Development and single-laboratory validation of a reversed-phase liquid chromatography-electrospray-tandem mass spectrometry method for identification and determination of acrylamide in foods.
A rapid and accurate method using reversed-phase liquid chromatography-tandem mass spectrometry interfaced with electrospray was developed for determination of acrylamide in cooked food samples. A simplified sample treatment procedure using an extraction step with acidified water without cleanup was developed. A C18 column with an aqueous formic acid-methanol mixture as the mobile phase was used under isocratic conditions. The method was validated in-house for robustness, limits of detection (LOD) and quantitation (LOQ), linearity, recovery, and accuracy both on standard and baked-product and potato flour matrixes. Good results in the low ppb level were obtained for LOD (< 15 microg/kg) and LOQ (< 25 microg/kg) of acrylamide in samples. Excellent linearity (r2 = 0.999-1.000) was established over 2 orders of magnitude by performing statistical tests. The absence of both constant and proportional systematic errors demonstrated good method accuracy. Excellent results were obtained for intraday repeatability (RSD < 1.5%) and between-day precision (RSD < 5%). Extraction recoveries from food products were calculated in the 97 +/- 3-99 +/- 2% (n = 6) range with a labeled internal standard (13C3-acrylamide). The applicability of the method to determination of acrylamide in cooked food products was demonstrated.
Calbiani
Francesca
F
Consorzio Interuniversitario di Ricerca Metodologie Analitiche e Controllo Qualità, Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica, Università degli Studi di Parma, Parco Area delle Scienze 17/A, 43100 Parma, Italy.
Careri
Maria
M
Elviri
Lisa
L
Mangia
Alessandro
A
Zagnoni
Ingrid
I
D000178:Acrylamides / Q000032:analysis*; D000465:Algorithms; D002138:Calibration; D002853:Chromatography, Liquid; D005504:Food Analysis; D007202:Indicators and Reagents; D012015:Reference Standards; D015203:Reproducibility of Results; D012997:Solvents; D021241:Spectrometry, Mass, Electrospray Ionization
D000178:Acrylamides; D007202:Indicators and Reagents; D012997:Solvents