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1.
Two procedures are described for the determination of residues of triadimenol and compared on cereal material. After extraction, purification is carried out by Florisil column chromatography in method I and by semi-preparative High-Performance Liquid Chromatography in method II. Triadimenol residues are quantified by gas chromatography with a thermoionic detector. With method I, interference was observed but not with method II. This specific procedure has been tested on other plant materials. Recoveries in the range of 90–98% indicate that this procedure is suitable for residue analysis of this fungicide with detection limits of 0·008 mg kg?1 in wheat grains, 0·03 mg kg?1 in wheat straw and 0·004–0·008 mg kg?1 in other plants. Maximum residue limits in France are: 0·1 mg kg?1 in grain, 2·0 mg kg?1 in straw and 1·0 mg kg?1 in other vegetables and fruit.  相似文献   

2.
In order to obtain residue data from the application of the algicide endothal in Italian rice paddy fields, two experiments were carried out using a 50 g kg?1 granular formulation in a small pond and the same granular and two liquid formulations in actual paddy fields of the Italian rice growing area. Endothal decay in the pond water was very rapid, reaching residue levels of 0·01-1·02 mg litre?1 in two days and 0·004-0·01 mg litre?1 at the third day. The muddy soil of the pond was free from measurable endothal residues( <0·02 mg kg?1). In the paddy-field waters, the endothal decay was slower, with an average half-life time of 3·3 days, independently of the type of formulation. The actual residues in water after 6 days ranged from 0·3 to 1·3 mg litre?1 according to the initial amount of product applied, and, consequently, to the initial concentration in water. Rice samples collected at the normal harvest time from the two paddy fields, treated with three different formulations, showed no endothal residue at the minimum detectable level of 0·01 mg kg?1.  相似文献   

3.
Alternaria species, mostly A. alternata, have occasionally been found in some years on olive samples collected in Puglia (southern Italy). A survey was consequently made on the occurrence of the major Alternaria mycotoxins, i.e. alternariol (AOH), alternariol methyl ether (AME), altenuene (ALT), altertoxin-I (ATX-I), and tenuazonic acid (TA) in olives and products of their processing (oil and husks). The toxigenicity of Alternaria strains isolated from olives, and the possible transfer of mycotoxins into the oil, were also investigated. Four out of 13 olive samples were contaminated by 2–4 Alternaria mycotoxins. The highest contamination was found in a badly damaged sample containing 2.9, 2.3, 1.4 and 0.3 mg kg?1 of AME, AOH, ALT and ATX-I, respectively. No mycotoxins were detected in olive oil destined for human consumption (6 samples) or olive husks (3 samples) collected from oil-mills after the first pressing of olives. An oil sample produced in our laboratory by processing the most contaminated olive sample, contained AOH (0.79 mg kg?1) and AME (0.29 mg kg?1). The estimated amount of mycotoxin transferred into the oil was 4%, for AME, 1.8% for AOH, and zero for ALT and TA (considering oil yield as 15%). The A. alternata strains isolated from olive produced much more mycotoxins when cultured on rice (up to 3 orders of magnitude for TA) than on olive.  相似文献   

4.
The dissipation of mecoprop in wheat (Triticum aestivum L.) and oat (Avena sativa L.) was monitored over a growing season following post-emergence application of the dimethylamine salt of mecoprop to each crop at 1·1 kg ha?1. Residues of mecoprop, as its methyl ester, were determined gas chromatographically using electrolytic conductivity detection. Initial residues in wheat (119 (±20) mg kg?1) and oat (95·3 (± 10·0) mg kg?1) on the day of application (four-leaf stage of wheat and four- to five-leaf stage of oat) decreased to 0·1 to 0·2 mg kg?1, respectively, within six weeks. Residues were non-detectable in the mature seed of both crops. Recoveries of mecoprop were in the order of 90% from the green tissue and seed of both crops fortified at 0·05 mg kg?1.  相似文献   

