Dispersive micro-solid phase extraction combined with gas chromatography-chemical ionization mass spectrometry for the determination of N-nitrosamines in swimming pool water samples

A simple sample pretreatment technique, dispersive micro-solid phase extraction, was applied for the extraction of N-nitrosodimethylamine (NDMA) and other four N-nitrosamines (NAs) from samples of swimming pool water. The parameters affecting the extraction efficiency were systematically investigated. The best extraction conditions involved immersing 75 mg of carbon molecular sieve, Carboxen (TM) 1003 (as an adsorbent), in a 50-mL water sample (pH 7.0) containing 5% sodium chloride in a sample tube. After 20 min of extraction by vigorous shaking, the adsorbent was collected on a filter and the NAs desorbed by treatment with 150 mu L of dichloromethane. A 10-mu L aliquot was then directly determined by large-volume injection gas chromatography with chemical ionization mass spectrometry using the selected ion storage mode. The limits of quantitation were < 0.9 ng/L. The precision for these analytes, as indicated by relative standard deviations, were < 8% for both intra- and inter-day analyses. Accuracy, expressed as the mean extraction recovery, was between 62% and 109%. A preliminary analysis of swimming pool water samples revealed that NDMA was present in the highest concentration, in the range from n.d. to 100 ng/L.