638
GC CHROMATOGRAMS |
FOODS, FLAVORS & FRAGRANCES
Food Contaminants
GC_FF00977
Column:
Rtx
®
-5MS, 30m, 0.25mm ID, 0.25µm (cat.# 12623)
Sample:
melamine, cyanuric acid, ammelide, ammeline, benzoguanamine
in dry cat food (10µg/mL prederivatized)
Inj.:
1µL, splitless (hold 1 min.), 3.5mm splitless inlet liner (cat.# 22286)
Inj. temp.:
280°C
Carrier gas:
helium, constant flow
Flow rate:
1mL/min.
Oven temp.:
75°C to 320°C @ 15°C/min. (hold 4 min.)
Det:
MS
Transfer line temp.: 290°C
Ionization:
EI
Mode:
SIM
1. cyanuric acid
2. ammelide
3. ammeline
4. melamine
5. benzoguanamine
Melamine Spike in Cat Food
Rtx®-5MS
Reliable
identifications
in matrix.
QuEChERS Extract of NIST SRM 2974a Freeze-Dried Mussel Tissue (GCxGC contour plot)
GC_FF1197
Column
Rxi
®
-17Sil MS 30 m, 0.25 mm
ID, 0.25 µm (cat.# 14123)
Rxi
®
-1ms 1.2 m, 0.15 mm ID,
0.15 µm (cat.# custom)
Sample
NIST SRM 2974a freeze-dried
mussel tissue with incurred
residues
Diluent:
Acetonitrile
Injection
Inj. Vol.:
1 µL splitless (hold 1 min.)
Liner:
Gooseneck Splitless (4mm)
w/Semivolatiles Wool
(cat.# 20798-231.1)
Inj. Temp.:
250 °C
Purge Flow:
40 mL/min.
Oven
Oven Temp:
Rxi
®
-17Sil MS: 90 °C (hold 1
min.) to 320 °C at 3.75 °C/min.
(hold 2.67 min.)
Rxi
®
-1ms: 95 °C (hold 1 min.)
to 325 °C at 3.75 °C/min.
(hold 2.67 min.)
Carrier Gas
He
Modulation
Modulator
Temp. Offset:
20 °C
Second Dimension
Separation Time: 3 sec.
Hot Pulse Time:
0.9 sec.
Cool Time
between Stages: 0.6 sec.
Detector
TOFMS
Transfer
Line Temp.:
300 °C
Analyzer Type:
TOF
Source Temp.:
250 °C
Electron Energy: 70 eV
Mass Defect:
-20 mu/100 u
Solvent Delay
Time:
5 min.
Tune Type:
PFTBA
Ionization Mode: EI
Acquisition Range: 45 to 550 amu
Spectral
Acquisition Rate: 100 spectra/sec
Instrument
LECO Pegasus 4D
GCxGC-TOFMS
Notes PAHs (shown in box) elute in a relatively
narrow band and are identified by the white peak
marker dots.
Peaks
1. Naphthalene
2. 2-Methylnaphthalene
3. 1-Methylnaphthalene
4. Biphenyl
5. 2,6-Dimethylnaphthalene
6. Acenaphthylene
7. Acenaphthene
8. 2,3,5-Trimethylnaphthalene
9. Fluorene
10. Phenanthrene
11. Anthracene
12. 1-Methylphenanthrene
13. Fluoranthene
14. Pyrene
15. Benzo(a)anthracene
16. Chrysene
17. Benzo(b)fluoranthene
18. Benzo(k)fluoranthene
19. Benzo(j)fluoranthene
20. Benzo(e)pyrene
21. Benzo(a)pyrene
22. Perylene
23. Dibenz(a,h)anthracene
24. Indeno(1,2,3-cd)pyrene
25. Benzo(ghi)perylene
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Melamine GC/MS
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Mar 2011
