Grapes. Several grape trials were carried out in Australia during the years 1992 to 1995, but in all of them the application rates or the number of applications or both were higher than those specified in proposed GAP.
The trials in 1992-1993 were with high volume sprays to the point of run-off. The reported residues are the averages of samples from duplicate trials at the same rates (Anderson, 1993). The 1994-1995 trials were also with high-volumes prays applied to the foliage (Armstrong, 1995).
In a large number of trials with red and white grapes at different locations in France between 1990 and 1992 (Gocha, 1995a) the plot sizes ranged from 11 m2 to 48 m2 with 5 to 22 vines in each plot. Most trials were with 4 replicates while some others were single or in duplicate. One or two applications were made. Samples were harvested at intervals of 0 to 89 days after the (last) application. Only a few of these trials were according to GAP. The original GLC method used in 1990 measured tebufenozide residues with an LOD of 0.04 mg/kg. The extraction and methylation steps were slightly modified for the 1991 analyses to reach an LOD of 0.025 mg/kg. In 1992, using different chromatographic and methylation conditions, the laboratory was able to reach an LOD of 0.01 mg/kg in both solid and liquid substrates. This method was validated (Mellet, 1993a). Grape samples from two trials were processed to wine or spirit.
Three trials in France in 1992 for processing studies (DeWilde et al., 1995a) were conducted with treated and untreated plots without replicates. The plot sizes were chosen according to the quantity of sample to be harvested but were not less than 1 ha. Two trials in 1993 in France for processing studies (DeWilde et al., 1995b) complied with GAP. The plot sizes were not less than 1.4 ha. Applications were made with a motorized knapsack sprayer. Samples were harvested when the grapes reached the maturity required for commercial wine production.
The residues in the trials which accorded with French GAP ranged from 0.05 to 0.28 mg/kg.
Five trials in Germany were according to proposed GAP (Ulrich et al., 1994). The plot sizes were not less than 0.58 ha. The applications were carried out with a motorized knapsack sprayer. At the last sampling about 200 kg of grapes were taken from at least 30 vines from two trials for processing to must and wine. Samples were analysed by GLC. Four similar trials, again according to proposed GAP, were carried out by Kaiser (1994).
Residues in the grapes from the German trials at the proposed 28-day PHI ranged from 0.21 to 0.5 mg/kg.
Four trials at two different locations in Italy (Kaiser and Holzwarth, 1994) were at excessive rates and the grapes were vinified. The limit of determination was 0.02 mg/kg for grapes, and 0.01 mg/kg for must, new wine and potable wine.
Two trials in Thailand (Ishii and Higuchi, 1995) were not according to GAP or GLP. The results of the supervised trials on grapes are shown in Table 24. Table 24. Residues of tebufenozide in grapes. Underlined residues are from treatments according to GAP.
