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PubMed1997

Capillary electrophoresis of pesticides.

Pesticides are important and diverse environmental and agricultural species. Their determination in pesticide formulations, in feed and food, and in complex environmental matrices (e.g., water, soil, sludge, sediments, etc.) often requires separation methods of high efficiency, unique selectivity and high sensitivity. As shown in this comprehensive review, capillary electrophoresis meets these requirements and has proved to be a suitable microseparation technique for the analysis of a wide variety of chiral and achiral pesticides. It is also shown that by combining selective precolumn derivatization schemes, sensitive detection methods (e.g., laser induced fluorescence detection) and trace enrichment techniques, capillary electrophoresis (CE) is capable of determining pesticides at trace levels as those usually encountered in environmental samples.

Electrophoresis, Capillary↗
PubMed2005

Quantitative analysis of six pesticides in fruits by capillary electrophoresis-electrospray-mass spectrometry.

A method to identify and quantify six pesticide residues - dinoseb, pirimicarb, procymidone, pyrifenox, pyrimethanil, and thiabendazole - in peaches and nectarines using capillary electrophoresis-electrospray ionization-quadrupole ion trap-tandem mass spectrometry (CE-ESI-MS/MS) is described. Separation was carried out using a buffer of 0.3 M ammonium acetate at pH 4 with 10% methanol. Pesticide residues present in peach and nectarine samples were preconcentrated by solid-phase extraction using C(18), eluted with CH(2)Cl(2), concentrated to dryness, and redissolved in buffer to obtain lower detection limits. The recoveries of the analytes ranged from 58 to 99% and the relative standard deviations were 9 to 19%. Under optimized CE-MS/MS conditions the minimum detectable levels for the six pesticides in spiked peach samples were between 0.01 mg/kg for pirimicarb and 0.05 mg/kg for procymidone with pressure injection of 50 mbar for 5 s (5 nL) at a signal-to-noise ratio of 3, which constitutes a severalfold increase in sensitivity compared to CE-MS, using a single quadrupole, and to conventional CE-UV. The potential of the method was demonstrated by analyzing different samples taken from regional agricultural cooperatives. The pesticides most often detected were thiabendazole and procymidone.

Electrophoresis, Capillary↗
PubMed2006

Asthma history, occupational exposure to pesticides and the risk of non-Hodgkin's lymphoma.

We previously reported that, although asthma did not increase the risk of non-Hodgkin's lymphoma (NHL), the risk from pesticide exposures was higher among asthmatics than that among nonasthmatics. To further evaluate this finding, we analyzed data from a population-based case-control study of NHL conducted in Iowa, Detroit, Los Angeles and Seattle. Cases (n = 668) diagnosed with NHL from 1998 to 2000 and controls (n = 543) randomly selected from the same geographical areas as that of the cases were included in this analysis. Odds ratios (OR) for the risk of NHL from potential occupational exposure to pesticides tended to be higher among asthmatics (OR = 1.7; 95% CI 0.3-9.1) when compared with that among nonasthmatics (OR = 0.9; 95% CI 0.6-1.5). The risks of NHL associated with pesticide exposure were also higher among asthmatics who had history of hospitalization (OR = 2.1; 95% CI 0.2-29.0) or daily medication for asthma (OR = infinite) than those among asthmatics who did not have such histories. Our results support the previous finding that the risk of NHL from pesticide exposure may be greater among asthmatics.

Adult↗
PubMed2006

Cancer incidence among pesticide applicators exposed to metolachlor in the Agricultural Health Study.