5.
The depletion of zeta‐cypermethrin residues in bovine tissues and milk was studied. Beef cattle were treated three times at 3‐week intervals with 1 ml 10 kg?1 body weight of a 25 g litre?1 or 50 g litre?1 pour‐on formulation (2.5 and 5.0 mg zeta‐cypermethrin kg?1 body weight) or 100 mg kg?1 spray to simulate a likely worst‐case treatment regime. Friesian and Jersey dairy cows were treated once with 2.5 mg zeta‐cypermethrin kg?1 in a pour‐on formulation. Muscle, liver and kidney residue concentrations were generally less than the limit of detection (LOD = 0.01 mg kg?1). Residues in renal‐fat and back‐fat samples from animals treated with 2.5 mg kg?1 all exceeded the limit of quantitation (LOQ = 0.05 mg kg?1), peaking at 10 days after treatment. Only two of five kidney fat samples were above the LOQ after 34 days, but none of the back‐fat samples exceeded the LOQ at 28 days after treatment. Following spray treatments, fat residues were detectable in some animals but were below the LOQ at all sampling intervals. Zeta‐cypermethrin was quantifiable (LOQ = 0.01 mg kg?1) in only one whole‐milk sample from the Friesian cows (0.015 mg kg?1, 2 days after treatment). In whole milk from Jersey cows, the mean concentration of zeta‐cypermethrin peaked 1 day after treatment, at 0.015 mg kg?1, and the highest individual sample concentration was 0.025 mg kg?1 at 3 days after treatment. Residues in milk were not quantifiable beginning 4 days after treatment. The mean concentrations of zeta‐cypermethrin in milk fat from Friesian and Jersey cows peaked two days after treatment at 0.197 mg kg?1 and 0.377 mg kg?1, respectively, and the highest individual sample concentrations were 2 days after treatment at 0.47 mg kg?1 and 0.98 mg kg?1, respectively. © 2001 Society of Chemical Industry  相似文献   

6.
Laboratory studies were conducted to determine the effect of the naturally derived compound spinosad on Ceratitis capitata Wied. (Diptera, Tephritidae). The organophosphate fenthion was used as a standard. Direct dose-dependent mortality and reduced fecundity were observed in oral treatment of adults with spinosad. The LC90 values 14 h and seven days after treatment were 19·50 and 0·49 mg litre−1 respectively. Fenthion was less active (the LC50 eight days after treatment was 1·17 mg litre−1) and did not affect the fecundity of the fly. Adults were also very susceptible to spinosad and fenthion via residual contact. For spinosad, 100% mortality was recorded 48 h after treatment for a dose of 10 mg litre−1. Spinosad was more effective than fenthion in suppressing larval development when neonate larvae were reared on treated diet supplemented with a range of concentrations from 0·02 to 0·83 mg kg−1 diet. Last-instar larvae were much less susceptible to spinosad or fenthion when exposed via dipping or when they pupated in treated medium and both products had similar performance. A lack of ovicidal activity was observed in direct egg-treatments with spinosad but significant reductions from 1 mg litre−1 onwards were recorded for fenthion.  相似文献   

7.
A study was carried out to assess the feasibility of monitoring the exposure of barn owls (Tyto alba) to an anticoagulant rodenticide, flocoumafen, by analysis of residues in regurgitated pellets following consumption of flocoumafen-contaminated mice. Mice were fed on a diet containing [14C]flocoumafen, equivalent to 12 mg kg?1, and killed 24 h later. A single [14C]flocoumafen-contaminated mouse was fed to each of four captive barn owls, equivalent to 0·11-0·23 mg kg?1 per bird, followed on seven successive days by control diet (i.e. undosed mice). The [14C]flocoumafen dose was eliminated by the owls over the eight-day period in pellets (44%, range 35–55%) and faeces (18%, range 11–21%), with the highest residues being observed in samples from the first 24-h period. Further detailed analysis of the pellets confirmed that flocoumafen residues in the first-day pellets represented 15% (range 8–26%) of the original flocoumafen residues ingested by the barn owls. Calculations based on these data and typical flocoumafen residues in live captured rodents (following baiting) confirm that pellet residue analysis is a sensitive and appropriate method for the non-invasive monitoring of exposure of barn owls to flocoumafen. There were no symptoms of anticoagulant poisoning in any of the birds; two of the birds were successfully paired the next season and produced fledgelings.  相似文献   

