil was sampled and subjected to physical and chemical fractionation before and after incubation for 7 days with the earthworm Apporectodea caliginosa. No significant change in the soil physical and chemical fractionation of the atrazine related 14C-residues and organic carbon was observed in this study due to the activity of the A. caliginosa. The smaller size soil fractions (Microaggregates and Colloids) were highly enriched with aged atrazine 14C-residues equivalents and organic carbon. Also the humic acid extracted using a simple alkaline extraction have were also enriched with aged atrazine 14C-residues equivalents. The low organic carbon content of the soil, the absence of relatively fresh organic matter and the long ageing time might explain the limited bioavailability of the atrazine related 14C-residues to the earthworm. This finding is of particular importance given that the soil used here was aged under natural environmental conditions compared to laboratory studies. Earthworms are important species in soil ecology and thus, the question of the bioavailability of aged pesticide residues to such organism is critical. The bioavalability of the atrazine 14C-residues equivalent was absent in the current study illustrating that those aged residues posed minimal risk to earthworms.

  16. Highly sensitive terahertz spectroscopy of residual pesticide using nano-antenna

    NASA Astrophysics Data System (ADS)

    Lee, Dong-Kyu; Kim, Giyoung; Son, Joo-Hiuk; Seo, Minah

    2016-02-01

    In this report, a novel type of highly sensitive small molecule sensing tool has been employed to detect residual pesticide molecules including e. g. methomyl using terahertz (THz) time-domain spectroscopy (TDS) system with nano-slotantenna array. Enhance THz wave by the nano-slot-antenna array induces strong THz field enhancement around nano antenna and thus increases an absorption cross section leading to the detection sensitivity upto ppm level even in solution state. Measured spectrums in transmission and reflection show an excellent performance in both sensitivity and selectivity. We also tested the performance of our nano-antenna array in reflection imaging geometry to simply detect the contained residual pesticide at the real fruit surface as it is, without any extraction or sampling preprocess. The clear difference in the obtained THz reflection image distinguishes the stained area with methomyl from the bare area. Our observation can offer the possibility for further application as a prompt and an accurate small molecule monitoring tool in real time. A quantitative analysis tool for such small molecule can be also developed by this method.

  17. Simultaneous determination of pyrethroids from pesticide residues in porcine muscle and pasteurized milk using GC.

    PubMed

    Khay, Sathya; Abd El-Aty, A M; Choi, Jeong-Heui; Shin, Eun-Ho; Shin, Ho-Chul; Kim, Jin-Suk; Chang, Byung-Joon; Lee, Chi-Ho; Shin, Sung-Chul; Jeong, Ji Yoon; Shim, Jae-Han

    2009-01-01

    The principal goal of this work was to develop an efficient method for the simultaneous determination of four pyrethroid (PYR) insecticides, cyfluthrin, cyhalothrin, cypermethrin, and deltamethrin, in porcine muscle and pasteurized milk using liquid-liquid extraction (LLE). Sample extraction was carried out with and without additional column cleanup procedures, and the final determination was made using GC with electron-capture detector (ECD). The pesticide identity was confirmed using GC-MS in the SIM mode. Since there were minor differences between the extraction procedures, extraction without the additional cleanup procedure was used throughout the work. The method was validated by fortifying blank samples with half, two, and four times the maximum residue limit (MRL) of each PYR. The average recoveries (n = 6) ranged from 83.5 to 99.2% and 82.9 to 109% in porcine muscle and pasteurized milk, respectively. The repeatability of measurements expressed as RSDs, was in the range of 1.7-11.9 and 1.5-10.3% in porcine muscle and pasteurized milk, respectively. The LODs ranged from 3.3 to 9 and 3 to 8.1 ppm, whereas the LOQs ranged from 10 to 27.4 and 9 to 24.6 ppm, in porcine muscle and pasteurized milk, respectively. The applicability of the method was demonstrated by analyzing real samples collected from major cities in the Republic of Korea. No residues of the selected pesticides were detected in any of the samples. PMID:19107766

  18. 75 FR 11171 - Notice of Filing of Several Pesticide Petitions for Residues of Pesticide Chemicals in or on...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-03-10

    ... limited to: Crop production (NAICS code 111). Animal production (NAICS code 112). Food manufacturing (NAICS code 311). Pesticide manufacturing (NAICS code 32532). This listing is not intended to...

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

    PubMed

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

    2012-05-01

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

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

    PubMed

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

    2010-12-01

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

  1. Age-related differences in neurotoxicity produced by organophosphorus and N-methyl carbamate pesticides

    EPA Science Inventory

    Potential pesticide effects in infants and toddlers have received much attention in the scientific literature and the public media, including the concern for increased response to acute or shortterm exposures. Age-related differences in the acute neurotoxicity of acetylcholinest...

  2. Pesticide exposure of two age groups of women and its relationship with their diet.

    PubMed

    Rivas, Ana; Cerrillo, Isabel; Granada, Alicia; Mariscal-Arcas, Miguel; Olea-Serrano, Fatima

    2007-08-15

    The widespread presence of organochlorine (OC) pesticides in human samples may be explained by the environmental exposure of the population. Foods are considered a constant source of exposure, despite compliance with maximum permitted residue levels. This study aimed to examine the relationship between nutritional habits of women in Southeast Spain and their serum concentrations of OCs. A semi-quantitative questionnaire was used to estimate the frequency of consumption of foods by two age groups of women, pre-menopausal (Pre-M) and post-menopausal (Post-M), and their serum pesticide levels were measured by gas chromatography (GC) with electron capture detector and confirmed by GC and mass spectrometry. The Pre-M group showed significantly higher serum concentrations of all OCs studied with the exception of DDE. The groups significantly differed in consumption of all food groups with the exception of fruit. In the Pre-M group, the mean serum p,p-DDT concentration was significantly associated with milk/yoghurt (p<0.045) and red meat (p<0.023), serum o,p-DDT with red meat (p<0.049), serum aldrin with eggs (p<0.038) and poultry (p<0.024), and serum DDE with eggs (p<0.025). In the Post-M group, serum lindane was associated with fresh and cured cheese (p<0.001), red meat (p<0.001) and white and oily fish (p<0.001), and both serum DDE and dieldrin were associated with fresh cheese, cured cheese, red meat, and white and oily fish (p<0.001). These results confirm foods as a source of human exposure to persistent organic molecules. Consideration should be given to the reduction of permitted residue levels to minimize this threat to human and animal health. PMID:17477954

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

    PubMed

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

    2016-01-15

    Extreme and uncontrolled usage of pesticides produces a number of problems for vegetation and human health. In this study, the existence of organophosphates (OPs), organochlorines (OCs), pyrethroids (PYs) and fungicides (FUs) were investigated in persimmons/jujubes and their planted soils, which were collected from China. One OP (dimethoate), three OCs (DDT, quintozene and aldrin), six PYs (bifenthrin, fenpropathrin, cyhalothrin, cypermethrin, fenvalerate and deltamethrin) and two FUs (triadimefon and buprofezin) were found in 36.4% of persimmons and 70.8% of jujubes, with concentrations from 1.0 μg/kg to 2945.0 μg/kg. The most frequently detected pesticides in the two fruits were fenpropathrin in persimmons and cypermethrin in jujubes, with the detection frequencies of 30.0% and 22.7%, respectively. The residues of 4.5% (persimmon) and 25.0% (jujube) of samples were higher than the maximum residue limits (MRLs) of China. Compared with the fruits, more types of pesticides and higher residues were observed in their planted soils. The most frequently detected pesticides were HCH in persimmon soil and DDT in jujube soil, with the detection frequencies of 10.9% and 12.7%, respectively. For the tested samples, 39.1% of fruit samples and 63.0% of soil samples with multiple residues (containing more than two pesticides) were noted, even up to 8 residues in fruits and 14 residues in soils. Except for cyhalothrin, the other short-term risks for the tested pesticides in the fruits were below 10%, and the highest long-term risk was 14.13% for aldrin and dieldrin. There was no significant health risk for consumers via consumption of the two fruits. PMID:26544891

  4. Pesticide/Food Risk Greatest under Age Six.

    ERIC Educational Resources Information Center

    Raloff, J.

    1989-01-01

    Summarizes the Natural Resources Defense Council's report that cancer risks from pesticides are higher than Environmental Protection Agency's (EPA) criteria for children. Describes some responses of the EPA on the report. (YP)

  5. Comprehensive multi-residue method for the target analysis of pesticides in crops using liquid chromatography-tandem mass spectrometry.

    PubMed

    Hiemstra, Maurice; de Kok, André

    2007-06-22

    A liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS) multi-residue method for the simultaneous target analysis of a wide range of pesticides and metabolites in fruit, vegetables and cereals has been developed. Gradient elution has been used in conjunction with positive mode electrospray ionization tandem mass spectrometry to detect up to 171 pesticides and/or metabolites in different crop matrices using a single chromatographic run. Pesticide residues were extracted/partitioned from the samples with acetone/dichloromethane/light petroleum. The analytical performance was demonstrated by the analysis of extracts from lettuce, orange, apple, cabbage, grape and wheat flour, spiked at three concentration levels ranging from 0.01 to 0.10 mg/kg for each pesticide and/or metabolite. In general, recoveries ranging from 70 to 110%, with relative standard deviations better than 15%, were obtained. The recovery and repeatability data are in good accordance with EU guidelines for pesticide residue analysis. The limit of quantification for all targeted pesticides and metabolites tested was 0.01 mg/kg. The selectivity and robustness of the LC-MS/MS method was demonstrated by a 1-year comparison of its analytical results with those obtained from our validated GC and LC multi-residue methods applied to more than 3500 routine samples. The validated LC-MS/MS method has been implemented in our analytical scheme since 2004, replacing four of the conventional detection methods, i.e. GC-flame-photometric detection (acephate, methamidophos, etc.), GC-nitrogen-phosphorus detection, LC-UV detection (carbendazim, thiabendazole, imazalil and prochloraz) and LC-fluorescence detection (N-methylcarbamate pesticides). During a 3-year period, the LC-MS/MS method has been applied to the analyses of more than 12,000 samples. PMID:17442324

  6. 75 FR 60452 - Notice of Filing of Several Pesticide Petitions for Residues of Pesticide Chemicals in or on...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-09-30

    ... identification (ID) number and the pesticide petition number (PP) of interest as shown in the body of this... pesticide petition number of interest as shown in the body of this document. EPA's policy is that all... not know your identity or contact information unless you provide it in the body of your comment....

  7. 75 FR 28009 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-05-19

    ... the use of special characters, any form of encryption, and be free of any defects or viruses. Docket..., papaya, star apple, black sapote, mango, sapodilla, canistel, and mamey sapote at 0.20 ppm; and tea at 15...) under 40 CFR 180.920 when used as a pesticide inert ingredient in pesticide formulations. A...

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

    PubMed

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

    2013-01-01

    A rapid multi-residue method for determination of pesticide residues in processed foods manufactured from agricultural products was examined. Five mL water was added to 5 g sample in a polypropylene tube, and the tube was left to stand at room temperature for 30 min. Then, 20 mL acetonitrile was added to the sample. The mixture was homogenized in a high-speed homogenizer, followed by salting out with 1 g NaCl and 4 g anhydrous MgSO4. After centrifugation, the organic layer was purified on a graphitized carbon/PSA cartridge column. After removal of the solvent, the extract was resolved in methanol-water and analyzed with LC-MS/MS. The recoveries of 93 pesticides fortified into 5 kinds of processed foods [Chinese cabbage kimchi, marmalade, raisin, umeboshi (pickled plum) and worcester sauce] were examined at the concentrations of 0.02 and 0.1 μg/g (n=5). The recoveries of 61 pesticides in all foods were 70-120% with relative standard deviation below 20% at both concentrations. Seventy-four processed foods obtained from markets in Japan were examined with this method. Pesticide residues over the maximum residue limit (0.01 μg/g) were detected in 2 processed foods. PMID:24389475

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

    PubMed

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

    2013-05-01

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

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

    PubMed

    Zhao, Chunjie; Bai, Lu; Ou, Yingfu; Li, Dan; Xin, Chunhong

    2009-01-01

    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. PMID:19930806

  11. Monitoring multi-class pesticide residues in fresh fruits and vegetables by liquid chromatography with tandem mass spectrometry.

    PubMed

    Frenich, A Garrido; Vidal, J L Martínez; López, T López; Aguado, S Cortés; Salvador, I Martínez

    2004-09-10

    A new analytical method was developed using liquid chromatography with tandem mass spectrometry for the routine analysis of 31 multi-class pesticide residues and applied to approximately 50 fresh fruit and vegetable samples (green bean, cucumber, pepper, tomato, eggplant, watermelon, melon and zucchini). Extraction of the pesticides with ethyl acetate was carried out. The optimal ionisation conditions were selected for each pesticide in the same run. The procedure was validated and the values of some merit figures, such as recovery, precision, linear range, detection limit and quantification limit for each pesticide were calculated together with its calculated expanded uncertainty (U). The average recoveries in cucumber obtained for each pesticide ranged between 74 and 105% at two different fortification levels (n = 10 each) that ranged between 9 and 250 ng g(-1) (depending on the pesticide). The uncertainty associated to the analytical method was lower than 23% for all compounds tested. The calculated limits of detection and quantitation were typically <1 ng g(-1) that were much lower than the maximum residue levels established by European legislation. PMID:15481257

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

    PubMed

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

    2016-02-01

    The present study was undertaken to monitor organochlorine, organophosphate, and synthetic pyrethroid pesticide residues in butter (n = 55) and ghee (n = 56) samples collected from three different regions of Punjab. The estimation of pesticide residues was done by multiple residue analytical technique using gas chromatography equipped with GC-ECD and GC-FTD. The confirmation of residues was done on gas chromatography mass spectrometry in both selective ion monitoring (SIM) and scan mode. Results indicated the presence of hexacholorocyclohexane (HCH) and p,p' DDE as predominant contaminant in both butter and ghee. Residues of HCH were detected in 25 and 23% samples of butter and ghee, respectively, while residues of p,p' DDE were recorded in 29 and 25% of butter and ghee samples, respectively. None of the butter and ghee sample violated the MRL values of 200 ng g(-1) for HCH and 1250 ng g(-1) for dichorodiphenyl tricholorethane (DDT). The presence of endosulfan, cypermethrin, fenvalerate, deltamethrin, and chlorpyrifos were observed in a few butter and ghee samples at traces. The spatial variation for comparative occurrence of pesticide residues indicated higher levels in the south-western region of Punjab. Additionally, the temporal variation indicated the significant reduction of HCH and DDT levels in butter and ghee in Punjab. PMID:26781716

  13. Pesticide residue analysis and its relationship to hazard characterisation (ADI/ARfD) and intake estimations (NEDI/NESTI).

    PubMed

    Renwick, Andrew G

    2002-10-01

    Over 800 pesticides are currently approved for use in one or more EU countries. The maximum residue levels (MRL) for agricultural pesticides are derived from field trials conducted under good agricultural practice (GAP). The MRL is a legally enforceable limit related to GAP. The results from field trials would only be used to establish MRLs if the estimated intake of residues did not exceed the acceptable daily intake (ADI) or acute reference dose (ARfD). However, the MRL is not linked to the ADI or ARfD, and could result in intakes considerably below the ADI/ARfD. This disconnection between hazard characterisation (ADI/ARfD) and potential exposure assessment (MRL) means that risk characterisation of pesticide residues is less transparent than for other chemicals present in human food. Residue levels at or below the MRL would not give intakes that exceed the ADI/ARfD but, despite this, there is public concern over such residues. Residue levels above the MRL have to be analysed on a case-by-case basis to determine if the intake could exceed the health-based limits. Other causes of public concern, such as the presence of multiple residues, are currently under investigation. PMID:12400449

  14. Qualitative and quantitative analysis of organophosphorus pesticide residues using temperature modulated SnO(2) gas sensor.

    PubMed

    Huang, Xingjiu; Liu, Jinhuai; Pi, Zongxin; Yu, Zengliang

    2004-10-01

    Qualitative and quantitative analysis of organophosphorus pesticide residues (acephate and trichlorphon) using temperature modulated SnO(2) gas sensor were studied. The testing method employed only a single SnO(2)-based gas sensor in a rectangular temperature mode to perform the qualitative analysis of pure pesticide vapor and a binary vapor mixture in the air. Experimental results showed that in the range 250-300 degrees C and at the modulating frequency of 20mHz the high selectivity of the sensor could be achieved. The quantitative analysis of the pure pesticide vapor and their mixture were performed by fast Fourier transformation (FFT). The higher harmonics of the FFT characterized the non-linear properties of the response at the sensor surface. The amplitudes of the higher harmonics exhibited characteristic variations that depend on the concentration and the kinetics of pesticide species on the sensor surface. PMID:18969637

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

    PubMed

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

    2016-01-01

    A validation study was carried out on a rapid method for the simultaneous determination of pesticide residues in vegetables and fruits by LC-MS/MS. Preparation of the test solution was performed by a solid-phase extraction technique with QuEChERS (STQ method). Pesticide residues were extracted with acetonitrile using a homogenizer, followed by salting-out and dehydration at the same time. The acetonitrile layer was purified with C18 and PSA mini-columns. The method was assessed for 130 pesticide residues in 14 kinds of vegetables and fruits at the concentration level of 0.01 μg/g according to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan. As a result 75 to 120 pesticide residues were determined satisfactorily in the tested samples. Thus, this method could be useful for a rapid and simultaneous determination of multi-class pesticide residues in various vegetables and fruits. PMID:27558229

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

    PubMed

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

    2012-08-01

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

  17. Residues of organochlorine pesticides, polychlorinated biphenyls, and mercury in bald eagle eggs and changes in shell thickness--1969 and 1970

    USGS Publications Warehouse

    Wiemeyer, Stanley N.; Mulhern, B.M.; Ligas, F.J.; Hensel, R.J.; Mathisen, J.E.; Robards, F.C.; Postupalsky, S.

    1972-01-01

    Twenty-three bald eagle eggs collected in Alaska, Maine, Michigan, Minnesota, and Florida during 1969 and 1970 were analyzed for organochlorine pesticides, polychlorinated biphenyls, and mercury. All eggs contained residues of DDE, dieldrin, PCB's, and mercury. Average residue concentrations were lowest in eggs from Alaska. Significant eggshell thinning has occurred among eggs from most major areas sampled. Some eggs contained DDE residues of the same magnitude as those that produced shell thinning in experimental species. High dieldrin residues in some eggs could be having an adverse effect on reproductive success.

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

    NASA Astrophysics Data System (ADS)

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

    2011-12-01

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

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

    PubMed

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

    2014-11-01

    Flow injection combined with tandem mass spectrometry (MS/MS) was investigated for the rapid detection of highly polar pesticides that are not amenable to multi-residue methods because they do not partition into organic solvents and require dedicated chromatographic conditions. The pesticides included in this study were amitrole, chlormequat, cyromazine, daminozide, diquat, ethephon, fosetyl-Al, glufosinate, glyphosate and its metabolite aminomethylphosphonic acid, maleic hydrazide, mepiquat and paraquat. The composition of the flow-injection solvent was optimized to achieve maximum MS/MS sensitivity. Instrumental limits of detection varied between <0.05 and 1 pg. Fruit, vegetable, cereal, milk and kidney samples were extracted with water (1% formic acid in case of paraquat/diquat) and ten times diluted in either methanol/0.1% formic acid, methanol/0.1% ammonia or acetonitrile/0.1% ammonia, depending on the pesticide. The ion suppression observed depended strongly on both the matrix and the pesticide. This could be largely compensated for by matrix-matched calibration, but more accurate quantification was obtained by using isotopically labelled standards (commercially available for most of the pesticides studied). The method detection limits ranged from 0.02 mg/kg for chlormequat and mepiquat to 2 mg/kg for maleic hydrazide and were 0.05-0.2 mg/kg for most other pesticide/matrix combinations. This was sufficiently low to test compliance with EU maximum residue limits for many relevant pesticide/commodity combinations. The method substantially reduces the liquid chromatography-MS/MS capacity demand which for many laboratories is prohibitive for inclusion of these pesticides in their monitoring and surveillance programmes. PMID:24518902

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

    PubMed

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

    2014-08-01

    A method for residual determination of 5 pyrethroid pesticides in Anoectochilus roxburghii by cloud point extraction-back extraction-GC-MS was established. PEG 6000 was used as extraction agent and isooctane was used for back-extractant. The con- tent was calculated by external standard method. The linear range was from 15 to 2 000 μg x kg(-1) with the good correlation coefficients (0.955-0.999). The recoveries at spiked concentrations of 50-500 μg x kg(-1) ranged from 85.12% to 101.6%. The limit of detection and quantification of 5 pyrethroid pesticides were in the range of 0.63-3.10 μg x kg(-1) and 2.10-10.31 μg x kg(-1), respectively. The proposed method can be applied to the determination of pyrethroid pesticides residues in A. roxburghii. PMID:25507544

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

    PubMed

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

    2014-08-01

    A method for residual determination of 5 pyrethroid pesticides in Anoectochilus roxburghii by cloud point extraction-back extraction-GC-MS was established. PEG 6000 was used as extraction agent and isooctane was used for back-extractant. The con- tent was calculated by external standard method. The linear range was from 15 to 2 000 μg x kg(-1) with the good correlation coefficients (0.955-0.999). The recoveries at spiked concentrations of 50-500 μg x kg(-1) ranged from 85.12% to 101.6%. The limit of detection and quantification of 5 pyrethroid pesticides were in the range of 0.63-3.10 μg x kg(-1) and 2.10-10.31 μg x kg(-1), respectively. The proposed method can be applied to the determination of pyrethroid pesticides residues in A. roxburghii. PMID:25423822

  2. Determination of neonicotinoid pesticide residues in vegetables and fruits with solid phase extraction and liquid chromatography mass spectrometry.

    PubMed

    Obana, Hirotaka; Okihashi, Masahiro; Akutsu, Kazuhiko; Kitagawa, Yoko; Hori, Shinjiro

    2003-04-23

    A rapid and simple extraction method for the simultaneous analysis of five neonicotinoid insecticides has been developed. Twelve different fruit and vegetable matrixes were extracted with methanol and cleaned up using a graphitized carbon solid phase extraction cartridge loading with a 20% methanol solution. The concentrated eluate after methanol elution was then analyzed for pesticide residues by liquid chromatography/mass spectrometry in the APCI positive mode. The five pesticides including nitenpyram, thiamethoxam, imidacloprid, acetamiprid, and thiacloprid were recovered at 70-95% at spike levels of 0.1 and 1 mg/kg in bell pepper, cucumber, eggplant, grape, grapefruit, Japanese radish, peach, pear, potato, rice, and tomato. Relative standard deviations were less than 10% for all of the recovery tests. The proposed method is fast, easy to perform, and could be utilized for regular monitoring of pesticide residues. PMID:12696927

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

    NASA Astrophysics Data System (ADS)

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

    2015-09-01

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

  4. Application of the precolumn back-flush technology in pesticide residue analysis: a practical view.

    PubMed

    Hildmann, Fanny; Kempe, Günther; Speer, Karl

    2013-07-01

    Precolumn back-flushing is a matrix minimization technique in GC in which the carrier gas flow of the precolumn is reversed after the transfer of the highest boiling analyte to the analytical column. Practical details concerning this technology have rarely been published although it is widely used. This paper now focuses on the practical implementation of precolumn back-flushing for pesticide residue analysis of complex food matrices. Fitting the analytical column into the precolumn was found to be essential for comparable analyte responses with and without back-flushing. The effectiveness of the reverse column flow technique is mainly affected by the transfer time after which back-flushing starts. The transfer time was found to depend on which kind of injected matrix is used and the state of the precolumn. For the regular adaptation of the transfer time in routine analysis, a simple test was introduced in which 13-C-labeled deltamethrin and indeno[1,2,3-c,d]pyrene were added to the prepared extract. Chromatograms, LOQ and RSD of up to 99 pesticides in citrus oil and liver extracts proved a clearer identification and enhanced quantification using precolumn back-flushing compared to measurements without this technology. Furthermore, reduced system maintenance could be achieved through back-flushing. PMID:23606674

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

    PubMed

    Raina-Fulton, Renata

    2015-01-01

    Pesticide residue methods have been developed for a wide variety of food products including cereal-based foods, nutraceuticals and related plant products, and baby foods. These cereal, fruit, vegetable, and plant-based products provide the basis for many processed consumer products. For cereal and nutraceuticals, which are dry sample products, a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method has been used with additional steps to allow wetting of the dry sample matrix and subsequent cleanup using dispersive or cartridge format SPE to reduce matrix effects. More processed foods may have lower pesticide concentrations but higher co-extracts that can lead to signal suppression or enhancement with MS detection. For complex matrixes, GC/MS/MS or LC/electrospray ionization (positive or negative ion)-MS/MS is more frequently used. The extraction and cleanup methods vary with different sample types particularly for cereal-based products, and these different approaches are discussed in this review. General instrument considerations are also discussed. PMID:26525234

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

    PubMed

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

    2014-07-01

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

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

    SciTech Connect

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

    2015-09-25

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

  8. In Utero Pesticide Exposure and Leukemia in Brazilian Children < 2 Years of Age

    PubMed Central

    Ferreira, Jeniffer Dantas; Couto, Arnaldo Cézar; Pombo-de-Oliveira, Maria S.

