Analysis of Acrylamide in Processed Foods in Japan

Since announcement of presence of acrylamide in processed foods by University of Stockholm and National Food Administration of Sweden at a press conference in 24 April 2002, we have recognized this issue as a substantial matter of food safety and started analysis of acrylamide in processed foods in Japan by LC-MS/MS and GC-MS. Here we report the methods and results of the analyses on 63 samples covering 31 product types.

Figure 1

LC-MS/MS conditions

HPLC
apparatus	Nanospace SI-2 (Shiseido, Tokyo, Japan)
column	Atlantis dC18 (2.1 x 150 mm,3 µm, Waters, MA, USA)
pre-column	OptiGuard mini C18 (1.0 x 15 mm, Optimize Technologies, OR, USA)
solvent	10 % MeOH
flow rate	100 µL/min
injection volume	2 µL
column temperature	40 °C
retention time	5.4 min
recording time	12 min (4.8E0.2 min to MS)
MS
apparatus	API 3000 (Applied Biosystems, CA, USA)
ionization	ESI+
detection	SRM (acrylamide m/z 72->55, internal standard m/z 75->58)
ion source	TurboIonSpray
nebulizer gas flow	4
curtain gas flow	10
ion source temp	450 °C
ion spray voltage	5200 V
orifice voltage	26 V
dwell time	95 msec
pause time	5 msec
acquisition duration	10 min
limit of detection	0.2 ng/mL (5 fmol)
limit of quantitation	0.8 ng/mL (22 fmol)

GC-MS conditions

apparatus QP2010 (Shimadzu, Kyoto, Japan)
column CP-Sil 24 CB (0.25 mm i.d. x 30 m, 0.25 µm film thickness, Varian, CA, USA)
carrier gas He
flow rate 1.43 mL/min
injection volume 1 µL
injection temperature 120 °C
temp. program 85 °C (1 min) E(25 °C/min)E75 °C (6 min) E(40 °C/min)E50 °C (7.52 min)
retention time 8.1 min
acquisition duration 16 min
ionization EI+ (70 eV)
detection SIM (acrylamide m/z 150 & 152, internal standard m/z 153 & 155)
interface temp. 280°C
ion source temp. 200°C
limit of detection 12 ng/mL (52 fmol) as 2,3-dibromopropanamide
limit of quantitation 40 ng/mL (170 fmol) as 2,3-dibromopropanamide

Figure 2

These analyses were carried out on single randomly selected samples from supermarkets. It is highly likely that there are variations in acrylamide concentration among production lots and among foods within a product type due to difference in the processing condition. Survey over wider range of foods with larger number of samples including home cooked foods is necessary for risk assessment.

References

Ono H., Chuda Y., Ohnishi-Kameyama M., Yada H., Ishizaka M., Kobayashi H., and Yoshida M., Analysis of acrylamide by LC-MS/MS and GC-MS in processed Japanese foods, Food Addit. Contam., 20, 215-220 (2003).
Tareke, E., Rydberg, P., Karlsson, P., Eriksson, S., and Törnqvist M., Analysis of acrylamide, a carcinogen formed in heated foodstuffs. J. Agric. Food Chem., 50, 4998-5006 (2002).
Rosén, J. and Hellenäs, K., Analysis of acrylamide in cooked foods by liquid chromatography tandem mass spectrometry. The Analyst, 127, 880-882 (2002).
Castle, L., Determination of acrylamide monomer in mushroom grown on polyacrylamide gel. J. Agric. Food Chem., 41, 1261-1263 (1993).
Castle, L., Campos, M., and Gilbert, J., Determination of acrylamide monomer in hydroponically grown tomato fruit by capillary gas chromatography-mass spectrometry. J. Sci. Food. Agric., 54, 549-555 (1991).
Food Standards Agency, Paper and board packaging: not likely to be a source of acrylamide in food.
http://www.foodstandards.gov.uk/multimedia/pdfs/27acryl.pdf
U. S. Food and Drug Administration, Center for Food Safety and Applied Nutrition, Detection and quantitation of acrylamide in foods (draft).
http://www.cfsan.fda.gov/~dms/acrylami.html

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apparatus	QP2010 (Shimadzu, Kyoto, Japan)
column	CP-Sil 24 CB (0.25 mm i.d. x 30 m, 0.25 µm film thickness, Varian, CA, USA)
carrier gas	He
flow rate	1.43 mL/min
injection volume	1 µL
injection temperature	120 °C
temp. program	85 °C (1 min) E(25 °C/min)E75 °C (6 min) E(40 °C/min)E50 °C (7.52 min)
retention time	8.1 min
acquisition duration	16 min
ionization	EI+ (70 eV)
detection	SIM (acrylamide m/z 150 & 152, internal standard m/z 153 & 155)
interface temp.	280°C
ion source temp.	200°C
limit of detection	12 ng/mL (52 fmol) as 2,3-dibromopropanamide
limit of quantitation	40 ng/mL (170 fmol) as 2,3-dibromopropanamide