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The pre-analytical step preceding peptide extraction from the plasma matrix is crucial since peptides are often cleaved in vivo and ex vivo by several specific and nonspecific proteases. Kowalka et al.[1] recently validated a new Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS) assay for PYY1-36 and PYY3-36 in human plasma using three different guidelines: the 2018 Food and Drug Administration (FDA) guideline for bioanalytical method validation, the 2014 Clinical and Laboratory Standards Institute (CLSI) C62-A guideline and the penultimate 2011 European Medicines Agency (EMA) guideline on bioanalytical method validation updated in 2015. [Extracted from the article]