8.
A goat was dosed orally with [14C]tefluthrin, twice daily for 4 days, at a rate equivalent to 10.9 mg kg?1 in its diet. Within 16 h of the final dose, 70.1% of the dose had been excreted (urine 41.4%, faeces 28.7%). Extensive metabolism occurred in the goat by ester cleavage and oxidation at a variety of positions on the molecule. Low radioactive residues were detected in the milk (0.076 mg kg?1), fat (0.076 mg kg?1) and muscle (0.016 mg kg?1), with tefluthrin as the largest individual component of the residue (milk 66.5%, fat 76.7%, muscle 34.2%). Higher residues were present in the kidney (0.3 mg kg?1) and liver (1.0 mg kg?1) and only a small percentage of this residue was due to tefluthrin (kidney 3.4%, liver 6.1%). The remainder of the residue in the kidney and liver was a complex mixture of metabolites. Most of the kidney metabolites were identified, but a high proportion of the liver residue was due to six unidentified polar compounds.  相似文献   

9.
Strawberries were sprayed with solutions of 200, 300 and 500 mg dimethoate litre?1 and analysed for dimethoate residues up to 21 days after the final spraying. The residues were found to be below the National Health and Medical Research Council limit of 2 mg kg?1, 1, 2 and 4 days after spraying. Consequently, the withholding period of 7 days could be reduced to 3 days to allow uninterrupted picking of the ripe strawberry crop.  相似文献   

10.
Foliar applications of synthetic pyrethroids were made to several crops to determine residue levels at various intervals after application. On onions, residues of cypermethrin, permethrin and fenvalerate were negligible > 0.1 mg kg?1, 7 days after application. On lettuce, residues of fenvalerate and permethrin were 0.8 mg kg?1. On celery, residues of fenvalerate did not decline and ranged from 0.12 to 0.25 mg kg?1 during the 14-day period. On green bush-beans, residues of permethrin and cypermethrin did not decline during the 14-day period and ranged from 0.1 to 0.6 mg kg?1. By day 7, residues of cyfluthrin, cypermethrin, deltamethrin, fenvalerate and permethrin on strawberries were less than the acceptable maximum tolerance of 0.1 mg kg?1 with the exception of cypermethrin, applied at the rate of 0.14 kg a.i. ha?1 which gave a residue of 0.14 mg kg?1.  相似文献   

11.
In a dietary toxicity study, laying hens received a diet containing the rodenticide flocoumafen at concentrations of 1.5, 5, 10 and 50 mg kg?1 for five consecutive days. The LC50 at termination following a 28-day observation period was 16.4 mg kg?1. Livers of birds which received doses of flocoumafen between 5 and 50 mg kg?1 had concentrations of flocoumafen (1.5 nmol g?1) that were independent of dose. The data indicate the presence in hen liver of a saturable high-affinity flocoumafen binding site with similar characteristics and capacity to that of the quail and rat. Residues of flocoumafen in samples of breast and leg muscle were low in all exposure groups. Higher, dose-related residues were found in samples of abdominal fat and skin-associated fat and there was a clear demonstration of the transfer of dose-related residues into eggs. In a separate study in which hens were dosed with [14C]flocoumafen for five consecutive days at a daily rate of 1 and 4 mg kg?1 body weight, the majority (68 %) of the daily radioactive dose was eliminated over the following 24 hours via excreta. Residues in liver at death or when killed accounted for < 1 % of the cumulative administered radioactivity. Residues in eggs were located primarily in the yolk with maximum concentrations 1.0 mg kg?1 or 0.18% of the low dose; 2.1 mg kg?1 or 0.06% of the high dose as [14C]flocoumafen equivalents were observed at 10 days after start of dosing. Some 40 % of the total activity in the yolk was unchanged flocoumafen.  相似文献   

