This study was conducted to validate the semi-quantitative food frequency questionnaire that was developed to assess the intakes of fatty acids, as well as energy, carbohydrates, fat, protein, minerals and vitamins in Korean adults. The validity of the semi-quantitative food frequency questionnaire was tested on 78 subjects (31 men, 47 women) aged 34 to 66 years. The semi-quantitative food frequency questionnaire included 93 food items and was validated on two 3-day dietary records. The mean intakes and the Spearman Correlation Coefficients between the semi-quantitative food frequency questionnaire and the two 3-day dietary records were analyzed for each nutrient and food group level. The mean nutrient intakes obtained from the semi-quantitative food frequency questionnaire were estimated to be greater than those of the two 3-day dietary records. The Spearman Correlation Coefficients between the energy-adjusted nutrient intakes from the semi-quantitative food frequency questionnaire and the two 3-day dietary records ranged from 0.24 for polyunsaturated fatty acids to 0.55 for fat in men and from 0.29 for polyunsaturated fatty acids to 0.55 for saturated fatty acids in women, respectively. The Spearman Correlation Coefficients for food intake ranged from 0.11 for teas and beverages to 0.58 for grains and their products in men, -0.04 for potatoes and starches to 0.73 for milk and dairy products in women. Foods consumed regularly had lower intra-person variation and tended to have higher observed correlation coefficients. These results indicate that the semi-quantitative food frequency questionnaire is a useful tool for estimating nutrient intakes, particularly of total fat and saturated fatty acid intakes.