Determination of acrylamide in drinking water by large-volume direct injection and ion-exclusion chromatography–mass spectrometry

Acrylamide, a known neurotoxin and putative human carcinogen, has been included among the substances to be monitored in drinking water according to the European Union Directive 98/83 on potable water. This paper reports a new method based on the combination of ion-exclusion chromatographic separation and MS detection. Samples of drinking water have been directly injected in the microbore ICE-AS1 column and detected in the selected-ion monitoring mode by a single quadrupole system with electrospray ionization. Chromatographic conditions, such as eluent composition and flow rate, have been optimized by a central composite design experiment. Statistical analysis of data showed that the amount of acetonitrile fraction in the eluent mixture, composed by acetonitrile and formic acid solution, is the variable that most influences retention of the acrylamide peak. After optimization of MS detection parameters, this method has been validated for spiked drinking water samples. The effect of large-volume injection (up to 500 μl) has been also explored. Linearity was evaluated from 0.5 to 5 μg l−1. Repeatability, expressed as R.S.D., was 16 and 12% at 0.5 and 1 μg l−1, respectively. The limit of detection was 0.20 ppb with 500 μl injection volume.