Bilimbi fruit (Averrhoa bilimbi L.) contains bioactive compounds with antioxidant and α-glucosidase inhibitory potential. This study compared 70% ethanolic extracts prepared by maceration and ultrasound-assisted extraction (UAE) in terms of yield, total phenolic content (TPC), total flavonoid content (TFC), DPPH radical-scavenging activity, α-glucosidase inhibition, and LC-HRMS metabolite profiles. Maceration produced a higher yield than UAE (16.23% vs. 11.16%), whereas TPC and TFC were comparable. UAE showed lower DPPH IC₅₀ (37.06 ± 0.27 vs. 51.59 ± 0.21 µg/mL) and α-glucosidase IC₅₀ (23.94 vs. 33.45 µg/mL) than maceration. LC-HRMS yielded 24 tentative or probable metabolite annotations, of which seven were selected for focused interpretation. Because each extraction method was performed once and analytical measurements were technical replicates, between-method differences are descriptive. LC-HRMS findings were qualitative and do not establish quantitative enrichment or compound-specific causality.
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