Extraction of acrylamide from cooked foodstuffs using ISOLUTE® Multimode cartridges

Introduction

This method describes the clean-up of acrylamide from cooked foodstuffs, using a multimode retention mechanism (hydrophobic, cation and anion exchange) for retention of interfering food components. The analytical technique is LC-MS-MS.

Acrylamide is a very small, highly water soluble molecule, with negligible hydrophobic character. When the aqueous food extract is applied to the ISOLUTE® Multimode SPE cartridge, the acrylamide passes through unretained, while more hydro- phobic, or ionic interferences are retained by a variety of retention mechanisms.

It may be necessary to further pre-concentrate the extract after clean up. If so, we recommend the use of ISOLUTE®  ENV+ SPE cartridges.

Figure 1: Structure of acrylamide

Extraction procedure

Format

ISOLUTE®  Multimode 300 mg/3 mL, part number 904-0030-B

Pre-treatment

1. Homogenize sample (2–4 g) with water (40 mL).
2. Add internal standard (800 μL).
3. Homogenize to extract the sample (2 min., 9,500 rpm).
4. Centrifuge the extract (3,600 g, 10 min).
5. Collect the supernatant.

Condition

Solvate the cartridge with acetonitrile (1 mL).

Equilibration

Rinse with water (2 x 2 mL).

Sample loading

Apply the supernatant to the cartridge (3 mL).

Equilibration

Rinse with water (2 x 2 mL).

Sample loading

Apply the supernatant to the cartridge (3 mL).

Interference elution

N/A

Analyte elution

1. Discard the first portion (1 mL), and collect the remaining
2. Pass through a syringe filter (0.22 µm).
3. Collect and pass through a centrifuge spin filter (16,800 g, 10–20 ) until sufficient volume has been collected for analysis.

Analytical method

LC-MS/MS

Reagents

1. Acetonitrile (HPLC-grade).
2. Water (Milli-Q).
3. Internal standard (deuterated acrylamide 0 µg/mL) in water.

Additional information:

1. If not analysing samples directly after homogenization, store at -20 Celsius until required.
2. If analysing potato crisps (potato chips), extra centrifugation may be required. Freeze the extract to precipitate out. Thaw, then centrifuge (16,800 g, 10 min).

References

Analysis of acrylamide in cooked foods by liquid chromatography tandem mass spectrometry. Rosen, -J et al Analyst, 2002, 127; 880-882.

Literature number: IST1076A

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