This review highlights developments in mycotoxin analysis and sampling over a period between mid-2009 and mid-2010. It covers the major mycotoxins aflatoxins, Alternaria toxins, ergot alkaloids, fumonisins, ochratoxin, patulin, trichothecenes, and zearalenone. New and improved methods for mycotoxins continue to be published. Immunological-based method developments continue to be of wide interest in a broad range of formats. Multimycotoxin determination by LC-MS/MS is now being targeted at the specific ranges of mycotoxins and matrices of interest or concern to the individual laboratory. Although falling outside the main emphasis of the review, some aspects of natural occurrence have been mentioned, especially if linked to novel method developments.