AI10382-GC-MS-Food Safety-Analysis - page 170

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Experimental Details
Consumables
Part Number
Cartridge type:
HyperSep Hypercarb SPE cartridge, 500 mg/6 mL
60106-402
Column:
TraceGOLD TG-WaxMS, 30 m × 0.25 mm × 0.25 μm 26088-1420
Septum:
Thermo Scientific BTO, 17 mm
31303211
Liner:
Thermo Scientific™ Splitless FocusLiner™,
45354032
3 × 8 × 105 mm
Column ferrules:
100% graphite ferrules for Thermo Scientific™ 29053488
TRACE™ injector, 0.1–0.25 mm i.d.
Column ferrules:
Graphite/Vespel
®
for transfer line 0.1–0.25 mm i.d.
29033496
Vials and closures:
Thermo Scientific™ Chromacol™ 9 mm screw,
2-SVW(A)
2 mL vial, amber
Chromacol 9 mm screw caps with silicone/PTFE septa 9-SC(B)-ST101
Syringe filter:
Thermo Scientific™ Target2™ 30 mm GMF syringe
F2500-20
filter membrane, 3.1 µm pore size
Plastic syringe:
Thermo Scientific 3 mL plastic disposable syringes
S7510-3
Sample Handling Equipment
Part Number
HyperSep glass block manifold
60104-232
Instrumentation
Thermo Scientific™ TRACE GC Ultra™ gas chromatograph
Thermo Scientific™ DSQ™ II single quadrupole mass spectrometer
Thermo Scientific™ TriPlus™ Autosampler
Chemicals and Reagents
Part Number
Fisher Scientific™ HPLC grade water
W/0106/17
Fisher Scientific HPLC grade methanol
M/4056/17
Fisher Scientific Analytical grade formic acid
F/1900/PB08
Sample Pretreatment
The potato chips were finely crushed with mortar and pestle and 1 g was weighed into a vial. A 1 g portion of the sample
was spiked with 25, 50, 100, 250, 500, and 1000 ng/g of acrylamide standard in 2% formic acid / water. The sample
was then filtered through a filter membrane.
Sample Preparation
Compounds:
Acrylamide and acrylamide-d
3
(internal standard)
Matrix:
Potato chips
Conditioning stage:
Add 4 mL methanol, 4 mL water, and 4 mL 2% formic acid / water to
the SPE cartridge.
Application stage:
Apply 1 mL of extract in 2% formic acid / water under vacuum
at 1 mL/min to the SPE cartridge.
Washing stage:
Add 1 mL water to the SPE cartridge and dry for 20 min under vacuum.
Elution stage:
Apply 4 mL methanol to the SPE cartridge.
Additional stage:
Evaporate methanolic extract and reconstitute with 1 mL of 1 µg/mL of
internal standard in methanol to the SPE cartridge.
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