638
GCCHROMATOGRAMS |
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 1min.), 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 4min.)
Det:
MS
Transfer line temp.: 290°C
Ionization:
EI
Mode:
SIM
1. cyanuric acid
2. ammelide
3. ammeline
4. melamine
5. benzoguanamine
MelamineSpike inCatFood
Rtx®-5MS
Reliable
identifications
inmatrix.
QuEChERSExtractofNISTSRM2974aFreeze-DriedMusselTissue (GCxGCcontourplot)
GC_FF1197
Column
Rxi
®
-17Sil MS 30m, 0.25mm
ID, 0.25µm (cat.# 14123)
Rxi
®
-1ms 1.2m, 0.15mm ID,
0.15µm (cat.# custom)
Sample
NIST SRM 2974a freeze-dried
mussel tissuewith incurred
residues
Diluent:
Acetonitrile
Injection
Inj. Vol.:
1µL splitless (hold 1min.)
Liner:
Gooseneck Splitless (4mm)
w/SemivolatilesWool
(cat.# 20798-231.1)
Inj.Temp.:
250 °C
Purge Flow:
40mL/min.
Oven
OvenTemp:
Rxi
®
-17Sil MS: 90 °C (hold 1
min.) to 320 °C at 3.75 °C/min.
(hold 2.67min.)
Rxi
®
-1ms: 95 °C (hold 1min.)
to 325 °C at 3.75 °C/min.
(hold 2.67min.)
Carrier Gas
He
Modulation
Modulator
Temp. Offset:
20 °C
SecondDimension
SeparationTime: 3 sec.
Hot PulseTime:
0.9 sec.
CoolTime
between Stages: 0.6 sec.
Detector
TOFMS
Transfer
LineTemp.:
300 °C
AnalyzerType:
TOF
SourceTemp.:
250 °C
Electron Energy: 70 eV
Mass Defect:
-20mu/100 u
Solvent Delay
Time:
5min.
TuneType:
PFTBA
IonizationMode: 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 thewhite 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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MelamineGC/MS
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Mar 2011
