Detection of N-nitrosamines in water supplies is an environmental and public health issue because many N-nitrosamines are classified as probable human carcinogens. Some analytical methods are inadequate for detecting N-nitrosodimethylamine (NDMA) at low ng/L concentrations in water due to poor extraction efficiencies and nonselective and nondistinctive GC/MS electron ionization techniques. Development of a selective, sensitive, and affordable benchtop analytical method for eight N-nitrosamines, at relevant drinking water concentrations was the primary objective of this project. A solid-phase extraction method using Ambersorb 572 and LiChrolut EN was developed in conjunction with GC/MS ammonia positive chemical ionization (PCI). Ammonia PCI shows excellent sensitivity and selectivity for N-nitrosamines, which were quantified using both isotope dilution/surrogate standard and internal standard procedures. Method detection limits for all investigated N-nitrosamines ranged from 0.4 to 1.6 ng/L. Applying our extraction method to authentic drinking water samples with dissolved organic carbon concentrations of 9 mg/L, we were able to detect N-nitrosodimethylamine (2-180 ng/L) as well as N-nitrosopyrrolidine (2-4 ng/L) and N-nitrosomorpholine (1 ng/L), two N-nitrosamines that have not been reported in drinking water to date. With high recoveries of standards and analytes, the described internal standard method offers a valuable new approach for investigating several N-nitroso compounds at ultratrace levels in drinking water.