Country, year |
Form. |
Application |
PHI, days |
Residue, mg/kg |
Ref, comments |
||
No. |
kg ai/ha |
kg ai/hl |
|||||
Australia |
SC |
5 |
0.044-0.12 |
0.006 |
0 |
1.31 |
Anderson, 1993 |
1992-1993 |
|
|
|
|
7 |
1.01 |
|
|
|
|
|
|
14 |
0.821 |
|
|
|
|
|
|
28 |
0.571 |
|
Australia |
SC |
5 |
0.129-0.192 |
0.010 |
0 |
1.91 |
Anderson, 1993 |
1992-1993 |
|
|
|
|
7 |
1.51 |
|
|
|
|
|
|
14 |
1.21 |
|
|
|
|
|
|
28 |
0.871 |
|
Australia |
WP |
5 |
0.036 |
0.006 |
0 |
1.0 |
Armstrong, 1995a |
1994-1995 |
|
|
l |
|
7 |
0.98 |
|
|
|
|
|
|
14 |
0.7 |
|
|
|
|
|
|
28 |
0.32 |
|
Australia |
WP |
5 |
0.058 |
0.010 |
0 |
1.6 |
Armstrong, 1995a |
1994-1995 |
|
|
|
|
7 |
2.0 |
|
|
|
|
|
|
14 |
1.7 |
|
|
|
|
|
|
28 |
1.12 |
|
Australia |
SC |
5 |
0.036 |
0.006 |
0 |
1.1 |
Armstrong, 1995a |
1994-1995 |
|
|
|
|
7 |
1.9 |
|
|
|
|
|
|
14 |
0.9 |
|
|
|
|
|
|
28 |
0.5 |
|
Australia |
SC |
5 |
0.058 |
0.010 |
0 |
1.2 |
Armstrong, 1995a |
1994-1995 |
|
|
|
|
7 |
0.63 |
|
|
|
|
|
|
14 |
0.9 |
|
|
|
|
|
|
28 |
0.42 |
|
Australia |
WP |
5 |
0.09-0.15 |
0.006 |
0 |
0.61 |
Armstrong, 1995a |
1994-1995 |
|
|
|
|
7 |
1.4 |
|
|
|
|
|
|
14 |
1.3 |
|
|
|
|
|
|
28 |
0.71 |
|
Australia |
WP |
5 |
0.144-0.24 |
0.010 |
0 |
1.6 |
Armstrong, 1995a |
1994-1995 |
|
|
|
|
7 |
2.0 |
|
|
|
|
|
|
14 |
1.2 |
|
|
|
|
|
|
28 |
1.8 |
|
Australia |
SC |
5 |
0.09-0.15 |
0.006 |
0 |
1.4 |
Armstrong, 1995a |
1994-1995 |
|
|
|
|
7 |
1.1 |
|
|
|
|
|
|
14 |
1.2 |
|
|
|
|
|
|
28 |
1.1 |
|
Australia |
SC |
5 |
0.144-0.24 |
0.010 |
0 |
1.96 |
Armstrong, 1995a |
1994-1995 |
|
|
|
|
7 |
2.4 |
|
|
|
|
|
|
14 |
1.3 |
|
|
|
|
|
|
28 |
1.67 |
|
France |
SC |
1 |
0.10 |
0.10 |
65 |
0.08 |
Gocha, 1995a |
1990 |
SC |
2 |
0.05 |
0.05 |
53 |
0.13 |
LOD 0.04 mg/kg |
France |
SC |
1 |
0.10 |
0.10 |
89 |
0.09 |
Gocha, 1995a |
1990 |
SC |
2 |
0.05 |
0.05 |
76 |
0.04 |
|
France |
SC |
1 |
0.10 |
0.10 |
78 |
0.29 |
Gocha, 1995a |
1990 |
SC |
2 |
0.050 |
0.050 |
64 |
0.21 |
|
France |
SC |
1 |
0.10 |
|
71 |
0.05 |
Gocha, 1995a |
1990 |
SC |
1 |
0.150 |
|
71 |
0.09 |
|
France |
SC |
2 |
0.15 |
0.05 |
29 |
0.43 |
