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PubMed2001

Analysis of organophosphorus pesticides in honeybee by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry.

Pesticides applied in extended agricultural fields may be controlled by means of bioindicators, such as honeybees, in which are the pesticides bioaccumulate. Liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) experiments with positive (PI) and negative (NI) ion modes were optimized for the analysis of 22 organophosphorus pesticides in honeybee samples. The extraction required 3 g of sample, which was extracted with acetone. The extract was purified with coagulating solution and reextracted with Cl(2)CH(2). Pesticides studied could be detected by both ionization modes except for parathion, parathion-methyl, and bromophos, which did not give signals in PI mode, and triazophos, which was not detected in NI mode. Fragmentation voltage and vaporizer temperature were optimized to achieve the highest sensitivity. The spectra profile of each pesticide in PI mode showed the [M + H](+) ion as the main signal, whereas in NI mode only fragment ions were shown. The detection limit obtained in selected ion monitoring mode ranged from 1 to 15 microg kg(-1). The average recoveries from spiked honeybees at various concentration levels (0.5-5 mg kg(-1)) exceeded 65% with relative standard deviations of 4-15%. The method was applied to real samples, in which residues of coumaphos and dimethoate were detected.

Animals↗
PubMed2003

Assessment of pesticide residues in honey samples from portugal and Spain.

Fifty samples of honey collected from local markets of Portugal and Spain during year 2002 were analyzed for 42 organochlorine, carbamate, and organophosphorus pesticide residues. An analytical procedure based on solid-phase extraction with octadecyl sorbent followed by gas chromatography-mass spectrometry (GC-MS), for organochlorines, and by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS), for organophosphorus and carbamates, has been developed. Recoveries of spiked samples ranged from 73 to 98%, except for dimethoate (40%), with relative standard deviations from 3 to16% in terms of repeatability, and from 6 to 19% in terms of reproducibility. Limits of quantification were from 0.003 to 0.1 mg kg(-)(1). Most of the pesticides found in honey were organochlorines. Among them, gamma-HCH was the most frequently detected in 50% of the samples, followed by HCB in 32% of the samples and the other isomers of HCH (alpha-HCH and beta-HCH) in 28 and 26% of the samples, respectively. Residues of DDT and their metabolites were detected in 20% of the samples. Of the studied carbamates, both methiocarb and carbofuran were detected in 10% of the samples, pirimicarb in 4% and carbaryl in 2%. The only organophosphorus pesticides found were heptenophos in 16%, methidathion in 4%, and parathion methyl in 2% of honey samples. Results indicate that Portuguese honeys were more contaminated than Spanish ones. However, honey consumers of both countries should not be concerned about the amounts of pesticide residues found in honeys available on the market.

Carbamates↗
PubMed2005

Evaluation of supercritical fluid extraction/aminopropyl solid-phase "in-line" cleanup for analysis of pesticide residues in rice.

Supercritical fluid extraction (SFE) and the use of aminopropyl solid-phase material for "in-line" cleanup was evaluated for residue analysis of 22 GC-amenable pesticides in wild- and white-rice samples with a fat content of 1.9 and 0.4%, respectively. After optimizing the extraction conditions on glass beads as inert material and evaluating the fat amount extracted from rice by SFE, the use of Florisil, Celite, Extrelut, Hydromatrix, and an aminopropyl material as fat-retention materials for SFE "in-line" cleanup was assessed, aminopropyl being the most suitable material for this cleanup of fat. Pesticide mean recoveries obtained from rice samples, at fortification levels around 0.5 mg/kg, by means of the SFE/in-line cleanup method finally proposed (15-mL CO2 volume, 50 degrees C temperature, 200 atm pressure, 200 muL of methanol static modifier, and a 1-cm layer of aminopropyl at the bottom of the extraction vessel), ranged between 74 and 98%, except for captafol and dimethoate for which mean recoveries lower than 21% were determined.