Metolachlor is one of the most widely used herbicides in the United States. We evaluated the incidence of cancer among pesticide applicators exposed to metolachlor in the Agricultural Health Study, a prospective cohort study of licensed pesticide applicators in Iowa and North Carolina. A total of 50,193 pesticide applicators were included. Detailed information on pesticide exposure and lifestyle factors was obtained from self-administered enrollment questionnaires completed between 1993 and 1997; average length of follow-up was 7.33 years. Two metolachlor exposure metrics were used : (i) lifetime days personally mixed or applied metolachlor and (ii) intensity-weighted lifetime days (lifetime days x an intensity level). Poisson regression analysis was used to estimate relative risks (RR) and 95% confidence intervals (95%CI) for cancer subtypes by tertiles of metolachlor exposure. No clear risk for any cancer subtype was found for exposure to metolachlor. A significantly decreased RR was found for prostate cancer in the highest category of lifetime days exposure (RR = 0.59; 95%CI, 0.39-0.89) and in the second highest category of intensity-weighted lifetime days exposure (RR = 0.66; 95%CI, 0.45-0.97); however, the test for trend was not significant for either exposure metric. A nonsignificantly increased risk was found for lung cancer with lifetime days exposure in the highest category (RR = 2.37; 95%CI, 0.97-5.82, p-trend = 0.03) but not with intensity-weighted lifetime days. Given the widespread use of metolachlor and the frequent detection of metolachlor in both surface and ground water, future analyses of the AHS will allow further examination of long-term health effects, including lung cancer and the less common cancers.

Acetamides↗
PubMedDate not supplied

Toxicological evaluation of mixtures of ten widely used pesticides.

Toxicities of pesticidal mixtures in biological systems have not been explored adequately. Therefore, mixtures of ten widely used pesticides were evaluated for their toxicity in ICR male mice (21-24 g). Mice were given four mixtures of alachlor, aldrin, atrazine, 2,4-dichlorophenoxyacetic acid, DDT, dieldrin, endosulfan, lindane, parathion and toxaphene, at 0.01, 0.1, 1.0 and 10 ppm of each of these pesticides, in drinking water for 90 days ad libitum. Also, two mixtures at 2.5 and 5 mg kg-1 of each pesticide in 7.5% Tween-80 in water were administered to additional groups of mice by oral intubation daily for up to 14 days. In relation to the control, the 90-day exposure caused a dose-dependent increase in the liver/body weight ratio (3-44%), a decrease in the pentobarbital (60 mg kg-1, i.p.)-induced sleep time (11-79%) and an increase in the metabolism of aniline (233-399%), amidopyrine (79-231%), phenacetin (127-318%) and benzo[a]pyrene (286-1633%) in the 9000 g hepatic supernatants from the mixture-treated mice. Proliferation, dilatation and fragmentation of the endoplasmic reticulum and scattering of ribosomes were noticed with mixture livers. In the 5 mg kg-1 group, 90% of the animals died by Day 8; incidence of death was considerably less in the 2.5 mg kg-1 group. The serum cholinesterase activity was inhibited by ca. 50% in the 2.5 and 5 mg kg-1 groups on either one or both of Days 8 and 15; the liver/body weight ratio increased by 24-79% and the pentobarbital-induced sleep time decreased by 80-96%.(ABSTRACT TRUNCATED AT 250 WORDS)

Administration, Oral↗
PubMed2002

Prediction of aqueous solubility of drugs and pesticides with COSMO-RS.

The COSMO-RS method, originally developed for the prediction of liquid-liquid and liquid-vapor equilibrium constants based on quantum chemical calculations, has been extended to solid compounds by addition of a heuristic expression for the Gibbs free energy of fusion. By this addition, COSMO-RS is now capable of a priori prediction of aqueous solubilities of a wide range of typical neutral drug and pesticide compounds. Only three parameters in the heuristic expression have been fitted on a data set of 150 drug-like compounds. On these data an rms deviation of 0.66 log-units was achieved. Later, the model was tested on a set of 107 pesticides, which have been critically selected based on two experimental data sources and by a crosscheck with an independent HQSAR model. On this data set an rms of 0.61 log-units was achieved, without any adjustments to the structurally extremely diverse pesticides. This result verifies the ability of this extended COSMO-RS to predict aqueous solubilities of drugs and pesticides of almost arbitrary structural classes. The new method is COSMO-RSol.

