Science.gov

Sample records for aged pesticide residues

  1. 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

  2. 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.

  3. Pesticidal residues in animal tissues

    USGS Publications Warehouse

    DeWitt, J.B.; Menzie, C.M.; Adomaitis, V.A.; Reichel, W.L.

    1960-01-01

    Tests with penned starlings, rats, pheasants, and ducks indicated that each species differs in sensitivity to the various pesticides. Residues in tissues are proportional to the degree of exposure during area treatment and they are also found in animals shot six or more months after treatment. The presence of more than 20-30 ppm of DDT, 20 ppm of chlordan, and 6-20 ppm of heptachlor epoxide in quail tissues indicated that the birds had ingested lethal dosages of the pesticides.

  4. Pesticide residues in olive oil.

    PubMed

    Lentza-Rizos, C; Avramides, E J

    1995-01-01

    The attacks of pests and diseases and the presence of weeds make it necessary to apply pesticides to olive trees to ensure crop protection. Residues of these compounds may remain and contaminate the oil produced. For the analysis of pesticide residues in olive oil, the most common methods are multiresidue methods for fatty substrates, based on partitioning between hexane or light petroleum and acetonitrile. Recently, other methods have been applied, such as ready-to-use, disposable minicolumns or direct injection of oil into a capillary gas chromatograph equipped with a precolumn with an oil recovery tank. Although several pesticides are registered in oil-producing countries for use on olive trees, available literature on the level and fate of residues is very limited. However, it is clear that fat-soluble pesticides tend to concentrate in the oil, both after full coverage and bait spraying, and their use close to harvest should therefore be avoided. Because it is sometimes necessary to use such pesticides late in autumn because of their effectiveness in cases of severe attack, residue trials should be carried out to determine the residue concentration in oil and to set a reasonable preharvest safety interval. Data produced by such trials would permit the establishment of MRLs (tolerances) in olive oil to cover cases where the residues, although relatively high, are not of toxicological significance for consumers (risk assessment). Such is the case with corn oil and the fat-soluble insecticide methyl pirimiphos, registered in the U.S. for use on corn. The U.S. EPA tolerance for methyl pirimiphos in corn is 8 mg/kg, whereas it is 11 times higher (88 mg/kg) for corn oil because it is known to concentrate in the oil. Similar provisions for olive oil, based on data from residue trials according to Good Agricultural Practice, the long-term toxicity of each pesticide as expressed by its ADI for man, and olive oil consumption patterns, would facilitate international trade

  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. 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.…

  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 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 ...

  9. 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

  10. Determination of Pesticide Residues in Cannabis Smoke

    PubMed Central

    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

  11. 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.

  12. 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...

  13. 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...

  14. 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...

  15. 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...

  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. Pesticide residue levels in Argentinian pasteurised milk.

    PubMed

    Maitre, M I; de la Sierra, P; Lenardon, A; Enrique, S; Marino, F

    1994-10-14

    Pasteurised milk--120 samples--was analysed (in Santa Fe City, Argentina) to determine organochlorinated pesticides. Almost all samples showed the presence of such residues; the compounds more frequently detected being: heptachlor and its epoxide (98%) and hexachlorocyclohexane .HCH. alpha and gamma isomers. Residues of aldrin and dieldrin; chlordane (alpha and gamma); endosulfan (I and II); DDT (o,p-DDT, p,p'-DDE, o,p-DDD, p,p'-DDD) as well as hexachlorocyclobenzene (HCB) were also found. Despite their presence high concentrations are sporadic, the mean values being less than FAO/OMS tolerance limits. Relations between maxima concentrations and seasons were not found.

  18. 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)

  19. Pesticide residues in birds and mammals

    USGS Publications Warehouse

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

    1973-01-01

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

  20. Evaluation of pesticide residues in fruits and vegetables from Algeria.

    PubMed

    Mebdoua, Samira; Lazali, Mohamed; Ounane, Sidi Mohamed; Tellah, Sihem; Nabi, Fahima; Ounane, Ghania

    2017-06-01

    A total of 160 samples of 13 types of fresh fruits and vegetables from domestic production and import were analysed to detect the presence of pesticide residues. Analysis was performed by multi-residual extraction followed by gas chromatography-mass spectrometry. In 42.5% of the tested samples, no residues were found and 12.5% of samples contained pesticide residues above maximum residue limits. Risk assessment for long-term exposure was done for all pesticides detected in this study. Except chlorpyrifos and lambda-cyhalothrin, exposure to pesticides from vegetables and fruits was below 1% of the acceptable daily intake. Short-term exposure assessment revealed that in seven pesticide/commodity combinations, including three pesticides (chlorpyrifos, deltamethrin and lambda-cyhalothrin), the acute reference dose had been exceeded.

  1. [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.

  2. 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

    ... AGENCY 40 CFR Part 180 Withdrawal of a Pesticide Petition for Residues of Pesticide Chemicals in or on... establishment or modification of regulations for residues of pesticide chemicals in or on various commodities... regulations in 40 CFR part 174 or part 180 for residues of pesticide chemicals in or on various...

  3. 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.

  4. 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...

  5. 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....

  6. 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

    ... AGENCY Notice of Withdrawal of Pesticide Petitions for Residues of Pesticide Chemicals in or on Various... withdrawal of pesticide petitions (0G7716, 8F7489, 9E7635, and 9F7587) proposing the establishment or modification of regulations for residues of pesticide chemicals in or on various commodities. The...

  7. 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.

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

    PubMed

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

    2014-02-01

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

  9. Residues of organochlorine pesticides in surface soil and raw ...

    EPA Pesticide Factsheets

    The central Asian Republic of Tajikistan has been an area of extensive historical agricultural pesticide use as well as large scale burials of obsolete banned chlorinated insecticides. The current investigation was a four year study of legacy organochlorine pesticides in surface soil and raw foods in four rural areas of Tajikistan. The four study areas included the pesticide burial sites of Konibodom and Vakhsh, and family farms of Garm and Chimbuloq villages. These areas were selected to represent a diversity of pesticide disposal histories and to allow assessment of local pesticide contamination in Tajikistan. Each site was visited multiple times and over 500 samples of surface soil and raw foods were collected and analyzed for twenty legacy organochlorine pesticides. Various local food products were sampled to represent the range of raw foods potentially containing residues of banned pesticides, including dairy products, meat, edible plant and cotton seed products. The pesticide analytes included DDTs (DDT, DDD, DDE), lindane isomers (α, β, γ, δ BHC), endosulfan isomers (endosulfan I, II, sulfate), other cyclodienes (aldrin, α and γ chlordanes, dieldrin, endrin, endrin aldehyde and ketone, heptachlor, heptachlor epoxide), and methoxychlor. Pesticide analytes were selected based on availability of commercial standards and known or suspected historical pesticide use and burial. Pesticide contamination was highest in soil at each of the four sites, and ge

  10. Setting Tolerances for Pesticide Residues in Foods

    EPA Pesticide Factsheets

    Pesticides are widely used in producing food and may remain in small amounts in or on fruits, vegetables, grains, and other foods. EPA ensures the safety of the food supply regulating the amount of pesticide that may remain on food. Learn how we do this.

  11. Pesticide residues in cereal crop grains in Poland in 2013.

    PubMed

    Malinowska, Elżbieta; Jankowski, Kazimierz; Sosnowski, Jacek; Wiśniewska-Kadżajan, Beata

    2015-06-01

    This paper presents the results of the audit on pesticide residues in cereal grains throughout Poland in 2013. The number of all samples of cereal grains was 380. Altogether 292 active substances of plant protection products were checked in the audit. Qualitative and quantative analyses were done according to Polish Standard PN-EN 15562:2008, using the LC-MS/MS technique. The methods (QuEChERS) is based on extraction of residues of plant protection products from a sample using acetonitrile. In the samples analyzed, 62 % of them did not contain any pesticide residues, 34 % of samples of cereal grains contained such residues but below the maximum residue limit, 3 % contained residues over the maximum limit, whereas 1 % of the samples contained illegal substances. The lowest amounts of pesticide residues were found in cereal grains coming from fields with cereal mixtures and in Avena grains, while the highest amounts were in Hordeum and Triticum grains. The substances found most often were fungicide residues. In northern and southern regions of Poland (Silesian, Pomeranian, and Kuyavian-Pomeranian voivodeships), cereal grains with pesticide residues were much more common than in other regions of Poland.

  12. 40 CFR 158.2082 - Experimental use permit biochemical pesticides residue data requirements table.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... pesticides residue data requirements table. 158.2082 Section 158.2082 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Biochemical Pesticides § 158.2082 Experimental use permit biochemical pesticides residue data requirements table. (a)...

  13. 40 CFR 158.2040 - Biochemical 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 Biochemical pesticides residue data... (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Biochemical Pesticides § 158.2040 Biochemical pesticides residue data requirements table. (a) General. Sections 158.100 through 158.130 describe how to...

  14. 40 CFR 158.2082 - Experimental use permit biochemical pesticides residue data requirements table.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... pesticides residue data requirements table. 158.2082 Section 158.2082 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Biochemical Pesticides § 158.2082 Experimental use permit biochemical pesticides residue data requirements table. (a)...

  15. 40 CFR 158.2040 - Biochemical 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 Biochemical pesticides residue data... (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Biochemical Pesticides § 158.2040 Biochemical pesticides residue data requirements table. (a) General. Sections 158.100 through 158.130 describe how to...

  16. 40 CFR 158.2040 - Biochemical 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 Biochemical pesticides residue data... (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Biochemical Pesticides § 158.2040 Biochemical pesticides residue data requirements table. (a) General. Sections 158.100 through 158.130 describe how to...

  17. 40 CFR 158.2082 - Experimental use permit biochemical pesticides residue data requirements table.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... pesticides residue data requirements table. 158.2082 Section 158.2082 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Biochemical Pesticides § 158.2082 Experimental use permit biochemical pesticides residue data requirements table. (a)...

  18. 40 CFR 158.2082 - Experimental use permit biochemical pesticides residue data requirements table.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... pesticides residue data requirements table. 158.2082 Section 158.2082 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Biochemical Pesticides § 158.2082 Experimental use permit biochemical pesticides residue data requirements table. (a)...

  19. 40 CFR 158.2040 - Biochemical 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 Biochemical pesticides residue data... (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Biochemical Pesticides § 158.2040 Biochemical pesticides residue data requirements table. (a) General. Sections 158.100 through 158.130 describe how to...

  20. 40 CFR 158.2082 - Experimental use permit biochemical pesticides residue data requirements table.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... pesticides residue data requirements table. 158.2082 Section 158.2082 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Biochemical Pesticides § 158.2082 Experimental use permit biochemical pesticides residue data requirements table. (a)...

  1. 40 CFR 158.2040 - Biochemical 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 Biochemical pesticides residue data... (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Biochemical Pesticides § 158.2040 Biochemical pesticides residue data requirements table. (a) General. Sections 158.100 through 158.130 describe how to...

  2. 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

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

    PubMed Central

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

    2014-01-01

    Few studies have investigated organochlorine pesticide residue content in freshwater plankton communities in Thailand. As a result, this study looks to examine the concentration of organochlorine pesticide residues in plankton collected from Khlong 7 (canal) at Rangsit agricultural area, central Thailand from June 2006 to February 2007. The results from this study show that plankton communities were composed of microphytoplankton, microzooplankton, and mesozooplankton. The average method recoveries varied from 84% to 103% with a relative standard deviation between 0.20% and 3.72%. The concentrations of organochlorine pesticide residues during a one-year-period were in the range of 0.10–3.65 ng/g wet wt and contained DDT and derivatives > Σ endosulfan > Σ HCH > Σ heptachlor > aldrin and dieldrin > endrin and endrin aldehyde > methoxychlor, respectively. Moreover, the residues of Σ HCH, DDT and derivatives, and methoxychlor were higher during wet season than dry season (t-test, p ≤ 0.05). PMID:18777151

  4. Organochlorine pesticide residues in plankton, Rangsit agricultural area, central Thailand.

    PubMed

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

    2008-12-01

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

  5. Pesticide residues in essential oils: evaluation of a database.

    PubMed

    Klier, B; Knödler, M; Peschke, J; Riegert, U; Steinhoff, B

    2015-01-01

    In the context of a revision of the European Pharmacopoeia (Ph. Eur.) general monograph Essential oils (2098), the need to include a test for pesticides is being discussed. According to published literature, some oils, mainly those produced by cold pressing (e.g. citrus oils), can contain relevant amounts of pesticide residues, whereas distilled oils showed positive findings in only a few cases. Recent evaluation of a database containing 127 517 sets of data compiled over 8 years, showed positive results in 1 150 cases (0.90 per cent), and the limits of Ph. Eur. general chapter 2.8.13 Pesticide residues or Regulation (EC) 396/2005, both applicable to herbal drugs, were exceeded in 392 cases (0.31 per cent, equivalent to 34.1 per cent of the positive results), particularly in cases of oils produced by cold pressing. From these results, it can be concluded that a general test on pesticides in the Ph. Eur. general monograph on essential oils is not required for most oils used in medicinal products. Therefore, it is proposed to limit the testing of essential oils for pesticide residues to those cases where potential residues are more of a concern, either due to the type of production process or to those processes where pesticides are actively used during cultivation of the plant (e.g. as documented according to Good Agricultural and Collection Practice (GACP)). Furthermore, in order to assess any potential risk, an approach using the Acceptable Daily Intake (ADI) can be made.

  6. Organochlorine and organophosphorus pesticide residues in food from Egyptian local markets.

    PubMed

    Dogheim, S M; Gad Alla, S A; el-Syes, S M; Almaz, M M; Salama, E Y

    1996-01-01

    A market basket survey was conducted to monitor organochlorine and organophosphorus pesticide residues in potatoes, citrus fruits, and fish collected from local Egyptian markets. Maximum Residue Limits (MRLs) of the Codex Committee on Pesticide Residues for gamma-hexachlorocyclohexane (HCH) in potatoes were exceeded in 8 samples and for DDT in 2 samples. The aging of HCH and DDT indicated a recent use of both pesticides during the potato storage period between cultivation seasons. However, such use is illegal because HCH mixture isomers (gammaxane) and DDT have been officially prohibited from agricultural use in Egypt since 1980. The highest residue levels of fenitrothion (3.8 ppm) in potatoes may be due to its repeated use before and after harvest. No organochlorine pesticide residues were found in citrus fruits. None of the detected organophosphorus pesticides exceeded their MRLs. HCH and DDT residue limits were exceeded in 5 and 7 fish samples, respectively, collected from 12 markets throughout the country. The heptachlor MRL was violated in only one fish sample (3.9 ppm).

  7. Organophosphorus pesticide residues in milled rice (Oryza sativa) on the Chinese market and dietary risk assessment.

    PubMed

    Chen, Chen; Li, Yun; Chen, Mingxue; Chen, Zhijun; Qian, Yongzhong

    2009-03-01

    The present study investigates the occurrence of acetylcholinesterase (AChE)-inhibiting organophosphorus (OP) pesticide residues in milled rice samples obtained form local markets in China during the period 2004-2006 and estimates their cumulative exposure. Concentrations of OP pesticides were determined by gas chromatography with flame photometric detection (GC-FPD). The results showed that 9.3% of the samples contained detectable residues of at least one of the seven target OP pesticides (chlorpyrifos, dichlorvos, omethoate, methamidophos, parathion-methyl, parathion and triazophos) mainly used for agriculture in China, with concentrations ranging 0.011-1.756 mg kg(-1). Rice consumption data was obtained from an individual food consumption survey. Relative potency factors (RPFs) for each pesticide were calculated with methamidophos as the index compound (IC), using 1- or 2-year chronic non-observed adverse effect levels (NOAEL) for AChE inhibition, mostly in rat brain, obtained from international evaluations of pesticides. Exposure to AChE-inhibiting pesticides for the population above 7 years old at P99.9 represented 52-94.5% of the acceptable daily intake (ADI) expressed as methamidophos. Estimated exposure for children aged 2-4 and 4-7 years at P99.9 were 119 and 104.3% of the ADI level, respectively. This study suggests that a yearly monitoring program for OP pesticide residues and strict implementation of the national safety standard for milled rice is necessary.

  8. Screening and evaluation of fruit samples for four pesticide residues.

    PubMed

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

    2005-01-01

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

  9. 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.

  10. 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.

  11. 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.

  12. Determination of pesticide residues in sewage sludge: a review.

    PubMed

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

    2010-01-01

    Pesticides are widely applied to protect plants from diseases, weeds, and insect damage, and they usually come into contact with soil where they may undergo a variety of transformations and provide a complex pattern of metabolites. Spreading sewage sludge on agricultural lands has been actively promoted by national authorities as an economic way of recycling. However, as a byproduct of wastewater treatment, sewage sludge may contain pesticides and other toxic substances that could be incorporated into agricultural products or be distributed in the environment. This article reviews the determination of pesticides in sewage sludge samples. Sample preparation including pretreatment, extraction, and cleanup, as well as the subsequent instrumental determination of pesticide residues, are discussed. Extraction techniques such as Soxhlet extraction, ultrasound-assisted extraction, pressurized liquid extraction, supercritical fluid extraction, and matrix solid-phase dispersion and their most recent applications to the determination of pesticides in sewage sludge samples are reviewed. Determination of pesticides, generally carried out by GC and HPLC coupled with different detectors, especially MS for the identification and quantification of residues, is summarized and discussed.

  13. Reduction of pesticide residues in tomatoes and other produce.

    PubMed

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

    2013-03-01

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

  14. 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)

  15. 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

  16. 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.

  17. 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...

  18. 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...

  19. 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...

  20. 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...

  1. 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...

  2. 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...

  3. 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...

  4. 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...

  5. 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...

  6. 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

  7. 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

    1997-12-03

    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.

  8. Organochlorine pesticides residue in lakes of Khorezm, Uzbekistan

    USGS Publications Warehouse

    Rosen, Michael R.; Nishonov, Bakhriddin; Fayzieva, Dilorom; Saito, L.; Lamers, J.

    2009-01-01

    The Khorezm province in northwest Uzbekistan is a productive agricultural area within the Aral Sea Basin that produces cotton, rice and wheat. Various organochlorine pesticides were widely used for cotton production before Uzbekistan's independence in 1991. In Khorezm, small lakes have formed in natural depressions that receive inputs mostly from agricultural runoff. Samples from lake waters and sediments, as well as water from the Amu Darya River (which is the source of most of the lake water) have been analyzed to study variations in the concentrations of organochlorine pesticides residues during the year. Low concentrations of DDT, DDD, DDE, a-HCH and y-HCH compounds were found in water and sediment samples. The concentration of persistent organochlorine pesticides (DDT and HCH) in water and sediment is much lower than the maximum permissible concentrations that exist for water and soil. According to these preliminary results, the investigated lakes in Khorezm appear to be suitable for recreation or for aquaculture.

  9. 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.

  10. The Organochlorine Pesticides Residue Levels in Karun River Water

    PubMed Central

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

    2013-01-01

    Background The organochlorine pesticides (OCPs) are among the most commonly used in water streams around the world. Most of these contaminants are highly hydrophobic and persist in sediments of rivers and lakes. Studies have suggested that OCPs may affect the normal function of the human and wildlife endocrine systems. Objectives The aim of this study is to determine the concentrations of selected organochlorine pesticides residues [OP'DDT, PP'DDT, alderin, dieldrin, heptachlor, (α,ß,γ,δ) HCH, (α, ß) endosulfan and metoxychlor] in samples from Karun River water at Khuzestan province in Iran , by GC-µ-ECD. Materials and Methods Water was extracted with n-hexane and then purified by passing through a glass column packed with Florisil and Na2SO4, which was then eluted with ether: hexane solution v/v. Results In general, all of 12 investigated organochlorine pesticides (OCPs) were detected. Regardless of the kind of OCPs, the highest OCP pollution level in Karun River were seen from August to November 2009 ranging 71.43 – 89.34 µg/L, and the lowest were seen from Dec 2010 to March 2011 at levels of 22.25 - 22.64 µg/L. The highest and lowest mean concentrations of 12 investigated pesticides were ß-Endosulfan and pp' DDT with 28.51and 0.01 µg/L respectively. Conclusions Comparison of total organochlorine pesticides residues concentration with WHO guidelines revealed that the Karun River had total OCPs residues above the probable effect level (0.2-20 µg/L, P < 0.05), which could pose a risk to aquatic life. PMID:24624185

  11. Pesticide residues in fruits and vegetables in Ghana: a review.

    PubMed

    Donkor, Augustine; Osei-Fosu, Paul; Dubey, Brajesh; Kingsford-Adaboh, Robert; Ziwu, Cephas; Asante, Isaac

    2016-10-01

    Pesticides are known to improve agriculture yield considerably leading to an increase in its application over the years. The use of pesticides has shown varying detrimental effects in humans as well as the environment. Presently, enough evidence is available to suggest their misuse and overuse in the last few decades in most developing nations primarily due to lack of education, endangering the lives of farmers as well as the entire population and environment. However, there is paucity of data especially over long durations in Ghana resulting in the absence of effective monitoring programs regarding pesticide application and subsequent contamination in fruits and vegetables. Therefore, this review discusses comprehensively pesticide type and use, importation, presence in fruits and vegetables, human exposure, and poisoning in Ghana. This is to alert the scientific community in Ghana of the need to further research into the potential implications of pesticide residues in food commodities in order to generate a comprehensive and reliable database which is key in drafting policies simultaneous with food regulation, suitable monitoring initiatives, assessment, and education to minimize their effects thereon.

  12. 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.

  13. 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

  14. Design of a novel noninvasive spectrometer for pesticide residues monitor

    NASA Astrophysics Data System (ADS)

    Ren, Zhong; Liu, Guodong; Huang, Zhen

    2014-11-01

    Although the gas or liquid chromatography had been widely used into pesticide residues monitoring, some drawbacks such as time-consuming, complicated operation and especially the destructivity for samples were existed. To overcome the limits of destructive detection methods, the noninvasive detection method based on spectroscopy was used to detect the pesticide residues in this paper. To overcome low resolution and light-efficiency due to the drawbacks of the classical plane and holography concave gratings, a novel noninvasive spectrometer for pesticide residues monitor (PRM) based on volume holography transmission (VHT) grating was designed. Meanwhile, a custom-built splitting light system for PRM based on the VHT grating was developed. In addition, the linear charge coupled device (CCD) with combined data acquisition (DAQ) card and the virtual-PRM based on LabVIEW were respectively used as the spectral acquisition hardware and software-platform. Experimental results showed that the spectral resolution of this spectrometer reached 2nm, and the VHT grating's diffraction efficiency was gotten via the simulation experiment.

  15. 77 FR 3229 - Codex Alimentarius Commission: Codex Committee on Pesticide Residues (CCPR)

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-01-23

    ... No. FSIS-2011-0035] Codex Alimentarius Commission: Codex Committee on Pesticide Residues (CCPR....) positions that will be discussed at the 44th Session of the Codex Committee on Pesticide Residues (CCPR) of... SESSION OF THE CCPR CONTACT: Lois Rossi, Director of Registration Division, Office of Pesticide...

  16. Use of Combined Uncertainty of Pesticide Residue Results for Testing Compliance with Maximum Residue Limits (MRLs).

    PubMed

    Farkas, Zsuzsa; Slate, Andrew; Whitaker, Thomas B; Suszter, Gabriella; Ambrus, Árpád

    2015-05-13

    The uncertainty of pesticide residue levels in crops due to sampling, estimated for 106 individual crops and 24 crop groups from residue data obtained from supervised trials, was adjusted with a factor of 1.3 to accommodate the larger variability of residues under normal field conditions. Further adjustment may be necessary in the case of mixed lots. The combined uncertainty of residue data including the contribution of sampling is used for calculation of an action limit, which should not be exceeded when compliance with maximum residue limits is certified as part of premarketing self-control programs. On the contrary, for testing compliance of marketed commodities the residues measured in composite samples should be greater than or equal to the decision limit calculated only from the combined uncertainty of the laboratory phase of the residue determination. The options of minimizing the combined uncertainty of measured residues are discussed. The principles described are also applicable to other chemical contaminants.

  17. 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.

  18. 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.

  19. 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

  20. 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.

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

    PubMed Central

    LEILI, Mostafa; PIRMOGHANI, Amin; SAMADI, Mohammad Taghi; SHOKOOHI, Reza; ROSHANAEI, Ghodratollah; POORMOHAMMADI, Ali

    2016-01-01

    Background: The objective of this study was to determine the residual concentrations of ethion and imidacloprid in cucumbers grown in greenhouse. The effect of some simple processing procedures on both ethion and imidacloprid residues were also studied. Methods: Ten active greenhouses that produce cucumber were randomly selected. Ethion and imidacloprid as the most widely used pesticides were measured in cucumber samples of studied greenhouses. Moreover, the effect of storing, washing, and peeling as simple processing procedures on both ethion and imidacloprid residues were investigated. Results: One hour after pesticide application; the maximum residue levels (MRLs) of ethion and imidacloprid were higher than that of Codex standard level. One day after pesticide application, the levels of pesticides were decreased about 35 and 31% for ethion and imidacloprid, respectively, which still were higher than the MRL. Washing procedure led to about 51 and 42.5% loss in ethion and imidacloprid residues, respectively. Peeling procedure also led to highest loss of 93.4 and 63.7% in ethion and imidacloprid residues, respectively. The recovery for both target analytes was in the range between 88 and 102%. Conclusion: The residue values in collected samples one hour after pesticides application were higher than standard value. The storing, washing, and peeling procedures lead to the decrease of pesticide residues in greenhouse cucumbers. Among them, the peeling procedure has the greatest impact on residual reduction. Therefore, these procedures can be used as simple and effective processing techniques for reducing and removing pesticides from greenhouse products before their consumption. PMID:28032066

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

    PubMed

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

    2012-11-01

    The objective of this study was to determine the levels of organochlorine pesticides HCB, α-β-γ-HCH, p,p'-DDE, o,p'-DDT and p,p'-DDT in 150 adipose tissue of inhabitants of Tabasco, Mexico. The following pesticides were detected: p,p'-DDE in 100% of samples at mean 1.034 mg/kg; p,p'-DDT in 96.7% at mean 0.116 mg/kg; o,p'-DDT in 78.7% at mean 0.022 mg/kg and β-HCH in 58.0% at mean 0.049 mg/kg. The pooled sample was divided according to sex of donors (75 female and 75 male). Significantly higher levels of all organochlorine pesticides in females were found. The sample was divided into three age's ranges (15-28, 29-45 and 46-84 years). The mean and median levels of β-HCH, p,p'-DDE and Σ-DDT increase significantly (p < 0.05) from the first to the second and third group. The presence of organochlorine pesticide residues in Tabasco inhabitants is still observed, indicating sources of exposure to the pesticides.

  3. LC-MS/MS determination of pesticide residues in fruits and vegetables.

    PubMed

    Stachniuk, Anna; Szmagara, Agnieszka; Czeczko, Renata; Fornal, Emilia

    2017-03-29

    The aim of the research is to evaluate pesticide residue contamination of fresh and frozen fruits and vegetables, agricultural raw material, purchased from Polish farmers for production of frozen fruits and vegetables, and the estimation of the multiresidue method effectiveness expressed as the proportion of pesticides detected in food samples to the total number of pesticides analyzed by multiresidue methods. A total of 144 samples (of black currants, red currants, raspberries, cherries, strawberries, blackberries, cauliflowers and broccoli) were analyzed using LC-MS/MS method for the determination of 60 pesticides. QuEChERS extraction, matrix-matched calibration and dynamic multiple reaction monitoring method were used. Residues of 15 compounds, mainly fungicides and insecticides, were detected in 46 samples. The percentage of samples with residues above the maximum residue levels (MRL) was 15%, whereas samples with residues below MRL were 17%. A total of 13 samples contained more than one pesticide residue. Pesticide residues were detected most often in samples of black currants (50%), broccoli (36.4%), raspberries (29%) and red currants (21.8%). The most frequently detected pesticides were carbendazim and acetamiprid. The proportion of pesticides detected during our study to the total number of analyzed pesticides amounted to 25%. It was compared to literature findings. For three fourth of multiresidue methods, the proportion was below 50% for methods developed for the analysis of less than 100 pesticides, and below 30% for methods developed for the analysis of more than 100 pesticides. It appears that a lot of efforts and means is lost on pesticides never or rarely detected in examined samples. The workload and cost effectiveness of the development and application of multiresidue methods along with the range of pesticides covered by the method should be carefully and thoroughly considered anytime when a new method or workflow is developed. Including non

  4. 78 FR 76589 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-12-18

    ... 25, 2012, and January 16, 2013, concerning a new active ingredient (AI) and several pesticide petitions (PP) filed for residues of pesticide chemicals. The name of an AI was changed during the registration assessment process. This document corrects the name of an AI and also corrects a PP...

