Note
DOI: 10.1002/bkcs.10033 B. Kim and S.-W. Hyung
Stability Monitoring of Acrylamide in Potato Chip Certified
Reference Material
Byungjoo Kim* and Seok-Won Hyung
Korea Research Institute of Standards and Science, Daejeon, Yuseong-gu 305-340, Korea.
*E-mail: byungjoo@kriss.re.kr
Received July 8, 2014, Accepted September 24, 2014, Published online January 5, 2015
Keywords: Potato chip CRM, Acrylamide, Stability
The international chemical metrology community is striving
to increase comparability and reliability of measurement
results obtained by different laboratories around the world.
The community has realized that measurement results can
be harmonized by making them traceable to the International
System of Units (SI) through comparison with national and
international standards. In this respect, certified reference
materials (CRMs) are used by laboratories to validate and
verify analytical methods, and to assure the quality of the
analytical procedure.1–3 Laboratories choose CRMs that are
similar to the samples to be analyzed in terms of matrix
types, analytes, and concentrations.4 Therefore, national
metrology institutes (NMIs) continue to produce CRMs nec-
essary for the dissemination of SI-traceable national and inter-
national standards to laboratories involved with chemical
analysis.
Our laboratory, the NMI of Korea, has been developing
CRMs for chemical analysis of environmental, food, and clin-
ical samples. In cases of CRMs for organic analysis area,
ensuring their stability during long-term storage under desig-
nated storage conditions is a critical factor, as many organic
compounds of interest are air-sensitive, light-sensitive,
degrade thermally or in acidic/alkaline conditions, and/or
easily evaporate out of sample matrix.5,6 For these reasons,
CRM producers have to continually monitor the stability of
the CRMs that they developed.
In 2004, this laboratory launched a project to develop a
CRM that can be used to determine acrylamide concentrations
in food. The impetus for initiating the project was the emer-
gence of food safety concerns, related with acrylamide, that
were triggered by a 2002 report from a Swedish group. The
Swedish study found that traditional carbohydrate-rich foods
(potato chips, cookies, etc.), processed or cooked at high tem-
perature, contain relatively high levels of acrylamide, a possi-
ble carcinogenic substance.7 Subsequently, government
health agencies and international organizations initiated pro-
grams for the surveillance of acrylamide in food, which
included the standardization of sampling protocols and analyt-
ical techniques. At the same time, many food processors
changed their processing methods to reduce the levels of acryl-
amide in their products. Although in 2004 the reliability of
acrylamide measurement in food was an international concern
Bull. Korean Chem. Soc. 2015, Vol. 36, 399–401 © 2015 Korean Chemical Society, Seoul & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
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and several analytical methods were used,6,8 there were no
commercially available CRMs for acrylamide.
In response to this need, in 2007, our laboratory began pro-
ducing a CRM, called KRISS CRM 108-10-003, for the anal-
ysis of acrylamide in potato chips. Potato chips are known to
be a source of acrylamide and are representative of many car-
bohydrate-rich foods that are cooked at high temperatures.
Details regarding the development of this CRM were previ-
ously reported by our laboratory.6 We prepared 288 samples,
each containing 15 g of ground potato chip paste: a paste that
forms because of the presence of the high oil concentration in
the raw material. An isotope-dilution liquid chromatography-
mass spectrometry (ID-LC/MS) method developed in this lab-
oratory8 was used as a higher order reference method for the
certification and stability monitoring of acrylamide in the
developed CRM. When developing the CRM, the greatest
concerns were the potential instability of the CRM as a result
of the evaporation of the semivolatile acrylamide and the
unforeseen slow generation of acrylamide.9,10 Based on a pre-
liminary stability study using a test batch of CRM, –70  C was
designated as the storage temperature for the CRM.6 The cer-
tified concentration was (0.4546 ± 0.0057) mg/kg. The initial
expiry date was established as 42 months after the certification
date based on results from the 21-month stability monitoring.
The developed CRM has been disseminated upon request to
other laboratories.
This article reports on the test results that were obtained by
monitoring the stability of the potato chip CRM beyond the
initial 21-month test period. Our laboratory continued to mon-
itor the stability of the CRM on a periodic basis, analyzing
samples every 12–18 months up to 73 months after certifica-
tion, in order to ensure the validity of the expiry date. In addi-
tion, continued stability monitoring allowed the extension of
the expiry date. Results from the current extended stability test
are graphically shown in Figure 1, along with the results of the
previous stability monitoring tests.6 The analytical results
from samples obtained at 36, 48, 56, and 73 months after
the certification date agree with the initial certified value
within their uncertainties. It demonstrated that the acrylamide
in the CRM was stable up to 73 months. As a result, the expiry
date of the CRM was extended to 146 months, a period twice
as long as the 73-month stability monitoring period. All
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0.55
Stability monitoring of acrylamide in potato chip CRM at - 70 oC
0.53

