Residues of synthetic pyrethroid insecticides on horticultural crops

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.     

Uptake of phorate by lettuce

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.     

Behaviour of trifloxystrobin and tebuconazole on grapes under semi‐arid tropical climatic conditions

BACKGROUND: A mixture of trifloxystrobin and tebuconazole is excellent in controlling both powdery and downy mildew of grapes. The objective of the present work was to study the behaviour of trifloxystrobin and tebuconazole on grape berries and soil following treatment with Nativo 75 WG, a formulation containing both fungicides (trifloxystrobin 250 + tebuconazole 500 g kg^?1). This study was carried out for planned registration of this mixture for use on grapes in India. RESULTS: Initial residue deposits of trifloxystrobin and tebuconazole on grapes were below their maximum residue limit (MRL) of 0.5 and 2 mg kg^?1, respectively, when Nativo 75 WG was applied at the recommended dose of 175 g product ha^?1. The residues dissipated gradually to 0.02 and 0.05 mg kg^?1 by 30 days, and were below the quantifiable limit of 0.01 mg kg^?1 at the time of harvest (60 days after the last treatment). Trifloxystrobin and tebuconazole dissipated at a pre‐harvest interval (PHI) of 36 and 34 days, respectively, from the recommended treatment dose. The acid metabolite of trifloxystrobin, CGA 321 113, was not detected in grape berries at any point in time. Soil at harvest was free of any pesticide residues. CONCLUSION: Residue levels of both trifloxystrobin and tebuconazole were below MRLs when grapes were harvested 30 days after the last of four applications of 175 g product ha^?1 (trifloxystrobin 44 g AI ha^?1, tebuconazole 88 g AI ha^?1) under the semi‐arid tropical climatic conditions of India. Copyright © 2010 Society of Chemical Industry     

Disappearance of carbosulfan residues in peaches

The disappearance kinetics of the carbamate insecticide, carbosulfan, applied at 2 kg AI ha^?1 (‘Marshal’ 250 g litre^?1 EC) in peaches was studied. Degradation took place in two consecutive stages (0–28 and 28–57 days), with half-lives of 7.4 and 17.5 days, respectively. The residues obtained 57 days after treatment did not exceed 0.2 mg kg^?1. When treatments were carried out 30, 21 and 14 days before the probable date of harvest (date of fruit maturation) with two doses (1.0 and 2.0 g formulated product litre^?1) and two volumes applied (750 and 1500 litre ha^?1), the residual levels detected were between 0.122 mg kg^?1 (30 days before harvest) and 0.4 mg kg^?1 (14 days before harvest). The major metabolite, carbofuran, was never detected above its determination limit of 0.004 mg kg^?1 throughout the whole study.     

Residues of cypermethrin,fenvalerate and deltamethrin on cauliflower

Following the application of Cypermethrin, fenvalerate and deltamethrin to a cauliflower crop at rates of 50, 50 and 12 g a.i. ha^-1, the maximum initial deposits of these insecticides on heads and leaves were 1.10 and 0.75, 1.14 and 0.60, and 0.32 and 0.12 mg kg^-1, respectively. These residue values for fenvalerate were less than the maximum residue limit (MRL) of 2 mg kg^-1 for this crop. While the maximum initial deposits of Cypermethrin and deltamethrin on cauliflower leaves were less than their respective MRL values of 1 and 0.2 mg kg^-1 for brassica leafy vegetables, it took one day for their residues on cauliflower heads to decline below this level.     

Influence of block and cell size,growing medium and insecticide dose on the behaviour and uptake of phorate by lettuce and uptake of carbofuran and chlorfenvinphos by calabrese

Phorate residues in peat blocks and lettuce were determined following incorporation of the insecticide into different block and ‘Speedling’ cell sizes. Between-block variability was influenced little by block size. Phorate oxidation was most extensive in the largest blocks containing the smallest dose. Total residue concentrations in the lettuce declined from the time of planting to harvest, although accumulation of insecticide continued and was related more to dose than to block or cell size. Residues in the lettuce at harvest exceeded the proposed maximum limit of 0.2 mg kg^?1 in some treatments. Residues at planting comprised mainly the parent sulphoxide and sulphone, but by harvest, the oxygen analogue sulphoxide and sulphone predominated. Lettuce weight was not influenced by dose but was related directly to block size. Carbofuran and chlorfenvinphos residues were determined in calabrese sown into two sizes of blocks. At planting time, carbofuran residue concentrations were 100 times greater than those of chlorfenvinphos but residues of both insecticides in the mature heads were < 0.01 mg kg^?1. Seedling weights in both sowings declined with increasing concentrations of the insecticides. It was concluded that manipulations of block size and the dose of insecticide need to be evaluated for individual insecticide/crop combinations to exploit the technique fully.     

