The occurrence of mycotoxins in foods and feeds has long been recognized as a potential hazard for human and animal health due to its severe toxic and carcinogenic properties. Among various mycotoxins, aflatoxins (AFs), ochratoxin A (OTA) and zearalenone (ZON) are most important because of many contamination cases in the world. In this study, a simple and rapid multiresidue method to quantify AFB1, AFB2, AFG1, AFG2, OTA and ZON was developed. The simultaneous determination of these 6 mycotoxins was performed using immunoaffinity column for clean-up and liquid chromatography/electrospray tandem mass spectrometry (LC-MS/MS) for quantification. Cereal samples were extracted with 80% methanol followed by a Vicam AOZTM immunoaffinity column clean-up. Mycotoxins were eluted from the column with methanol and quantified using Selected Reaction Monitoring (SRM) mode in LC-MS/MS with an electrospray ionization (ESI) interface. A mobile phase of methanol-water was used. Average recoveries of AFs, OTA and ZON spiked in cereals ranged 65 - 95%, 66 - 83% and 69 - 86%, respectively. Good accuracy and precision results were also obtained in intra-day and inter-day analysis. The limit of quantitation (LOQ) of AFB1, AFB2, AFG1, AFG2, OTA and ZON were 0.1, 0.2, 0.1, 0.3, 0.03 and
2 ppb, respectively. Thirty-five commercial cereal products including thirteen wheat samples, seven oat samples, six rice samples and nine corn samples were analyzed. The results showed that OTA was detected in four samples ranging from 0.05 to 0.07 ppb, and ZON was detected in two samples ranging from 2.73 to 4.73 ppb. This rapid, easy and highly efficient method was successfully developed. Six common mycotoxins could be analyzed in a single 20-min run. The method could be applied to routine cereal analysis, thus dramatically shortening the analysis time.