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[Organochlorine residues in eggs of night heron breeding in Yuantouzhu, Wuxi and their functions as bioindicator].

This study analyzed chlorinated pesticides in eggs of night heron breeding in Yuantouzhu, Tai lake. The HCH isomers, DDT, DDD, DDE, endrine and heptachlor epoxide were detected out in egg samples. The residue level and the percent of detection of beta-HCH and p,p'-DDE were significantly high. The mean value of p,p'-DDE was 0.906 microgram/g dry weight. Most of the chlorinated pesticides in samples from Wuxi were higher than those of Gongqing city, Jiangxi province. Oppositely, the hatching rate of night heron egg in Wuxi region was lower than that in Gongqing city. It may be related to the difference of DDE residual levels. Using organochlorine residue in eggs of water-fowls as an indicator for environmental quality assessment is feasible.

Animals↗

Nationwide residues of organochlorine compounds in wings of adult mallards and black ducks, 1976-77.

Organochlorine residues in wings of adult mallards and black ducks were monitored nationwide during the 1976-77 hunting season. DDE was found in all samples. Levels were unchanged since the 1972-73 collections in all migratory routes except the Pacific Flyway, in which residue levels declined significantly. Dieldrin levels had not changed in any flyway and residues remained low. PCB levels declined significantly in the Atlantic Flyway but remained stable in other flyways. Heptachlor epoxide, mirex, endrin, hexachlorobenzene, and chlordane isomers were detected in low amounts in some samples.

Animals↗

[Supercritical fluid extraction and gas chromatographic analysis of four organochlorine pesticides in vegetable].

Supercritical fluid extraction(SFE) of pesticide residues of chlorothalonil, aldrin, dieldrin, and endrin from chives was evaluated. A mixture of vegetable sample: anhydrous magnesium sulfate(2:3) was used for extraction. The extract was analyzed by GC/ECD. The optimum SFE conditions for the pesticides in spiked samples were studied by orthogonal experiment. The chosen conditions were 30.40 MPa, 40 degrees C, 1 min static time, dynamic extraction with 15 mL of CO2, and collection in 3 mL of ethyl acetate. All the pesticides were extracted satisfactorily from their matrix.

Chive↗

[Bioindication of organochlorine pesticides by night heron in Taihu wetland ecosystem].

Based on field ecological investigation on the colony of herons in Yuantouzhu of Taihu in 1999, the regurgitated foods by chicks of night heron were collected for prey type identification and chemical analysis. Besides, eggs of night heron, and sediments and waters in foraging habitats were sampled for chemical analysis as well. alpha-HCH, beta-HCH, gamma-HCH, Aldrin, Dieldrin, Endrin, Heptachlor, Heptachlor epoxide, p,p'-DDE, p,p'-DDD, o,p'-DDT and p,p'-DDT were determined in laboratory by gas chromatography. The results indicated that HCH isomers, DDT and its metabolites could be detected in various environments and preys of night heron, although the organochlorined chemicals were banned for almost 20 years. Moreover, The results showed that eggs of night heron could accumulate organochlorine pesticides by as much as a factor of 10(3)-10(4), which can make chemical analysis much easier. So they are good bio-indicators for organochlorine contamination level in wetland environments.

China↗

[Microwave extraction technique].

A new microwave aided extraction (MAE) technique is introduced in this paper. It gives the extraction method as well as reagents, equipment and conditions used in the technique. In temperature controlled pressurized vessels, polar solvent (eg. acetone) and the combinations of polar and non-polar solvents can be heated to approximately 100 degrees C above their normal boiling points. It is told that the higher the extraction temperature the more the recovery is. The ratio of polar to non-polar solvents affects not only the microwave heating rate but also the extraction recovery. The highest recovery ratios are gotten at the solvent ratio of three parts of acetone to two parts of hexane. We can see from the pesticides chromatogram with MAE, that very little break-down of endrin or DDT are detected and they are well below the EPA specified tolerance limits. We can find from the comparison of MAE with sonication and Soxhlet extraction techniques that microwave extraction technique has not only higher average recoveries (%) but also good precision (RSD, %). The data and comparison results illustrate that the microwave extraction is a rapid method (about 15 minutes) with less solvent consumption (about 30-50 mL), good recovery, and easy to be controlled automatically in comparison with the Soxhlet extraction, sonication and other extraction methods.

Chemical Fractionation↗

[Simultaneous determination of 25 persistent organic pollutants in rice by gas chromatography-mass spectrometry with selected ion monitoring mode].