Artificial Intelligence↗
PubMed1980

Effect of five pesticides on the mycelial growth of some soil and pathogenic fungi.

The effect of three doses (the lowest is the recommended dose in the field) of 5 pesticides namely: Ceresan, Orthocid (fungicides), VCS-438 (herbicide), and Dursban and Dipterex (insecticides) on the mycelial dry weight of Aspergillus fumigatus. Fusarium moniforme, Pencillium italicum, and Sclerotium ceprivorum was tested 2, 4, 6, 8 and 10 days after treatment. All the pesticides induced inhibition of mycelial growth of the test fungi. Only VCS-438 at the low dose was stimulatory to F. moniliforme after 4 and 6 days and to P. italicum after 4 days. The rate of inhibition was influenced by the type of fungus, the age of the mycelium, and the dose of the pesticide. At the end of the experiment the two fungicides were detoxified by the test fungi with a rate higher than that of the other pesticides.

Antifungal Agents↗
PubMed2005

Use of automated direct sample introduction with analyte protectants in the GC-MS analysis of pesticide residues.

Automated large-volume direct sample introduction, or difficult matrix introduction (DMI), was investigated in the determination of 44 pesticide residues possessing a wide range of physico-chemical properties (volatility, polarity, pK(a)) in fruit-based baby food by means of gas chromatography-mass spectrometry (GC-MS) with a quadrupole mass analyzer. DMI has advantages over traditional injection because large volumes (up to 30 microL) of potentially dirty sample extracts can be injected into the GC-MS, but nonvolatile matrix components that would normally contaminate the inlet are removed after every injection. The extra matrix and glass surfaces involved in DMI, however, make the system more prone to the matrix-induced chromatographic enhancement effect, which adversely affects quantification of several pesticides. To overcome this problem, matrix-matched calibration standards and/or the use of analyte protectants were applied in the DMI approach, and the analysis of extracts was also compared before and after undergoing clean-up by dispersive solid-phase extraction. For best quantification, clean-up was still needed, and the combination of matrix-matching with analyte protectants gave the most reproducible results. Depending on the application, however, the addition of analyte protectants (a mixture of 3-ethoxy-1,2-propanediol, L-gulonic acid 3-lactone, and D-sorbitol) to sample extracts and calibration standards in solvent (non-matrix matched), gave satisfactory quantification for most of the 44 pesticides tested. The lowest calibration levels for 34 of the 44 pesticides were < or = 10 ng/g, which meets the standard required by the European Union Baby Food Directive (2003/13/EC).

Calibration↗
PubMed2006

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

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).

Beverages↗
PubMed2006

Comparing ecological risks of pesticides: the utility of a Risk Quotient ranking approach across refinements of exposure.

Environmental risk assessment of pesticides and other chemicals often uses the Risk Quotient (RQ) method to characterize risk quantitatively. An RQ is calculated by dividing an environmental exposure value by a toxicity end-point value. Tier 1 RQs, which are characterized by highly conservative toxicity and exposure assumptions, are used primarily for screening out negligible risks in regulatory decision making. It has been argued that the tier 1 RQ approach is valuable for making direct comparisons of quantitative risk between pesticides. However, an outstanding question is whether relative risks among pesticides would change if refinements of exposure are incorporated into the RQ calculations. This study tested that hypothesis. Aquatic ecological risk assessments were conducted for 12 herbicide and 12 insecticide active ingredients used on agricultural crops in the USA. The pesticides were chosen because surface-water monitoring data for them were available as part of the United States Geological Survey's National Water-Quality Assessment Program (NAWQA). Ecological receptors and effects evaluated were aquatic non-vascular plants (acute risk), aquatic vertebrates (acute risk) and aquatic invertebrates (acute risk) for the herbicides and aquatic vertebrates (acute and chronic risk) and aquatic invertebrates (acute and chronic risk) for the insecticides. The data indicate that there were significant statistical correlations between numerical rankings of tier 1 RQs and RQs using refined environmental exposures. The results support the hypothesis that numerical ranking of RQs for the purpose of comparing potential ecological risks is a valid approach because the rankings are significantly correlated regardless of the degree of exposure refinement.