Gocha, 1995a |
1990 |
SC |
2 |
0.20 |
0.07 |
29 |
0.25 |
|
|
SC |
2 |
0.15 |
0.05 |
22 |
0.56 |
|
France |
SC |
2 |
0.15 |
0.04 |
18 |
0.19 |
Gocha, 1995a |
1990 |
SC |
2 |
0.20 |
0.05 |
18 |
0.12 |
|
|
SC |
2 |
0.15 |
0.04 |
12 |
0.16 |
|
France |
SC |
1 |
0.15 |
0.05 |
74 |
<0.04 |
Gocha, 1995a |
1990 |
SC |
1 |
0.15 |
0.05 |
81 |
<0.04 |
|
|
SC |
1 |
0.20 |
0.06 |
81 |
<0.04 |
|
France |
SC |
1 |
0.10 |
0.022 |
77 |
0.05 |
Gocha, 1995a |
1990 |
SC |
1 |
0.15 |
0.033 |
77 |
0.07 |
|
France |
SC |
1 |
0.10 |
0.10 |
48 |
0.17 |
Gocha, 1995a |
1990 |
SC |
1 |
0.20 |
0.20 |
48 |
0.20 |
|
France 1990 |
SC |
1 |
0.096 |
0.042 |
56 |
<0.04 |
Gocha, 1995a |
France 1990 |
SC |
1 |
0,096 |
0.046 |
56 |
<0.04 |
Gocha, 1995a |
France 1990 |
SC |
1 |
0.096 |
0.064 |
77 |
0.06 |
Gocha, 1995a |
France 1990 |
SC |
1 |
0.096 |
0.064 |
38 |
0.08 |
Gocha, 1995a |
France |
SC |
2 |
0.100 |
0.100 |
0 |
0.33 |
Gocha, 1995a |
1990 |
|
|
|
|
7 |
0.23 |
|
|
|
|
|
|
14 |
0.26 |
|
|
|
|
|
|
29 |
0.43 |
|
|
|
|
|
|
58 |
0.24 |
|
France |
SC |
2 |
0.100 |
0,050 |
0 |
0.29 |
Gocha, 1995a |
1990 |
|
|
|
|
7 |
0.53 |
|
|
|
|
|
|
14 |
0.49 |
|
|
|
|
|
|
30 |
0.21 |
|
|
|
|
|
|
45 |
0.19 |
|
|
|
|
|
|
60 |
0.18 |
|
France |
SC |
1 |
0.20 |
0.10 |
80 |
0.19 |
Gocha, 1995a |
1990 |
SC |
1 |
0.40 |
0.20 |
80 |
0.32 |
LOD 0.025 mg/kg |
France |
SC |
1 |
0.144 |
0.021 |
66 |
0.05 |
|
1991 |
SC |
1 |
0.12 |
0.018 |
59 |
0.06 |
|
|
SC |
1 |
0.144 |
0.021 |
59 |
0.07 |
|
France |
SC |
1 |
0.144 |
0.048 |
0 |
0.14 |
Gocha, 1995a |
1991 |
SC |
1 |
0.144 |
0.048 |
2 |
0.13 |
|
|
SC |
1 |
0.144 |
0.048 |
7 |
0.05 |
|
|
SC |
1 |
0.144 |
0.048 |
14 |
0.05 |
|
|
SC |
1 |
0.144 |
0.048 |
21 |
0.05 |
|
France |
SC |
1 |
0.144 |
0.041 |
58 |
0.03 |
Gocha, 1995a |
1991 |
SC |
1 |
0.12 |
0.034 |
50 |
0.05 |
|
|
SC |
1 |
0.144 |
0.041 |
50 |
0.03 |
|
France |
SC |
1 |
0.10 |
0.067 |
78 |
<0.025 |
Gocha, 1995a |
1991 |
SC |
1 |
0.10 |
0.067 |
78 |
0.72 |
|
|
SC |
1 |
0.125 |
0.083 |
78 |
0.04 |
|
|
SC |
1 |
0.125 |
0.083 |
78 |
0.07 |
|
France |
SC |
1 |
0.144 |
0.032 |
72 |
0.14 |
Gocha, 1995a |