Build-up and subsequent decline of residues of quintozene and hexachlorobenzene in lettuce in sequential crops

The build-up and decline of quintozene and hexachlorobenzene residues in protected lettuce, resulting from one to five treatments of the soil (each of 35 g m-2) with a quintozene formulation, have been studied. Residue levels were monitored in each experimental crop during growth until harvest. Residues in the soil at harvest were also determined. Quintozene residues in the harvested lettuce were in the range < 0.02–0.80 mg kg^?1 and those of hexachlorobenzene were in the range < 0.02–0.05 mg kg^?1 (expressed on a fresh weight basis). Residue levels in the soil were 5.4–231 mg kg^?1 for quintozene, and 0.20–5.4 mg kg^?1 for hexachlorobenzene (expressed on a dry weight basis). Under the experimental conditions of the trial there was no significant build-up of quintozene or hexachlorobenzene in harvested lettuce, even after five treatments to the same site.     

Repellent action of permethrin,cypermethrin and resmethrin against black flies (Simulium spp.) attacking cattle

Permethrin, cypermethrin, and resmethrin were tested under field conditions as repellents to protect cattle from black flies (Simulium spp.). The chemicals were applied topically to the entire body surface of steers. Ethanolic solutions of technical permethrin, at doses of 1, 2, 4 and 6 mg a. i. kg^?1 of body weight, effectively repelled black flies by preventing at least 70% of the flies present from taking a blood meal for up to 8 days, and for at least 11 days at a dose of 12 mg a. i. kg^?1. Aqueous mixtures of a 20% permethrin emulsifiable concentrate (e. c.), at doses of 1, 2 and 6 mg a. i. kg^?1, effectivelyrepelled black flies for 2, 10 and 11 days, respectively. Aready-to-use 5% permethrin dust, at doses of 1, 2, and 4 mg a. i. kg^?1, effectively repelled black flies for 4, 5 and 8 days, respectively. Ethanolic solutions of technical cypermethrin, at doses of 1 and 2 mg a. i. kg^?1, repelled black flies for 3 and 4 days, respectively. Aqueous mixtures of a 40% cypermethrin e. c., at doses of 2 and 4 mg a. i. kg^?1, repelled black flies for at least 5 days. Ethanolic solutions of technical resmethrin, at doses of 2 and 6 mg a. i. kg^?1, repelled black flies for 1 and 2 days, respectively.     

Residues in blackcurrants,fodder peas,spinach and potatoes treated with sublethal doses of 2,4,5-T to simulate wind drift damage

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.     

Organophosphorothioates and synergised synthetic pyrethroids as grain protectants on bulk wheat

Organophosphorothioates and synergised synthetic pyrethroids were used in duplicate field trials carried out on bulk wheat in commercial silos in Queensland and New South Wales. Laboratory bioassays using malathion-resistant strains of insects were carried out on samples of treated grain at intervals over 9 months. These established that all treatments were generally effective. Deltamethrin (2 mg kg^?1)+ piperonyl butoxide (8 mg kg^?1), fenitrothion (12 mg kg^?1)+ fenvalerate (1 mg kg^?1)+ piperonyl butoxide (8 mg kg^?1), fenitrothion (12 mg kg^?1)+ phenothrin (2 mg kg^?1)+ piperonyl butoxide (8 mg kg^?1) and pirimiphos-methyl (4 mg kg^?1)+ permethrin (1 mg kg^?1)+ piperonyl butoxide (8 mg kg^?1) controlled common field strains of Sitophilus oryzae (L.) and Rhyzopertha dominica (F.). Against a highly resistant strain of S. oryzae, deltamethrin (2 mg kg^?1)+ piperonyl butoxide (8 mg kg^?1) was superior to the remaining treatments. All treatment combinations completely prevented progeny production in Tribolium castaneum (Herbst), T. confusum Jacquelin du Val and in Ephestia cautella (Walker). Residues of deltamethrin, fenvalerate, permethrin and phenothrin were determined and shown to be highly persistent on stored wheat. During milling, residues accumulated in the bran fractions and were reduced in white flour. They were not significantly reduced during baking.     