  5. A Multi Residue GC-MS Method for Determination of 12 Pesticides in Cucumber

    PubMed Central

    Nasiri, Azadeh; Amirahmadi, Maryam; Mousavi, Zahra; Shoeibi, Shahram; Khajeamiri, Alireza; Kobarfard, Farzad

    2016-01-01

    Cucumber is one of the main vegetables in Iranian food basket. A wide range of pesticides are used for crops protection during the cultivation of vegetables such as cucumber due to heavy pest infestation. Analysis of pesticide residues in food and other environmental commodities have become essential requirement for consumers, producers, and food quality control authorities. This study was aimed at determination of pesticides residues in cucumber as a main vegetable in Iranian food basket. A reliable, rapid and accurate method based on spiked calibration curves and modified QuEChERS sample preparation was developed for determination of 12 pesticide residues in cucumber by gas chromatography-mass spectrometry (GC/MS). The use of spiked calibration standards for constructing the calibration curve substantially reduced adverse matrix-related effects. The recovery of pesticides at 5 concentration levels (n = 3) was in the range of 80.6-112.3. The method was proved to be repeatable with RSD lower than 20%. The limits of detection and quantification for all pesticides were <10 ng/g and <25 ng/g, respectively. The developed method was used for simultaneous determination of the selected pesticides in 60 greenhouse and garden cucumber samples. Among the 60 analyzed samples, 41.7% of them were contaminated with pesticide residues which 31.7% of samples had pesticide residues lower than maximum residue limit and 10% of samples had residue higher than maximum residue limit. PMID:28243277

  6. 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

  7. 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...

  8. 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...

  9. 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...

  10. 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...

  11. 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...

  12. 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.

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

    PubMed

    Centner, Terence; Eberhart, Nicholas

    2014-05-08

    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.

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

    EPA Pesticide Factsheets

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

  15. 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

  16. 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.

  17. 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.

  18. 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.

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

    PubMed

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

    2012-11-30

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

  20. 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.

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

    PubMed

    Watanabe, Minae; Ueno, Eiji; Inoue, Tomomi; Ohno, Haruka; Ikai, Yoshitomo; Morishita, Toshio; Oshima, Harumi; Hayashi, Rumiko

    2013-01-01

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

  2. 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...

  3. 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...

  4. 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...

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

    PubMed

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

    2014-01-01

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

  6. Cumulative risk assessment of pesticide residues in food.

    PubMed

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

    2008-08-15

    There is increasing need to address the potential risks of combined exposures to multiple residues from pesticides in the diet. The available evidence suggests that the main concern is from dose addition of those compounds that act by the same mode of action. The possibility of synergy needs to be addressed on a case-by-case basis, where there is a biologically plausible hypothesis that it may occur at the levels of residues occurring in the diet. Cumulative risk assessment is a resource-intense activity and hence a tiered approach to both toxicological evaluation and intake estimation is recommended, and the European Food Safety Authority (EFSA) has recently published such a proposal. Where assessments have already been undertaken by some other authority, full advantage should be taken of these, subject of course to considerations of quality and relevance. Inclusion of compounds in a cumulative assessment group (CAG) should be based on defined criteria, which allow for refinement in a tiered approach. These criteria should include chemical structure, mechanism of pesticidal action, target organ and toxic mode of action. A number of methods are available for cumulating toxicity. These are all inter-related, but some are mathematically more complex than others. The most useful methods, in increasing levels of complexity and refinement, are the hazard index, the reference point index, the Relative Potency Factor method and physiologically based toxicokinetic modelling, although this last method would only be considered should a highly refined assessment be necessary. Four possible exposure scenarios are of relevance for cumulative risk assessment, acute and chronic exposure in the context of maximum residue level (MRL)-setting, and in relation to exposures from the actual use patterns, respectively. Each can be addressed either deterministically or probabilistically. Strategies for dealing with residues below the limit of detection, limit of quantification or limit

  7. 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.

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

    PubMed

    Suárez-Jacobo, A; Alcantar-Rosales, V M; Alonso, D; Heras-Ramírez, M E; Elizarragaz-De La Rosa, D; Lugo-Melchor, O Y; Gaspar-Ramirez, O

    2017-04-04

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

  9. 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.

  10. 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

  11. Multiple pesticide residues in live and poisoned honeybees - Preliminary exposure assessment.

    PubMed

    Kiljanek, Tomasz; Niewiadowska, Alicja; Gaweł, Marta; Semeniuk, Stanisław; Borzęcka, Milena; Posyniak, Andrzej; Pohorecka, Krystyna

    2017-02-08

    Study combines data about the exposure of honeybees to pesticides from plant protection products and veterinary medicinal products. Residues of 200 pesticide and pesticide metabolites in 343 live and 74 poisoned honeybee samples, obtained during the years of 2014-2015, were determined by LC-MS/MS and GC-MS/MS. In 44% of live honeybee 48 different pesticide residues were found, mainly amitraz metabolites (DMF, DMPF) and chlorpyrifos. In 98% of poisoned honeybee 57 pesticides and metabolites were detected, mainly chlorpyrifos, dimethoate and clothianidin. In total 84 different pesticides were detected both in live and poisoned honeybees, they indicate 30 various modes of action. Differences between mean number of pesticide residues detected in live and poisoned honeybees clearly indicate the impact of multiple pesticides on honeybee health. Possible impact of systemic fungicides on the health of honeybees was studied. Applicability of hazard quotient counted as ratio between concentration of pesticides in honeybees and lethal dose in the interpretation whether detected concentration indicates acute toxic effects was shown.

  12. 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...

  13. 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...

  14. 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...

  15. 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...

  16. 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...

  17. 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...

  18. 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...

  19. [Quantitative Analysis of Dimethoate Pesticide Residues in Honey by Surface-Enhanced Raman Spectroscopy].

    PubMed

    Sun, Xu-dong; Dong, Xiao-ling

    2015-06-01

    The feasibility of a combination method of surface-enhanced Raman spectroscopy (SERS) technology and linear regression algorithm was investigated for rapid quantitative analysis of pesticide residues in honey. The total of 30 samples was applied in the experiment with dimethoate pesticide residues range from 1 ppm to 10 ppm. The samples were divided into calibration set (20) and prediction set (10). The substrate of Klarite with an inverted pyramidal structure was adopted for improvement of the relative intensity of the majority of Raman shift peaks. The comparative analysis was carried out between SERS spectra of dimethoate pesticide residues in honey samples and conventional Raman spectra of dimethoate standard sample. And four characteristic Raman shift peaks at the wavenumbers of 867, 1 065, 1 317 and 1 453 cm(-1) were found, which were related with the vibrational information of dimethoate molecule. The relationship was developed by linear regression algorithm between the intensity of Raman shift and the concentration of dimethoate pesticide residues. The 10 new samples in the prediction set were applied to evaluate the performance of the models. By comparison, the optimal model was obtained with the characteristic Raman shift peak of 867 cm(-1). The higher correlation coefficient of prediction of 0.984 and lower root mean square error of prediction of 0.663 ppm were obtained. The detection limit of this method was 2 ppm, which was close to the maximum levels of pesticide residue detection limits. Experimental results showed that it was feasible to rapidly analyze quantitative of pesticide residues in honey with the combination method of SERS technology and linear regression algorithm. Compared with the conventional method coupled with the suitable pretreatment, the combination method of SERS technology and linear regression method could analyze the dimethoate pesticide residues in honey, and it also provided an optional method for rapid quantitative analysis

  20. 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.

  1. Honey bees (Apis mellifera) reared in brood combs containing high levels of pesticide residues exhibit increased susceptibility to Nosema (Microsporidia) infection.

    PubMed

    Wu, Judy Y; Smart, Matthew D; Anelli, Carol M; Sheppard, Walter S

    2012-03-01

    Nosema ceranae and pesticide exposure can contribute to honey bee health decline. Bees reared from brood comb containing high or low levels of pesticide residues were placed in two common colony environments. One colony was inoculated weekly with N. ceranae spores in sugar syrup and the other colony received sugar syrup only. Worker honey bees were sampled weekly from the treatment and control colonies and analyzed for Nosema spore levels. Regardless of the colony environment (spores+syrup added or syrup only added), a higher proportion of bees reared from the high pesticide residue brood comb became infected with N. ceranae, and at a younger age, compared to those reared in low residue brood combs. These data suggest that developmental exposure to pesticides in brood comb increases the susceptibility of bees to N. ceranae infection.

  2. 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

    ... from the requirement of a tolerance in 40 CFR 180.1299 for residues of the plant growth regulator...: Gina Burnett, Biopesticides and Pollution Prevention Division (7511P), Office of Pesticide Programs... K. Reilly, Acting Director, Biopesticides and Pollution Prevention Division, Office of...

  3. 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.

  4. Identification of the main pesticide residue mixtures to which the French population is exposed.

    PubMed

    Crépet, A; Tressou, J; Graillot, V; Béchaux, C; Pierlot, S; Héraud, F; Leblanc, J Ch

    2013-10-01

    Owing to the intensive use of pesticides and their potential persistence in the environment, various pesticide residues can be found in the diet. Consumers are therefore exposed to complex pesticide mixtures which may have combined adverse effects on human health. By modelling food exposure to multiple pesticides, this paper aims to determine the main mixtures to which the general population is exposed in France. Dietary exposure of 3337 individuals from the INCA2 French national consumption survey was assessed for 79 pesticide residues, based on results of the 2006 French food monitoring programmes. Individuals were divided into groups with similar patterns of co-exposure using the clustering ability of a Bayesian nonparametric model. In the 5 groups of individuals with the highest exposure, mixtures are formed by pairs of pesticides with correlations above 0.7. Seven mixtures of 2-6 pesticides each were characterised. We identified the commodities that contributed the most to exposure. Pesticide mixtures can either be components of a single plant protection product applied together on the same crop or be from separate products that are consumed together during a meal. Of the 25 pesticides forming the mixtures, two--DDT and Dieldrin--are known persistent organic pollutants. The approach developed is generic and can be applied to all types of substances found in the diet in order to characterise the mixtures that should be studied first because of their adverse effects on health.

  5. [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.

  6. 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.

  7. A novel device based on a fluorescent cross-responsive sensor array for detecting pesticide residue

    NASA Astrophysics Data System (ADS)

    Huang, Jing; Hou, Changjun; Lei, Jincan; Huo, Danqun; Luo, Xiaogang; Dong, Liang

    2016-11-01

    In this paper, a novel, simple, rapid, and low-cost detection device for pesticide residue was constructed. A sensor array based on a cross-responsive mechanism was designed. The data collection and processing system was used to detect fluorescent signal of the sensor arrays, and to extract unique patterns of the tested pesticide residue. Four selected pesticides, carbendazim, diazine, fenvalerate, and pentachloronitrobenzene, were detected by the proposed device. Unsupervised pattern recognition methods, hierarchical cluster analysis and principal component analysis, were used to analyze the data. The results showed that the methods could 100% discriminate the four pesticide residues. According to the standard regression linear curve of the fluorescence intensity and the concentration of pesticide, the quantitative value of the pesticide was detected, and the device obtained responses at concentrations below 8 ppb, and it has a good linear relationship in the range of 0.01-1 ppm. According to the results, the proposed detection device showed excellent selectivity and discrimination ability for the pesticide residues. However, our preliminary study demonstrated that the proposed detection device has excellent potential application for the safety inspection of food.

  8. 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.

  9. [Investigation on the detection of pesticide residue in vegetable based on infrared spectroscopy].

    PubMed

    Li, Wen-xiu; Xu, Ke-xin; Wang, Yan; Lei, Zhen-lin; Zhang, Zhen-hou

    2004-10-01

    In this paper, the mid-infrared Attenuated Total Reflection (ATR) spectra of two slathered pesticides dichlorvos and trichlorfon in vegetable juice solution have been investigated. It can be concluded that within characteristic absorption region of the two pesticides in the mid-infrared range, the pigments inside the vegetable have no effect on the pesticide' s absorbance; pesticides in standard solution and vegetable juice solution share almost the same absorbance characteristics. These results indicate that: the authors can use the model built by the absorbance data of pesticides in water solution to simulate their absorbance in vegetable solution, then based upon infrared spectroscopy, the direct detection of pesticide residue on the vegetable can be achieved; it also provides a possible way of rapid detection on vegetable in the future.

  10. 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.

  11. 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.

  12. Aging reduces the bioavailability of even a weakly sorbed pesticide (carbaryl) in soil.

    PubMed

    Ahmad, Riaz; Kookana, Rai S; Megharaj, Mallavarapu; Alston, Angus M

    2004-09-01

    We investigated bioavailability and biodegradation of carbaryl (1-naphthyl methylcarbamate) in a soil with a long history of pesticide contamination from a storage facility located at Mamoon Kanjan, Pakistan. Carbaryl is weakly sorbed and generally considered to be easily degradable in soil. Extraction studies revealed that 49% of the total carbaryl in soil (88.0 mg kg(-1)) was not water-extractable and also not bioavailable, as demonstrated by inoculation of the contaminated soil with a carbaryl-degrading, mixed bacterial culture. Inoculation of the contaminated soil with the carbaryl-degrading culture showed that the bacteria were capable of degrading only the available (i.e., water-extractable) fraction of the pesticide. When the soil was pulverized in a ball mill to enhance the release of residue, an additional 19% of the carbaryl became bioavailable. A significant proportion of residue (approximately 33%) remained unavailable. The long (>12 years) contact time between the pesticide and soil (i.e., aging), allowing possible sequestration into soil nanopores and the organic matter matrices, is suggested to have rendered the pesticide unavailable for microbial degradation. High concentration (88.0 mg kg(-1)) in soil facilitated its persistence and sequestration. Results from the present study demonstrate that even a weakly sorbed and easily degradable pesticide, carbaryl, is effectively sequestrated in soil with time, rendering it partly inaccessible to microorganisms and affecting the bioavailability of the compound.

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

    NASA Astrophysics Data System (ADS)

    Al-Mutlaq, Khalid F.

    2006-12-01

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

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

    PubMed

    Kobayashi, Maki; Ohtsuka, Kenji; Tamura, Yasuhiro; Tomizawa, Sanae; Kinoshita, Teruaki; Kamijo, Kyoko; Iwakoshi, Keiko; Sato, Chizuko; Nagayama, Toshihiro; Takano, Ichiro

    2013-01-01

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

  15. Pesticide residues in ground water of the San Joaquin Valley, California

    NASA Astrophysics Data System (ADS)

    Domagalski, Joseph L.; Dubrovsky, Neil M.

    1992-01-01

    A regional assessment of non-point-source contamination of pesticide residues in ground water was made of the San Joaquin Valley, an intensively farmed and irrigated structural trough in central California. About 10% of the total pesticide use in the USA is in the San Joaquin Valley. Pesticides detected include atrazine, bromacil, 2.4-DP, diazinon, dibromochloropropane, 1,2-dibromoethane, dicamba, 1,2-dichloropropane, diuron, prometon, prometryn, propazine and simazine. All are soil applied except diazinon. Pesticide leaching is dependent on use patterns, soil texture, total organic carbon in soil, pesticide half-life and depth to water table. Leaching is enhanced by flood-irrigation methods except where the pesticide is foliar applied such as diazinon. Soils in the western San Joaquin Valley are fine grained and are derived primarily from marine shales of the Coast Ranges. Although shallow ground water is present, the fewest number of pesticides were detected in this region. The fine-grained soil inhibits pesticide leaching because of either low vertical permeability or high surface area; both enhance adsorption on to solid phases. Soils of the valley floor tend to be fine grained and have low vertical permeability. Soils in the eastern part of the valley are coarse grained with low total organic carbon and are derived from Sierra Nevada granites. Most pesticide leaching is in these alluvial soils, particularly in areas where depth to ground water is less than 30m. The areas currently most susceptible to pesticide leaching are eastern Fresno and Tulare Counties. Tritium in water molecules is an indicator of aquifer recharge with water of recent origin. Pesticide residues transported as dissolved species were not detected in non-tritiated water. Although pesticides were not detected in all samples containing high tritium, these samples are indicative of the presence of recharge water that interacted with agricultural soils.

  16. Pesticide residues in ground water of the San Joaquin Valley, California

    USGS Publications Warehouse

    Domagalski, J.L.; Dubrovsky, N.M.

    1992-01-01

    A regional assessment of non-point-source contamination of pesticide residues in ground water was made of the San Joaquin Valley, an intensively farmed and irrigated structural trough in central California. About 10% of the total pesticide use in the USA is in the San Joaquin Valley. Pesticides detected include atrazine, bromacil, 2.4-DP, diazinon, dibromochloropropane, 1,2-dibromoethane, dicamba, 1,2-dichloropropane, diuron, prometon, prometryn, propazine and simazine. All are soil applied except diazinon. Pesticide leaching is dependent on use patterns, soil texture, total organic carbon in soil, pesticide half-life and depth to water table. Leaching is enhanced by flood-irrigation methods except where the pesticide is foliar applied such as diazinon. Soils in the western San Joaquin Valley are fine grained and are derived primarily from marine shales of the Coast Ranges. Although shallow ground water is present, the fewest number of pesticides were detected in this region. The fine-grained soil inhibits pesticide leaching because of either low vertical permeability or high surface area; both enhance adsorption on to solid phases. Soils of the valley floor tend to be fine grained and have low vertical permeability. Soils in the eastern part of the valley are coarse grained with low total organic carbon and are derived from Sierra Nevada granites. Most pesticide leaching is in these alluvial soils, particularly in areas where depth to ground water is less than 30m. The areas currently most susceptible to pesticide leaching are eastern Fresno and Tulare Counties. Tritium in water molecules is an indicator of aquifer recharge with water of recent origin. Pesticide residues transported as dissolved species were not detected in non-tritiated water. Although pesticides were not detected in all samples containing high tritium, these samples are indicative of the presence of recharge water that interacted with agricultural soils. ?? 1992.

  17. 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.

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

    PubMed

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

    2013-09-01

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

  19. 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.

  20. 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.

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

    PubMed

    Wan, Michael T

    2013-01-01

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

  2. 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

  3. 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 requirements table. 158.2130 Section 158.2130 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY... this table to determine the residue chemistry data requirements and the substance to be tested for...

  4. 40 CFR 158.2172 - Experimental use permit 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 Experimental use permit microbial pesticides residue data requirements table. 158.2172 Section 158.2172 Protection of Environment ENVIRONMENTAL.... Sections 158.100 through 158.130 describe how to use this table to determine the residue chemistry...

  5. Monitoring and Risk Assessment of Pesticide Residues in Commercially Dried Vegetables

    PubMed Central

    Seo, Young-Ho; Cho, Tae-Hee; Hong, Chae-Kyu; Kim, Mi-Sun; Cho, Sung-Ja; Park, Won-Hee; Hwang, In-Sook; Kim, Moo-Sang

    2013-01-01

    We tested for residual pesticide levels in dried vegetables in Seoul, Korea. A total of 100 samples of 13 different types of agricultural products were analyzed by a gas chromatography-nitrogen phosphate detector (GC-NPD), an electron capture detector (GC-μECD), a mass spectrometry detector (GC-MSD), and a high performance liquid chromatography-ultraviolet detector (HPLC-UV). We used multi-analysis methods to analyze for 253 different pesticide types. Among the selected agricultural products, residual pesticides were detected in 11 samples, of which 2 samples (2.0%) exceeded the Korea Maximum Residue limits (MRLs). We detected pesticide residue in 6 of 9 analyzed dried pepper leaves and 1 sample exceeded the Korea MRLs. Data obtained were then used for estimating the potential health risks associated with the exposures to these pesticides. The estimated daily intakes (EDIs) range from 0.1% of the acceptable daily intake (ADI) for bifenthrin to 8.4% of the ADI for cadusafos. The most critical commodity is cadusafos in chwinamul, contributing 8.4% to the hazard index (HI). This results show that the detected pesticides could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring is recommended. PMID:24471124

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

    PubMed

    Kuranchie-Mensah, Harriet; Yeboah, Philip O; Nyarko, Elvis; Golow, Abledze A

    2013-04-01

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

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

    PubMed

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

    2011-05-01

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

  8. [Study of pesticide residues in agricultural products for the "Positive List" system].

    PubMed

    Akiyama, Yumi; Yoshioka, Naoki; Ichihashi, Keiko

    2005-12-01

    During a 3-year monitoring survey (April 2002-March 2005) of pesticide residues in agricultural products, 592 samples (324 domestic; 268 imported) collected in Hyogo prefecture, Japan were analyzed. The number of pesticides tested increased from 232 in FY 2002 to 323 in FY 2004. The purpose of the study was to clarify the residue status by accumulating information about pesticides detected frequently, to allow effective and efficient regulation under the new "Positive List" legislation to be implemented in FY 2006. Overall, 47% of domestic and 61% of imported samples contained detectable residues and ca. 60% of positive samples contained multiple residues. The limit of quantitation was set at 0.01 microg/g and the limit of detection was 0.001-0.003 microg/ g. Most of the residues were present at low concentrations: 80% of the detections in samples excluding imported citrus fruits were < 0.05 microg/g. More than 5 different pesticides (> 0.01 microg/g) were detected simultaneously in 13 samples. The sum of the ratios of residues to MRLs was calculated as one of the indexes to represent the risk of multiple residues, and they exceeded 100% in 3 imported frozen vegetables; baby kidney bean, spinach, Welsh onion. Samples in violation of the Food Sanitation Law were not found in our survey, but 1.9% of the samples might be in conflict with the new "Positive List" legislation.

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

    PubMed

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

    2014-11-01

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

  10. Risk assessment of oncogenic potency of pesticide residues in fruits and vegetables.

    PubMed

    Keikotlhaile, B M; Spanoghe, P; Steurbaut, W

    2011-01-01

    Pesticides are used in agriculture to improve food security by assuring good harvest, however, they can have harmful effects in human beings and animals. One of the harmful effects of pesticides is their carcinogenicity. Exposure to oncogenic compounds may result in cancer to the exposed animal or person. In this paper, exposure assessment of oncogenic potency of pesticides was performed from raw and processed fruits and vegetables. The oncogenic risk was calculated by multiplying the estimated daily intake (EDI) of the pesticide residue with the oncogenic potency factor (Q*) of the concerned pesticide. The total potential oncogenic risk was calculated to be 2.76 x 10(-3) before processing and 8.97 x 10(-4) after processing. The risk was higher than the EPA acceptable limit of 1 x10(-6). Despite the calculated levels exceeding the EPA acceptable limit, food processing activities reduced the dietary oncogenic risk to an average 33.8%.

  11. [Preparation of samples for proficiency testing of pesticide residue analysis in processed foods].

    PubMed

    Okihashi, Masahiro; Osakada, Masakazu; Uchida, Kotaro; Nagayoshi, Haruna; Yamaguchi, Takahiro; Kakimoto, Kensaku; Nakayama, Yukiko; Obana, Hirotaka

    2010-01-01

    To conduct proficiency testing for the analysis of pesticide residues in processed foods, fortified samples of retort curry and pancake were examined. In the case of retort curry, heating and mixing were necessary at the time of preparation to provide a homogenous analytical sample. A mixture of 4 carbamates and 11 organophosphorus pesticides was spiked and 14 of them showed consistent results in the samples. In the case of pancake, 10 kinds of pesticides were added to the pastry. The prepared pastry was them cooked. The relative concentrations of most of the pesticides in the pancake were not affected and all the pesticides showed consistent results in the samples. These results showed that the two tested samples were suitable for proficiency testing.

  12. 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.

  13. Organochlorine pesticide residues in fish from southern Italian rivers

    SciTech Connect

    Amodio-Cocchieri, R.; Arnese, A.

    1988-02-01

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

  14. Rapid Multi-Residue Analysis of Pesticides in Pulses by LC-MS/MS.

    PubMed

    Iwakoshi, Keiko; Otsuka, Kenji; Tamura, Yasuhiro; Tomizawa, Sanae; Masubuchi, Tamako; Yamaki, Yumiko; Nakagawa, Yukiko; Masuda, Ryoko; Suto, Shota; Kokaji, Yoshie; Shindo, Tetsuya; Takano, Ichiro

    2016-01-01

    Rapid multi-residue analysis of pesticides in pulses was developed using LC-MS/MS. Pesticide residues in 5 g of homogenized pulses were extracted with 30 mL of acetonitrile and salted out with 4 g of anhydrous magnesium sulfate and 2 g of sodium chloride in the presence of citrate buffer in a disposable tube. The resulting residues were extracted with 30 mL of acetonitrile, and co-extractives were removed on a handmade four-layer column, consisting of a layer of Z-Sep/C18 (20 mg/50 mg) dry particles on top of a three-layer, custom-made (pre-packed) column (lower bed: 60 mg of PSA, middle bed: 30 mg of GC, and top bed: 60 mg of C18) packed in a 10 mm internal diameter polypropylene column (3 mL). The developed method showed good recoveries of pesticides in soybean, lentil, white kidney bean and garbanzo. According to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan, recovery tests were conducted in soybeans fortified with 107 kinds of pesticides at the levels of 0.01 and 0.1 μg/g, respectively. At each concentration 2 samples were extracted on 5 separate days. Pesticides in the test solution were determined by LC-MS/MS using scheduled MRM. As regards the trueness of this method for 107 pesticides in soybeans, 97 pesticides were in the range of 70-120% with satisfactory repeatability and within-run reproducibility. This new method is expected to be applicable for routine examination of pesticide residues in soybeans.

  15. Neonicotinoids transference from the field to the hive by honey bees: Towards a pesticide residues biomonitor.

    PubMed

    Silvina, Niell; Florencia, Jesús; Nicolás, Pérez; Cecilia, Pérez; Lucía, Pareja; Abbate, Silvana; Leonidas, Carrasco-Letelier; Sebastián, Díaz; Yamandú, Mendoza; Verónica, Cesio; Horacio, Heinzen

    2017-03-01

    The beehive as a quantitative monitor of pesticide residues applied over a soybean crop was studied through a semi field experiment of controlled exposure of honey bees to pesticides in macro tunnels. The distribution within exposed beehives of pesticides commonly used in soybean plantation, was assessed. Residue levels of insecticides in soybean leaves, honey bees, wax, honey and pollen were analyzed. The transference from pesticides present in the environment into the beehive was evidenced. The obtained results allow relating pesticide concentrations present in the environment with traces found in foraging bees. Therefore, pesticide transference ratios could be calculated for each detected compound (acetamiprid, imidacloprid and thiamethoxam) which showed a linear inverse trend with their 1-octanol/water partition coefficient (Kow). The least transferred pesticide to the hive (acetamiprid) has the highest vapor pressure (Vp). This study gives new insights on the usefulness of monitoring the environment through beehives aiming to evaluate if agroecosystems remain sustainable. It also contributes to generate valuable information for model building aiming to predict environmental quality through beehive's analysis.

  16. Organochlorine pesticides residues in bottled drinking water from Mexico City.

    PubMed

    Díaz, Gilberto; Ortiz, Rutilio; Schettino, Beatriz; Vega, Salvador; Gutiérrez, Rey

    2009-06-01

    This work describes concentrations of organochlorine pesticides in bottled drinking water (BDW) in Mexico City. The results of 36 samples (1.5 and 19 L presentations, 18 samples, respectively) showed the presence of seven pesticides (HCH isomers, heptachlor, aldrin, and p,p'-DDE) in bottled water compared with the drinking water standards set by NOM-127-SSA1-1994, EPA, and World Health Organization. The concentrations of the majority of organochlorine pesticides were within drinking water standards (0.01 ng/mL) except for beta-HCH of BW 3, 5, and 6 samples with values of 0.121, 0.136, and 0.192 ng/mL, respectively. It is important monitoring drinking bottled water for protecting human health.

  17. 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.

  18. 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

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

    PubMed Central

    Chapman, S

    2003-01-01

    Objectives: To review the Australian tobacco industry's knowledge of pesticide residue on Australian tobacco and its policies and practices on resisting calls by tobacco control advocates that consumers should be informed about pesticide residue as well as additives. Methods: Review of previously internal industry documents relevant to pesticides and additives in Australian tobacco located from the Master Settlement Agreement websites. Results: Between 1972 and 1994 Philip Morris Australia was aware that its leaf samples were often contaminated with pesticide residue, sometimes including organochlorine levels described by PM's European laboratories as being "extremely high". Consumers were not advised of the contamination nor products withdrawn. From 1981, the industry also resisted calls to declare fully the extent of use and long term safety data on all additives used in their products. They developed standard public responses that were evasive and misleading and, in 2000, implemented voluntary additive disclosure which allowed the companies to continue to avoid disclosure of any ingredient they deemed to be a trade secret. There was extensive use of ozone depleting freon in Australian tobacco manufacturing. Again, the industry kept this information away from consumers. Conclusions: Australian smokers are unable to make informed decisions about smoking because pesticide and additive disclosure remains voluntary. The Australian government should regulate tobacco to require full disclosure including information on the likely health consequences of inhaling pesticide and additive pyrolysis products. PMID:14645948

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

    PubMed

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

    2007-01-01

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

  1. 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.

  2. 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.

  3. Effects of food processing on pesticide residues in fruits and vegetables: a meta-analysis approach.

    PubMed

    Keikotlhaile, B M; Spanoghe, P; Steurbaut, W

    2010-01-01

    Pesticides are widely used in food production to increase food security despite the fact that they can have negative health effects on consumers. Pesticide residues have been found in various fruits and vegetables; both raw and processed. One of the most common routes of pesticide exposure in consumers is via food consumption. Most foods are consumed after passing through various culinary and processing treatments. A few literature reviews have indicated the general trend of reduction or concentration of pesticide residues by certain methods of food processing for a particular active ingredient. However, no review has focused on combining the obtained results from different studies on different active ingredients with differences in experimental designs, analysts and analysis equipment. In this paper, we present a meta-analysis of response ratios as a possible method of combining and quantifying effects of food processing on pesticide residue levels. Reduction of residue levels was indicated by blanching, boiling, canning, frying, juicing, peeling and washing of fruits and vegetables with an average response ratio ranging from 0.10 to 0.82. Baking, boiling, canning and juicing indicated both reduction and increases for the 95% and 99.5% confidence intervals.

  4. 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.

  5. 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.