Animals↗
PubMed2006

Modelling the effects of alcohol ethoxylates on diffusion of pesticides in the cuticular wax of Chenopodium album leaves.

Cuticular waxes represent the first and, in most cases, the limiting barrier for foliar uptake of pesticides from solution. Sorption of pesticides in reconstituted cuticular wax (wax/water partition coefficients) of Chenopodium album L. and in isolated cuticular membranes (cuticle/water partition coefficients) of Prunus laurocerasus L. was determined. Diffusion coefficients of pesticides in reconstituted cuticular wax of C. album leaves were size-dependent, increasing with increasing molar volume. In the presence of alcohol ethoxylates, diffusion coefficients were enhanced by up to two orders of magnitude, and size selectivity was significantly decreased. The accelerating effect and the decrease in size selectivity were attributed to plasticisation of the cuticular wax by the alcohol ethoxylates increasing the fluidity in the wax. A free volume model adopted from polymer science was successfully applied to predict diffusion coefficients of pesticides on the basis of the transport properties of the wax (size selectivity and crystallinity), the molar volume of the diffusing compound and the accelerator concentration in the wax.

Chenopodium album↗
PubMed2006

Impact of correlation between pesticide parameters on estimates of environmental exposure.

Monte Carlo techniques are increasingly used in pesticide exposure modelling to evaluate the uncertainty in predictions arising from uncertainty in input parameters and to estimate the confidence that should be assigned to modelling results. The approach typically involves running a deterministic model repeatedly for a large number of input values sampled from statistical distributions. A key decision in setting up a probabilistic analysis is whether there is correlation between any of the inputs to the analysis. Pesticide properties are often the most sensitive in exposure assessment. Analysis of the literature demonstrated that there are examples of both positive and negative correlation between the sorption and degradation behaviour of a pesticide, but that general trends are not apparent at present. The inclusion of even weak correlation between sorption and degradation was found to greatly influence a probabilistic analysis of leaching through soil. Correlation will reduce the predicted extent of leaching for pesticides, and it is recommended to set the correlation to zero unless the experimental data support an alternative assumption (i.e. where the correlation is statistically significant (P <or= 0.05) and experimental artefacts can be excluded).

Environmental Exposure↗
PubMed2001

The concentration of pesticides in sediments from Kolleru Lake in India.

Kolleru Lake is the largest natural freshwater lake in India. Sediment samples were collected at different locations from Kolleru Lake at different seasons in a year over a period of three years and analyzed for eight selected pesticides. In general, pesticides were present at all locations. The selected pesticides alpha-BHC, gamma-BHC, malathion, chlorpyrifos and endosulfan were present at higher concentrations than isodrin, dieldrin and p,p'-DDT. The concentrations of alpha-BHC, gamma-BHC malathion, chlorpyrifos, isodrin, endosulfan, dieldrin and p,p'-DDT in sediments were 1.2-388, 1.4-212, from below the minimum detection limit (BDL)-186, 1.1-292, BDL-38.6, BDL-206, BDL-128 and BDL-191 micrograms kg-1 dry weight, respectively. The aim of this study is to evaluate baseline data, to try to account for the concentration of pesticides in sediments and to discuss their potential to affect human beings and aquatic organisms.

Ecosystem↗
PubMed2003

Pesticide usage in some vegetable crops in Great Britain: real on-farm applications.

