AI10382-GC-MS-Food Safety-Analysis - page 20

AN20549_E 07/12S
Application Note 20549
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Relative Abundance
Time (min)
5
0
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
6
8 10 12 14 16 18 20 22 24 26
1
2
3
4
5
6
7
8 9
10
11
12
13
Figure 2: TIC for the GC/MS analysis of cucumber matrix spiked
with 10 µg/g of each pesticide in full scan (50-450 m/z).
See Table 2 for identified peaks. Unidentified peaks are matrix
peaks
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Conclusion
The QuEChERS sample preparation method provided
high recoveries and good reproducibility. The QuEChERS
– GC/MS method was found to be linear in the
concentration range of 25 to 1000 ng/g spiked matrix.
The TraceGOLD TG-5MS GC column provided good
chromatographic resolution of the pesticides studied.
References
1. M. Anastassiades, S.J. Lehotay, D. Stajnbaher and F.J.
Schenck, J AOAC Int 86 (2003) 412.
2. Foods of plant origin - Determination of pesticide
residues using GC/MS and/or LC-MS/MS following
acetonitrile extraction/partitioning and clean-up by
dispersive SPE –QuEChERS method. European Standard
EN15662:2008
Pesticides
t
R
(min) Linearity Nominal concentration
ng/g
Measured concentration
(n=6) ng/g.
Average %
Recovery (n=6)
Recovery
%RSD (n=6)
1. Dichlobenil
4.52
0.9988
50
58.7
117.4
2.1
2. Tribromoanisol
6.60
0.9990
50
54.3
108.5
6.0
3. Sulfotep
6.95
0.9984
50
59.8
119.6
2.3
4. Hexachlorobenzene
7.49
0.9983
50
55.2
110.4
2.8
5. Parathion
10.90 0.9979
50
53.0
106.0
5.9
6. Triphenylphosphine (IS)
13.41
-
-
-
-
-
7. EPN
17.90 0.9985
50
46.1
92.1
6.7
8. Azinphos methyl
19.20 0.9984
50
37.6
75.2
4.9
9. Permethrin isomer a
21.38 0.9987
50
49.8
99.5
8.9
10. Permethrin isomer b
21.58 0.9985
50
50.9
101.9
4.8
11. Fenvalerate isomer a
24.60 0.9985
50
47.7
95.4
8.9
12. Fenvalerate isomer b
25.02 0.9973
50
50.6
101.2
7.2
13. Deltamethrin
25.84 0.9949
50
51.7
103.3
6.8
Table 2: Summary of Results
Unidentified peaks in Figure 2 are impurity/matrix peaks
1...,10,11,12,13,14,15,16,17,18,19 21,22,23,24,25,26,27,28,29,30,...225
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