CIPAC/4683/R: Walloon Agricultural Research Centre - (CRA-W) Pesticides Research Department
CIPAC/4683/R: Walloon Agricultural Research Centre - (CRA-W) Pesticides Research Department
CIPAC/4683/R: Walloon Agricultural Research Centre - (CRA-W) Pesticides Research Department
REPORT TO CIPAC
by Olivier PIGEON
1
CIPAC/4683/R
1.1 Specificity
The analysis of reagent blanks (method without sample) and untreated net samples in
comparison with the analysis of standard solutions, spiked untreated net samples and
treated net samples showed the absence of compound interfering with the determination of
deltamethrin, deltamethrin R-isomer and piperonyl butoxide.
Representative chromatograms
FID1 A, (RE21898A\001F0201.D)
5.788 - Standard Interne
15.771 - Deltamethrin
90
80
70
60
50
40
30
20
10
0
2 4 6 8 10 12 14 16 min
2
CIPAC/4683/R
FID1 A, (RE21898A\003F0802.D)
90
80
70
15.730 - Deltamethrin
60
50
40
30
20
10
0
2 4 6 8 10 12 14 16 min
FID1 A, (RE21898A\005F1402.D)
5.791 - Standard Interne
pA
90
80
70
60
50
15.692 - Deltamethrin
40
30
20
10
0
2 4 6 8 10 12 14 16 min
3
CIPAC/4683/R
FID1 A, (RE21898A\006F5301.D)
pA
90
80
70
60
50
30
20
10
0
2 4 6 8 10 12 14 16 min
FID1 A, (RE21898A\031F3901.D)
5.787 - Standard Interne
pA
90
80
15.725 - Deltamethrin
70
8.388 - Piperonil Butoxide
60
50
15.111 - Deltamethrin R-Isomer
40
30
20
10
0
2 4 6 8 10 12 14 16 min
4
CIPAC/4683/R
FID1 A, (RE21898A\033F4201.D)
15.750 - Deltamethrin
90
80
70
60
40
30
20
10
0
2 4 6 8 10 12 14 16 min
5
CIPAC/4683/R
FID1 B, (RE21672A\007F0402.D)
14.898 - deltamethrin
pA
45
35
5.423
30
25
15.112
20
15
10
0
2 4 6 8 10 12 14 16 m in
FID1 B, (RE21672A\018F2102.D)
5.515 - dipropyl phthalate
14.882 - deltamethrin
pA
45
35
30
5.442
25
5.476
5.666
5.605
20
15
10
0
2 4 6 8 10 12 14 16 m in
6
CIPAC/4683/R
Deltamethrin
The linearity was demonstrated over a range of concentrations from 5 µg/mL to 50 µg/mL
expressed as deltamethrin by measuring detector response factor (deltamethrin to internal
standard area ratio) versus deltamethrin concentration for a series of 5 standard solutions
of deltamethrin of 5, 12, 24, 36 and 50 µg/mL). Linear regression (least squares method)
was calculated on the mean of minimum 2 injections of each standard solution.
1.6
y = 0.0330x - 0.0030
1.4
R² = 0.9999
1.2
Response factor
0.8
0.6
0.4
0.2
0
0 10 20 30 40 50 60
Concentration of deltamethrin (µg/mL)
The response factor (deltamethrin to internal standard area ratio) is linear in the range from
5 µg/mL to 50 µg/mL (R² > 0.99).
7
CIPAC/4683/R
Piperonyl butoxide
The linearity was demonstrated over a range of concentrations from 24 µg/mL to 240
µg/mL expressed as piperonyl butoxide by measuring detector response factor (piperonyl
butoxide to internal standard area ratio) versus piperonyl butoxide concentration for a
series of 5 standard solutions of piperonyl butoxide of 24, 60, 120, 180 and 240 µg/mL).
Linear regression (least squares method) was calculated on the mean of minimum 2
injections of each standard solution.
10
y = 0.0434x + 0.0397
R² = 1.0000
8
Response factor
0
0 50 100 150 200 250
The response factor (piperonyl butoxide to internal standard area ratio) is linear in the
range from 24 µg/mL to 240 µg/mL (R² > 0.99).
8
CIPAC/4683/R
1.3 Repeatability
The repeatability of the method is very good (RSD < 2% for deltamethrin content and <
3% for deltamethrin R-isomer content).
9
CIPAC/4683/R
Deltamethrin
The average recovery for deltamethrin on mosquito net for each fortification level is in the
range 90-110 % with a RSD < 5 %.
10
CIPAC/4683/R
Piperonyl butoxide
The average recovery for piperonil butoxide on mosquito net for each fortification level is
in the range 90-110 % with a RSD < 5 %.
11
CIPAC/4683/R
deltamethrin 0.01
100
90
80
70
60
50
0 5 10 15 20 25
12
CIPAC/4683/R
100
90
80
70
60
50
0 5 10 15 20 25
140
130
120
110
Recovery %
100
90
80
70
60
50
0 5 10 15 20 25
13
CIPAC/4683/R
100
90
80
70
60
50
0 5 10 15 20 25
100
90
80
70
60
50
0 5 10 15 20 25
14
CIPAC/4683/R
100
90
80
70
60
50
0 5 10 15 20 25
The control of the performance of the analytical method performed during analysis of more
than 830 samples show mean recoveries of 95-99 % with RSD ranging from 1.9% to 8.3%
depending on the concentration level. Very few recoveries are outside the warning limit
(green line) and all the recoveries are within the action limit of the quality control chart.
Recoveries performed concurrently with the analysis of samples show therefore a good
accuracy and within laboratory reproducibility of the analytical method.
15
CIPAC/4683/R
5.00
4.50 y = 0.9849x + 0.0141
R² = 0.9919
4.00
3.50
Deltamethrin VF (g/kg)
3.00
2.50
2.00
1.50
1.00
0.50
0.00
0.00 1.00 2.00 3.00 4.00 5.00
3. Conclusion
The analytical method was successfully validated. The control of the performance of the
analytical method performed concurrently with the analysis of more than 830 samples
showed also a good accuracy and a good within laboratory reproducibility. The proposed
method is considered appropriate for the determination of deltamethrin and/or piperonyl
butoxide in Long-Lasting (incorporated into polyethylene) Insecticidal Mosquito Nets.
Acknowledgements
The author wish to gratefully thank the WHO Pesticides Evaluation Scheme, the LN
manufacturers Vestergaard Frandsen and Intelligent Insect Control, the IRD/CREC, the
London School of Tropical Hygiene & Medicine, The Institute of Tropical Medicine and
the personnel (LN Team) of the Pesticides Research Department of the Walloon
Agricultural Research Centre (CRA-W).
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