  6. [Simultaneous analysis of residual pesticides in fruit, vegetables, brown rice, and oolong tea by LC-MS/MS].

    PubMed

    Namikawa, Mikio; Shibata, Sayo; Shiomi, Tetsuo; Nakagawa, Tomoyuki; Ban, Soichiro; Tomita, Yoko; Semura, Shunsuke; Nakao, Yoshie; Banno, Yukinori; Kawakami, Masahiro

    2014-01-01

    According to "The validity evaluation guideline of the testing methodology on the residual pesticides in food" of the Ministry of Health, Labour and Welfare of Japan, we carried out validity evaluation of a simultaneous analysis method for residual pesticides in various products with the QuEChERS method using a C18 mini column and/or an EnviCarb/PSA mini column for purification. Multi-ingredient simultaneous analysis with high sensitivity in a short time was achieved with LC-MS/MS. Validation was achieved for 269 pesticides among 302 pesticides in eight kinds of fruit, vegetables, and brown rice and 204 pesticides among 233 pesticides in oolong tea. Finally, 151 pesticides in oolong tea and from 234 to 259 pesticides in fruit, vegetables, and brown rice met the values specified in the guideline.

  7. Monitoring of organophosphorus pesticide residues in vegetables of agricultural area in Venezuela.

    PubMed

    Quintero, América; Caselles, María J; Ettiene, Gretty; de Colmenares, Nélida G; Ramírez, Tibisay; Medina, Deisy

    2008-10-01

    The purpose of this study was to determine the residues of seven pesticides organophosphorus (methamidophos, diazinon, chlorpyriphos, parathion-methyl, dimethoate, malathion and tetrachlorvinphos), in some vegetables like: potato, lettuce, tomato, onion, red pepper and green onion cultivated in José María Vargas County in Táchira State, Venezuela. The research permitted to detect that 48.0% of the samples were contaminated with some of the pesticides studied. Methamidophos was founded in the vegetables in the rank of 6.3%-65.5%. The results show that 16.7% of the samples tested have residues higher than the maximum limits permitted.

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

    PubMed

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

    2001-01-01

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

  9. Detection of toxic heavy metals and pesticide residue in herbal plants which are commonly used in the herbal formulations.

    PubMed

    Rao, Mruthyumjaya Meda; Kumarmeena, Ajay; Galib

    2011-10-01

    Herbal formulations are getting popular throughout the world and commercialized extensively for various medicinal properties. WHO has emphasized the need for quality assurance of herbal products, including testing of heavy metals and pesticides residues. In view of WHO guidelines, single herbal drugs used in herbal formulations were collected from local market, for testing heavy metals and persistent pesticides residue. Therefore, in the present case, we have examined few local samples of certain herbs viz. Emblica officinalis, Terminalia chebula, Terminalia belerica, and Withania somnifera. The present studies were selected for estimation of four heavy metals namely Arsenic, Cadmium, Lead, and Mercury. Apart from these, pesticide residue Viz. Organochlorine pesticides, Organophosphorus pesticides, and Pyrethroids were analyzed in the four samples of single crude drugs. Heavy metals and pesticide residue were found below detection limits in all the samples.

  10. 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

  11. 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

    ... AGENCY Notice of Receipt of a Pesticide Petition Filed for Residues of Polymeric Polyhydroxy Acid in or... establishment of a regulation for residues of the plant growth regulator, polymeric polyhydroxy acid, in or on... polymeric polyhydroxy acid in or on all food commodities. EPA has determined that the pesticide...

  12. 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.

  13. Use of semipermeable membrane devices (SPMDS) to determine bioavailable organochlorine pesticide residues in streams receiving irrigation drainwater

    USGS Publications Warehouse

    Petty, Jimmie D.; Huckins, James N.; Martin, D.B.; Adornato, T.G.

    1995-01-01

    The semipermeable membrane device (SPMD), consisting of a neutral lipid (triolein) enclosed in polyethylene layflat tubing, is very effective in sequestering bioavailable organochlorine (OC) pesticides in the environment. We used SPMDs to sequester OC pesticide residues in streams receiving irrigation drainwater and found toxaphene, the DDT complex, dieldrin, and endrin. Ambient water concentrations of the OC pesticides were calculated using an algorithm developed previously. Toxaphene residues were estimated to range from 300 to 7,000 ng/L.

  14. 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.

  15. 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.

  16. 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

  17. Gas chromatographic evaluation of pesticide residue contents in nectarines after non-toxic washing treatments.

    PubMed

    Pugliese, P; Moltó, J C; Damiani, P; Marín, R; Cossignani, L; Mañes, J

    2004-10-01

    Washing with aqueous solutions of citric acid, ethanol, glycerol, hydrogen peroxide, potassium permanganate, sodium metabisulfite, sodium laurylsulfate (SLS), sodium hypochlorite, and urea is evaluated for pesticide residue reduction in nectarines and compared with simple tap water washing. Residues of pesticides commonly utilized in nectarines (chlorpyrifos, fenarimol, iprodione, malathion, methidathion, myclobutanil, parathion and pirimicarb) are extracted with ethyl acetate and anhydrous sodium sulfate, extract is concentred and analyzed by GC with nitrogen-phosphorus detection. The formation of possible toxic by-products (chlorpyrifos oxon, malaoxon, methidaoxon and paraoxon methyl) is studied by GC-MS. No toxic by-products are identified in the extracts of the washed samples for the washing-time and concentrations studied, but high levels of sodium hypochlorite, hydrogen peroxide and potassium permanganate form oxons from the organophosphorus pesticides. Ethanol, glycerol and SLS solutions removed near the 50% of the pesticide residues. The other solutions were not more effective than tap water washing. The amount of pesticide removed by washings is related to its water solubility and octanol-water partition coefficient.

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

    NASA Astrophysics Data System (ADS)

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

    2016-10-01

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

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

    PubMed

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

    2006-01-01

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

  20. 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.

  1. 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.

  2. 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.

  3. 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...

  4. 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.

  5. 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%.

  6. Analysis of pesticide residues in hops and their extraction by liquid CO2 during the production of hop extracts.

    PubMed

    Williams, C S; Eastoe, B V; Slaiding, I R; Walker, M D

    1994-01-01

    A method has been developed for analysing pesticide residues in whole hops, hop pellets and hop extracts by GC-MS. Five batches of hop pellets containing nine different pesticides (triadimefon, dicofol, mephosfolan, bupirimate, cyhalothrin, tetradifon, endosulfan, pyrazophos and total bisdithiocarbamates) were extracted with liquid CO2. Pesticide concentrations in the original hop pellets and the extracts were determined. The pesticides were concentrated by the extraction process (concentration factor 1.3-8.3), except for the bisdithiocarbamates, which were not extracted. When the same amount of bitterness was added into the brewing process using liquid CO2 extract as opposed to hop pellets, for most of the pesticides proportionately less pesticide was added. However, for two pesticides (dicofol and triadimefon) corrected residue levels were similar to, or in some cases slightly higher than, those in hop pellets.

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

    PubMed

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

    2014-08-01

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

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

    PubMed

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

    2014-12-01

    The main aim of the present investigations was to compare the pesticide load in integrated pest management (IPM) with non-IPM crops of rice fields. The harvest samples of Basmati rice grain, soil, and irrigation water, from IPM and non-IPM field trials, at villages in northern India, were analyzed using multi-pesticide residue method. The field experiments were conducted for three consecutive years (2008-2011) for the successful validation of the modules, synthesized for Basmati rice, at these locations. Residues of tricyclazole, propiconazole, hexconazole, lambda cyhalothrin, pretilachlor chlorpyrifos, DDVP, carbendazim, and imidacloprid were analyzed from two locations, Dudhli village of Dehradun, Uttrakhand and Saboli and Aterna village of Sonepat, Haryana. The pesticide residues were observed below detectable limit (BDL) (<0.001-0.05 μg/g) in all 24 samples of rice grains and soil under IPM and non-IPM trials. Residues were below detection level (<0.001-0.05 μg/L) in irrigation water samples (2008-09). Residues of tricyclazole and carbendazim, analyzed from same locations, revealed pesticide residues as BDL (<0.001-0.05 μg/g) in all 40 samples of Basmati rice grains and soil. It was also observed as BDL (<0.001-0.05 μg/L) for 12 water samples (2009-2010). The residues of tricyclazole, propioconazole, chlorpyrifos, hexaconazole, pretilachlor, and λ-cyhalothrin were also found as BDL (<0.001-0.05 μg/g) in 40 samples of Basmati rice grains and soil and 12 water samples (<0.001-0.05 μg/L) (2010-2011).

  9. Gas chromatographic determination of pesticide residues in white mustard.

    PubMed

    Słowik-Borowiec, Magdalena; Szpyrka, Ewa; Walorczyk, Stanisław

    2015-04-15

    A new analytical method employing gas chromatography coupled to electron capture and nitrogen phosphorus detection (GC-ECD/NPD) has been developed and validated for the screening and quantification of 51 pesticides in a matrix of high chlorophyll content - white mustard (Sinapis alba L.). For preparation of the sample extract, the citrate buffered QuEChERS procedure was followed. However certain changes were made to adapt the method to our needs and available laboratory resources. The sample size was reduced to 5 g, 10 mL water was added and exchange of solvent before GC analysis was done. The samples spiked with the target pesticides at the concentration level 0.01 mg/kg and a higher level (depending on the compound) yielded average recoveries in the range of 70-120% with relative standard deviations (RSDs) 0-19% except for HCB, S-metolachlor and teflubenzuron, and displayed very good linearity (R(2)>0.99) for nearly all the analytes. Limit of quantification was 0.01 mg/kg for the majority of the analytes. The expanded measurement uncertainties were estimated employing a "top-down" empirical model as being between 6% and 32% and yielding an average value of 18% (coverage factor k=2, confidence level 95%).

  10. Stability of pesticides' residues under ultraviolet germicidal irradiation.

    PubMed

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

    2011-06-01

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

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. Multi-residue determination of pesticides in vegetables by gas chromatography/ion trap mass spectrometry.

    PubMed

    Tao, C-J; Hu, J-Y; Li, J-Z; Zheng, S-S; Liu, W; Li, C-J

    2009-01-01

    To monitor possible contamination of edible vegetables by common pesticides, an analytical method using gas chromatography combined with ion trap spectrometry (GC-IT/MS) was developed to measure simultaneously up to 39 pesticide residues, belonging to organophosphors, organochlorines, pyrethroids or carbamates classes, left on four kinds of popular vegetables. The procedure entails addition of acetone, dichloromethane, and sodium chloride to a small amount of vegetable, then the mixture was shaken intensively and centrifuged for phase separation. An aliquot of the organic layer was cleanup using solid-phase extraction (SPE) cartridges filled with graphitized carbon black (GCB) in combination with acidic aluminum oxide. Gas chromatography with ion trap mass spectrometer was then used for qualitative and quantitative determination of the pesticides. The GCB combination with acidic aluminum oxide was found more suitable than florisil, aluminum oxide and silicon dioxide for sample cleanup with recoveries above 70% for most pesticides in removing the majority of co-extracted matrices. Variation coefficients of the repeatability typically smaller than 20% have been achieved for a wide range of the investigated pesticides. A set of critical instrument parameters for the GC-IT/MS Varian system in the MS mode was established. Based on optimization work conducted in this study, the 39 pesticides were separated successively with the limits of detection between 0.02 and 0.1 mg/kg.

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

    PubMed

    Wang, Jian; Cheung, Wendy; Leung, Daniel

    2014-01-29

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

  17. A natural matrix (pureed tomato) candidate reference material containing residue concentrations of pesticide chemicals.

    PubMed

    Armishaw, P; Millar, R

    2001-06-01

    NARL (the Australian National Analytical Reference Laboratory) is preparing a pureed tomato reference material spiked with residue concentrations of a range of pesticide chemicals relevant to the Australian horticultural industry. Traceable certified pesticide concentration values will be established using both isotope dilution mass spectrometry primary methods (developed within NARL) and measurements carried out by a number of experienced laboratories. As far as we are aware, there is no other similar CRM available anywhere in the world. The need for such a material is evident from the results of interlaboratory proficiency studies conducted by NARL among Australian and Asia-Pacific residue testing laboratories. Many participants are experiencing difficulties with the analysis of pesticide residues in fruit and vegetables at concentrations of regulatory significance. Chemicals such as methamidophos (an organophosphorus pesticide widely used on tomato crops) are causing particular problems. In a pilot study, a number of units of control (unspiked tomato) and the candidate reference material were prepared and packaged into lacquered steel cans which were sealed and sterilised by immersion in boiling water. Accelerated stability testing of the packaged material was conducted using isochronous measurement. All of the pesticides showed some degree of degradation after 4 weeks of storage at 50 degrees C, and after 168 days of storage at room temperature. However, all appeared to be stable after 168 days of freezer storage. Homogeneity testing involved duplicate test portions taken from every 50th unit of reference material. An experimental protocol was devised with the aim of minimising the analytical variability and assuring the quality of the data generated. There is some degree of inhomogeneity in the prepared material and a small fill trend is also indicated. Potential improvements to the spiking and preparation procedure have been identified and it is planned to

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

    PubMed

    Ikeura, Hiromi; Hamasaki, Sadahiro; Tamaki, Masahiko

    2013-05-01

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

  19. 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

  20. 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.

  1. 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.

  2. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-11-01

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

  4. Unit-to-unit variability of pesticide residues in fruit and vegetables.

    PubMed

    Hill, Alan R C; Reynolds, Stewart L

    2002-08-01

    Pesticide residue levels (36 pesticides and some of their metabolites) were determined in the individual units taken from large samples of apples, bananas, celery, kiwi fruit, oranges, peaches and nectarines, pears, plums, potatoes, and tomatoes. The 65 large samples (generally about 100-110 units, but only 45 units of celery) were purchased at retail or wholesale outlets in the UK. The lots from which the samples were drawn originated from 17 different countries. Average concentrations in the samples were in the approximate range 0.002-2 mg kg(-1). Unit-to-unit variability factors (97.5th percentile mg kg(-1)/average mg kg(-1)), for the pesticide/product combination data sets in which >10% of samples contained measurable residues (n = 106), were in the range 1.4-9.6 (11.1 based on a value of zero for data below reporting limits). Analytical variance contributed only a small proportion (up to 11%) to the overall variance of the 106 data sets. There was no evidence of a relationship between the variability factor and the commodity, country of origin, residue concentration or the physicochemical characteristics of the pesticide. The extent of variability appears to be determined at or about the time of pesticide application. Taking non-detectable residues as half the reporting limits, the frequency distribution of variability factors was approximately log-normal, with a geometric mean of 3.4. The corresponding 95% probability limits of the variability factors were calculated to be 1.6 and 7.6.

  5. Relationship between the adsorption capacity of pesticides by wood residues and the properties of woods and pesticides.

    PubMed

    Rodriguez-Cruz, Sonia; Andrades, Maria S; Sanchez-Camazano, Maria; Sanchez-Martin, Maria J

    2007-05-15

    With the aim to explore the potential use of wood residues in technologies aimed at preventing the pollution of soil and water, we studied the adsorption of four non-ionic pesticides (linuron, alachlor, metalaxyl, and chlorpyrifos) and two ionic pesticides (dicamba and paraquat) with a Kow range of -4.5 to 4.7 by nine types of wood with lignin content in the 18.2-26.9% range. The Freundlich Kf values were considered as indicators of the adsorption capacity. A statistical study was carried out using simple and multiple correlations to establish the degree to which the different parameters of the woods and of the pesticides were involved in adsorption. In the case of the non-ionic pesticides, positive and negative significant correlations were observed between Kf and the lignin (r = 0.73-0.83, p < 0.05-0.01), and soluble C contents of the woods (r = 0.66-0.84), p < 0.1-0.01). For dicamba, a correlation between Kf and pH (r = -0.66, p < 0.1) of the woods was found, while for paraquat, this was seen between Kf and the cation exchange capacity (r = 0.71, p < 0.1) of the woods. No significant correlation was observed between Kf and the total C content of the woods. A highly significant correlation between Kf and Kow values (r > or = 0.93, p < 0.01) was found in the adsorption of the pesticides by the woods (with the exception of paraquat) showing that this parameter is very important in this adsorption process. The determination coefficient of the multiple correlation between Kf and the parameters Kow, soluble C, and lignin contents accounts for nearly 100% of the variability in adsorption for non-ionic pesticides. Based on the results of our study and of those of the literature related to the adsorption of aromatic hydrocarbons, we used the Kow values to define a predictive model of adsorption of hydrophobic organic compounds in general by the woods.

  6. Pesticides

    MedlinePlus

    ... and pets. Proper disposal of pesticides is also important - it can help protect the environment. Biologically-based pesticides are becoming more popular. They often are safer than traditional pesticides. Environmental Protection Agency

  7. 77 FR 15012 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-03-14

    ... growing, subgroup 13-07G at 1.4 parts per million (ppm); cucumber at 1.3 ppm; and rapeseed, subgroup 20A... aged radiochemical residue samples from metabolism studies. The methods have been validated...

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

    PubMed

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

    1979-12-01

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

  9. 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

  10. Pesticides residues and metals in plant products from agricultural area of Belgrade, Serbia.

    PubMed

    Ethorđević, Tijana; Ethurović, Rada

    2012-03-01

    The objective of study was to assess the levels of selected metals and pesticides in plant products from agricultural area of Belgrade, Serbia in order to indicate their possible sources and risks of contamination and to evaluate their sanitary probity and safety. The concentrations of cadmium, copper, iron, manganese, nickel, lead and zinc were below limits established by national and international regulations (maximum found concentrations were 0.028, 1.91, 11.16, 1.77, 0.605, 0.073 and 1.76 mg kg(-1) respectively). Only residue of one of examined pesticides was found in amount below MRL (bifenthrin 2.46 μg kg(-1)) in only one of analysed samples, while others were below detection limits. Obtained results indicate that crops from examined agricultural areas are unpolluted by contaminants used for plant protection and nutrition, indicating good agricultural practice regarding pesticides and fertilizer usage as well as moderate industrial production within examined areas.

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

    PubMed

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

    2012-11-01

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

  12. 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.

  13. Organochlorine pesticide residues in bed sediments of the San Joaquin River and its tributary streams, California

    USGS Publications Warehouse

    Gilliom, R.J.; Clifton, D.G.

    1987-01-01

    The distribution and concentrations of organochlorine pesticide residues in bed sediments were assessed from samples collected at 24 sites in the San Joaquin River and its tributaries in the San Joaquin Valley, California. Sampling was designed to collect the finest grained bed sediments present in the vicinity of each site. One or more of the 14 pesticides analyzed were detected at every site. Pesticides detected at one or more sites were chlordane, DDD, DDE, DDT, dieldrin, endosulfan, mirex, and toxaphene. Pesticides not detected were endrin, heptachlor, heptachlor epoxide, lindane, methoxychlor, and perthane. The most frequently detected pesticides were DDD (83% of sites), DDE (all sites), DDT (33% of sites), and dieldrin (58% of sites). Maximum concentrations of these pesticides, which were correlated with each other and with the amount of organic carbon in the sample, were DDD, 260 micrograms/kg; DDE, 430 micrograms/kg; DDT, 420 micrograms/kg; and dieldrin, 8.9 micrograms/kg. Six small tributary streams that drain agricultural areas west of the San Joaquin River had the highest concentrations. Water concentrations and loads were estimated for each pesticide from its concentration in bed sediments, the concentration of suspended sediment, and streamflow. Estimated loadings of DDD, DDE, DDT, and dieldrin from tributaries to the San Joaquin River indicate that most of the loading to the river at the time of the study was probably from the westside tributaries. Estimated water concentrations exceeded the aquatic life criterion for the sum of DDD, DDE, and DDt of 0.001 microgram/L at nine of the 24 sites sampled. Five of the nine sites are westside tributaries and one is the San Joaquin River near Vernalis. (Author 's abstract)

  14. Residues of organochlorine pesticides in surface soil and raw foods from rural areas of the Republic of Tajikistan.

    PubMed

    Barron, Mace G; Ashurova, Zebunisso J; Kukaniev, Mukhamadcho A; Avloev, Hakbarqul K; Khaidarov, Karim K; Jamshedov, Jamshed N; Rahmatullova, Oygul S; Atolikshoeva, Sunbula S; Mamadshova, Sakina S; Manzenyuk, Oksana

    2017-05-01

    The central Asian Republic of Tajikistan has been an area of extensive historical agricultural pesticide use as well as large scale burials of banned chlorinated insecticides. The current investigation was a four year study of legacy organochlorine pesticides in surface soil and raw foods in four rural areas of Tajikistan. Study areas included the pesticide burial sites of Konibodom and Vakhsh, and family farms of Garm and Chimbuloq villages. These areas were selected to represent a diversity of pesticide disposal histories and to allow assessment of local pesticide contamination in Tajikistan. Each site was visited multiple times and over 500 samples of surface soil and raw foods were collected and analyzed for twenty legacy organochlorine pesticides. Various local food products were sampled to represent the range of raw foods potentially containing residues of banned pesticides, including dairy products, meat, edible plant and cotton seed products. The pesticide analytes included DDTs (DDT, DDD, DDE), lindane isomers (α, β, γ, δ BHC), endosulfan isomers (endosulfan I, II, sulfate), other cyclodienes (aldrin, α and γ chlordanes, dieldrin, endrin, endrin aldehyde and ketone, heptachlor, heptachlor epoxide), and methoxychlor. Pesticide analytes were selected based on availability of commercial standards and known or suspected historical pesticide use and burial. Pesticide contamination was highest in soil and generally low in meat, dairy, and plant products. DDT was consistently the highest measured individual pesticide at each of the four sampling areas, along with BHC isomers and endosulfan II. Soil concentrations of pesticides were extremely heterogeneous at the Vakhsh and Konibodam disposal sites with many soil samples greater than 10 ppm. In contrast, samples from farms in Chimbuloq and Garm had low concentrations of pesticides. Pesticide contamination in raw foods was generally low, indicating minimal transfer from the pesticide sites into local food

  15. 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

    ... manufacturing (NAICS code 311). Pesticide manufacturing (NAICS code 32532). This listing is not intended to be... Subjects Environmental protection, Agricultural commodities, Feed additives, Food additives, Pesticides...

  16. 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

    ... production (NAICS code 112). Food manufacturing (NAICS code 311). Pesticide manufacturing (NAICS code 32532... Environmental protection, Agricultural commodities, Feed additives, Food additives, Pesticides and...

  17. 76 FR 2110 - Notice of Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-01-12

    ... production (NAICS code 112). Food manufacturing (NAICS code 311). Pesticide manufacturing (NAICS code 32532... Environmental protection, Agricultural commodities, Feed additives, Food additives, Pesticides and...

  18. Assessing the risks of pesticide residues to consumers: recent and future developments.

    PubMed

    Harris, C A; Renfrew, M J; Woolridge, M W

    2001-12-01

    Assessing exposure of consumers to pesticide residues is an area of regulatory science that has rapidly developed over the last decade. From simplistic, deterministic models calculating lifetime exposure for adults only, assessment procedures have diversified so that more realistic estimates of long term exposures for adults, schoolchildren, toddlers and infants and short term exposures for adults and toddlers (who generally bound the more extreme consumer patterns) are now carried out. The final assessment of risk still remains a simplistic numeric comparison against hazard assessment based on a wide range of toxicity studies incorporating the appropriate safety or uncertainty factors. As development of risk assessments continues, the use of probabilistic models is becoming an invaluable information tool for quantitative risk management and aiding assessment of cumulative exposure. This paper examines the recent developments in risk assessment and consumer perception of the risks of pesticide residues, and speculates where the future developments in these areas may lie.

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

    PubMed

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

    2012-10-01

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

  20. Pesticide residue variability--implications for Codex MRLs and world trade.

    PubMed

    Dornseiffen, J W; van Eck, W H

    2000-07-01

    A number of developments have taken place in addressing consumer risk to pesticide residues. Progress is being made to harmonize an international database to allow short exposure assessments to be carried out on a routine basis and a number of initiatives have been arranged to support this process. Since Codex Alimentarius Commission has adopted these proposals, they will become an integral part of the process for assessing and accepting Codex MRLs in the future.

  1. 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.

  2. Preparation of activated carbons from agricultural residues for pesticide adsorption.

    PubMed

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

    2010-09-01

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

  3. Pesticide residues and heavy metals in Lake Victoria Nile perch, Lates niloticus, belly flap oil.

    PubMed

    Ogwok, P; Muyonga, J H; Sserunjogi, M L

    2009-05-01

    Oil was extracted from the belly flaps of varied sizes of Nile perch caught from Lake Victoria (Uganda). The oil was analyzed for pesticide residues and heavy metals. Total residual concentration of dichlorodiphenyltrichloroethane, endosulfan, hexachlorocyclohexane, hexachlorobenzene, heptachlor, chlordane, endrin, aldrin and chlorofenvinphos increased significantly (p < 0.05) with fish size. Mercury and lead were detected in most samples while arsenic and cadmium were below detection limits. Nile perch may, therefore, accumulate significant amount of chemical contaminants. Levels of contaminants in Nile perch oil were, in general, within limits considered acceptable by the stringent German Food Law for human consumption.

  4. 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.

  5. Persistence and distribution of pesticide residues in fresh agricultural food consumed in the province of Bologna.

    PubMed

    Girotti, Stefano; Ferri, Elida N; Errani, Ermanno

    2009-02-01

    The presence of pesticide residues in fresh vegetables and fruit have been qualitatively and quantitatively determined at the laboratories of the Regional Agency for Environmental Protection (ARPA), Division of the Province of Bologna. More than 1,700 samples have been tested by routine analyses. The possible risks for consumers have been evaluated by various parameters. The most important ones were: the amount of each residue; the respective ADI (Acceptable Daily Intake) limit; the contemporary presence of different residues; an estimation of the daily intake, based on the amount of fruit and vegetables consumed per person. It has been possible to evaluate that the daily intake of pesticide residues in the province of Bologna during the period 2003-06 resulted lower than the ADI limits concerning the vegetables. According to the information on fruit consumption the daily intake of omethoate (O,O-dimethyl S-methylcarbamoylmethyl phosphorothioate) resulted higher than its ADI limit, of dicofol (2,2,2-trichloro-1,1-bis(trichloromethyl)benzenemethanol) very close to the admitted limit, under the respective limits for all the other residues.

  6. 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.

  7. 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.

  8. 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.…

  9. [Rapid Detection of Trace Dimethoate Pesticide Residues Based on Colorimetric Spectroscopy].

    PubMed

    Li, Wen; Sun, Ming; Li, Min-zan; Sun, Hong

    2015-07-01

    In order to detect dimethoate pesticide residues rapidly and safely, a feasible method based on colorimetric spectroscopy was developed. Because dimethoate is one of organophosphorus pesticides containing sulfur, its sulfenyl can react with Pd2+ to produce a yellow complex named palladium sulfide. PdCl2 was used as the color agent, which was dissolved in acetic acid instead of the common concentrated hydrochloric acid. The dimethoate solution was prepared by dissolving the commercial pesticides into distilled water at different concentrations. The pesticide samples were reacted with the same amount of PdC2 solution respectively. The absorbance spectra of the samples after coloring reaction were measured in the region of 300-900 nm by a spectrophotometer. The result showed that the effect of using acetic acid instead of concentrated hydrochloric acid was not only safe but also preferable, and 0.5 mg x kg(-1) was the minimum concentration of the pesticide that could be distinguished in the spectra. The result met the pesticide residue detecting requirements of part fruits and vegetables in the national standard GB2763-2012 regulations. Further studies on random 40 dimethoate samples from 0.5 to 88 mg x kg(-1) were carried out. Thirty samples were randomly selected to establish the training model and remaining 10 samples were used to test the model. The preprocessing methods were carried on the spectrum data such as normalization and smoothing to get a better effect through comparison their prediction results with the correlation coefficient (r) and the root mean square error of cross-validation (RMSEP). The principal component analysis (PCA) method and partial least squares (PLS) method were used to establish prediction models respectively in the different wave ranges. By calculating the correlation coefficient of dimethoate samples in 350-900 nm the maximum of 0.9572 was obtained at wavelength 458 nm, so 453-463 and 400-600 nm were selected as feather regions

  10. 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.

  11. Residues of organochlorine and synthetic pyrethroid pesticides in honey, an indicator of ambient environment, a pilot study.

    PubMed

    Malhat, Farag M; Haggag, Mohamed N; Loutfy, Naglaa M; Osman, Mohamed A M; Ahmed, Mohamed Tawfic

    2015-02-01

    Samples of honey were screened to monitor residues of organochlorine and pyrethroid pesticides. The study meant to examine the quality of honey, and to use honey as a bioindicator of environmental contamination. Residue levels were determined by gas chromatography (GC-μECD). Samples had a wide spectrum of organochlorine and synthetic pyrethroids pesticides, with hexachlorobenzene (HCB) as the most frequently detected organochlorine, followed by permethrin, heptachlor epoxide. Only one sample had a concentration of γ-HCH higher than maximum residue limit of honey (0.01 mg kg(-1)). Residues of organochlorines detected, indicate the presence of some fresh supplies, despite the ban imposed on their use. The study confirmed that honey bee and beehive matrices could be used as gauge for monitoring environment contamination. From public health point of view, the observed levels of pesticide residues in honey do not pose a serious health risk to the consumers, but raises questions of the source of organochlorines.