The persistence and activity of insecticide spary deposits on woven polypropylene fabric

Wettable powder formulations of the organophosphorus insecticides, fenitrothion and pirimiphos-methyl, and the pyrethroids, permethrin and deltamethrin, have been compared for persistence and activity on woven polypropylene fabric; the residues produced in maize kept under the test sheets have also been measured. The test insects were Sitophilus oryzue (L.) and Tribolium custuneum (Herbst). Permethrin at 41 and 83 mg m^?2 was completely effective for the full 12 weeks of the experiment. Deltamethrin at 6.2 and 12.5 mg m^?2 was almost equally effective but after 4 weeks the deposit was slower acting against S. oryzae. The organophosphorus compounds were effective only up to 2 weeks at 250 mg m^?2 and up to 4 weeks at 500 mg m^?2. No residues could be detected under the pyrethroids but the organophosphorus insecticides gave residues of 2–4 mg kg^?1 on a thin layer of grain. This residue was biologically effective against the test insects.     

Toxico‐kinetics,recovery efficiency and microsomal changes following administration of deltamethrin to black Bengal goats

A study of the toxico‐kinetics, recovery percentage from different substrates, cytotoxicity and role of cytochrome P₄₅₀ and b₅ of liver microsome in the metabolism of deltamethrin were carried out in female black Bengal goat. The ALD₅₀ value of deltamethrin in goat by intravenous route lies between 0.2 and 0.6 mg kg^?1. Intravenous disposition kinetics using a dose of 0.2 mg kg^?1 showed that the maximum blood concentration of deltamethrin was recorded at 0.5 min, followed by rapid decline, and a minimum concentration was detected at 6 min after administration. The following values were obtained : Vd_area 0.148 (± 0.02) litre kg^?1; t_1/2 (α) 0.22 (± 0.02) min; t_1/2 (β) 2.17 (± 0.37) min; K_el 1.05 (± 0.24) min^?1; AUC 4.30(± 0.45) µg min ml^?1; Cl_B 0.05 (± 0.006) litre kg^?1 min^?1; T～B 1.93 (± 0.58); fc 0.40(± 0.05). After 10 min, liver retained the maximum residue, and heart, adrenal gland, kidney, spleen, fat and brain also held the insecticide; liver, fat, heart and spleen retained residue after 30 min, and bone, liver and fat retained residue after 60 min of intravenous administration. Oral absorption of deltamethrin was poor and inconsistent, and approximately 65% of administered dose was recovered from faeces and gastrointestinal contents. The excretion of deltamethrin through urine was meagre, and only 0.01 and 0.013% of the administered dose was recovered after 3 and 5 days of oral administration respectively. All the tissues retained the residue after 3 days; while fat, rumen, reticulum, omasum, abomasum, large and small intestine and bone retained the residue after 5 days of oral administration; and the percentage recoveries were 1.73 and 0.027 respectively. Deltamethrin reduced the level of cytochrome P₄₅₀ content of liver microsomal pellet of goat after 5 days of oral administration. Histopathological examination of liver, kidney, heart, spleen brain and lung sections of treated goats did not reveal any pathological changes. © 2001 Society of Chemical Industry     

Accumulation of endosulfan residues in fish and their predators after aerial spraying for the control of tsetse fly in Botswana

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.     