Chromatography, Supercritical Fluid↗
PubMed2006

Organophosphate levels in apple composites and individual apples from a treated Canadian orchard.

Azinphos-methyl, phosalone, and phosmet were applied individually to separate rows of trees within a commercial apple orchard in Quebec, Canada, during the 2003 agricultural season. Apples were collected for residue analysis immediately prior to the harvesting of the remaining apples for market distribution and were prepared for analysis as both individual apples and as composites of eight individuals. Analysis of the three applied compounds, as well as five organophosphate insecticides that were not applied, was performed using gas chromatography-mass spectrometry. Azinphos-methyl, phosalone, and phosmet, which were applied, were detected in all samples analyzed at concentrations ranging from 0.004 ng/g to 2260 ng/g. Methidathion was not observed in any sample. Chlorpyrifos, diazinon, dimethoate, and malathion concentrations ranged from below method detection limits to 0.71 ng/g, and the detection frequency for these compounds ranged from 20% to 100%. Residues measured in this study were all below the Canadian maximum residue limit for apples. Variability factors ranged from 2 to 19 for all compounds observed in this study. Composite samples may not accurately reflect the extremes of exposure from consumption of single servings of apples.

Canada↗
PubMed2006

Insecticide dissipation after repeated field application to a Northern Thailand Ultisol.

Nontarget effects of pesticides may occur when the active ingredients have a long persistence in the environment. The half-lives of six insecticides commonly used in Thai fruit orchards under tropical field conditions were determined. A mixture of endosulfan-alpha and -beta, chlorpyrifos, malathion, dimethoate, and mevinphos was applied five times in 10-day intervals onto an Ultisol (lychee plantation ground-covered with grass vegetation, northwestern Thailand). On days 1, 3, 5, 7, and 10 after each application, composite samples of the topsoil (0-10 cm) were collected and exhaustively extracted. Fitting a first-order model to the datasets revealed rapid initial dissipation [half-lives from 2.2 +/- 0.4 (malathion) to 5.4 +/- 1.3 days (chlorpyrifos)]. Volatilization appeared to be a major process of pesticide dissipation, especially for malathion and mevinphos. Because 8% of the applied endosulfan-alpha and -beta had been converted to the sulfate metabolite within 1 day after the first application, also microbial degradation contributed significantly to pesticide dissipation. Nevertheless, no trend in half-lives over the five application cycles could be observed, indicating that accelerated microbial degradation did not occur for these insecticides following the five applications. Precipitation and soil moisture were key parameters of dissipation, but dissipation processes were too complex to be generalized for all substances studied. Despite their short half-lives, all pesticides except mevinphos accumulated in soil (up to 656%; endosulfan-alpha), and this accumulation correlated significantly with the hydrophobicity of the substances (r = 0.88). This was interpreted as an aging process, and it was concluded that pesticide aging must be considered relevant also in tropical environments, where it has received very limited attention so far.

Chemical Phenomena↗
PubMed2003

Determination of organophosphorus pesticides and related compounds in water samples by membrane extraction and gas chromatography.

A membrane extraction-gas chromatography method was developed for determination of organophosphorus pesticides and related compounds including methamidophos, DDVP, dimethoate, methyl parathion, parathion, thiophosphoric acid trimethyl ester, and thiophosphoramidic acid dimethyl ester in water samples. In this method, surface-modified acetic cellulose membranes were used to extract the target analytes in water samples, the extracted analytes were back-extracted into a small amount of methanol, and gas chromatography with pulsed flame photometric detector (GC-PFPD) was used to determine the concentrations of target analytes in the extracts. The recoveries obtained for the target analytes spiked into the water samples ranged from 66 to 94%. The method detection limit for each target analyte was 0.05 microg L(-1). The method developed in this study had shown the advantages of being cheap, simple, fast, and reliable. It had been used successfully to determine the concentrations of target analytes in river water samples.

Chromatography, Gas↗
PubMed2004

Genetic analysis and cross-resistance spectrum of a laboratory-selected chlorfenapyr resistant strain of two-spotted spider mite (Acari: Tetranychidae).