    2012-01-01

    Background: An association between pesticide exposure and cancer has been suggested. Infant leukemia is a rare neoplasm and its association with maternal pesticide exposure has been poorly explored. Objectives: We investigated the association between pesticide exposure during pregnancy and leukemia in children < 2 years of age. Methods: A hospital-based case–control study was carried out in 13 Brazilian states during 1999–2007. Mothers of 252 cases and those of 423 controls were interviewed. Information on pesticide exposures 3 months before pregnancy, throughout pregnancy, and during breastfeeding was obtained. Unconditional logistic regression was used to estimate adjusted odds ratios (aORs) for associations between pesticide exposures and leukemia. Results: Associations with ever use of pesticides during pregnancy were observed for acute lymphoid leukemia (ALL) (aOR = 2.10; 95% CI: 1.14, 3.86) and acute myeloid leukemia (AML) (aOR = 5.01; 95% CI: 1.97, 12.7) in children 0–11 months of age, and with ALL (aOR = 1.88; 95% CI: 1.05, 5.23) at 12–23 months of age. According to reported maternal exposure to permethrin, higher risk estimates were verified for children 0–11 months of age (aOR = 2.47; 95% CI: 1.17, 5.25 for ALL; and aOR = 7.28; 95% CI: 2.60, 20.38 for AML). Maternal pesticide exposure related to agricultural activities showed an aOR of 5.25 (95% CI: 1.83, 15.08) for ALL, and an aOR of 7.56 (95% CI: 1.83, 31.23) for AML. Conclusions: These results support the hypothesis that pesticide exposure during pregnancy may be involved in the etiology of acute leukemia in children < 2 years of age. PMID:23092909

  9. Quantitative Identification of Biogenic Nonextractable Pesticide Residues in Soil by (14)C-Analysis.

    PubMed

    Poßberg, Claudia; Schmidt, Burkhard; Nowak, Karolina; Telscher, Markus; Lagojda, Andreas; Schaeffer, Andreas

    2016-06-21

    Quantification of nonextractable residues (NER) of pesticides in soil is feasible by use of radioactively labeled compounds, but structural information on these long-term stabilized residues is usually lacking. Microorganisms incorporate parts of the radiolabeled ((14)C-) carbon from contaminants into microbial biomass, which after cell death enters soil organic matter, thus forming biogenic nonextractable residues (bioNER). The formation of bioNER is not yet determinable in environmental fate studies due to a lack of methodology. This paper focuses on the development of a feasible analytical method to quantify proteinaceous carbon, since proteins make up the largest mass portion of bacterial cells. The test substance (14)C-bromoxynil after 56 days forms more than 70% of NER in soil. For further characterization of NER the amino acids were extracted, purified, and separated by two-dimensional thin-layer chromatography (TLC). Visualization of the (14)C-amino acids was performed by bioimaging, unambiguous identification by GC-MS and LC-MS/MS. Our analysis revealed that after 56 days of incubation about 14.5% of the (14)C-label of bromoxynil was incorporated in amino acids. Extrapolating this content based on the amount of proteins in the biomass (55%), in total about 26% of the NER is accounted for by bioNER and thus is not environmentally relevant. PMID:27192605

  10. [Cumulative risk assessment for consumers of agricultural crops polluted with one chemical class pesticide residues (case of triazole fungicides)].

    PubMed

    Koval'chuk, N M; Omel'chuk, S T

    2011-01-01

    Different indices of cumulative risk assessment of combination of residues of pesticides which may simultaneously be present in raw agricultural crops, based on toxic evaluation of such combination have been presented. Risk for population health due to consumption of raw agricultural crops with triazole residues is acceptable on hazard index, point of departure index and cumulative risk index, exceeds allowable level on criterion "total margin of exposure". PMID:22768736

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

    PubMed

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

    2015-11-01

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

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

  13. Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables

    Technology Transfer Automated Retrieval System (TEKTRAN)

    This article describes the comparison of different versions of an easy, rapid, and low-cost sample preparation approach for the determination of pesticide residues in fruits and vegetables by concurrent use of gas and liquid chromatography (GC and LC) coupled to mass spectrometry (MS) for detection....

  14. Extension of the QuEChERS Method for Pesticide Residues in Cereals to Flaxseeds, Peanuts, and Doughs

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A simple method was evaluated for the determination of pesticide residues in flaxseeds, doughs, and peanuts using gas chromatography-time-of-flight mass spectrometry (GC-TOF) for analysis. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, which was previously optimized f...

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

    PubMed

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

    2008-07-01

    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

  16. Residues in food and feed topic area at the 13th IUPAC International Congress of pesticide chemistry

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The organizers of two symposia in the “Residues in Food and Feed” topic area held at the 13th IUPAC International Congress of Pesticide Chemistry introduce the papers that were contributed to this special section in the Journal. The symposia were titled “Taking Advantage of Advanced Analytical Tool...

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  18. Relationship of (known) control values to (unknown) test values in proficiency studies of pesticide residues.

    PubMed

    Horwitz, W; Wood, R

    2000-01-01

    Proficiency studies have been suggested as an alternative source of information for evaluating method performance characteristics when results from interlaboratory method performance studies conforming to internationally recognized protocols are not available. To explore this possibility, results were examined from ongoing proficiency studies of pesticide residue analyses in celery, carrot, and grape purees, and in wine. Statistical performance parameters were calculated from 18 data sets analyzed as unknowns by about 60 analysts for 12 analytes in the 25-1,000 microg/kg range, and from presumably parallel control (spike) analyses conducted by about half of the participants. A surprising finding was that recovery of known, independent control additions by the participant did not correlate with the recoveries determined as unknowns in the exercise. The data suggest that censoring or truncating of control data has occurred. The question of substitution of proficiency data for method performance data cannot be answered until the problem of unbiased reporting of control data is resolved. PMID:10772178

  19. 78 FR 1798 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-01-09

    ... (NAICS code 111). Animal production (NAICS code 112). Food manufacturing (NAICS code 311). Pesticide manufacturing (NAICS code 32532). B. What should I consider as I prepare my comments for EPA? 1. Submitting...

  20. 77 FR 63782 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on a Commodity

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-10-17

    ... code 111). Animal production (NAICS code 112). Food manufacturing (NAICS code 311). Pesticide manufacturing (NAICS code 32532). B. What should I consider as I prepare my comments for EPA? 1. Submitting...

  1. 76 FR 69692 - Withdrawal of a Pesticide Petition for Residues of Pesticide Chemicals in or on Various Commodities

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-11-09

    ... 23, 2010 (75 FR 57942) (FRL-8845-4), which announced the submission of a pesticide petition (PP... formulations of the active ingredients potassium iodide and potassium thiocyanate. On September 9, 2011,...

  2. [Toxicological evaluation of pesticide and chemical residues in control of biological processes in vegetables under glass and plastics].

    PubMed

    Goedicke, H J

    1988-01-01

    The cultivation of vegetables under glass and plastics is one of the most intensive application fields of pesticides and chemicals for regulation of biological processes. Therefore it may potentially occur a relatively high residues contamination of the crops. The author reveals in a survey the residue situation of usual insecticides, acaricides, fungicides, and chemicals for regulation of biological processes on tomatoes, cucumbers, and lettuce in comparison with the maximum residue limit after cold fogging application. The residues of benomyl, carbendazim, and ethylen-bis-dithiocarbamate are detailed discussed in the light of the latest toxicological findings. The results the residues of 11 agents on the crops show that after the corresponding preharvest interval the residues constitute 1.7-78% of the maximum residue limit. The conclusion is drawn that the cold fogging application of the agents under glass and plastics does not result in food hygienic toxicological problems. PMID:3068546

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

    PubMed

    Liu, Nan; Gao, Zhixian; Ma, Hongwei; Su, Pu; Ma, Xinhua; Li, Xiaoli; Ou, Guorong

    2013-03-15

    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-β-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-β-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. PMID:23084755

  4. Pesticides

    MedlinePlus

    ... Heindel JJ, Zoeller RT. Endocrine-disrupting chemicals and human disease. In: Jameson JL, ed. Endocrinology: Adult and Pediatric . 7th ed. Philadelphia, PA: Elsevier Saunders; 2015:chap 153. Karr CJ, Solomon GM, Brock-Utne AC. Health effects of common home, lawn, and garden pesticides. Pediatr ...

  5. Paraoxonase 1 Polymorphism and Prenatal Pesticide Exposure Associated with Adverse Cardiovascular Risk Profiles at School Age

    PubMed Central

    Andersen, Helle R.; Wohlfahrt-Veje, Christine; Dalgård, Christine; Christiansen, Lene; Main, Katharina M.; Nellemann, Christine; Murata, Katsuyuki; Jensen, Tina K.; Skakkebæk, Niels E.; Grandjean, Philippe

    2012-01-01

    Background Prenatal environmental factors might influence the risk of developing cardiovascular disease later in life. The HDL-associated enzyme paraoxonase 1 (PON1) has anti-oxidative functions that may protect against atherosclerosis. It also hydrolyzes many substrates, including organophosphate pesticides. A common polymorphism, PON1 Q192R, affects both properties, but a potential interaction between PON1 genotype and pesticide exposure on cardiovascular risk factors has not been investigated. We explored if the PON1 Q192R genotype affects cardiovascular risk factors in school-age children prenatally exposed to pesticides. Methods Pregnant greenhouse-workers were categorized as high, medium, or not exposed to pesticides. Their children underwent a standardized examination at age 6-to-11 years, where blood pressure, skin folds, and other anthropometric parameters were measured. PON1-genotype was determined for 141 children (88 pesticide exposed and 53 unexposed). Serum was analyzed for insulin-like growth factor I (IGF-I), insulin-like growth factor binding protein 3 (IGFBP3), insulin and leptin. Body fat percentage was calculated from skin fold thicknesses. BMI results were converted to age and sex specific Z-scores. Results Prenatally pesticide exposed children carrying the PON1 192R-allele had higher abdominal circumference, body fat content, BMI Z-scores, blood pressure, and serum concentrations of leptin and IGF-I at school age than unexposed children. The effects were related to the prenatal exposure level. For children with the PON1 192QQ genotype, none of the variables was affected by prenatal pesticide exposure. Conclusion Our results indicate a gene-environment interaction between prenatal pesticide exposure and the PON1 gene. Only exposed children with the R-allele developed adverse cardiovascular risk profiles thought to be associated with the R-allele. PMID:22615820

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

    PubMed

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

    2012-03-01

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

  7. SORPTION OF AGED DICAMBA RESIDUES IN SOIL

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The effect of aging on dicamba (3,6-dichloro-2-methoxybenzoic acid) and a major metabolite, 3,6-dichlorosalicylic acid (3,6-DCSA) on sorption was determined in an unamended and a carbon-amended sandy loam soil. During the incubation, sequential solvent extraction with 0.01 N CaCl2 and aqueous aceto...

  8. Extension of the QuEChERS method for pesticide residues in cereals to flaxseeds, peanuts, and doughs.

    PubMed

    Koesukwiwat, Urairat; Lehotay, Steven J; Mastovska, Katerina; Dorweiler, Kelly J; Leepipatpiboon, Natchanun

    2010-05-26

    A simple method was evaluated for the determination of pesticide residues in flaxseeds, doughs, and peanuts using gas chromatography-time-of-flight mass spectrometry (GC-TOF) for analysis. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, which was previously optimized for cereal grain samples, was evaluated in these fatty matrices. This extraction method involves first mixing the sample with 1:1 water/acetonitrile for an hour to swell the matrix and permit the salt-out liquid-liquid partitioning step using anhydrous MgSO(4) and NaCl. After shaking and centrifugation, cleanup is done by dispersive solid-phase extraction (d-SPE) using 150 mg of anhydrous MgSO(4), 150 mg of PSA, and 50 mg of C-18 per milliliter of extract. This method gave efficient separation of pesticides from fat and removal of coextracted substances better than gel permeation chromatography or use of a freeze-out step, which involved excessive use of solvent and/or time. The optimized analytical conditions were evaluated in terms of recoveries, reproducibilities, limits of detection, and matrix effects for 34 representative pesticides using different types of flaxseeds, peanuts, and doughs. Use of matrix-matched standards provided acceptable results for most pesticides with overall average recoveries between 70 and 120% and consistent RSDs <20% for semipolar pesticides and <26% for lipophilic pesticides. The recoveries of these latter types of pesticides depended on the fat content in the matrices and partitioning factor between the lipids and acetonitrile. We believe that the consistency of the pesticide recoveries for different samples in multiple experiments and the physicochemical partitioning explanation for <70% recoveries of lipophilic pesticides justify compensation of results for the empirically determined recovery values. In any case, this method still meets 10 ng/g detection limit needs for lipophilic pesticides and may be used for qualitative screening

  9. Water aging reverses residual stresses in hydrophilic dental composites.

    PubMed

    Park, J W; Ferracane, J L

    2014-02-01

    Dental composites develop residual stresses during polymerization due to shrinkage. These stresses may change with time because of relaxation and water sorption in the oral environment. This phenomenon is likely dependent on the composition of the materials, specifically their hydrophilic characteristics, and could result in deleterious stresses on restorative materials and tooth structure. The purpose of this experiment was to use the thin ring-slitting method to compare the residual stress generated within composite materials of varying hydrophilicity when aged in wet and dry conditions after polymerization. Water sorption, solubility, elastic modulus, and residual stresses were measured in 6 commercial composites/cements aged in water and dry conditions. The self-adhesive resin cement showed the highest water sorption and solubility. All composites showed initial residual contraction stresses, which were maintained when aged dry. Residual stresses in 2 of the self-adhesive cements and the polyacid-modified composite aged in wet conditions resulted in a net expansion. This experiment verified that residual shrinkage stresses in dental composites can be reversed during aging in water, resulting in a net expansion, with the effect directly related to their hydrophilic properties. PMID:24272790

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

    PubMed

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

    2015-01-01

    The objective of this study was to determine the levels of pesticides in the fish Prochilodus costatus caught in São Francisco River, one of most important rivers in Brazil. Thirty-six fish were captured in three different areas, and samples of the dorsal muscle and pooled viscera were collected for toxicological analysis. We evaluated the presence of 150 different classes of insecticides, fungicides, herbicides and acaricides by multiresidue analysis technique using liquid chromatography-tandem mass spectrometry (LC-MS/MS), with the limit of detection of 5 ppb. In this study, organophosphorus and carbamate pesticides were detected at the highest levels in the caught fish. Among the 41 organophosphorus pesticides surveyed, nine types were detected (chlorpyrifos, diazinon, dichlorvos, disulfoton, ethion, etrimfos, phosalone, phosmet and pyrazophos) in the muscle, viscera pool, or both in 22 (61.1%) fish. Sampled tissues of 20 (55.6%) fish exhibited at least one of the eight evaluated carbamate pesticides and their metabolites: aldicarb, aldicarb sulfoxide, carbaryl, carbofuran, carbosulfan, furathiocarb, methomyl and propoxur. Fungicides (carbendazim, benalaxyl, kresoxim-methyl, trifloxystrobin, pyraclostrobin and its metabolite BF 500 pyraclostrobin), herbicides (pyridate and fluasifop p-butyl), acaricide (propargite) and pyrethroid (flumethrin) were also detected. In conclusion, P. costatus fish caught in the São Francisco River contained residues of 17 different pesticides, in both muscles and the viscera pool, indicating heavy environmental contamination by pesticides in the study area. PMID:25844860

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

    PubMed

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

    2014-01-01

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

  12. Development of a new cucumber reference material for pesticide residue analysis: feasibility study for material processing, homogeneity and stability assessment.

    PubMed

    Grimalt, Susana; Harbeck, Stefan; Shegunova, Penka; Seghers, John; Sejerøe-Olsen, Berit; Emteborg, Håkan; Dabrio, Marta

    2015-04-01

    The feasibility of the production of a reference material for pesticide residue analysis in a cucumber matrix was investigated. Cucumber was spiked at 0.075 mg/kg with each of the 15 selected pesticides (acetamiprid, azoxystrobin, carbendazim, chlorpyrifos, cypermethrin, diazinon, (α + β)-endosulfan, fenitrothion, imazalil, imidacloprid, iprodione, malathion, methomyl, tebuconazole and thiabendazole) respectively. Three different strategies were considered for processing the material, based on the physicochemical properties of the vegetable and the target pesticides. As a result, a frozen spiked slurry of fresh cucumber, a spiked freeze-dried cucumber powder and a freeze-dried cucumber powder spiked by spraying the powder were studied. The effects of processing and aspects related to the reconstitution of the material were evaluated by monitoring the pesticide levels in the three materials. Two separate analytical methods based on LC-MS/MS and GC-MS/MS were developed and validated in-house. The spiked freeze-dried cucumber powder was selected as the most feasible material and more exhaustive studies on homogeneity and stability of the pesticide residues in the matrix were carried out. The results suggested that the between-unit homogeneity was satisfactory with a sample intake of dried material as low as 0.1 g. A 9-week isochronous stability study was undertaken at -20 °C, 4 °C and 18 °C, with -70 °C designated as the reference temperature. The pesticides tested exhibited adequate stability at -20 °C during the 9-week period as well as at -70 °C for a period of 18 months. These results constitute a good basis for the development of a new candidate reference material for selected pesticides in a cucumber matrix. PMID:25627789

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

    PubMed

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

    2012-09-15

    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

  14. Lead, cadmium and organochlorine pesticide residues in hunted red deer and wild boar from northern Italy.

    PubMed

    Chiari, Mario; Cortinovis, Cristina; Bertoletti, Marco; Alborali, Loris; Zanoni, Mariagrazia; Ferretti, Enrica; Caloni, Francesca

    2015-01-01

    The objectives of the present study were to assess heavy metal cadmium (Cd), lead (Pb) and organochlorine pesticide concentrations in tissues of red deer (Cervus elaphus) and wild boar (Sus scrofa) from nine hunting areas and to evaluate related risk factors for the host animal. Over a period of 2 years, a total of 1055 and 210 masseters, 424 and 201 livers, 642 and 152 kidneys were collected from wild boar and red deer, respectively, and concentrations of Cd, Pb and organochlorine pesticides were determined. Comparing the two species, Cd concentration in the kidney (3.72 mg/kg), liver (0.67 mg/kg) and muscle (0.02 mg/kg) of wild boar was found to be significantly higher than in the organs of red deer (1.02 mg/kg in the kidneys, 0.07 mg/kg in the liver and 0.006 mg/kg in muscle). Mean Pb concentrations were found to be similar in both animals, with 0.39, 0.52 and 2.60 mg/kg detected in the wild boar kidney, liver and muscle, respectively, and 0.24, 0.21 and 2.04 mg/kg in the respective organs of the red deer. No difference in concentrations were found based on age class, location of tissue sample or contaminant in the case of wild boar. By contrast, a significantly lower Cd concentration was found in the kidney of the young red deer. The search for organochlorine pesticides in both red deer and wild boar produced negative results with values below the limits of detection. Due to the high levels of renal Cd and muscle Pb detected in wild boar and red deer, further research needs to be carried out in an effort to identify the source of contamination and preserve the health of animals and humans. PMID:26365428

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

    PubMed

    Blasco, Cristina; Picó, Yolanda; Andreu, Vicente

    2009-05-01

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

  16. [Determination of endosulfan pesticide residues in Litopenaeus vannamai by capillary gas chromatography].

    PubMed

    Liu, Xiaosong; Huang, Daxin; Lu, Shengyu

    2007-05-01

    A method is described for the determination of endosulfan pesticide residues in Litopenaeus vannamai by capillary gas chromatography. The residues of alpha-endosulfan and beta-endosulfan were extracted from the sample with ethyl acetate, and the extract was cleaned up using a neutral alumina column and an active carbon column after concentrated and then eluted with a mixture of n-hexane-ethyl acetate (1 : 1, v/v). During the process of purification, the flow rate of eluent was controlled within 3 mL/min. The eluate was collected and evaporated to 1 mL for analysis. The determination was performed on a gas chromatograph equipped with an electron capture detector. The retention time was used for qualification and the external calibration standard was used for quantitation. The results obtained showed that the recoveries were 80.5% - 97.3% for alpha-endosulfan and 81.1% - 109.5% for beta-endosulfan. The limit of detection (LOD) was 0. 002 mg/kg, and the limit of quantitation (LOQ) was 0. 007 mg/kg for both. The precision of the method, expressed as the relative standard deviation for the within-laboratory repeatability, was generally below 8.5%. The method was used for the analysis of Litopenaeus vannamai samples from Guangxi Province, a Litopenaeus vannamai aquiculture area in south China. PMID:17679437

  17. Seasonal trends in organochlorine pesticide residues in raw bovine milk from rural areas of Haryana, India.

    PubMed

    Kaushik, C P; Kaushik, A; Sharma, H R

    2014-01-01

    Seasonal trends in organochlorine pesticides residues namely, 1,2,3,4,5,6-hexachlorocyclohexane (HCH) isomers, 1,1,1-trichloro-2,2-bis (p-chlorophenyl) ethane (DDT) and its metabolites and endosulfan stereo isomers were investigated in raw bovine milk samples from rural areas of Ambala, Gurgaon and Hisar districts of the state of Haryana for winter, summer, and post-monsoon seasons. Highest concentration of HCH and DDT was found in 43 % and 53 % milk samples, respectively in post-monsoon season whereas highest values of endosulfan was reported in 36 % samples during winter season. During the study period only 2 % milk samples exceeded the maximum residue limit recommended by WHO for ΣHCH, 1 % samples each for α-HCH and γ-HCH, 9 % samples for β-HCH as recommended by PFAA and 30 % samples for ΣDDT as prescribed by FAO. No statistical difference in the mean concentration of ∑HCH and ∑Endosulfan could be observed in any of the three districts. However, ∑DDT concentration showed marked difference [F(2, 25) = 12.42, p = 0.00018)] among the three districts. PMID:24154613

  18. Pesticide residues in bovine milk from a predominantly agricultural state of Haryana, India.

    PubMed

    Sharma, H R; Kaushik, A; Kaushik, C P

    2007-06-01

    One hundred forty seven samples of bovine milk were collected from 14 districts of Haryana, India during December 1998-February 1999 and analysed for the presence of organochlorine pesticide (OCPs) residues. summation operator HCH, summation operator DDT, summation operator endosulfan and aldrin were detected in 100%, 97%, 43% and 12% samples and with mean values of 0.0292, 0.0367, 0.0022 and 0.0036 microg/ml, respectively. Eight percent samples exceeded the maximum residue limit (MRL) of 0.10 mg/kg as recommended by WHO for summation operator HCH, 4% samples of 0.05 mg/kg for alpha-HCH, 5% samples of 0.01 mg/kg for gamma-HCH, 26% samples of 0.02 mg/kg for beta-HCH as recommended by PFAA and 24% samples of 0.05 mg/kg as recommended by FAO for summation operator DDT. Concentrations of beta-HCH and p,p'-DDE were more as compared to other isomers and metabolites of HCH and DDT. PMID:17180431

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

    PubMed

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

    2012-03-01

    Eight pesticide residues in tomato samples collected in the area of Souss Massa Valley (Southern Morocco) were analyzed. The detected residue levels ranged from 0.001 to 0.400 mg kg(-1) for dicofol, from 0.003 to 0.170 mg kg(-1) for procymidone, from 0.001 to 0.250 mg kg(-1) for chlorothalonil, from 0.050 to 0.500 mg kg(-1) for bifenthrin, from 0.001 to 0.010 mg kg(-1) for λ-cyhalothrin, from 0.001 to 0.300 mg kg(-1) for cypermethrin, from 0.010 to 1 mg kg(-1) for deltamethrin and from 0.003 to 1.123 mg kg(-1) for endosulfan. European MRL for endosulfan in tomatoes set in 0.500 mg kg(-1), was exceeded in 8 samples, and MRL for deltamethrin set in 0.300 mg kg(-1) for tomatoes was exceeded in 2 samples. PMID:22210446

  20. [Dietary risk assessment for pesticide residues in food of plant origin during the plant protection product's registration process].

