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1.
Residues of the herbicide dinoseb were determined gas chromatographically in lentils which had been treated at two locations in Saskatchewan with post-emergence applications of dinoseb at 1.4 and 1.7 kg ha?1. Herbicide residues, determined at selected times after application, were not detected at the limit of detection of the analytical method (0.05 mg kg?1) in either the seed and straw at maturity, or in the green foliage six to eight weeks after application. Recoveries of dinoseb were 76% from fortified green foliage at the 0.1 mg kg?1 level, and 64% from fortified seed at the 0.05 mg kg?1 level.  相似文献   

2.
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   

3.
A method was developed for the extraction and HPLC analysis of the plant growth regulator maleic hydrazide (MH) from garlic bulbs. Recovery of MH from fortified garlic tissue was 75.8(±6.1)% at the 1 and 2 mg kg?1 fortification levels. MH residues were determined by HPLC in cloves of garlic bulbs following treatment at three sites in southern Ontario with foliar applications at 3.75 kg ha?1. MH residues in the cloves were in the order of 3 mg kg?1 at two sites, and 11 mg kg?1 at the third side.  相似文献   

4.
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   

5.
Two analytical methods are presented for the determination of 2,4-D in oranges. The screening procedure uses a commercial ELISA kit, designed for the determination of 2,4-D in water. Good semi-quantitative screening data were obtained provided that the standard solutions used to construct the calibration curve were prepared in blank orange extract. The limited quantification range of the kit was due to the narrow linear range and differences in response to 2,4-D when present as the free acid and as various esters. A GC-MS confirmatory technique involved extraction of 2,4-D from oranges by homogenisation with methanol, filtration and esterification/transesterification with boron trifluoride-methanol. Recoveries for three spiking levels (0·2, 1·0 and 2·0 mg kg-1) for 2,4-D and 2,4-D isopropyl ester were within the range 75–120%. In a small survey of retail oranges, 10 samples were screened using the ELISA kit and four were found to have >0·2 mg 2,4-D kg-1. All four residues were confirmed by GC-MS. The ELISA procedure involves approximately half the staff effort of the GC-MS procedure. © 1997 SCI.  相似文献   

6.
Carbaryl residues in wheat grain have been determined in methanol extracts using normal-phase high-pressure liquid chromatography (h. p. l. c.) with ultraviolet detection. A single-injection, clean-up and analysis technique was used to allow more rapid analysis of samples after extraction. A detection limit of 0.1 mg kg?1 in a 50 g sample of wheat was achieved. Recoveries of 86% at the 1 mg kg?1 level and 90-99% at the 5 mg kg?1 level were obtained for fortified grain samples. Methanol was found to be a superior extractant for carbaryl from wheat when compared with hexane, acetone and dichloromethane. Twelve samples containing aged carbaryl residues were analysed by the h. p. l. c. technique and by a colorimetric procedure which allowed statistical analysis of errors. For the h. p. l. c. method (excluding sampling error), a relative standard deviation of 4.4% was obtained.  相似文献   

7.
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   

8.
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   

9.
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   

10.
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   

11.
The herbicides bentazone, 2,4-D, MCPA, propanil, molinate, and tiocarbazil, and the insecticide phenthoate, were applied to ricefields in Sardinia at rates equivalent to maximum aqueous concentrations of 0.4-2.8 mg kg?1, assuming the water to be 20 cm deep. Their concentrations in water were measured by high-performance liquid chromatography. Residues in 162 water samples, collected from 16 ricefields 1, 4, 7, 10, 12, 18, 21 and 120 days after the last spraying, were all below the limit of determination (0.03 mg kg?1). Residues in 40 water samples taken from five drainage canals were also less than 0.03 mg kg?1.  相似文献   

12.
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   

13.
A method is described for the analysis of small amounts of hydrazine in maleic hydrazide formulations. Following derivative formation with pentafluorobenz-aldehyde, the pentafluorobenzaldehyde azine was extracted with hexane and determined by gas-liquid chromatography with electron-capture detection. Recoveries of 72-80% were obtained from samples fortified with 1 and 10 μg of hydrazine. The limit of detection was 0.05 mg kg?1. Fourteen commercial formulations with maleic hydrazide concentrations ranging from 180-360 g litre?1 were investigated. The hydrazine content of the maleic hydrazide used in these formulations ranged from less than 0.05 to 53 mg kg?1. During the storage of two samples at 50°C for 10 weeks, the hydrazine contents increased from 2.2 to 124 and 0.4 to 54 mg litre?1, respectively.  相似文献   

