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acrylamide testing

Acrylamide is used primarily to make polyacrylamide.  It is sometimes used to clarify water, acting as a coagulant.  Both EPA and the World Health Organization have set a limit on residual acrylamide in drinking water of 0.5 ug/L.

In California, the current Prop. 65 No Significant Risk Level (NSRL) is 0.2 ug/day.  However, recently Swedish researchers reported finding very high levels of acrylamide in fried foods (potato chips, median 1200 ug/kg; french fries, 450 ug/kg) and baked foods (cereal and breads, 100-200 ug/kg).1

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H2C=CHCNH2

Acrylamide

(2-propenamide)

WHO Acrylamide

FDA Acrylamide Action Plan

C&EN: Acrylamide Mystery Solved


Acrylamide Testing

There are a few analytical alternatives for trace analysis of acrylamide monomer.  Both HPLC (liquid chromatography) and GC (gas chromatography) based techniques can be used to determine trace amounts of acrylamide.  

Both the Swedish group and FDA have evaluated a GCMS and an LC-MS/MS method for acrylamide.  LC-MS/MS equipment is not commonly available.  Both methods appear to give the same results.1,2

EPA 8316 uses HPLC with UV detection at 195 nm giving a detection limit of ~10 ug/L in water.  But this short wavelength is not very selective for acrylamide, i.e. interferences are likely, and the sensitivity is not adequate for water or Prop. 65 levels. 

EPA 8032 uses GC-ECD after bromination of the acrylamide.  This 

method is much more selective for acrylamide, and detection limits are much lower, 0.03 ug/L.  However, in foods, the acrylamide may suffer from interferences and poor extraction efficiency.  

One modification of EPA 8032 that has been found to work well by WCAS and others1 is an isotope dilution technique coupled with GCMS.  Acrylamide-d3 is added as an isotope dilution standard prior to a modified EPA 8032 extraction followed by GCMS analysis.  The GCMS chromatogram below is a sample of corn chips which was found to contain approximately 400 ug/kg acrylamide.  The detection limit for a  50 mL water sample is ~ 0.1 ug/L.  The detection limits in 10 g food samples is ~3 ug/kg.

For a quotation...

1Tareke, et al., J.Ag.Food Chem. 2002, 50, 4998-5006.

2Roach, et al., J.Ag.Food Chem. 2003, 51, 7547-7554.

 

GCMS of corn chips for acrylamide using EPA 8032

Mass Spectrum of Acrylamide Derivative


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