PESTICIDE RESIDUES IN FOOD - 1984 Sponsored jointly by FAO and WHO EVALUATIONS 1984 The monographs Data and recommendations of the joint meeting of the FAO Panel of Experts on Pesticide Residues in Food and the Environment and the WHO Expert Group on Pesticide Residues Rome, 24 September - 3 October 1984 Food and Agriculture Organization of the United Nations Rome 1985 AMITRAZ Explanation Amitraz was reviewed by the 1980 JMPR. 1/ A temporary ADI of 0.0005 mg/kg was estimated and a number of temporary MRLs proposed. Additional residue data on whole olives from supervised trials were required by 1984 and additional residue data on citrus fruit and further trials on hops, eggplant and onions were considered desirable. The present meeting was informed that the use of amitraz on olives has not been developed commercially. Residues data on pears and citrus were made available, as well as new information on plant metabolism. RESIDUES IN FOOD AND THEIR EVALUATION USE PATTERN Amitraz is registered in a number of territories for the control of various mite species of citrus (Panonychus citri, Tetranychus spp., Phyllocoptruta oleivora). Cultural practices and agronomic needs differ among these territories. For example, higher rates of amitraz are required to control infestations of Tetranychus spp. than for other mite species. Similarly, application volumes vary depending on local practice and the number and size of trees. Thus, approved uses are often expressed differently in the different territories. These have been standardized in terms of maximum spray concentration and an approximate equivalent rate of amitraz per hectare in Table 1. The use of amitraz has been approved recently in the Netherlands on strawberries for the control of spider mite at 38 g/100 1 up to flowering and after the last picking (1981), and on eggplant, peppers and tomatoes in glasshouses for the control of spider mite at 76 g/l 1000m2 by swingfog or pulsfog only, with a three-day interval between last application and harvesting (1981/82). Its use on pig, cattle and sheep has been approved since 1980. 1/ See Annex 2 for FAO and WHO documentation TABLE 1. Registration Status of the Use of Amitraz on Citrus Approved application rates Withholding period Spray concentration Approximate Territory (days) (%a.i.) g a.i./ha Cyprus 14 0.04 600 Ecuador 14 0.12 500 Iran NA 0.02 400 Italy 14 0.04 400 Japan 14 0.02 1 200 Malaysia 7 0.04 400 Morocco 28 0.01 1 200 Republic of Korea NA 0.02 900 Spain 7 0.04 400 Taiwan province of China 14 0.02 400 Turkey 28 0.04 400 RESIDUES RESULTING FROM SUPERVISED TRIALS Apples and Tomatoes Apple and tomato samples from amitraz trials were analysed for amitraz and its metabolite BTS 27 271. An analytical procedure was used that involved the conversion of amitraz to BTS 27 271 and the assay of the total BTS 27 271 residue. The maximum residue of BTS 27 271 in apples 28 days after a single spray application of amitraz was found to be 0.24 mg/kg. In tomatoes, three days after a single spray application of amitraz, the maximum residue of BTS 27 271 was found to be 0.46 mg/kg (Table 2). Citrus Residues on citrus grown in the United States have been determined by the "total residue" method, in which all residues containing the 2,4-dimethyl-analine moiety are measured and the residue