    PubMed

    Struciński, Paweł; Góralczyk, Katarzyna; Czaja, Katarzyna; Hernik, Agnieszka; Korcz, Wojciech; Ludwicki, Jan K

    2006-01-01

    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

  1. Greater Cognitive Decline with Aging among Elders with High Serum Concentrations of Organochlorine Pesticides

    PubMed Central

    Kim, Se-A; Lee, Yu-Mi; Lee, Ho-Won; Jacobs, David R; Lee, Duk-Hee

    2015-01-01

    Although cognitive decline is very common in elders, age-related cognitive decline substantially differs among elders and the determinants of the differences in age-related cognitive decline are unclear. We investigated our hypothesis that the association between age and cognition was stronger in those with higher serum concentrations of organochlorine (OC) pesticides, common persistent and strongly lipophilic neurotoxic chemicals. Participants were 644 elders aged 60-85, participating in the National Health and Nutrition Examination Survey 1999-2002. Six OC pesticides (p,p'-dichlorodiphenyltrichloroethane (DDT), p,p'-dichlorodipenyldichloroethylene (DDE), β-hexachlorocyclohexane, trans-nonachlor, oxychlordane, and heptachlor epoxide) were evaluated. “Lower cognitive function” was defined as having a low Digit-Symbol Substitution Test (DSST) score (<25th percentile of DSST score, cutpoint 28 symbols substituted). Higher levels of β-hexachlorocyclohexane, trans-nonachlor, oxychlordane, and heptachlor epoxide modified the associations between age and lower cognitive function (Pinteraction<0.01, 0.03, <0.01, and 0.02, respectively). Elders in the 3rd tertile of these chemicals demonstrated a greater risk of lower cognitive function with aging, compared to those in the combined 1st and 2nd tertiles. Among those with highest OC pesticides (3rd tertile), the odds ratio for the risk of lower cognitive function was about 6 to 11 for the highest quintile of age (80-85 years) vs. the first quintile of age (60-63 years), while the association between age and lower cognitive function became flatter in those with lower OC pesticides (combined 1st and 2nd tertiles). Both DDT and DDE showed no interaction, with lower DSST scores for higher age irrespective of serum concentrations of DDT or DDE. Even though DSST score measures only one aspect of cognition, several OC pesticides modified aging-related prevalence of low cognitive score, a finding which should be evaluated in

  2. Younger age at onset of sporadic Parkinson's disease among subjects occupationally exposed to metals and pesticides

    PubMed Central

    Farb, David H.; Ozer, Josef; Feldman, Robert G.; Durso, Raymon

    2014-01-01

    An earlier age at onset of Parkinson's disease (PD) has been reported to be associated with occupational exposures to manganese and hydrocarbon solvents suggesting that exposure to neurotoxic chemicals may hasten the progression of idiopathic PD. In this study the role of occupational exposure to metals and pesticides in the progression of idiopathic PD was assessed by looking at age at disease onset. The effects of heritable genetic risk factors, which may also influence age at onset, was minimized by including only sporadic cases of PD with no family history of the disease (n=58). Independent samples Student t-test revealed that subjects with occupational exposure to metals and/or pesticides (n=36) were significantly (p=0.013) younger than unexposed controls (n=22). These subjects were then divided into three groups [high (n=18), low (n=18), and unexposed (n=22)] to ascertain if duration of exposure further influenced age at onset of PD. One-way ANOVA revealed that subjects in the high exposure group were significantly (p=0.0121) younger (mean age: 50.33 years) than unexposed subjects (mean age: 60.45 years). Subjects were also stratified by exposure type (metals vs. pesticides). These results suggest that chronic exposure to metals and pesticides is associated with a younger age at onset of PD among patients with no family history of the disease and that duration of exposure is a factor in the magnitude of this effect. PMID:26109889

  3. Assessment of pesticide residues in two arable soils from the semi-arid and subtropical regions of China.

    PubMed

    Wang, Ligang; Zhao, Zhenhua; Jiang, Xin; Wu, Jinshui; Martens, Dieter

    2005-10-01

    The residues of 31 chlorinated hydrocarbons (CHCs), 25 chlorophenols (CPs), 30 organophosphorus (OP) and pyrethroid (PRT) in two arable soils from the semi-arid and subtropical regions of China were assessed. Data obtained indicate that the main compounds of CHC pesticide residues in the semi-arid soil were 4,4'-DDE (25.3 ng/g) and beta-HCH (14.1 ng/g), which totally accounted to about 90% of total CHC residues detected. The total content of CHC residues detected in the subtropical soil was only 3.1 ng/g, of which approximately 50% was beta-HCH. However, the total content of CP residues in both of the soils was about 11 ng/g. In the semi-arid soil, only parathion-methyl amongst the 30 compounds of OP and PRT residues was detected (32.5 ng/g), whilst malathion and parathion-methyl (8.7 and 17.7 ng/g, respectively) detected in the subtropical soil. Based on these results, it was suggested the environmental risk of pesticide residues ranked in an order as CHCs (mainly as 4,4'-DDE, beta-HCH) > OP (parathion-methyl) > CPs for the semi-arid soil, and as OPs (parathion-methyl and malathion) > CPs > CHCs (beta-HCH) for the subtropical soil. PMID:16240205

  4. Flesh residue concentrations of organochlorine pesticides in farmed and wild salmon from British Columbia, Canada.

    PubMed

    Kelly, Barry C; Ikonomou, Michael G; Higgs, David A; Oakes, Janice; Dubetz, Cory

    2011-11-01

    The present study reports measured levels of organochlorine pesticides (OCPs) in commercial salmon feed (n = 8) and farmed Atlantic, coho, and chinook salmon (n = 110), as well as wild coho, chinook, chum, sockeye, and pink salmon (n = 91). Flesh residue concentrations (ng/g wet weight) of dichlorodiphenyltrichloroethanes (DDTs), hexachlorocyclohexanes (HCHs), chlordanes, chlorobenzenes (CBz) and cyclodiene pesticides (e.g., dieldrin, mirex) were 2 to 11 times higher (p < 0.05) in farmed salmon compared with wild salmon. Concentrations were positively correlated with flesh lipid levels. Farmed Atlantic salmon (12-15% lipid) typically exhibited the greatest OCP burdens compared with other salmon species. However, when expressed on a lipid weight basis, concentrations of OCPs (ng/g lipid weight) in wild salmon, in many cases, exceeded those levels in farmed salmon. Observed interspecies and site-specific variations of OCP concentrations in farmed and wild salmon may be attributed to divergent life history, prey/feed characteristics and composition, bioenergetics, or ambient environmental concentrations. Calculated biomagnification factors (BMF = C(F)/C(D), lipid wt) of OCPs in farmed salmon typically ranged between two and five. Biomagnification of chemicals such as DDTs, chlordanes, and mirex was anticipated, because those compounds tend to exhibit high dietary uptake and slow depuration rates in fish because of relatively high octanol-water partition coefficients (K(OW)s > 10⁵). Surprisingly, less hydrophobic pesticides such as hexachlorocyclohexanes and endosulfans (K(OW) s < 10⁵) consistently exhibited a high degree of biomagnification in farmed salmon species (BMFs > 5). This is contrary to previous laboratory and field observations demonstrating fish BMFs less than 1 for low K(OW) chemicals, because of efficient respiratory elimination of those compounds via gills. The results suggest that ambient seawater concentrations and

  5. Efficiency of QuEChERS approach for determining 52 pesticide residues in honey and honey bees.

    PubMed

    Calatayud-Vernich, Pau; Calatayud, Fernando; Simó, Enrique; Picó, Yolanda

    2016-01-01

    A comparison between QuEChERS and other pesticide extraction procedures for honey and honey bee matrices is discussed. Honey bee matrix was extracted by solvent based procedure whereas solid phase extraction was the protocol for the honey matrix. The citrate buffered QuEChERS method was used for both matrices. The methods were evaluated regarding cost (equipment and reagents), time, accuracy, precision, sensitivity and versatility. The results proved that the QuEChERS protocol was the most efficient method for the extraction of the selected pesticides in both matrices. •QuEChERS is the most economical and less time-consuming procedure.•SPE and solvent-based extraction procedures show equivalent recoveries to QuEChERS.•QuEChERS can be used to extract pesticide residues from both matrices. PMID:27331025

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

    PubMed

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

    2014-06-01

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

  7. 75 FR 46924 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-08-04

    ... in the body of this document, by one of the following methods: Federal eRulemaking Portal: http://www... number and the pesticide petition number of interest as shown in the body of this document. EPA's policy... body of your comment. If you send an e- mail comment directly to EPA without going through...

  8. 78 FR 70007 - Receipt of a Pesticide Petition Filed for Residues of a Pesticide Chemical in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-11-22

    ... adverse human health impacts or environmental effects from exposure to the pesticides discussed in this...-incorporated protectant (PIP), Bacillus thuringiensis Cry1F protein, in or on soybean. The petitioner believes... include: Crop production (NAICS code 111). Animal production (NAICS code 112). Food manufacturing...

  9. 76 FR 69690 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-11-09

    ..., and be free of any defects or viruses. Docket: All documents in the docket are listed in the docket...-10 at 2.5 ppm; fruit, pome, group 11-10 at 4.0 ppm; persimmon at 1.9 ppm; and tea at 20 ppm. This... a pesticide inert ingredient ultraviolet (UV) protectant in herbicide formulations at no more than...

  10. 76 FR 10584 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-02-25

    ... the use of special characters, any form of encryption, and be free of any defects or viruses. Docket..., nutmeat at 0.35 ppm; peanut, hay at 90 ppm; tea, dried leaves at 50 ppm and to increase tolerances in or...), under 40 CFR 180.950 when used as an inert ingredient in pesticide formulations as an aid in the...

  11. 76 FR 20667 - Notice of Withdrawal of Pesticide Petitions for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-04-13

    ... (75 FR 60452) (FRL-8837- 2) (EPA-HQ-OPP-2010-0547), which announced the filing of a pesticide petition... propionate). EPA issued a notice in the Federal Register of April 8, 2009 (74 FR 15976) (FRL-8409-4) (EPA-HQ... mosaic tobamovirus). EPA issued a notice in the Federal Register of March 10, 2010 (75 FR 11171)...

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

    PubMed

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

    2016-03-01

    The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/PDMS fiber increased with increasing spiking levels, yielding significant (R(2) > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity. PMID:26964527

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

    PubMed

    Hu, Beizhen; Cai, Haijiang; Song, Weihua

    2012-09-01

    A method was developed for the determination of eight pesticide residues (fipronil, imidacloprid, acetamiprid, buprofezin, triadimefon, triadimenol, profenofos, pyridaben) in tea by liquid chromatography-tandem mass spectrometry. The sample was extracted by accelerated solvent extraction with acetone-dichloromethane (1:1, v/v) as solvent, and the extract was then cleaned-up with a Carb/NH2 solid phase extraction (SPE) column. The separation was performed on a Hypersil Gold C, column (150 mm x 2. 1 mm, 5 microm) and with the gradient elution of acetonitrile and 0. 1% formic acid. The eight pesticides were determined in the modes of electrospray ionization (ESI) and multiple reaction monitoring (MRM). The analytes were quantified by matrix-matched internal standard method for imidacloprid and acetamiprid, by matrix-matched external standard method for the other pesticides. The calibration curves showed good linearity in 1 - 100 microg/L for fipronil, and in 5 -200 microg/L for the other pesticides. The limits of quantification (LOQs, S/N> 10) were 2 p.g/kg for fipronil and 10 microg/kg for the other pesticides. The average recoveries ranged from 75. 5% to 115.0% with the relative standard deviations of 2.7% - 7.7% at the spiked levels of 2, 5, 50 microg/kg for fipronil and 10, 50, 100 microg/kg for the other pesticides. The uncertainty evaluation for the results was carried out according to JJF 1059-1999 "Evaluation and Expression of Uncertainty in Measurement". Items constituting measurement uncertainty involved standard solution, weighing of sample, sample pre-treatment, and the measurement repeatability of the equipment were evaluated. The results showed that the measurement uncertainty is mainly due to sample pre-treatment, standard curves and measurement repeatability of the equipment. The method developed is suitable for the conformation and quantification of the pesticides in tea. PMID:23285969

  14. Behavior of Multiclass Pesticide Residue Concentrations during the Transformation from Rose Petals to Rose Absolute.

    PubMed

    Tascone, Oriane; Fillâtre, Yoann; Roy, Céline; Meierhenrich, Uwe J

    2015-05-27

    This study investigates the concentrations of 54 multiclass pesticides during the transformation processes from rose petal to concrete and absolute using roses spiked with pesticides as a model. The concentrations of the pesticides were followed during the process of transforming the spiked rose flowers from an organic field into concrete and then into absolute. The rose flowers, the concrete, and the absolute, as well as their transformation intermediates, were analyzed for pesticide content using gas chromatography/tandem mass spectrometry. We observed that all the pesticides were extracted and concentrated in the absolute, with the exception of three molecules: fenthion, fenamiphos, and phorate. Typical pesticides were found to be concentrated by a factor of 100-300 from the rose flowers to the rose absolute. The observed effect of pesticide enrichment was also studied in roses and their extracts from four classically phytosanitary treated fields. Seventeen pesticides were detected in at least one of the extracts. Like the case for the spiked samples in our model, the pesticides present in the rose flowers from Turkey were concentrated in the absolute. Two pesticides, methidathion and chlorpyrifos, were quantified in the rose flowers at approximately 0.01 and 0.01-0.05 mg kg(-1), respectively, depending on the treated field. The concentrations determined for the corresponding rose absolutes were 4.7 mg kg(-1) for methidathion and 0.65-27.25 mg kg(-1) for chlorpyrifos. PMID:25942486

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

    PubMed

    Sapbamrer, Ratana; Hongsibsong, Surat

    2014-07-01

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

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

    PubMed

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

    2007-05-01

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

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

    PubMed

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

    2015-07-15

    Various drug residues, pesticides and phthalates are ubiquitous in the environment. Their presence in the environment has attracted considerable attention due to their potential impacts on ecosystem functioning and on public health. In this work, 14 drug residues, 24 pesticides and 6 phthalates have been quantified in three matrices (in the dissolved phase, associated to suspended solid matter (SSM), and in sediment) collected from fifteen watercourses and rivers located in a highly industrialized zone at the cross-border area of Northern France and Belgium. The extractions have been carried out using accelerated solvent extraction (ASE) for solid matrices (SSM and sediment) and using solid phase extraction (SPE) for liquid matrix. The final extract was analyzed using GC-MS technique. Among the three classes of compounds, phthalates have been found at highest level compared to pesticides and drug residues. The Σ6PAE concentrations were ranging from 17.2±2.58 to 179.1±26.9μgL(-1) in dissolved phase, from 2.9±0.4 to 21.1±3.2μgL(-1) in SSM and from 1.1±0.2 to 11.9±1.8μgg(-1)dw in sediment. The Σ14drug residue concentrations were lower than 1.3μgL(-1) in the dissolved phases, lower than 30ngL(-1) associated to SSM and from nondetectable levels to 60.7±9.1ngg(-1)dw in sediment. For pesticides, all compounds were below the LOQ values in dissolved phase and in sediment, and only EPTC could be quantified in SSM. PMID:25829293

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

    PubMed

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

    2015-09-01

    This study aims to investigate the concentrations of organophosphorus pesticides (OPs) in fresh vegetables. A total of Z14 samples from seven types of vegetables were collected from the suburb in Changchun City. The OPs were analyzed by gas chromatography coupled with flame photometric detector (GC-FPD). Target hazard quotients (THQ) were applied to estimate the potential health risk to inhabitants. Results showed that OPs concentrations exceeded the Maximum Residue Limit (MRL) in more than 23. 4% samples, and were not detected in only 7. 9% samples. Detection rates of OPs was as follow in the decreased order: diazinon (82. 2%) > phorate (45. 8%) > dimethoate (29. 4%) > parathion-methyl (27. 6%) > omethoate (23. 8%) > dichlorvos (22. 9%) > fenitrothion (21%) > fenthion (18. 7%) > parathion (18. 2%) > methamidophos (17. 3%) > malathion (12. 1%). The percentages above MRL for leaves were higher than for non-leafy vegetables. The order of percentages of OPs above MRL was as follows: green onion (82. 5%) > radish (37. 5%) > red pepper (17. 2%) > Chinese vegetable (14. 3%) > cucumber (3. 2%) > eggplant (2. 9%) > tomato (0%). 49. 5% vegetables samples showed more than one OP. The average target hazard quotients (ave THQ) were all less than one and the average Hazard Index (ave HI) was 0. 462, so that inhabitants who expose average OP levels may not experience adverse health effects. PMID:26717714

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

    PubMed

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

    2014-07-01

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

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

    NASA Astrophysics Data System (ADS)

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

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

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

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

    PubMed

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

    2014-01-01

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

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

    PubMed

    Sykes, Mark; Thompson, Michael; Reynolds, Stewart

    2013-05-01

    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

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

    PubMed

    Witczak, Agata; Abdel-Gawad, Hassan

    2012-01-01

    Organic and conventional crops were studied by identifying the relationship between persistent organic pollutants in cereals, vegetables and soil. The residues of organochlorine pesticides and polychlorinated biphenyls (PCBs) were determined in grains (rye and wheat), vegetables (carrots and beets) and soil collected from the fields. PCB residues recorded in the beets from organic farming were as high as 3.71 ppb dry weight (dry wt.), while in the soil from conventional farming of beets 0.53 ppb dry wt. Among vegetables, higher concentrations of pesticides were detected in organically grown beets (190.63 ppb dry wt.). Soil samples from the organic farming contained lower levels of organochlorine pesticide residues compared to the conventional farming. Taking into account toxicity equivalent (TEQ), the conventionally grown carrots accumulated the most toxic PCBs. Non-ortho and mono-ortho PCBs were also noted in the grain of conventionally grown rye and amounted to 3.05 pg-TEQ/g wet wt. PMID:22428896

  5. Pesticide, PCB, and lead residues and necropsy data for bald eagles from 32 states - 1978-81

    USGS Publications Warehouse

    Reichel, W.L.; Schmeling, S.K.; Cromartie, E.; Kaiser, T.E.; Krynitsky, A.J.; Lamont, T.G.; Mulhern, B.M.; Prouty, R.M.; Stafford, C.J.; Swineford, D.M.

    1984-01-01

    In 1978?81, 293 bald eagles (Haliaeetus leucocephalus) from 32 states were necropsied and analyzed for organochlorine pesticides, polychlorinated biphenyls (PCB), and lead residues. DDE was found in all carcasses; PCB, DDD, trans-nonachlor, dieldrin and oxychlordane were next in order of percent frequency of detection. The median levels of DDE and PCB have declined when compared with previous collections. Five specimens contained high levels of dieldrin in their brains which may have contributed to their deaths. Seventeen eagles contained liver lead residues greater than 10 ppm and probably died of lead poisoning. Trauma and shooting are the most common causes of death.

  6. Pesticide, PCB, and lead residues and necropsy data for bald eagles from 32 states, 1978-81

    USGS Publications Warehouse

    Reichel, W.L.; Schmeling, S.K.; Cromartie, E.; Kaiser, T.E.; Krynitsky, A.J.; Lamont, T.G.; Mulhern, B.M.; Prouty, R.M.; Stafford, C.J.; Swineford, D.M.

    1984-01-01

    In 1978a??81, 293 bald eagles (Haliaeetus leucocephalus) from 32 states were necropsied and analyzed for organochlorine pesticides, polychlorinated biphenyls (PCB), and lead residues. DDE was found in all carcasses; PCB, DDD, trans-nonachlor, dieldrin and oxychlordane were next in order of percent frequency of detection. The median levels of DDE and PCB have declined when compared with previous collections. Five specimens contained high levels of dieldrin in their brains which may have contributed to their deaths. Seventeen eagles contained liver lead residues greater than 10 ppm and probably died of lead poisoning. Trauma and shooting are the most common causes of death.

  7. Residues in Food and Feed Topic Area at the 13th IUPAC International Congress of Pesticide Chemistry.

    PubMed

    Lehotay, Steven J; Riter, Leah S; Saha, Manasi

    2015-05-13

    The organizers of two symposia in the "Residues in Food and Feed" topic area held at the 13th IUPAC International Congress of Pesticide Chemistry introduce the papers that were contributed to this special section in the Journal. The symposia were titled "Taking Advantage of Advanced Analytical Tools" and "Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods". The oral and poster sessions generated much interest and discussion among the attendees, and some highlights are described in this introductory paper. PMID:25660997

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

    PubMed Central

    Stoner, Kimberly A.; Eitzer, Brian D.

    2013-01-01

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

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

    PubMed

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

    2016-09-14

    Monitoring of pesticides and veterinary drug residues is required to enforce legislation and guarantee food safety. Liquid chromatography-mass spectrometry (LC-MS) is the prevailing technique for assessing both types of residues because LC offers a versatile and universal separation mechanism suitable for non-gas chromatography (GC) amenable and the majority of GC-amenable compounds. This characteristic becomes more relevant when LC is coupled to MS because the high sensitivity and specificity of the detector allows to apply generic sample preparation procedures, which simultaneously extract a wide variety of residues with different physico-chemical properties. Determination of metabolites and degradation products, non-target suspected screening of an increasing number of residues, and even unknowns identification are also becoming inherent LC-MS advantages thanks to the latest advances. For routine analysis and, in particular, for official surveillance purposes in food control, analytical methods properly validated following strict guidelines are needed. After a brief introduction and an outline of the legislation applicable around the world, aspects such as improvement of specificity of high-throughput methods, resolution and mass accuracy of identification strategies and quantitative accuracy are critically reviewed in this article. In them, extraction, separation and determination are emphasized. The main objective is to offer an assessment of the state of the art and identify research needs and future trends in determining pesticide and veterinary drug residues in food by LC-MS. PMID:27566339

  10. 76 FR 6465 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-02-04

    ... 180 for residues of the herbicide glyphosate, N-(phosphonomethyl) glycine, in or on corn, field, forage at 13 ppm to support the use of glyphosate in RHS seed corn production. Adequate enforcement methods are available for analysis of residues of glyphosate and its metabolite AMPA in or on plant...

  11. 76 FR 22067 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-04-20

    ... tolerance for the combined residues of the herbicide glyphosate, N (phosphonomethyl)glycine, and its metabolite, N-acetyl-glyphosate (expressed as glyphosate) on canola, seed. An analytical method was developed, and validated, for the determination of glyphosate and degradate residues in transgenic crop and...

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

    PubMed

    Walorczyk, Stanisław

    2012-01-27

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

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

    PubMed

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

    2016-02-01

    A multiresidue analytical method for the determination of 250 pesticide residues in vegetables was developed by using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target compounds were extracted with acetonitrile containing 1% (v/v) acetic acid, purified by a mixed sorbent of MgSO4, primary secondary amine (PSA), graphitized carbon black (GCB) and C18, separated on a Waters ACQUITY™ UPLC BEH C18 column (100 mm x 2. 1 mm, 1.7 µm) and detected by UPLC-MS/MS. Anhydrous magnesium sulfate was used as a dewatering agent. The effects of the amounts of MgSO4, PSA, GCB and C18 added on the recoveries of 250 pesticides were investigated. The results showed that the purification effect was best when 300 mg MgSO4, 200 mg PSA, 10 mg GCB and 100 mg C18 in 2 mL of the extract were added. For the 250 pesticide residues, the limits of detection (LODs) of the method were from 0. 01 to 50. 00 g/kg. The recoveries obtained ranged from 60. 1% to 120% at three spiked levels in Chinese chives with the relative standard deviations between 3. 5% and 19. 5% using matrix matched external standard method. The results showed that the method is able to meet requirements of the multiresidue detection of the 250 pesticides in vegetable. The method has the advantages of rapidity, simplicity, high sensitivity and better purification effect. It is suitable for the rapid determination of the common pesticides in vegetables, and it provides a strong guarantee for the risk assessments of the quality and safety of vegetables. PMID:27382720

  14. 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.

    PubMed

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

    2013-01-01

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

  15. Human health risk assessment of pesticide residues in market-sold vegetables and fish in a northern metropolis of China.

    PubMed

    Fang, Yanyan; Nie, Zhiqiang; Yang, Yanmei; Die, Qingqi; Liu, Feng; He, Jie; Huang, Qifei

    2015-04-01

    With growing concerns about food safety and stricter national standards in China, attention has focused on vegetables and fish as they are an important part of the Chinese daily diet, and pesticide residues can accumulate in these foodstuffs. The local consumption habits of vegetables and fish were determined using questionnaires distributed in the major regions of the northern metropolis. Then, the samples of fruit-like vegetables, leafy and root vegetables, and five species of fish (freshwater and marine) were collected from supermarkets and traditional farmers' markets in the city. The concentrations and profiles of pesticide residues (hexachlorocyclohexane (HCH), dichlorodiphenyl trichloroethane (DDT), and endosulfan) in the samples were determined and compared. For the vegetables, the concentration ranges of ΣDDT, ΣHCH, and Σendosulfan were not detectable (ND) to 10.4 ng/g fresh weight (f.w.), ND to 58.8 ng/g f.w., and ND to 63.9 ng/g f.w., respectively. For the fish samples, the corresponding values were 0.77-25.0 ng/g f.w., 0.02-1.42 ng/g f.w., and 1.22-22.1 ng/g f.w., respectively. Only one celery sample exceeded the maximum residue limits (MRLs) of HCH residues set by Chinese regulations (GB2763-2014). The estimated daily intakes (EDIs) and hazard ratios (HRs) were calculated using data from the recently published Exposure Factors Handbook for the Chinese Population. The EDIs and HRs showed that the levels of organochlorine pesticide (OCP) residues in vegetables and fish in this area are safe. PMID:25395327

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

    PubMed

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

    2016-08-01

    A simple multi-residue method based on modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach was established for the determination of 17 organochlorine (OC), 15 organophosphorous (OP) and 7 synthetic pyrethroid (SP) pesticides in an economically important medicinal plant of India, Senna (Cassia angustifolia), by gas chromatography coupled to electron capture and flame thermionic detectors (GC/ECD/FTD) and confirmation of residues was done on gas chromatograph coupled with mass spectrometry (GC-MS). The developed method was validated by testing the following parameters: linearity, limit of detection (LOD), limit of quantification (LOQ), matrix effect, accuracy-precision and measurement uncertainty; the validation study clearly demonstrated the suitability of the method for its intended application. All pesticides showed good linearity in the range 0.01-1.0 μg mL(-1) for OCs and OPs and 0.05-2.5 μg mL(-1) for SPs with correlation coefficients higher than 0.98. The method gave good recoveries for most of the pesticides (70-120%) with intra-day and inter-day precision < 20% in most of the cases. The limits of detection varied from 0.003 to 0.03 mg kg(-1), and the LOQs were determined as 0.01-0.049 mg kg(-1). The expanded uncertainties were <30%, which was distinctively less than a maximum default value of ±50%. The proposed method was successfully applied to determine pesticide residues in 12 commercial market samples obtained from different locations in India. PMID:27153296

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

    PubMed

    Young, S J; Kamps, L R

    1982-07-01

    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

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

    PubMed

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

    2016-01-01

    South Korea has a unique food culture. South Koreans enjoy wrapping meat and eating or making kimchi (traditionally fermented Korean food) and eating using raw leafy vegetables, stalk and stem vegetables. Therefore, there is a high chance of being exposed to pesticide residues of vegetables. The objective of this study was to investigate pesticide residues in leafy vegetables, stalk and stem vegetables from South Korea. A total of 8496 samples were mainly collected from Gwangju and Jeonnam area (the largest production region of leafy vegetables, stalk and stem vegetables) in South Korea from 2010 to 2014. A total of 230 pesticides were used for multi-residue analysis of pesticides. Among 8496 samples, 61 different pesticides (1029 times) were detected in 890 samples, of which 118 samples (1.4%) exceeded the Korea maximum residue limits (MRLs). Samples exceeding the MRLs were mostly found in leafy vegetables (brassica lee ssp. namai, leafy lettuce, spinach, perilla leaves, crown daisy, marsh mallow, aster scaber, pimpinella brachycarpa) and Chinese chive. Procymidone, dimethomorph and azoxystrobin were the most frequently found pesticides. A risk assessment of pesticides exceeding the MRLs was evaluated by calculating the estimated daily intake (EDI) and the acceptable daily intake (ADI). The ratio of EDI to ADI was 0.003-30.4%. PMID:26571090

  19. The potential for using ozone to decrease pesticide residues in honey bee comb

    Technology Transfer Automated Retrieval System (TEKTRAN)

    As a strong oxidizer, ozone is known to breakdown some organic pesticides, and we evaluated the potential for using a gaseous fumigation of ozone to decontaminate honeycomb and empty honey bee hives. Honey bees are inadvertently exposed to pesticides when they forage for nectar and pollen in agricul...