A multi-residue analytical method for the simultaneous determination of persistent organic pollutants (POPs) in rice samples was developed. POPs were extracted from rice with ethyl acetate/n-hexane (80:20, v/v) by sonication, and determined by gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode. A fused silica capillary column DB-35MS (30 m x 0.25 mm i.d. x 0.25 microm) was employed. Operating conditions were as follows: injector port temperature, 300 degrees C; column temperature, programming; carrier gas, helium; flow rate, 1.0 mL/min; sample size, 1 microL with splitless injection. The mass spectrometric detector (MSD) was operated in electron impact ionization mode with an ionizing energy of 70 eV. Analysis was performed with selected ion monitoring (SIM) using one target and one or two qualifier ion. POPs were confirmed by their retention times, their qualifier and target ions, and their qualifier/target abundance ratios. Recovery studies were performed at 0.05, 0.1, and 0.5 mg/L spiked levels of each POPs, and the recoveries obtained ranged from 81.99% to 100.60% with relative standard deviations between 2.37% and 18.48%. The detection limits of the method ranged from 0.1 to 5 ng/g for the different POPs except endrin, trans-chlordane and cis-chlordane. The results show that the method developed is sensitive and reliable.

Chlordan↗

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

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.

Capillary Electrochromatography↗

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

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

Butter↗

Pesticide/herbicide pollutants in the Kafue River and a preliminary investigation into their biological effect through catalase levels in fish.

The study determined the types of pesticide/herbicide pollutants in water, sediment and fish from the Kafue River. A preliminary investigation of the oxidative stress from these pesticides/herbicides was also assessed by measurement of catalase activity. Water, sediment and fish samples were collected upstream, midstream and downstream the Kafue river in Chingola, Kitwe, Kafue National Park and Kafue Town. Water, sediment and fish muscle were sampled and analysed for pesticides using Gas chromatography. For catalase activity fish liver samples only were examined. The pesticides/herbicides detected in all samples collectively included: Heptachlor, pp'-DDE, Cypermethrin, Chlordane, Toxaphene, Terbufos, Kelthane, Endosulfan, Dieldrin, pp'-DDD, pp'-DDT, Atrazine, Disulfoton, d-trans-Allethrin and Endrin. On the other hand, catalase activity was detected in all fish liver samples from all sites. Its levels increased significantly from Chingola upstream to sites downstream with highest being in Kafue town. This study therefore, demonstrates that there is widespread contamination of the Kafue River with pesticides/ herbicides. It also demonstrates that organochlorides are found throughout the river especially in fish samples. The spectrum of pesticides/herbicides was much wider in fish probably due to bioaccumulation. It was also observed that fish are subjected to oxidative stress as determined by catalase levels. The stress is more pronounced downstream where the catalase levels were significantly higher than Chingola. The observation that more pesticide varieties are also found downstream may suggest a likely causative effect of the pesticides on oxidative stress although this needs further investigation. This study further tentatively highlights the potential dangers of these agro-related substances to dependants of the Kafue River water body and the need to carry out risk assessments and thereafter institute corrective measures to help reduce contamination and adverse effects.

Animals↗

Biological monitoring of organochlorides using the limnic bivalves Anodontites trapesialis (Lam., 1819).

The mussel Anodontites trapesialis (Lam, 1819) was used as an indicator of organochloride pollutants in the Canoas River, located in the municipality of Mococa (21 degrees 25'08''S and 47 degrees W), State of São Paulo, Brazil. Biological monitoring was performed for one year at the site of an orange grove on the left bank of the river. Forty-five animals were placed in aluminum enclosures on the river bottom at this site and 4 animals were sacrificed for pesticide analysis at 3-month intervals, each corresponding to one season of the year. Pesticides were extracted by the method of Bedford et al., (1968), modified, and the analyses were performed by gas phase chromatography equipped with an electron capture detector. The animals were found to have been exposed to DDT, Lindane and Heptachlor. Variation in Aldrin and Dieldrin levels was not significant enough to permit inferences. Endrin was not detected in any of the analyses.

Animals↗

Matrix solid phase dispersion (MSPD) extraction and gas chromatographic screening of nine chlorinated pesticides in beef fat.