12.
BACKGROUND: The purpose of this work was to determine residues of acaricides in recycled Spanish beeswax. RESULTS: Chlorfenvinphos, fluvalinate, amitraz, bromopropylate, acrinathrin, flumethrin, coumaphos, chlorpyrifos, chlordimeform, endosulfan and malathion residues were determined by GC‐µECD/NPD/MS detection. Owing to the extreme instability of amitraz, this analyte was transformed into the stable end‐metabolite 2,4‐dimethylaniline, later derivatised with heptafluorobutyric anhydride and determined by GC‐µECD/MS. Recoveries from spiked samples ranged from 86 to 108%, while quantification limits varied from 0.10 to 0.30 mg kg?1 using GC‐µECD/NPD, and from 12 to 85 µg kg?1 by GC‐MSD. Of a total of 197 samples analysed, only eight samples (4%) were free of residues of chlorfenvinphos (0.019–10.6 mg kg?1), fluvalinate was present in 93.6% of samples analysed (0.027 –88.7 mg kg?1), while coumaphos was confirmed in only five of the 134 samples analysed at concentrations of less than 195 µg kg?1. The remaining acaricides were identified with different levels of incidence at concentrations from 12 to 231 µg kg?1. CONCLUSIONS: Residues of acaricides were found in an extensive number of beeswax samples. The contamination with chlorfenvinphos and tau‐fluvalinate was very relevant, particularly as chlorfenvinphos is not legally authorised for use in beekeeping. The possible impacts of the main acaricides detected on larval and adult honey bees are discussed. Copyright © 2010 Society of Chemical Industry  相似文献   

13.
Blackcurrants, treated with 0.1 kg of 2,4,5-T ha?1 (as esters of mixed C4–C6 alcohols; ‘Tormona 80’), contained 0.1 mg of 2,4,5-T residues kg?1 in the berries at ripeness 29 days after treatment. Total residues in the berries were not reduced during growth and ripening, although the residue concentrations declined in the same period due to growth dilution. In spinach leaves from old plants, treated with 0.1 kg ha?1, 0.05 mg of 2,4,5-T kg?1 was found 14 days after treatment. Fodder peas showed no residues (< 0.002 mg kg?1) at harvest 62 days after treatment with 2,4,5-T esters. After application of 0.1 kg ha?1 on potato plants, the disappearance of 2,4,5-T was rapid during the first month, but residues were translocated into the tubers and reached a constant level of 0.02 mg kg?1 after 1 month until harvest at 108 days after treatment. In all crops, visible effects were observed after treatment with 0.1 kg ha?1. After the application at 0.01 kg ha?1, phytotoxic effects were observed only in blackcurrants, but negligible residues were found in all the test crops.  相似文献   

14.
The persistence of cyproconazole and quinalphos on/in grapes was investigated when both compounds were applied to vines at the locally recommended application frequencies and rates and at double these rates, using commercially available formulations. Residues of cyproconazole applied at recommended and double the recommended rates of application in/on grapes immediately after the last application were 0-049 (±0.034) and 0.077 (±0.008) mg kg?1, respectively, reduced to 0.011 (±0.003) and 0.018 (±0.010) mg kg?1 respectively seven days after the last application. The corresponding residue levels of quinalphos immediately following the last application were 1.42 (±0.10) and 3.36 (±0.07) mg kg?1, reduced to 0.043 (±0.002) and 0.072 (±0.028) mg kg?1 respectively 21 days after the last application. Cyproconazole, being systemic, is rapidly absorbed by the grape tissues and its residues dissipate with a half-life of three to four days, while quinalphos, being non-systemic, dissipates faster with a half-life of two or three days. The residues of both pesticides were analysed by a GLC-NPD system.  相似文献   