1991 |
SC |
1 |
0.12 |
0.027 |
61 |
0.13 |
|
|
SC |
1 |
0.144 |
0.032 |
61 |
0.17 |
|
France |
SC |
1 |
0.12 |
0.040 |
66 |
0.09 |
Gocha, 1995a |
1991 |
SC |
1 |
0.144 |
0.048 |
66 |
0.11 |
|
France |
SC |
1 |
0.144 |
0.048 |
20 |
0.24 |
Gocha, 1995a |
1992 |
SC |
1 |
0.144 |
0.048 |
29 |
0.13 |
LOD 0.01 mg/kg |
|
SC |
1 |
0.144 |
0.048 |
39 |
0.44 |
|
France |
SC |
1 |
0.144 |
0.048 |
21 |
0.12 |
Gocha, 1995a |
1992 |
SC |
1 |
0.144 |
0.048 |
30 |
0.07 |
|
|
SC |
1 |
0.144 |
0.048 |
56 |
0.08 |
|
France |
SC |
1 |
0.144 |
0.044 |
21 |
0.06 |
Gocha, 1995a |
1992 |
SC |
1 |
0.144 |
0.044 |
30 |
0.04 |
|
|
SC |
1 |
0.144 |
0.044 |
61 |
0.14 |
|
France |
SC |
1 |
0.144 |
0.048 |
0 |
0.72 |
Gocha, 1995a |
1992 |
SC |
2 |
0.144 |
0.048 |
3 |
0.81 |
|
|
|
|
|
|
7 |
0.9 |
|
|
SC |
2 |
0.144 |
0.048 |
14 |
0.29 |
|
|
|
|
|
|
21 |
0.07 |
|
France 1992 |
SC |
2 |
0.144 |
0.048 |
21 |
0.28 |
Gocha, 1995a |
France |
SC |
2 |
0.144 |
0.048 |
14 |
0.68 |
Gocha, 1995a |
1992 |
|
|
|
|
|
0.81 |
|
France 1992 |
SC |
2 |
0.144 |
0.048 |
7 |
1.07 |
Gocha, 1995a |
France |
SC |
2 |
0.144 |
0.048 |
3 |
3.7 |
Gocha, 1995a |
1992 |
|
|
|
|
|
2.7 |
|
France 1992 |
SC |
2 |
0.144 |
0.048 |
0 |
4.2 |
Gocha, 1995a |
France 1992 |
SC |
1 |
0.144 |
0.048 |
65 |
0.04 |
Gocha, 1995a |
France 1992 |
SC |
2 |
0.144 |
0.048 |
30 |
0.05 |
Gocha, 1995a |
France 1992 |
SC |
2 |
0.144 |
0.048 |
21 |
0.26 |
Gocha, 1995a |
France 1992 |
SC |
2 |
0.144 |
0.144 |
50 |
0.17 |
Gocha, 1995a |
France |
SC |
3 |
0.144 |
0.096 |
40 |
0.18 |
DeWilde, 1995a |
1992 |
|
|
|
|
|
|
average of 2 analyses |
France |
SC |
3 |
0.144 |
0.048 |
41 |
0.06 |
DeWilde, 1995a |
1992 |
|
|
|
|
|
|
average of 2 analyses |
France |
SC |
3 |
0.144 |
0.048 |
25 |
0.08 |
DeWilde, 1995a |
1992 |
|
|
|
|
|
|
average of 2 analyses |
France |
SC |
3 |
0.144 |
0.048 |
19 |
0.18 |
DeWilde, 1995b |
1993 |
|
|
|
|
|
|
average of 2 analyses |
France 1993 |
SC |
3 |
0.144 |
0.048 |
21 |
0.28 |
DeWilde, 1995b |
Germany |
SC |
4 |
0.079-0.206 |
0.013-0.040 |
0 |
0.59 |
Ulrich, 1994 |
1992 |
|
|
|
|
7 |
0.48 |