expressed as amitraz equivalent. (The residue method recommended by JMPR/Codex determines the sum of amitraz and its metabolite N-(2,4-dimethylphenyl)-N'-methylformamidine (BTS 27 271). Residue values determined by the "total amitraz" method may be converted to equivalent values determined as BTS 27 271 by dividing by a factor of 1.8.) Grapefruit Following one to three applications of amitraz at up to 24 oz/acre (1 lb/acre = 1.12 kg/ha), mean residues in grapefruit over a period of 1 to 14 days ranged from <0.05-1.04 mg/kg, with an over-all mean of 0.49 mg/kg (Table 3). Lemon Following one or two applications of amitraz at a rate of 24 oz/acre, mean residues in lemons over a period of 1 to 12 days ranged from 0.44 to 1.23 mg/kg in lemons, with an over-all mean of 0.81 mg/kg (Table 4). Lime Following one to three applications of amitraz at up to 5 oz/acre, mean residues in limes over a period of 1 to 14 days ranged from 0.16 to 2.11 mg/kg, with an over-all mean of 0.84 mg/kg (Table 5). Tangerine and Tangelo Following a single application of 24 oz/acre of amitraz to tangerines, mean residue levels over a period of 1 to 12 days were 0.79 to 1.49 mg/kg, with an over-all mean of 1.16 mg/kg. For tangelo, following one or two applications, the equivalent residue levels were 0.73 to 1.85 mg/kg and 0.86 mg/kg, respectively (Table 6). TABLE 2. Amitraz Residues in Tomatoes from Supervised Trials, The Netherlands Application Year No. Rate Formulation Residues1 Reference (kg a.i./ha) (mg/kg) 1974 1 1.14 40 0.40 (0.29-0.46) Goodall & Somerville, 1974 1974 1 1.14 40 0.27 (0.17-0.36) Greve & Hogendoorn, 1975 1979 1 76 g a.i./ pulsfog 0.11 (0.08-0.17) Netherlands, 1 000 m2 1979 1980 1 80 g a.i./ pulsfog 0.15 (0.10-0.21) ) (glass- 1000 m2 ) van Adrichem & house) ) Vogelezang, ) 1981 1980 1 81 g a.i./ swingfog 0.05 (0.02-0.07) ) (glass- 1 000 m2 ) house) ) 1 Measured three days after application; determined and expressed as N-2,4-dimethylphenyl-M-methylformamidine. TABLE 3. Amitraz Residues in Grapefruit from Supervised Trials, United States Application Rate No. Spray volume Interval Residues (mg/kg) Reference (oz a.i./ (gal/acre) (days) Range Mean acre) 4.5 300 1 0.17 - 0.19 0.18 Ford, 1981b 8 0.10 - 0.15 0.13 15 0.11 - 0.12 0.11 29 0.07 - 0.08 0.08 43 0.06 - 0.07 0.07 9 300 1 0.33 - 0.38 0.36 Ford, 1981b 8 0.18 - 0.27 0.23 15 0.15 - 0.18 0.17 29 0.12 - 0.16 0.14 43 0.09 - 0.13 0.11 24 1 800 7 0.18 - 0.37 0.28 Upjohn & 7.5 100 1 0.32 Boots, 7 0.18 1974 - 1981 14 <0.05 15 100 1 0.61 7 0.43 14 <0.05 24 3 1 0.82 - 1.27 1.04 Ford, 1981d 7 0.71 - 1.09 0.98 14 0.84 - 1.02 0.92 Note: 1 lb/acre = 1.12 kg/ha; 1 U.S. gal/acre = 9.36 l/ha TABLE 4. Amitraz Residues in Lemons from Supervised Trials, United States Application Rate No. Spray volume Interval Residues (mg/kg) Reference (oz a.i./ (gal/acre) (days) Range Mean acre) 48 1 200 1 1.86 - 1.93 1.90 Ford, 1981a 7 1.17 - 1.37 1.26 14 1.11 - 1.15 1.13 28 0.73 - 0.79 0.76 56 0.38 - 0.41 0.40 112 0.12 - 0.20 0.17 24 180 1 1.14 - 1.24 1.19 Ford 1981d 7 0.99 - 0.99 0.99 24 2 180 1 1.19 - 1.26 1.23 7 0.66 - 0.93 0.80 24 2 40 1 0.57 - 1.04 0.81 12 0.34 - 0.70 0.52 24 2 500 1 0.68 - 0.81 0.73 24 2 1 200 1 0.59 - 0.64 0.62 7 0.40 - 0.47 0.44 TABLE 5. Amitraz Residues in Limes from Supervised Trials, United States Application Rate No. Spray