AI10382-GC-MS-Food Safety-Analysis - page 137

Duration
Retention
Precursor
Quantifier
Qualifier
Ion
Collision
Segment
(min)
PAH and IS Time (min)
Ion
Ion
Ion
Ratio
Energy
1
10.50
Naph
8.66
127.9
102.0
77.8
0.38
15
2
2.50
Acy
12.13
152.0
151.1
126.0
0.11
10
Ace
12.35
154.0
153.0
152.0
0.12
10
3
1.50
Fln
13.37
165.9
165.0
162.9
0.05
10
4
3.00
Ant
15.87
178.0
176.0
152.0
0.70
30
Phe
15.95
178.0
176.0
152.0
0.70
30
Ant-D10
15.89
188.1
160.2
158.2
0.40
30
5
4.50
Flu
19.13
202.0
201.1
200.1
0.40
10
Pyr
19.97
202.0
201.0
200.1
0.40
10
6
3.70
B(a)A
23.48
228.1
226.0
202.1
0.15
20
Chr
23.71
228.1
226.2
202.2
0.15
20
Chr-D12
23.65
240.2
238.1
215.1
0.11
30
5MChr
24.98
242.1
241.1
227.5
0.15
30
7
3.80
B(b)F
26.75
252.1
250.1
226.1
0.18
30
B(k)F
26.82
252.1
250.1
226.1
0.18
30
B(a)P
27.96
252.1
250.1
226.1
0.18
30
B(a)P-D12
27.87
264.1
260.1
236.0
0.38
30
8
5.50
I(1,2,3-c,d)P
30.96
276.1
274.0
250.0
0.05
35
B(g,h,i)P
31.99
276.1
274.0
250.0
0.05
35
BgP-D12
31.86
288.2
286.1
125.1
0.06
35
D(a,h)A
30.97
278.0
276.0
226.1
0.05
35
Table 1: Parameters for SRM analysis of PAHs grouped according to Figure 1
Hydrocarbon
Empirical Formula Molecular Ion Retention Time
n
-decane
C
10
H
22
142.1
3.99
n
-undecane
C
11
H
24
156.2
4.97
n
-dodecane
C
12
H
26
170.2
6.14
n
-tridecane
C
13
H
28
184.2
7.30
n
-tetradecane
C
14
H
30
198.2
8.42
n
-pentadecane
C
15
H
32
212.2
9.50
n
-hexadecane
C
16
H
34
226.2
10.51
n
-heptadecane
C
17
H
36
240.2
11.45
pristane
C
19
H
40
268.3
11.24
n
-octadecane
C
18
H
38
254.3
12.41
phytane
C
20
H
42
282.3
12.30
n
-nonadecane
C
19
H
40
268.3
13.28
n
-eicosane
C
20
H
42
282.3
14.14
n
-docosane
C
22
H
46
310.3
15.90
n
-tetracosane
C
24
H
50
338.3
17.73
n
-hexacosane
C
26
H
54
366.4
19.56
n
-octacosane
C
28
H
58
394.4
21.35
n
-triacontane
C
30
H
62
422.4
23.08
n
-dotriacontane
C
32
H
66
450.5
24.77
n
-tetratricontane
C
34
H
70
478.5
26.45
Table 2: Aliphatic hydrocarbons monitored in oysters spiked with NIST 1494
Average amount
Average amount
Hydrocarbon
[µg/g] (n=2)
PAH
[µg/g] (n=2)
n
-pentadecane
407
Naph
19
n
-hexadecane
1484
Acy
436
n
-heptadecane
1329
Ace
96
Pristane
928
Fln
144
n
-octadecane
337
Ant
11857
Phytane
118
Phe
11287
n
-nonadecane
330
Flu
958
n
-eicosane
289
Pyr
547
n
-docosane
188
B(a)A
29
n
-tetracosane
146
CHR
804
n
-hexacosane
82
B(b)F
428
n
-octacosane
43
B(k)F
40
n
-triacontane
31
B(a)P
2
n
-dotriacontane
23
B(g,h,i)P
7
n
-tetratricontane
10
I(1,2,3-c,d)P
2
D(h)A
3
Table 4: Composition of Crude oil from Gulf of Mexico. Characteristic
pristane/C-17 ratio (0.7) phytane/C-18 ratio (0.35) were observed.
PAH
Assigned Value [ng/g]
Measured Value [ng/g]
Recovery [%]
B(a)A
14.06 ± 1.00
17.39
124
B(a)P
5.52 ± 1.00
5.11
92
I(1,2,3-c,d)P
0.85 ± 0.50
0.69
81
B(g,h,i)P
8.54 ± 0.2
7.37
86
Table 3: Analysis of spiked oysters with NIST 1582 crude oil
1...,127,128,129,130,131,132,133,134,135,136 138,139,140,141,142,143,144,145,146,147,...225
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