15.
Residues of endosulfan insecticide (α- and β-isomers, and ‘endosulfan sulphate’) in fish and their predators were measured during and after operations to control tsetse fly in the Okavango Delta, Botswana. Six ultra-low-volume doses of endosulfan 35% e.c. (6–12 g a.i. ha?1) were applied from the air in a period of 12 weeks over 2500 km2. The concentration of residues found in living fish was up to 0.19 mg kg?1 wet wt in caudal muscle, and usually < 0.8 mg kg?1 wet wt in pooled viscera (maximum 2.8 mg kg?1). These values returned to near-normal within 3 months after cessation of spraying, but residues were still detectable after 12 months. By comparison, fish killed by spraying contained a maximum residue level (whole-body) of 1.5 mg kg?1 wet wt. The residue level in fish was approximately proportional to their fat content. Lean fish were more susceptible to poisoning than fat fish. The proportion of the ‘endosulfan sulphate’ metabolite in fish increased at least six times with respect to the parent isomers (α+β) during the period of spraying, but more advanced stages of metabolic breakdown were not monitored. Residue levels in fish predators (fish-eating birds and crocodiles) were similar to those in their prey, and the risk to them was consequently low.  相似文献   

16.
In a greenhouse metabolism study, sunflowers were seed‐treated with radiolabelled imidacloprid in a 700 g kg?1 WS formulation (Gaucho® WS 70) at 0.7 mg AI per seed, and the nature of the resulting residues in nectar and pollen was determined. Only the parent compound and no metabolites were detected in nectar and pollen of these seed‐treated sunflower plants (limit of detection <0.001 mg kg?1). In standard LD50 laboratory tests, imidacloprid showed high oral toxicity to honeybees (Apis mellifera), with LD50 values between 3.7 and 40.9 ng per bee, corresponding to a lethal food concentration between 0.14 and 1.57 mg kg?1. The residue level of imidacloprid in nectar and pollen of seed‐treated sunflower plants in the field was negligible. Under field‐growing conditions no residues were detected (limit of detection: 0.0015 mg kg?1) in either nectar or pollen. There were also no detectable residues in nectar and pollen of sunflowers planted as a succeeding crop in soils which previously had been cropped with imidacloprid seed‐treated plants. Chronic feeding experiments with sunflower honey fortified with 0.002, 0.005, 0.010 and 0.020 mg kg?1 imidacloprid were conducted to assess potential long‐term adverse effects on honeybee colonies. Testing end‐points in this 39‐day feeding study were mortality, feeding activity, wax/comb production, breeding performance and colony vitality. Even at the highest test concentration, imidacloprid showed no adverse effects on the development of the exposed bee colonies. This no‐adverse‐effect concentration of 0.020 mg kg?1 compares with a field residue level of less than 0.0015 mg kg?1 ( = limit of detection in the field residue studies) which clearly shows that a sunflower seed dressing with imidacloprid poses no risk to honeybees. This conclusion is confirmed by observations made in more than 10 field studies and several tunnel tests. © 2001 Society of Chemical Industry  相似文献   

17.
Determination of sugarbeet herbicides such as chloridazon, metamitron and phenmedipham in soil samples is described. After extraction with acetone, pesticides were determined by HPLC on an RP-18 column using methanol/water as mobile phase. Average recoveries were 82% for chloridazon, 93% for metamitron and 77% for phenmedipham. Quantification limits were 3·5 μg kg?1 for chloridazon, 6·3 μg kg?1 for metamitron and 3·6 μg kg?1 for phenmedipham.  相似文献   

18.
The long-term fate of the acaricide, fenbutatin oxide, in soil has been investigated. Residues of the compound and its two principal metabolites have been determined in soil samples obtained from citrus orchards in Italy and Spain where the product had been applied commercially over a period of 6–10 years. The average fenbutatin oxide content in the upper 0–15 cm soil layer ranged from ? 1 mg kg?1 to 5 mg kg?1 in sites receiving single and double applications per year. The residues were located primarily (> 95%) in the top 0–30 cm layer and there was virtually no movement of the compound through the soil to lower depths. Below 0.5 m depths, the sites contained average concentrations of ? 0.01 mg kg?1, the limit of determination. No significant build-up of residues was observed and the data indicate an approximate half-life in soil of just less than one year. Residues of the two metabolites, dihydroxy-bis(2-methyl-2-phenylpropyl)stan-nane and 2-methyl-2-phenylpropyl stannonic acid, were on average 11% and 16% of the fenbutatin oxide concentration, respectively. As with fenbutatin oxide, there was no significant movement through the soil to lower levels.  相似文献   