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

    PubMed Central

    Phopin, Kamonrat; Boonpangrak, Somchai; Prachayasittikul, Virapong

    2016-01-01

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

  1. Focused microwave assistance for extracting some pesticide residues from strawberries into water before their determination by SPME/HPLC/DAD.

    PubMed

    Falqui-Cao, C; Wang, Z; Urruty, L; Pommier, J J; Montury, M

    2001-11-01

    A novel and simple method for the determination of some pesticide residues in strawberries using both focused microwave-assisted extraction (FMAE) and solid-phase micro extraction (SPME), coupled with high-performance liquid chromatography (HPLC), has been developed. The pesticides were first extracted from strawberries with water and the assistance of focused microwaves at 30 W for 7 min. Then, an aliquot of the resulting aqueous extract was subjected to SPME with a 60-microm thick poly(dimethylsiloxane)/divinylbenzene (PDMS/DVB) fiber for 45 min at room temperature, with the solution being stirred at 1000 rpm. The extracted pesticides on the SPME fiber were desorbed into the SPME/HPLC interface for quantitative analysis with a diode array detector (DAD). The whole sample pretreatment procedure before chromatographic analysis did not use any organic solvents or involve any blending or centrifugation steps. The five compounds (carbendazim, diethofencarb, azoxystrobine, napropamide, and bupirimate) were chosen because they cannot be analyzed easily by GC. The efficiency of this relatively fast procedure was comparable to that of previously reported methods, with detection limits at low microg/kg levels and linear responses in the range from 0.05 to 1 mg/kg of pesticide in strawberries, with RSDs between 3 and 7.3%, depending on the analyte. In all but one case results obtained by this method for field-incurred samples were comparable to those obtained with traditional methods. PMID:11714287

  2. 75 FR 11173 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-03-10

    ... preamble for FR Doc. 2010-2382 published in the Federal Register of Thursday, February 4, 2010 (75 FR 5790... tolerances in 40 CFR part 180 for residues of the ``insecticide'' fluazifop-p-butyl in various...

  3. 75 FR 864 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-01-06

    ... residues of the fungicide cyazofamid, 4-chloro-2-cyano-N,N-dimethyl-5- (4-methylphenyl)-1H-imidazole-1-sulfonamide and its metabolite CCIM, 4- chloro-5-(4-methylphenyl)-1H-imidazole-2-carbonitrile, expressed...

  4. 77 FR 59577 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-09-28

    ... preamble for FR Doc. 2012-17899, published in the Federal Register of Wednesday, July 25, 2012 (77 FR 43562... tolerances for residues of the herbicide pyroxasulfone and its metabolites in or on wheat (grain,...

  5. Current status of persistent organic pesticides residues in air, water, and soil, and their possible effect on neighboring countries: a comprehensive review of India.

    PubMed

    Yadav, Ishwar Chandra; Devi, Ningombam Linthoingambi; Syed, Jabir Hussain; Cheng, Zhineng; Li, Jun; Zhang, Gan; Jones, Kevin C

    2015-04-01

    Though the use of pesticides has offered significant economic benefits by enhancing the production and yield of food and fibers and the prevention of vector-borne diseases, evidence suggests that their use has adversely affected the health of human populations and the environment. Pesticides have been widely distributed and their traces can be detected in all areas of the environment (air, water and soil). Despite the ban of DDT and HCH in India, they are still in use, both in domestic and agricultural settings. In this comprehensive review, we discuss the production and consumption of persistent organic pesticides, their maximum residual limit (MRL) and the presence of persistent organic pesticides in multicomponent environmental samples (air, water and soil) from India. In order to highlight the global distribution of persistent organic pesticides and their impact on neighboring countries and regions, the role of persistent organic pesticides in Indian region is reviewed. Based on a review of research papers and modeling simulations, it can be concluded that India is one of the major contributors of global persistent organic pesticide distribution. This review also considers the health impacts of persistent organic pesticides, the regulatory measures for persistent organic pesticides, and the status of India's commitment towards the elimination of persistent organic pesticides. PMID:25540847

  6. Analysis of Trends of the Types of Pesticide Used, Residues and Related Factors among Farmers in the Largest Vegetable Producing Area in the Philippines

    PubMed Central

    Lu, Jinky Leilanie

    2010-01-01

    The objective of study is to provide an analysis of data trends on the type of pesticide used, exposure factors, and the pesticide-related concerns among the farmers from 2005 to 2010 in one of the largest vegetable producing areas in the Philippines. This is to determine and analyze changes that have occurred for the last five years in order to provide necessary basis in promoting safe usage of pesticides. It is shown in the studies that the most commonly used type of pesticide was Tamaron (methamidophos) which is an organophosphate. The top five pesticide-related symptoms confirm findings in other studies. The risk factors to pesticide exposure were also identified in the reviewed studies such as improper mixing and loading of pesticides, and re-entering previously sprayed area. Pesticide residues were also found in vegetables, soil and water samples. This points to environmental contamination due to pesticide. It is suggested that government agencies implement programs on monitoring, surveillance, information dissemination, and training on proper use of pesticides, and seek alternative farming such as organically grown vegetables, or use of integrated pest management as well as good agricultural practices. PMID:25649105

  7. Determination of five pesticide residues in oranges by matrix solid-phase dispersion and liquid chromatography to estimate daily intake of consumers.

    PubMed

    Valenzuela, A I; Picó, Y; Font, G

    2001-01-01

    Residues of benzoylphenylurea insecticides (diflubenzuron, hexaflumuron, and flufenuxuron), carboxamide acaricides (hexythiazox), and carbamate insecticides (benfuracarb) were determined in 150 orange fruit samples from September 1998 to June 1999, to estimate exposure of the Valencian population to oranges contaminated with these newly developed pesticides. The method for monitoring these residues is based on matrix solid-phase dispersion and liquid chromatography with UV or atmospheric pressure chemical ionization/mass spectrometry (APCI/MS) detection. Orange samples representing 11 varieties were collected from an agricultural cooperative and examined for the 5 pesticides. In 74.6% of all analyzed samples, the pesticide residues were below detection limits, which ranged from 0.002 to 0.05 mg/kg. Residues were detected in 25.4% of the samples, with higher incidences of diflubenzuron, flufenuxuron, hexythiazox, and benfuracarb; hexaflumuron residues were detected only occasionally. Two different pesticides exceeded maximum residue limits (MRLs) in 4 (2.7%) of the orange samples. Diflubenzuron surpassed 1 mg/kg MRL in 3 samples and flufenuxuron exceeded the 0.3 mg/kg MRL in 3 samples. The estimated daily intake of the 5 pesticide residues during the period was 0.077 microg/kg body weight per day. This value is much lower than the total admissible daily intake proposed by the Food and Agricultural Organization and the World Health Organization. PMID:11417653

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

    PubMed

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

    2016-07-01

    An ultrasensitive method for the simultaneous analysis of pesticides residues in tobacco was developed with online size exclusion chromatography with gas chromatography and tandem mass spectrometry. Tobacco samples were extracted with the solvent mixture of cyclohexane and acetone (7:3, v/v) and centrifuged. Then, the supernatant liquors were injected directly into the online size exclusion chromatography with gas chromatography and tandem mass spectrometry without any other purification procedures after being filtered with a 0.22 μm organic phase filter. The matrix interferences were effectively removed and recoveries of most pesticides were in the range of 72-121%. Especially, for chlorothalonil, the analysis efficiency of this method was much more favorable than that of the general method, in which dispersive solid-phase extraction was used as an additional purified procedure. In addition, the limits of quantitation of this method were from 1 to 50 μg/kg. Therefore, a rapid, cost-effective, labor-saving method was proposed in the present work, which was suitable for the analysis of 41 pesticide residues in tobacco. PMID:27197809

  9. [Determination of 213 pesticide residues in milk and milk power by gas chromatography-triple quadrupole tandem mass spectrometry].

    PubMed

    Wang, Jing; Ai, Lianfeng; Ma, Yusong; Zhang, Haichao; Li, Wei; Yu, Meng

    2015-11-01

    On the basis of the optimization of solid phase extraction adsorbent, eluting solvent types and amounts, a gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS) method was established for the determination of 213 pesticide residues in milk and milk power. The samples were extracted by acetonitrile, cleaned-up with an ENVI-Carb/NH2 solid-phase extractant, and determined by GC-MS/MS using external standard method. The linear ranges were from 10 to 1 000 μg/L for 197 pesticides, from 50 to 1 000 μg/L for the other 16 pesticides with the correlation coefficients higher than 0.99. The limits of detection (LODs, S/N = 3) varied over the range of 0.03 to 7.59 μg/kg, and limits of quantification (LOQs, S/N = 10) ranged from 0.10 to 21.94 μg/kg. The average recoveries in different matrices were in the range of 66.9% - 120.1% with the relative standard deviations (RSDs) of 1.23% - 17.6%. This method is simple, rapid, sensitive and reliable for meeting the requirements for the simultaneous identification and quantification of the multi-residues in milk and milk power. PMID:26939364

  10. Evaluation of serum pesticide residue levels and liver function in persons exposed to dairy products contaminated with heptachlor

    SciTech Connect

    Stehr-Green, P.A.; Wohlleb, J.C.; Royce, W.; Head, S.L.

    1988-01-15

    The authors studied a group of 45 dairy farm family members who had consumed undiluted raw milk products known to be contaminated with residues of the pesticide heptachlor at concentrations as high as 89.2 ppm (fat basis). They compared results of serum pesticide assays for these exposed persons with results for an unexposed group of 94 persons from the same geographic area and the results from the Second National Health and Nutrition Examination Survey. The exposed group had significantly higher mean levels of primary heptachlor metabolites-i.e., heptachlor epoxide and oxychlordane than the unexposed group. In the exposed group, 21.2% had evaluated serum concentrations of these same metabolites; this rate was significantly greater than the rates in both the unexposed farm family members (heptachlor epoxide, 3.8%; oxychlordane, 6.3%) and the Second National Health and Nutrition Examination Survey sample (2.5% for both metabolites). However they found no evidence of related acute and/or subacute hepatic effects in these exposed persons regardless of their serum concentrations of pesticide residues.

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

    PubMed

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

    2016-09-01

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

  12. Study of Inhibition, Reactivation and Aging Processes of Pesticides Using Graphene Nanosheets/Gold Nanoparticles-Based Acetylcholinesterase Biosensor

    SciTech Connect

    Zhang, Lin; Long, Linjuan; Zhang, Weiying; Du, Dan; Lin, Yuehe

    2012-09-10

    Organophosphate (OP) and carbamate pesticides exert their toxicity via attacking the hydroxyl moiety of serine in the 'active site' of acetylcholinesterase (AChE). In this paper we developed a stable AChE biosensor based on self-assembling AChE to graphene nanosheet (GN)-gold nanoparticles (AuNPs) nanocomposite electrode for investigation of inhibition, reactivation and aging processes of different pesticides. It is confirmed that pesticides can inhibit AChE in a short time. OPs poisoning is treatable with oximes while carbarmates exposure is insensitive to oximes. The proposed electrochemical approach thus provides a new simple tool for comparison of pesticide sensitivity and guide of therapeutic intervention.

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

    USGS Publications Warehouse

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

    2008-01-01

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

  14. Analytical method for 44 pesticide residues in spinach using multi-plug-filtration cleanup based on multiwalled carbon nanotubes with liquid chromatography and tandem mass spectrometry detection.

    PubMed

    Qin, Yuhong; Huang, Baoyong; Zhang, Jingru; Han, Yongtao; Li, Yanjie; Zou, Nan; Yang, Jianguo; Pan, Canping

    2016-05-01

    Spinach is one of the most commonly planted vegetables worldwide. A high chlorophyll content makes spinach a complicated matrix in pesticide residue analysis. In this study, a rapid clean-up method was developed for the analysis of pesticide multi-residues in spinach followed by liquid chromatography with tandem mass spectrometry. A modified QuEChERS method with multiwalled carbon nanotubes and carbon material was adopted in the multi-Plug Filtration Cleanup procedure. This method was validated for 44 representative pesticides spiked at two concentration levels of 10 and 100 μg/kg. The pesticides of different physicochemical properties were registered on spinach in China. The recoveries were between 76 and 114% for major pesticides with relative standard deviations of less than 15%, except for quizalofop-P-ethyl, pyrimethanil, and carbendazim. Matrix-matched calibration curves were performed with the coefficients of determination higher than 0.995 for the studied pesticides for concentration levels of 10-500 μg/kg. The limits of quantitation ranged from 2 to 10 μg/kg. The developed method was successfully applied to determine pesticide residues in Chinese market spinach samples. PMID:26968118

  15. Relationship between Urinary Pesticide Residue Levels and Neurotoxic Symptoms among Women on Farms in the Western Cape, South Africa

    PubMed Central

    Motsoeneng, Portia M.; Dalvie, Mohamed A.

    2015-01-01

    Background: This cross-sectional study aimed to investigate the relationship between urinary pesticide residue levels and neurotoxic symptoms amongst women working on Western Cape farms in South Africa. Method: A total of 211 women were recruited from farms (n = 121) and neighbouring towns (n = 90). Participant assessment was via a Q16 questionnaire, reporting on pesticide exposures and measurement of urinary OP metabolite concentrations of dialkyl phosphates (DAP) and chlorpyriphos, 3,5,6-trichloropyridinol (TCPY) and of pyrethroid (PYR) metabolite concentrations (3- phenoxybenzoic acid (3PBA), 4-fluoro-3-phenoxybenzoic acid (4F3PBA), cis-2,2-dibromovinyl-2,2-dimethylcyclopropane-1-carboxylic acid (DBCA), and the cis- and trans isomers of 2,2-dichlorovinyl-2,2-dimethylcyclopropane-1-carboxylic acid. Results: Median urinary pesticide metabolites were slightly (6%–49%) elevated in the farm group compared to the town group, with 2 metabolites significantly higher and some lower in the farm group. The prevalence of all Q16 symptoms was higher amongst farm women compared to town women. Three Q16 symptoms (problems with buttoning, reading and notes) were significantly positively associated with three pyrethroid metabolites (cis- and trans-DCCA and DBCA), although associations may due to chance as multiple comparisons were made. The strongest association for a pyrethroid metabolite was between problems with buttoning and DBCA (odds ratio (OR) = 8.93, 95% confidence interval (CI):1.71–46.5. There was no association between Q16 symptoms and OP metabolites. Conclusions: Women farm residents and rural women from neighbouring towns in the Western Cape are exposed to OP and PYR pesticides. The study did not provide strong evidence that pesticides are associated with neurotoxic symptoms but associations found could be explored further. PMID:26042367

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

    PubMed Central

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

    2016-01-01

    A method is described for multi-residue, high-throughput determination of trace levels of 22 organochlorine pesticides (OCPs) and 5 pyrethroid pesticides (PYPs) in Chinese medicinal (CM) health wines using a QuEChERS (quick, easy, cheap, effective, rugged, and safe) based extraction method and gas chromatography-electron capture detection (GC-ECD). Several parameters were optimized to improve preparation and separation time while still maintaining high sensitivity. Validation tests of spiked samples showed good linearities for 27 pesticides (R = 0.9909–0.9996) over wide concentration ranges. Limits of detection (LODs) and quantification (LOQs) were measured at ng/L levels, 0.06–2 ng/L and 0.2–6 ng/L for OCPs and 0.02–3 ng/L and 0.06–7 ng/L for PYPs, respectively. Inter- and intra-day precision tests showed variations of 0.65–9.89% for OCPs and 0.98–13.99% for PYPs, respectively. Average recoveries were in the range of 47.74–120.31%, with relative standard deviations below 20%. The developed method was then applied to analyze 80 CM wine samples. Beta-BHC (Benzene hexachloride) was the most frequently detected pesticide at concentration levels of 5.67–31.55 mg/L, followed by delta-BHC, trans-chlordane, gamma-BHC, and alpha-BHC. The validated method is simple and economical, with adequate sensitivity for trace levels of multi-class pesticides. It could be adopted by laboratories for this and other types of complex matrices analysis. PMID:26883080

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

    NASA Astrophysics Data System (ADS)

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

    2016-02-01

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

  18. Investigation of preconcentration strategies for the trace analysis of multi-residue pesticides in real samples by capillary electrophoresis.

    PubMed

    da Silva, Clóvis L; de Lima, Elizabete C; Tavares, Marina F M

    2003-10-01

    In this work, on-line preconcentration strategies were investigated for the multi-residue analysis of pesticides in drinking water and vegetables using micellar electrokinetic chromatography. Among the on-line strategies, sweeping and stacking with reverse migration of micelles (SRMM), with and without the insertion of a plug of water before sample injection, were contrasted. A new version of SRMM was also introduced. The modification consisted of momentarily applying a positive voltage at the inlet vial right after sample has been injected, increasing the efficiency by which the analytes are captured. Nine pesticides from different classes, carbendazim (benzimidazole), simazine, atrazine, propazine and ametryn (triazine), diuron and linuron (urea), carbaryl and propoxur (carbamate), were baseline separated in less than 6 min with a electrolyte composed of 20 mmol l(-1) phosphate buffer at pH 2.5, containing 25 mmol l(-1) sodium dodecyl sulfate and 10% methanol. Limits of detection (LODs) in the order of 2-46 microg l(-1) for the pesticides under investigation were obtained solely using the on-line strategies. Enrichment factors of 3-18-fold were obtained. These factors were computed as the improvement of the concentration LODs with respect to the reference condition (injection of 10 s at 2.5 kPa pressure). The proposed methodologies were applied to the analysis of pesticides in complex matrices such as carrot extracts where the detection of 2.5 microg l(-1) was illustrated. By combining off-line solid-phase extraction and the proposed on-line strategies, the detection of pesticides in drinking water at the 0.1 microg l(-1) level was conceived. PMID:14558617

  19. Neurobehavioral Deficits and Increased Blood Pressure in School-Age Children Prenatally Exposed to Pesticides

    PubMed Central

    Harari, Raul; Julvez, Jordi; Murata, Katsuyuki; Barr, Dana; Bellinger, David C.; Debes, Frodi; Grandjean, Philippe

    2010-01-01

    Background The long-term neurotoxicity risks caused by prenatal exposures to pesticides are unclear, but a previous pilot study of Ecuadorian school children suggested that blood pressure and visuospatial processing may be vulnerable. Objectives In northern Ecuador, where floriculture is intensive and relies on female employment, we carried out an intensive cross-sectional study to assess children’s neurobehavioral functions at 6–8 years of age. Methods We examined all 87 children attending two grades in the local public school with an expanded battery of neurobehavioral tests. Information on pesticide exposure during the index pregnancy was obtained from maternal interview. The children’s current pesticide exposure was assessed from the urinary excretion of organophosphate metabolites and erythrocyte acetylcholine esterase activity. Results Of 84 eligible participants, 35 were exposed to pesticides during pregnancy via maternal occupational exposure, and 23 had indirect exposure from paternal work. Twenty-two children had detectable current exposure irrespective of their prenatal exposure status. Only children with prenatal exposure from maternal greenhouse work showed consistent deficits after covariate adjustment, which included stunting and socioeconomic variables. Exposure-related deficits were the strongest for motor speed (Finger Tapping Task), motor coordination (Santa Ana Form Board), visuospatial performance (Stanford-Binet Copying Test), and visual memory (Stanford-Binet Copying Recall Test). These associations corresponded to a developmental delay of 1.5–2 years. Prenatal pesticide exposure was also significantly associated with an average increase of 3.6 mmHg in systolic blood pressure and a slight decrease in body mass index of 1.1 kg/m2. Inclusion of the pilot data strengthened these results. Conclusions These findings support the notion that prenatal exposure to pesticides—at levels not producing adverse health outcomes in the mother

  20. Alternative QuEChERS-based modular approach for pesticide residue analysis in food of animal origin.

    PubMed

    Lichtmannegger, Karolina; Fischer, Roman; Steemann, Franz Xaver; Unterluggauer, Hermann; Masselter, Sonja

    2015-05-01

    The approach for pesticide residue analysis in food of animal origin differs strongly from the one established for food of plant origin, as laboratories mainly focus on conventional methods for the analysis of non-polar pesticides known to accumulate in fatty tissues. However, these group-specific methods are very laborious and cost intensive and typically require extraction of fat components followed by extensive clean-up steps to remove matrix constituents. This work highlights the development and validation of a straightforward QuEChERS-derived clean-up procedure enabling facile, precise, and reliable identification and quantitation of pesticide residues in food of animal origin, which can be extended to various other commodities with moderate fat content and applied to replace traditional group-specific methods. Two additional methods for lean and highly fatty commodities complete this well-established "simplified modular system". The proposed method was in-house validated in terms of accuracy and precision, recovery and linearity as well as specificity and sensitivity on two representative commodities for food of animal origin (egg and meat). For the majority of the more than 80 pesticides investigated, satisfactory results were obtained. Procedural matrix calibration was applied for screening purposes in conjunction with GC-MS/MS or LC-MS/MS as integral part of the approach. Apparent recoveries for most of the compounds ranged from 70 to 120 % (RSD < 20%) at spiking levels of 0.01 (LOQ level) and 0.05 mg/kg. Accuracy of the method has been demonstrated by application to reference material from previous EU proficiency tests. Only in case of positive screening results a standard addition approach was applied for precise quantitation. PMID:25772564

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

    PubMed Central

    Rooseboom, Astrid; van Dam, Ruud; Roding, Marleen; Arondeus, Karin; Sunarto, Suryati

    2007-01-01

    The ethyl acetate-based multi-residue method for determination of pesticide residues in produce has been modified for gas chromatographic (GC) analysis by implementation of dispersive solid-phase extraction (using primary–secondary amine and graphitized carbon black) and large-volume (20 μL) injection. The same extract, before clean-up and after a change of solvent, was also analyzed by liquid chromatography with tandem mass spectrometry (LC–MS–MS). All aspects related to sample preparation were re-assessed with regard to ease and speed of the analysis. The principle of the extraction procedure (solvent, salt) was not changed, to avoid the possibility invalidating data acquired over past decades. The modifications were made with techniques currently commonly applied in routine laboratories, GC–MS and LC–MS–MS, in mind. The modified method enables processing (from homogenization until final extracts for both GC and LC) of 30 samples per eight hours per person. Limits of quantification (LOQs) of 0.01 mg kg−1 were achieved with both GC–MS (full-scan acquisition, 10 mg matrix equivalent injected) and LC–MS–MS (2 mg injected) for most of the pesticides. Validation data for 341 pesticides and degradation products are presented. A compilation of analytical quality-control data for pesticides routinely analyzed by GC–MS (135 compounds) and LC–MS–MS (136 compounds) in over 100 different matrices, obtained over a period of 15 months, are also presented and discussed. At the 0.05 mg kg−1 level acceptable recoveries were obtained for 93% (GC–MS) and 92% (LC–MS–MS) of pesticide–matrix combinations. PMID:17563885

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

    PubMed Central

    Chowdhury, Md. Alamgir Zaman; Banik, Sanjoy; Uddin, Borhan; Moniruzzaman, Mohammed; Karim, Nurul; Gan, Siew Hua

    2012-01-01

    Several types of organophosphorous and carbamate pesticides have been used extensively by the farmers in Bangladesh during the last few decades. Twenty seven water samples collected from both paddy and vegetable fields in the Savar and Dhamrai Upazilas in Bangladesh were analyzed to determine the occurrence and distribution of organo-phosphorus (chlorpyrifos, malathion and diazinon) and carbamate (carbaryl and carbofuran) pesticide residues. A high performance liquid chromatograph instrument equipped with a photodiode array detector was used to determine the concentrations of these pesticide residues. Diazinon and carbofuran were detected in water samples collected from Savar Upazila at 0.9 μg/L and 198.7 μg/L, respectively. Malathion was also detected in a single water sample at 105.2 μg/L from Dhamrai Upazila. Carbaryl was the most common pesticide detected in Dhamrai Upazila at 14.1 and 18.1 μg/L, while another water sample from Dhamrai Upazila was contaminated with carbofuran at 105.2 μg/L. Chlorpyrifos was not detected in any sample. Overall, the pesticide residues detected were well above the maximum acceptable levels of total and individual pesticide contamination, at 0.5 and 0.1 μg/L, respectively, in water samples recommended by the European Economic Community (Directive 98/83/EC). The presence of these pesticide residues may be attributed by their intense use by the farmers living in these areas. Proper handling of these pesticides should be ensured to avoid direct or indirect exposure to these pesticides. PMID:23202689

  3. 76 FR 33183 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-06-08

    ... CFR 174.532; March 16, 2011; 76 FR 14289 (FRL-8866- 5) when Bacillus thuringiensis eCry3.1Ab protein... tolerance for residues of the plant-incorporated protectant, Bacillus thuringiensis eCry3.1Ab protein...

  4. 78 FR 79359 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-12-30

    ... at 0.1 ppm. Per the Federal Register of October 10, 2007 (72 FR 57492) (FRL-8149-9) supported by Data... accordance with procedures set forth in 40 CFR part 2. 2. Tips for preparing your comments. When submitting... monitoring of food with residues at or above the levels set or proposed in the tolerances. The...

  5. 75 FR 57942 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-09-23

    ... developed and used to quantitate residues of oxytetracycline by using liquid chromatography mass...,4,2-dioxazin-3-yl)methanone O- methyloxime, in or on raw agricultural commodities listed under crop... chromatography/mass spectroscopy/mass spectrometry (HPLC/MS/MS) detection is available for enforcement...

  6. 76 FR 36479 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-06-22

    ... petition was previously announced in the Federal Register of August 11, 2010 (75 FR 48667) (FRL-8840-6... 40 CFR part 180 for residues of the insecticide thiamethoxam, (3-[(2-chloro-5- thiazolyl) methyl... for detecting and measuring levels of thiamethoxam in or on raw agricultural commodities. This...

  7. 75 FR 14154 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-03-24

    ... CFR part 180 for residues of the herbicide glyphosate, N-(phosphonomethyl) glycine, in or on corn... glyphosate and its metabolite AMPA in or on plant and livestock commodities. These methods include: Gas... glyphosate. Contact: Erik Kraft, (703) 308-9358; e-mail address: kraft.erik@epa.gov . 5. PP 9F7657....

