Acrylamide by QuEChERS Extraction with LC–MS-MS Detection

Acrylamide is a neurotoxic compound classified as a probable human carcinogen and genotoxicant (1). In 2002, researchers in Sweden uncovered the presence of acrylamide in certain fried and baked foods at relatively high levels (2). Acrylamide is formed during cooking at high temperatures through the Maillard reaction of asparagine and reducing sugars. This application provides a quick and easy method for the extraction of acrylamide from a variety of food matrices.

Extraction and Clean-up Materials

Extraction Procedure

a) Add 5 g of homogenized sample to a 50 mL centrifuge tube.

b) Fortify with an internal standard.

c) Add 10 mL of reagent water, vortex briefly.

d) Allow ≥15 min for hydration.

e) Add 10 mL of acetonitrile, vortex briefly.

f) Add salts from Mylar pouch (ECMSSC50CT-MP).

g) Shake vigorously for 1 min.

h) Centrifuge at 5000 rpm for 10 min.

i) Supernatant is ready for cleanup.

QuEChERS Cleanup

a) Add 1 mL of supernatant to the 2 mL centrifuge tube (CUMPS15C18CT).

b) Vortex for 30 s.

c) Centrifuge at 5000 rpm for 10 min.

d) Transfer 500 µL of extract into vial for analysis.

LC–MS–MS Instrumentation

Figure 1: Chromatogram of a 10 ng/mL matrix-matched std.

LC: Thermo Accela 1250 pump

• Column: Sepax C18, 150 mm × 2.1 mm, 3 µm

• Guard: Restek C18 2.1 × 20 mm

• Column temperature: Ambient

• Injection volume: 20 µL

• Mobile phase: A: water; B: methanol

• Gradient: 0–3 min: 100% A; 5–6 min: 100% B; 7–12 min: 100% A

• Flow rate: 200 µL/min

MS–MS: Thermo TSQ Vantage

• Ion source: positive APCI

Figure 2: Calibration curve with a 10–1000 ng/mL concentration range.

Conclusions

A QuEChERS method has been successfully developed for the extraction and purification of acrylamide in various food matrices. PSA and C18 in the dSPE step eliminates the need for hexane defatting and results in clean extracts.

References

(1) Zhang et al., Chemical Reviews, 109, 4375–4397 (2009).

(2) Swedish National Food Administration, Information on acrylamide in food. April 24, 2002, www.slv.se.

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