19.
The effect of the ecdysone agonists RH-2485 (proposed name methoxyfenozide) and tebufenozide (RH-5992), was examined on eggs and larvae of the southwestern corn borer, Diatraea grandiosella Dyar. Both compounds exhibited a concentration-dependent ovicidal activity. More than 95% of eggs died when egg masses were dipped in solutions of 100 or 200 mg liter-1 of either compound in acetone+distilled water (1+1 by volume). Although some eggs treated with 1 or 10 mg liter-1 of the compounds hatched, the survival rate was low. Newly hatched larvae were fed for seven days on an artificial diet containing RH-2485 or tebufenozide. The LC50 values were 0·049 mg kg-1 for RH-2485 and 0·185 mg kg-1 for tebufenozide, showing that RH-2485 was about four times more active than was tebufenozide. Although increasing the time of exposure to either compound decreased the LC50 value significantly, the relative potency of RH-2485 versus tebufenozide was not changed. Newly ecdysed 4th-instar larvae fed with diets containing 0·125, 0·25 or 0·5 mg kg-1 RH-2485 or tebufenozide ceased feeding approximately 8 h after exposure, indicating that larvae had prematurely entered a molting cycle. Larvae treated with RH-2485 ecdysed earlier and died more quickly than those treated with tebufenozide. Ingestion of sublethal concentrations of RH-2485 (0·005 and 0·01 mg kg-1) or tebufenozide (0·03 and 0·06 mg kg-1) retarded larval growth, and decreased pupal weight and adult emergence. Increasing exposure time to tebufenozide tended to increase the larval mortality, significantly retarded larval growth, and decreased the mean weights of male and female pupae and adult emergence. RH-2485 (0·125 and 0·25 mg kg-1) and tebufenozide (0·25 and 0·5 mg kg-1) were lethal to newly hatched larvae, even after diets containing these compounds were held for 20 days at 30°C under long days (16 h light: 8 h dark). Our results suggest that field trials to assess the potential of RH-2485 and tebufenozide to control D. grandiosella are warranted. © 1998 SCI  相似文献   

20.
Following experimental and commercial applications to soil of a granular formulalation of phorate (O,O-diethyl S-ethylthiomethyl phosphorodithioate), residues in the soil and in lettuce were determined by gas-liquid chromatography. When applied by the bow-wave method as a continuous logarithmically-changing dose ranging from approximately 0.9 to 16.0 kg a.i. ha?1, the proportional rate of oxidation in soil of phorate sulphoxide to phorate sulphone was inversely related to dose. Ten weeks after application, total phorate residues in the soil had declined by about 35% at all dose levels. Residues in mature lettuce, from the 1-5 kg ha?1 dose-range, comprised the parent and oxygen analogue sulphoxides and sulphones; the relative proportions of the individual metabolites were independent of dose. Over this dose-range, total residue concentrations in the crop became proportionally slightly greater with increasing dose. When single doses of 1.1, 2.0 or 2.2 kg a.i. ha?1 were applied at drilling, the total residue concentrations in the lettuce declined from 5 mg kg?1 in seedlings from some treatments to <0.05 mg kg?1 at harvest. In plants raised in peat blocks containing 10 or 20 mg a.i. per block, however, residues in seedlings totalled 45-47 mg kg?1 and declined to only 0.7 mg kg?1 at harvest. It was concluded that bowwave applications of phorate when field-sowing lettuce were unlikely to lead to unacceptable residues in the harvested crop, but that residues in lettuce raised in phorate-treated peat blocks may be unacceptably high.  相似文献   

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