restekapp07 - page 162

For permission to reproduce any portion of this application note, please contact Restek’s publications/graphics department by phone (ext. 2128) or FAX.
Product Listing
CarboPrep, andRestek logo are trademarks of RestekCorporation.
Figure 3
Acrylamide can be detected in reduced fat potato chips,
using a Stabilwax
®
capillary GCcolumn.
CarboPrep
SPECartridges
SPE Cartridge
Tube Volume,
BedWeight
Surface Area
qty.
cat#
CarboPrep
200 3mL, 250mg
200m
2
/gm 50-pk.
26088
CarboPrep
200 6mL, 500mg
200m
2
/gm 30-pk.
26087
CarboPrep
90 3mL, 250mg
90m
2
/gm 50-pk.
26091
CarboPrep
90 6mL, 500mg
90m
2
/gm 30-pk.
26092
Ordering Information
| Stabilwax
®
Columns (FusedSilica)
(Crossbond
®
Carbowax
®
—provides oxidation resistance) Stable to 250°C
Theprocedureweused inour analysis of potato chipswas as follows:
1. Analyticallyweigh 1g crushed potato chips.
2. Combine chip samplewith 10mL0.1% formic acid solution
andmix on awrist action shaker for 20minutes.
3. Refrigerate extract for easier removal of oily top layer.
4. Filter supernatant through a 0.45µm nylon syringe filter
(cat.#26071); remove and store for cleanup and analysis.
5. ConditionCarboPrep™200SPE tube, 6mL, 500mg (cat.#26087):
a. 2mLacetone
b. 2mL0.1% formic acid
6. Apply 2mLof filtered, extracted chip solution to SPE tube.
Allow sample solution to pass through tubewith only gravity
flow.
7. Wash SPE tube:
a. 0.5 - 1.0mLwater; pass through tube quickly.
b. Usevacuum for up to1minute todry excesswater from tube.
8. Elutewith 2mLof acetone, using gravity only. Eluate is ready
for GC-FID analysis.
The chromatogramwe obtained from the analysis of a reduced fat
potato chip extract is shown in Figure 3. The chip samplewas
spikedwith 100µg (50µg/mL) of acrylamide for this analysis. The
amount of acrylamide in the reduced fat chip sample alonewas
below the quantitation limit of this procedure.
Discussion
Gas chromatography offers a rapid, cost-effective approach to
screening for acrylamide in food samples such as potato chips. The
Stabilwax
®
capillary column exhibits excellent selectivity for acry-
lamide, evenwhen analyzing complexmatrices, such as food sam-
ples. Detection limits on the order of 0.01µg/mL (10 ppb) in solu-
tion can be achieved. CarboPrep™ 200 sample preparation car-
tridges provide excellent flow properties for rapid cleanup of sam-
ples, using either vacuum pressure or gravity. The chromatographic
grade, graphitized carbon packingmaterial demonstrates repro-
ducible recovery. This strong adsorbent has awide range of selec-
tivity, resulting in high capacity, even for analytes not usuallywell
retained by reversed phaseC18 adsorbents. For additional sensitiv-
ity, extracted acrylamide can be brominated, then quantified using
an electron capture detector (ECD).
4
References
1. Hileman, Bette,
C&ENews
, July, 2002.
2. Schildhouse, Jill,
FoodProduct Design
, July, 2002.
3.
4. USEPAMethod 8032A
ID df (µm)
temp. limits 15-Meter 30-Meter 30-Meter 6/pk. 60-Meter
0.25mm 0.10
40 to 250°C
10605
10608
10611
0.25
40 to 250°C
10620
10623
10626
0.50
40 to 250°C
10635
10638
10641
0.32mm 0.10
40 to 250°C
10606
10609
10612
0.25
40 to 250°C
10621
10624
10627
0.50
40 to 250°C
10636
10639
10642
1.00 40 to 240/250°C 10651
10654
10654-600
10657
0.53mm 0.10
40 to 250°C
10607
10610
10613
0.25
40 to 250°C
10622
10625
10628
0.50
40 to 250°C
10637
10640
10643
1.00 40 to 240/250°C 10652
10655
10655-600
10658
1.50 40 to 230/240°C 10666
10669
10672
2.00 40 to 220/230°C 10667
10670
Stabilwax
®
15m, 0.53 ID, 0.50µm (cat.# 10637)
Sample:
1g of potato chip spikedwith 100µg acrylamide
Inj.:
1.0µL, 0.5min hold
Liner:
2mm splitlesswithwool (cat.# 20830)
Inj. temp.:
260°C
Carrier gas:
helium, constant pressure
Linear velocity: 62cm/sec.@ 100°C
Oven temp.:
100°C (hold 0.5min.) to 200°C@ 15°C/min.
Det.:
FID@ 260°C
1. acrylamide
blank
GC_FF00643
1...,152,153,154,155,156,157,158,159,160,161 163,164,165,166,167,168,169,170,171,172,...324
Powered by FlippingBook