  8. DETERMINATION OF PYRETHROID PESTICIDE RESIDUES FROM RAT TISSUE USING TWO-DIMENSIONAL LCMS

    EPA Science Inventory

    Pyrethroids are a synthetic class of pesticides that elicit neurobehavioral effects in mammals. They are applied occupationally and residentially creating the potential for human exposure. Determining relationships between parent pyrethroid tissue concentrations and neurotoxic ...

  9. 75 FR 9596 - Notice of Filing of a Pesticide Petition for Residues of a Aspergillus flavus AF36 on Corn Food...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-03-03

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

  10. Chronic dietary exposure to pesticide residues and associated risk in the French ELFE cohort of pregnant women.

    PubMed

    de Gavelle, Erwan; de Lauzon-Guillain, Blandine; Charles, Marie-Aline; Chevrier, Cécile; Hulin, Marion; Sirot, Véronique; Merlo, Mathilde; Nougadère, Alexandre

    2016-01-01

    Dietary exposure to pesticide residues may present a risk to public health, especially for sensitive populations such as pregnant women. To characterize this risk, this study assessed chronic dietary exposure to pesticide residues based on the French ELFE cohort. A self-administered food frequency questionnaire (FFQ) about the last three months of pregnancy filled in by pregnant women in 2011 was used in combination with occurrence data from French Total Diet Studies completed by the results of national monitoring programs on pesticide residues in food. The dietary intake of pesticides (μg/kg of body weight/day) was estimated for 14,099 pregnant women with a complete FFQ, for 317 substances under two occurrence scenarios to handle left-censored data: a lower-bound scenario (LB), where undetected results were set to zero, and an upper-bound scenario (UB), where undetected results were set to the detection limit if the substance was expected to be found in food and zero if it was not. The risk was assessed for 284 substances with a toxicological reference value (TRV) and a good coverage level of the diet potentially contributing to pesticide intake. The cumulative risk was also assessed for seven effects on nervous and thyroid systems using the hazard index and the Cumulative Assessment Groups defined by EFSA. Substances with the highest exposure levels under the LB scenario were, in decreasing order, imazalil, piperonyl butoxide, chlorpropham, thiabendazole, iprodione and propargite. Under the LB scenario, only for lindane did women have a statistically significant probability of exceeding the TRV (2.4%). Under the UB scenario, risk could not be excluded for nine other substances. A better management of left-censored data and more sensitive analyses of the main food contributors might help to refine the UB exposure and risk assessments. A statistically significant cumulative risk was found for neurochemical effects related to high intake levels of three

  11. Influence of different planting seasons of six leaf vegetables on residues of five pesticides.

    PubMed

    Fan, Sufang; Deng, Kailin; Yu, Chuanshan; Zhao, Pengyue; Bai, Aijuan; Li, Yanjie; Pan, Canping; Li, Xuesheng

    2013-09-25

    To investigate the influence of different planting seasons on the dissipation of pesticides, field experiments of thiophanate-methyl, metalaxyl, fluazifop-P-butyl, chlorpyrifos, and λ-cyhalothrin on six crops including pakchoi, rape, crown daisy, amaranth, spinach, and lettuce were designed and conducted. In this study, a high-performance liquid chromatography and electrospray ionization-tandem mass spectrometer with multiple reaction monitoring was used to simultaneously determine thiophanate-methyl and its metabolite carbendazim, metalaxyl, and fluazifop-P-butyl in various samples; gas chromatography with an electron capture detector was used to detect chlorpyrifos and λ-cyhalothrin. The limits of quantitation (LOQs) of these six pesticides were in the range of 0.001-0.01 mg kg(-1) for all samples, and the average recoveries of all pesticides ranged from 60.1 to 119.1% at 0.01 and 0.1 mg kg(-1) spiked levels. The relative standard deviation (RSD) ranged from 1.1 to 13.9%. All maximal concentrations of the six pesticides in six leaf vegetables in autumn were higher than in summer in Beijing. For most pesticides half-lives in autumn were longer than in summer. The results showed that the initial concentration, maximal concentration, and half-lives of pesticides were influenced not only by environmental factors such as light, heat, moisture, and rainy climate but also by plant matrices. PMID:23978278

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

    PubMed

    Oellig, Claudia

    2016-05-01

    Propolis is a very complex mixture of substances that is produced by honey bees and is known to be a rather challenging matrix for residue analysis. Besides resins, flavonoids and phenols, high amount of wax is co-extracted resulting in immense matrix effects. Therefore a suitable clean-up is crucial and indispensable. In this study, a reliable solid phase extraction (SPE) clean-up was developed for pesticide residue analysis in propolis. The clean-up success was quickly and easily monitored by high-performance thin-layer chromatography with different detection possibilities. The final method consists of the extraction of propolis with acetonitrile according to the QuEChERS method followed by an effective extract purification on dual-layer SPE cartridges with spherical hydrophobic polystyrene-divinylbenzene resin/primary secondary amine as sorbent and a mixture of toluene/acetone (95:5, v/v) for elution. Besides fat-soluble components like waxes, flavonoids, and terpenoids, more polar compounds like organic acids, fatty acids, sugars and anthocyanins were also removed to large extent. Method performance was assessed by recovery experiments at spiking levels of 0.5 and 1mg/kg (n=5) for fourteen pesticides that are relevant for propolis. Mean recoveries determined by HPLC-MS against solvent standards were between 40 and 101%, while calculation against matrix-matched standards provided recoveries of 79-104%. Precision of recovery, assessed by relative standard deviations, were below 9%. Thus, the developed dual-layer SPE clean-up enables the reliable pesticide residue analysis in propolis and provides a suitable alternative to time-consuming clean-up procedures proposed in literature. PMID:27059398

  13. 78 FR 13295 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-02-27

    ... isomer, (1Z)-[2-[[6-(2-chlorophenoxy)-5-fluoro- 4-pyrimidinyl]oxy]phenyl](5,6-dihydro-1,4,2-dioxazin-3-yl...-isomers is summed to give total residue. Contact: Heather Garvie, (703) 308-0034, email address: garvie... isomer, (1Z)-[2-[[6- (2-chlorophenoxy)-5-fluoro-4-pyrimidinyl]oxy]phenyl](5,6-dihydro-1,4,2-...

  14. Development and validation of a cellular biosensor detecting pesticide residues in tomatoes.

    PubMed

    Flampouri, Kelly; Mavrikou, Sophie; Kintzios, Spiridon; Miliadis, George; Aplada-Sarlis, Pipina

    2010-03-15

    Two of the most important categories of pesticides used in agricultural practice are organophosphates and dithiocarbamates. Their extensive and inappropriate use has rendered their reliable monitoring at trace levels more and more necessary. This study presents the construction of a rapid and sensitive cellular biosensor test based on the measurement of changes of the cell membrane potential of immobilized cells, according to the working principle of the Bioelectric Recognition Assay (BERA). The cells were immobilized by entrapment in a sodium alginate bead and directly applied in different pesticide dilutions and agricultural samples. The pesticides used were the organophosphate insecticide diazinon and the dithiocarbamate fungicide propineb. Two different cell types, N2a (neuroblastoma) and Vero (fibroblast) were used as the biosensory elements in order to investigate their differential response against the pesticides. In this way, we hoped to increase the selectivity of the assay. Based on the observed patterns of response, we demonstrate that the sensor can be used for the qualitative and, in some concentrations, quantitative detection of the pesticides with a high degree of reproducibility. The lowest detected concentration was 3nM. Finally, for the investigation of the effects of different pesticides on the accumulation of cytosolic Ca(2+), we conducted a fluorescent assay on N2a cells treated with tomato sample extracts, which were replicates of the E.U. proficiency test sample. The tomato samples were either organically grown or contained 14 different pesticides. The experimental results showed a higher increase of the intracellular Ca(2+) concentration in cells treated with non-organic samples compared to the cells treated with organic samples. PMID:20152413

  15. The interaction between natural organic matter in raw waters and pesticide residues: a three dimensional excitation-emission matrix (3DEEM) fluorescence investigation.

    PubMed

    Beale, David J; Porter, Nichola A; Roddick, Felicity A

    2013-01-01

    This paper examines the interaction between dissolved natural organic matter and pesticide residues, both of which are found in raw water sources, using three dimensional excitation-emission matrix (3DEEM) fluorescence spectroscopy. It was observed that pesticide residue at 0.1 mg L(-1) formed a complex with humic-like fluorophores that are commonly found in raw water samples. Applying 3DEEM fluorescence to investigate the humic fractions, it was found that identification of changes in water sources was possible, and, importantly, the presence of a number of pesticides was able to be determined. In addition, the formation of this complex, and the influence of soluble cations and anions upon it, was shown to impact the efficiency of analytical extraction procedures for pesticides; however, 3DEEM fluorescence could be an approach to account for such losses. PMID:23752373

  16. Dual-layer solid-phase extraction based on molecular imprinting technology: Seeking a route to enhance selectivity for trace analysis of pesticide residues in olive oil.

    PubMed

    Garcia, Raquel; Carreiro, Elisabete P; Nunes, José; da Silva, Marco Gomes; Freitas, Ana Maria Costa; Burke, Anthony J; Cabrita, Maria João

    2016-07-01

    Aiming to introduce a multiresidue analysis for the trace detection of pesticide residues belonging to organophosphorus and triazine classes from olive oil samples, a new sample preparation methodology comprising the use of a dual layer of "tailor-made" molecularly imprinted polymers (MIPs) SPE for the simultaneous extraction of both pesticides in a single procedure has been attempted. This work has focused on the implementation of a dual MIP-layer SPE procedure (DL-MISPE) encompassing the use of two MIP layers as specific sorbents. In order to achieve higher recovery rates, the amount of MIP layers has been optimized as well as the influence of MIP packaging order. The optimized DL-MISPE approach has been used in the preconcentration of spiked organic olive oil samples with concentrations of dimethoate and terbuthylazine similar to the maximum residue limits and further quantification by HPLC. High recovery rates for dimethoate (95%) and terbuthylazine (94%) have been achieved with good accuracy and precision. Overall, this work constitutes the first attempt on the development of a dual pesticide residue methodology for the trace analysis of pesticide residues based on molecular imprinting technology. Thus, DL-MISPE constitutes a reliable, robust, and sensitive sample preparation methodology that enables preconcentration of the target pesticides in complex olive oil samples, even at levels similar to the maximum residue limits enforced by the legislation. PMID:27062483

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

    PubMed

    Wu, Yan; Jiang, Bing; Xu, Yigang; Zhao, Wei; Meng, Xiangrui; Zhou, Yuan; Yu, Jiahui; Zu, Yuangang

    2015-03-01

    A sensitive and convenient liquid chromatography-tandem mass spectrometric method was developed for the determination of 16 pesticides such as imidacloprid, prochloraz, difenoconazole, azoxystrobin, and thiamethoxam in fruits and vegetables. After compared with methanol and acetone-cyclohexane (1:2, v/v), acetonitrile was chosen as the extraction solvent. The samples were extracted by acetonitrile in high-speed homogenization. The extraction solution was cleaned up by liquid-liquid extraction, and the supernatant was collected. In this work, QuEChERS exhibited much higher efficiency than Carbon-NH2 solid-phase extraction in purification. The pigments and organic acids were removed by purge line (150 mg primary secondary amine (PSA) sorbent and 900 mg absolute magnesium sulfate), leading to the decrease of the background interferences. The average recoveries of the 16 pesticides were almost in the range of 75%-111% at the three spiked levels, and the relative standard deviations were less than 16%. The qualitative analysis and quantitative analysis were investigated by LC-MS/MS and matrix-matched calibration curves. The results showed that the method of QuEChERS combined with LC-MS/MS is rapid, accurate and sensitive for the determination of the 16 pesticide residues in fruits and vegetables. PMID:26182463

  18. Persistent organic pesticide residues in sediments of Vasai Creek near Mumbai: Assessment of sources and potential ecological risk.

    PubMed

    Singare, Pravin U

    2015-11-15

    Thirteen persistent organic pesticides were investigated in the sediments of Vasai Creek near Mumbai to evaluate their pollution levels and potential risks. It was observed that ΣOCPs level was in the range of 597-1538ng/g dw, with an average value of 1115.25ng/g dw. The level of ΣOPPs was in the range of 492-1034ng/g dw, with an average value of 798.15ng/g dw. The values o,p'-DDT/p,p'-DDT ratio gives an indication of use of technical DDT as the prime source of DDT, while the α/γ-BHC ratio indicate that BHCs in study area might have been received from fresh lindane. The results of an ecological risk assessment showed that sediment bound organic pesticides are of more ecotoxicological concern as they might create adverse ecological risk to the marine breeding habitats. These pesticides residues may get remobilize and released to overlying waters creating adverse effects on terrestrial and aquatic organisms. PMID:26428625

  19. Analysis of pesticide residues on museum objects repatriated to the Hupa tribe of California.

    PubMed

    Palmer, Peter T; Martin, Matthew; Wentworth, Gregory; Caldararo, Niccolo; Davis, Lee; Kane, Shawn; Hostler, David

    2003-03-15

    In the past, it was common practice for museum professionals and private collectors to apply a variety of pesticide agents to objects in their collections to preserve them from depredations by microorganisms, fungi, and other pests. The Native American Graves Repatriation and Protection Act allows federally recognized tribes to request that museums return objects taken from their ancestors. Given that poor records were kept on the treatment of individual objects, it is unknown whether specific objects are contaminated with these pesticide agents. Although chemical analysis represents the only reliable means to determine the types and levels of pesticides on these objects, surprisingly few publications document the extent of this contamination in museum collections. This paper reports on the determination of arsenic, mercury, and several organic pesticides on 17 objects that were recently repatriated to the Hupa tribe in northern California. Four samples were taken from each object: two for arsenic and mercury analysis via flame atomic absorption spectrophotometry and two for organic pesticide analysis via gas chromatography/mass spectrometry. Percent levels (wt/wt) of mercury were detected on many samples, and 0.001 to 0.183% (wt/wt) levels of p-dichlorobenzene, naphthalene, thymol, lindane, and/or DDT were detected on many of the samples. These results indicate that Hupa tribal members should not wear these objects in religious ceremonies, proper precautions should be followed when dealing with potentially contaminated objects, and that more serious consideration should be given to this issue at a national level. PMID:12680658

  20. Evaluation of the QuEChERS method and gas chromatography-mass spectrometry for the analysis pesticide residues in water and sediment.

    PubMed

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

    2011-01-01

    A method for the determination of pesticide residues in water and sediment was developed using the QuEChERS method followed by gas chromatography--mass spectrometry. The method was validated in terms of accuracy, specificity, linearity, detection and quantification limits. The recovery percentages obtained for the pesticides in water at different concentrations ranged from 63 to 116%, with relative standard deviations below 12%. The corresponding results from the sediment ranged from 48 to 115% with relative standard deviations below 16%. The limits of detection for the pesticides in water and sediment were below 0.003 mg L⁻¹ and 0.02 mg kg⁻¹, respectively. PMID:21165598

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

    PubMed

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

    2014-01-01

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

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

    PubMed

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

    2015-10-01

    A method for rapid screening and confirmation of 205 pesticide residues in rice was developed by combining QuEChERS and high performance liquid chromatography-triple quadrupole-linear ion trap mass spectrometry (LC-Q-TRAP/MS). The rice samples were extracted with acetonitrile, and then cleaned up with primary secondary amine (PSA), anhydrous magnesium sulfate (MgSO4) and C18 adsorbent. Finally, the samples were detected by LC-Q-TRAP/MS in multiple reaction monitoring with information-dependent acquisition of enhanced product ion (MRM-IDA-EPI) mode followed with database searching. A total of 205 pesticide residues were confirmed by retention times, ion pairs and the database searching using EPI library, and quantified by external standard method. All the pesticides showed good linearities with linear correlation coefficients all above 0.995. The limits of quantification (LOQs) for the 205 pesticides were 0.5-10.0 μg/kg. The average recoveries of the 205 pesticides ranged from 62.4% to 127.1% with the relative standard deviations (RSDs) of 1.0% - 20.0% at spiked levels of 10 μg/kg and 50 μg/kg, and only 20 min were needed for the analysis of an actual rice sample. In brief, the method is fast, accurate and highly sensitive, and is suitable for the screening and confirmation of pesticide residues in rice. PMID:26930966

  3. Enhanced Dissipation of Triazole and Multiclass Pesticide Residues on Grapes after Foliar Application of Grapevine-Associated Bacillus Species.

    PubMed

    Salunkhe, Varsha P; Sawant, Indu S; Banerjee, Kaushik; Wadkar, Pallavi N; Sawant, Sanjay D

    2015-12-23

    Disease management in vineyards with fungicides sometimes results in undesirable residue accumulations in grapes at harvest. Bioaugmentation of the grape fructosphere can be a useful approach for enhancing the degradation rate and reducing the residues to safe levels. This paper reports the in vitro and in vivo biodegradation of three triazole fungicides commonly used in Indian vineyards, by Bacillus strains, namely, DR-39, CS-126, TL-171, and TS-204, which were earlier found to enhance the dissipation rate of profenophos and carbendazim. The strains utilized the triazoles as carbon source and enhanced their in vitro rate of degradation. Myclobutanil, tetraconazole, and flusilazole were applied in separate vineyard plots at field doses of 0.40 g L(-1), 0.75 mL L(-1), and 0.125 mL L(-1), respectively. Residue analysis of field samples from the treated fields reflected 87.38 and >99% degradations of myclobutanil and tetraconazole, respectively, by the strain DR-39, and 90.82% degradation of flusilazole by the strain CS-126 after 15-20 days of treatment. In the respective controls, the corresponding percent degradations were 72.07, 58.88, and 54.28, respectively. These Bacillus strains could also simultaneously degrade the residues of profenofos, carbendazim, and tetraconazole on the grape berries and can be useful in multiclass pesticide residue biodegradation. PMID:26492206

  4. Mobilization of soil bound residue of organochlorine pesticides and polycyclic aromatic hydrocarbons in an in-vitro gastrointestinal model

    PubMed Central

    TAO, SHU; LI, LI; DING, JUNNAN; ZHONG, JUNJUN; ZHANG, DIYU; LU, YAN; YANG, YIFENG; WANG, XILONG; LI, XIQING; CAO, JUN; LU, XIAOXIA; LIU, WENXIN

    2011-01-01

    A previous study on mobilization of organochlorine pesticides (OCPs) in contaminated soils from the field revealed that the total amount of OCPs measured in digestive fluid and chyme of an in-vitro gastrointestinal model was higher than the quantity directly extracted using a solvent extraction without digestion, providing a clue that the bound residue of OCPs might be mobilized. This hypothesis was tested in this study for both OCPs and polycyclic aromatic hydrocarbons (PAHs). Three contaminated surface soil samples with different organic carbon (OC) contents were collected from the field, and extracted with a solvent with and without digestion in an in-vitro gastrointestinal model. It was found that bound residues of OCPs and PAHs were mobilized to a certain extent during digestion. The ratios of the mobilized bound residues over the total quantities extracted after digestion (Rb) varied from 0 to 0.96 for individual compounds. The Rb was positively correlated with OC content. Among the five constitutes of digestive juice, bile salt was the only one that served to mobilize the bound residues and the extractability of bile salt was constant over a concentration range from 2 to 20 mg/mL. The mobilization process followed typical first-order kinetics. The calculated rate constants suggest that mobilization was fast and 90% of extracted bound residues of OCPs and PAHs were mobilized within 2.4 and 4.8 h, respectively. PMID:21175124

  5. Multi-residue analysis of pesticides in traditional Chinese medicines using gas chromatography-negative chemical ionisation tandem mass spectrometry.

    PubMed

    Nie, Jing; Miao, Shui; Lehotay, Steven J; Li, Wen-Ting; Zhou, Heng; Mao, Xiu-Hong; Lu, Ji-Wei; Lan, Lan; Ji, Shen

    2015-01-01

    In this study, a residue analysis method for the simultaneous determination of 107 pesticides in traditional Chinese medicines (TCMs), Angelica sinensis, A. dahurica, Leonurus heterophyllus Sweet, Pogostemon cablin and Lonicera japonica Thunb., was developed using gas chromatography coupled with tandem mass spectrometry in negative chemical ionisation mode (GC-NCI-MS/MS). NCI has advantages of high sensitivity and selectivity to chemicals with electron-withdrawing groups, and yields low background interference. For sample preparation, QuEChERS (quick, easy, cheap, effective, rugged and safe) was applied. Due to the unique characteristics of TCMs, the clean-up step was optimised by adjusting amounts of primary secondary amine, C18, graphitised carbon black and silica sorbents. Validation was mainly performed by determining analyte recoveries at four different spiking concentrations of 10, 50, 100 and 200 ng g(-1), with seven replicates at each concentration. Method trueness, precision, linearity of calibration curves, lowest calibrated levels (LCLs) and matrix effects were determined to demonstrate method and instrument performance. Among the 107 pesticides tested, approximately 80% gave recoveries from 80% to 110% and < 10% relative standard deviation (RSD). The LCLs for nearly all pesticides were 5 ng g(-1), and as low as 0.1 ng g(-1) for dichlofenthion, endosulfan sulphate, flumetralin, isofenphos-methyl, methyl-pentachlorophenyl sulphide and trifluralin. The results indicate that GC-NCI-MS/MS is an excellent technique for quantitative and qualitative analysis of targeted GC-amenable pesticides at ultra-trace levels, especially in complex matrices such as TCMs. PMID:26125677

  6. Comparison of pesticide residues in surface water and ground water of agriculture intensive areas

    PubMed Central

    2014-01-01

    The organochlorines (OClPs) and organophosphates (OPPs) pesticides in surface and ground water having intensive agriculture activity were investigated to evaluate their potential pollution and risks on human health. As per USEPA 8081 B method, liquid-liquid extraction followed by Gas-Chromatographic technique with electron capture detector and mass selective detector (GC-MS) were used for monitoring of pesticides. Among organochlorines, α,β,γ,δ HCH’s, aldrin, dicofol, DDT and its derivatives, α,β endosulphan’s and endosulphan-sulphate were analysed; dichlorovos, ethion, parathion-methyl, phorate, chlorpyrifos and profenofos were determined among organophosphates. As compared to ground water, higher concentrations of OClPs and OPPs were found in surface water. Throughout the monitoring study, α - HCH (0.39 μg/L in Amravati region),α - endosulphan (0.78 μg/L in Yavatmal region), chlorpyrifos (0.25 μg/L in Bhandara region) and parathion-methyl (0.09 μg/L in Amravati region) are frequently found pesticide in ground water, whereas α,β,γ-HCH (0.39 μg/L in Amravati region), α,β - endosulphan (0.42 μg/L in Amravati region), dichlorovos (0.25 μg/L in Yavatmal region), parathion-methyl (0.42 μg/L in Bhandara region), phorate (0.33 μg/L in Yavatmal region) were found in surface water. Surface water was found to be more contaminated than ground water with more number of and more concentrated pesticides. Among pesticides water samples are found to be more contaminated by organophosphate than organochlorine. Pesticides in the surface water samples from Bhandara and Yavatmal region exceeded the EU (European Union) limit of 1.0 μg/L (sum of pesticide levels in surface water) but were within the WHO guidelines for individual pesticides. PMID:24398360

  7. Organochlorine pesticide and polychlorinated biphenyl residues in human milk from Rome (Italy) and surroundings

    SciTech Connect

    Dommarco, R.; Muccio, A.D.; Camoni, I.; Gigli, B.

    1987-12-01

    Organochlorine (OC) pesticides and polychlorinated biphenyls (PCBs) in human milk have been the subject of many studies. Surveys carried out in Italy are all eight years old with the exception of the latest work. Because of recent improvements in analytical methodology, the authors believe an up-to-date study would provide additional information. Thus, this paper presents a survey of the levels of human milk contamination, in Rome and surroundings, by organochlorine pesticides and PCBs. This survey is a part of a larger monitoring program covering also geographical areas outside of Rome.

  8. Organochlorine pesticide residues in different Indian cereals, pulses, spices, vegetables, fruits, milk, butter, Deshi ghee, and edible oils.

    PubMed

    Kaphalia, B S; Takroo, R; Mehrotra, S; Nigam, U; Seth, T D

    1990-01-01

    A total of 244 samples of cereals (wheat flour, rice, and maize), pulses (arhar, moong, gram, lentil, and black gram), spices (turmeric, chili, coriander, and black pepper), vegetables (potato, onion, spinach, cabbage, brinjal, and tomato), fruits (mango, guava, apple, and grape), milk, butter, Deshi ghee, and edible oils (vegetable, mustard, groundnut, and sesame) collected from different cities of Northern Province (Utter Pradesh) were analyzed by gas liquid chromatography for the presence of organochlorine pesticide residues. Residues of hexachlorocyclohexane (HCH) and 2,2-bis(p-chlorophenyl)-1,1,1-trichloroethane (DDT) were detected in about 85% of the total samples of cereals, spices, milk, butter, Deshi ghee, and edible oils analyzed in the present study. However, the residue levels were either very small (less than 0.06 ppm) or not detected at all in pulses, vegetables, and fruits as compared with very high concentrations in wheat flour (4.42 and 0.12 ppm), butter (1.19 and 4.85 ppm), mustard oil (1.26 and 2.42 ppm), Deshi ghee (1.10 and 3.84 ppm), vegetable oil (1.02 and 0.59 ppm), groundnut oil (0.51 and 1.49 ppm), and chili (0.48 and 1.92 ppm). The levels of HCH and DDT residues detected in rice, maize, turmeric, corlander, black pepper, and all the vegetables and fruits were also lower than those found in wheat flour, oil, and fat samples analyzed in the present study. These findings suggest that a restricted and controlled use of such persistent pesticides may be useful for decreasing their contamination levels in different food items. PMID:1698760

  9. QuEChERS Adaptability for the Analysis of Pesticide Residues in Beehive Products Seeking the Development of an Agroecosystem Sustainability Monitor.