The last decade has seen an increasing requirement throughout the United Kingdom (UK) for accurate, timely information on pesticide usage on fresh produce such as vegetables to satisfy government legislation and provide data as part of the registration and review process of pesticides. These data, collected by the Department for Environment, Food and Rural Affair's Pesticide Usage Survey Group (PUSG), provide information on current and past usage patterns and allow the impact of use on the environment, operator and consumer to be more accurately assessed from actual usage patterns rather than worst-case scenarios. Surveys of commercially grown carrot, Brussels sprouts and onion crops in Great Britain were undertaken at regular intervals between 1986 and 1999, using fully stratified samples of growers. Only on Brussels sprouts was there a significant decline in pesticide use over this period, but the frequency of treatments increased on all three crops, reflecting the recent introduction of more active molecules and lower dose rates. The implications for growers of EU Directive 91/44 are discussed if active ingredients are lost because they fail to achieve Annex 1 listing.

Agriculture↗
PubMed2004

Pesticide residues in food--acute dietary exposure.

Consumer risk assessment is a crucial step in the regulatory approval of pesticide use on food crops. Recently, an additional hurdle has been added to the formal consumer risk assessment process with the introduction of short-term intake or exposure assessment and a comparable short-term toxicity reference, the acute reference dose. Exposure to residues during one meal or over one day is important for short-term or acute intake. Exposure in the short term can be substantially higher than average because the consumption of a food on a single occasion can be very large compared with typical long-term or mean consumption and the food may have a much larger residue than average. Furthermore, the residue level in a single unit of a fruit or vegetable may be higher by a factor (defined as the variability factor, which we have shown to be typically x3 for the 97.5th percentile unit) than the average residue in the lot. Available marketplace data and supervised residue trial data are examined in an investigation of the variability of residues in units of fruit and vegetables. A method is described for estimating the 97.5th percentile value from sets of unit residue data. Variability appears to be generally independent of the pesticide, the crop, crop unit size and the residue level. The deposition of pesticide on the individual unit during application is probably the most significant factor. The diets used in the calculations ideally come from individual and household surveys with enough consumers of each specific food to determine large portion sizes. The diets should distinguish the different forms of a food consumed, eg canned, frozen or fresh, because the residue levels associated with the different forms may be quite different. Dietary intakes may be calculated by a deterministic method or a probabilistic method. In the deterministic method the intake is estimated with the assumptions of large portion consumption of a 'high residue' food (high residue in the sense that the pesticide was used at the highest recommended label rate, the crop was harvested at the smallest interval after treatment and the residue in the edible portion was the highest found in any of the supervised trials in line with these use conditions). The deterministic calculation also includes a variability factor for those foods consumed as units (eg apples, carrots) to allow for the elevated residue in some single units which may not be seen in composited samples. In the probabilistic method the distribution of dietary consumption and the distribution of possible residues are combined in repeated probabilistic calculations to yield a distribution of possible residue intakes. Additional information such as percentage commodity treated and combination of residues from multiple commodities may be incorporated into probabilistic calculations. The IUPAC Advisory Committee on Crop Protection Chemistry has made 11 recommendations relating to acute dietary exposure.

Animals↗
PubMed2006

Application of hollow fiber supported liquid membrane extraction to the simultaneous determination of pesticide residues in vegetables by liquid chromatography/mass spectrometry.

A new analytical procedure using a hollow fiber supported liquid membrane (HFSLM) has been developed for the simultaneous determination of pesticide residues in vegetables by liquid chromatography (LC) coupled with electrospray mass spectrometry (MS). The extraction technique requires minimal sample preparation and solvent consumption. Optimum extraction conditions have been evaluated with respect to sample pH, ionic strength, liquid membrane composition, extraction time, stirring rate and acceptor composition. The extraction method has been validated for matrices such as cucumber, tomato and pepper, indicating that cucumber can be selected as representative matrix for routine analysis of these food commodities. Linear ranges of pesticides in vegetable samples were 10 to 200 microg/kg, and the repeatability of the method was less than 20% for the lowest calibration point. The limits of detection ranged from 0.06 to 2.7 microg/kg and the limits of quantification from 0.2 to 9.0 microg/kg, which were low enough to determine the pesticide residues at concentrations below or equal to the maximum residue levels (MRLs) specified by European Union. The method was finally applied to the determination of more than 20 pesticides in market vegetable samples and the concentrations found in these samples were always lower than the MRLs. This new approach can be considered as a powerful alternative to the traditional extraction techniques.