Studies with permethrin against bodylice in Egypt

Approximately 350 people, the inhabitants of two villages in the Fayum district of Egypt, were individually dusted with 50 g of powder containing 2.5 or 5.0 g permethrin kg^?1. The inhabitants of a third village were left untreated as a control. Before treatment, approximately two-thirds of the population of all three villages were infested with bodylice. Fourteen days after treatment, the permethrin dust at the lower strength reduced the infestation by 98.8% and at the higher strength by 100%. The dust containing 5 g permethrin kg^?1 maintained a high level of residual control (80.5%) for at least 91 days. The other gave a lower level of control at this time. Urine samples, taken from subjects in each of the treated villages before and after dusting, were analysed for permethrin metabolites. Results indicated that the maximum amount of permethrin absorbed, orally, through the skin, or by inhalation, was 39 μg kg^?1 body weight, 24 h after treatment. No residue was found 30 days and 60 days after treatment. It was concluded that there was a very substantial safety margin when permethrin dusts were used on man for bodylice control.     

Protective action of fenvalerate,deltamethrin, and four stereoisomers of permethrin against black flies (Simulium spp.) attacking cattle

Fenvalerate, deltamethrin, (1R)-cis-permethrin, (1R)-trans-permethrin and (1S)-trans-permethrin, applied topically to the entire body surface of steers at a rate of 1 mg a.i. kg⁻¹, provided 70% or better protection from black flies on cattle for 16, 9, 8, 6 and 6 days, respectively. The (1S)-cis stereoisomer of permethrin was ineffective as a protectant against black flies at a rate of 1 mg a.i. kg⁻¹ when applied as a total body spray. One poly(vinyl chloride) ear tag containing 10% permethrin, in each ear of steers, provided protection from black fly attack for up to 13 days under field conditions. Poly(vinyl chloride) ear tags containing 8% fenvalerate, installed in each ear of steers, did not provide satisfactory protection from black flies under field conditions.     

Residues of the algicide endothal in water,soil and rice,after paddy field applications

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.     

Dissipation rates of insecticides in six minor vegetable crops grown on organic soils in Ontario,Canada

Dissipation rates of diazinon, endosulfan, leptophos, methamidophos, methomyl, parathion and pirimicarb were studied on five minor vegetable crops, including cos and head lettuce, endive, cauliflower and Chinese cabbage. Residues from foliar treatment generally followed an exponential rate of decline. The number of days for residues to drop to below acceptable tolerances was highly dependent on the magnitude of the initial residue; large variations in initial residues were observed between years, between insecticides, and between crop types. Residues of five insecticides and two fungicides used in furrow treatments for onions intended for pickling were determined in the onions at harvest and after pickling. Fensulfothion and fonofos levels were below the accepted tolerance of 0.1 mg kg^?1 at harvest, while chlorfenvinphos, chlorpyrifos and ethion were present above this level; fungicide residues were not detected. Following pickling, only ethion residues were still present in the onions at levels greater than 0.1 mg kg^?1.     

Pyrethroid insecticide residues on vegetable crops

Pyrethroid insecticides were applied on various vegetable crops as foliar treatments to determine dissipation rates. On Chinese broccoli (Guy Lon), Chinese mustard (Pak Choi) and Chinese cabbage (Kasumi, napa), fenvalerate was persistent with residues of 0.10, 0.14 and 0.11 mg kg-1, respectively, by day 21. Cypermethrin residues on head lettuce were below 0.1 mg kg-1 by day 10 but on the leafier romaine and endive varieties it was more persistent and required 14-19 days to dissipate below this concentration. After three applications, residues of cypermethrin in harvested carrots and of permethrin in eggplant were not detected on the day of application. On asparagus, deltamethrin and cypermethrin residues declined to less than 0.1 mg kg-1 by days 1 and 2, respectively; permethrin was more persistent, requiring more than 2 days to decline to less than 0.1 mg kg-1. Deltamethrin on dry (cooking) and Spanish onions was not detected on the day of application. On tomatoes, the concentration of permethrin was 0.093 mg kg-1 on the day of application and declined to about 0.05 mg kg-1 after 2-4 days. In general, permethrin, cypermethrin and deltamethrin residues declined to acceptable concentrations within an acceptable pre-harvest interval. Fenvalerate may be too persistent on these speciality crops unless a maximum residue limit > 0.1 mg kg-1 is permitted.     

The metabolism of tefluthrin in the goat

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.     

Residues of zeta‐cypermethrin in bovine tissues and milk following pour‐on and spray application

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