The Global Monitoring Plan of the Stockholm Convention sets a framework for the analysis of persistent organic pollutants (POPs); therein, the congeners recommended for analysis in the core matrices are listed (see chapter 2 of the “Guidance on the global monitoring plan for persistent organic pollutants”, UNEP 2013). A protocol is needed to ensure that these compounds are always analysed correctly in various laboratories and in the same way. This procedure covers polychlorinated biphenyls (PCB) and organochlorine pesticides (OCP). The present protocol describes the method for sample preparation, extraction, purification and analysis of six indicator PCB and OCPs (see Table 1) in human milk, human serum and air.