0.51

0.49
Acrylamide (mg/kg)

0.47

0.45

0.43

0.41

0.39

0.37

0.35

Figure 1. Stability study results of acrylamide in a potato chip paste CRM stored at –70  C. The horizontal solid line marks the certified value, and
the dashed line indicates its expanded uncertainty intervals (at 95% confidence level). Results (■) from continuing stability monitoring carried
out in this study are presented in parallel with results (◆) reported in our previous article.6

analytical procedures were performed in accordance with a
guideline established and maintained in this laboratory and
with ISO Guide 35.11
The study, which continued to monitor acrylamide stability
of the potato chip paste samples, confirmed that the acryla-
mide in the CRM stored at –70  C was stable up to 73 months.
Although the temperature-driven evaporation of acrylamide
in the CRM was observed at −20  C or higher temperature dur-
ing our 2007 study,6 acrylamide was still found to be stable at –
70  C. This study also proved that that the continued genera-
tion of acrylamide from the food matrix at –70  C storage tem-
perature was negligible. In a previous study at our
laboratory,12 semivolatile and degradable organophosphorus
pesticides in a Chinese cabbage CRM (KRISS CRM# 108-
05-003) were found to be stable for 3 years at –70  C. Results
from the present study are aligned with the results generated
from monitoring the cabbage CRM. The two studies indicate
that low-temperature storage can be a solution for achieving
the long-term stability of CRMs that are used for organic anal-
ysis. The findings will allow CRM producers and users to
select the required storage conditions for their CRMs.
potato chips formed a thick paste due to the cooking oil present
in the chips. The paste was homogenized with a standard mixer
under argon gas and bottled into wide-bore amber bottles
with 15 g of sample per bottle. A total of 288 samples were
prepared and stored in a –70  C freezer.
Analytical Method. Details for the ID-LC/MS analytical
method used for the certification and stability monitoring
of the CRM were reported in our previous articles.6,8 At
each designated time point of stability monitoring (36, 48,
56, 72 months), three of the 288 amber bottles were opened
and two subsamples (3 g) from each of the three samples were
analyzed by the ID-LC/MS method. The same uncertainty
evaluation protocol employed in the certification was used
for the measurement results from stability monitoring.
Acknowledgment. This work was supported by the Korea
Research Institute of Standards and Science under the project
“Establishing Measurement Standards for Organic Analysis”
(Grant 14011050).
References

Experimental Methodology
Preparation of Reference Material. Details on the prepara-
tion and certification of the CRM were reported in our previ-
ous article,6 and only a brief summary is provided here. The
CRM was prepared from a commercial brand potato chips
obtained from a local market. The raw material contained nat-
urally occurring acrylamide ranging from 0.3 to 0.8 mg/kg.
About 7.8 kg of potato chips was processed by grinding and
sieving to remove particles larger than 500 μm. The ground
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Bull. Korean Chem. Soc. 2015, Vol. 36, 399–401 © 2015 Korean Chemical Society, Seoul & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim www.bkcs.wiley-vch.de 400
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Note KOREAN CHEMICAL SOCIETY

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