Sample　pretreatment　is　an　essential　step　in　chromatographic　analysis.　Solid　phase　extraction　(SPE)　is　a　widely　used　sample　pretreatment　method.　In　SPE,　the　quality　of　the　adsorbent　directly　affects　the　adsorption　and　enrichment　efficiency　of　the　target　compounds　as　well　as　the　sensitivity　and　selectivity　of　the　pretreatment　and　subsequent　analysis.　Therefore,　the　selection　and　development　of　adsorbents　has　become　a　research　hotspot.　Microporous　organic　networks　(MONs)　are　a　novel　type　of　covalent　organic　materials　that　are　synthesized　by　the　Sonogashira　reaction　of　aromatic　alkynes　and　aromatic　halides.　These　networks　have　the　advantages　of　modifiable　structures,　large　specific　surface　areas,　high　porosity,　and　simple　synthesis　methods.　This　paper　reviews　the　synthesis　and　functional　modification　methods　of　MONs,　with　an　emphasis　on　their　applications　in　sample　pretreatment.　Future　development　trends　are　also　prospected.　In　terms　of　synthesis,　the　preparation　methods　for　MON-based　materials　have　progressed　from　reflux　and　solvothermal　synthesis　to　room-temperature　synthesis,　the　conditions　of　which　tend　to　be　milder　and　more　efficient.　In　terms　of　functional　modification,　the　introduction　of　macromolecules　and　active　groups　(including　amino,　hydroxyl,　and　carboxylic　groups)　can　increase　the　selectivity　and　active　sites　of　MON-based　materials.　The　combination　of　MONs　with　Fe3O4,　SiO2,　and　metal　organic　frameworks　yields　core-shell-structured　MONs.　Furtherly,　they　can　be　calcined　and　etched　to　form　porous　carbon　structures　or　hollow　multilayer　materials.　Functionalized　MONs　and　their　composite　materials　have　multiple　interaction　mechanisms　(e.　g.,　hydrogen　bonding,　hydrophobic,　electrostatic,　and　π-π　interactions)　with　various　target　compounds,　thereby　realizing　their　efficient　extraction.　MONs　can　be　used　as　adsorbent　materials　in　SPE,　Solid　phase　microextraction,　dispersed　solid　phase　extraction,　magnetic　solid　phase　extraction,　and　other　pretreatment　methods.　When　combined　with　chromatography　and　chromatography-mass　spectrometry,　MONs　achieve　good　adsorption　effects　and　high　sensitivity,　demonstrating　the　application　potential　of　these　materials　in　sample　pretreatment.