A laboratory susceptible strain of Tetranychus urticae was selected with chlorfenapyr resulting in a resistant strain. After 12 cycles of exposure, the resistance ratio (RR) calculated from the LC50s of susceptible and selected strain was 580. The resistant strain was screened with 16 currently used acaricides for cross-resistance. Cross-resistance was detected with amitraz (RR = 19.1), bifenthrin (RR = 1.3), bromopropylate (RR = 7.5), clofentezine (RR = 29.6) and dimethoate (RR = 17.6). No cross-resistance was detected with the new molecules acequinocyl, bifenazate and spirodiclofen. Mortality caused by chlorfenapyr in the F1 progeny from reciprocal crosses between both strains indicated that the mode of inheritance was incomplete recessive. Mortality in F2 progeny indicated that the resistance was under the control of more than one gene. Synergist experiments with S,S,S-tributylphosphorotrithioate (DEF), piperonylbutoxide (PBO) and diethylmaleate (DEM), which are inhibitors of esterases, monooxygenases and glutathion-S-transferases respectively, suggested a major role of esterases in the resistance to chlorfenapyr.

Animals↗
PubMed2002

Dissolved insecticides and polychlorinated biphenyls in the Pearl River Estuary and South China Sea.

Persistent organic pollutants (POPs) such as organochlorine (OCl) insecticides and polychlorinated biphenyls (PCB), together with the new generation of organophosphorus (OP) insecticides, are of global concern, due to their widespread occurrence, persistence, bioaccumulation and hormone disruption potential. This paper represents an attempt to study the source and transportation of such pollutants in estuarine and coastal environments as an integrated ecosystem, by determining the levels of 18 OCl insecticides, 21 PCB congeners, and 17 OP insecticides in the Pearl River Estuary and South China Sea. The total concentrations varied from 126-1198 ng l(-1) for OCl insecticides, 33.38-1064 ng l(-1) for PCB congeners, and 4.44-6356 ng l(-1) for OP insecticides in the Pearl River Estuary. In comparison, their levels in the South China Sea were significantly lower, varying from 57.09-202 ng l(-1) for OCl insecticides, 21.72-144 ng l(-1) for PCBs, and 1.27-122 ng l(-1) for OP insecticides, respectively. The predominance of beta-HCH in HCHs, and DDE in DDTs in all water samples was clearly observed, suggesting beta-HCH and DDE's resistance to further degradation. The PCBs were dominated by those with 3-6 chlorines. The distribution characteristic of OP insecticides shows that five compounds (methamidophos, dimethoate, malathion, dichlorvos and omethoate) accounted for 56% and 72% of the total OP insecticide concentration. The relationship between pollutant concentrations and salinity in the estuary showed that they were all removed during the mixing process, therefore behaving non-conservatively.

China↗
PubMed2003

Analysis of pesticide residues in lettuce by large volume-difficult matrix introduction-gas chromatography-time of flight-mass spectrometry (LV-DMI-GC-TOF-MS).

A multi-residue method is described that eliminates the need for a clean-up step and thus allows the rapid determination of pesticides in crude extracts of lettuce. Samples were extracted with a mixture of ethyl acetate, Na2SO4 and NaHCO3 and the crude extracts analysed directly using large volume-difficult matrix introduction (LV-DMI) in combination with gas chromatography-time of flight-mass spectrometry (GC-TOF-MS). The LV-DMI procedure described was evaluated for the analysis of dimethoate, pyrimethanil, chlorothalonil, vinclozolin, furalaxyl and oxadixyl. Satisfactory response was obtained at the lowest calibrated level (LCL) of 0.0025 microg ml(-1), with good linearity over the range 0.0025-0.5 microg ml(-1) (0.005-1.0 mg kg(-1) equivalent). Average recoveries between 73 and 118% were obtained at the 0.01-0.5 mg kg(-1) levels with RSD values < or = 13%.