  12. Comparison of two sample preparation methods for analysis of organochlorine pesticides residues in fish muscle.

    PubMed

    Witczak, Agata; Patrzykąt, Agnieszka

    2011-01-01

    The aim of this study was to compare recoveries of organochlorine pesticides (heptachlor, α-HCH, β-HCH, γ-HCH, op'-DDD, pp'-DDD, pp'-DDE, op'-DDT, pp'-DDT) from fish muscle dried by two alternative methods: (i) grinding with anhydrous sodium sulphate and (ii) freeze drying. Pesticide residues content was determined by gas chromatography-mass spectrometry (GS-MS) method. For four pesticides (γ-HCH, α-HCH, heptachlor and pp;-DDD) in four of five fish species, higher recoveries were obtained from the freeze-dried samples. For five remaining pesticides, correlations between fish species and drying method were not found. The results of this study do not clearly indicate which drying method caused lower losses of analytes. Recoveries from the freeze-dried samples ranged from 69.9 to 117.6 %, while recoveries from the samples ground with sodium sulphate varied from 64.4 to 126.7 %. Either of the methods gave satisfactory recoveries and they both can be used interchangeably.

  13. Assessment of organochlorine pesticide residues in raw food samples from open markets in two African cities.

    PubMed

    Nuapia, Yannick; Chimuka, Luke; Cukrowska, Ewa

    2016-12-01

    This study investigates the level of organochlorine pesticides in the raw food from open markets in Kinshasa, Democratic Republic of Congo (DRC), and Johannesburg, South Africa. It assesses the potential health risks associated with the organochlorine pesticide residues. The Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method has been developed for sample preparation. A total of 120 food samples (beans, cabbage, beef, and fish) were obtained from the open markets. The mean concentrations of organochlorine pesticides in raw foods collected from the Johannesburg market were significantly higher (p < 0.05) than those from the Kinshasa market. DDE recorded the highest mean concentration (253.58 ± 4.78 μg kg(-1)) in beef from Johannesburg, and α-BHC recorded the lowest mean concentration (38.54 ± 7.46 μg kg(-1)) in beans from Kinshasa. The investigation of health risk estimates revealed that the number of organochlorine pesticides exceeded the reference dose in the collected food samples.

  14. 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.

  15. 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).

  16. 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

  17. Monitoring of organochlorine pesticide residue levels in adipose tissue of Veracruz, Mexico inhabitants.

    PubMed

    Waliszewski, Stefan M; Caba, M; Herrero-Mercado, M; Saldariaga-Noreña, H; Meza, E; Zepeda, R; Martínez-Valenzuela, C; Infanzon, R; Hernández-Chalate, F

    2011-11-01

    The objective of the present study was to monitor the levels of organochlorine pesticides HCB, α-β-γ-HCH, pp'DDE, op'DDT and pp'DDT in 150 adipose tissue samples of Veracruz, Mexico inhabitants. In analyzed samples, the following pesticides were detected: p,p'-DDE in 100% of the samples at mean 1.643 mg/kg; p,p'-DDT in 99.3.% of the samples at mean 0.227 mg/kg; β-HCH in 97.3% of the samples at mean 0.063 mg/kg; and op'DDT in 93.3% of the samples at mean 0.022 mg/kg. Comparing mean, median and geometric mean concentrations of organochlorine pesticides shows a decrease in values from mean to median and to geometric mean which points out a prevalence of lower concentrations among the total samples and the existence of occasional cases of extreme exposure expressed in range values. The pooled samples divided according to sex, showed only significant differences of pp'DDE median concentrations between sexes. The other organochlorine pesticides indicated no statistical differences between sexes, including the pp'DDE/pp'DDT ratio. The samples grouped according to age, showed that the third tertile was more contaminated for both sexes, indicating age as a positively associated factor with organochlorine pesticide levels in adipose tissue of Veracruz inhabitants. Comparing organochlorine pesticide levels between 2008 and 2010 years, a decreased tendency for β-HCH, pp'DDE, Σ-DDT and pp'DDE/pp'DDT ratio levels was observed.

  18. Hazard index, a tool for a long term risk assessment of pesticide residues in some commodities, a pilot study.

    PubMed

    Gad Alla, Sohair A; Loutfy, Naglaa M; Shendy, Amr H; Ahmed, Mohamed Tawfic

    2015-12-01

    Samples of some vegetables were analyzed for pesticides residues using the accredited (QuEChERS) method. The method allowed the determination of 215 compounds of different pesticide chemical groups. LC-MS/MS and GC-MS/MS were used for residues quantification. In a total number of 116 samples, no pesticides residues were detected in 34 samples (29.3%), while 82 samples (70.7%) had detectable pesticide residues, with some samples exceeding the MRLs levels established by the Codex Alimentarius Commission. The hazard index (HI %), representing the long--term risk assessment was in the range of 0.01%-15.04% of the ADI's. The highest exposure was observed for ethion, followed by chlorpyifos, both of them are organophosphates, at 15.04% and 2.45% of ADI respectively. The acute (short-term) exposure was also estimated. Results showed a potential risk for children posed by 3 pesticides, meanwhile, residues of one pesticides showed potential risk to adults (>100% of ARfD). The present work is an attempt to provide a model for the use of WHO template for calculating the short term intake. This model is especially useful for developing countries where information about consumption rate is rather meager.

  19. Pesticides

    MedlinePlus

    ... herbicides for destroying weeds and other unwanted vegetation, insecticides for controlling a wide variety of insects, fungicides ... Is It Safe? Movie (English & Spanish Versions) Some Natural Pesticide Alternatives (English) (114KB) Some Natural Pesticide Alternatives ( ...

  20. Organochlorine pesticide residues in drinking water in the rural areas of Haryana, India.

    PubMed

    Kaushik, C P; Sharma, H R; Kaushik, A

    2012-01-01

    Drinking water samples collected from rural areas of three districts of Haryana during pre-monsoon and post-monsoon periods were analysed for the presence of organochlorine pesticide residues. The main source of drinking water in rural areas, i.e. groundwater in Ambala and Gurgaon districts and surface water supply in Hisar district, was found to be contaminated with isomers of HCH and endosulfan and metabolites of DDT, whereas dieldrin remained below detection limits. During the study period, the mean values observed for total HCH, DDT and endosulfan were 87.6, 848.2, and 27.4 ng/L and 99.8, 275.3 and 164.2 ng/L, respectively, for Ambala and Gurgaon districts. In the case of Hisar district, the values were 78.5, 115.9, and 53.0 ng/L, respectively. During the study period, 37% of the samples exceeded the total pesticide level of 500 ng/L indicated in the EECD directive for drinking water. Seasonal variations of pesticide residues were also observed during the study period.

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

    PubMed

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

    2011-07-27

    A rapid, specific, and sensitive method based on the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) method and a cleanup using dispersive solid-phase extraction with MgSO(4), PSA, and C18 sorbents has been developed for the routine analysis of 14 pesticides in strawberries. The analyses were performed by three different analytical methodologies: gas chromatography (GC) with electron capture detection (ECD), mass spectrometry (MS), and tandem mass spectrometry (MS/MS). The recoveries for all the pesticides studied were from 46 to 128%, with relative standard deviation of <15% in the concentration range of 0.005-0.250 mg/kg. The limit of detection (LOD) for all compounds met maximum residue limits (MRL) accepted in Portugal for organochlorine pesticides (OCP). A survey study of strawberries produced in Portugal in the years 2009-2010 obtained from organic farming (OF) and integrated pest management (IPM) was developed. Lindane and β-endosulfan were detected above the MRL in OF and IPM. Other OCP (aldrin, o,p'-DDT and their metabolites, and methoxychlor) were found below the MRL. The OCP residues detected decreased from 2009 to 2010. The QuEChERS method was successfully applied to the analysis of strawberry samples.

  2. Analysis of a database of pesticide residues on plants for wildlife risk assessment.

    PubMed

    Baril, Alain; Whiteside, Mélanie; Boutin, Céline

    2005-02-01

    Current methods to estimate exposure of wildlife to pesticides from diet depend on a database of published residue concentrations on crop plants normalized to a standard application rate to obtain a residue from a unit dosage (RUD). This database, first published in the early 1970s, was updated in the 1990s. For each category of crops, maximum and mean residues are determined and used to extrapolate concentrations on plants across application rates in calculations of risk. The present study aims to update the database, to examine the validity of extrapolating RUD values across application rates, and to improve the categorization of crops using crop morphology and cultivation methods. The slope of the linear regression of residue concentrations against application rate in 41 trials was significantly different from one in all but five cases. This supports the assumption that residue concentrations are directly proportional to the application rate, although less than half the variance in residue concentrations was explained by the linear model. Residues on leaves were partitioned into eight categories of crops using information regarding plant morphology and cultivation method. Fruit size was an additional variable useful for segregating residues into four categories: Small fruits, large fruits, pods, and grains. The proposed changes increase the amount of variance explained in the residue database from 19 to 32%. Depending on the crop category, residues on fruits were 2- to 16-fold lower than those on leaves. Residue concentrations on leaves of short plants were more than fourfold higher than those on leaves of tall plants. Descriptive statistics are provided for each of the proposed crop categories.

  3. 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

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

    NASA Astrophysics Data System (ADS)

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

    2011-05-01

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

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

    PubMed

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

    2015-10-01

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

  6. 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.

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

    PubMed

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

    2006-04-01

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

  8. 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.

  9. 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

    ... of Receipt of Pesticide Petition Filed for Residues of Potassium Peroxymonosulfate in or on Various... for residues of potassium peroxymonosulfate in or on various commodities. DATES: Comments must be... antimicrobial, potassium peroxymonosulfate, in or on poultry; eggs, meat, fat and meat byproducts; swine;...

  10. Monitoring Pesticide Residues in Fruits and Vegetables at Two of the Biggest Fresh Produce Markets in Africa.

    PubMed

    Mutengwe, Mbulaheni T; Chidamba, Lizyben; Korsten, Lise

    2016-11-01

    In most countries, fresh produce sold at local markets is usually not analyzed for agricultural chemical residues as export products are, which raises concerns about the perceived safety levels of local food supplies in contrast with exported products. The aim of this study was to determine pesticide residue levels in fruits and vegetables sold at two of the biggest fresh produce markets in Africa. A total of 199 fruit and vegetable samples were collected between 2012 and 2014 and analyzed for 74 pesticides commonly used in the horticultural sector. Of the samples analyzed, 91% were compliant with set maximum residue levels (MRLs). The remaining samples either contained unregistered chemicals (8%) or exceeded set MRL values (1%). Products containing more than one pesticide residue constituted 4.02% of all samples tested. Imazalil and iprodione were found to be the most frequently detected pesticides (12 samples each). Boscalid, endosulfan, profenofos, and procymidone were associated with the most noncompliance, including exceeding MRL values or being unregistered for the specific crop. The establishment of a national pesticide monitoring program is essential for the country and would ensure that pesticides are used in accordance with good agricultural practices.

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

    NASA Astrophysics Data System (ADS)

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

    2017-01-01

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

  12. 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.

  13. [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.

  14. Heavy metal, polychlorinated biphenyl and organochlorine pesticide residues in marine organisms: risk evaluation for consumers.

    PubMed

    Marcotrigiano, G O; Storelli, M M

    2003-09-01

    This survey provides information on the levels of heavy metal, polychlorinated biphenyl and organochlorine pesticide residues in marine organisms to ascertain whether these concentrations exceeded the prescribed legal limits. In order to assess the potential human health impact, the weekly intake was estimated. Most of the organisms analysed showed higher levels of mercury than the maximum permissible limit, while cadmium and lead were below the proposed permissible limits in all samples. The estimated intake was far above the established Provisional Tolerable Weekly Intake for all metals, except for total mercury.

  15. Targeted pesticide residue analysis using triple Quad LC-MS/MS.

    PubMed

    Alder, Lutz

    2011-01-01

    The determination of pesticide residues by HPLC-MS/MS requires decisions on a multitude of analytical parameters. This includes the selection of eluents, columns and ion sources, but also the optimization of the tandem mass spectrometer for the selected target analytes. Another aspect is the use of the restricted acquisition time between two chromatographic data points. An appropriate selection of all these parameters as well as the measures to avoid interference by cross talks and wrong quantitative results by matrix effects is discussed in this chapter.

  16. Use of Carbon Nanotubes for the Analysis of Pesticide Residues in Fruits and Vegetables.

    PubMed

    Abdulrauf, Lukman Bola; Tan, Guan Huat

    2016-11-01

    This review presents the application of carbon nanotubes as sorbent materials in the analysis of pesticide residues in fruits and vegetables. The advantages, limitations, and challenges of carbon nanotubes, with respect to their use in analytical chemistry, are presented. The efficiency of their application as extraction sorbent materials (in terms of LOD, LOQ, linearity, relative recovery, and RSD) in SPE, solid-phase microextraction, multi-plug filtration clean-up, matrix solid-phase dispersion, and the quick, easy, cheap, effective, rugged and safe method is reported. The synthesis, functionalization, purification, and characterization methods of carbon nanotubes are also discussed.

  17. Some applications of solid phase micro extraction (SPME) in the analysis of pesticide residues in food.

    PubMed

    Volante, M; Cattaneo, M; Bianchi, M; Zoccola, G

    1998-05-01

    The Solid Phase Micro-Extraction (SPME) technique was applied to analyze chlorpropham in potatoes and amitraz in honey. The homogenized sample, suspended in water and stirred, was extracted with a 100 microns thick polidimetylsiloxane fiber and desorbed into the injection port of a gas chromatograph/mass-spectrometer (quadrupole) operating in single ion monitoring. Sensitivities down to 0.01 mg/Kg and linear responses in the range of 0.01-0.1 mg/Kg were obtained. The results of SPME pesticide residue analysis in potatoes corresponded to those obtained with a traditional multiresidue method.

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

    PubMed Central

    Toumi, Khaoula; Vleminckx, Christiane; van Loco, Joris; Schiffers, Bruno

    2016-01-01

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

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

    PubMed

    Toumi, Khaoula; Vleminckx, Christiane; van Loco, Joris; Schiffers, Bruno

    2016-09-23

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

  20. 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.

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

    PubMed

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

    2016-11-01

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

  2. 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.

  3. 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

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

    PubMed

    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.

  5. 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

  6. Residues of currently and never used organochlorine pesticides in agricultural soils from Zhejiang Province, China.

    PubMed

    Zhang, Anping; Fang, Li; Wang, Junliang; Liu, Weiping; Yuan, Hejin; Jantunen, Liisa; Li, Yi-Fan

    2012-03-28

    Studies on residues of currently and never used organochlorine pesticides (OCPs) facilitate the assessment of the contamination level, distribution, sources, transportation, and trend of these selected OCPs in China. In this work we investigated the concentration levels of endosulfans and chlordane, which are currently used, and the never used aldrin and dieldrin in the province of Zhejiang, a rainy, and hilly tea-growing province in eastern China. The average/mean residue levels of OCPs was in the order ∑endosulfan > ∑chlordane > aldrin > dieldrin. The residue level was in good agreement with the usage of OCPs in Zhejiang. The spatial distribution showed that the residues of OCPs in soils from the mountain area were always higher than those in soils from the plains. The distribution characteristics were related to usage for current-use OCPs and temperature for never used OCPs. The isomeric ratios and enantiomeric fractions are useful tools to identify the degradation preference of contaminants. The wide range of ratios between trans-chlordane (TC) and cis-chlordane (CC) indicated that the degradation of the two isomers of chlordane was different at different sites. Nonracemic residues of TC and CC were observed in most soils; this is significant since the enantiomers have different toxicities.

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

    PubMed

    Turgut, Cafer; Ornek, Hakan; Cutright, Teresa J

    2011-02-01

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

  8. Chronic dietary risk characterization for pesticide residues: a ranking and scoring method integrating agricultural uses and food contamination data.

    PubMed

    Nougadère, Alexandre; Reninger, Jean-Cédric; Volatier, Jean-Luc; Leblanc, Jean-Charles

    2011-07-01

    A method has been developed to identify pesticide residues and foodstuffs for inclusion in national monitoring programs with different priority levels. It combines two chronic dietary intake indicators: ATMDI based on maximum residue levels and agricultural uses, and EDI on food contamination data. The mean and 95th percentile of exposure were calculated for 490 substances using individual and national consumption data. The results show that mean ATMDI exceeds the acceptable daily intake (ADI) for 10% of the pesticides, and the mean upper-bound EDI is above the ADI for 1.8% of substances. A seven-level risk scale is presented for substances already analyzed in food in France and substances not currently sought. Of 336 substances analyzed, 70 pesticides of concern (levels 2-5) should be particularly monitored, 22 of which are priority pesticides (levels 4 and 5). Of 154 substances not sought, 36 pesticides of concern (levels 2-4) should be included in monitoring programs, including 8 priority pesticides (level 4). In order to refine exposure assessment, analytical improvements and developments are needed to lower the analytical limits for priority pesticide/commodity combinations. Developed nationally, this method could be applied at different geographic scales.

  9. 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

  10. 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.

  11. Pesticide and plasticizer residues in bergamot essential oils from Calabria (Italy).

    PubMed

    Di Bella, Giuseppa; Saitta, Marcello; La Pera, Lara; Alfa, Maria; Dugo, Giacomo

    2004-08-01

    Organophosphorus and organochlorine pesticides, phosphorated plasticizers, chloroparaffins and phthalate esters contamination in bergamot essential oils produced in Calabria in the crop years 1999-2000 was studied by HRGC in connection with detectors FPD, ECD, MS. Residues of dicofol and tetradifon were found in oils from both crop years. The mean dicofol concentration was 0.26 mg/l in samples from 1999 and 0.20 mg/l in those from 2000; the mean tetradifon content was 0.06 mg/l for both the crop years. Among plasticizers, residues of diisobutyl phthalate, di-n-butyl phthalate, and bis(2-ethylhexyl) phthalate were found in samples from crop years 1999 and 2000, the mean content were 1.22 and 1.23 mg/l, 1.51 and 1.65 mg/l, 1.38 and 1.42 mg/l respectively.

  12. 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.

  13. 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.

  14. Distribution, fate and effects of pesticide residues in tropical coastal lagoons of northwestern Mexico.

    PubMed

    Carvalho, F P; Gonzalez-Farias, F; Villeneuve, J P; Cattini, C; Hernandez-Garza, M; Mee, L D; Fowler, S W

    2002-11-01

    Analyses of pesticide residues in sediments, water and biota of the Altata-Ensenada del Pabellon coastal lagoon system in Sinaloa, Mexico, showed the presence of organochlorine and organophosphorus compounds. For all the compounds analysed, concentrations in sediments were higher near the points of water discharge from ponds and drainage from the agricultural area. Among the organochlorines, total DDTs displayed the largest sedimentary reservoir, followed by total endosulfans and chlorpyrifos. In sediments, as well as in biota, pp'-DDT concentrations were lower than those of DDT metabolites, which confirms the reduction in the previous massive use of this compound in agriculture. Endosulfan is currently used in the region and endosulfan residues in lagoon sediments attained levels considered to be toxic to meiofauna, therefore constituting an ecological risk to lagoon ecosystems. There was a large sedimentary reservoir of chlorpyrifos but its ecotoxicological risk is difficult to assess due to lack of adequate comparative data. Nevertheless, concentrations of chlorpyrifos which approach acute toxic levels for shrimp were recorded in lagoon water. This suggests that drainage from agricultural fields during high runoff may, on occasion, cause mass mortality of shrimp and fish Organophosphorus pesticides are widely regarded to degrade very rapidly in aquatic systems. Experimental research performed with 14C-labelled chlorpyrifos and parathion has shown that they may be stabilised for relatively long periods of time through sediment-water partitioning. This extension of their environmental half-lives increases their potential for impacting on coastal ecosystems. Since organophosphorus pesticides are highly toxic for aquatic organisms at concentrations generally lower than organochlorines, their presence in the lagoon water and sediment is a matter for much concern. The increased use of tropical coastal lagoons for shrimp and fish farming requires the implementation of

  15. Organochlorine pesticide residues in cow's milk from a tropical region of Mexico.

    PubMed

    Pardío, V T; Waliszewski, K N; Landín, L A; Bautista, R G

    2003-03-01

    A monitoring study was conducted to assess the magnitude of DDT [(1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane)] and HCH (hexachlorocyclohexane) contamination of bovine milk from the central tropical region of Mexico as the chemicals are extensively used in livestock and public-health programmes. Among pesticide residues analysed, the milk samples collected from Tlalixcoyan showed a mean level of gamma-HCH (0.128 mg x kg(-1)), which was significantly higher than residues in milk samples from Medellin (0.049 mg x kg(-1)) and Paso San Juan (0.022 mg x kg(-1)). The mean level of pp'-DDE in Medellin samples (0.039 mg x kg(-1)) was significantly higher than in Paso San Juan (0.018 mg x kg(-1)) and Tlalixcoyan (0.024 mg x kg(-1)) milk samples. The pp'-DDT mean level from Medellin milk samples (0.089 mg x kg(-1)) was significantly higher than the levels detected in the other two areas. The highest mean Sigma-DDT level detected in Medellin samples (0.146 mg x kg(-1)) was three times the FAO/WHO tolerance level. The highest acceptable daily intakes calculated for Sigma-DDT were 0.017 microg x kg(-1) bw day(-1) for adults and 0.530 microg x kg(-1) bw day(-1) for infants; for gamma-HCH residues, they were 0.021 microg x kg(-1) bw day(-1) for adults and 0.666 microg x kg(-1) bw day(-1) for infants, indicating that infants are more exposed to pesticide residues. Results indicate that cattle exposure to HCH and DDT results in high levels in dairy milk and a potential health risk for consumers.

  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. The organochlorine pesticides residues in the invasive ductal breast cancer patients.

    PubMed

    Yang, Jing-Zhe; Wang, Zhu-Xin; Ma, Li-Hui; Shen, Xing-Bin; Sun, Yu; Hu, Da-Wei; Sun, Li-Xin

    2015-11-01

    Investigation of organochlorine pesticides residues (important environmental contamination causing malignant transformation) in breast cancer patients is valuable to understanding their roles in breast cancer. 75 invasive ductal carcinoma (IDC) patients were enrolled with control of 79 benign breast diseases patients and control of 80 healthy women. Morning fasting blood specimens and adipose tissue specimens beside the primary lesion were detected with gas chromatograph. In blood specimens, both levels of β-HCH and PCTA were higher in IDC than those in both controls (both p<0.05), and increasingly higher among the three IDC degrees. In adipose tissue specimens, all levels of β-HCH, PCTA and pp'-DDE were higher in IDC than those in control (all p<0.05) and increasingly higher among three IDC degrees. The levels of β-HCH, PCTA in both blood specimens and adipose tissue specimens were higher in estrogen receptor (ER) positive IDC than those in ER negative IDC (all p<0.05). The higher level of organochlorine pesticides residues in blood and adipose tissue specimens of IDC infers its association with IDC, but the details remains to reveal, and this study may helpful in this field.

  18. 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.

  19. 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.

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

    PubMed

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

    2007-01-01

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

  1. Shell thickness-dependent Raman enhancement for rapid identification and detection of pesticide residues at fruit peels.

    PubMed

    Liu, Bianhua; Han, Guangmei; Zhang, Zhongping; Liu, Renyong; Jiang, Changlong; Wang, Suhua; Han, Ming-Yong

    2012-01-03

    Here, we report the shell thickness-dependent Raman enhancement of silver-coated gold nanoparticles (Au@Ag NPs) for the identification and detection of pesticide residues at various fruit peels. The Raman enhancement of Au@Ag NPs to a large family of sulfur-containing pesticides is ~2 orders of magnitude stronger than those of bare Au and Ag NPs, and there is a strong dependence of the Raman enhancement on the Ag shell thickness. It has been shown for the first time that the huge Raman enhancement is contributed by individual Au@Ag NPs rather than aggregated Au@Ag NPs with "hot spots" among the neighboring NPs. Therefore, the Au@Ag NPs with excellent individual-particle enhancement can be exploited as stand-alone-particle Raman amplifiers for the surface identification and detection of pesticide residues at various peels of fruits, such as apple, grape, mango, pear, and peach. By casting the particle sensors onto fruit peels, several types of pesticide residues (e.g., thiocarbamate and organophosphorous compounds) have been reliably/rapidly detected, for example, 1.5 nanograms of thiram per square centimeter at apple peel under the current unoptimized condition. The surface-lifting spectroscopic technique offers great practical potentials for the on-site assessment and identification of pesticide residues in agricultural products.

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

    PubMed

    Schilirò, T; Gorrasi, I; Longo, A; Coluccia, S; Gilli, G

    2011-10-01

    Food is likely to be one of the most important routes of human exposure to endocrine disrupting compounds (EDCs). In the present study, we evaluated the total estrogenic activity of fruits and vegetables, which was calculated using the human breast cancer cell line (MCF-7 BUS) proliferation assay (E-screen), in relation to pesticide residues. We analysed 44 food samples, 30 fruits and 14 vegetables. Of these samples, 10 did not contain any pesticide residues. The other 34 samples contained from 1 to 7 pesticide residues in concentrations ranging from 0.03 to 1.91 ppm. Estrogenic activity was detected in the 59% of samples tested. The positive controls used were 17-β-estradiol (E2), the phytoestrogen genistein and the pesticide endosulfan. The average value of estradiol equivalency quantity (EEQ) for all positive samples was 0.15±0.32 μg/100g. A low correlation was found between the concentration of pesticide residues and the EEQ values (Spearman correlation r=0.376 and p=0.012). Using values obtained from the literature, we compared the estrogenic activity of food samples with the intrinsic content of phytoestrogens, but we found no correlations. Our results also suggested that the calculated intake of dietary EDCs might represent a concentration comparable to the normal endogenous estrogen concentration in human blood.

  3. Pesticide residues and estrogenic activity in fruit and vegetables sampled from major fresh produce markets in South Africa.

    PubMed

    Mutengwe, Mbulaheni Thomas; Aneck-Hahn, Natalie Hildegard; Korsten, Lise; Van Zijl, Magdalena Catherina; De Jager, Christiaan

    2016-01-01

    Food is likely to be one of the major pathways through which people are exposed to endocrine-disrupting chemicals. With the exception of residual effects, there are concerns that a number of naturally occurring and synthetic chemicals exert adverse effects upon endocrine systems in wildlife and humans. The current study reports selected pesticide concentrations and the total estrogenic activity of fruit and vegetables using the recombinant yeast oestrogen screen (YES) and T47D-KBluc reporter gene assays. A total of 53 food samples (27 fruit and 26 vegetables) from Johannesburg and Tshwane fresh produce markets (in South Africa) were analysed. Of these, 17 contained one to three different pesticide residues with concentrations ranging between 0.01 and 0.68 mg kg(-1), whereas in the rest of the samples no residues were detected. All pesticides detected except in one sample were below the maximum residue level (MRL), but others were unauthorised for use in specified fruit and vegetables. Estrogenic activity was detected in 26.4% (14 samples) of the samples tested, and the estradiol equivalents ranged from 0.007 to 2 pg g(-1). Although the estrogenic activity was low, it may contribute to adverse health effects. Continuous monitoring for pesticides in fruit and vegetables is important in view of the unauthorised pesticides detected in produce from South Africa and the endocrine-disrupting chemical activity found.

  4. 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

    2012-05-09

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

  5. 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.

  6. 77 FR 26477 - Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-05-04

    ... INFORMATION CONTACT: Andrew Bryceland, Biopesticides and Pollution Prevention Division (7511P), Office of... Director, Biopesticides and Pollution Prevention Division, Office of Pesticide Programs. BILLING CODE...

  7. 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

    ... production (NAICS code 112). Food manufacturing (NAICS code 311). Pesticide manufacturing (NAICS code 32532... . List of Subjects Environmental protection, Agricultural commodities, Feed additives, Food...

  8. 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

    ... manufacturing (NAICS code 311). Pesticide manufacturing (NAICS code 32532). This listing is not intended to be... . List of Subjects Environmental protection, Agricultural commodities, Feed additives, Food...

  9. Organochlorine pesticide residues in human milk and estimated daily intake (EDI) for the infants from eastern region of Saudi Arabia.

    PubMed

    Hajjar, M Jamal; Al-Salam, Ahmad

    2016-12-01

    This study presents the level of organochlorine pesticide (OC) residues in human milk samples collected from donor mothers aged from 18 to 30 years old, from four cities in Eastern district of Saudi Arabia (Al-Hassa, Al- Khobar, Al-Jubail, and Al-Dammam). Pesticides residues were extracted from the samples and analyzed using GC-MS. The results showed that, only pp'DDE and p,pDDD, were found in 82.5% and 70% of analyzed samples respectively, the total DDT were at level of 0.37, 0.32, 0.30 and 0.46 μg/L in the four cities respectively and were far below the MRL of 50 μg/L (FAO/WHO). The estimated daily intake (EDI) of DDT ingested by infant weight 3.5 kg ranged between 0.06 and 0.10 μg/kg, which is less than the ADI issued by (EFSA, 2014). Lindane (γ-HCH) found in 91.25% of the analyzed samples at level of 0.37, 0.35, 0.35 and 0.29 μg/L. The EDIs of Lindane by infant were far below the ADI of 5 μg/kg bw/day. Dieldrin and Enderin were found in 27.5% and 58.8% of samples respectively and were lower than MRL issued by FAO/WHO, but the (EDI) was higher than the ADI issued by EFSA. The isomer A-heptachlor was detected in 51% of the samples, at levels were 15 times lower than the MRL issued by FAO/WHO, but EDIs by infants were 2-4 times higher than the ADI issued by EFSA. However, the results of the four studied areas in Saudi Arabia showed no statistically different among locations (p > 0.05).