A multiresidue technique is presented for the extraction and quantitative gas chromatographic screening of 9 insecticides (lindane, heptachlor, aldrin, heptachlor epoxide, p,p'-DDE, dieldrin, endrin, p,p'-TDE, and p,p'-DDT) as residues in beef fat. Beef fat was fortified by adding the 9 insecticides, plus dibutyl chlorendate as internal standard, to 0.5 g portions of beef fat and blending with 2 g C18 (octadecylsilyl)-derivatized silica. The C18/fat matrix blend was fashioned into a column by adding the blend to a 10 mL syringe barrel containing 2 g activated Florisil. The insecticides were then eluted from the column with 8 mL acetonitrile, and a 2 microL portion of the acetonitrile eluate was then directly analyzed by gas chromatography with electron capture detection. Unfortified blank controls were treated similarly. The acetonitrile eluate contained all of the pesticide analytes (31.25-500 ng/g) and was free of interfering co-extractants. Correlation coefficients for the 9 extracted pesticide standard curves (linear regression analysis, n = 5) ranged from 0.9969 (+/- 0.0021) to 0.9999 (+/- 0.0001). Average relative percentage recoveries (85 +/- 3.4% to 102 +/- 5.0%, n = 25 for each insecticide), inter-assay variability (6.0 +/- 1.0% to 14.0 +/- 6.7%, n = 25 for each insecticide), and intra-assay variability (2.5-5.1% n = 5 for each insecticide) indicated that the methodology is acceptable for the extraction, determination, and screening of these residues in beef fat.

Animals↗

Multiresidue matrix solid phase dispersion (MSPD) extraction and gas chromatographic screening of nine chlorinated pesticides in catfish (Ictalurus punctatus) muscle tissue.

A multiresidue technique for extraction and gas chromatographic screening of 9 insecticide (lindane, heptachlor, aldrin, heptachlor epoxide, p,p'-DDE, dieldrin, endrin, p,p'-TDE, and p,p'-DDT) residues in catfish (Ictalurus punctatus) muscle tissue is presented. The 9 insecticides, plus dibutyl chlorendate internal standard, were fortified into catfish muscle tissue (0.5 g) and blended with 2 g C18 (octadecylsilyl derivatized silica reverse-phase material). The C18/muscle tissue matrix blend was fashioned into a column by adding the blend to a 10 mL syringe barrel containing 2 g activated Florisil. The insecticides were then eluted from the column with acetonitrile (8 mL), and a portion (2 microL) of the acetonitrile eluate was then directly analyzed by gas chromatography with electron capture detection. Unfortified blank controls were treated similarly. The resultant extracts contained pesticide analytes (31.25-500 ng/g) free of interfering compounds when analyzed. Correlation coefficients for the 9 extracted pesticide standard curves (linear regression analysis, n = 5) ranged from 0.9967 (+/- 0.0018) to 0.9999 (+/- 0.0001). Average percentage recoveries (82 +/- 4.8% to 97 +/- 3.6%, n = 25 for each insecticide), interassay (5.0 +/- 2.7% to 16.9 +/- 6.5%, n = 25 for each insecticide) and intraassay (1.8 to 4.7%, n = 5 for each insecticide) variabilities were indicative of an acceptable methodology for the analysis and screening of these residues in catfish muscle tissue.

Animals↗

Inhibition of gamma-aminobutyric acid-stimulated chloride flux in mouse brain vesicles by polychlorocycloalkane and pyrethroid insecticides.

Selected polychlorocycloalkane and pyrethroid insecticides were evaluated as inhibitors of gamma-aminobutyric acid (GABA)-dependent chloride flux into mouse brain vesicles. The inhibitory potencies of the polychlorocycloalkane insecticides, measured as concentrations producing 50% inhibition, spanned a 1200-fold concentration range in the following order of decreasing potency: 12-ketoendrin; isobenzan; endrin; dieldrin; heptachlor epoxide; aldrin; heptachlor; and lindane. For the cyclodienes, inhibition of chloride uptake was closely correlated with both mammalian toxicity and the ability to displace the binding of [35S]t-butylbicyclophosphorothionate (TBPS). However, lindane was much less potent as an inhibitor of GABA-dependent chloride uptake than would be expected from its acute toxicity or potency as an inhibitor of [35S]TBPS binding. Mirex and chlordecone were poor inhibitors of GABA-dependent chloride uptake, indicating that other sites are likely to be involved in their toxic action. The pyrethroid insecticide deltamethrin gave 50% inhibition of GABA-dependent chloride uptake at 25 microM, but the extent of inhibition was not increased at higher concentrations. In addition, the nontoxic enantiomer of deltamethrin produced dose-dependent inhibition in the chloride flux assay with a potency about 10-fold less than deltamethrin. These results demonstrate the utility of this functional assay to identify compounds that act at the GABAA receptor-ionophore complex and implicate this complex as the principal site of neurotoxic action for cyclodiene insecticides. Although lindane and deltamethrin also altered GABAA receptor-ionophore function, their low potencies and the incomplete stereospecificity of deltamethrin inhibition suggest that this complex is not involved in the neurotoxic action of lindane and alpha-cyano-substituted pyrethroids.

Animals↗

Sulfuric acid cleanup and KOH-ethanol treatment for confirmation of organochlorine pesticides and polychlorinated biphenyls: application to wastewater samples.

