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AcrylamideAnalysis byGasChromatography
Introduction
Howmuch acrylamide is in that French fry? Is this potato chip
safe to eat? Since the release of a report by Sweden’sNational
FoodAdministration inApril 2002, consumers have had something
else to think about when choosingwhat to eat.Acrylamide is a
toxic and potentially cancer-causing chemical, although the toxico-
logical effects on humans are still under investigation. The topic of
acrylamide in foods, especially in fried and baked goods, has gen-
erated a significant amount of interest in 2002. TheUnited
Kingdom’s Food StandardsAgency, theCenter for Science in the
Public Interest (CSPI), and theUSFood&DrugAdministration
(FDA) are among the groups that have begun testing for acry-
lamide in food products.
Researchers are postulating that acrylamide is formed in relatively
high concentrationswhen carbohydrate-rich foods such as potatoes,
rice, and cereals are cooked at highheat.
1,2
This seems tobe particu-
larly truewhen the products are fried. Rawor boiled starchy foods do
not seem to formdetectable amounts of acrylamide. Of the products
tested, the highest levels of acrylamidewere found inpotato chips
andFrench fries, on the order of 400 - 1200ppb. By comparison, the
WorldHealthOrganization (WHO) has specified amaximum con-
centrationof 0.5µg/L(0.5ppb) acrylamide indrinkingwater.
1
The FDAhas published a draft method for the analysis of acry-
lamide in foods byLC/MS/MS.
3
The procedure calls for a reversed
phaseC18 column and a highly aqueousmobile phase (0.1%
acetic acid, 0.5%methanol). Becausemany of the samplematrices
can be quite complex, solid phase extraction is used to remove
interferences prior to the chromatographic analysis. Positive ion
electrospray is used for themass spectral interface, with quantifi-
cation based on comparison to a
13
C isotopically labeled internal
standard. Themethod has been validated for a limited number of
matrices, such as potato chips and French fries, and public and pri-
vate researchers are in the process of validating the LC/MS/MS
approach for other food products.
Gas chromatography (GC) has been used to quantify acrylamide in
a variety of industrial and environmental applications.With
increasing interest in acrylamide analysis, we investigated the fea-
sibility of usingGC to screen for this compound in food samples.
GC is a low-cost, efficient way to detect semivolatile compounds,
and as an analytical tool is available inmany food laboratories. In
this note, we describe aGC approach to analyzing acrylamide, and
discuss sample pretreatment using solid phase extraction.
Methodology&Results
We used the followingGC conditions in analyzing both acrylamide
standards and food samples:
Column:
Stabilwax
®
- 15m, 0.53 ID, 0.50µm film (cat.#10637)
Inj.:
1.0µL, 0.5min. hold
Liner:
2mm splitlesswithwool (cat.# 20830)
Injector 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.
Detector:
FID@260°C
#59485
Figure 1
AStabilwax
®
column is an excellent choice for
acrylamide analysis by capillary GC.
Figure 2
Acrylamide standard solutionswere tested over a concentration
range of 0.02 - 5 ppm (20 - 5000 µg/L) inwater. A plot of peak
counts vs. concentration shows awide linear range for the
GC assay, withR
2
= 0.99996.
12000
10000
8000
6000
4000
2000
0
area counts
0.00
1.00
2.00
3.00
4.00
5.00
6.00
ppmAcrylamide
The chromatogram produced by injecting 1µLof a 25µg/mL (25
ppm) acrylamide standard is shown in Figure 1. Figure 2 is the lin-
earity plot for standard solutions over a range of 20 - 5000 ppb.
The sample preparationmethodwe followedwas based on the
draft U.S. Food&DrugAdministrationmethod
Detection and
Quantitation of Acrylamide inFoods
dated June 20, 2002.
3
Stabilwax
®
15m, 0.53 ID, 0.50µm (cat.# 10637)
Sample:
25µg/mL acrylamide standard inwater
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
GC_FF00642
1. acrylamide
Chromatographic conditions listed in text.
