The　accumulation　and　spatial　distribution　of　intracellularnanoplasticparticles　provide　useful　information　about　their　spatiotemporal　toxicologicaleffects　mediated　by　the　physicochemical　parameters　of　nanoplasticsin　living　cells.　In　this　study,　a　sample　injection-transfer　methodwas　designed　with　an　accuracy　of　up　to　femtoliters　to　attoliters　tomatch　the　volume　required　for　ultranarrow-bore　open-tubular　liquidchromatography.　The　separation　and　concentration　quantification　ofmixed　polystyrenes　in　different　regions　in　living　cells　were　achievedby　directly　transferring　picoliter/femtoliter　volumes　of　intracellularcytoplasm　to　an　ultranarrow-bore　open-tubular　chromatographic　column.The　measurement　of　pollutant　concentration　in　different　areas　of　asmall-volume　target　(single　cell)　was　realized.　This　method　is　expectedto　be　used　in　the　qualitative　and　quantitative　analyses　of　complex,mixed,　and　label-free　nanoplastics　(a　few　nm　in　size)　in　the　subregionsof　living　cells.