The efficacy of sulfuric acid cleanup and KOH-ethanol hydrolysis confirmation was studied for 22 organochlorine pesticides and 2 polychlorinated biphenyls (PCBs). Mean recoveries for different treatment times are given. The method was applied to analysis of several wastewater samples by gas chromatography with electron capture detection. Organochlorine compounds were extracted by using separatory funnels and 15% diethyl ether in hexane as extractant. All the compounds studied could be analyzed except trifluralin, dichloran, dieldrin, and endrin, which were destroyed after treatment with concentrated H2SO4. The pesticides found most commonly in the samples analyzed were fenson, tetradifon, lindane, methoxychlor, and dicofol.

Chromatography, Gas↗

Multiresidue gas chromatographic method for determining organochlorine pesticides in meats: validation study for swine and beef fats.

A validation of a previously studied method for determining organochlorine residues in poultry fat was conducted to extend the usefulness of the method to beef and swine fats. The validation samples consisted of 16 materials all analyzed in duplicate. Fortification levels ranged from 0.02 to 1.2 ppm for alpha-BHC, lindane, cis- and trans-chlordane, octachlor epoxide, o,p'- and p,p'-DDT, p,p'-DDE, p,p'-TDE, hexachlorobenzene, heptachlor epoxide, dieldrin, endrin, methoxychlor, mirex, and toxaphene. The average recovery was 101% with a range of 79-113%, not including toxaphene. The ranges of coefficients of variation were CVo = 0-23.37% and CVx = 3.74-26.19%. The results were comparable to the previous collaborative study of the same method for poultry fat. The extended method has been adopted official first action.

Animals↗

Gas-liquid chromatographic determination of chlorinated norbornene derivatives in fish.

1,2,3,4,7,7-Hexachloro-2,5-norbornadiene (I), 1,2,3,4,5-endo,7,7-heptachloro-2-norbornene (II), and 1,2,3,4,7,7-hexachloro-5,6-endo-epoxy-2-norbornene (III) have been identified as contaminants in Mississippi River fish by combined gas-liquid chromatography (GLC)-mass spectrometry. The method used to determine residues of these compounds, which are associated with production of the pesticide endrin, is similar to the AOAC multiresidue method for chlorinated pesticides. The residues are extracted from the sample with acetonitrile, transferred to petroleum ether, and chromatographed on a Florisil column. Compounds I and II are eluted from the Florisil with petroleum ether and compound III is eluted with ethyl ether-petroleum ether (6 + 94). The concentrated eluates are analyzed by using electron capture GLC. The method provides adequate recoveries of all 3 chlorinated norbornene derivatives and allows quantitation at or below the 0.05 ppm level in fish with a 20 mg sample equivalent injection.

Animals↗

Organochlorine pesticide, PCB, and PBB residues and necropsy data for bald eagles from 29 states--1975-77.

During 1975-77, 168 bald eagles (Haliaeetus leucocephalus) found moribund or dead in 29 states were analyzed for organochlorine pesticides and polychlorinated biphenyls (PCBs); 32 specimens from 13 states were analyzed for polybrominated biphenyls (PBBs). PCBs were present in 166 bald eagle carcasses and DDE was found in 165. TDE and dieldrin were identified in 137 samples, trans-nonachlor in 118, and oxychlordane in 90. Brains of five eagles contained possible lethal levels of dieldrin, and two eagles possibly died of endrin poisoning. Nine eagle livers, analyzed because of suspected lead poisoning, contained high levels of lead. Twenty percent of the eagles died from shooting, the most common cause of death; this cause of death, however, has declined.

Animals↗

Multiresidue gas chromatographic method for determining organochlorine pesticides in poultry fat: collaborative study.

A gas chromatographic electron capture detector method is described for the quantitative determination of organochlorine pesticide residues in poultry fat. The samples are rendered and cleaned up using automated gel permeation chromatography. The collaborative samples consisted of 10 fortified samples and one incurred residue sample, all in duplicate. Fortification levels ranged from 0.15 to 1.0 ppm for alpha-BHC, lindane, cis- and trans-chlordane, octachlor epoxide, o,p' and p,p'-DDT, p,p'-DDE, p,p'-TDE, hexachlorobenzene, heptachlor epoxide, dieldrin, endrin, methoxychlor, mirex, and toxaphene. The average recovery was 91.9% with a range of 81-102%. The ranges of coefficients of variation were: CVo = 3.39-14.79%; CVL = 0-16.6%; and CVx = 5.82-19.0%. The results indicate accuracy and precision comparable to other official methodology. The method has been adopted official first action.

Adipose Tissue↗