volume Interval Residues (mg/kg) Reference (oz a.i./ (gal/acre) (days) Range Mean acre) 7.5 250 86 <0.05 Ford, 1981c 15 86 <0.05 24 40 1 2.07 - 2.15 2.11 7 1.18 - 2.17 1.68 7.5 100 1 0.41 7 0.27 14 0.16 15 1 0.64 7 0.28 14 0.23 24 3 40 1 1.37 - 2.07 1.72 12 0.60 - 1.11 0.86 TABLE 6. Amitraz Residues in Tangerines and Tangelos from Supervised Trials, United States Application Rate No. Spray volume Interval Residues (mg/kg) Reference (oz a.i./ (gal/acre) (days) Range Mean acre) TANGERINE 24 40 1 0.86 - 2.11 1.49 Upjohn & 12 0.63 - 0.85 0.74 Boots, 1981b TANGELO 24 500 97 0.26 - 0.38 0.32 Upjohn & 24 40 1 1.13 - 2.57 1.85 Boots, 12 0.73 - 0.97 0.85 1981a 24 2 500 1 0.65 - 1.07 0.86 14 0.72 - 0.73 0.73 Orange The application rate of 24 oz/acre is that approved under an experimental use permit in the United States and for which a temporary tolerance of 2 mg/kg has been established. At this rate, the range of residue values in oranges over a period of 1 to 7 days following a single application was 0.18 to 1.25 mg/kg, with an overall mean of 0.48 mg/kg. Following two applications, the equivalent values were 0.32 to 1.01 mg/kg and 0.59 mg/kg. Following three applications, the range of mean values over a period of 1 to 21 days was 0.26 to 2.20 mg/kg, with an overall mean of 0.188 mg/kg (Table 7). Residues of amitraz in oranges, grown in the United States, treated at higher rates (i.e. 40 oz/acre or 2.8 kg/ha) were within the range of expected values, as were those crops treated at lower rates (Table 8). The analytical method used to determine residues in or on oranges grown in Japan measured amitraz and its metabolite BTS 27 271 separately. Studies undertaken in Japan are summarized in Tables 9 and 10. In the former, the data indicate that the majority of the residues are in the peel, with residues being predominantly present as the metabolite BTS 27 271. The second study (Table 10) confirms the low residues (generally less than 0.01 mg/kg of the parent compound following a preharvest interval of 15 days.) Two studies were conducted in China in 1982 and 1983 to determine the persistence and residue distribution of amitraz in oranges. The first study determined the residues of amitraz from trials conducted on oranges grown in Guangdong. In 1983 this study was repeated in Guangdong and Guangxi. The method of analysis used to measure residues was the same as that used in the United States, which determines amitraz and its metabolites containing the 2,4-dimethylaniline moiety. These studies are unpublished but are summarized in Tables 11 and 12. These data confirm the general levels of amitraz residues found in other studies and their distribution within the fruit. The residues of 2,4-dimethylaniline (BTS 24 868) in two samples of commercially grown oranges were determined using an analytical method that had been initially developed for BTS 24 868 residues in pears. Peel and flesh were analysed separately. The recoveries of BTS 24 868 from control oranges ('Valencia' and 'Maroc Late'), fortified at either 0.1 or 0.05 mg/kg, gave an over-all mean and standard deviation of 82.4 ± 15.7 percent. Mean BTS 24 868 residues in the peel of control oranges fortified with 0.25 mg/kg of either amitraz, BTS 27 271 or BTS 27 919 were found to range from 0.012 to 0.026 mg/kg (equivalent to 