A study was undertaken to determine the extent of loss of nitrite during the analytical workup of cured meats for nitrite analysis. Two extraction techniques were compared: (A) a relatively long (2 hr) and hot (80 degrees C) procedure carried out at the natural pH of the sample, and (B) the method of Sen and Donaldson that specifies an alkaline solution and much milder conditions (20 min at 50 degrees C at pH 8) for extraction. The data obtained suggest that considerable losses of nitrite can occur with the former procedure, especially in acidic samples. The overall percentage recoveries of added nitrite by the 2 methods ranged between 20 and 112, and 80 and 114, respectively. Average percentage recoveries for the acidic (pH less than 5) samples only were 47.2 for Method A as compared with 100.2 for Method B.