Quantitation of acrylamide in food products by liquid chromatography/mass spectrometry.
A simple and inexpensive liquid chromatography/mass spectrometry (LC/MS) method was developed for the quantitation of acrylamide in various food products. The method involved spiking the isotope-substituted internal standard (1-C13 acrylamide) onto 6.00 g of the food product, adding 40 mL distilled/deionized water, and heating at 65 degrees C for 30 min. Afterwards, 10 mL ethylene dichloride was added and the mixture was homogenized for 30 s and centrifuged at 2700 x g for 30 min, and then 8 g supernatant was extracted with 10, 5, and 5 mL portions of ethyl acetate. The extracts were combined, dried with sodium sulfate, and concentrated to 100-200 microL. Acrylamide was determined by analysis of the final extract on a single quadrupole, bench-top mass spectrometer with electrospray ionization, using a 2 mm id C18 column and monitoring m/z = 72 (acrylamide) and m/z = 73 (internal standard). For difficult food matrixes, such as coffee and cocoa, a solid-phase extraction cleanup step was incorporated to improve both chromatography and column lifetime. The method had a limit of quantitation of 10 ppb, and coefficients of determination (r2) for calibration curves were typically better than 0.998. Acceptable spike recovery results were achieved in 11 different food matrixes. Precision in potato chip analyses was 5-8% (relative standard deviation). This method provides an LC/MS alternative to the current LC/MS/MS methods and derivatization gas chromatography/mass spectrometry methods, and is applicable to difficult food products such as coffee, cocoa, and high-salt foods.
Eberhart
B Loye
BL
The Procter and Gamble Co., Winton Hill Business Center, 6300 Center Hill Ave, Cincinnati, OH 45224, USA.
Ewald
Deborah K
DK
Sanders
Robert A
RA
Tallmadge
Daniel H
DH
Zyzak
David V
DV
Strothers
Melissa A
MA
D000085:Acetates / Q000032:analysis; D020106:Acrylamide / Q000032:analysis*; D002099:Cacao; D002623:Chemistry Techniques, Analytical / Q000295:instrumentation / Q000379:methods*; D002845:Chromatography; D002853:Chromatography, Liquid / Q000379:methods*; D003069:Coffee; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D013058:Mass Spectrometry / Q000379:methods*; D011208:Powders; D012015:Reference Standards; D015203:Reproducibility of Results; D011198:Solanum tuberosum; D013431:Sulfates / Q000494:pharmacology; D013696:Temperature
D000085:Acetates; D003069:Coffee; D011208:Powders; D013431:Sulfates; C012036:sodium sulfate; D020106:Acrylamide; C007650:ethyl acetate