4.8 to 10.3 percent artefactual conversion of the parent compounds to BTS 24 868). Residues of BTS 24 868 in the flesh of oranges from the two commercial orchards analysed were below the limit of detection (0.003 mg/kg), as were the total amitraz-derived residues (limit of detection 0.025 mg/kg). Residues of BTS 24 868 in the peel of these oranges were 0.022 mg/kg (Grower 1) and 0.040 mg/kg TABLE 7. Amitraz Residues in Oranges from Supervised Trials, United States Application1 Rate No. Spray volume Interval Residues (mg/kg) Reference (oz a.i./ (gal/acre) (days) Range Mean acre) 1 1 900 1 0.11 - 0.50 0.26 Upjohn & 7 0.12 - 0.46 0.25 Boots 1 1 300 1 0.24 - 0.25 0.25 1974-1981 7 0.17 - 0.24 0.21 1 100 1 1.00 - 1.49 1.25 7 0.86 - 1.19 1.03 1 100 1 0.62 - 0.79 0.71 7 0.44 - 0.61 0.53 1 180 1 0.24 - 0.71 0.48 7 0.14 - 0.22 0.18 1 1 800 7 0.26 - 0.37 0.31 1 1 800 1 0.31 - 0.36 0.34 2 100 1 0.58 - 0.88 0.73 Upjohn & 7 0.39 - 0.71 0.55 Boots, 2 1 300 1 0.30 - 0.35 0.33 1974-1981 7 0.32 - 0.32 0.32 2 100 1 0.63 - 1.38 1.01 10 0.47 - 0.76 0.62 2 180 1 0.60 - 0.71 0.66 7 0.40 - 0.53 0.47 3 1 1.85 - 2.42 2.20 Ford, 1981c 7 1.13 - 1.54 1.46 14 0.98 - 1.23 1.07 21 0.68 - 1.54 1.11 Table 7 (continued) Application1 Rate No. Spray volume Interval Residues (mg/kg) Reference (oz a.i./ (gal/acre) (days) Range Mean acre) 3 1 0.47 - 0.59 0.52 7 0.28 - 0.42 0.35 14 0.38 - 0.42 0.40 21 0.19 - 0.33 0.26 3 1 0.57 - 1.37 0.88 7 0.52 - 1.32 0.82 21 0.69 - 1.45 1.14 3 1 0.60 - 0.80 0.73 7 0.37 - 0.74 0.55 1 Rate of application was 24 oz a.i./acre in all trials TABLE 8. Amitraz Residues in Oranqes from Supervised Trials, United States Application Rate Spray volume Interval Residues (mg/kg) Reference (oz a.i./ (gal/acre) (days) Range Mean acre) 19.8 1 000 1 0.99 - 1.09 1.06 Ford, 1980 7 0.69 - 0.92 0.79 14 0.55 - 0.65 0.59 27 0.38 - 0.46 0.42 49 0.16 - 0.28 0.23 119 0.10 - 0.14 0.11 141 0.09 - 0.09 0.09 40 1 000 1 0.62 - 0.69 0.65 Ford, 1981a 7 0.42 - 0.49 0.46 14 0.34 - 0.48 0.40 28 0.31 - 0.36 0.34 58 0.27 - 0.34 0.31 40 1 000 1 1.67 - 1.94 1.79 Ford, 1981a 7 1.16 - 1.35 1.25 14 0.83 - 0.95 0.89 28 0.48 - 0.54 0.52 56 0.20 - 0.22 0.21 40 1 000 1 0.58 - 0.66 0.63 Ford, 1981a 8 0.46 - 0.59 0.53 15 0.49 - 0.52 0.51 31 0.51 - 0.55 0.52 57 0.41 - 0.49 0.45 TABLE 8. (continued) Application Rate Spray volume Interval Residues (mg/kg) Reference (oz a.i./ (gal/acre) (days) Range Mean acre) 19.8 1 000 1 0.64 - 0.85 0.73 Ford, 1980 8 0.50 - 0.53 0.51 14 0.43 - 0.48 0.46 28 0.26 - 0.31 0.29 56 0.15 - 0.16 0.15 112 0.06 - 0.08 0.07 147 0.05 - 0.05 0.05 4.5 300 1 0.19 - 0.27 0.25 Ford, 1981b 8 0.10 - 0.15 0.13 15 0.12 - 0.14 0.13 29 0.09 - 0.12 0.10 43 0.08 - 0.12 0.10 9 300 1 0.39 - 0.45 0.41 Ford, 1981b 8 0.23 - 0.34 0.28 15 0.23 - 0.28 0.26 29 0.13 - 0.16 0.14 43 0.14 - 0.16 0.15 TABLE 9. Amitraz and BTS 27 271 Residues in Oranqes from Supervised Trials, Japan1 Residue (mg/kg) 2 Reference Interval Compound (days) analysed Peel Pulp Whole fruit 20 Amitraz 0.01 <0.007 <0.01 Takano, BTS 27 271 0.77 0.176 0.35 1974 30 Amitraz 0.01 <0.007 <0.01 BTS 27 271 0.46 0.116 0.19 40 Amitraz - - - BTS 27 271 0.26 0.098 0.13 50 Amitraz - - - BTS 27 271 0.08 0.073 0.07 1 Spray concentration 0.02% amitraz. 