14.
A sensitive method for the detection and estimation of residues of the molluscicide, niclosamide, in bananas is described. The procedure involves extraction of the molluscicide, purification of the extract by solvent partition and column chromatography, formation of the heptafluorobutyryl derivative of 2-chloro-4-nitroaniline in 99% yield and determination of the derivative by gas—liquid chromatography with electron-capture detection. Recoveries from fortified bananas were 89 and 79% at levels of 0.02 and 0.2 mg kg?1, respectively. The sensitivity of the method was such that 0.6 pg of the pure derivative could be detected, based on twice the background noise level on the chromatograph.  相似文献   

15.
Organophosphorus insecticide residues have been monitored for two years in virgin olive oil after dimethoate and fenthion treatments to control the olive fruit fly. No dimethoate residues were detected in any of the samples. For the first and second years, 50% and 21%, respectively, of the samples contained no detectable fenthion residues, while 4% and 6%, respectively had residue concentrations exceeding the Codex Alimentarious Maximum Residue Limit (1 mg kg?1). The mean concentration was 0·236 mg kg?1 oil and the estimated daily intake of fenthion 0·0002 mg kg?1 body weight (Acceptable Daily Intake 0·001 mg kg?1 body weight). The parent compound was the most important residue in fresh samples, while aged samples contained a higher amount of the metabolite fenthion sulfoxide. The contribution of the oxygen analogues (P= 0 metabolites) of fenthion to the total residue concentration was<5% in most cases.  相似文献   

16.
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   

17.
A method is described for the analysis of soils for residues of the herbicide diclofop-methyl, methyl (RS)-2-[4-(2,4-dichlorophenoxy)phenoxy]propionate, and its breakdown product diclofop, (RS)-2-[4-(2,4-dichlorophenoxy)phenoxy]propionic acid. Diclofop-methyl undergoes hydrolysis in the soil to diclofop, which also has herbicidal activity. A procedure, using a 1% phosphoric acid solution for extraction purposes, has been developed and gives good recoveries of both diclofop-methyl and diclofop at the 0.5 and 0.05 mg kg?1 levels. After methylation, gas-liquid chromatography with electron-capture detection is used to determine total residue concentrations.  相似文献   

18.
A method is described for the estimation of residues of the carbamate insecticide promacyl [5-methyl-m-cumenyl butyryl(methyl)carbamate] and its metabolites that are hydrolysable to isothymol (m-cymen-5-ol), using high-performance liquid chromatography with electrochemical detection to determine the isothymol. Clean-up of samples relied on the steam volatility of phenols. Recoveries at the 0.1 mg kg?1 level varied from 72–88% for fat tissue and 81–91% for liver. The limits of detection were found to be 0.01 mg kg?1 for and 0.02 mg kg?1 for liver. A comparative study of the chromatography of sample extracts using both ultraviolet detection and electrochemical detection showed a substantial decrease in the level of interfering co-eluates in the latter method. A field trial, involving a single spray application of the formulated acaricide on milking cattle, revealed residues in the butter fat comparable with those found in a previous investigation.  相似文献   

19.
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   

20.
Diflubenzuron, 1-(4-chlorophenyl)-3-(2,6-difluorobenzoyl)urea was used to control the pine looper population in about 1160 ha of Scots pine stand in eastern Finland in summer 1984. The control measure was effective, resulting in the collapse of the population in the treated area. Residues of diflubenzuron and two of its metabolites, 4-chloroaniline and 4-chlorophenylurea, were determined in water, pine needles, litter, humus, boleti and other wild mushrooms, bilberry (Vaccinium myrtillus L.) and cowberry (Vaccinium vitis-idaea L.) samples taken from this area. In water samples taken from the treated area diflubenzuron was still detected at concentrations of 0.1 μg litre?1 2 months after application. No diflubenzuron was detected in this area the following year, nor outside the treated area. Neither metabolite was detected at any time. The sum of diflubenzuron and its metabolites in the litter layer was, on average, 0.7mg kg?1 both 1 week and 1 month after the application. The next year, however, it had increased to 1.4 mg kg?1. Diflubenzuron and its metabolites were not detected in the humus layer. The amount of diflubenzuron residues in the pine needles was, on average, 3.0 mg kg ?1 1 day after the application, but in 2 months the level had decreased to 0.2-0.3 mg kg ?1 or was not detectable. The following year the sum of diflubenzuron and its metabolites in two pine-needle samples was 0.3 and 1.6 mg kg ?1. The sum of diflubenzuron and its metabolites in wild mushrooms was, on average, 0.07 mg kg ?1 1 week after the application, but the following year no residues were detected. No residues were found in the boletus samples. The residues of diflubenzuron and its two metabolites in bilberries totalled, on average, 0.2 mg kg ?1 1 day after the application, and 6 μg kg ?1 the following year. The sum of diflubenzuron and metabolites in cowberries was, on average, 0.2 mg kg ?1 1 month after application.  相似文献   

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