Chromatography, Gas↗
PubMed2002

Estrogenicity of organophosphorus and pyrethroid pesticides.

Although organophosphorus and pyrethroid pesticides are considered environmental contaminants, their estrogenic potentials are still ubiquitous and unclear. The present study was undertaken to evaluate the estrogenic activities of nine pesticides (phoxim, malathion, monocrotophos, dimethoate, opunal, fenvalerate, cypermethrin, permethrin, and deltamethrin) using three in vitro methods [E-Screen assay, estrogen receptor (ER) competitive binding assay, and pS2 expression assay]. All the pyrethroid pesticides tested induced MCF-7 cell proliferation significantly, while organophosphorus pesticides did not. The estrogenic potency were ranked as permethrin > fenvalerate > cypermethrin > deltamethrin. The proliferation induced by cypermethrin, permethrin, and deltamethrin was blocked by ICI 182.780, while fenvalerate only partly inhibited it. In addition, pyrethroid pesticides inhibited the binding of [3H]estradiol to ER, while the organophosphorus failed to do so. Fenvalerate, permethrin, and cypermethrin induced pS2 mRNA expression with varying potency, while there were no significant effects in deltamethrin-treated groups. Our findings provide evidence to support the idea that pyrethroid pesticides tested produce an ER-specific, agonist response. Fenvalerate induced MCF-7 cell proliferation by a mechanism not involving ER-mediated pathway. Organophosphorus pesticides tested showed no estrogenic potential. Compared with the pS2 expression assay, E-Screen was a more sensitive and useful assay for screening of the xenoestrogenic chemicals.

Animals↗
PubMed2004

Chronic dietary risk for pesticide residues in food in Brazil: an update.

The objective was to conduct a dietary risk assessment of pesticides registered in Brazil up to 14 January 2004. The theoretical maximum daily intake (TMDI) was calculated for 275 compounds using the Brazilian maximum residue limits (MRL) and food consumption. The chronic dietary risk assessment was conducted by comparing the TMDI with the Brazilian acceptable daily intake (ADI) or, when not available, with the ADI from other sources. The TMDI was higher than the ADI (%ADI>100) in at least one Brazilian region for eight pesticides, including five organophosphorus insecticides. For these compounds, the higher TMDI (expressed as %ADI) ranged from 140 (metam sodium) to 14,000 (methyl bromide). Rice, beans, citrus and tomato were the commodities that contributed most to ingestion. Change in pesticide use patterns and the establishment of ADIs by the Brazilian government have reduced the number of compounds for which the TMDI exceeded the ADI in the last 4 years. Risk assessment methodology based on TMDI calculation, however, is conservative as it assumes that the food supply is always treated with all the registered pesticides for that crop and that one always consumes food containing residues at the tolerance level. Furthermore, for six compounds with TMDI exceeding the ADI, a more realistic estimation of the pesticide daily intake was conducted using monitoring residue data from the Brazilian National Pesticide Residue Program. For these compounds, the higher refined intakes ranged from 2% (dimethoate) to 180% (fenitrothion) of the ADIs. The implementation of a national pesticide residue monitoring programme by the government was important to allow the refinement of the risk assessment. However, adequate daily food consumption data are still needed to assess better the public health risk to Brazilian consumers from food produced from crops treated with pesticides.

Brazil↗
PubMed2005

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

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

Food Analysis↗
PubMed2006

Monitoring of pesticide residues in apples, lettuce and potato of the Slovene origin, 2001-04.

