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Excessive absorption of migrating substances from food contact materials can affect human health. Thus, it is essential to analyze the migration of contaminant from food contact materials. However, comprehensive analysis has been challenged by low concentration of migrating substances, manifold and complex matrix interference of food contact materials. Therefore, appropriate sample pretreatment methods should be applied before instrumental detection, which is essential to improve the analytical efficiency, sensitivity, and reliability. This paper systematically reviews the development of sample pretreatment methods for analysis of migrating substances from food contact materials in the past decade. To extract volatile and semi‐volatile substances, headspace extraction, headspace solid phase microextraction, and purge and trap technique are discussed. For non‐volatile substances, solid–liquid extraction and field‐assisted extraction are usually used to extract them from food contact materials, while liquid–liquid extraction, solid phase extraction, and their corresponding microextraction techniques play important roles on enrichment process. In addition, new progress in developments of sample pretreatment methods of food contact materials is summarized, covering new devices, specific adsorbents, and sample preparation methods for rapid detection. An outlook of future prospect of sample pretreatment, especially for non‐targeted analysis of non‐intentionally added substances is briefly discussed.

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To expand the application of pillararene in chromatographic separation, we designed and fabricated a pillar[5]quinone‐amine polymer coated silica through quinone‐amine reaction by facile one‐pot synthesis method, which was applied as a stationary phase for high‐performance liquid chromatography. Separation of hydrophobic compounds, hydrophilic compounds, halogenated aromatic compounds, and 11 aromatic positional isomers was achieved successfully in this stationary phase. Reverse‐phase separation mode and hydrophilic‐interaction separation mode were proved to exist, indicating the potential application of the mix‐mode stationary phase. Studies of chromatographic retention behavior and molecular simulation showed that multiple interactions might play an important role in the separation process, including hydrophobic interaction, hydrogen‐bonding interaction, aromatic π‐π interaction, electron donor‐acceptor interaction, and host‐guest interaction. Column repeatability and stability were tested, which showed relative standard deviations of retention time less than 0.2% for continuous 11 injections, and the durability relative standard deviations of retention time were less than 0.91% after 90 days. This novel design strategy would broaden the application of pillararene‐based covalent organic polymer in chromatography and separation science.