2 Residues of amitraz and BTS 27 271 analysed separately. TABLE 10. Amitraz Residues in Oranges from Supervised Trials, Japan Spray Part No. of Interval Residue volume1 analysed applications (days) (mg/kg)2 Reference (1/ha) Lab.A Lab. B 8 000 Flesh 0 - <0.01 <0.01 Nissan & 2 15 <0.01 <0.01 Boots, 2 30 <0.01 <0.01 1972 3 7 <0.01 <0.01 3 15 <0.01 <0.01 3 30 <0.01 <0.01 Peel 0 - <0.01 <0.01 2 15 <0.01 0.01 2 30 <0.01 0.01 3 7 0.09 0.10 3 15 0.10 0.07 3 30 0.02 0.02 6 000 Flesh 0 - <0.01 <0.01 2 15 <0.01 <0.01 2 30 <0.01 <0.01 3 7 <0.01 <0.01 3 15 <0.01 <0.01 3 30 <0.01 <0.01 Peel 0 - <0.01 <0.01 2 15 <0.01 <0.01 2 30 <0.01 <0.01 3 7 0.08 0.08 3 15 <0.01 <0.01 3 30 <0.01 <0.01 1 Spray concentration 0.01% amitraz. 2 Residue determined as amitraz alone. TABLE 11. Amitraz Residues in Oranges from Supervised Trials, China1 Residues (mg/kg) Interval Applications Days Peel Pulp Whole fruit Range Mean Range Mean Range Mean 1 0 0.98-1.13 1.04 0.026-0.046 0.034 0.44-0.51 0,47 20 0.50-0.60 0.56 0.015-0.063 0.059 0.21-0.25 0.23 40 0.31-0.55 0.42 0.068-0.083 0.074 0.15-0.27 0.20 2 0 1.25-1.94 1.66 0.08-0.10 0.09 0.58-0.63 0.61 7 1.12-1.27 1.20 0.09-0.13 0.11 0.38-0.44 0.41 14 0.83-0.95 0.89 0.09-0.13 0.11 0.28-0.32 0.30 2 20 0.74-0.82 0.77 0.09-0.17 0.12 0.24-0.32 0.28 25 0.68-0.73 0.71 0.13-0.16 0.15 0.27-0.29 0.28 30 0.63-0.69 0.66 0.13-0.13 0.13 0.24-0.24 0.24 35 0.57-0.73 0.65 0.10-0.15 0.13 0.22-0.27 0.25 40 0.73-0.82 0.77 0.13-0.16 0.15 0.28-0.30 0.29 1 Spray concentration 0.01% amitraz; application rate 2 600 l/ha; residues determined by "total residue" method. TABLE 12. Amitraz Residues in Oranges from Supervised Trials, China1 Residues (mg/kg) Interval Applications Days Peel Pulp Whole fruit Range Mean Range Mean Range Mean 1 0 1.83-1.91 1.88 0.004-0.008 0.006 0.72-0.83 0.77 20 0.55-0.62 0.58 0.06-0.11 0.09 0.24-0.29 0.27 40 0.26-0.43 0.33 0.05-0.08 0.07 0.13-0.19 0.16 2 0 1.47-1.56 1.51 0.06-0.10 0.08 0.53-0.54 0.54 20 0.46-0.50 0.48 0.13-0.14 0.13 0.23-0.31 0.26 40 0.36-0.38 0.37 0.10-0.14 0.12 0.18-0.20 0.19 1 0 1.11-1.13 1.12 0.014-0.016 0.015 0.49-0.54 0.51 20 0.57-0.59 0.58 0.08-0.12 0.10 0.27-0.29 0.28 40 0.36-0.53 0.46 0.06-0.09 0.08 0.16-0.24 0.20 2 0 1.29-1.95 1.61 0.08-0.09 0.09 0.24-0.70 0.50 20 0.35-0.36 0.36 0.09~0.13 0.11 0.17-0.19 0.18 40 0.25-0.32 0.28 0.07-0.08 0.07 0.12-0.15 0.13 1 Spray concentration 0.01% amitraz; application rate 3 000 l/ha; residues determined by "total residue" method. (Grower 2) with the corresponding total amitraz-derived residues being 0.14 and 0.35 mg/kg. Expressed as a percentage of the total amitraz-derived residue, the BTS 24 868 residues ranged from 15.6 to 18.3 percent. This is outside the range of artefactual conversion of the known metabolites to BTS 24 868 and, therefore, indicates that approximately 50 percent of the BTS 24 868 residues in peel are "true" residues. However, when calculated on a whole fruit basis by combining the results from peel and flesh, a maximum value of less than 0.01 mg/kg BTS 24 868 was obtained (McGibbon, 1984b). Pear A method has been developed for the analysis of 2,4-dimethylaniline residues (BTS 24 868) in pears. The recoveries of BTS 24 868 from control pears ('Williams','Bon Chretian' and 'Conference'), fortified at either 0.1 or 0.05 mg/kg, gave an over-all mean and standard deviation of 74.3 ± 12.4 percent. Mean BTS 24 868 residues in control pears fortified with 0.5 mg/kg of either amitraz, BTS 