Apples, lettuce and potatoes (404 samples) produced in the Republic of Slovenia were analysed for pesticide residues at the Agricultural Institute of Slovenia, Ljubljana, in 2001-04. Sampling from eight agricultural production areas was performed at market producers at the harvesting of products or in storehouses after the pre-harvest interval of plant protection products used. Samples exceeding the maximum residue levels were the following: three apple samples (2.0%) containing 0.33-2.24 mg kg(-1) (phosalone and tolylfluanid), three lettuce samples (3.1%) containing 0.14-6.36 mg kg(-1) (dimethoate, dithiocarbamates and metalaxyl) and 36 potato samples (23.1%) containing 0.06-0.51 mg kg(-1) (dithiocarbamates). Residues of two or more active substances were found in 73 apple samples (48.3%), of which the maximum residue limit (MRL) was exceeded by three samples (2.0%) with the values ranging from 0.33 to 2.24 mg kg(-1), and nine lettuce samples (9.3%), for which the MRL was exceeded by three samples (3.1%) with values from 0.14 to 6.36 mg kg(-1). In potato samples, only residues of dithiocarbamates or no residues at all were found. Residues of the dithiocarbamate group were the most frequently found, i.e. in 66 apple samples (43.7%), 30 lettuce samples (30.9%) and 38 potato samples (24.4%).

Agriculture↗
PubMedDate not supplied

Determination of methamidophos residues in food remnants.

Over the past 7 years, acute food poisoning arising from the consumption of methamidophos-tainted vegetables has occurred sporadically in Hong Kong. To enable prompt remedial and regulatory actions to be taken, a simple and rapid gas chromatographic method was developed to determine methamidophos residues in food remnants. Samples were homogenized and extracted with acetone. Acetone in the resultant extract was removed by rotary evaporation, leaving behind an aqueous solution. After washing with petroleum ether and addition of sodium sulphate, the aqueous solution was re-extracted with chloroform. The chloroform extract was concentrated to dryness and the residue was reconstituted in absolute ethanol for determination by gas chromatography with flame photometric detection. The method was found to be applicable also to the determination of acephate, dimethoate, omethoate and trichlorfon. Mean recoveries of the five organo-phosphorus pesticides at two fortification levels, viz. 1 mg/kg and 10 mg/kg, ranged from 74 to 113%. Relative standard deviations lay between 1.3 and 6.1%. Method detection limits ranged from 0.02 to 0.04 mg/kg. In 1994, 75 food poisoning cases in Hong Kong were suspected to be related to the consumption of methamidophos-tainted vegetables; 13 food remnants were received for analysis, four of them were found to contain high concentrations of methamidophos.

Chromatography, Gas↗
PubMed2006

Dissipation and leaching of (14)C-monocrotophos in Soil Columns under subtropical climate.

Dissipation and leaching behavior of 14C-monocrotophos was studied for 365 days under field conditions using PVC cylinders. The first set (24 cylinders) was spiked with 1.0 microCi 14C-labeled monocrotophos along with 1.06 mg unlabeled monocrotophos to give a concentration of 2 mg kg -1 in the soil up to 15 cm depth. The second set (24 cylinders) received 14C-labeled monocrotophos along with other non-labeled insecticides viz., dimethoate @ 300 g a.i ha-1, deltamethrin @ 12.5 g a.i ha-1, endosulfan @ 750 g a.i ha-1, cypermethrin @ 60 g a.i ha-1, and triazophos @ 600 g a.i ha-1 at an interval of 15 days each as recommended for the cotton crop. 14C-monocrotophos dissipated faster, up to 45% in first 90 days in columns treated with only monocrotophos compared to 25% in columns that received monocrotophos along with other insecticides. However, both the columns showed similar residues 180 days onward. After 180 days of treatment, 46% radiolabeled residues were observed, which reduced up to 39.6% after 365 days. Leaching of 14C-monocrotophos to 15-30 cm soil layer was observed in both the experimental setups. In the 15-30 cm soil layer of both soil columns, up to 0.19 mg 14C-monocrotophos kg-1d. wt. soil was detected after 270 days.

Adsorption↗
PubMed2006

Application of automated mass spectrometry deconvolution and identification software for pesticide analysis in surface waters.