    PubMed

    Niell, Silvina; Jesús, Florencia; Pérez, Cecilia; Mendoza, Yamandú; Díaz, Rosana; Franco, Jorge; Cesio, Verónica; Heinzen, Horacio

    2015-05-13

    Beehive products could be powerful monitors of pesticide residues originating in agroecosystems during production cycles. Their ready availability provides enough samples to perform analytical determinations, but their chemical complexity makes residue analysis a real challenge. Taking advantage of the plasticity of QuEChERS coupled to LC-MS/MS, validated methodologies were developed for bees, honey, beeswax, and pollen and applied to real samples for the simultaneous determination of 19 of the most employed pesticides in intensive cropping fields. Beehives placed in Uruguayan agroecosystems accumulated the pesticides thiacloprid, imidacloprid, methomyl, carbaryl, hexythiazox, azoxystrobin, pyraclostrobin, tebuconazole, and haloxyfop-methyl at 0.0001-0.01 mg/kg levels. The oscillations on the amount and occurrence of residue findings for specific apiaries were correlated statistically with the sampling season and the agroecosystem where the beehives were located, showing the potential of bees and bee products to record relevant information to survey the chemicals applied in their surroundings. PMID:25880394

  10. Simultaneous multi-determination and transfer of eight pesticide residues from green tea leaves to infusion using gas chromatography.

    PubMed

    Cho, Soon-Kil; Abd El-Aty, A M; Rahman, Md Musfiqur; Choi, Jeong-Heui; Shim, Jae-Han

    2014-12-15

    A method for determining eight pesticide (cyhalothrin, flufenoxuron, fenitrothion, EPN, bifenthrin, difenoconazole, triflumizole, and azoxystrobin) residues in made green tea as well as a tea infusion (under various brewing water temperatures; 60, 80, and 100°C) using gas chromatography (GC) micro-electron capture detector (μECD) was developed and validated. The extraction method adopted the relatively commonly used approach of solid sample hydration, with the green tea hydrated before being extracted through salting out with acetonitrile followed by a cleanup procedure. The analytes were confirmed using GC-coupled to tandem mass spectrometry (GC/MS/MS) with a triple quadrupole. The linearity of the calibration curves yielded determination coefficients (R(2)) >0.995. Recoveries were carried out using blank samples spiked with all analytes at two levels. The results demonstrated that all pesticides were recovered within the range of 77-116% with a relative standard deviation (RSD) ⩽14%. The quantification limits of 0.015-0.03 mg/kg were lower than the maximum residue limits (MRLs) set by the Korea Food and Drug Administration (KFDA) for all analytes (0.05-10mg/kg). The infusion study indicated that cyhalothrin, flufenoxuron, and bifenthrin did not infuse into the tea brew from the made tea. Increases in brewing time resulted in increased transfer of azoxystrobin, fenitrothion, and difenoconazole from the made tea to the brew; however, this was not the case with triflumizole or EPN. We conclude that transfer of pesticides appeared to be dependent on their water solubilities and drinking a cup of tea is recommended to be at a water temperature of 60°C. PMID:25038708

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

    PubMed

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

    2012-07-01

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

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

    NASA Astrophysics Data System (ADS)

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

    This monitoring study of 40 samples of cow's milk collected from different locations at Gharbia Governorate during the four different seasons of the years 2005-2006, was conducted to determine the contamination levels of seven pesticide residues including four organophosphorus (chlorpyrifos, diazinon, dimethoate and malathion) and three synthetic pyrethroides (cypermethrin, deltamethrin and fenvelerate), as well as five heavy metals (copper, iron, cadmium, zinc and lead). The results showed that there were no contamination with investigated pesticide residues found in all analyzed samples, except for malathion, which was detected in a single sample with a negligible existence (0.018 mg kg-1), by ratio of (0.02%) of all samples. In relation to heavy metals detection, data revealed that all milk samples were contaminated with heavy metals all year around. The contamination with heavy metals was generally dominated at summer season. Level of lead was higher than other metals. The mean levels of Cu, Fe, Cd, Zn and Pb were 0.251, 0.607, 0.159, 0.371 and 2.462 mg kg-1, respectively. Cu, Fe and Zn level were under the permissible limits, while the Cd and Pb were exceeded the permissible limits, indicating serious heavy metals pollution in the region.

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  14. ANALYTICAL METHODS FOR A NATIONAL STUDY OF CHEMICAL RESIDUES IN FISH - II. PESTICIDES AND POLYCHLORINATED BIPHENYLS

    EPA Science Inventory

    Analytical methods and a quality assurance plan have been developed to determine the concentration of a select group of bioaccumulatable chemicals in fish tissue. he analytes include PCBs and 21 pesticides and industrial chemicals. he methodology has been used to conduct a survey...

  15. Assessing the distribution and human health risk of organochlorine pesticide residues in sediments from selected rivers.

    PubMed

    Ogbeide, Ozekeke; Tongo, Isioma; Ezemonye, Lawrence

    2016-02-01

    Sediment samples from major agricultural producing areas in Edo state Nigeria were analysed for α-HCH, γ-HCH, β-HCH and ∑DDT with the aim of elucidating contamination profiles, distribution characteristics, carcinogenic and non-carcinogenic risk of these compounds in these regions. Analysis was done using a gas chromatography (GC) equipped with electron capture detector (ECD), while health risk assessment was carried out using the Incremental Lifetime Cancer Risk (ILCR) and the chronic daily intake (CDI). Results showed varying concentrations of α-HCH, γ-HCH, β-HCH and ∑DDT pesticides in sediment samples with hexachlorocyclohexane (∑HCHs) (4.6 µg/g/dw) being the dominant contaminants as it was widely detected in all samples and stations. Source identification revealed that the current levels of HCHs and DDT in sediments were attributed to both historical use and fresh usage of these pesticides. Risk estimates using ILCR and CDI showed that the risk of cancer and non-cancer effects was highest when exposure route was through ingestion. Furthermore, model projections highlights children as high risk population groups for non-dietary exposure to OCPs. These findings suggests the need for increased monitoring programmes, with a wider scope for both currently used pesticides and legacy/banned pesticides. PMID:26476770

  16. Are pesticide residues associated to rice production affecting oyster production in Delta del Ebro, NE Spain?

    PubMed

    Ochoa, Victoria; Riva, Carmen; Faria, Melissa; Köck-Schulmeyer, Marianne; de Alda, Miren López; Barceló, Damià; Fernandez Tejedor, Margarita; Roque, Ana; Ginebreda, Antoni; Barata, Carlos

    2012-10-15

    Pesticide usage in Delta del Ebro (NE Spain) during the rice growing season has been associated with oyster episodes of mortality that occur early in summer. However, there are no studies that have directly evaluated pesticide levels and effects in oysters (Crassotrea gigas) cultured in Ebro's Bays. In this study pesticide levels in water, metal body burdens and up to 12 different biochemical markers were monitored in gills and digestive glands of oysters transplanted from May to June in 2008 and 2009. Biochemical responses evidenced clear differences in oysters from 2008 and 2009. Oysters transplanted in 2009 showed their antioxidant defenses unaffected from May to June and consequently increased levels of tissue damage measured as lipid peroxidation and DNA strand breaks and of mortality rates. Conversely oysters transplanted in 2008 increase their antioxidant defenses from May to June, had low levels of lipid peroxidation and DNA damage and low mortality rates. Some pesticides in water such as bentazone and propanil together with high temperatures and salinity levels were related with tissue damage in oyster transplanted in 2008 but the observed large differences between years indicate that abiotic factors alone could not explain the high mortalities observed in 2009. An analysis of recent reported studies pointed out in the direction that in addition to abiotic factors the use of oysters sensitive to diseases may explain the observed responses. PMID:22940045

  17. 76 FR 3601 - Codex Alimentarius Commission: Meeting of the Codex Committee on Pesticide Residues

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-01-20

    ... From the Federal Register Online via the Government Publishing Office DEPARTMENT OF AGRICULTURE.... Department of Agriculture (USDA), and the Office of Pesticide Programs, U.S. Environmental Protection Agency... organizations, the Food and Agriculture Organization (FAO) and the World Health Organization (WHO)....

  18. DETERMINATION OF PESTICIDE RESIDUES IN BIOLOGICAL EXTRACTS BY RETENTION TIME LOCKING CAPILLARY GAS CHROMATOGRAPHY MASS SPECTROMETRY

    EPA Science Inventory

    The widespread use of pesticides in agricultural and urban areas (golf course and residential lawn applications) is largely responsible for the presence of these compounds in many water bodies. Transported by storm-waters, irrigation runoffs, wind, and treated and untreated sewag...

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

    PubMed

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

    2015-05-01

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

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

    PubMed

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

    2016-06-15

    Pesticide residues exceeding standard in green tea is a widespread problem of the world's attention, containing organochlorine pesticides (OCPs), organophosphorus pesticides (OPPs), and pyrethroids. In this research, three dimensionally honeycomb Mg-Al layered double oxide (TDH-Mg-Al-LDO) combined with graphitized carbon black (GCB), packed as a column, was used as a novel solid phase extraction sorbent, applying in simultaneous determination of 15 pesticide residues in green tea coupled with GC-MS. Compared with different type of SPE column, it showed that TDH-Mg-Al-LDO exhibited great advantages in the extraction of 15 pesticide residues from green tea, which was seldom reported before. Different experiment conditions, such as combination order of Mg-Al-LDO and GCB, dosage of sorbents, type and volume of eluting solvent were thoroughly studied and optimized. The limits of detection (LODs) of 15 pesticides ranged from 0.9 to 24.2ng/g and the limits of quantifications (LOQs) were ranging from 3.0 to 80.0ng/g. The recoveries using this method at three spiked concentration levels (10, 100 and 500ng/g for Fenthion, P,P'-DDE, O,P'-DDT, P,P'-DDD and Bifenthrin, 100, 500 and 2000ng/g for the others) range from 71.1 to 119.0%. The relative standard deviation (RSD) was from 0.1 to 7.6% in all case. The result indicated that the proposed analytical method had been successfully applied for the simultaneous determination of 15 pesticide residues in commercial green tea. PMID:27183089

  1. Determination of Trichlorfon Pesticide Residues in Milk via Gas Chromatography with μ-Electron Capture Detection and GC-MS.

    PubMed

    Hem, Lina; Khay, Sathya; Choi, Jeong-Heui; Morgan, E D; Abd El-Aty, A M; Shim, Jae-Han

    2010-06-01

    The pesticide trichlorfon is readily degraded under experimental conditions to dichlorvos. A method has therefore been developed by which residues of trichlorfon in milk are determined as dichlorvos, using gas chromatography with μ-electron capture detection. The identification of dichlorvos was confirmed by mass spectrometry. Milk was extracted with acetonitrile followed by centrifugation, freezing lipid filtration, and partitioning into dichloromethane. The residue after partitioning of dichloromethane was dissolved in ethyl acetate for gas chromatography. Recovery concentration was determined at 0.5, 1.0, and 2.0 of times the maximum permitted residue limits (MRLs) for trichlorfon in milk. The average recoveries (n = 6) ranged from 92.4 to 103.6%. The repeatability of the measurements was expressed as relative standard deviations (RSDs) ranging from 3.6%, to 6.7%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.7 and 11.1 μg/l, respectively. The accuracy and precision (expressed as RSD) were estimated at concentrations from 25 to 250 μg/l. The intra- and inter-day accuracy (n = 6) ranged from 89.2%to 91% and 91.3% to 96.3%, respectively. The intra- and inter-day precisions were lower than 8%. The developed method was applied to determine trichlorfon in real samples collected from the seven major cities in the Republic of Korea. No residual trichlorfon was detected in any samples. PMID:24278518

  2. Residues of organochlorine pesticides and polycyclic aromatic hydrocarbons in farm-raised livestock feeds and manures in Jiangsu, China.

    PubMed

    Zhao, Ling; Dong, Yuan-Hua; Wang, Hui

    2013-04-15

    The residual levels of 8 organochlorine pesticides (OCPs) and 15 priority polycyclic aromatic hydrocarbons (PAHs) were determined in pig, chicken, and cow feed and manure samples collected from feedlots in Jiangsu province, China. The mean residuals of OCPs ranged from 25.35 to 65.62 ng g(-1) in feeds and from 33.46 to 90.89 ng g(-1) in manures. Among 4 hexachlorocyclohexanes (HCHs), α-HCH was the most abundant compound, with a high occurrence above 80% in all kinds of animal feeds and manures. For dichlorodiphenyltrichloroethanes (DDTs), the predominance of p,p'-DDE and p,p'-DDT of total DDTs was also clearly observed. Composite profiles of HCHs and DDTs in feeds indicated that the residuals of lindane and DDTs could be attributed to new inputs in the past several years. The mean residuals of all of the PAHs varied from 128.94 to 389.66 ng g(-1) in manures. The mean concentrations of seven carcinogenic PAHs in manures varied from 16.80 to 79.70 ng g(-1). Of the 15 priority PAHs, phenanthrene was the most dominant PAH species and accounted for approximately 50% of the total PAHs in all animal manures. The distribution of PAHs with different rings showed that PAHs with 3 rings were the primary components in the tested manures. PMID:23058310

  3. Occupational pesticide exposure in early pregnancy associated with sex-specific neurobehavioral deficits in the children at school age.

    PubMed

    Andersen, Helle R; Debes, Fróði; Wohlfahrt-Veje, Christine; Murata, Katsuyuki; Grandjean, Philippe

    2015-01-01

    Prenatal exposure to pesticides may affect neurodevelopment, while the impact of modern pesticides is unclear. From 1997-2001, women working in greenhouse horticultures were recruited at the beginning of their pregnancy. Based on detailed interview of the women and their employers, those categorized as occupationally exposed to pesticides were moved to unexposed work functions or went on paid leave, while women without any exposure were considered unexposed controls. Of the resulting birth cohort of 203 children, 133 (65%) were examined at age 6 to 11 years together with 44 newly recruited children of same age whose mothers were not occupationally exposed to pesticides in pregnancy. All children underwent a standardized examination including a battery of neurodevelopmental tests. Maternal occupational pesticide exposure in early pregnancy was associated with prolonged brainstem auditory evoked potential latencies in the children as a whole and with impaired neuropsychological function in girls, while no effect was apparent in boys. In girls, language and motor speed functions were significantly inversely associated with prenatal exposure, and a non-significant tendency toward decreased function was also seen for other neuropsychological outcomes. A structural equation model that combined all these test results showed an overall impaired neuropsychological function in girls prenatally exposed to pesticides. Thus, our findings suggest an adverse effect of maternal occupational pesticide exposure on their children's neurodevelopment, despite the fact that the exposures occurred solely during early pregnancy and under well regulated working conditions, where special measures to protect pregnant women were applied. PMID:25450661

  4. Liquid chromatography Orbitrap mass spectrometry with simultaneous full scan and tandem MS/MS for highly selective pesticide residue analysis.

    PubMed

    Del Mar Gómez-Ramos, María; Rajski, Łukasz; Heinzen, Horacio; Fernández-Alba, Amadeo R

    2015-08-01

    This paper describes the application of LC/Q-Orbitrap MS for the analysis of pesticide residues in fruit and vegetable commodities. LC/Q-Orbitrap MS working in full scan simultaneously with a single MS/MS scan was used to analyse 139 pesticide residues in QuEChERS extracts of tomato, pepper, orange and green tea. Full scan data were obtained at a resolution of 70,000 whereas MS/MS data were obtained at a resolution of 17,500. Quantitation and detection was carried out using full scan data while MS/MS data were used only for identification. MS/MS scans did not have a negative influence on quantitation under the applied conditions. Some peak area reproducibility problems were the consequence of the low sensitivity for some compounds (aldicarb, chlorpyriphos methyl, fenitrothion and fipronil) under the applied conditions. The relation between the operational parameters (viz. automatic gain control (AGC) target, maximum injection time (IT), underfill ratio, isolation window and apex trigger) and the number of automatically identified compounds was investigated. Mass error and minimal intensity of selected fragment ions were also studied. Various working modes were compared, such as full scan with single MS/MS scan and full scan with multiple MS/MS scans. In both cases, the number of automatically reported pesticides was the same. However full scan with single MS/MS scan ensured more points per peak in full scan mode and better peak area reproducibility. The evaluation of the identification and quantitation capabilities of the instrument was performed through the analysis of 100 real samples. The samples were also analysed by LC-QqQ MS/MS and the results of both analytical systems were compared. The comparison revealed that the two instruments were consistent with each other. They found the same pesticides and neither false positive nor false negatives were reported. Nevertheless the Q-Orbitrap MS allowed one to work in high resolution mass spectrometry, increasing the

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

    PubMed

    Oellig, Claudia; Schwack, Wolfgang

    2012-10-19

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

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

    PubMed

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

    2013-10-01

    A novel design for a rapid clean-up method was developed for the analysis of pesticide residues in fruit and vegetables followed by LC-ESI-MS/MS. The acetonitrile-based sample extraction technique was used to obtain the extracts, and further clean-up was carried out by applying the streamlined procedure on a multiplug filtration clean-up column coupled with a syringe. The sorbent used for clean-up in this research is multiwalled carbon nanotubes, which was mixed with anhydrous magnesium sulfate to remove water from the extracts. This method was validated on 40 representative pesticides and apple, cabbage, and potato sample matrices spiked at two concentration levels of 10 and 100 μg/kg. It exhibited recoveries between 71 and 117% for most pesticides with RSDs < 15%. Matrix-matched calibrations were performed with the coefficients of determination >0.995 for most studied pesticides between concentration levels of 10-500 μg/L. The LOQs for 40 pesticides ranged from 2 to 50 μg/kg. The developed method was successfully applied to the determination of pesticide residues in market fruit and vegetable samples. PMID:23939876

  7. Residues of organochlorine pesticides in milk gland secretion of cows in perinatal period

    SciTech Connect

    Sitarska, E.; Klucinski, W.; Winnicka, A. ); Ludwicki, J. )

    1991-12-01

    Persistent organochlorine (OC) compounds such as DDT and its derivatives, isomers of hexachlorocyclohexane (HCH), hexachlorobenzene (HCB) and polychlorinated biphenyls (PCBs) may pose toxicological and ecological impact due to their persistence in some biological compartments. Despite the fact that agriculture has discontinued the use of the majority of these pesticides in many countries, the considerable differences in their concentrations in samples of human and animal origin are evidence that biological magnification via the food chain still exists in the case of OC compounds. This phenomenon may by illustrated by the close relationship between OC compound concentration in the fat of human and cow milk. The purpose of the present study was to determine the rate of excretion of the OC pesticide complex including their metabolites in the perinatal and postnatal period during various gland secretion phases.

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

    PubMed

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

    2014-09-15

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

  9. Assessment of organochlorine pesticides residues in higher plants from oil exploration areas of Niger Delta, Nigeria.

    PubMed

    Sojinu, O Samuel; Sonibare, Oluwadayo O; Ekundayo, Olusegun O; Zeng, Eddy Y

    2012-09-01

    The concentrations and distributions of organochlorine pesticides (OCPs) in some higher plant samples collected from oil exploration areas of the Niger Delta, Nigeria were examined. The concentrations of Σ(25)OCP ranged from 82 to 424, 44 to 200 , 34 to 358, 33 to 106 and 16 to 75 ng/g in Olomoro, Oginni, Uzere, Irri and Calabar plants, respectively. The compositional profiles of the analysed OCPs in most of the plants showed no fresh inputs in the area. The OCPs detected in the samples could have resulted from pesticide usage for intense farming activities cum the use of pesticides to control household pests and insects in the area. Drilling fluids and corrosion inhibitors used in petroleum explorations also have chlorinated compounds as additives thereby serving as potential sources of OCPs. Among the studied plants, elephant grass showed high bioaccumulation and phytoremediation potentials of OCPs. The ΣHCH concentrations exceeded the allowable daily intake limit thereby serving as potential threat to humans. PMID:22789817

  10. Effect of pesticide residues on health and different enzyme levels in the blood of farm workers from Gadap (rural area) Karachi-Pakistan.

    PubMed

    Azmi, M Ahmed; Naqvi, S N H; Azmi, M Arshad; Aslam, M

    2006-09-01

    Persons from 14 different fruit and vegetable farm stations from Gadap (rural area), Karachi-Pakistan were examined for the presence of pesticide (cypermethrin, deltamethrin, polytrin-C, diazinon, monocrotophos, DDT and DDE) residues in their blood samples. The present study is concerned with effects of residue on the enzyme levels (GPT, GOT and ALP) as well as the health hazards of pesticide exposed persons. There is a significant increased in the enzyme levels at different stations. Exposed persons complained about liver and kidney dysfunctions and RTI. It may be concluded that exposure of multiple pesticides for prolonged period has affected the normal functioning of different organ systems and possibly produced characteristics clinical effects such as hepatitis, dyspnea and burning sensation in urine. PMID:16487989

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

    PubMed

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

    2015-01-01

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

  12. Persistent organochlorine pesticide residues in tissues and eggs of white-backed vulture, Gyps bengalensis from different locations in India.

    PubMed

    Muralidharan, S; Dhananjayan, V; Risebrough, Robert; Prakash, V; Jayakumar, R; Bloom, Peter H

    2008-12-01

    Organochlorine pesticide residues were determined in tissues of five Indian white-backed vultures and two of their eggs collected from different locations in India. All the samples had varying levels of residues. p,p'-DDE ranged between 0.002 microg/g in muscle of vulture from Mudumali and 7.30 microg/g in liver of vulture from Delhi. Relatively higher levels of p,p'-DDT and its metabolites were documented in the bird from Delhi than other places. Dieldrin was 0.003 and 0.015 microg/g while p,p'-DDE was 2.46 and 3.26 microg/g in egg one and two respectively. Dieldrin appeared to be lower than the threshold level of 0.5 microg/g. p,p'-DDE exceeded the levels reported to have created toxic effects in eggs of other wild birds. Although varying levels of DDT, HCH, dieldrin, heptachlor epoxide and endosulfan residues were detected in the vulture tissues, they do not appear to be responsible for the present status of population in India. PMID:18806909

  13. Determination of nicotinyl pesticide residues in vegetables by micellar electrokinetic capillary chromatography with quantum dot indirect laser-induced fluorescence.

    PubMed

    Chen, Guan-Hua; Sun, Juan; Dai, Yong-Jia; Dong, Min

    2012-07-01

    A new assay was developed by use of micellar electrokinetic capillary chromatography with indirect LIF fluorescence for the determination of thiamethoxam, acetamiprid, and imidacloprid residues in vegetables, in which the cadmium telluride quantum dots (QDs) synthesized in aqueous phase were used as fluorescent background substance and their excitation and emission wavelengths matched with LIF detector by engineering their size. The factors that affected the peak height and the resolution were optimized. The running buffer was composed of 4.4 μM cadmium telluride QDs as fluorescent background substance, 40 mM borate and 60 mM SDS, and its pH was adjusted to 8.0. The separation voltage was 25 kV. Under the optimum conditions, the detection limits were 0.05, 0.01, and 0.009 mg/kg; the linear dynamic ranges were 0.5-30, 0.1-30, and 0.1-30 mg/L; and the average recoveries of spiked samples were 72.0-101.2, 74.0-106.7, and 77.8-105.1% for thiamethoxam, acetamiprid, and imidacloprid, respectively. The assay can meet the requirement of maximum residue limits to these three pesticides in the regulations of European Union and Japan, and has been applied for determining their residues in vegetables. PMID:22821497

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

    PubMed

    Mekonen, Seblework; Ambelu, Argaw; Spanoghe, Pieter

    2014-06-01

    Samples of maize, teff, red pepper, and coffee (green bean and coffee bean with pulp) were collected from a local market in the Jimma Zone, Ethiopia. Samples were analyzed for the occurrence of cypermethrin, permethrin, deltamethrin, chlorpyrifos ethyl, DTT and its metabolites, and endosulfan (α, β). In the analytical procedure, the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction methodology with dispersive solid phase extraction clean up (d-SPE) technique was applied. Validation of the QuEChERS method was satisfactory. Recovery percentages of most pesticides were in the range of 70% to 120%, with good repeatability (%relative standard deviation < 20). The limit of detection and limit of quantification varied between 0.001 µg/g and 0.092 µg/g and between 0.002 µg/g and 0.307 µg/g, respectively. The main pesticides detected were DDT, endosulfan, cypermethrin, and permethrin. All of the pesticides analyzed were detected in red pepper and green coffee bean. Residues of DDT in coffee pulp significantly differed (p < 0.01) from other food items except for red pepper. The concentration of pesticides in the food items varied from 0.011 mg/kg to 1.115 mg/kg. All food items contained 1 or more pesticides. Two-thirds of the samples had residues below corresponding maximum residue limits, and the remaining one-third of samples were above the maximum residue limits. These results indicate the need for a good pesticide monitoring program to evaluate consumer risk for the Ethiopian people. PMID:24648104

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

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

    PubMed

    Oellig, Claudia; Schwack, Wolfgang

    2014-07-18

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

  19. Assessment of health risk from organochlorine pesticides residues in high-fat spreadable foods produced in Poland.

    PubMed

    Witczak, Agata; Abdel-Gawad, Hassan

    2014-01-01

    Currently, butter and margarine are food products attracting wide customer interest. Every day, consumers around the world buy these products for human consumption. Butter is obtained from milk fat, while margarine is derived from vegetable oils. The content of organochlorine pesticide (OCP) residues was examined in both types of these high fatty products. A gas chromatograph with MSD (HP 5973) detector was used for the determination of pesticides such as α-HCH, β-HCH, γ-HCH, DDT, DDD, DDE, aldrin, dieldrin, endrin, heptachlor and heptachlor epoxide. The examined products had diverse concentrations of the analyzed compounds. Visible was the division based on the origin of the product, which might be composed of animal or vegetable fats. The research has revealed the presence of OCP residues in all examined spreads. Quantities of organochlorine compounds did not pose an immediate danger to the consumers' health. Human and environmental health risk assessment was carried out by the estimation of lifetime average daily dose (LADD) and non-carcinogenic health hazard quotient (HQ). Total estimated LADD ranged between 1.3 × 10(-5) and 3.1 × 10(-5) mg kg(-1) d(-1) for butter, and 1.9 × 10(-6) and 4.6 × 10(-6) mg kg(-1) d(-1) for margarine and mix spread. The HQ ranged between 1.1 × 10(-4) and 3.7 × 10(-4) for butter, and 1.4 × 10(-5) and 9.0 × 10(-6) for margarine and mix spread for adults. These estimated HQs were within the safe acceptable limits, indicating a negligible risk to the residents of the study area. PMID:25310807

  20. Residues of organochlorine pesticides and polychlorinated biphenyls and autopsy data for bald eagles, 1971-72

    USGS Publications Warehouse

    Cromartie, E.; Reichel, W.L.; Locke, L.N.; Belisle, A.A.; Kaiser, T.E.; Lamont, T.G.; Mulhern, B.M.; Prouty, R.M.; Swineford, D.M.

