Residues resulting from supervised trials

Supervised trials data were available on residues of flumethrin in the milk of cattle, sheep and goats and the tissues of cattle and sheep, and for residues of the metabolite flumethrin acid (BFN 553A) in the tissues of cattle. Data were also provided on residues in honey and beeswax from supervised trials in bee hives.

Cattle (Tables 7-10). Supervised trials were reported from Australia, South Africa, Germany and Japan, with applications by dipping, spraying and pour-on. The Meeting was informed of additional Australian studies to be completed in 1996.

Table 7.	Flumethrin residues in cattle fat from 1994-95 Australian trials. Australian government submission.
Table 8.	Flumethrin residues in cattle tissues (including older Australian trials). Submissions by the manufacturer.
Table 9.	Flumethrin acid (metabolite BNF 5533A) residues in cattle tissues. Submission by the manufacturer (trials conducted in accordance with GLP).
Table 10.	Flumethrin residues in cattle milk. Submission by the manufacturer.

Table 7. Flumethrin residues in loin (subcutaneous) and renal fat of cattle from 1994-95 supervised trials in Australia (Webster et al., 1996; Queensland and New South Wales, 1996)

Pre-slaughter interval, days	Sample	Residues, mg/kg, after indicated treatment
Plunge Dips1		Treatment2
		D1	D2	D3	D4
2	Loin fat	<0.005	-	<0.005	<0.005
		<0.005	-	<0.005	<0.005
		0.041	-	<0.005	<0.005
	Renal fat	<0.005	-	<0.005	<0.005
		<0.005	-	<0.005	<0.005
		0.047	-	<0.005	<0.005
4	Loin fat	<0.005 (3)3	<0.005 (3)	<0.005 (3)	<0.005 (3)
	Renal fat	<0.005 (3)	<0.005(2)	<0.005 (3)	<0.005 (3)
			0.006
7	Loin fat	<0.005 (3)	<0.005 (3)	<0.005 (3)	<0.005 (3)
	Renal fat	<0.005 (3)	<0.005 (3)	<0.005 (3)	<0.005 (3)
15	Loin fat	<0.005 (3)	<0.005 (3)	<0.005 (3)	<0.005 (3)
	Renal fat	<0.005	<0.005	<0.005	<0.005
		0.008	<0.005	<0.005	<0.005
		<0.005	<0.005	<0.005	<0.005
21	Loin fat	All 12 residues <0.005
	Renal fat	All 12 residues <0.005
30	Loin fat	<0.005	<0.005	<0.005	0.009
		<0.005	<0.005	<0.005	<0.005
		<0.005	<0.005	<0.005	<0.005
	Renal fat	<0.005	<0.005	0.011	0.013
		<0.005	<0.005	<0.005	<0.005
		<0.005	<0.005	<0.005	<0.005

Pre-slaughter interval, days	Sample	Residues, mg/kg, after indicated treatment
Pour-on applications4		Treatment
		P1	P2
2	Loin fat	<0.005	0.015
		<0.005	0.014
		<0.005	0.013
	Renal fat	<0.005	0.04
		<0.005	0.034
		<0.005	0.023
4	Loin fat	0.023	0.028
		<0.005	0.025
		0.029 [0.04]5	0.023
	Renal fat	0.032	0.058
		<0.005	0.022
		0.026 [0.04]5	0.035
7	Loin fat	0.013 [0.015]5	0.031
		0.011	0.018
		0.008	0.019
	Renal fat	0.015 [0.015]5	0.037
		0.020	0.036
		0.015	0.022
10	Loin fat	<0.005	0.022
		0.014	0.022
		0.009	0.029
	Renal fat	<0.005	0.044
		0.019	0.038
		0.014	0.097
15	Loin fat	0.011	0.052
		0.007	0.020
		0.011	0.020
	Renal fat	0.012	0.14 (confirmed)
		0.014	0.038
		0.034	0.035
21	Loin fat	0.006	0.017
		0.008	0.011
		0.040 [0.06]5	0.016
		0.017 [0.025]5	0.015
		0.010	0.022
		0.029	0.019
	Renal fat	0.014	0.036
		0.021	0.026
		0.11 [0.06]5	0.049
		0.024 [0.025]5	0.026
		0.014	0.054
		0.042	0.033
30	Loin fat	0.020	0.014
		0.008	0.017
		0.008	0.020
	Renal fat	0.027	0.027
		0.029	0.030
		0.011	0.027
45	Loin fat	<0.005	0.023
		<0.005	0.012
		0.009	0.029
	Renal fat	0.018	0.051
		0.024	0.028
		0.020	0.044

¹ Generally 3 animals for each treatment and pre-slaughter interval, each sample from a different fat depth and the renal fat values corresponding successively to the loin fat values.

² D1: dipped once according to GAP.

D2: dipped twice, but the animals were also used to stir the dip. Complied with GAP.

D3: dipped twice. Not strictly GAP because retreatment interval was 3 days and GAP minimum is 10 days.

D4: dipped twice, but the animals were used as stirrers for both dips. Not strictly GAP because the retreatment interval was 7 days instead of minimum of 14 days implied by label.

P1: one application according to GAP.

