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Method
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Method |
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Sample pretreatment
600 mg dried and homogenized sample is extracted using 5 ml of milliQ water. 1 ug of internal standard 13C3 acrylamide in solution (CIL) is added to the extract. After 10 minutes of centrifugation (6000 rpm), 3 ml of the upper layer is brought on a extreluut- 3BT column (Merck). Using 15 ml of ethylacetate, acrylamide is eluted from the column. Ethyl acetate is evaporated under a gentle stream of nitrogen down to approximately 0.5 ml.
Chromatographic conditions
The ethylacetate solution is analysed using gas chromatography. Separation is obtained using a CP-Wax 57 (Varian) column (length 25 m, internal diameter 0.32 mm, film 1.2 um) and helium as the carrier gas with a constant flow of 5.4 ml/min. Split-less injection of 3 ul is performed. Oven temperature is kept at 50 °C for 1 minute, after which the temperature is increased with 30 °C/min towards 220 °C. After 12 minutes of constant temperature of 220 °C the oven is cooled down and stabilized before next injection.
Detection is performed using on-line chemical ionization mass spectrometry in positive ion mode, using methane as ionization gas. The Characteristis ions m/z 72 (acrylamide) and m/z 75 (13C3 acrylamide) are monitored for quantification.
Analytical equipment
GC: HP6890 (Hewlet Packard)
MSD (mass selective detector): HP5973 (Hewlet Packard)
Amounts in ppm or ppb are based on the amount flour, unless stated otherwise.
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FAQ
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Quelles sont les principales caractéristiques du Beta-Glucane de Levure ?
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