27 271 or BTS 27 919 were found to range from 0.006 to 0.018 mg/kg (equivalent to 1.5 to 4.3 percent conversion of the parent compounds to BTS 24 868). The mean residues of BTS 24 868 in commercially-grown pears treated with amitraz under normal field practice ranged from 0.002 to 0.005 mg/kg, with a minimum detectable level estimated at 0.001 mg/kg. The level of total amitraz-derived residues in the treated pears was found to be in the range 0.10 - 0.20 mg/kg. The ratio of BTS 24 868 residues in the treated fruit to the total amitraz-derived residue was calculated as 1.2 to 3.9 percent. This is within the range of artefactual conversion of coexisting amitraz and its metabolites. It follows, therefore, that there is no evidence to suggest that specific BTS 24 868 residues exist in the treated pears (McGibbon, 1984a). Citrus and Processed By-products Studies have been conducted on the distribution of amitraz residues in citrus and on the effects of processing. In 'Valencia' and 'Navel' oranges, approximately 80 percent of the residue present at harvest was in or on the peel. Residues were more evenly distributed in 'Hamlin' oranges, primarily because of their thinner peel. In grapefruit, approximately 90 percent of the residue occured in the peel. These studies are summarized in Table 13. In processing studies dry citrus pulp from processed oranges contained residues some four to seven times higher than in fresh fruit. Residues in citrus molasses were approximately 50 percent lower than those in dry pulp. The remaining fractions contained levels at or below those detected in fresh fruit. TABLE 13. Amitraz Residues in Citrus Peel and Flesh from Supervised Trials Amitraz (mg/kg) Fruit Application Days variety rate after Peel Whole Peel Edible Flesh Reference (% a.i.) application (%) fruit flesh (%) Valencia 0.03 58 27.4 0.31 0.92 0.06 15 Ford, 1981a orange Navel 0.03 112 29.4 0.08 0.20 0.04 32 Ford, 1981a orange Navel 0.03 x 2 57 32.2 0.45 1.35 0.05 7 Ford, 1981a orange Hamlin 0.015 145 20.8 0.057 0.11 0.038 53 Ford, 1980 orange 0.015 + oil 145 22.2 0.096 0.20 0.067 55 0.015 145 20.2 0.045 0.10 0.031 53 0.015 + oil 145 20.2 0.051 0.10 0.030 47 Grapefruit 0.01 1 31.3 0.19 0.62 0.005 1.7 Ford, 1980 8 28.1 0.14 0.44 0.007 3.9 15 25.8 0.11 0.44 0.011 6.7 29 26.0 0.07 0.24 0.010 10.6 43 27.9 0.07 0.27 0.015 12.6 0.02 1 37.0 0.37 0.88 0.002 0.4 8 28.9 0.27 0.65 0.008 2.9 15 27.7 0.15 0.53 0.012 5.6 29 30.2 0.16 0.37 0.018 9.4 43 28.8 0.12 0.35 0.015 9.6 FATE OF RESIDUES In Plants Previous studies (FAO/WHO, 1981b) have shown that amitraz degrades rapidly to yield predominantly BTS 27 271 [N-(2,4-dimethylphenyl)-N'-methylformamidine] and smaller amounts of BTS 27 919 (2,4-dimethylformanilide). Pears Radiolabelled amitraz was applied to commercially grown pears (var. 'Conference') at two sites in the United Kingdom (Levington and Nottingham). An E.C. formulation was used at a spray concentration of 0.06 percent a.i. (i.e. identical to that used in the United States). Samples of fruit were analysed at maturity 29 days (Levington) and 61 days (Nottingham) after treatment. At harvest, 48.2 percent of the applied radioactivity remained in the fruit, of which BTS 27 271 (14.0 percent) and BTS 27 919 (5.3 percent) were the main metabolites characterized. Amitraz accounted for less than 1 percent, with BTS 24 868 and BTS 28 037 (N,N'-bis-dimethylphenylformamidine) each comprising a further 1.2 percent, although in the case of BTS 24 868 the amount detected may well be artefactual. Uncharacterized polar compounds accounted for 34.8 percent, while the remainder of the radioactivity (41.0 percent was fibre-bound (McGibbon & Kelly, 1984b). Lemons Amitraz was applied to the fruit of lemon trees (cv. 