We have developed a liquid-chromatographic method using atmospheric pressure chemical ionization (APCI)-mass spectrometry (MS) detection in positive mode. This method was used to separate and identify 15 sterols and 2 dihydroxy triterpenes in saponified oils, enabling the analysis of these compounds directly from saponified samples without recourse to thin-layer chromatography; this fact thus significantly simplifies the process. The analyses were made using a Waters Atlantis 5 mm dC 18 15062.1 mm column with a gradient of acetonitrile/water (0.01% acetic acid) at a flow rate of 0.5 mL/min and a column temperature of 30 7C. The quantification of several of these compounds in soybean oil, palm oil, seed oil, sunflower oil, olive-pomace oil and virgin olive oil was carried out using their commercial standards, and the results were compared satisfactorily with the official method.