  10. Organochlorine pesticide residue levels in blood serum of inhabitants from Veracruz, Mexico.

    PubMed

    Waliszewski, Stefan M; Caba, M; Herrero-Mercado, M; Saldariaga-Noreña, H; Meza, E; Zepeda, R; Martínez-Valenzuela, C; Gómez Arroyo, S; Villalobos Pietrini, R

    2012-09-01

    The objective of the present study was to monitor the levels of organochlorine pesticides HCB; α-, β-, γ-HCH; pp'DDE; op'DDT; and pp'DDT in blood serum of Veracruz, Mexico inhabitants. Organochlorine pesticides were analyzed in 150 blood serum samples that constituted that which remained after clinical analyses, using gas chromatography-electron-capture detection (GC-ECD). The results were expressed as milligrams per kilogram on fat basis and micrograms per liter on wet weight. Only the following pesticides were detected: p,p'-DDE was the major organochlorine component, detected in 100% of samples at mean 15.8 mg/kg and 8.4 μg/L; p,p'-DDT was presented in 41.3.% of monitored samples at mean 3.1 mg/kg and 1.4 μg/L; β-HCH was found in 48.6% of the samples at mean 4.9 mg/kg and 2.7 μg/L; op'DDT was determined to be in only 3.3% of monitored samples at mean 2.7 mg/kg and 1.4 μg/L. The pooled samples divided according to sex showed significant differences of β-HCH and pp'DDE concentrations in females. The samples grouped according to age presented the third tertile as more contaminated in both sexes, indicating age as a positively associated factor with serum organochlorine pesticide levels in Veracruz inhabitants.

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

    PubMed

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

    2010-12-01

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

  12. Pesticide residue free fruits: the aim of Trentino apple production system.

    PubMed

    Baldessari, M; Giuliani, G; Chiesa, S; Larcher, R; Ioriatti, C; Angeli, G

    2013-01-01

    Chemical analyses performed in 2011 on the 575 samples of apples in Trentino (Italy), there are in average 3.24 active ingredient per sample. Moreover, in 98% of the samples with detectable residues, the level did not exceed 30% of the official MRL This result is achieved thanks to the implementation of the guide lines for integrated production by the 8000 fruit growers, to an extension service which justifies the need of the treatment and gives advice on which pesticide fit better for the time-pest combination, to the systematic check up of the sprayers, to the correct sizing of mix volumes to spray according to the size of the canopy, to the selection of active ingredients based on their residual activity in field tests, and to the systematic monitoring of the level of residues found on representative samples of the product at harvest. With these assumptions, the next goal is to eliminate all traces of insecticides and acaricides now present only in 30% of the samples. This aim could be achieved by extending the use of pheromone mating disruption to control fruit feeding Lepidoptera, as well as by promoting the use of short persistent residue products during the final part of the season. Results of some of the experimental field trials are presented and discussed.

  13. [Validation study on a multi-residue method for determination of pesticide residues in agricultural products by new automatic pretreatment equipment (FASRAC) and GC-MS/MS].

    PubMed

    Okuda, Taiki; Koshi, Naohiro; Matsumura, Atsushi; Yamamoto, Reo; Oyanagi, Tatsuya; Matsuda, Takahiro; Hashimoto, Akihiko; Hatakeyama, Osamu; Kobayashi, Kazuhiro; Nagao, Yasuhiro; Yamada, Toshihiro

    2014-01-01

    A validation study was performed on a multiresidue method for determination of pesticide residues in agricultural products according to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan. FASRAC (Food Automatic Analytical Systems for Residual Agricultural Chemicals) automatically performs extraction of pesticide residues from agricultural products with acetonitrile, filtration, constant volume, mixing with the use of air, mixing acetonitrile with buffer solvent, separation, and dehydration with sodium sulfate. The extract was purified with a GC/NH2 column. For wheat flour and soybeans, a purification step with a C18 column was added before a GC/NH2 column. After removal of the solvent, the extract was resolved in n-hexane/acetone solvent for GC-MS/MS analysis. In the case of manual analysis, pesticide residues were analyzed according to official multiresidue methods and purification steps were the same as in FASRAC. Recovery tests were performed with wheat flour, soybeans, spinach and apples, by addition of 302 pesticides at the concentrations 0.01 mg/kg. The results indicate that automatic extraction using FASRAC is superior to manual analysis in trueness, repeatability and within-run reproducibility. Specially, automatic extraction using FASRAC is superior to manual analysis in trueness because it is optimized in various respects, for example reextraction at salting-out.

  14. [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.

  15. Proposal for field-based definition of soil bound pesticide residues.

    PubMed

    Boesten, J J T I

    2016-02-15

    The environmental significance of soil bound pesticide residues (SBPR) is potentially large because approximately one third of the applied mass of the pesticides in agriculture ends up as SBPR. At EU level, there is little regulatory guidance available on the environmental risk assessment of SBPR in spite of some 50 years of SBPR research. This lack of guidance is partially caused by the fact that the current definitions of SBPR are founded on non-extractability in soil in the laboratory whereas for the environmental risk assessment not the soil in the laboratory but the soil in the field is the system of interest. Therefore a definition of SBPR is proposed that is based on the field soil: a molecule (further called 'the mother molecule') is soil bound if a relevant part of this molecule has become part of the solid phase in the soil and if this relevant part will never be released again to the liquid phase in soil under relevant field conditions in the form of this mother molecule or in the form of another molecule that may possibly raise environmental or human toxicological concerns. This mother molecule may be the parent substance that is applied to the soil but it may also be a metabolite of this parent substance. A consequence of the definition is that the SBPR terminology becomes more precise because the mother molecule of the soil bound residue has to be specified. A further consequence is that very strong but reversible sorption of molecules such as paraquat is not considered soil-bound residue anymore (as may be demonstrated by a self-exchange extraction procedure). Furthermore, the definition requires that risk managers have to define what they consider as 'relevant field conditions' (e.g. include also changes of agricultural fields into forests?).

  16. 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.

  17. [Determination of residual pesticides in processed foods manufactured from livestock foods and seafoods using ion trap GC/MS].

    PubMed

    Makabe, Yuhki; Miyamoto, Fumio; Hashimoto, Hiroyuki; Nakanishi, Kiyoko; Hasegawa, Yasuyuki

    2010-01-01

    A simultaneous method using iontrap gas chromatography/mass spectrometry (GC/MS) was developed for the determination of pesticide residues in four processed foods (frozen Chinese dumpling, eel kabayaki, corned beef and retort curry). Pesticide residues were extracted from samples with ethyl acetate-cyclohexane (1:1) in the presence of anhydrous sodium sulfate. The extract was concentrated and the residue was dissolved in n-hexane. The lipids in the extract were removed by acetonitrile-n-hexane partitioning, following which the acetonitrile layer was cleaned up using a C(18) mini-cartridge column and a graphite carbon/PSA silica (GCB/PSA) mini-cartridge column. The limits of quantification of compounds in 4 processed foods were below 0.01 microg/g. The recoveries of 292 compounds spiked at 0.1 microg/g in 4 kinds of processed foods, and 210 to 262 pesticides showed acceptable recoveries of 70-120% with low repeatability (15%) and intermediate precision (<20%) only at the 0.1 microg/g spiked level. This method is expected to be useful for multi-residue analysis of pesticide residues in processed foods manufactured using livestock and seafoods as the main raw materials.

  18. Pesticide and transformation product detections and age-dating relations from till and sand deposits

    USGS Publications Warehouse

    Warner, K.L.; Morrow, W.S.

    2007-01-01

    Pesticide and transformation product concentrations and frequencies in ground water from areas of similar crop and pesticide applications may vary substantially with differing lithologies. Pesticide analysis data for atrazine, metolachlor, alachlor, acetochlor, and cyanazine and their pesticide transformation products were collected at 69 monitoring wells in Illinois and northern Indiana to document occurrence of pesticides and their transformation products in two agricultural areas of differing lithologies, till, and sand. The till is primarily tile drained and has preferential fractured flow, whereas the sand primarily has surface water drainage and primary porosity flow. Transformation products represent most of the agricultural pesticides in ground water regardless of aquifer material - till or sand. Transformation products were detected more frequently than parent pesticides in both the till and sand, with metolachlor ethane sulfonic acid being most frequently detected. Estimated ground-water recharge dates for the sand were based on chlorofluorocarbon analyses. These age-dating data indicate that ground water recharged prior to 1990 is more likely to have a detection of a pesticide or pesticide transformation product. Detections were twice as frequent in ground water recharged prior to 1990 (82%) than in ground water recharged on or after 1990 (33%). The highest concentrations of atrazine, alachlor, metolachlor, and their transformation products, also were detected in samples from ground water recharged prior to 1990. These age/pesticide detection relations are opposite of what would normally be expected, and may be the result of preferential flow and/or ground-water mixing between aquifers and aquitards as evident by the detection of acetochlor transformation products in samples with estimated ground-water ages predating initial pesticide application. ?? 2007 American Water Resources Association.

  19. 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....

  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 CBI... protection, Agricultural commodities, Feed additives, Food additives, Pesticides and pests, Reporting...

  1. 78 FR 6274 - Withdrawal of Pesticide Petitions for Residues of Pesticide Chemicals in or on Various Commodities

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-01-30

    ...), which announced the filing of a pesticide petition (PP 0E7754) by Quimica Agronomica de Mexico, S. de R... Quimica Agronomica de Mexico) notified EPA that it was withdrawing this petition. Contact: Shaunta Hill...), which announced the filing of pesticide petition (PP 0E7755) by Quimica Agronomica de Mexico, S. de...

  2. 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.

  3. 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.

  4. 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.

  5. Determination of multiclass pesticide residues in apple juice by gas chromatography-mass spectrometry with large-volume injection.

    PubMed

    Wang, Jian-Hua; Zhang, Yi-Bing; Wang, Xiu-Lin

    2006-10-01

    This study presents two GC-MS SIM methods, in combination with large-volume injection programmed-temperature vaporization (LVI-PTV) injection, for the determination of 141 pesticide residues in apple juice. The sample was extracted with ACN, and coextractives were removed with primary/secondary amine sorbent. ACN extract (20 microL) was injected into a PTV injection port in solvent vent mode, and the pesticides were determined by GC-MS using retention time locking software. Deuterium-labeled pesticides (surrogate standards) were used for analytical quality control. In the validation experiments, pesticides recoveries were found to be 70-121% with RSDs of 4.6-21% (n = 6).

  6. 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.

  7. Pesticides

    MedlinePlus

    ... control. Examples of different kinds of pesticides include insecticides, rodenticides, and herbicides, to name a few. Top ... can lead to severe toxicity requiring hospitalization. Organophosphate insecticides also work by increasing the amount of acetylcholine ...

  8. 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...

  9. 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.

  10. Comparison of the relative dissipation rates of endosulfan pesticide residues between oolong and green tea.

    PubMed

    Xia, H; Ma, X; Tu, Y

    2008-01-01

    The dissipation behaviour of endosulfan in dry made-tea leaves of oolong and green tea was compared to establish whether there was any difference in dissipation rates between the two teas. The dissipation of endosulfan in oolong and green tea corresponded with a first-order kinetics curve. The average half-life of endosulfan (n = 12) was 1.60 +/- 0.44 days in green tea and 2.01 +/- 0.55 days in oolong tea, showing a statistically significant difference, and indicating that the dissipation of the pesticide was significantly slower in oolong tea than that in green tea. Although the initial levels of residual endosulfan were lower in oolong tea, due to the slower dissipation rate, the residues 5-7 days after application were higher in oolong than in green tea. It is suggested that the minimum interval between endosulfan application and tea leaf harvesting is 7 days for green tea and 10 days for oolong tea in the case where the maximum residue limit of endosulfan in made-tea is fixed as 10 mg kg(-1).

  11. Applications of solid-phase microextraction for the analysis of pesticide residues in fruits and vegetables: a review.

    PubMed

    Abdulra'uf, Lukman Bola; Chai, Mee Kin; Tan, Guan Huat

    2012-01-01

    This paper reviews the application of various modes of solid-phase microextraction (SPME) for the analysis of pesticide residues in fruits and vegetables. SPME is a simple extraction technique that eliminates the use of solvent, and it is applied for the analysis of both volatile and nonvolatile pesticides. SPME has been successfully coupled to both GC and LC. The coupling with GC has been straightforward and requires little modification of existing equipment, but interfacing with LC has proved challenging. The external standard calibration technique is widely used for quantification, while standard addition and internal or surrogate standards are mainly used to account for matrix effects. All parameters that affect the extraction of pesticide residues from fruits and vegetables, and therefore need to be optimized, are also reviewed. Details of the characteristics of analytical procedures and new trends in fiber production using sol-gel technology and molecularly imprinted polymers are discussed.

  12. 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)

  13. 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.

  14. 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.

  15. 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.

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

    PubMed

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

    2012-01-01

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

  17. [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".

  18. [Determination of organophosphorous pesticide residues in red wine by solid phase microextraction-gas chromatography].

    PubMed

    Hu, Yuan; Liu, Wenmin; Zhou, Yanming; Guan, Yafeng

    2006-05-01

    A method for the determination of 12 organophosphorus pesticide residues (OPs) in red wine by fiber solid phase microextraction (SPME) coupled with gas chromatography (GC) was developed and validated. The SPME phase was prepared by sol-gel technology of physical incorporation. The extraction conditions were optimized with the results of stirring rate of 1,250 r/min, NaCl mass concentration of 150 g/L, and extraction time of 30 min. With the sample volume of 25 mL, the relative standard deviations (RSD) of peak areas for most of OPs were below 5%, and the detection limits of OPs were in the range of 5 ng/L-0.38 microg/L. It can be seen from the results that this method has the potential to analyze OPs in other beverages and soft drinking materials.

  19. Validation of an Efficient Method for the Determination of Pesticide Residues in Fruits and Vegetables Using Ethyl Acetate for Extraction

    Technology Transfer Automated Retrieval System (TEKTRAN)

    In this study, a version of the “quick, easy, cheap, effective, rugged, and safe” (QuEChERS) method was modified to use ethyl acetate (EtOAc) rather than acetonitrile (MeCN) for extraction in the determination of multiple pesticide residues in fruits and vegetables. EtOAc is better suited than MeCN...

  20. 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...

  1. 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...

  2. 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...

  3. 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...

  4. 75 FR 17715 - Notice of Receipt of a Pesticide Petition Filed for Temporary Tolerance Exemption for Residues of...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-04-07

    ..., Virginia, Washington, and West Virginia. PDJ is intended for use as a plant growth regulator. DATES... tolerance exemption for residues of the plant growth regulator, prohydrojasmon (PDJ), in or on red apple... Pollution Prevention Division (7511P), Office of Pesticide Programs, Environmental Protection Agency,...

  5. 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

  6. 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.

  7. 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

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

    PubMed Central

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

    2015-01-01

    STUDY QUESTION Is consumption of fruits and vegetables with high levels of pesticide residues associated with lower semen quality? SUMMARY ANSWER Consumption of fruits and vegetables with high levels of pesticide residues was associated with a lower total sperm count and a lower percentage of morphologically normal sperm among men presenting to a fertility clinic. WHAT IS KNOWN ALREADY Occupational and environmental exposure to pesticides is associated with lower semen quality. Whether the same is true for exposure through diet is unknown. STUDY DESIGN, SIZE, DURATION Men enrolled in the Environment and Reproductive Health (EARTH) Study, an ongoing prospective cohort at an academic medical fertility center. Male partners (n = 155) in subfertile couples provided 338 semen samples during 2007–2012. PARTICIPANTS/MATERIALS, SETTING, METHODS Semen samples were collected over an 18-month period following diet assessment. Sperm concentration and motility were evaluated by computer-aided semen analysis (CASA). Fruits and vegetables were categorized as containing high or low-to-moderate pesticide residues based on data from the annual United States Department of Agriculture Pesticide Data Program. Linear mixed models were used to analyze the association of fruit and vegetable intake with sperm parameters accounting for within-person correlations across repeat samples while adjusting for potential confounders. MAIN RESULTS AND THE ROLE OF CHANCE Total fruit and vegetable intake was unrelated to semen quality parameters. High pesticide residue fruit and vegetable intake, however, was associated with poorer semen quality. On average, men in highest quartile of high pesticide residue fruit and vegetable intake (≥1.5 servings/day) had 49% (95% confidence interval (CI): 31%, 63%) lower total sperm count and 32% (95% CI: 7%, 58%) lower percentage of morphologically normal sperm than men in the lowest quartile of intake (<0.5 servings/day) (P, trend = 0.003 and 0

  9. 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.

  10. 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.

  11. 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

  12. Pressurised fluid extraction (PFE) as an alternative general method for the determination of pesticide residues in rape seed.

    PubMed

    Pihlström, Tuija; Isaac, Giorgis; Waldebäck, Monica; Osterdahl, Bengt-Göran; Markides, Karin E

    2002-04-01

    A pressurised fluid extraction (PFE) multi-method has been developed for the determination of pesticide residues in rape seed. The method was validated for 25 different pesticides and metabolites. The reliability and efficiency of PFE for extracting pesticide residues from rape seed was investigated. The traditional extraction solvent, hexane saturated with acetonitrile, was used at elevated temperature and pressure. With increased temperature, the extraction kinetics were improved but at the same time more co-extractives were obtained in the form of lipids. When 1 g of rape seed was extracted at temperatures from 60 degrees C to 150 degrees C, the lipid content extracted was found to be as high as 17-26%. An additional clean-up step was therefore required and lipid co-extractives were effectively removed by gel permeation chromatography. The interpretation of the chromatograms and the quantification of the results were satisfactorily improved by the removal of interfering lipids. The developed method was used to extract vinclozolin and iprodione from incurred samples, resulting in a concentration in accordance with the results using conventional liquid-liquid extraction (LLE) between hexane and acetonitrile and also supercritical fluid extraction (SFE) using carbon dioxide. The results of the present study suggest that PEE is a good alternative extraction technique for the determination of pesticide residues in oil seed. Despite the necessity for a lipid-removal clean-up step, the PFE technique facilitated the extraction process by faster extractions and the possibility of automated analysis.

  13. Residues of organochlorine pesticides, polychlorinated biphenyls, and mercury and autopsy data for bald eagles, 1969 and 1970

    USGS Publications Warehouse

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

    1972-01-01

    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. 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.

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

    PubMed

    Scholtz, M T; Bidleman, T F

    2007-05-01

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

  16. [Validation Study on a Multi-Residue Method for Determination of Pesticide Residues in Vegetables and Fruits by using General Matrix Standard Solutions].

    PubMed

    Fukui, Naoki; Takatori, Satoshi; Yamaguchi, Satoko; Kitagawa, Yoko; Yoshimitsu, Masato; Osakada, Masakazu; Kajimura, Keiji; Obana, Hirotaka

    2015-01-01

    Quantitative methods using the matrix-matched standard solutions approach are widely used for multi-residue pesticide determination by GC-MS/MS to deal with the issue of matrix effects. However, preparing matrix-matched standard solutions in analyses of many kinds of samples is very time-consuming. In order to solve this problem, a method that employs general matrix standard solutions has been developed using polyethylene glycol (PEG), extract of vegetables-fruit juice (VFJm) and triphenyl phosphate (named the PEG-VFJm method). Here, a validation study for 168 pesticides was performed on three kinds of samples [potato, spinach and apple] at concentrations of 0.010 and 0.050 μg/g. In these three commodities, 144 to 158 pesticides satisfied the required criteria using the matrix-matched method and 129 to 149 pesticides satisfied the same criteria using the PEG-VFJm method. Our results suggest that application of general matrix standard solutions would enable rapid and effective analyses of pesticides.

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

    PubMed

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

    2014-01-01

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

  18. 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.

  19. Concentrations of organochlorine pesticides (OCPs) residues in foodstuffs collected from traditional markets in Indonesia.

    PubMed

    Shoiful, Ahmad; Fujita, Hiroyuki; Watanabe, Isao; Honda, Katsuhisa

    2013-02-01

    A total 23 of organochlorine pesticides (OCPs) residues were determined in five groups of foodstuffs, i.e.: vegetables (carrot, potato, cucumber, corn, and onion), rice, pulses (green bean and soybean), nuts (peanut), and fish (milkfish), which collected from traditional markets in three big cities of Indonesia; Jakarta, Bogor, and Yogyakarta. OCPs were only detected in fatty foodstuffs, such as soybean, peanut, and milkfish. The concentration of HCB (expressed as ng g(-1) on a whole basis), ΣDrins, ΣDDTs, ΣHeptachlors, and ΣHCHs were in the range of <0.3-0.74 ng g(-1), <0.03-0.42 ng g(-1), <0.02-0.41 ng g(-1), <0.03-0.14 ng g(-1), and <0.03-0.06 ng g(-1), respectively, which were far below the maximum residue limits (MRLs) as established by FAO/WHO. These very low concentrations of OCPs residues in foodstuffs indicated that OCPs were used only in past time and no recent input into the environment. Furthermore, the estimated daily intake (EDI) of HCB, ΣDDTs, ΣDrins, ΣHeptachlors, and ΣHCHs in five group foodstuffs, which were 60% of total daily diet of Indonesian, were 0.09 ng kg(-1) bw d(-1), 0.04 ng kg(-1) bw d(-1), 0.01 ng kg(-1) bw d(-1), 0.003 ng kg(-1) bw d(-1), and 0.002 ng kg(-1) bw d(-1), respectively. These results were far below the acceptable daily intake (ADI) as established by FAO/WHO, which indicated that consumption of foodstuffs from Indonesia were at little risk to human health in term of OCPs at present.

  20. [Characteristics of organochlorine pesticide residues in agricultural soil of Chongming Island in Shanghai].

    PubMed

    Lü, Jin-Gang; Bi, Chun-Juan; Chen, Zhen-Lou; Zhou, Jie-Cheng

    2011-08-01

    Thirty surface soil samples were collected to investigate the residue concentrations of organochlorine pesticides (OCPs) in agricultural soil of Chongming Island in July 2008. Those samples were extracted using accelerated solvent extraction (ASE) and determined by gas chromatography with an electron capture detector (GC-microECD). Results showed that the concentrations of OCPs (dry weight) ranged between 3.11-117.47 ng x g(-1), with mean value of 26.25 ng x g(-1). Two major contaminants of OCPs were DDTs and HCHs, the concentration of which varied from 0.14 ng x g(-1) to 77.89 ng x g(-1) and from 1.14 ng x g(-1) to 22.43 ng x g(-1), respectively. At the same times, hexachlorobenzene (0.23-11.63 ng x g(-1)), aldrin (0.03-0.75 ng x g(-1)), heptachlor epoxide (0.05-1.44 ng x g(-1)), dieldrin (0.05-5.33 ng x g(-1)), endrin (ND-14.66 ng x g(-1)) and mirex (0.03-10.58 ng x g(-1)) could also be detected. Most of DDTs had been degraded to DDD and DDE, with the major compounds of DDE (about 64.7%), and the recent existed DDT was the residue of early input. All of the four isomers of HCHs were detected, and the contents of alpha-HCH (about 48.1%) and beta-HCH (about 33.4%) were the maximum. The highest OCPs residues appeared in the soil of farm cultivation compared to greenhouse cultivation and ordinary open-air cultivation.

  1. 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.

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

    PubMed

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

    2012-09-19

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

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

    PubMed

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

    2017-06-01

    To investigate pesticide residue concentrations and potential human health risk, a study was conducted in 118 leafy vegetable samples collected in 2014-2015 from the North Central agricultural areas of Chile. The pesticide residues were determined using the multiresidue QuEChERS method by gas chromatography as well as high-performance liquid chromatography. The results indicated that 27% of the total samples contained pesticide residues above the maximum residue limits of each active ingredient. The maximum estimated daily intake obtained for carbon disulphide (CS2), methamidophos, azoxystrobin and cypermethrin were 0.57, 0.07, 0.06 and 0.05 mg kg(-1), respectively, which was higher than their acceptable daily intake. It is concluded that inhabitants of the North Central agricultural area of Chile are not exposed to health risks through the consumption of leafy vegetables with the exception of methamidophos. Nevertheless, the high levels of methamidophos detected in leafy vegetables could be considered a potential chronic health risk.

  4. 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

    ...) number and the pesticide petition number (PP) of interest as shown in the body of this document, by one... of interest as shown in the body of this document. EPA's policy is that all comments received will be... identity or contact information unless you provide it in the body of your comment. If you send an...

  5. 75 FR 80489 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-12-22

    ... 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... in the body of your comment. If you send an e- mail comment directly to EPA without going...

  6. 77 FR 50661 - Notice of Filing of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-08-22

    ... method of analysis is aqueous organic solvent extraction, column cleanup and quantitation by LC/MS/MS. In animals, the method of analysis involves base hydrolysis, organic extraction, column cleanup and...-harvest applications. FD&C Blue 1 is already approved as a pesticide inert ingredient and has...

  7. Approaches for grouping of pesticides into cumulative assessment groups for risk assessment of pesticide residues in food.

    PubMed

    Colnot, Thomas; Dekant, Wolfgang

    2017-02-01

    The European Food Safety Authority (EFSA) is developing approaches to cumulative risk assessment of pesticides by assigning individual pesticides to cumulative assessment groups (CAGs). For assignment to CAGs, EFSA recommended to rely on adverse effects on the specific target system. Contractors to EFSA have proposed to allocate individual pesticides into CAGs relying on NOAELs for effects on target organs. This manuscript evaluates the assignments by applying EFSAs criteria to the CAGs "Toxicity to the nervous system" and "Toxicity to the thyroid hormone system (gland or hormones)". Assignment to the CAG "Toxicity to the nervous system" based, for example, on neurochemical effects like choline esterase inhibition is well supported, whereas assignment to the CAG "Toxicity to the thyroid hormone system (gland or hormones)" has been based in the examined case studies on non-reproducible effects seen in single studies or on observations that are not adverse. Therefore, a more detailed effects evaluation is required to assign a pesticide to a CAG for a target organ where many confounders regarding effects are present. Relative potency factors in cumulative risk assessment should be based on benchmark doses from studies in one species with identical study design and human relevance of effects on specific target organs should be analyzed to define minimal margins of exposure.

  8. 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

    ... 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 CBI... 40 CFR Part 180 Environmental protection, Agricultural commodities, Feed additives, Food...

  9. 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

    ... (NAICS code 111). ] Animal production (NAICS code 112). Food manufacturing (NAICS code 311). Pesticide manufacturing (NAICS code 32532). This listing is not intended to be exhaustive, but rather provides a guide for....elizabeth@ epa.gov . List of Subjects Environmental protection, Agricultural commodities, Feed...

  10. 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

    ...), requests to establish tolerances in 40 CFR part 180 for residues of the insecticide, acetamiprid, (1E)-N... CFR part 180 for the combined residues of the insecticide, flonicamid, N-(cyanomethyl)-4... of residues. However, because of the natural occurrence of ] compounds that interfere with...

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

    PubMed

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

    2016-08-01

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

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

    PubMed

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

    2012-01-01

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

  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.

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

    PubMed

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

    2011-12-01

    The aim of this study was to determine the presence of pesticides in drinking water from six aqueducts in a region of intense agricultural activity in the state of Merida, Venezuela. The study was conducted for four continuous weeks, between May and June 2008. Pesticide residues were analyzed by solid phase extraction (SPE) and liquid chromatography (HPLC) with diode array detector (DAD). The method SPE-HPLC-DAD met the criteria of analytical validation, with good linearity (R2: 0.9840 to 0.9999), precision (coefficient of inter-day variability from 1.47 to 6.25%), accuracy (relative standard deviation 0.9 to 9.20%) and sensitivity (LOD < or = 0.012 microg/L; LOQ < or = 0.030 microg/L, except mancozeb with 0.400 microg/L). Seven of the thirteen selected pesticides have a recovery rate between 100% and 70%, the rest between 61% and 37%. Ten pesticides of the following chemical groups, were detected in 72 samples analyzed: organophosphates, carbamates, triazines and urea derivatives. The pesticides with the highest frequency of detection were: carbofuran and atrazine (39%), malathion (25%), dimethoate and metribuzin (19%). The pesticides found at high levels were diazinon (26.31 microg/L), methamidophos (10.99 microg/L), malathion (2.03 microg/L) and mancozeb (1.27 microg/L). Pesticide levels did not exceed the maximum allowed by Venezuelan law, however, according to international standards (EU and EPA-USA) values were above the maximum permissible levels. This study demonstrates the urgent need for systematic monitoring of the quality of water for human consumption in regions of high agricultural productivity.

  15. [Determination of 99 pesticide residues in Paeoniae Radix Alba by gas chromatography-triple quadrupole tandem mass spectrometry].

    PubMed

    Liu, Xiaoqin; Tong, Ling; Meng, Wenting; Sun, Guoxiang

    2015-08-01

    A method was established for the simultaneous determination of 99 pesticide residues with combination of solid-phase extraction technique ( SPE) and gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS). The sample was extracted with ethyl acetate, and cleaned-up by an amino SPE column. The extract was determined by GC-MS/MS in multi-reaction monitoring (MRM) mode, and matrix-matched internal standard method was applied to quantify the pesticides. The results of all the 99 pesticides showed good linearity in the range of 0.001-0.25 mg/L, with correlation coefficients (r2) > 0.99. The limits of quantification (LOQs) were between 0.001-0.050 mg/kg. The recoveries were between 66.7% and 128.0% with RSD values typically lower than 18.3% at three spiked levels of 0.05, 0.10 and 0.20 mg/kg. This method has been applied to determine thirteen batches of commercially available samples, chlorpyriphos-ethyl and p,p'-DDE were detected in four batches of Paeoniae Radix Alba. The method is highly accurate, reliable and sensitive for monitoring the 99 pesticide residues in Paeoniae Radix Alba.