A new approach to surface water analysis has been investigated in order to enhance the detection of different organic contaminants in Nathan Creek, British Columbia. Water samples from Nathan Creek were prepared by liquid/liquid extraction using dichloromethane (DCM) as an extraction solvent and analyzed by gas chromatography mass spectrometry method in scan mode (GC-MS scan). To increase sensitivity for pesticides detection, acquired scan data were further analyzed by Automated Mass Spectrometry Deconvolution and Identification Software (AMDIS) incorporated into the Agilent Deconvolution Reporting Software (DRS), which also includes mass spectral libraries for 567 pesticides. Extracts were reanalyzed by gas chromatography mass spectrometry single ion monitoring (GC-MS-SIM) to confirm and quantitate detected pesticides. Pesticides: atrazine, dimethoate, diazinone, metalaxyl, myclobutanil, napropamide, oxadiazon, propazine and simazine were detected at three sampling sites on the mainstream of the Nathan Creek. Results of the study are further discussed in terms of detectivity and identification level for each pesticide found. The proposed approach of monitoring pesticides in surface waters enables their detection and identification at trace levels.

Automation↗
PubMed2001

Organic pollutants in surface waters from Portugal using chemometric interpretation.

Surface water samples from 45 sampling points across Portugal have been analyzed monthly by automated Solid Phase Extraction (SPE) and Gas Chromatography-Mass Spectrometry (GC/MS) in SIM and SCAN modes. Sampling was carried out during a period of six months (April-September, 1999), in order to determine the levels of contamination of 72 organic compounds mainly selected from the EC Council Directive list (CEC 76/464/EEC). Atrazine, simazine, deethylatrazine, alachlor, metolachlor, Irgarol, terbuthylazine, tributhylphosphate, 2,4,6-trichlorophenol, 2-chlorophenol, 3-chlorophenol, pentachlorophenol, dimethoate, lindane, linuron, propanil, o,p'-DDD, o,p'-DDT, o,p'-DDE and malathion were the main detected compounds. Although Irgarol, terbuthylazine, deethylatrazine and deisopropylatrazine are not listed in the EC Directive, these herbicides and transformation products are currently in use and they were also included in the monitoring program and detected at some sites. Fifty-nine percent of the samples were below 0.1 microg l(-1), the detection limit required the EEC Drinking Water Directive (DWD). Some compounds were detected at values higher than the DWD, e.g. atrazine (2.7 microg l(-1)) and alachlor (5.43 microg l(-1)) in April. Simazine was also present with a high value (2.3 microg l(-1)) in September. Tributhylphosphate (5.40 microg l(-1)) and 2,4,6-trichlorophenol (2.31 microg l(-1)) were also found at high concentrations near industrial sites. Chemometric interpretation of the more representative contaminants was performed by means of Principal Component Analysis, allowing the resolution of the more relevant contamination sources and the description of their temporal and spatial (geographical) distributions.

Environmental Monitoring↗
PubMed2001

Insecticide residues in cotton crop soil.

Dimethoate, monocrotophos, triazophos, deltamethrin, cypermethrin and endosulfan were applied to a cotton crop soil located at Nurpur village, Punjab, India. The insecticides were applied sequentially at recommended dosages in cotton fields by foliar application in 1995, 1996 and 1998. Soil samples were collected from the cotton crop farms and extracted with acetone. The extracted material was analysed by a gas liquid chromatograph (GLC) equipped with an 63Ni electron-capture detector (ECD-63Ni). Recovery data was obtained by fortifying soil with insecticide. The average recoveries from the fortified soil samples were 76-92% for organophosphorous compounds and 90-98% for synthetic pyrethroids and organochlorines. The results showed that the insecticide residues under study were present in the range of 1.16 to 41.97 ng g(-1) d.wt.soil. The pattern of dissipation of the insecticides used was similar for the duration of the crop. Half lives of the insecticides ranged from 7 to 22 days. Except endosulfan none of the other insecticides used were leached below 15 cm. Endosulfan was found to be rapidly degraded in the soil and formed a sulfate metabolite. Persistence and dissipation pattern in soils with history of exposure to the insecticide compared to non-history soils were similar.

Chromatography, Gas↗