    1975-01-01

    Thirty-seven bald eagles found sick or dead in 18 States during 1971-72 were analyzed for organochlorine pesticides and polychlorinated biphenyls (PCB's). DDE and PCB's were detected in all bald eagle carcasses; 30 carcasses contained DDD and 28 contained dieldrin. Four eagles contained possibly lethal levels of dieldrin and nine eagles had been poisoned by thallium. Autopsies revealed that illegal shooting was the most common cause of mortality. Since 1964 when data were first collected, 8 of the 17 eagles obtained from Maryland, Virginia, South Carolina, and Florida possibly died from dieldrin poisoning; all four specimens from Maryland and Virginia were from the Chesapeake Bay Tidewater area.

  1. Determination of chlorinated pesticide residues in foods. II. Simultaneous analysis of chlorinated pesticide and phthalate ester residues by using AgNO3-coated Florisil column chromatography for cleanup of various samples.

    PubMed

    Suzuki, T; Ishikawa, K; Sato, N; Sakai, K I

    1979-05-01

    A simplified method suitable for simultaneous analysis of chlorinated pesticide and phthalate ester residues in various foods was developed. Chemical residues were quantitatively extracted from fatty and vegetable samples with acetonitrile as follows: Chemical standard in 0.5 mL ethanol solution was added to 10 g homogenized sample. After 3 hr, pork and beef were extracted 3 times with 20 mL portions of acetonitrile. The acetonitrile layers were diluted with water and extracted with n-hexane. Rice samples were combined with 10 mL water, 5 mL acetonitrile and 1 mL ethanol and extracted 3 times with 20 mL portions of n-hexane. The n-hexane concentrate from each sample was submitted to AgNO3-coated Florisil column chromatography. The AgNO3 coating adequately adsorbed interfering coextractives. Extracts of fish and vegetable samples were separated into 2 fractions by the above column chromatography. Supplemental cleanup procedures were also developed to accurately determine phthalate esters eluted in the second fraction. Satisfactory gas chromatograms were obtained for most samples. PMID:479097

  2. Analyses of human milk samples collected in Hawaii for residues of organochlorine pesticides and polychlorobiphenyls

    SciTech Connect

    Takei, G.H.; Kauahikaua, S.M.; Leong, G.H.

    1983-01-01

    This work has revealed that the chlorinated hydrocarbon residues found in human milk samples collected from residents in the State of Hawaii were statistically the same residues found in mainland human milk samples. Moreover, the levels at which these residues were detected in Hawaiian samples were comparable to those detected in mainland samples, and differences between the two groups of samples were not apparent. The close correlation between residue analyses was unexpected considering Hawaii's geographic isolation and the distinct ethnic diets of its populations. They do indicate, however, that the uptake of chlorinated hdyrocarbon contaminants by the population of this state is not specific and is most likely due to some physiological means of entry which is common to the populations of the mainland states.

  3. Multi-residue analysis of 26 organochlorine pesticides in Alpinia oxyphylla by GC-ECD after solid phase extraction and acid cleanup.

    PubMed

    Zhao, Xiangsheng; Zhou, Yakui; Kong, Weijun; Gong, Bao; Chen, Deli; Wei, Jianhe; Yang, Meihua

    2016-04-01

    A simple and effective multi-residue method was developed and validated for the analysis of 26 organochlorine pesticide residues in Alpinia oxyphylla by a gas chromatography with an electron capture detector (GC-ECD). The target pesticides were extracted by sonication and cleaned up with florisil solid phase extraction and sulphuric acid. Some crucial parameters, including extraction solvent and time, sorbent type, elute solvent and concentration of sulphuric acid were optimized to improve the performance of sample preparation procedure. The optimized method gave high sensitivity with detection limit ranging from 0.1 to 2.0μg/kg. Matrix-matched calibration was employed for the quantification, and a wide linear range (from 1.0 to 1000μg/kg) with r(2) values ranging from 0.9971 to 0.9998 was obtained. For the majority of the tested pesticides, the average recoveries were in acceptable range (between 70% and 110%) with relative standard deviation values below 15.0%. Matrix effect was evaluated for target compounds through the study of ratio of peak area obtained in the solvent and blank matrix. The proposed method was applied to simultaneously analyze 26 pesticides in 55 batches of Alpinia oxyphylla samples. 3 samples were found to be positive with four pesticides (α-BHC, quintozene, trans-chlordane and op'-DDD), which were confirmed by gas chromatography-mass spectrometry (GC-MS) in selective ion monitoring (SIM) mode. PMID:26990736

  4. Evaluation of different sample treatments for determining pesticide residues in fat vegetable matrices like avocado by low-pressure gas chromatography-tandem mass spectrometry.

    PubMed

    Moreno, J L Fernández; Liébanas, F J Arrebola; Frenich, A Garrido; Vidal, J L Martínez

    2006-04-01

    A multi-residue method has been developed for determining 65 pesticide residues in greasy vegetable matrices such as avocado. Conventional organic solvent extraction assisted by a high-speed homogenizer was compared to pressurized liquid extraction (PLE) as extraction techniques. Following this, the lipophilic extract was purified using gel permeation chromatography (GPC). Alternative clean-up methods were also evaluated, as solid-phase extraction cartridges individually used and downstream coupled, but less effective lipophilic separation was archived. The pesticide residue determination was carried out using low-pressure gas chromatography coupled to tandem mass spectrometry (LP-GC-MS-MS), showing the applicability of this type of GC columns for the analysis of fat vegetable matrices. The proposed methodology was validated in avocado matrix. The recoveries were in the range 70-110%, with RSD values lower than 19%, at 12 and 50 microg/kg spiking levels. The limits of quantitation (LOQs) were in the range 0.04-8.33 microg/kg and the limits of detection (LODs) were between 0.01 and 2.50 microg/kg. All of them were lower than the maximum residue levels (MRLs) set by the European Union (EU) in avocado. The proposed method was evaluated analyzing pesticide residues in real avocado samples. PMID:16480726

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

    PubMed

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

    2014-01-01

    The effect of home canning (including washing, boiling, cooling, adding solution and sterilisation) on residue levels of imidacloprid, diflubenzuron, abamectin, pyriproxyfen and β-cypermethrin and chlorothalonilin on button crimini was assessed. Residues of imidacloprid, diflubenzuron, abamectin and pyriproxyfen were measured by UPLC-MS/MS; the residues of β-cypermethrin and chlorothalonil were measured by GC. Results showed that washing resulted in a 3.8% reduction of the initial residue level of imidacloprid (p ≤ 0.05). From washing to sterilisation the processing effect was significant compared with raw crimini (p ≤ 0.05), but processing through cooling and adding solution had no effect. For diflubenzuron, from raw crimini to sterilisation the processing effect was significant by comparison with the initial level (p ≤ 0.05); the processing effect was not obvious between two sequential steps, and the sequential steps have list: washing and boiling, boiling and cooling, boiling and adding of solution, cooling and adding solution. The changes in abamectin levels were also significant from raw crimini to sterilisation compared with raw crimini (p ≤ 0.05), but the changes were not obvious from boiling to adding solution and amongst them. For pyriproxyfen, washing resulted in a 39% reduction, but changes were not obvious from washing to sterilisation, p ≤ 0.05 between two consecutive steps. The whole procedure could significantly decrease residues of β-cypermethrin (p ≤ 0.05); washing could significantly reduce residues of β-cypermethrin; the effects of last procedures were complicated, and p ≤ 0.05 between two consecutive steps. Washing resulted in an 80% reduction of chlorothalonil; after washing there were no detectable residues. After the whole process, the processing factors for imidacloprid, diflubenzuron, abamectin, pyriproxyfen, β-cypermethrin and chlorothalonil were 0.40, 0.22, 0.04, 0.85, 0.28 and 0, respectively. PMID:24761834

  6. Study on Carrier Material of Immobilization Acetylcholinesterase For Biosensor in Detectionof Organophosphorus Pesticide Residues

    NASA Astrophysics Data System (ADS)

    Sun, Xia; Wang, Xiangyou; Jia, Chuandong

    A comparison between several immobilization materials of AChE on surface of glassy carbon electrode(GCE) was presented. The immobilization methods employed crosslinking method with glutaraldehyde as a cross-linking agent and bovine serum albumin(BSA) as a protectant, AChE was immobilized on different membranes including nylon membrane, cellulose nitrate membrane and chitosan membrane respectively. The enzyme membrane was then fixed on the surface of glassy carbon electrode(GCE) with O-ring to prepare an amperometric biosensor for the detection of organophosphorus pesticides. The activity of immobilization AChE was detected by measuring the oxidation current of thiocholine, the results showed that the activity of immobilization AChE were all different with different membrane as carrier material.Compared with nylon membrane and cellulose nitrate membrane, chitosan membrane was obviously good. So chitosan membrane can be selected as immobilized AChE carrier material.

  7. Shell thinning and pesticide residues in Texas aquatic bird eggs, 1970

    USGS Publications Warehouse

    King, K.A.; Flickinger, Edward L.; Hildebrand, H.H.

    1978-01-01

    Significant decreases in eggshell thickness were found in 15 of 22 species of aquatic birds in Texas in 1970. Shell thickness reductions of 9 to 15 percent were found in white pelicans (Pelecanus erythrorhynchos), brown pelicans (P .occidentalis), and great blue herons (Ardea herodias). DDT family compounds were found in all eggs, and mean residues ranged from 0.4 ppm in white ibis (Eudocimus albus) to 23.2 ppm in great egrets (Casmerodius albus). GDDT residues were negatively correlated with shell thickness in five species; PCBs were negatively correlated in two. Residues in marine birds were generally lower and more uniform than levels in birds feeding in fresh and brackish water. DDT and dieldrin residues were higher in eggs from colonies near agricultural areas where these insecticides were heavily used; higher PCB residues were consistently associated with urban and industrial areas. Populations of five species have declined and deserve continued study: brown pelican, reddish egret (Dichromanassa rufescens), white-faced ibis (Plegadis chihi), laughing gull (Larus atricilla), and Forster's tern (Sterna forsteri). Population trends of four other species were undetermined and should be followed closely in future years.

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

    PubMed

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

    2013-02-01

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

  9. Pesticide residues on the external surfaces of field crop sprayers: occupational exposure.

    PubMed

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

    2005-06-01

    There is a general perception, amongst farmers and researchers, that post-application residues on the external surfaces of sprayers are negligible compared with residues remaining on the internal surfaces, although there have been few attempts to verify this assumption. The aim of this study was to investigate, using cotton glove sampling, operator exposure resulting from three typical operations: entering and working in the cab, general handling of the sprayer and maintenance practices. Samples were analysed for azoxystrobin, carbendazim, chlorothalonil, cyanazine, cypermethrin, epoxiconazole, flusilazole, isoproturon, kresoxim-methyl, metazachlor, pendimethalin, pirimicarb and tebuconazole. Isoproturon, pendimethalin, chlorothalonil and carbendazim were detected >1 mg per glove pair on the cotton gloves, but on the whole there was variability in residue levels between and within compounds. Comparison of results with occupational exposure limits indicated that residues were such that they may not necessarily be considered insignificant. It may therefore be prudent to develop more efficient methods for the external decontamination of sprayers and/or raise awareness of the findings. PMID:15650013

  10. Variability of pesticide residues in cauliflower units collected from a field trial and market places in Greece.

    PubMed

    Prodhan, M D H; Papadakis, Emmanouil-N; Papadopoulou-Mourkidou, Euphemia

    2016-09-01

    To estimate the variability of pesticide residue levels present in cauliflower units, a total of 142 samples were collected from a field trial of a cooperative farmer, and 120 samples were collected from different market places in Thessaloniki, Greece. The collected samples were extracted using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction technique, and the residues were determined by liquid chromatography-tandem mass spectrometry. The developed method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD), and limit of quantification (LOQ). The average recoveries for all the analytes, derived from the data of control samples fortified at 0.01, 0.05, 0.1, and 0.2 mg/kg, ranged from 74 to 110% with a relative standard deviation of ≤8%. The correlation coefficient (R(2)) was ≥0.997 for all the analytes using matrix-matched calibration standards. The LOD values ranged from 0.001 to 0.003 mg/kg, and the LOQ was determined at 0.01 mg/kg for all the sought analytes. The matrix effect was found to be at a considerable level, especially for cypermethrin and deltamethrin, amounting to +90% and +145%, respectively. For the field samples, the unit-to-unit variability factors (VFs) calculated for cypermethrin and deltamethrin were 2.38 and 2.32, respectively, while the average VF for the market basket samples was 5.11. In the market basket samples, residues of cypermethrin, deltamethrin, chlorpyrifos, and indoxacarb were found at levels ≥LOQ and their respective VFs were 7.12, 5.67, 5.28, and 2.40. PMID:27229457

  11. Dynamics of pesticide residues in nectar and pollen of mustard (Brassica juncea (L.) Czern.) grown in Himachal Pradesh (India).

    PubMed

    Choudhary, Amit; Sharma, D C

    2008-09-01

    Residues dynamics of Endosulfan (525.00 g a.i. ha(-1)), Imidacloprid seed treatment (21 g a.i. kg(-1)), Lambdacyhalothrin (75.00 g a.i. ha(-1)) and Spiromesifen (225.00 g a.i. ha(-1)) in nectar and pollen of mustard, Brassica juncea (L.) Czern. grown in Himachal Pradesh (India) were determined through bioassay (using Drosophila melanogaster Meig. as test organism) and GC (Gas chromatographic) and HPLC (High performance liquid chromatographic) methods. In general chromatographic methods were more sensitive for the determination of above given pesticides compared to bioassay method. Average recoveries in nectar samples varied between 82.85 and 88.90% by bioassay and 91.20 and 93.55% by chromatographic techniques. In pollen samples, recoveries varied between 81.44 and 86.44% by bioassay and 88.50 and 91.30% by chromatographic methods. Imidacloprid residues were neither found in nectar nor in pollen samples at the time of sampling i.e. 50% of flowering. The order of average half life of residues was: Lambdacyhalothrin (12.45 h) < Spiromesifen (19.99 h) < Endosulfan (27.49 h) for nectar and Spiromesifen (9.69 h) < Lambdacyhalothrin (12.44 h) < Endosulfan (17.84 h) for pollen samples. It was found that Imidcloprid seed treatment was practically harmless to honey bees, whereas a waiting period of 5 days must be observed on crops sprayed with these chemicals during blooms to avoid any accidental hazards to honey bees. PMID:17952621

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

    PubMed Central

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

    2010-01-01

    A method for the determination of pesticide residues in water and sediment was developed using the QuEChERS method followed by gas chromatography – mass spectrometry. The method was validated in terms of accuracy, specificity, linearity, detection and quantification limits. The recovery percentages obtained for the pesticides in water at different concentrations ranged from 63 to 116%, with relative standard deviations below 12%. The corresponding results from the sediment ranged from 48 to 115% with relative standard deviations below 16%. The limits of detection for the pesticides in water and sediment were below 0.003 mg L−1 and 0.02 mg kg−1, respectively. PMID:21165598

  13. Fate of 14C-ethion insecticide in the presence of deltamethrin and dimilin pesticides in cotton seeds and oils, removal of ethion residues in oils, and bioavailability of its bound residues to experimental animals.

    PubMed

    Abdel-Gawad, Hassan; Mahdy, Fathia; Hashad, Adly; Elgemeie, Galal H

    2014-12-24

    Ethyl-1-(14)C-ethion and some of its degradation products have been prepared for comparison purposes. Cotton plants were treated with (14)C-ethion alone and in the presence of deltamethrin and dimilin pesticides under conditions simulating local agricultural practice. (14)C-Residues in seeds were determined at harvest time; about 47.5% of (14)C-activity was associated with oil. After further extraction of seeds with ethanol, the ethanol-soluble (14)C-residues accounted for 10.6% of the total seed residues, whereas the cake contained about 37.3% of the total residues as bound residues in the case of ethion only. The bound residues decreased in the presence of deltamethrin and dimilin pesticides and amounted to 8.1 and 10.4% of the total residues, respectively. About 95% of the (14)C-activity in the crude oil could be eliminated by simulated commercial processes locally used for oil refining. Chromatographic analysis of crude cotton oil revealed the presence of ethion monooxon, O,O-diethyl phosphorothioate, and O,O-diethyl phosphoric acid in addition to one unknown compound in the case of ethion alone or ethion and dimilin. The same degradation products are found in the case of ethion and deltamethrin in addition to ethion dioxon, whereas ethanol extract revealed the presence of ethion dioxon and O,O-diethyl phosphoric acid as free metabolites. Acid hydrolysis of the conjugated metabolites in the ethanol extract yielded O,O-diethyl S-hydroxymethyl phosphorodithioate. The bound residues were quite readily bioavailable to the rats. After feeding rats with the cake containing ethion-bound residues, a substantial amount (60%) of (14)C-residues was eliminated in the urine, whereas the (14)C-residues excreted in expired air and feces were 10 and 9%, respectively. About 11% of the radioactive residues were distributed among various organs. PMID:25420216

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

    PubMed

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

    2016-01-01

    A sensitive, accurate and reliable multi-class GC-MS/MS assay protocol for quantification and confirmation of 200 common agricultural pesticides in honey was developed and validated according to EU guidelines. A modified extraction procedure, based on QuEChERS method (quick, easy, cheap, effective, rugged and safe) was employed. Mass spectrophotometric conditions were individually optimized for each analyte to achieve maximum sensitivity and selectivity in MRM mode. The use of at least two reactions for each compound allowed simultaneous identification and quantification in a single run. The pesticides under investigation were separated in less than 31 min using the ultra-inert capillary column (DB-35MS). For all analytes, neat standard calibration curves in conjunction with correction for matrix effect were successfully employed. The detection limits of the assay ranged from 1.00 to 3.00 ng mL(-1) for the studied pesticides. The developed assay was linear over concentration range of 10.00-500.00 ng mL(-1), with correlation coefficient of more than 0.996. At the LOQ, 81% of the studied pesticides were efficiently recovered in the range of 70.00-120.00%, with CV% less than 15.00% while 99.3% compounds had mean percentage recovery of 60.00-140.00%, with CV% less than 21.00% (N=18, over three different days). The proposed assay was successfully applied for the analysis of the studied pesticide residues in one PT sample and 64 commercial honey samples collected over 1 year from different districts around Egypt. Results revealed that only one honey sample out of the 64 analyzed samples was contaminated with tau-Fluvalinate (10.00 μg kg(-1)). This wide scope assay protocol is applicable for monitoring pesticide residues in honey by national regulatory authorities and accredited labs; that should help ensure safety of such widely used product. PMID:26687165

  15. Organochlorine pesticide residues in eggs and tissues of house sparrow, Passer domesticus, from Tamil Nadu, India.

    PubMed

    Dhananjayan, V; Muralidharan, S; Ranapratap, S

    2011-12-01

    This study provides information on the current status of contamination by organochlorine pesticides (OCPs) in eggs and tissues of House Sparrow, Passer domesticus, in Tamil Nadu, India. The mean concentration of total hexachlorocyclohexane (∑HCH) and total dichloro-diphenyl-trichloroethane (∑DDT) in eggs ranged from 0.01 to 1.81 μg/g and 0.02 to 1.29 μg/g, respectively. Concentration of 1,1-dichloro-2,2-bis(p-chlorophenyl)ethylene (p,p'-DDE) ranged from below detectable limit (BDL) to 0.64 μg/g, representing more than 60% of the ∑DDTs. About 28% of samples had p,p'-DDE levels above the critical concentration associated with reproductive impairment. However, the mean concentrations of cyclodiene insecticides were less than 0.5 μg/g. Although OCPs levels detected in tissues are not indicative of toxicity, continuous monitoring is recommended. PMID:21979140

  16. New platform of biosensors for prescreening of pesticide residues to support laboratory analyses.

    PubMed

    Buonasera, Katia; Pezzotti, Gianni; Scognamiglio, Viviana; Tibuzzi, Arianna; Giardi, Maria Teresa

    2010-05-26

    Millions of tons of pesticides are applied worldwide annually in agriculture. Among them, herbicides such as triazines and ureas, originating from agricultural runoff, can contaminate soils and surface and ground waters with severe toxic effects on humans. Nowadays, different analytical techniques are available for the detection of these chemicals; however, most of them are expensive and time-consuming, especially in the case of routine analyses. For this reason, on the basis of results collected through many years of experience in the field of photosynthetic organisms, we designed a biosensor platform intended for the easy, low-cost, and fast prescreening of photosynthetic herbicides. The platform combines the possibilities of amperometric and optical transduction systems, which have proven to be highly sensitive (limits of detection = 10(-10)-10(-8) M). The use of genetically modified algae strengthens the power of the platform, allowing different subclasses of herbicides to be recognized. The system has been validated for the analysis of environmental water and is proposed to support laboratories involved in the control of water pollution. PMID:20020685

  17. Residues of organochlorine pesticides and PCBs in some Brazilian municipal solid waste compost.

    PubMed

    Lourencetti, Carolina; Favoreto, Rodrigo; Marchi, Mary R R; Ribeiro, Maria L

    2007-08-01

    Persistent organic pollutants (POPs), organochlorine pesticides and polychlorinated biphenyls (PCBs), listed as per the Stockholm Convention (alpha -HCH, beta -HCH, gamma -HCH, p,p'-DDT, o,p'-DDT, p,p'-DDD, p,p'-DDE, aldrin, endrin, dieldrin, PCBs 28, 52, 118, 138, 153, and 180), were analyzed in municipal solid waste (MSW) compost samples from three different Brazilian composting plants located in three São Paulo State cities: Araras, Araraquara and São Paulo (Vila Leopoldinha). Quantitative and qualitative analyses were carried out using gas chromatography electron capture detection (GC-ECD) and gas chromatography mass spectrometry (GC-MS) (Ion Trap, electron impact ionization), respectively. The samples were analyzed in triplicate and the target POPs were not detected by GC-ECD. Twelve pollutants were identified in two samples when qualitative analysis (GC-MS) was used (beta -HCH, gamma -HCH, p,p'-DDT, o,p'-DDT, p,p'-DDD, and p,p'-DDE, PCBs 28, 118, 138, 153 and 180). The composting process has advantages such as urban solid waste reduction and landfill life-span increase, however the MSW compost quality, which can be utilized for agricultural purposes, should be evaluated and be controlled. This kind of study is the first step in making available information to answer questions regarding MSW compost for sustainable agricultural use, such as the pollutants accumulation in soil and in groundwater, and plants uptake. PMID:17701705

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

    PubMed

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

    2015-01-01

    The feasibility of using visible/near-infrared (Vis/NIR) spectroscopy was assessed for non-destructive detection of diazinon residues in intact cucumbers. Vis/NIR spectra of diazinon solution and cucumber samples without and with different concentrations of diazinon residue were analysed at the range of 450-1000 nm. Partial least squares-discriminant analysis (PLS-DA) models were developed based on different spectral pre-processing techniques to classify cucumbers with contents of diazinon below and above the MRL as safe and unsafe samples, respectively. The best model was obtained using a first-derivative method with the lowest standard error of cross-validation (SECV = 0.366). Moreover, total percentages of correctly classified samples in calibration and prediction sets were 97.5% and 92.31%, respectively. It was concluded that Vis/NIR spectroscopy could be an appropriate, fast and non-destructive technology for safety control of intact cucumbers by the absence/presence of diazinon residues. PMID:25789964

  19. [Rapid determination of 204 pesticide residues in tea by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry].

    PubMed

    Yu, Lu; Song, Wei; Lu, Yaning; Zhao, Muyu; Zhou, Fangfang; Hu, Yanyun; Zheng, Ping

    2015-06-01

    An analytical method was established for the simultaneous determination of 204 pesticide residues in tea by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS). The samples were extracted with acetonitrile, and cleaned-up by solid phase extraction (SPE) with a Carb-PSA cartridge, eluted with acetonitrile-toluene (3:1, v/v), determined by UPLC-Q-TOF/MS and quantified by external standard method. A data base of the accurate mass numbers and a library which contains the 204 pesticides were established. The automatic retrieval of detection results was carried on according to the characteristics of the compound, such as accurate mass, retention time, isotopic ratio, and so on. Based on the above results, the qualitative identifications of the 204 pesticides were accomplished without the contrast of standard substances. The results indicated that this method can be used to determine the 204 pesticides in tea. At the three spiked levels of 10, 20, 50 µg/kg, mean recoveries for the 204 pesticides in tea were between 68. 1% and 117. 2%, with the relative standard deviations (RSDs) ranging from 3.1% to 18.9%. The limits of quantification for the 204 pesticides were lower than 10 µg/kg. The method has been applied to four positive samples, and the results generally accord with the detection results by the method of GB/T 23205-2008. This method has the characteristics of high efficiency, as well as high sensitivity and accuracy, which can meet the requirement of the determination of the 204 pesticides in tea. PMID:26536763

  20. Validation and application of a multi-residue method, using accelerated solvent extraction followed by gas chromatography, for pesticides quantification in soil.