  16. Pesticide residues in Hemlock and Canadice Lakes and their tributaries in western New York, 1997-98

    USGS Publications Warehouse

    Eckhardt, David A.; Burke, Sarah

    2000-01-01

    In 1997, the U.S.Geological Survey (USGS) and the City of Rochester began a cooperative program to study the presence of pesticides (herbicides and insecticides) that occur at trace levels in Hemlock and Canadice Lakes and their tributaries. The most frequently detected pesticides in streamflow and lake-water samples were herbicides commonly used in agriculture ? atrazine, metolachlor, and simazine. None of the concentrations of these compounds in the samples exceeded Federal or State water-quality standards. Differences in the concentrations among stream samples can be attributed to land use and streamflow, and the timing of rainfall in relation to herbicide application. The north (lower) end of Hemlock Lake can receive pesticides in agricultural runoff from northern parts of its watershed and Canadice Creek. These pesticide inputs bypass most of the lake and could periodically affect the water quality periodically affect the water quality at the City of Rochester intake. Pesticide concentrations in samples from the intake during this study, however, were about 100 times less than current Federal and State standards for drinking water. Residues of DDT, dieldrin, and mirex are present in low concentrations in the bottom sediments of both lakes, but none were detected in water samples. The use of these insecticides was banned in 1972,and their persistence in the lakebed sediments is probably due to erosion of contaminated soils from agricultural lands.

  17. Pesticide residues in Hemlock and Canadice Lakes and their tributaries in western New York, 1997–98

    USGS Publications Warehouse

    Eckhardt, David A.; Burke, Sarah

    2000-01-01

    In 1997, the U.S.Geological Survey (USGS) and the City of Rochester began a cooperative program to study the presence of pesticides (herbicides and insecticides) that occur at trace levels in Hemlock and Canadice Lakes and their tributaries. The most frequently detected pesticides in streamflow and lake-water samples were herbicides commonly used in agriculture — atrazine, metolachlor, and simazine. None of the concentrations of these compounds in the samples exceeded Federal or State water-quality standards. Differences in the concentrations among stream samples can be attributed to land use and streamflow, and the timing of rainfall in relation to herbicide application.The north (lower) end of Hemlock Lake can receive pesticides in agricultural runoff from northern parts of its watershed and Canadice Creek. These pesticide inputs bypass most of the lake and could periodically affect the water quality periodically affect the water quality at the City of Rochester intake. Pesticide concentrations in samples from the intake during this study, however, were about 100 times less than current Federal and State standards for drinking water.Residues of DDT, dieldrin, and mirex are present in low concentrations in the bottom sediments of both lakes, but none were detected in water samples. The use of these insecticides was banned in 1972,and their persistence in the lakebed sediments is probably due to erosion of contaminated soils from agricultural lands.

  18. 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.

  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.

  20. 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.

  1. Selective pressurized liquid extraction for multi-residue analysis of organochlorine pesticides in soil.

    PubMed

    Hussen, Ahmed; Westbom, Rikard; Megersa, Negussie; Mathiasson, Lennart; Björklund, Erland

    2007-06-08

    A selective pressurized liquid extraction (SPLE) procedure capable of performing simultaneous extraction and clean-up has been demonstrated for multi-residue analysis of organochlorine pesticides (OCPs) in soil. The final method was performed at 100 degrees C for 3 x 10 min using acetone/n-heptane (1:1, v/v). Florisil was placed inside the extraction cell downstream the sample to remove interfering compounds. Extraction of two soil samples by SPLE gave a recovery which was over 80% for beta-endosulfan, endosulfan sulfate, p,p'-DDT and p,p'-DDE compared to PLE with off-line clean-up. The same trend was observed when applying the SPLE method to a certified reference soil sample (CRM 811-050) containing 13 OCPs, where the SPLE method gave 80-90% recovery vis-à-vis the PLE method with off-line clean-up. Feasibility of the SPLE method was further demonstrated by applying it to five real soil samples collected in Ethiopia.

  2. 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.

  3. 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

  4. Pesticide Tolerances

    EPA Pesticide Factsheets

    EPA regulates pesticides used to protect crops and sets limits on the amount of pesticide remaining in or on foods in the U.S. The limits on pesticides on foods are called tolerances in the U.S. (maximum residue limits (MRLs) in many other countries).

  5. 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.

  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 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.

  7. 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.

  8. 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.

  9. Spatio-temporal patterns of pesticide residues in the Turia and Júcar Rivers (Spain).

    PubMed

    Ccanccapa, Alexander; Masiá, Ana; Andreu, Vicente; Picó, Yolanda

    2016-01-01

    A study was conducted on the occurrence of 50 pesticides in water and sediments of Turia and Júcar Rivers (Valencian Community, Eastern Spain) for a period of two consecutive years each, 2010/2011 and 2012/2013, respectively to assess the contribution of agriculture and urban activities on pesticide pollution. The results showed that mean concentrations of pesticides ranged from pesticide whereas imazalil, thiabendazole, tolclofos methyl, ethion and carbofuran were those found at higher concentrations. Ubiquitous pesticides are those with long half-lives. The most polluted parts of the rivers were the headwaters and the mouth, which could be related to the agricultural practices and rainfall. Contrarily, in the abrupt part of the rivers of difficult access the contamination is low. Other quality parameters monitored in this study also corroborate the worst water quality in the alluvial plains that coincides with higher anthropic pressure. The temporal variations also indicated a strong relation of pesticide concentrations with hydrology, the higher the river flow, the higher number and frequency of pesticides but at lower concentrations. On the contrary, at lower river flows higher pesticide concentrations were detected. The risk assessment for aquatic biota pointed out that organophosphorus and fungicides are a threat to fish and daphnia and herbicides and fungicides are hazards for algae. Thus, the strict control of pesticide concentrations is important to preserve the aquatic ecosystems health.

  10. 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

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

    PubMed

    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.

  12. 76 FR 3885 - Notice of Receipt of a Pesticide Petition Filed for Residues of Pesticide Chemicals in or on...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-01-21

    ... the requirement of a tolerance for residues of Bacillus thuringiensis eCry3.1Ab protein under 40 CFR... exemption from the requirement of a tolerance for residues of the plant-incorporated protectant Bacillus..., sweet; and corn, pop in 40 CFR 174.532; when Bacillus thuringiensis eCry3.1Ab protein in corn is used...

  13. 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

    ...., Princeton, NJ 08540, requests to establish tolerances in 40 CFR part 180 for residues of the insecticide.... However, because of the natural occurrence of compounds that interfere with the measurement of triazoles...., Princeton, NJ 08540, requests to amend the tolerances in 40 CFR 180.466 for residues of the...

  14. 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

    ... Sciences Group Incorporated, 1150 18th Street NW., Suite 1000, Washington, DC 20036 (on behalf of Natural... tolerance for residues of the insecticide, Paecilomyces fumosoroseus var. Apopka strain 97, in or on all... tolerance for residues of the insecticide, Chromobacterium subtsugae strain PRAA4-1\\T\\, in or on all...

  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.

  16. [Validation study on a multi-residue analysis of pesticides in agricultural products by using phosphoric acid treatment and GC-MS/MS].

    PubMed

    Makabe, Yuhki; Takahashi, Hiroshi; Enomoto, Tomoko; Aikawa, Takehiko

    2014-01-01

    A rapid method for multi-residue determination of pesticides in agricultural products was validated. The sample was cut into pieces and placed into a mixer cup containing half weight amount of 10% phosphoric acid in order to suppress degradation of easily degraded pesticides, represented by captan, and then homogenized. Pesticides in the phosphoric acid-treated sample were extracted with acetonitrile using a homogenizer, followed by salting out with anhydrous magnesium sulfate and sodium chloride. The extract was cleaned up on a C18 and graphite carbon black/PSA mini-cartridge column. Some pesticides gave tailing peaks, but these peaks became sharp and symmetrical when polyethylene glycol (PEG) 300 was added to the test solution. Recovery tests were performed on nine kinds of agricultural products (brown rice, soybean, spinach, cabbage, potato, orange, apple, strawberry, and Japanese pear) fortified with 170 pesticides at 0.01 and 0.1 μg/g. Each concentration of pesticide residue was extracted from 2 samples on 5 separate days. The trueness of the method for 147-164 pesticides in each sample was 70-120% with satisfactory repeatability and within-run reproducibility. This method is expected to useful for multi-residue analysis of pesticides in agricultural products.

  17. 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%.

  18. Monitoring pesticide residues in greenhouse tomato by combining acetonitrile-based extraction with dispersive liquid-liquid microextraction followed by gas-chromatography-mass spectrometry.

    PubMed

    Melo, Armindo; Cunha, Sara C; Mansilha, Catarina; Aguiar, Ana; Pinho, Olívia; Ferreira, Isabel M P L V O

    2012-12-01

    A multiclass and multiresidue method for pesticide analysis in tomato was validated. Extraction and pre-concentration of the pesticide residues from acetonitrile extracts was performed by using dispersive liquid-liquid microextraction (DLLME) technique, followed by gas chromatography-mass detection. DLLME was performed using carbon tetrachloride as extractive solvent and acetonitrile extract as dispersive solvent, in order to increase enrichment factor of the extraction procedure. Validation parameters indicated the suitability of the method for routine analyses of thirty pesticides in a large number of samples. In general, pesticide recoveries ranged between 70% and 110% and repeatability ranged between 1% and 20%. The proposed method was applied to the monitoring of pesticides in tomatoes grown during winter in greenhouses. Among the compounds considered in this work, cyprodinil was found in tomato at concentrations of 0.33mg/kg, other pesticides like azoxystrobin, fenhexanid, tolyfluanid, λ-cyhalothrin and trifloxystrobin were also detected, but, not quantified.

  19. Hierarchical cluster analysis of matrix effects on 110 pesticide residues in 28 tea matrixes.

    PubMed

    Li, Yan; Pang, Guo-Fang; Fan, Chun-Lin; Chen, Xi

    2013-01-01

    Matrix effects on 110 pesticides in 28 tea matrixes of different varieties and origins by LC/MS/MS were studied, and most of the pesticides exhibited soft and medium signal suppression. To better understand the influence of the tea varieties and the physicochemical characteristics of pesticides on the matrix effects, the multivariate analysis tool called hierarchical cluster analysis was applied. Tea matrixes were grouped into three clusters: unfermented, fermented, and post-fermented teas. Any type of tea can be chosen from each cluster as a corresponding representative matrix within that cluster to make matrix-matched solutions, which could simplify analysis while guaranteeing its accuracy. Matrix effects on most pesticides were similar despite the physicochemical diversities of the pesticides.

  20. 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

    ... 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...

  1. 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

    ... tolerances for residues of the herbicide pyroxasulfone and its metabolites in or on wheat (grain, straw....,'' line 24, correct ``wheat, grain at 0.6 ppm'' to read ``wheat, straw at 0.6 ppm.'' List of...

  2. 75 FR 35801 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-06-23

    ... developed to measure the pyraflufen- ] ethyl and its metabolites by aqueous organic solvent extraction... of a tolerance for residues of Acetic acid ethenyl, polymer with oxirane (CAS No. 25820-49-9)...

  3. 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... chromatography/mass spectroscopy/mass spectrometry (HPLC/MS/MS) detection is available for enforcement...

  4. 76 FR 38158 - Withdrawal of Pesticide Petitions for Residues of Pesticide Chemicals in or on Various Commodities

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-06-29

    ...-(-)-lactide-meso-lactide polymer). EPA issued a notice in the Federal Register of October 22, 2010 (75 FR... for residues of D(+)-lactide-L-(-)-lactide- meso-lactide polymer (CAS Reg. No. 9051-89-2) when used...

  5. 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

  6. The status of pesticide residues in the drinking water sources in Meiliangwan Bay, Taihu Lake of China.

    PubMed

    Na, Ta; Fang, Zhou; Zhanqi, Gao; Ming, Zhong; Cheng, Sun

    2006-12-01

    The study was carried out to assess the levels of pesticide residues in the water of Meiliangwan Bay, Taihu Lake of China. The most commonly employed organochlorine pesticides (OCPs), organophosphorus pesticides (OPPs) and herbicide atrazine were analyzed. The water samples were collected seasonally from Meiliangwan Bay within a period of one year. The pesticides were analyzed by gas chromatography (GC) with microECD or NPD after solid-phase extraction (SPE), which was confirmed by GC with an ion trap mass spectrometry (MS). The mean concentrations were 1.98 ng/l for lindane, 0.378 ng/l for heptachlor epoxide, 0.367 ng/l for p,p'-DDE, 0.496 ng/l for p,p'-DDD, 1.06 ng/l for p,p'-DDT and 51.6 ng/l for dichlorvos, 39.0 ng/l for demeton, 346 ng/l for dimethoate, 4.12 ng/l for methyl parathion, 11.6 ng/l for malathion, 2.17 ng/l for parathion and 217 ng/l for atrazine. Generally, low concentrations of OCP were found, whereas the concentrations of the OPPs and atrazine in the water of Taihu Lake were relatively high. Heptachlor epoxide and lindane were the two most commonly encountered OCPs while dichlorvos, demeton and dimethoate were found to have much higher concentrations and occurrences than other OPPs.

  7. Determination of pesticide residues in milk using a QuEChERS-based method developed by response surface methodology.

    PubMed

    Jeong, In-Seek; Kwak, Byung-Man; Ahn, Jang-Hyuk; Jeong, Seung-Hwan

    2012-07-15

    Response surface methodology (RSM) was employed to optimise a rapid and easy sample preparation method for the determination of 14 different pesticide residues in milk. The recovery of each pesticide was investigated by a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe)-based method with respect to 3 variables, the amounts of sodium acetate (Na Acetate), primary secondary amine (PSA), and octadecylsilane (C18). After optimisation, the maximum predicted recovery was the 99.73% rate for myclobutanil under the optimised conditions of 1.70 g Na Acetate, 600.00 mg PSA, and 489.96 mg C18. The recovery rates of the other 9 hydrophilic pesticides were ranged from 82.01% to 98.84%. However, the recovery rates for the 4 lipophilic pesticides (2,4'-DDE, 4,4'-DDE, 2,4'-DDT, and 4,4'-DDT) were <80% because they were removed by C18 along with the other fatty compounds. This method could be implemented in many laboratories to reduce inspection time and cost.

  8. Levels of organochlorine pesticide residues in butter samples collected from the Black Sea Region of Turkey.

    PubMed

    Aksoy, Abdurrahman; Dervisoglu, Muhammed; Guvenc, Dilek; Gul, Osman; Yazici, Fehmi; Atmaca, Enes

    2013-01-01

    The aim of the present study was to evaluate the levels of 9 organochlorine compounds (aldrin, hexachlorobenzene, 2,4-DDE, 4,4-DDE, 2,4-DDT, 4,4-DDT, and α-, β-, and γ-HCH) in butter samples collected in the Eastern, Middle and Western Black Sea Regions of Turkey between October 2009 and June 2010. The liquid-liquid extraction method was used to extract the organochlorine compounds from the samples and the measurements were performed by using a gas chromatograph-electron capture detector system. DDT metabolites, aldrin, hexachlorobenzene (HCB), and α-, and γ-HCH were not detected in the samples but β-HCH was detected in 3 of a total of 88 samples. In the first period, only one sample from the West Black Sea Region was β-HCH positive (0.014 mg kg(-1)). The other β-HCH positive samples collected in Middle and West Black Sea Regions in the second period had a concentration of 0.066 and 0.019 mg kg(-1), respectively. All concentrations of the detected compounds exceeded the legal limits of 0.003 mg kg(-1) for β-HCH, as prescribed by the Turkish Food Codex, and therefore pose a potential health risk for consumers. The contamination detected is most likely due to the past usage of β-HCH in agriculture and its long term persistence in the environment. These results strongly suggest that further research should be focused on the detection of pesticide residues in agricultural areas across the nation.

  9. 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.

  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. [Determination of pesticide residues from seed coating reagent in agricultural products using ultra performance liquid chromatography-tandem mass spectrometry].

    PubMed

    Chen, Yue; Wang, Jinhua; Lu, Xiaoyu; Wang, Wanchun; Huang, Mei; Xu, Chaoyi

    2008-11-01

    An ultra performance liquid chromatography-tandem mass spectrometric method (UPLC-MS/MS) has been developed for the simultaneous determination of eight pesticide residues from seed coating in fruits, vegetable and grain. The sample was extracted by methanol-water (1:1, v/v) and determined by ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry in positive mode (ESI+) and multiple reaction monitoring (MRM) mode. The UPLC analyses were performed on an Acquity UPLC C18 column with gradient eluation. The utility of the method was demonstrated by the analysis of crude extracts, with no sample clean up, from soybean. The linear range was 1 - 200 microg/L. The correlation coefficients (r) were under 0.997. The average recoveries of eight pesticides in samples (from 0.006 to 1.2 mg/kg) ranged from 60% to 110%, and the relative standard deviations (RSDs) were less than 10%. The results indicate that the method is easier, faster, more sensitive, and suitable for the qualitative and quantitative confirmation of pesticide residues from seed coating reagent in fruit, vegetable and grain samples.

  12. 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

    2016-09-07

    Gas chromatography with electron ionization and full scan high resolution mass spectrometry with an Orbitrap mass analyzer (GC-EI-full scan Orbitrap HRMS) was evaluated for residue analysis. Pesticides in fruit and vegetables were taken as an example application. The relevant aspects for GC-MS based residue analysis, including the resolving power (15,000 to 120,000 FWHM at m/z 200), scan rate, dynamic range, selectivity, sensitivity, analyte identification, and utility of existing EI-libraries, are assessed and discussed in detail. The optimum acquisition conditions in full scan mode (m/z 50-500) were a resolving power of 60,000 and an automatic-gain-control target value of 3E6. These conditions provided (i) an optimum mass accuracy: within 2 ppm over a wide concentration range, with/without matrix, enabling the use of ±5 ppm mass extraction windows (ii) adequate scan speed: minimum 12 scans/peak, (iii) an intra-scan dynamic range sufficient to achieve LOD/LOQs ≤0.5 pg in fruit/vegetable matrices (corresponding to ≤0.5 μg kg(-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

  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. 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

  15. 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.

  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. 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

  18. 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.

  19. Comparison of accelerator mass spectrometry with gas chromatography for the determination of pesticide residues in individual items in the diets of wild birds and mammals.

    PubMed

    Brown, Peter; Garner, Colin; Glass, Richard; Ridgway, Chris; Hart, Andy

    2004-06-16

    Methods to refine the assessment of exposure of wild birds and mammals to pesticides required measurement of pesticide residues in very small samples of their diets. Sample sizes were in the 1-100 mg range, and the target residue for measurement was 0.01 mg/kg. Gas chromatography-mass spectrometry (GC-MS) with large volume injection was compared with the use of an accelerator mass spectrometer (AMS) to measure residues of pesticide labeled at near-background levels with carbon-14. The GC-MS method was able to detect residues down to 0.1 ng per item of diet, and the AMS detected the radiolabel down to 1 mBq (0.06 disintegration per minute, 1 ng of pesticide at the specific activity used) per sample. The target residue level was achieved by the GC-MS method for samples down to 10 mg. The GC method appeared to be best suited to monitoring residues in field studies, and the AMS shows great potential for use in laboratory experiments concerning pesticide degradation.

  20. 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

  1. 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....

  2. 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

    ... tolerance for residues of the plant-incorporated protectant, Bacillus thuringiensis eCry3.1Ab protein in... CFR 174.532; March 16, 2011; 76 FR 14289 (FRL-8866- 5) when Bacillus thuringiensis eCry3.1Ab...

  3. 78 FR 3377 - Notice of Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-01-16

    ... ] its metabolites and degradates, in or on rice at 3.0 ppm. There are adequate validated methods that... in rice. There is also successful method validation available for multi-residue DFG method S19 for determination of tricyclazole in rice by GS/MS detection. Contact: Erik Kraft, (703) 308-9358, email...

  4. 76 FR 43231 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-07-20

    ... of food with residues at or above the levels set in these tolerances. The Analytical Chemistry... present therein as a result of the application of methoxyfenozide to growing crops as listed in paragraph... commodities in the table below, when present therein as a result of the application of methoxyfenozide...

  5. 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 ...

  6. Impaired antioxidant gene expression by pesticide residues and its relation with other cellular biomarkers in Nile Tilapia (Oreochromis niloticus) from Lake Burullus.

    PubMed

    El Nahas, Abeer F; Abdel-Razek, Mohamed A S; Helmy, Nashwa M; Mahmoud, Shawky; Ghazy, Haneen A

    2017-03-01

    Organochlorines and Organophosphorus are the most commonly used pesticides. These pesticides constitute a considerable contaminating threat due to their excessive agricultural usage which in turn contaminates the aquatic system through agricultural drainage. The aim of this study was to evaluate water and tissue residues of both pesticides in O. niloticus obtained from three different sections in Lake Burullus, Egypt. Assessment of relative change in mRNA levels of GST and Vtg (oxidative stress indicator) was done and its relation with other cellular biomarkers including apoptosis, which is assessed by Cellular apoptosis susceptibility transcript level (CAS), comet assay and micronucleus assays (genotoxicity indicator). Pesticide residue levels in water are fluctuating. In fish tissues, most residues were higher than those found in water and were associated with down regulation of hepatic GST gene and Vtg expression. CAS gene involved in apoptosis, its transcript is down regulated in middle and western sections of the lake with higher pesticide residues. Different degrees of DNA damages in O. niloticus' liver cells were demonstrated by comet assay. Significant increase in the micronucleated cells in the three sections of the lake was observed; the western section fish showed the highest number. Persistent exposures of fish to pesticide caused impairment of antioxidant gene expression. This negatively affects apoptosis associated with damaging DNA and chromosome fragments.

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

    PubMed

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

    2013-05-01

    It is important to have a reliable method to analyze pesticides in tea, a beverage commonly consumed in Iran. A validated method was developed for the determination of 20 pesticides in tea based on QuEChERS sample preparation and capillary gas chromatography-quadrupole mass spectrometry in selective ion monitoring mode (GC-MS/SIM) using triphenyl methane (TPM) solution as an internal standard. We used fortified, extracted, and cleaned-up tea samples instead of calibration standards for quantitation, which substantially reduced adverse matrix-related effects and negative recovery affected by graphite carbon black (GCB) on pesticide analysis. The recovery of pesticides at 3 concentration (40, 60, and 240 ng/g) ranged from 79.5% to 111.4% (n = 3). The method had acceptable repeatability with RSDr < 20%. The limits of quantification (LOQ) for all pesticides were ≤20 ng/g. The analytical results of the proposed method were in good agreement with proficiency test results (FAPAS, 19116). The recoveries and repeatabilities were in accordance with the criteria set by SANCO Guideline. The validated method was suitable for the analysis of pesticides in tea.

  8. 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.

  9. Pesticide residues in heterogeneous plant populations, a model-based approach applied to nematicides in banana (Musa spp.).

    PubMed

    Tixier, Philippe; Chabrier, Christian; Malézieux, Eric

    2007-03-21

    Nematicides are widely used to control plant-parasitic nematodes in intensive export banana (Musa spp.) cropping systems. Data show that the concentration of fosthiazate in banana fruits varies from zero to 0.035 g kg-1, under the maximal residue limit (MRL=0.05 mg kg-1). The fosthiazate concentration in fruit is described by a Gaussian envelope curve function of the interval between pesticide application and fruit harvest (preharvest interval). The heterogeneity of phenological stages in a banana population increases over time, and thus the preharvest interval of fruits harvested after a pesticide application varies over time. A phenological model was used to simulate the long-term harvest dynamics of banana at field scale. Simulations show that the mean fosthiazate concentration in fruits varies according to nematicide application program, climate (temperature), and planting date of the banana field. This method is used to assess the percentage of harvested bunches that exceed a residue threshold and to help farmers minimize fosthiazate residues in bananas.

  10. Acetonitrile extraction and dual-layer solid phase extraction clean-up for pesticide residue analysis in propolis.

    PubMed

    Oellig, Claudia

    2016-05-06

    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.

  11. Pesticide residues intake of French adults under increased consumption of fresh fruits and vegetables--a theoretical study.

    PubMed

    Barnat, Saida; Boisset, Michel; Casse, Francine; Catteau, Michel; Lecerf, Jean-Michel; Veschambre, Daniel; Periquet, Alain

    2010-02-01

    The increase of fresh vegetable and fruit (FVF) intake could contribute to the prevention of obesity and several major pathologies and thus represents a major public health goal in industrial countries. Nutritional recommendations for increased consumption of FVF could lead to ingestion of unwanted amounts of pesticides. This study was undertaken to evaluate theoretical exposure of French adults to pesticide residues under increasing amounts of FVF intake. Balanced menus with 200 - 400 - 600 - 800 and 1200 g FVF/day were established. Amounts of active substances brought by every FVF vector, at the maximum residue level (MRL) were summed up to determine the intake for each active substance. Values were compared to the Acceptable Daily Intake (ADI) to point out any potential over exposure. A maximalistic approach was adopted and no reducing factor due to processing was taken into account. It was found that under minimal recommended consumption of fruit and vegetables (400 g/d), no active substance reached the ADI, but 18 vs 144 were over 10% of the ADI. Raising FVF to 600 g/d increased the number of active substances over 10 % of the ADI to 24, but again in no case was the ADI exceeded. Doubling the intake to 800 g/d gives values over the ADI for 2 active substances only (cyhexatin and thirame). It was concluded that the increase in fruit and vegetables up to 800 g per day should not expose adults over the ADIs for a majority of authorized pesticides. In this regard, residues levels of ten active substances in fruit and vegetables should deserve particular attention.

  12. Residue levels of organochlorine pesticides in cattle meat and organs slaughtered in selected towns in West Shoa Zone, Ethiopia.

    PubMed

    Letta, Bayessa D; Attah, Louis E

    2013-01-01

    Residue levels of organochlorine pesticides (OCP) in a total of 90 cattle samples comprising meat, liver and kidney collected from carcasses slaughtered in six towns in West Shoa Zone, Ethiopia, (Ambo, Guder, Ginchi, Gedo, Holeta and Tikur Inchini), have been determined. The pesticides were extracted by solid phase extraction (SPE) and quantification was carried out using gas chromatography-mass spectrometry (GC-MS). A good linearity (r(2) > 0.998) was found in the range 0.001-7.00 mg/kg for the samples studied. Most of the pesticides had recoveries in the range 81-99% and values of relative standard deviation (RSD) <7.2% for repeatability and reproducibility, showing good accuracy and precision of the method. The concentration level of the studied organochlorines followed the order: p, p' dichloro-diphenyl-trichloroethane (DDT) > endosulfan>o,p'-DDT >lindane>dieldrin>endrin>aldrin>chlorothanolin while the order of contamination in the analyzed organs was liver > kidney > meat. Heat treatment of the meat, kidney and liver samples (boiling for 90 min.) produced an overall reduction of 62.2%, 44.5%, 37.7%, 29%, 31%, 34.3% and 30.8% in lindane, o, p'-DDT, endosulfan, p, p'-DDT, chlorothanolin, aldrin, dieldrin, and endrin, respectively. Although the residual contents of the organochlorines detected in all the contaminated samples analyzed from the six cities were below the respective maximal permissible levels set by international organizations, samples from Holeta town were more contaminated and may necessitate effective monitoring as bioaccumulation of these residues may pose health problems in human beings.

  13. High-throughput analytical techniques for determination of residues of 653 multiclass pesticides and chemical pollutants in tea, Part II: comparative study of extraction efficiencies of three sample preparation techniques.

    PubMed

    Fan, Chun-Lin; Chang, Qiao-Ying; Pang, Guo-Fang; Li, Zeng-Yin; Kang, Jian; Pan, Guo-Qing; Zheng, Shu-Zhan; Wang, Wen-Wen; Yao, Cui-Cui; Ji, Xin-Xin

    2013-01-01

    aged tea samples was recovered with Method 1, more than 10% higher than with Method 2 (30-50% higher on average). For green tea, 193 (GC/MS/MS) and 197 (GC/MS) pesticides and chemical pollutants accounted for 96.5% (GC/MS/MS) and 98.0% (GC/MS) with Method 1 higher than with Method 2. For woolong tea, 191 (GC/MS/MS) and 194 (GC/MS) pesticides and chemical pollutants accounted for 95% (GC/MS/MS) and 96% (GC/MS/MS) with Method 1, higher than with Method 2, respectively. In other words, there were definite differences in the test results for aged tea samples between Method 1 and Method 2, which suggests that Method 1 was capable of extracting more residual pesticides and chemical pollutants from the precipitated 165-day-aged tea samples. The reason can be traced to the possibility that Method 1 (high-speed homogenizing) has better extraction efficiency than Method 2 (vortex and oscillation). Therefore, Method 1 was chosen as the sample preparation technique for multiresidue pesticide and chemical pollutant analysis in tea.

  14. 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.

  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.

  16. 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

  17. Benefits and pitfalls of the application of screening methods for the analysis of pesticide residues in fruits and vegetables.