'Four Seasons') maintained under glass. An E.C. formulation was used at a spray concentration of 0.06 percent a.i. Samples of fruit were harvested at maturity 32 days after treatment. At harvest, 89.5 percent of the applied radioactivity remained in or on the fruit, of which 72.5 percent was found in the peel. BTS 27 271 (27.2 percent) and BTS 27 919 (9.0 percent) were the main metabolites characterized. Unchanged amitraz comprised 12.4 percent, while BTS 28 037 and BTS 24 868 accounted for 2.2 and 2.8 percent, respectively, of the total radioactivity recovered, with the possibility that BTS 24 868 was produced as an artefact. Uncharacterized polar compounds accounted for 25.1 percent while the remainder of the radioactivity (13.2 percent) was fibre-bound. (McGibbon & Kelly, 1984a). These new data confirm the previous findings that amitraz is metabolized within a relatively short time. The major metabolites remaining at harvest are BTS 27 271 and BTS 27 919. The presence of any significant residues of BTS 24 868 is not indicated by either the metabolism studies or the investigations aimed at specific analysis for residues of the metabolite. A diagrammatic representation of the metabolism of amitraz in plants is given in Figure 1.NATIONAL MAXIMUM RESIDUE LIMITS The following MRLs from the Netherlands were reported to the meeting: Pome fruit 0.5 mg/kg Strawberries 0.05 mg/kg Bell peppers 0.2 mg/kg Eggplant 0.2 mg/kg Tomatoes 0.2 mg/kg Milk 0.05 mg/kg Meat 0.05 mg/kg Other food 0 (0.05) mg/kg Limits include and are expressed as N-2,4-dimethylphenyl-N-methylformamidine. APPRAISAL The meeting examined new residues data on citrus fruit and noted that with a 14-day interval between last application and harvest, most residue levels were less than the temporary MRL for oranges of 0.5 mg/kg (for amitraz plus N-2,4-dimethylphenyl-N'- methylformamidine), even at the relatively high rates of use in the trials in the United States (and approved under an experimental use permit). The meeting confirmed its previous estimate. Although the maximum residues in some citrus samples were about 2 mg/kg, it is not known if the high rates used will be recognized as good agricultural practice and the meeting, therefore, decided not to include these in its evaluation. REFERENCES Ford, J.J. Persistence of amitraz on Florida-grown Hamelin oranges. 1980 Report RI 34-017-06 (R 82) submitted by FBC to FAO. (Unpublished) Ford, J.J. Persistence of the acaricide amitraz on California Citrus - 1981a Part II. Report RESID/82/15 (R 133) submitted by FBC to FAO. 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See Also: Toxicological Abbreviations Amitraz (ICSC) Amitraz (Pesticide residues in food: 1980 evaluations) Amitraz (Pesticide residues in food: 1983 evaluations) Amitraz (Pesticide residues in food: 1984 evaluations) Amitraz (JMPR Evaluations 1998 Part II Toxicological)