Chromatography, High Pressure Liquid↗
PubMed1998

Buffer zones for reducing pesticide drift to ditches and risks to aquatic organisms.

Pesticide drift from field sprayers fitted with different types of spray nozzles was investigated under various wind speed conditions. Droplet drift was measured adjacent to the sprayed field, on the ditch bank, and in the ditch. Measurements were carried out in the normal sprayed situation and with an unsprayed buffer zone 3 or 6 m wide. The results indicate that there are major differences between spray nozzles. Drift deposition increases with wind speed. In the sprayed situation and with a wind speed of 0.5 m/s, there was a maximum of 6.0% drift deposition halfway down the ditch bank and no drift deposition in the ditch. At 3 m/s wind speed these figures are 25.1 and 2.2%, respectively. At 5 m/s wind speed, 7.2% drift deposition was measured in the ditch. Risk assessment (cf. SLOOTBOX model) carried out with 17 pesticides used in the study area indicated that at this wind speed, 8 of the 17 pesticides investigated posed a risk to aquatic organisms. Creation of a 3-m buffer zone decreases drift deposition in the ditch by a minimum of 95%. Adjacent to the buffer zone only 4 of the 17 pesticides investigated posed a (minor) risk to aquatic organisms. With a 6-m buffer zone no drift deposition in the ditch could be measured (wind speed maximum, 4.5 m/s). Creating unsprayed crop edges offers good possibilities for the protection of aquatic ecosystems. Socioeconomic research among farmers indicates that buffer zones, such as unsprayed cereal edges and unsprayed grass strips, could well be adopted in agricultural practice.

Agriculture↗
PubMed1995

Pesticide residues in urine of adults living in the United States: reference range concentrations.

We measured 12 analytes in urine of 1000 adults living in the United States to establish reference range concentrations for pesticide residues. We frequently found six of these analytes: 2,5-dichlorophenol (in 98% of adults); 2,4-dichlorophenol (in 64%); 1-naphthol (in 86%); 2-naphthol (in 81%); 3,5,6- trichloro-2-pyridinol (in 82%); and pentachlorophenol (in 64%). The 95th percentile concentration (95th PC) for 2,5-dichlorophenol (indicative of p-dichlorobenzene exposure) was 790 micrograms/liter; concentrations ranged up to 8700 micrograms/liter. 2,4-Dichlorophenol concentrations ranged up to 450 micrograms/ liter, and the 95thPC was 64 micrograms/liter. 1-Naphthol and 2-naphthol (indicative of naphthalene exposure) had 95thPCs of 43 and 30 micrograms/liter, respectively; concentrations of 1-naphthol ranged up to 2500 micrograms/liter. Chlorpyrifos exposure was indicated by 3,5,6-tricholoro-2-pyridinol concentrations of 13 (95thPC) and 77 micrograms/liter (maximum observed). Pentachlorophenol had a 95thPC of 8.2 micrograms/liter. Other analytes measured included 4-nitrophenol (in 41%); 2,4,5-trichlorophenol (in 20%); 2,4,6-trichlorophenol (in 9.5%); 2,4-dichlorophenoxyacetic acid (in 12%); 2-isopropoxyphenol (in 6.8%); and 7-carbofuranphenol (in 1.5%). The 95thPCs of these analytes were < 6 micrograms/liter. p-Dichlorobenzene exposure is ubiquitous; naphthalene and chlorpyrifos are also major sources of pesticide exposure. Exposure to chlorpyrifos appears to be increasing. Although pentachlorophenol exposure is frequent, exposure appears to be decreasing. These reference range concentrations provide information about pesticide exposure and serve as a basis against which to compare concentrations in subjects who may have been exposed to pesticides.

2,4-Dichlorophenoxyacetic Acid↗