LOD 0.02 mg/kg |
|
|
|
|
|
14 |
1.1 |
|
|
|
|
|
|
28 |
0.28 |
|
Germany |
SC |
4 |
0.074-0.196 |
0.013-0.040 |
0 |
0.37 |
Ulrich, 1994 |
1992 |
|
|
|
|
7 |
0.20 |
LOD 0.02 mg/kg |
|
|
|
|
|
14 |
0.44 |
|
|
|
|
|
|
28 |
0.5 |
|
Germany |
SC |
4 |
0.075-0.210 |
0.0130.040 |
0 |
0.5 |
Ulrich, 1994 |
1992 |
|
|
|
|
7 |
0.28 |
LOD 0.02 mg/kg |
|
|
|
|
|
14 |
0.79 |
|
|
|
|
|
|
28 |
0.24 |
|
Germany |
SC |
4 |
0.074-0.204 |
0.013-0.040 |
0 |
0.33 |
Ulrich, 1994 |
1992 |
|
|
|
|
7 |
0.53 |
LOD 0.02 mg/kg |
|
|
|
|
|
14 |
0.47 |
|
|
|
|
|
|
28 |
0.27 |
|
Germany |
SC |
4 |
0.075-0.207 |
0.013-0.040 |
0 |
0.54 |
Ulrich, 1994 |
1992 |
|
|
|
|
7 |
0.57 |
|
|
|
|
|
|
14 |
0.4 |
|
|
|
|
|
|
28 |
0.40 |
|
Germany |
SC |
4 |
0.070-0.200 |
0.012-0.036 |
0 |
0.52 |
Kaiser, 1994a |
1993 |
|
|
|
|
7 |
0.95 |
LOD 0.02 mg/kg |
|
|
|
|
|
14 |
0.16 |
|
|
|
|
|
|
28 |
0.21 |
|
Germany |
SC |
4 |
0.076-0.197 |
0.012-0.036 |
0 |
0.33 |
Kaiser, 1994a |
1993 |
|
|
|
|
7 |
0.50 |
LOD 0.02 mg/kg |
|
|
|
|
|
14 |
0.15 |
|
|
|
|
|
|
28 |
0.26 |
|
Germany |
SC |
4 |
0.070-0.193 |
0.012-0.036 |
0 |
0.46 |
Kaiser, 1994a |
1993 |
|
|
|
|
7 |
0.42 |
LOD 0.02 mg/kg |
|
|
|
|
|
14 |
0.64 |
|
|
|
|
|
|
28 |
0.22 |
|
Germany |
SC |
4 |
0.072-0.196 |
0.012-0.036 |
0 |
0.46 |
Kaiser, 1994a |
1993 |
|
|
|
|
7 |
0.32 |
LOD 0.02 mg/kg |
|
|
|
|
|
14 |
0.28 |
|
|
|
|
|
|
28 |
0.42 |
|
Italy |
SC |
2 |
0.238-0.240 |
0.012 |
0 |
0.5 |
Kaiser, 1994b |
1992 |
|
|
|
|
21 |
0.56 |
|
Italy |
SC |
2 |
0.48 |
0.024 |
0 |
0.8 |
Kaiser, 1994b |
1992 |
|
|
|
|
21 |
0.86 |
|
Italy |
SC |
2 |
0.216-0.240 |
0.012 |
0 |
0.37 |
Kaiser, 1994b |
1992 |
|
|
|
|
21 |
0.26 |
|
Italy |
SC |
2 |
0.48 |
0.024 |
0 |
0.72 |
Kaiser, 1994b |
1992 |
|
|
|
|
21 |
0.84 |
|
Thailand |
SC |
8 |
0.10 |
0.005 |
0 |
0.91 |
Ishii, 1995a |
1994 |
|
|
|
|
7 |
0.52 |
LOD ± 0.01 mg/kg |
|
|
|
|
|
14 |
0.15 |
|
|
|
|
|
|
21 |
0.18 |
|
|
|
|
|
|
35 |
0.14 |
|
Thailand |
SC |
8 |
0.10 |
0.005 |
0 |
0.53 |
Ishii, 1995a |
1994 |
|
|
|
|
7 |
0.20 |
LOD 0.01 mg/kg |
|
|
|
|
|
14 |
0.10 |
|
|
|
|
|
|
21 |
0.18 |
|
1 Mean of duplicate trials