The DomZ High Priest - Beyond Good and Evil
Multiple stages and it's tough at the end when you have to figure out its pattern and be nimble with your hand shot thing.
Miasma Parasite/Raem/Memiroa - Final Fantasy: Crystal Chronicles. Long as fuck, even when you're playig on multiplayer. Also pretty hard too.
Various Colossi - Shadow of the Colossus. IMO, the hardest are the land snake, the giant eel, the tortoise crab thing, and the gecko. The last one is hard too just because it takes a while to get close to him and he shakes around a lot too.
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