A simple and sensitive liquid chromatographictandem mass spectrometric (LC/MS/MS) method has been developed and validated to confirm and quantify acrylamide monomer (AA) in drinking water using [13C3] acrylamide as internal standard (IS). After a preconcentration by solid-phase extraction with spherical activated carbon, analytes were chromatographed on lonPac ICE-AS1 column (9 × 250 mm) under isocratic conditions using acetonitrile-water-0.1 M formic acid (43 + 52 + 5, v/v/v) as the mobile phase. Analysis was achieved using a triple-quadrupole mass analyzer equipped with a turbo ion spray interface. For confirmation and quantification of the analytes, MS data acquisition was performed in the multireaction monitoring mode, selecting 2 precursor ion to product ion transitions for both AA and IS. The method was validated for linearity, sensitivity, accuracy, precision, extraction efficiency, and matrix effect. Linearity in tap water was observed over the concentration range 0.1-2.0 μg/L. Limits of detection and quantification were 0.02 and 0.1 μg/L, respectively. Interday and intraday assays were performed across 3 validation levels (0.1, 0.5, and 1.5 μg/L). Accuracy (as mean recovery) ranged from 89.3 to 96.2% with relative standard deviation <7.98%. Performance characteristics of this LC/MS/MS method make it suitable for regulatory confirmatory analysis of AA in drinking water in compliance with European Union and U.S. Environmental Protection Agency standards.
Determination of low-level acrylamide in drinking water by liquid chromatography/tandem mass spectrometry / L., Lucentini; E., Ferretti; E., Veschetti; L., Achene; L., Turrio Baldassarri; M., Ottaviani; Bogialli, Sara. - In: JOURNAL OF AOAC INTERNATIONAL. - ISSN 1060-3271. - 92:1(2009), pp. 263-270.
Determination of low-level acrylamide in drinking water by liquid chromatography/tandem mass spectrometry
BOGIALLI, Sara
2009
Abstract
A simple and sensitive liquid chromatographictandem mass spectrometric (LC/MS/MS) method has been developed and validated to confirm and quantify acrylamide monomer (AA) in drinking water using [13C3] acrylamide as internal standard (IS). After a preconcentration by solid-phase extraction with spherical activated carbon, analytes were chromatographed on lonPac ICE-AS1 column (9 × 250 mm) under isocratic conditions using acetonitrile-water-0.1 M formic acid (43 + 52 + 5, v/v/v) as the mobile phase. Analysis was achieved using a triple-quadrupole mass analyzer equipped with a turbo ion spray interface. For confirmation and quantification of the analytes, MS data acquisition was performed in the multireaction monitoring mode, selecting 2 precursor ion to product ion transitions for both AA and IS. The method was validated for linearity, sensitivity, accuracy, precision, extraction efficiency, and matrix effect. Linearity in tap water was observed over the concentration range 0.1-2.0 μg/L. Limits of detection and quantification were 0.02 and 0.1 μg/L, respectively. Interday and intraday assays were performed across 3 validation levels (0.1, 0.5, and 1.5 μg/L). Accuracy (as mean recovery) ranged from 89.3 to 96.2% with relative standard deviation <7.98%. Performance characteristics of this LC/MS/MS method make it suitable for regulatory confirmatory analysis of AA in drinking water in compliance with European Union and U.S. Environmental Protection Agency standards.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.