    PubMed

    Malato, Octavio; Lozano, Ana; Mezcua, Milagros; Agüera, Ana; Fernandez-Alba, Amadeo R

    2011-10-21

    The goal of this study was to expand knowledge on the performance of screening methods based on accurate mass measurements using a liquid chromatography electrospray quadrupole time-of-flight mass spectrometry (LC-ESI-QTOF-MS) system operating in full scan mode and with automatic identification based on the use accurate-mass databases. The study involved the analysis of 97 pesticides, in five matrices (tomato, pepper, zucchini, orange and leek) and at three concentration levels (20, 50 and 100 μg kg(-1)). Aspects concerning optimization of the search parameters, sensitivity, matrix effects, efficiency of the algorithm search, usefulness of fragment ions, etc., are evaluated in deep. Sensitivity requirements have been identified as the main obstacle affecting the automatic identification of pesticides, especially in complex matrices, where the ionization suppression reduces the detectability of analytes. In addition, we have detected some failures in the software used for automatic data processing in terms of analysis of isobaric compounds, use of isotopic clusters, spectral deconvolution and data processing speed that hamper the correct identification in some pesticide/matrix combinations. These drawbacks should be improved in the future for its effective implementation in routine residue analysis.

  18. [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.

  19. Organophosphate Pesticide Residues in Drinking Water from Artesian Wells and Health Risk Assessment of Agricultural Communities, Thailand.

    PubMed

    Jaipieam, S; Visuthismajarn, P; Sutheravut, P; Siriwong, W; Thoumsang, S; Borjan, M; Robson, M

    2009-01-01

    Organophosphate pesticide (OPPs) concentrations in artesian wells located in Thai agricultural and non-agricultural communities were studied during both wet and dry seasons. A total of 100 water samples were collected and subjects were asked to complete a survey. Gas chromatography flame photometric detector was used for OPP analysis. The average OPP concentration in the agricultural communities (0.085 and 0.418 microg/l in dry and wet season) was higher than in the non-agricultural communities (0.004 microg/l in both seasons). Ingestion of OPPs in contaminated water in the agricultural communities were estimated to be 0.187 and 0.919 microg/day during the dry and wet seasons, respectively, and 0.008 microg/day during both seasons in the non-agricultural communities. Agricultural communities were exposed to pesticide residues under the oral chronic reference dose. This study suggests that people in agricultural communities may be exposed to significantly greater levels of pesticides than non-agricultural populations during the dry and wet seasons (p < .001, .001).

  20. 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.

  1. Contamination of liquid milk and butter with pesticide residues in the Ludhiana district of Punjab state, India.

    PubMed

    Battu, R S; Singh, Balwinder; Kang, B K

    2004-11-01

    An analysis of 92 samples of liquid milk from Ludhiana, India, during 1999-2001 revealed the presence of DDT in 6 (7.4%) samples and of these 2 samples were found to exceed the maximum residue limit (MRL) of DDT fixed at 0.05 mg kg(-1) (on a whole milk basis). HCH residues were detected in 49 (53.3%) samples and constituted only gamma-HCH (lindane). The MRL of lindane is fixed at 0.01 mg kg(-1) (whole milk basis), and all 49 liquid milk samples exceeded this value. These results are indicative of contamination of bovine milk with pesticide residues as a result of the ban on the use of DDT and HCH in agriculture and public health programs. Similarly, analysis of 40 samples of butter showed the presence of DDT and HCH in 28 and 8 samples, respectively. However, none of the samples exceeded the MRL value of either DDT or any isomer of HCH. DDT residues comprised mainly p,p-DDE and p,p-TDE, whereas HCH residues were present as lindane in 6 samples, and 2 samples revealed the presence of beta-HCH. The estimated daily intake of lindane through the consumption of contaminated liquid milk exceeded its acceptable daily intake value for children. Interestingly, none of the liquid milk or butter samples revealed the presence of any commonly used organophosphorus or synthetic pyrethroid insecticides at their detection limit of 0.01 mg kg(-1).

  2. 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

  3. Using Three-Dimensional Fluorescence Spectrum Technology to Analyze the Effects of Natural Dissolved Organic Matter on the Pesticide Residues in the Soil.

    PubMed

    Lei, Hong-jun; Han, Yu-ping; Liu, Xin; Xu, Jian-xin

    2015-07-01

    The behavior of pesticide in soil is influenced by dissolved organic matter (DOM) through competition adsorption, adsorption, solubilization, accelerated degradation, and so on. Thus DOM and its components play an important role in the environmental risk in the soil ecosystem and groundwater environment. Currently, most studies focused on the short-term effect of high concentration of DOM on the pesticide residues. However, soil DOM is mainly at low level. Therefore, there is of some practical significance to probe into the environmental behavior of soil pesticides under natural level of DOM. Thus a site investigation was conducted in the farmland with long-term application history of pesticide. By using the three dimensional excitation-emission fluorescence matrix (3D-EEM) technology, together with the fluorescence regional integration (FRI) quantitative method, the long-term effects of pesticide residues under low concentration of natural DOM were analyzed. Results showed that: (1) The long-term effects of the natural DOM components on the environment behavior of most soil organochlorine pesticides were not significant except for a few pesticides such as y-HCH, p, p'-DDE, etc. (2) The influencing effects of DOM components on different type of pesticides were varied. Among which, the content of tyrosine component showed a significantly negative correlation (p < 0.05) with the concentration of y-HCH and p, p'-DDE. There were significant positive correlations (p < 0.05) between the byproducts of microbial degradation in DOM components and the concentration of heptachlor. There were also a significant positive correlation (p < 0.05) between the content of active humus component of humic acid in the DOM and the concentration of heptachlor epoxide. These results suggested that the distribution of different types of pesticides residue in the soil was influenced by different components at different levels of significance. (3) The humification degree of soil organic

  4. Pesticide and PCB residues in the upper Snake River ecosystem, Southeastern Idaho, following the collapse of the Teton dam 1976.

    PubMed

    Perry, J A

    1979-01-01

    The Teton Dam in Southeastern Idaho collapsed on June 5, 1976. The resulting flood damaged a large area and caused the release of toxicants into the Snake River. A pesticide recovery team in a helicopter worked the flooded area for three weeks and collected 1,104 containers, about 35% of which contained toxicants. It was estimated that less than 60% of the lost pesticide containers were recovered. This paper addresses the results of a one-time sampling effort designed to determine the magnitude of the chemical contamination. Over 300 samples of fish, plankton, waterfowl, sediments, water, stream drift, aquatic plants, and soil were taken. Pesticide residues were measured as microgram/kg (ppb) wet weight, whole animal basis. Rainbow trout had as much as 1432 micrograms/kg total DDT plus analogs, 66 micrograms/kg dieldrin, and 1010 micrograms/kg PCBs. Utah suckers had up to 1420 micrograms/kg total DDT plus analogs, 32 micrograms/kg dieldrin, and 1800 micrograms/kg PCB. Rocky Mountain whitefish had as much as 2650 micrograms/kg total DDT and analogs, 30 micrograms/kg dieldrin and 1400 micrograms/kg PCBs. These PCB and DDT levels were high, approaching the 2,000 micrograms/kg FDA proposed tolerance, but were below the 5,000 micrograms/kg present tolerance. Dieldrin levels were low and organophosphates were undetectable. An undeveloped area (the Fort Hall Bottoms) showed higher levels of contaminants than did an industrialized area (the lower Portneuf River). This apparent discrepancy remains unexplained. Very little pre-flood data on a whole fish basis were available for comparison (Johnson et al 1977). However, it does not appear that any human health hazard due to pesticide levels exists in this portion of the Snake River.

  5. 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.

  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. Integrated Pest Management Practices Reduce Insecticide Applications, Preserve Beneficial Insects, and Decrease Pesticide Residues in Flue-Cured Tobacco Production.

    PubMed

    Slone, Jeremy D; Burrack, Hannah J

    2016-09-22

    Integrated pest management (IPM) recommendations, including scouting and economic thresholds (ETs), are available for North Carolina flue-cured tobacco growers, although ETs for key pests have not been updated in several decades. Moreover, reported IPM adoption rates by flue-cured tobacco growers remain low, at < 40%, according to NC cooperative extension surveys conducted during the last four years. Previous research has suggested that timing insecticide treatments using currently available ETs can reduce the average number of applications to two or fewer per season. We conducted field-scale trials at nine commercial tobacco farms, three in 2104 and six in 2015, to quantify inputs associated with current scouting recommendations, to determine if current ETs were able to reduce insecticide applications as compared to grower standard practices, and to assess the impacts of reduced insecticide applications on end of season yield and pesticide residues. Two fields were identified at each farm and were scouted weekly for insects. One field was only treated with insecticides if pests reached ET (IPM), while the other field was managed per grower discretion (Grower Standard). IPM fields received an average of two fewer insecticide applications without compromising yield. More insecticide applications resulted in higher pesticide residues in cured leaf samples from Grower Standard fields than those from IPM fields. Reductions in insecticides and management intensity also resulted in larger beneficial insect populations in IPM fields.

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

    PubMed

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

    2013-01-01

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

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

    PubMed

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

    2014-07-01

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

  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.

  11. 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.

  12. High-Throughput Analytical Techniques for the Determination of the Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea, Part VII: A GC-MS, GC-MS/MS, and LC-MS/MS Study of the Degradation Profiles of Pesticide Residues in Green Tea.

    PubMed

    Chang, Qiao-Ying; Pang, Guo-Fang; Fan, Chun-Lin; Chen, Hui; Yang, Fang; Li, Jie; Wen, Bi-Fang

    2016-11-01

    GC-MS, GC-tandem MS (MS/MS), and LC-MS/MS were used to mathematically define the degradation profiles of pesticide residues in two field trials. Nineteen pesticides were studied in the first field trial and 11 in the second. The results of the field trials demonstrated that the degradation profiles of pesticide residues in green tea can be described with power functions to successfully estimate the amount of time, following pesticide application, pesticide residues appearing in tea in concentrations at and/or above the maximum residue limit (MRL) decrease to concentrations below the MRL. Stability tests on green tea samples stored at room temperature were conducted to determine whether pesticide-incurred green tea samples prepared according to the method used in the field trials would be suitable for the preparation of reference standards for laboratory-proficiency testing trials. This paper reports the results of a GC-MS, GC-MS/MS, and LC-MS/MS study, as well as the suitability of the samples prepared under these conditions for use as pesticide reference standards in tea analysis.

  13. 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

    ..., which means EPA will not know your identity or contact information unless you provide it in the body of... include your name and other contact information in the body of your comment and with any disk or CD-ROM... environmental effects from exposure to the pesticides discussed in this document, compared to the...

  14. 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...

  15. 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...

  16. Agricultural pesticide residues of farm runoff in the Okanagan Valley, British Columbia, Canada.

    PubMed

    Kuo, Jen-ni; Soon, Alicia Y; Garrett, Christine; Wan, Michael T K; Pasternak, John P

    2012-01-01

    The objectives of this study were to determine environmental occurrence and concentrations of selected currently-used-pesticides and some transformation products in agricultural farms in the Okanagan Valley (OKV), and to conduct a simple risk assessment of environmental pesticides levels detected in OKV on non-target aquatic organisms. The OKV is the tree fruit country of the Province of British Columbia where considerable amount of pesticides are applied annually. Water, sediment and soil samples were collected at eleven sites in early June and late September following rainfall events and/or extended periods of irrigation from drainage ditches and/or from small streams. Undisturbed reference sites were also sampled. Study results showed that forty of the eighty chemicals analyzed, including organochlorine, nitrogen-containing and organophosphate pesticides commonly used for OKV crops, were detected in runoff and small stream water samples. Among which, endosulfan-sulfate was the most frequently detected chemical. Also, azinophos-methyl (0.699-25.5 ng/L), diazinon (0.088-214 ng/L) exceeded, and α-, β- endosulfan, endosulfan sulphate approached the guidelines for the protection of aquatic life.

  17. 40 CFR 158.2130 - Microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ....2400 Storage Stability CR EP 1 885.2500 Magnitude of residue in plants CR EP 1 885.2550 Magnitude of residues in meat, milk, poultry, eggs CR EP 1 885.2600 Magnitude of residues in potable water, fish,...

  18. 40 CFR 158.2172 - Experimental use permit microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 885.2350 Analytical methods-animals CR TGAI 1 885.2400 Storage Stability CR EP 1 885.2500 Magnitude of residue in plants CR EP 1 885.2550 Magnitude of residues in meat, milk, poultry, eggs CR EP 1 885.2600 Magnitude of residues in potable water, fish, and irrigated crops CR EP 1 (d) Test notes. The following...

  19. 40 CFR 158.2172 - Experimental use permit microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 885.2350 Analytical methods-animals CR TGAI 1 885.2400 Storage Stability CR EP 1 885.2500 Magnitude of residue in plants CR EP 1 885.2550 Magnitude of residues in meat, milk, poultry, eggs CR EP 1 885.2600 Magnitude of residues in potable water, fish, and irrigated crops CR EP 1 (d) Test notes. The following...

  20. 40 CFR 158.2130 - Microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ....2400 Storage Stability CR EP 1 885.2500 Magnitude of residue in plants CR EP 1 885.2550 Magnitude of residues in meat, milk, poultry, eggs CR EP 1 885.2600 Magnitude of residues in potable water, fish,...

  1. 40 CFR 158.2130 - Microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ....2400 Storage Stability CR EP 1 885.2500 Magnitude of residue in plants CR EP 1 885.2550 Magnitude of residues in meat, milk, poultry, eggs CR EP 1 885.2600 Magnitude of residues in potable water, fish,...

  2. 40 CFR 158.2172 - Experimental use permit microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 885.2350 Analytical methods-animals CR TGAI 1 885.2400 Storage Stability CR EP 1 885.2500 Magnitude of residue in plants CR EP 1 885.2550 Magnitude of residues in meat, milk, poultry, eggs CR EP 1 885.2600 Magnitude of residues in potable water, fish, and irrigated crops CR EP 1 (d) Test notes. The following...

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

    PubMed

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

    2014-01-01

    The integrated pest management (IPM) modules of pesticide schedule on Basmati rice were validated at field experiments conducted in Northern India for consecutive 3 years (2005-2008). The pesticide residues were found below the detectable limit (<0.01-0.001 mg/kg) in soil and irrigation water samples of Kaithal region. In Dehra Dun region of Uttrakhand, the residues of carbendazim in rice grains and soil were detected below <0.01 mg/kg level. In second year experiments (2006-2007), only four non-IPM soil samples indicated the presence of chlorpyrifos and endosulfan in the range of ND <0.001 to 0.07 mg/kg, out of 45 samples analyzed. Carbendazim applied as seed treatment at Dehradun and Kaithal field trials was found below detectable limit in both IPM and non-IPM rice grains (<0.01 mg/kg) and irrigation water (0.01 μl/ml). Chlorpyrifos was detected in five water samples from Kaithal and one from Pant Nagar in the range of 0.003-0.006 μl/L, α- and β-isomer of endosulfan in the range of 0.005-0.03, and 0.005-0.02 μl/ml, respectively, in one sample from Pant Nagar and two from Kaithal, out of a total of 22 samples. In the region of Uttrakhand and Uttar Pradesh during 2007-2008, four non-IPM samples of soil indicated trace levels of endosulfan, out of 16 samples analyzed. The residues were detected below detection limit for carbendazim (<0.01 mg/kg) in soil samples of Dehradun IPM fields and for endosulfan and carbendazim (0.001-0.01 μl/L) in water samples each from IPM and non-IPM fields of Uttar Pradesh. The results of 3-year trials of IPM module indicated basmati rice as safe and economical with pesticide residue-free rice grains.

  4. 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

  5. Modelling of the long term fate of pesticide residues in agricultural soils and their surface exchange with the atmosphere: Part I. Model description and evaluation.

    PubMed

    Scholtz, M T; Bidleman, T F

    2006-09-15

    Sources of pesticides in the atmosphere can be releases of new material through current use, or emission/reemission from soil residues resulting from historical use. It is the latter aspect, soil residues, that is the focus of this study. This paper describes the application of a simple coupled atmosphere-soil pesticide exchange model that can assist in the interpretation of soil residue and air concentration measurements, and in the projection of short period field measurements to larger spatial scales and longer time periods. Only dry gaseous exchange (emission and deposition) between bare agricultural lands and the atmosphere is modelled. Wet deposition and particle associated deposition of pesticide are not included. Model results are compared with published co-located air and soil pesticide concentration measurements made on agricultural lands in the southern U.S. that have soil residues of lindane and the following six highly persistent pesticides: cis-, trans-chlordane, p,p'-DDE, dieldrin, trans-nonachlor and toxaphene. The study results show: (i) that measured air concentrations of toxaphene and p,p'-DDE above agricultural soils in the southern U.S. can be attributed to emissions due to local soil residues of these pesticides rather than to the regional background air concentrations; (ii) that both soil emissions and background air concentrations of dieldrin contribute significantly to the measured air concentrations; (iii) that measured air concentrations of cis- and trans-chlordane as well as trans-nonachlor and lindane are mainly due to the regional background with little contribution from local soil residues. An analysis of modelled summer day and night average soil-air exchange fluxes shows that toxaphene and p,p'-DDE soil residues are strong sources of emission to the atmosphere during both the day and night while the chlordanes, trans-nonachlor, lindane and dieldrin are deposited from the atmosphere to the soil during the night hours and emitted to

  6. 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.

  7. 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.

  8. Electrochemical biosensors for rapid determination of pesticide residues in agricultural products

    NASA Astrophysics Data System (ADS)

    Jiang, Xuesong; Wang, Jianping; Ying, Yibin; Ye, Zunzhong; Li, Yanbin

    2005-11-01

    The biosensors, consisting of immobilized antibodies which were for specific recognition to target molecules and electrodes which were able to convert the binding event between antigen and antibody to a detectable signal, were developed for rapid detection of organophosphate (OPs) pesticides. Anti-OPs antibodies were immobilized onto indium-tin-oxide (ITO) coated interdigitated microsensor electrodes (IMEs). The Faradaic impedance spectra, presented as Nyquist plots (Z' vs Z'') and Bode diagrams, (impedance vs frequency) were recorded in the frequency range from 1Hz to 100 kHz respectively. A linear relationship between the electron-transfer resistance and concentrations of OPs pesticide was found ranging from 0.1 ppm to 100 ppm. The regression equations were Y = 658 X +1861, with the correlation coefficient of 0.977. The biosensing procedure was simple and rapid, and could be completed within 1 h.

  9. 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.

  10. Employing Solid Phase Microextraction as Extraction Tool for Pesticide Residues in Traditional Medicinal Plants

    PubMed Central

    Gondo, Thamani T.; Mmualefe, Lesego C.; Okatch, Harriet

    2016-01-01

    HS-SPME was optimised using blank plant sample for analysis of organochlorine pesticides (OCPs) of varying polarities in selected medicinal plants obtained from northern part of Botswana, where OCPs such as DDT and endosulfan have been historically applied to control disease carrying vectors (mosquitos and tsetse fly). The optimised SPME parameters were used to isolate analytes from root samples of five medicinal plants obtained from Maun and Kasane, Botswana. The final analytes determination was done with a gas chromatograph equipped with GC-ECD and analyte was confirmed using electron ionisation mass spectrometer (GC-MS). Dieldrin was the only pesticide detected and confirmed with MS in the Terminalia sericea sample obtained from Kasane. The method was validated and the analyte recoveries ranged from 69.58 ± 7.20 to 113 ± 15.44%, with RSDs ranging from 1.19 to 17.97%. The method indicated good linearity (R2 > 0.9900) in the range of 2 to 100 ng g−1. The method also proved to be sensitive with low limits of detection (LODs) ranging from 0.48 ± 0.16 to 1.50 ± 0.50 ng g−1. It can be concluded that SPME was successfully utilized as a sampling and extraction tool for pesticides of diverse polarities in root samples of medicinal plants. PMID:27725893

  11. 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.

  12. [A Simultaneous Determination Method with Acetonitrile-n-Hexane Partitioning and Solid-Phase Extraction for Pesticide Residues in Livestock and Marine Products by GC-MS].

    PubMed

    Yoshizaki, Mayuko; Kobayashi, Yukari; Shimizu, Masanori; Maruyama, Kouichi

    2015-01-01

    A simultaneous determination method was examined for 312 pesticides (including isomers) in muscle of livestock and marine products by GC-MS. The pesticide residues extracted from samples with acetone and n-hexane were purified by acetonitrile-n-hexane partitioning, and C18 and SAX/PSA solid-phase extraction without using GPC. Matrix components such as cholesterol were effectively removed. In recovery tests performed by this method using pork, beef, chicken and shrimp, 237-257 pesticides showed recoveries within the range of 70-120% in each sample. Validity was confirmed for 214 of the target pesticides by means of a validation test using pork. In comparison with the Japanese official method using GPC, the treatment time of samples and the quantity of solvent were reduced substantially.

  13. Determination of pesticide residues in globe artichoke leaves and fruits by GC-MS and LC-MS/MS using the same QuEChERS procedure.

    PubMed

    Machado, Ignacio; Gérez, Natalia; Pistón, Mariela; Heinzen, Horacio; Cesio, María Verónica

    2017-07-15

    Aiming to select the most suitable sample preparation for the multiresidue analysis of pesticides in globe artichoke (Cynara cardunculus L.), a modified QuEChERS, a matrix solid phase dispersion and a dispersive ethyl acetate extraction were compared. Trueness and precision were determined at 0.2mgkg(-1) for the three methods. The modified QuEChERS showed the best performance. The scope of the method was enlarged to 35 GC and 63 LC amenable pesticides, its overall performance was evaluated and validated to artichoke leaves and fruits according to DG-SANTE Guidelines. Different matrix effects were observed for most of the pesticides which were higher for leaves than fruits. Difenoconazole and flutriafol suffered signal suppression in leaves extracts but showed positive matrix effects in fruits. All pesticides were analyzed at or below their Maximum Residue Levels fixed for globe artichoke by the European Union. The method was successfully applied for the analysis of commercial samples.

  14. [Determination of organochlorine pesticide residues in nine herbs by solid-phase extraction and capillary gas chromatography].

    PubMed

    Yan, Zheng; Feng, Di; Li, Shenjie; Zhao, Yakui; Yang, Hui

    2005-05-01

    The solid-phase extraction and capillary gas chromatography was introduced for determining 13 organochlorine pesticide residues including alpha-benzene hexachloride (BHC), betaBHC, gamma-BHC, delta-BHC, p,p'-dichloro-diphenyl-dichloroethylene (pp'-DDE), p,p'-dichloro-di-phenyl-dichloroethane (pp'-DDD), o,p'-dichloro-diphenyl-trichloroethane (op'-DDT), pp'-DDT, heptachlor (HEPT), aldrin, heptachlor epoxide (HCE), dieldrin and endrin in Scutellaria baicalensis, Salvia miltiorrhiza, Belamcanda chinensis, Paeoniae lactiflora, Angelica dahurica, Arisaema erubescens, Fructus arctii, Anemarrhena asphodeloides and Platycodon grandiflorum. The organochlorine pesticides were extracted from herbs with mixed solvents of acetone and n-hexane by ultrasonic and cleaned up by Florisil solid-phase extraction column. Then, the extract was separated by capillary column (30 m x 0.25 mm i.d. x 0.25 microm) and detected by electrochemical detector. The carrier gas was N2 (99.999%) with the flow rate of 1.4 mL/min. The split ratio was 1:2.2. The injector temperature was 220 degrees C and the detector temperature was 330 degrees C. The column temperature was increased by the rate of 20 degrees C/min from 100 degrees C to 190 degrees C (hold for 1. 0 min), then to 235 degrees C by the rate of 4 degrees C/min and hold for 7 min at 235 degrees C. The good linearities were obtained for 13 organochlorine pesticides. The detection limits were between 0.064-0.61 microg/L. The average recoveries were between 87.3%-102.3% and relative standard deviations of 1.3%-6.8%. The method is effective, fast and accurate.

  15. Concentration and bioaccumulation of organochlorine pesticide residues in herons and their prey in wetlands of Thermaikos Gulf, Macedonia, Greece.

    PubMed

    Albanis, T A; Hela, D; Papakostas, G; Goutner, V

    1996-04-05

    Concentrations of the principal organochlorine insecticides were determined in eggs and freshly dead chicks of the Squacco heron (Ardeola ralloides), Little Egret (Egretta garzetta) and Night Heron (Nycticorax nycticorax), as well as in frogs (Rana sp.), the main heron prey. Material was collected from the wetlands of the Thermaikos Gulf (Macedonia, northern Greece) in 1992 and 1993. Residues of the organochlorine pesticides alpha-BHC, beta-BHC, lindane, 4,4'-DDD, 4,4'-DDE, heptachlor and dieldrin were found in the eggs, chicks and prey of the herons. alpha-BHC, beta-BHC, and lindane had highest concentration in the Night Heron and lowest in the Little Egret. In all samples examined, the bioconcentration factors (BCF) of these compounds had very high values. BCF of pollutants for the eggs of the Squacco Heron were at lower levels than those of its chicks. BCF for frogs were in almost all cases lower than those for the other samples. Biomagnification factor (BMF) for 4,4'-DDE and beta-BHC had the highest values of all other compounds (except in the Night Heron). BMF for the eggs of the Squacco Heron were greater than for its chicks. Variation in the pesticide contents in the different heron species is attributed to different feeding habits; the exception being the occurrence of dieldrin in eggs only and 4,4'-DDE as a remnant of past spraying. Amounts of pesticides detected in this study are too low to affect eggshell thickness in the Squacco Heron or have other effects on the wildlife of the area.

  16. 40 CFR 158.2130 - Microbial pesticides residue data requirements table.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... EP 1 885.2200 Nature of the Residue in plants CR EP 1 885.2250 Nature of the Residue in animals CR EP 1 885.2300 Analytical methods - plants CR TGAI 1 885.2350 Analytical methods - animals CR TGAI 1 885... this section. 1. Required when the results of testing: i. Indicate the potential to cause adverse...

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

    PubMed

    Henry, L; Kishimba, M A

    2006-03-01

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

  18. Construction of genetically engineered bacteria that degrades organophosphorus pesticide residues and can be easily detected by the fluorescence.

    PubMed

    Li, Qin; Wang, Pan; Chen, Rui; Li, Wei; Wu, Yi-Jun

    2014-01-01

    Organophosphorus compounds (OPs) are widely used in agriculture and industry and there is increased concern about their toxicological effects in the environment. Bioremediation can offer an efficient and cost-effective option for the removal of OPs. Herein, we describe the construction of a genetically engineered microorganism (GEM) that can degrade OPs and be directly detected and monitored in the environment using an enhanced green fluorescent protein (EGFP) fusion strategy. The coding regions of EGFP, a reporter protein that can fluoresce by itself, and organophosphorus hydrolase (OPH), which has a broad substrate specificity and is able to hydrolyse a number of organophosphorus pesticides, were cloned into the expression vector pET-28b. The fusion protein of EGFP-OPH was expressed in E. coli BL21 (DE3) and the protein expression reached the highest level at 11 h after isopropyl beta-D-thiogalactopyranoside induction. The fluorescence of the GEM was detected by fluorescence spectrophotometry and microscopy, and its ability to degrade OPs was determined by OPH activity assay. Those GEM that express the fusion protein (EGFP and OPH) exhibited strong fluorescence intensity and also potent hydrolase activity, which could be used to degrade organophosphorus pesticide residues in the environment and can also be directly monitored by fluorescence.

  19. Heavy metal, organochlorine pesticide, and PCB residues in eggs and feathers of herons breeding in northern Italy.

    PubMed

    Fasola, M; Movalli, P A; Gandini, C

    1998-01-01

    We report on organochlorine pesticide and PCB concentrations in eggs of the little egret, Egretta garzetta, and the black-crowned night-heron, Nycticorax nycticorax, collected in 1993-1994, and on mercury, cadmium, and lead concentrations in feathers of 20-day-old nestlings collected from the same nests in 1994, from heronries near Pavia, northern Italy. Organochlorine pesticide and PCB residues were lower than those commonly associated with mortality and reduced reproductive success. As population levels of the species studied are not declining, these contaminants appear to have no significant adverse effect on reproduction in the heronries studied. DDE levels have decreased markedly in heron eggs since 1978. However, the presence of both DDT and beta-HCH, albeit at low levels, is notable, given that these compounds were banned in Italy in 1978 and 1988, respectively. Relatively high levels of Hg, Cd, and Pb in feathers suggest birds in their colonies are exposed to these contaminants, although both Cd and Pb may relate more to external than to internal contamination.

  20. 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.

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

    PubMed

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

    2014-12-15

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

  2. 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...

  3. 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...

  4. 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.

  5. The impact of seasonal variation on organochlorine pesticide residues in buffalo and cow milk of selected dairy farms from Faisalabad region.

    PubMed

    Sajid, Muhammad Wasim; Shamoon, Muhammad; Randhawa, Muhammad Atif; Asim, Muhammad; Chaudhry, Abdul Shakoor

    2016-10-01

    Two hundred milk samples from 20 randomly selected dairy farms were screened for the incidence of organochlorine pesticide residues to evaluate the safety of milk in Faisalabad region. The results revealed that overall buffalo milk samples in winter (85 %) and in summer (78 %) were more contaminated as compared to cow milk samples 83 and 75 % in respective seasons. The residues of cyhalothrin were found only in summer season in milk of both species. Permethrin residues were detected at higher levels than perfinofos while DDT and methamedophos were found undetectable. The mean levels of permethrin were 0.042 and 0.033 mg kg(-1)in buffalo milk samples and 0.045 and 0.043 mg kg(-1) in cow milk in winter and summer season, respectively. Perfinofos residues were found to be the least contaminated pesticides with mean values of 0.0006 and 0.0013 mg kg(-1), respectively in winter season, and 0.004 and 0.0025 mg kg(-1) in summer season. All analysed pesticide residues in milk samples in both seasons were below the maximum residual limit (MRL) values as described by European Union (EU) but milk samples contaminated with α, β-endosulfan and endosulphate exceeded their respective Food and Agriculture Organization's (FAO) established MRLs both in winter and summer.