P2: two applications at 7-day interval. GAP interval is 14 days.

³ Numbers in parentheses are the numbers of samples with the same residues.

⁴ At GAP rate of 10 g ai/l and according to label instructions requiring 1.5 to 3.6 mg/kg bw, according to the weight of the animals (see Table 6).

⁵ Values in square brackets are means of replicate analyses of fat from core samples of cartons of frozen product (same carcases) as distinct from loin and renal fat samples taken at slaughter.

Dip concentrations were checked by analysis before treatment. The multi-residue GLC method used is described in "Analytical methods". Although the reported limit of detection was 0.01 mg/kg, undetectable residues are recorded as <0.005 mg/kg. No information was provided on the length of time from slaughter to analysis, although the time from the start of the study until the final report was less than 14 months. The protocol called for sample storage at -40°C.

Figure 2 shows the variation of residues of flumethrin in loin and renal fat with time after one or two pour-on applications at GAP rates.

Figure 2. Average residues of flumethrin in loin (subcutaneous) fat and renal fat from one or two pour-on applications to cattle at GAP rates (Queensland and New South Wales, 1996).

Table 8. Residues of flumethrin in cattle tissues from supervised trials.

Table 8. Residues of flumethrin in cattle tissues from supervised trials. (a)

Table 8. Residues of flumethrin in cattle tissues from supervised trials. (b)

Table 8. Residues of flumethrin in cattle tissues from supervised trials. (c)

¹ Numbers correspond to tab numbers in 1996 Bayer submission, Vol. III:

24. Amelsfoort, 1984a; 25. Amelsfoort, 1984b; 26. Amelsfoort, 1984c; 28. Dorn and Maasfeld, 1989a; 32. Hopkins and Lindsay, 1981; 34. Lindsay and Hopkins, 1984; 36. Lindsay, 1983b; 40. Terblanche, 1980a.

² Duplicate analyses on each cow. Results are means of duplicates.
³ Reference 40 fat was described as perirenal fat, references 28 and 36 as "fat" and the rest "minced fat".

Table 9. Residues of flumethrin acid (BNF 5533A) in cattle tissues from supervised trials with a 1% pour-on flumethrin formulation, Germany, 1994 (Tesch and Doberschütz, 1994).

Treatment	No. of cattle	Pre- slaughter (days)	Flumethrin acid (BNF 5533A), mg/kg1
			fat (suet)2	liver	muscle	kidney
2 x 10 g ai/l, 10 days apart	6	1	0.03	0.05	0.01	0.03(2)
			0.02 (2)	0.04	<0.01(4)	0.02(2)
			<0.01 (2)	0.03	<0.002	<0.01 (2)
			<0.004	0.02
				<0.01
(2 mg/kg bw)	6	2	0.04	0.06	0.01	0,05
			0.02 (3)	0.05	<0.01(3)	0.03
			0.013	0.04	<0.002(2)	0,02
			0.01	0.03(2)		0.01(3)
				0.02
	6	4	<0.004(6)	0.02	<0.01(3)	0.03
				0.01(2)	<0.002(3)	<0.01(5)
				<0.01
				<0.002(2)
	6	7	0.02	0.01 (2)	<0.01	0.02
			<0.01	<0.004 (4)	<0.002(5)	<0.01
			<0.004(4)			<0.002(4)
	6	21	<0.004(6)	<0.004(6)	<0.002(6)	<0.002(6)
	6	35	<0.004(6)	<0.004(6)	<0.002(6)	<0.002(6)

¹ Limit of detection 0.002 mg/kg in kidney and muscle and 0.004 mg/kg in liver and fat; limit of determination 0.01 mg/kg in all tissues.

² Suet = loin or kidney fat

Table 10. Residues of flumethrin in cattle milk from supervised trials with pour-on and spray applications.

Table 10. Residues of flumethrin in cattle milk from supervised trials with pour-on and spray applications. (a)

Table 10. Residues of flumethrin in cattle milk from supervised trials with pour-on and spray applications. (b)

Table 10. Residues of flumethrin in cattle milk from supervised trials with pour-on and spray applications. (c)

¹ Numbers correspond to tab numbers in 1996 Bayer submission. Vol. III:

27. Amelsfoort, 1984d; 29. Dorn and Maasfeld, 1989b; 30. Dorn and Maasfeld, 1989c; 31. Gyr, 1984; 33. Lindsay and Gyr, 1981; 35. Lindsay, 1983a; 37. Lindsay, 1984a; 38. Lindsay, 1984b; 39. Ohta, 1988; 41. Terblanche, 1980b.

² For refs. 29 and 30 the residues are the means of the means of the morning and evening milkings of the 5 cows, except on day 1 where morning (M) and evening (E) means are recorded separately because they differed significantly. After day 2 there were no significant differences between the morning and evening milkings.

³ Calculated by authors from surface areas. Calculation from actual weights gives 1.4-1.6 mg/kg bw.

⁴ Numbers in parentheses following the residues are the numbers of samples with those values.

⁵ This trial is listed here as a spray. The submitted working paper summary lists it as a dip. The original report states that the cattle were "sprayed" with Bay L 6045 "dipwash" using a power spraypump.