Background:　Chiral　pollutants　present　significant　environmental　and　health　concerns,　with　neurotoxic　amino　acid　analogs　like　β-N-methylamino-L-alanine　(BMAA)　demonstrating　enantiomer-specific　bioaccumulation　in　aquatic　ecosystems.　Current　analytical　approaches　for　chiral　environmental　contaminants　rely　predominantly　on　chromatographic　techniques　that　require　extensive　sample　preparation　(typically　24　h),　limiting　field　deployment　and　high-throughput　screening　capabilities.　Detection　thresholds　for　these　compounds　(0.1–10　μg/L)　necessitate　sensitive　methodologies　that　maintain　stereochemical　integrity.　This　study　addresses　these　analytical　challenges　through　the　rational　design　of　chiral　cobalt　hydroxide　(CF–Co(OH)2)　nanomaterials　engineered　for　dual-mode　detection　and　separation　functionality.　Results:　A　hierarchical　porous　α-Co(OH)2　with　tunable　chirality　(R/S/RS　configurations)　and　morphologies　(square,　rough　surface,　snowflake,　flower-like)　via　micelle-templated　growth　strategies.　The　materials　demonstrated　dual　functionality:　(1)　Rapid　colorimetric　amino　acid　discrimination　within　5　min　with　precision　(RSD　=　4.9　%,　n　=　6),　validated　through　urinary　L-tryptophan　quantification　(17.1　±　0.4　μg/mL);　(2)　Ultrasensitive　BMAA　separation　via　SPE-HPLC-MS/MS　with　significantly　improved　detection　limits　(LOD　=　0.02　μg/kg)　and　processing　speed　(144　×　faster　than　conventional　methods).　The　colorimetric　detection　mechanism　exploits　BMAA＇s　ability　to　form　cobalt-amine　complexes　that　produce　concentration-dependent　yellow　coloration,　enabling　visual　detection　at　50　μg/kg　in　freshwater　samples.　Field　testing　successfully　detected　BMAA　in　crucian　carp　(0.39　±　0.03　μg/kg),　confirming　food-chain　biomagnification　with　excellent　recovery　(90.1–102.7　%)　across　diverse　matrices.　The　system＇s　chiral　specificity　exhibited　distinct　affinity　patterns　(BMAA:　R–Co(OH)2;　DAB:　S–Co(OH)2)　with　91.4　%　enantiomeric　excess　in　just　10　min　through　configuration-specific　＇three-point　binding＇　mechanisms　(intramolecular　binding　energy:　18.7　kcal/mol).　Significance:　This　research　establishes　morphology-programmable　chiral　materials　as　a　versatile　analytical　platform　for　rapid　on-site　environmental　monitoring　and　high-throughput　toxin　analysis.　The　developed　methodology　directly　addresses　World　Health　Organization　guidelines　for　algal　toxin　detection　in　drinking　water　while　providing　a　generalizable　approach　for　chiral　pollutant　discrimination　in　complex　environmental　and　biological　samples.　©　2025　Elsevier　B.V.