    PubMed

    Leyva-Morales, J B; Valdez-Torres, J B; Bastidas-Bastidas, P J; Betancourt-Lozano, M

    2015-01-01

    A multi-residue method was developed to determine different types of pesticides in soils. An extraction with pressure and temperature, through accelerated solvent extraction (dichloromethane:acetone, 50:50, v/v). The pesticides were determined by gas chromatography with several selective detectors: electron capture detector, pulsed flame photometric detector and thermionic specific detector. The following parameters were determined: limit of detection, limit of quantification, equipment linearity (working interval), method linearity as well as, method accuracy and precision. The average recoveries ranged between 76 and 106%, with the exception of chlorothalonil, which had an average recovery of 46%. Additionally, detection limits from 0.9 to 7.6ng g -: (1) and the quantification limits from 3.00 to 25.47ng g -: (1) were estimated. In terms of linearity and precision, the results obtained were in the ranges considered adequate (R(2) ≥ 0.98 and coefficient of variation (CV) ≤ 20%), with the exception of aldrin (R(2) = 0.946, CV = 35.79%), lindane (R(2) = 0.917, CV = 32.91%) and chlorothalonil (R(2) = 0.8184, CV = 81.35%). The proposed method was used to evaluate pesticides in real soil samples, detecting concentrations over 1000ng g -: (1) for some pesticides. The method was correctly validated and provided for the rapid determination of pesticides in soil. PMID:26041247

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

    PubMed

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

    2016-05-01

    Ozonated water dip technique was evaluated for the detoxification of six pesticides, i.e., chlorpyrifos, cypermethrin, azoxystrobin, hexaconazole, methyl parathion, and chlorothalonil from apple fruits. Results revealed that ozonation was better than washing alone. Ozonation for 15 min decreased residues of the test pesticides in the range of from 26.91 to 73.58%, while ozonation for 30 min could remove the pesticide residues by 39.39-95.14 % compared to 19.05-72.80 % by washing. Cypermethrin was the least removed pesticide by washing as well as by ozonation. Chlorothalonil, chlorpyrifos, and azoxystrobin were removed up to 71.45-95.14 % in a 30-min ozonation period. In case of methyl parathion removal, no extra advantage could be obtained by ozonation. The HPLC analysis indicated that ozonation also affected adversely the ascorbic acid and cyanidin-3-glucoside content of apples. However, 11 polyphenols studied showed a mixed trend. Gallic acid, 3,4-dihydroxybenzoic acid, catechin, epicatechin, p-coumaric acid, quercetin-3-O-glucoside, quercetin, and kaempferol were found to decrease while syringic acid, rutin, and resveratrol were found to increase in 30-min ozonation. PMID:27098519

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

    PubMed

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

    2015-05-15

    A quick and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method, using dynamic multiple reaction monitoring and a 1.8-μm particle size analytical column, was developed to determine 57 pesticides in tomato in a 13-min run. QuEChERS (quick, easy, cheap, effective, rugged, and safe) method for samples preparations and validations was carried out in compliance with EU SANCO guidelines. The method was applied to 58 tomato samples. More than 84% of the compounds investigated showed limits of detection equal to or lower than 5 mg kg(-1). A mild (<20%), medium (20-50%), and strong (>50%) matrix effect was observed for 72%, 25%, and 3% of the pesticides studied, respectively. Eighty-one percent of the pesticides showed recoveries ranging between 70% and 120%. Twelve pesticides were detected in 35 samples, all below the maximum residue levels permitted in the Brazilian legislation; 15 samples exceeded the maximum residue levels established by the EU legislation for methamidophos; and 10 exceeded limits for acephate and four for bromuconazole. PMID:25577051

  3. Multiresidue Method for Determination of 183 Pesticide Residues in Leeks by Rapid Multiplug Filtration Cleanup and Gas Chromatography-Tandem Mass Spectrometry.

    PubMed

    Zou, Nan; Han, Yongtao; Li, Yanjie; Qin, Yuhong; Gu, Kejia; Zhang, Jingru; Pan, Canping; Li, Xuesheng

    2016-08-10

    This study reports the development of a novel multiplug filtration cleanup (m-PFC) procedure for analysis of pesticide residues in leek samples followed by gas chromatography-tandem mass spectrometry detection. The leek samples were initially purified following the dispersive solid-phase extraction with different sorbents to determine the most suitable proportioning of sorbent materials; then, the m-PFC method was carried out by applying the streamlined procedure with syringes. Average recoveries of most pesticides were in the range from 70.2 to 126.0% with the relative standard deviation < 20% with the m-PFC process. The limits of detection were 0.03-3.3 μg kg(-1). The limits of quantification were 0.1-10 μg kg(-1). The m-PFC process is convenient and time-efficient, taking just a few seconds per sample. Finally, the developed method was successfully applied to the determination of pesticide residues in market samples. In that analysis, 35 pesticides were detected in 29 samples, with values ranging from 2.0 to 9353.1 μg kg(-1). PMID:26651870

  4. Atmospheric Aging of Semi-volatile Pesticides: Real Time Monitoring of Cypermethrin Photo- oxidation Using FTIR

    NASA Astrophysics Data System (ADS)

    Segal-Rosenheimer, M.; Dobuwski, Y.

    2007-12-01

    Pesticides are highly toxic compounds that unlike other pollutants are intentionally introduced, in large quantities, to the environment. The vast majority of them are applied to agricultural lands, but they are also widely used in urban areas as herbicides, insecticides and fungicides. Pesticides may be promoted into the atmosphere during their application via drift of aerosols, as well as by volatilization or dust erosion from treated surfaces after application. In the atmosphere, semi-volatile pesticides may remain as pure aerosols or become adsorbed upon background aerosols or surfaces. During transport or as deposited thin films, they undergo chemical degradation processes due to interaction with atmospheric oxidants and/or solar radiation. Although previous studies indicate that a major portion of applied pesticides wind up in the atmosphere, this is the medium about which we know the least regarding pesticides' fate. Quantitative data regarding aging processes of these hazard air pollutants are important in order to asses their environmental fate and impact. The present study investigates the heterogeneous reaction of thin film of cypermethrin, a common used insecticide, with atmospheric ozone and UV radiation. The reactions are monitored in real time using novel apparatus that combines ATR/FTIR and Long-path IR gas cell for examining the condensed and gas phases, respectively. The obtained data, including oxidation rate constants and photochemical quantum yields, are used to determine atmospheric lifetime of cypermethrin and its probability to reach non-target regions. Kinetic results from the oxidation of cypermethrin with different concentrations of ozone show that its atmospheric half-life time, with regard to ozone, is in the same order of magnitude as other known degradation processes in the soil and water compartments. Also is shown that some of the condensed phase products are more water soluble than the parent molecule, hence having higher potential

  5. Residue levels of organochlorine pesticides in some ecosystem components of Manzala Lake.

    PubMed

    Azab, M M; Darwish, A A; Mahmoud, Hend A; Sdeek, Fayza A

    2013-12-01

    To evaluate the organochlorine pesticide (OCP) contamination of Manzala Lake, its ecosystem was investigated during the winter season (December to March). The studied ecosystem components were water, sediment, aquatic weeds, and fishes in four locations. The samples were analyzed by gas chromatography with electron capture detector. Pollutant levels of total OCPs showed significantly high levels in the water areas of Round road (46.253 ng/ml), Port-Said Damietta road (19.301 ng/ml), followed by Bughas El-Rasoah (5.539 ng/ml), then Ashtoum El Gamel (natural reserve area now) (0.289 ng/ml). Organochlorines were detected in sediment only in Round road (3.359 μg/kg) and Port-Said Damietta road (0.171 μg/kg) by significant order while they were undetectable in Ashtoum El Gamel and Bughas El-Rasoah. Total OCPs in aquatic weeds ranged between 0.194 μg/kg in Port-Said Damietta and 0.026 μg/kg in Ashtoum El Gamel. While OCPs were 0.160 and 0.153 μg/kg in Round road and Bughas El-Rasoah, respectively. Concerning fish muscles OCPs were significantly higher in the Round road area (0.397 μg/kg) followed by the Port-Said Damietta road (0.258 μg/kg), and finally, Ashtoum El Gamel samples (0.126 μg/kg). The results revealed the direct relation for the accumulation of OCPs between studied ecosystem parameters at the Manzala Lake during the winter season. Results also demonstrated that fish samples collected from the Manzala Lake in the studied areas were contaminated with levels of organochlorines, not higher than the maximum permissible level recorded by FAO/WHO, and that the public is not at risk with fish consumption. PMID:23884913

  6. Residues of polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and organochlorine pesticides in organically-farmed vegetables.

    PubMed

    Zohair, Azza; Salim, Abou-Bakr; Soyibo, Adeola A; Beck, Angus J

    2006-04-01

    The residues of polyaromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) in soils from organic farms and their uptake by four varieties of organic-produced potatoes and three varieties of organic carrots from England were investigated. Samples of the soils, crop peels and cores were all Soxhlet-extracted in triplicate, cleaned up by open-column chromatography and analysed by a multi-residue analytical method using gas chromatography with mass selective detection. The concentrations of PAHs, PCBs and OCPs in soils from organic farms ranged from 590+/-43 to 2301+/-146 microg/kg, 3.56+/-0.73 to 9.61+/-1.98 microg/kg and 52.2+/-4.9 to 478+/-111 microg/kg, respectively. Uptake by different crop varieties were 8.42+/-0.93 to 40.1+/-4.9 microg/kg sigmaPAHs, 0.83+/-0.19 to 2.68+/-0.94 microg/kg sigmaPCBs and 8.09+/-0.83 to 133+/-27 microg/kg sigmaOCPs. Residue uptake from soils depended on plant variety; Desiree potato and Nairobi carrot varieties were more susceptible to PAH contamination. Likewise, uptake of PCBs and OCPs depended on potato variety. There were significant positive correlations between the PCB and OCP concentrations (P<0.05) in soils and carrots but no significant correlation was found between the concentrations of any contaminants in soils and potatoes. Peeling carrots and potatoes was found to remove 52-100% of the contaminant residues depending on crop variety and the properties of the contaminants. Soil-crop bioconcentration factors (BCFs) decreased with increasing logK(ow) for PAHs up to about 4.5 and for PCBs up to about 6.5, above which no changes were discernible for either class of contaminants. No relationship was observed between soil-crop BCFs and logK(ow) for OCPs, most likely because their concentrations were low and variable. PMID:16297429

  7. Residues of organochlorine pesticides and polychlorinated biphenyls and autopsy data for bald eagles, 1973-74.

    PubMed

    Prouty, R M; Reichel, W L; Locke, L N; Belisle, A A; Cromartie, E; Kaiser, T E; Lamont, T G; Mulhern, B M; Swineford, D M

    1977-12-01

    Eighty-six bald eagles found sick or dead during 1973-74 in 24 States were analyzed for organochlorine compounds. DDE was detected in all caracasses; polychlorinated biphenyls (PCB's) were found in all but two. Seventy-five carcasses contained TDE and/or dieldrin. Four eagles had possibly lethal levels of dieldrin in the brain. Bald eagles continue to retain high residue levels of organochlorine pollutants. Illegal shooting remained the most common cause of death but accounted for a smaller percentage of the mortalities than in the two previous biennial collections. PMID:416416

  8. Determination of organochlorine pesticide residue levels in chewable parts of the khat (Catha edulis) plant.

    PubMed

    Ligani, Shemsu; Hussen, Ahmed

    2014-11-01

    In this study, the levels of DDT and its metabolite residues were determined in chewable parts of Catha edulis plants grown in the southern part of Ethiopia. The levels of p,p'-DDT and p,p'-DDE were found to be in the range of 10.8-19.7 and 3.5-18.6 μg/kg, respectively. These data revealed that the residue being detected is from recent applications. The estimated daily intake of total DDT from C. edulis consumption was calculated to be in the range between 0.0278 and 0.0747 μg/kg, which is significantly lower than the FAO/WHO guideline. However, this may not guarantee safety, as the application of DDT extends to vegetables as well. Even though the use of DDT was banned in Ethiopia for agriculture purposes, detectable levels are still being observed. The results of the study necessitate the need for awareness creation among the people in the community. PMID:25260995

  9. Pesticides and total polychlorinated biphenyls residues in raw and cooked walleye and white bass harvested from the Great Lakes

    SciTech Connect

    Zabik, M.E.; Booren, A.M.; Daubenmire, S.; Pascall, M.A.; Zabik, M.J.; Welch, R.; Humphrey, H.

    1995-03-01

    To provide data for public health and other government officials to quantitate the degree of exposure a human might receive from consumption of commonly sought open water fish species prepared and cooked by commonly used methods, five species of Great Lakes fish were chosen. Data is presented for walleye harvested from Lakes Erie, Huron and Michigan which were baked and char-broiled as skin-on fillets with additional walleye from Lake Michigan being deep fat fried. Skin-on white bass fillets from Lakes Erie and Huron also were pan fried. Packed column PCB and pesticide analyses were conducted for all fish species by the Michigan Department of Public Health. The DDT complex (p,p{prime}DDT, p,p{prime}DDE and p,p{prime}DDD), dieldrin, hexa-chlorobenzene (HCB), chlorodane complex (alpha and gamma chlordane, oxychlordane, cis- and trans-nonachlor), toxaphene, heptachlor epoxide, and total PCBs (expressed as Arochlor{sup R} 1254) were found at above the minimum level of detection for many of the species studied. Residues were expressed as ppm wet tissue and then converted to micrograms per fillet to calculate the percentage loss due to cooking. 9 refs., 3 tabs.

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

    PubMed

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

    2013-01-01

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

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

    PubMed

    Wang, Ligang; Liang, Yongchao; Jiang, Xin

    2008-10-01

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

  12. Microflow liquid chromatography coupled to mass spectrometry--an approach to significantly increase sensitivity, decrease matrix effects, and reduce organic solvent usage in pesticide residue analysis.

    PubMed

    Uclés Moreno, Ana; Herrera López, Sonia; Reichert, Barbara; Lozano Fernández, Ana; Hernando Guil, María Dolores; Fernández-Alba, Amadeo Rodríguez

    2015-01-20

    This manuscript reports a new pesticide residue analysis method employing a microflow-liquid chromatography system coupled to a triple quadrupole mass spectrometer (microflow-LC-ESI-QqQ-MS). This uses an electrospray ionization source with a narrow tip emitter to generate smaller droplets. A validation study was undertaken to establish performance characteristics for this new approach on 90 pesticide residues, including their degradation products, in three commodities (tomato, pepper, and orange). The significant benefits of the microflow-LC-MS/MS-based method were a high sensitivity gain and a notable reduction in matrix effects delivered by a dilution of the sample (up to 30-fold); this is as a result of competition reduction between the matrix compounds and analytes for charge during ionization. Overall robustness and a capability to withstand long analytical runs using the microflow-LC-MS system have been demonstrated (for 100 consecutive injections without any maintenance being required). Quality controls based on the results of internal standards added at the samples' extraction, dilution, and injection steps were also satisfactory. The LOQ values were mostly 5 μg kg(-1) for almost all pesticide residues. Other benefits were a substantial reduction in solvent usage and waste disposal as well as a decrease in the run-time. The method was successfully applied in the routine analysis of 50 fruit and vegetable samples labeled as organically produced. PMID:25495653

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

    PubMed

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

    2011-12-01

    A superficial water quality survey in a watershed of the Paraíba do Sul River, the main water supply for the most populated cities of southeastern Brazil, was held in order to assess the impact of the expansion of agricultural activity in the near border of the Atlantic Rain Forest. The aim of this study was to investigate the presence of priority organochlorine pollutants in soils and superficial waters of Atlantic rainforest fragments in Teresópolis, Rio de Janeiro State. Soil sample preparations were compared by using ultrasound, microwave assisted extraction and Soxhlet extraction. Recoveries of matrix spiked samples ranged from 70 to 130%. Analysis of a certified soil material showed recoveries ranging from 71 to 234%. Although low concentrations of organochlorine residues were found in water and soil samples, this area is of environmental importance and concern, thus demanding a monitoring program of its compartments. PMID:21864959

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

    PubMed

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

    2014-11-01

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

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

    PubMed

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

    2016-02-26

    A method for the determination of 200 pesticides and pesticide metabolites in honeybee samples has been developed and validated. Almost 98% of compounds included in this method are approved to use within European Union, as active substances of plant protection products or veterinary medicinal products used by beekeepers to control mites Varroa destructor in hives. Many significant metabolites, like metabolites of imidacloprid, thiacloprid, fipronil, methiocarb and amitraz, are also possible to detect. The sample preparation was based on the buffered QuEChERS method. Samples of bees were extracted with acetonitrile containing 1% acetic acid and then subjected to clean-up by dispersive solid phase extraction (dSPE) using a new Z-Sep+ sorbent and PSA. The majority of pesticides, including neonicotionoids and their metabolites, were analyzed by liquid chromatography tandem mass spectrometry (LC-MS/MS) but some of pesticides, especially pyrethroid insecticides, were analyzed by gas chromatography tandem mass spectrometry (GC-MS/MS). The procedure was validated according to the Guidance document SANCO/12571/2013 at four concentration levels: 1, 5, 10 and 100 ng/g bees and verified in the international proficiency test. The analysis of bee samples spiked at the limit of quantification (LOQ) showed about 98% mean recovery value (trueness) and 97% of analytes showed recovery in the required range of 70-120% and RSDr (precision) below 20%. Linearity and matrix effects were also established. The LOQs of pesticides were in the range of 1-100 ng/g. The developed method allows determination of insecticides at concentrations of 10 ng/g or less, except abamectin and tebufenozide. LOQ values are lower than the median lethal doses LD50 for bees. The method was used to investigate more than 70 honeybee poisoning incidents. Data about detected pesticides and their metabolites are included. PMID:26830634

  16. Pesticide residues in chicken eggs - A sample preparation methodology for analysis by gas and liquid chromatography/tandem mass spectrometry.

    PubMed

    Hildmann, Fanny; Gottert, Christina; Frenzel, Thomas; Kempe, Guenther; Speer, Karl

    2015-07-17

    A sample preparation method was developed for the analysis of chicken eggs to determine 97 GC and 81 LC amenable residues, including organophosphates, organochlorines, pyrethroids, triazoles, carboxyl-containing compounds, and the indicator PCBs. Hereby, considerations were given to the recoveries of the analytes, the method's suitability for routine analysis, and the assessment of the clean-up effect, for which a simple thin layer chromatography was implemented to visualize the most important lipid classes. The procedure consisted of (I) the extraction by matrix solid phase dispersion, and the clean-up by means of (II) small-scale gel permeation chromatography (GPC) and (III) two different solid phase extractions (SPE) for GC and LC amenable analytes, as well as (IV) the quantification using GC-MS/MS and LC-MS/MS. Cyclohexane/ethyl acetate was chosen as extraction solvent due to its suitability for extracting strong non-polar but also more polar analytes. The classical GPC was scaled down to ensure a 50% lower solvent consumption. The comprehensive investigation of conventional and modern zirconium-oxide-coated SPE materials resulted in the selection of octadecyl-modified silica (C18) combined with primary secondary amine using acetonitrile as elution solvent for GC amenable analytes and pure C18 in combination with acidified methanol for LC amenable pesticides. Compared to the currently established EN 1528 method the sample preparation proposed offered a higher sample throughput and a lower solvent consumption. Furthermore, for the first time the clean-up effectiveness of the sample preparation steps was documented as shown by means of thin-layer chromatography. The validation of chicken eggs proved the fulfillment of the quality control criteria for 164 of the 178 analytes tested, mostly at the lowest validated level of 5μg/kg for pesticides and 0.5μg/kg for the single indicator PCBs. However, the analysis of strongly polar analytes was still problematic

  17. Prepubertal Organochlorine Pesticide Concentrations and Age of Pubertal Onset Among Russian Boys

    PubMed Central

    Lam, Thuy; Williams, Paige L.; Lee, Mary M.; Korrick, Susan A.; Birnbaum, Linda S.; Burns, Jane S.; Sergeyev, Oleg; Revich, Boris; Altshul, Larisa M.; Patterson, Donald G.; Turner, Wayman E.; Hauser, Russ

    2014-01-01

    Background In animal studies, organochlorine pesticide (OCP) exposure alters pubertal development, however, epidemiological data are limited and inconsistent. Objective To evaluate the associations of serum OCP concentrations [hexachlorobenzene (HCB), β-hexachlorocylohexane (β-HCH), and p,p′-dichlorodiphenyldichloroethylene (p,p′-DDE)] with male pubertal onset. Methods In Chapaevsk, Russia, a town environmentally contaminated with OCPs, 350 8–9 year old boys with measured OCPs were enrolled during 2003–2005 and were followed annually for eight years. We evaluated three measures of pubertal onset: testicular volume (TV) > 3 mL in either testis, or stage 2 or greater for genitalia (G2+), or pubic hair (P2+). We used multivariable interval-censored models to evaluate associations of OCPs (quartiles) with physician-assessed pubertal onset. Results In adjusted models, boys with higher HCB concentrations had later mean ages of TV > 3 mL and P2+ (but not G2+). Mean age at attaining TV > 3 mL was delayed 3.6 (95% CI: −2.6, 9.7), 7.9 (95% CI: 1.7, 14.0), and 4.7 months (95% CI: −1.4, 10.9) for HCB Q2, Q3, and Q4, respectively, compared to Q1 (trend p: 0.06). Boys with higher HCB concentrations reached P2+ 0.1 months earlier (95% CI: −5.8, 5.6) for Q2, 4.7 months later (95% CI: −1.0, 10.3) for Q3 and 4.6 months later (95% CI: −1.1, 10.3) for Q4 compared to Q1 (trend p: 0.04). There were no associations of serum β-HCH and p,p′-DDE concentrations with age of pubertal onset. Conclusion Higher prepubertal serum HCB concentrations were associated with later age of gonadarche and pubarche. PMID:25118086

  18. A multi-residue method for characterization and determination of atmospheric pesticides measured at two French urban and rural sampling sites.

    PubMed

    Baraud, Laurent; Tessier, Didier; Aaron, Jean-Jacques; Quisefit, Jean-Paul; Pinart, Johann

    2003-12-01

    The extensive use of pesticides to protect agricultural crops can result in the transfer of these compounds into the atmosphere and their diffusion towards urban areas. Precise evaluation of the geographic impact of this type of pollution is important environmentally. In this paper, analytical methods for the sampling, characterization, and determination of agricultural pesticides in air were developed; the methods were then applied in the Paris and Champagne regions. Sixteen pesticides belonging to nine chemical families were monitored. Sampling was carried out in urban (Paris) and rural (Aube district) sites, utilizing either a high-volume pump (12.5 m3 h(-1)) (urban site) or a low-volume pump (2.3 m3 h(-1)) for the rural site. Quartz filters and polyurethane foams (PUF) were used for sampling in all cases. After extracting the samples and concentrating the recovered solutions, high-performance liquid chromatography (HPLC) analysis with UV detection was performed. Identification of the pesticides was confirmed by applying to the HPLC measurements a novel UV-detection procedure based on the normalized absorbance variation with wavelength (Noravawa procedure). The presence of metsulfuron methyl, isoproturon, linuron, deltamethrin (and/or malathion), and chlorophenoxy acids (2,4-D and MCPP) was found at the urban sampling site at levels ranging from about 1 to 1130 ng m(-3) of air, depending on the compound and sampling period. On the rural sampling site residues of isoproturon, deltamethrin (and/or malathion), MCPP, and 2,4-D were generally detected at higher levels (19-5130 ng m(-3)) than on the urban site, as expected. The effects of the weather conditions and agricultural activity on the atmospheric concentrations of pesticides are discussed, as are long-range atmospheric transfer processes for these pesticides. PMID:13680058

  19. Organochlorine pesticide residuals in chickens and eggs at a poultry farm in Beijing, China.

    PubMed

    Tao, S; Liu, W X; Li, X Q; Zhou, D X; Li, X; Yang, Y F; Yue, D P; Coveney, R M

    2009-02-01

    Chicken organs, animal feed, droppings, and ambient air were sampled at a farm in Beijing to determine the concentrations of hexachlorocyclohexane isomers (HCHs) and dichlorodiphenyltrichloroethane and metabolites (DDTs). Mean fresh weight concentrations of HCHs and DDTs were 0.122+/-0.061 ng/g and 0.051+/-0.038 ng/g in the muscles. These values are 1-2 orders of magnitude lower than those reported in China in 1980. Contaminated feed was the main source of HCHs and DDTs. Only 12.8% of HCH and 3.3% of DDT of the amount consumed were excreted. Accumulated quantities of HCHs and DDTs increased during growth. However, concentrations of HCHs and DDTs did not increase because of dilution from rapid growth. Based on the observed residual levels in mature chicken and the average diet of residents of China, the contributions from chicken and egg consumption to per capita daily intake of HCHs and DDTs were 487% and 88% of those of fish consumption. PMID:18963306

  20. High-throughput pesticide residue quantitative analysis achieved by tandem mass spectrometry with automated flow injection.

    PubMed

    Nanita, Sergio C; Pentz, Anne M; Bramble, Frederick Q

    2009-04-15

    The use of automated flow injection with MS/MS detection for fast quantitation of agrochemicals in food and water samples was demonstrated in this study. Active ingredients from the sulfonylurea herbicide and carbamate insecticide classes were selected as model systems. Samples were prepared using typical procedures from residue methods, placed in an autosampler, and injected directly into a triple quadrupole instrument without chromatographic separation. The technique allows data acquisition in 15 s per injection, with samples being injected every 65 s, representing a significant improvement from the 15-30 min needed in typical HPLC/MS/MS methods. The availability of HPLC systems is an advantage since they can be used in flow-injection mode (bypassing the column compartment). Adequate accuracy, linearity, and precision (R(2) > 0.99 and RSD < 20%) were obtained using external standards prepared in each control matrix. The limit of quantitation (LOQ) achieved for all analytes was 0.01 mg/kg in food samples and 0.1 ng/mL in water; while limits of detection (LOD) were estimated to be about 0.003 mg/kg and 0.03 ng/mL in food and water, respectively. The advantages and limitations of flow injection MS/MS for ultratrace-level quantitative analysis in complex matrixes are discussed. PMID:19296591