A mechanochemical-assisted extraction (MCAE) method was proposed and investigated for the fast extraction of two kaempferol glycosides (kaempferol-3-O-[2-O-β-D-galactopyranosyl-6-O-α-L-rhamnopyranosyl]-β-D-glucopyranoside and kaempferol-3-O-[2-O-β-D-xylopyranosyl-6-O-α-L-rhamnopyranosyl]-β-D-glucopyranoside) from Camellia oleifera Abel. meal. The effects of operating parameters in terms of NaOH content, grinding time, extraction time, and ratio of solution to solid were evaluated by means of response surface methodology (RSM). Under the optimal conditions with a ratio of material to NaOH of 20:1 (g/g), a milling time of 15 min, and a ratio of solution to solid of 20:1 (mL/g) for 60 min, the maximum extraction yields of the two kaempferol glycosides reached 13.34 and 13.83%, respectively. The antioxidant activity of kaempferol glycosides extract was assessed by 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical-scavenging assay and ferric thiocyanate (FTC) assay. Compared with the heat reflux extraction (HRE) method, the yield and the antioxidant activities of the extracts from MCAE with water as solvent were higher and stronger.
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