  6. 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.

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

    PubMed

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

    2007-04-01

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

  8. Comparative estrogenic activity of wine extracts and organochlorine pesticide residues in food.

    PubMed

    Gaido, K; Dohme, L; Wang, F; Chen, I; Blankvoort, B; Ramamoorthy, K; Safe, S

    1998-12-01

    The human diet contains industrial-derived, endocrine-active chemicals and higher levels of naturally occurring compounds that modulate multiple endocrine pathways. Hazard and risk assessment of these mixtures is complicated by noadditive interactions between different endocrine-mediated responses. This study focused on estrogenic chemicals in the diet and compared the relative potencies or estrogen equivalents (EQs) of the daily consumption of xenoestrogenic organochlorine pesticides in food (2.44 micrograms/day) with the EQs in a single 200-ml glass of red cabernet wine. The reconstituted organochlorine mixture contained 1,1,1-trichloro-2-(p-chlorophenyl)-2-(o-chlorophenyl)ethane, 1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane, 1,1-dichloro-2,2-bis(p-chlorophenyl)ethylene, endosulfan-1, endosulfan-2, p,p'-methoxychlor, and toxaphene; the relative proportion of each chemical in the mixture resembled the composition reported in a recent U.S. Food and Drug Administration market basket survey. The following battery of in vitro 17 beta-estradiol (E2)-responsive bioassays were utilized in this study: competitive binding to mouse uterine estrogen receptor (ER); proliferation in T47D human breast cancer cells; luciferase (Luc) induction in human HepG2 cells transiently cotransfected with C3-Luc and the human ER, rat ER-alpha, or rat ER-beta; induction of chloramphenicol acetyltransferase (CAT) activity in MCF-7 human breast cancer cells transfected with E2-responsive cathepsin D-CAT or creatine kinase B-CAT plasmids. For these seven in vitro assays, the calculated EQs in extracts from 200 ml of red cabernet wine varied from 0.15 to 3.68 micrograms/day. In contrast, EQs for consumption of organochlorine pesticides (2.44 micrograms/day) varied from nondetectable to 1.24 ng/day. Based on results of the in vitro bioassays, organochlorine pesticides in food contribute minimally to dietary EQ intake.

  9. Analysis of pesticide residues by fast gas chromatography in combination with negative chemical ionization mass spectrometry.

    PubMed

    Húsková, Renáta; Matisová, Eva; Hrouzková, Svetlana; Svorc, Lubomír

    2009-08-28

    A combination of fast GC with narrow-bore column and bench top quadrupole mass spectrometer (MS) detector in negative chemical ionization (NCI) mode (with methane as reagent gas) is set up and utilized for the ultratrace analysis of 25 selected pesticides. The observed pesticides, belonging to the endocrine disrupting chemicals (EDCs), were from different chemical classes. A comparative study with electron impact (EI) ionization was also carried out (both techniques in selected ion monitoring (SIM) mode). The programmed temperature vaporizer (PTV) injector in solvent vent mode and narrow-bore column (15mx0.15mm I.D.x0.15microm film of 5% diphenyl 95% dimethylsiloxane stationary phase) were used for effective and fast separation. Heptachlor (HPT) as internal standard (I.S.) was applied for the comparison of results obtained from absolute and normalized peak areas. Non-fatty food matrices were investigated. Fruit (apple - matrix-matched standards; orange, strawberry, plum - real samples) and vegetable (lettuce - real sample) extracts were prepared by a quick and effective QuEChERS sample preparation technique. Very good results were obtained for the characterization of fast GC-NCI-MS method analysing EDCs pesticides. Analyte response was linear from 0.01 to 150microgkg(-1) with the R(2) values in the range from 0.9936 to 1.0000 (calculated from absolute peak areas) and from 0.9956 to 1.0000 (calculated from peak areas normalized to HPT). Instrument limits of detection (LODs) and quantification (LOQs) were found at pgmL(-1) level and for the majority of analytes were up to three orders of magnitude lower for NCI compared to EI mode. In both ionization modes, repeatability of measurements expressed as relative standard deviation (RSDs) was less than 10% which is in very good agreement with the criterion of European Union.

  10. Liquid-phase micro-extraction techniques in pesticide residue analysis.

    PubMed

    Lambropoulou, Dimitra A; Albanis, Triantafyllos A

    2007-03-10

    Modern trends in analytical chemistry are towards the simplification and miniaturization of sample preparation, as well as the minimization of organic solvent used. In view of this aspect, several novel micro-extraction techniques are being developed in order to reduce the analysis step, increase the sample throughput and to improve the quality and the sensitivity of analytical methods. One of the emerging techniques in this area is liquid-phase micro-extraction (LPME). It is a miniaturized implementation of conventional liquid/liquid extraction (LLE) in which only microliters of solvents are used instead of several hundred milliliters in LLE. It is quick, inexpensive and can be automated. In the last few years, LPME has been combined with liquid chromatography (LC) and capillary electrophoresis (CE), besides the generally used coupling to gas chromatography (GC), and has been applied to various matrices, including biological, environmental, and food samples. This work is aimed at providing an overview of the major developments of LPME, coupled with chromatography and CE, as reported in the literature. The paper will focus on the application of the technique to different matrices and the aim is to reveal the panorama of opportunities and to try to indicate the potential of LPME in pesticide analysis. A critical review of the first applications to pesticide analyses is presented in the main part of the manuscript. The optimization of LPME as well as advantages and disadvantages are discussed. It is concluded that, because of its high pre-concentration factor, LPME can be introduced with benefit into water analysis for several pesticide groups. In particular, the application of LPME to non-polar pesticides in environmental analysis appears to be promising. However, similar to other micro-extraction techniques, such as solid phase micro-extraction (SPME), serious limitations still remain when analyzing semi-solid and solid environmental, food or biological matrices

  11. [Occurrence of residues of organochlorine pesticides, nitromusk compounds and polychlorobiphenyls in Turkish canned fish products].

    PubMed

    Ozden, O; Kruse, R; Erkan, N

    2001-04-01

    In our study we elaborated an overview on the contamination grade of fish from Turkish waters by selected organochlorine pesticides, nitromusks and chlorobiphenyl congenres. We could demonstrate, that the tested fish species, being prior processed to canned products and brought to the market, contained particularly unmistakable amounts of the above mentioned analytes. Sardines, sardelles and trout gave results generally far below the German regulatory limits. However total DDT in pelamides reached an order of magnitude near the German limit of 0.5 mg/kg (based on wet weight). The necessity of enhanced systematic measurements for monitoring pollutants in fish from Turkish waters thus becomes evident.

  12. 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

  13. [Simultaneous determination of residues of organochlorine and pyrethroid pesticides in tea by microwave assisted extraction solid phase microextraction-gas chromatography].

    PubMed

    Yuan, Ning; Yu, Binbin; Zhang, Maosheng; Zeng, Jingbin; Chen, Xi

    2006-11-01

    The issue of residues including organochlorine and pyrethroid pesticides in tea has made a great attention of researchers and customers in the world. Although some analytical methods have well been established to detect these pesticides, the sample preparations are generally laborious, time-consuming, and some of the procedures caused environmental pollution. Solid phase microextraction (SPME) is a novel sample preparation technique since it is of simplicity, high efficiency and solvent free. SPME was firstly developed to address the need to facilitate environment monitoring. In recent years, great efforts have been made in the analysis of pesticide residues in agricultural products by SPME. In this research, a microwave assisted extraction solid phase microextraction-gas chromatography (MAE-SPME-GC) was applied for the simultaneous determination of organochlorine and pyrethroid pesticides, such as benzene hexa chlorides (alpha-BHC, beta-BHC, gamma-BHC and delta-BHC), 1-(2-chlorophenyl)-1-(4-chlorophenyl)-2, 2, 2-trichloroethane (o, p'-DDT), 2, 2-bis (4-chlorophenyl)-1, 1-dichloroethylene (DDE), 2, 2-bis (4-chlorophenyl)-1, 1-dichloroethane (DDD), 2-(2-chlorophenyl)-2-(4-chlorophenyl)-1, 1, 1-trichloroethane (p, p'-DDT), cypermethrin and fenvalerate. All the tested pesticides were baseline separated under the experimental conditions, except for DDD and o, p'-DDT. The concentration of each pesticide was calibrated by external standard method. The linearities were found to be in the correlation coefficient range of 0.970 5 to 0.998 4 for the tested pesticides between the mass concentrations and peak areas, except for fenvalerate. The recoveries, relative standard deviations and detection limits for the 10 pesticides were 64% - 121%, 10.4% -22.9%, and 1 - 50 ng/L, respectively. The proposed method was successfully applied to the determination of organochlorine pesticide residues in three kinds of teas from the local market. The experimental results demonstrated that

  14. [Isolation and identification of degradation bacteria Enterobacter aerogenes for pyrethriods pesticide residues and its degradation characteristics].

    PubMed

    Liao, Min; Zhang, Hai-jun; Xie, Xiao-mei

    2009-08-15

    By incubation experiment, the bacterial strain labeled as M6R9 was isolated from the tame sludge in water course of Pesticide Factory of Hangzhou, and was identified as Enterobacter aerogenes, which had highly efficient degradation for Bifenthrin, Fenpropathrin and Cypermethrin. By investigating the physiological characteristics of the strain, the results show that the bacterium is a gram-negative aerobe bacilli, size is (0.8-1.9) microm x (0.5-1.0) microm, and is capable of utilizing Bifenthrin, Fenpropathrin and Cypermethrin as sole carbon source. Under the condition of ventilation, (25-30) degrees C, inoculated amount at D(415 nm) 0.2, pH 7.0, pesticide concentration 100 mg x L(-1) and vibrational speed 180 r x min(-1), the degradation efficiencies to Bifenthrin, Fenpropathrin and Cypermethrin are the highest by strain M6R9. Under such condition, in the mixture culture medium with 100 mg x L(-1) Bifenthrin, Fenpropathrin and Cypermethrin, the degradation ratios are 55.74%, 55.11% and 55.96% after culturing 3 d, respectively, the degradation processes are fitted for first-order kinetic equation and the half lives (t(1/2)) are 65.4,70.7 and 68.6 h respectively. The degradation ability of Enterobacter aerogenes M6R9 on Bifenthrin, Fenpropathrin and Cypermethrin is positively correlated to inoculated amount,vibrational speed and ventilation.

  15. Residue patterns of currently, historically and never-used organochlorine pesticides in agricultural soils across China and associated health risks.

    PubMed

    Niu, Lili; Xu, Chao; Zhu, Siyu; Liu, Weiping

    2016-12-01

    Organochlorine pesticides (OCPs) with different usage states, such as currently, historically or never used, may show different behaviors and potential risks in the environment. It is essential to identify their distribution patterns and fates and to assess their associated health risks to humans. In this study, based on a nationwide sampling campaign across China, we determined the concentrations of currently (endosulfan), historically (chlordane and heptachlor) and never-used (aldrin, dieldrin and endrin) OCPs in agricultural soils. The total residue inventories of ∑Endosulfans, ∑Chlordanes, heptachlor and ∑Drins in soils were 260, 64.3, 54.2 and 88.6 t, respectively. The residues of endosulfan were influenced by current usage, showing a latitude transect trend. Drins were mainly from long-range transport, but the illegal usage in China still affected their residues. This finding indicates that endosulfan and drins in Chinese agricultural soils mainly follow the primary and secondary distribution pattern, respectively. Both primary and secondary distribution have a great impact on the distribution pattern of chlordane, which had been banned for only 4 years at the time we sampled. The health risks of these OCPs were estimated based on their concentrations. There were 0.813% and 1.63% of samples that exceeded the target values for chlordane and endrin according to the Netherlands guideline for unpolluted soil. Their residues in most of the samples posed no or few non-carcinogenic and carcinogenic risks to human beings. The results from this study will provide powerful support for pollution control and management.

  16. 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.

  17. 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.

  18. 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.

  19. Analytical methods for a national study of chemical residues in fish. 2. Pesticides and polychlorinated biphenyls

    SciTech Connect

    Marquis, P.J.; Hanson, R.L.; Larsen, M.L.; DeVita, W.M.; Butterworth, B.C.

    1994-01-01

    Analytical methods and a quality assurance plan have been developed to determine the concentration of a select group of bioaccumulatable chemicals in fish tissue. The analytes include Polychlorinated biphenyls (PCBs) and 21 pesticides and industrial chemicals. The methodology has been used to conduct a survey of chemical contaminants in fish from nearly 400 major watersheds in the United States. The methodology consists of the preparation of a single extract via soxhlet extraction, gel permeation and silica gel chromatography and quantification by HRGC/LRMS. The minimum level of detection for most analytes is near 1 ng/g. Rigorous quality assurance/quality control criteria have been developed to assure the generation of high quality data.

  20. Rapid analytical method for the determination of pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction prior to gas chromatography-tandem mass spectrometry.

    PubMed

    Prados-Rosales, R C; Luque García, J L; Luque de Castro, M D

    2003-04-18

    A rapid analytical method for determination of organochlorine pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction has been developed. The main factors affecting the extraction efficiency--namely microwave power, irradiation time, volume of extractant and number of cycles--were optimized by a two-level factorial fractional design. After extraction, a liquid-liquid extraction and a clean-up step including the use of Florisil macrocolumns were required prior to injection of the extracts into the chromatograph in order to isolate the pesticide residues from the lipid fraction of the original extract. The MS-MS ion preparation mode was selected due to the high sensitivity and selectivity it provides. Seed samples were used collected near a crop subjected to aerial pesticide application. Residues of hexachlorocyclohexane isomers and endosulfan were found in the seeds although they were not subjected to pesticide application, thus showing the spray-drift contamination. The validation of the proposed approach was carried out by comparison with the ISO 659-1988 reference extraction method obtaining similar, or even better efficiencies by the proposed approach.

  1. Solid-phase microextraction applied to the analysis of pesticide residues in honey using gas chromatography with electron-capture detection.

    PubMed

    Jiménez, J J; Bernal, J L; del Nozal, M J; Martín, M T; Mayorga, A L

    1998-12-31

    The possibilities of using solid-phase microextraction to determine residues of pesticides in honey have been examined. For this purpose, three types of fiber have been assayed: polyacrylate of 85 microns thickness, and polydimethylsiloxane of 7 and 100 microns thickness. They have been applied to the extraction of 21 pesticides of different chemical families. The effects of the temperature, extraction time and ionic strength on the microextraction have been studied, proposing the most adequate for each fiber. Under optimized conditions, precision, intervals of linearity and detection limits were evaluated.

  2. Application of gas chromatography/tandem quadrupole mass spectrometry to the multi-residue analysis of pesticides in green leafy vegetables.

    PubMed

    Walorczyk, Stanisław

    2008-12-01

    A new, sensitive and specific method has been developed for the simultaneous determination of 129 pesticides in lettuce and other green leafy vegetables. The samples were extracted with acetonitrile and co-extractives such as fatty acids and pigments were removed using dispersive solid-phase extraction (dispersive-SPE) with primary secondary amine (PSA) and graphitized carbon black (GCB). All pesticides were analyzed in a single injection gas chromatography/tandem quadrupole mass spectrometry (GC/MS/MS) acquisition method. Two multiple reaction monitoring (MRM) transitions of precursor ions fragmenting into product ions were recorded for the targeted pesticides, thus fulfilling the EU identification points system criteria for the identification of contaminants (2002/657/EC). Calibration curves were determined using matrix-matched standards, and exhibited excellent linearity at two orders of magnitude from 0.005 to 0.5 mg/kg for almost all the pesticides studied (R(2) > or = 0.99). The analytical performance was demonstrated by the analysis of lettuce samples spiked at five concentration levels ranging from 0.005 to 0.5 mg/kg for each pesticide. The recovery and repeatability results satisfied SANCO/2007/3131 criteria (i.e. average recoveries were in the range 70-120% with RSDs < or =20%) for 114 of the 129 pesticides at the 0.005 mg/kg spiking level, and for almost all pesticides at the higher spiking levels. The methodology was applied successfully to identify and quantify pesticide residues in leafy vegetable samples such as lettuce, cabbage and leek.

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

    PubMed Central

    Khamis, Farhat A.; Lugwisha, Esther H. J.

    2017-01-01

    This study investigated the levels of pesticides and metabolites in vegetables from major markets in Dar es Salaam city, Tanzania. Samples of fresh cabbage, spinach, and onions from the markets were analysed for pesticide residues. Extraction was performed using acetone followed by dichloromethane : cyclohexane mixture and the extracts were cleaned up using Florisil. The compounds were determined by gas chromatography-mass spectrometry (GC-MS). Pesticides and metabolites were detected in 72.2% of the samples. The detected pesticide residues and their highest mean concentrations were p,p′-DDT 4.00 × 10−3 mg/kg, p,p′-DDD 6.40 × 10−1 mg/kg, o,p′-DDD 1.00 × 10−2 mg/kg, α-endosulfan 6.00 × 10−1 mg/kg, β-endosulfan 2.10 × 10−1 mg/kg, chlorpyrifos 3.00 mg/kg, and cypermethrin 4.00 × 10−2 mg/kg. The most frequently detected compounds were p,p′-DDD and chlorpyrifos. The order of contamination was spinach > cabbage > onions. Generally, there were no significant variations in concentrations of pesticide residues among samples and sampling sites, which indicated similarities in contamination patterns. The concentrations of contaminants were above the maximum residue limits (MRLs) in 33.3–50% of the samples. The findings indicated risks and concerns for public health. PMID:28280510

  4. Interpretation of aged sorption studies for pesticides and their use in European Union regulatory leaching assessments.

    PubMed

    Beulke, Sabine; van Beinum, Wendy; Suddaby, Laura

    2015-04-01

    First-tier regulatory exposure assessments for pesticides assume that pesticide sorption is instantaneous and fully reversible. In European Union (EU) regulatory guidance, an increase in sorption over time ("aged sorption") can be considered at the higher tier to refine predicted environmental concentrations in groundwater. Research commissioned by the UK Chemicals Regulation Directorate (CRD), funded by the Department for Environment Food & Rural Affairs (Defra), formed the basis of a draft regulatory guidance document proposing 1) a protocol on how to measure aged sorption of parent compounds in laboratory studies, 2) procedures to fit kinetic models to the experimental data, 3) criteria to test the reliability of the parameters, and 4) procedures for use of the parameters in the groundwater exposure assessment. The draft guidance was revised after feedback from stakeholders and testing of the guidance was performed against real data sets by an independent consultancy. The Chemicals Regulation Directorate submitted the revised document to the European Food Safety Authority (EFSA) for scrutiny. This article gives an overview of the draft guidance and explains the reasoning behind the recommendations made.

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

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... EP 1 885.2250 Nature of the Residue in animals CR EP 1 885.2300 Analytical methods - plants CR TGAI 1 885.2350 Analytical methods-animals CR TGAI 1 885.2400 Storage Stability CR EP 1 885.2500 Magnitude of... results of testing: i. Indicate the potential to cause adverse human health effects or the...

  6. 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.

  7. Determination of low-level pesticide residues in soft drinks and sports drinks by liquid chromatography with tandem mass spectrometry: collaborative study.

    PubMed

    Miller, Kathleen D; Milne, Paul

    2008-01-01

    A collaborative study was conducted on a method for the measurement of 11 low-level pesticide residues in soft drinks and sports drinks by liquid chromatography with tandem mass spectrometry. The pesticide residues determined in this study were alachlor, atrazine, butachlor, isoproturon, malaoxon, monocrotophos, methyl paraoxon, phorate, phorate sulfone, phorate sulfoxide, and 2,4-dichlorophenoxyacetic acid (2,4-D). Blind fortification solutions containing 3 different levels of pesticide residues were provided to 9 collaborating laboratories to create test samples at concentrations of 0, 0.1, and 0.5 microg/L with a 10-fold concentration for phorate in a total of 6 matrixes (2 colas, 1 diet cola, 1 clear lemon-lime soft drink, 1 orange soft drink, and 1 sports drink). Good qualitative performance of the method was demonstrated for all pesticide residues. Reproducibility relative standard deviation (RSDR) ranged from 7 to 151% for alachlor, atrazine, butachlor, isoproturon, malaoxon, monocrotophos, methyl paraoxon, phorate, phorate sulfone, phorate sulfoxide, and 2,4-D at the 0.1 microg/L level (1.0 microg/L for phorate). At 0.5 microg/L (5.0 microg/L for phorate), RSDR ranged from 9 to 57% for alachlor, atrazine, butachlor isoproturon, malaoxon, monocrotophos, methyl paraoxon, phorate, phorate sulfone, phorate sulfoxide, and 2,4-D in all matrixes. Repeatability relative standard deviation (RSDr), applicable to the diet cola and sports drink, ranged from 0 to 124% for the 11 pesticide residues at the 0.1 microg/L level (1.0 microg/L for phorate). At 0.5 microg/L (5.0 microg/L for phorate), RSDr ranged from 4 to 26%. Recoveries for the 11 pesticide residues in all matrixes ranged from 84 to 300% at the 0.1 microg/L level (1.0 microg/L for phorate) and from 66 to 127% at the 0.5 microg/L (5.0 microg/L for phorate) level. Coefficients of determination (r2) of the matrix-matched calibration curves were > or = 0.95. It is recommended that the method be accepted by AOAC

  8. Determination of pesticide residues (> 0.5 microg/L) in soft drinks and sports drinks by gas chromatography with mass spectrometry: collaborative study.

    PubMed

    Miller, Kathleen D; Milne, Paul

    2008-01-01

    A collaborative study was conducted on a method for the measurement of 19 low-level pesticide residues in soft drinks and sports drinks by gas chromatography with mass spectrometry (GC/MS). The pesticide residues determined were 2,4'-dichlorodiphenyldichloroethylene (2,4'-DDE); 2,4'-dichlorodiphenyldichloroethane (2,4'-DDD); 4,4'-dichlorodiphenyldichloroethylene (4,4'-DDE); 2,4'-dichlorodiphenyltrichloroethane (2,4'-DDT); 4,4'-dichlorodiphenyltrichloroethane (4,4'-DDT); 4,4'-dichlorodiphenyldichloroethane (4,4'-DDD); alpha-endosulfan; endosulfan-sulfate; dieldrin; aldrin; ethion; chlorpyrifos; beta-endosulfan; malathion; methyl-parathion; alpha-hexachlorocyclohexane (alpha-HCH); beta-HCH; delta-HCH; and gamma-HCH. Blind fortification solutions containing 4 different levels of pesticide residues (0, 0.1, 0.5, and 1.0 microg/L) were provided to 8 collaborating laboratories who used them to create test samples in 6 matrixes (also provided): 2 colas, a diet cola, a clear lemon-lime soft drink, an orange soft drink, and a sports drink. Reproducibility (RSDR) for all 19 pesticide residues in all matrixes ranged from 7 to 151% at the 0.1 microg/L level, 11 to 121% at 0.5 microg/L, and 14 to 67% at 1.0 microg/L. Repeatability (RSDr), applicable to the diet cola and the sports drink, ranged from 1 to 76% for the 19 pesticide residues at the 0.1 microg/L level, 9 to 38% at 0.5 microg/L, and 9 to 38% at 1.0 microg/L. Recoveries for the 19 pesticide residues in all matrixes ranged from 77 to 645% at the 0.1 microg/L level, 60 to 231% at 0.5 microg/L, and 61 to 146% at 1.0 microg/L. It is recommended that the method be accepted by AOAC as Official First Action with a limit of quantification (LOQ) equal to 0.5 microg/L for 4,4'-DDT; 2,4'-DDT; 2,4'-DDD; 4,4'-DDE; 4,4'-DDD; 2,4'-DDE; aldrin; dieldrin; alpha-endosulfan; endosulfan-sulfate; chlorpyrifos; and ethion, and an LOQ equal to 1.0 microg/L for beta-endosulfan; alpha-HCH; beta-HCH; delta-HCH; gamma-HCH; methyl-parathion; and

  9. 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

  10. Pesticide residue analysis of a dietary ingredient by gas chromatography/selected-ion monitoring mass spectrometry using neutral alumina solid-phase extraction cleanup.

    PubMed

    Jeong, Mijeong Lee; Zahn, Michael; Trinh, Thao; Brooke, Fay A; Ma, Wenwen

    2008-01-01

    A sample cleanup procedure has been developed to remove coextractives that interfere with pesticide residue analysis of a dietary ingredient (Product B), an extract consisting of Scutellaria baicalensis and Acacia catechu. Samples were extracted using 1% acetic acid in acetonitrile, followed by solid-phase extraction and analysis by capillary gas chromatography with mass spectrometry in the selective-ion monitoring mode. Neutral alumina (alumina N) was found to be the most effective sorbent to remove coextractives from Product B; other materials that were tested but failed to remove interference were graphitized carbon black/primary-secondary amine (PSA), octadecylsilane (C18), Florisil, Oasis MCX, and strong anion exchange-PSA. The method was specifically developed for Product B, which was spiked with 41 organochlorine and organophosphorus pesticides, and resulted in the recovery of 80 to 120% at U.S. Pharmacopeia limits (0.06 to 4 microg/g) for the majority of the pesticides.

  11. Survey of residues of organochlorine pesticides in some marketable Egyptian fish.

    PubMed

    Abdallah, M A; Hassan, I M; Naguib, M M; Abodonia, M A

    1990-01-01

    One hundred random samples representing 34 species of marketable fish were collected from 8 Egyptian governorates during the period March 1986 to March 1988 and were analyzed for the presence of some organochlorine pesticides. The results showed the predominance of beta-BHC and lindane at maximum levels of 435.30 and 59.00 micrograms/kg, respectively, for fish samples obtained from Damietta governorate. The corresponding levels of aldrin, and o,p'-DDT were 34.27 and 734.10 micrograms/kg, respectively, for fish from the Red Sea governorate. gamma-Chlordane, p,p'-DDE, and p,p'-DDT were found in fish from Ismailia governorate at respective maximum levels of 36.17, 234.40, and 57.19 microgram/kg. Heptachlor was identified at 8.50 micrograms/kg in Port Said governorate fish and o,p'-DDE at 10.59 micrograms/kg in Suez governorate fish. Mirex, on the other hand, could not be detected in any of the samples investigated.

  12. 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.

  13. 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

    2016-01-04

    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.

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

    PubMed

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

    2010-11-01

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

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

    PubMed

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

    2008-06-01

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

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

    PubMed

    Liu, Hongmei; Kong, Weijun; Qi, Yun; Gong, Bao; Miao, Qing; Wei, Jianhe; Yang, Meihua

    2014-01-01

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

  17. 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.

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

    PubMed

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

    2014-04-30

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

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

    PubMed

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

    2014-06-15

    A modified QuEChERS (quick, easy, cheap, effective, rugged and safe) method using multi-walled carbon nanotubes (MWCNTs) as a dispersive solid phase extraction (d-SPE) absorbent was established for analysis of 78 pesticide residues in tea. A 6 mg MWCNT sample was selected as the optimised amount based on the distribution of pesticide recoveries and clean-up efficiency from 6 mL acetonitrile extracts. The matrix effects of the method were evaluated and matrix-matched calibration was recommended. The method was validated employing gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) at the spiked concentration levels of 0.05, 0.1 and 0.15 mg kg(-1). For most of the targeted pesticides, the percent recoveries range from 70% to 120%, with relative standard deviations (RSDs) <20%. The linear correlation coefficients (r(2)) were higher than 0.99 at concentration levels of 0.025-0.500 mg kg(-1). In this study, MWCNTs were proved to be a promising d-SPE absorbent with excellent cleanup efficiency, which could be widely applied for the analysis of pesticide residues.

  20. Multi-residue determination of pesticides in water using multi-walled carbon nanotubes solid-phase extraction and gas chromatography-mass spectrometry.

    PubMed

    Wang, Shuo; Zhao, Peng; Min, Guang; Fang, Guozhen

    2007-09-21

    A reliable multi-residue method which was based on solid-phase extraction (SPE) with multi-walled carbon nanotubes (MWCNTs) as adsorbent was developed for determination and quantitation of 12 pesticides (carbofuran, iprobenfos, parathion-methyl, prometryn, fenitrothion, parathion-ethyl, isocarbofos, phenthoate, methidathion, endrin, ethion, methoxychlor) in surface water by gas chromatography-mass spectrometry (GC-MS). Parameters that might influence the extraction efficiency such as the eluent volume, the sample flow rate and the sample loading volume were optimized. The experimental results showed the excellent linearity of 12 pesticides (R(2)>0.99) over the range of 0.04-4 microg L(-1), and the precisions (RSD) were 3.1-15.1% under the optimal conditions. The detection limits of proposed method could reach 0.01-0.03 microg L(-1) based on the ratio of chromatographic signal to base line noise (S/N=3). Good recoveries achieved with spiked water samples were in the range of 82.0-103.7%. The results indicated that MWCNTs have good adsorbability to the 12 pesticides tested in this study. With less cost, less analytical time and less solvent-consuming, the developed multi-residue method could be used to determine multi-class pesticides in water simultaneously.