Acrylamide has been found to occur in many cooked carbohydrate-rich foods and is of concern as a possible carcinogen. The
supported liquid extraction (SLE) method described in this application note achieves high recoveries of acrylamide in fried
potato chips (crisps). The method is sensitive enough to potentially measure levels as low as 10 ppb in a popular brand and
flavour and has also been tested in flavoured varieties that were both machine and hand fried.
Format: ISOLUTE® SLE+ 1 mL Sample Volume Columns, part number 820-0140-C
Sample pre-treatment: Add 10 mL water to 1 g crushed sample (previously spiked with 13C3 acrylamide internal standard), and mix for 1 h. Centrifuge and remove a 0.65 mL aliquot of the aqueous layer, taking care
not to include any of the thin upper oil layer.
Sample loading: Load the pre-treated sample (0.65 mL) onto the ISOLUTE SLE+ column. Apply a pulse of vacuum or positive pressure to initiate
flow. Allow the sample to absorb for 5 min.
Analyte elution: Elute with ethyl acetate–tetrahydrofuran, (1:1, v/v, 2 × 2.5 mL) and allow to flow under gravity into tubes containing 2
µL ethylene glycol. Apply vacuum or positive pressure to elute any remaining extraction solvent.
Post elution: Dry the volatile constituents of the eluate in a stream of air or nitrogen. Reconstitute in water (200 µL).
Instrument: Waters Acquity
Table 1: Positive ion mode – MRM parameters.
Column: Phenomenex Hydro 4 µm 50 mm × 2 mm C18 column with a C18 guard cartridge and on-line filter
Mobile phase A: 0.1% formic acid in water
Mobile phase B: 0.1% formic acid in methanol
Flow rate: 0.3 mL min-1
Injection volume: 10 µL
Gradient: Initial 100% A, hold for 0.6 min; Linear ramp to 100% B over 0.25 min (0.85 min), hold 1.65 min (2.5 min); Linear ramp to
100% A in 0.01 min (2.51 min), hold 2.49 min (5 min)
Column temperature: 40 °C
Sample temperature: 20 °C
Ions were selected on the basis of achieving maximum sensitivity using multiple reaction monitoring.
Instrument: Waters Quattro Premier
Figure 1: Chromatogram of untreated potato chip (crisp) extract showing level of incurred acrylamide.
Ionization mode: ES+
Desolvation temperature: 450 °C
Source temperature: 120 °C
Results and Conclusion
A method has been developed which measures acrylamide from a challenging matrix at highly sensitive levels. Despite acrylamide
being a relatively polar molecule, excellent separation was demonstrated between this and matrix interferences on the ISOLUTE
SLE+ material. The method delivers good recovery (90%), low %RSD (<10%), and is significantly easier, quicker, and more cost-effective
to perform than SPE-based procedures, making it ideal for routine analysis of fried and baked foods.
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