Emma Raducanu's Madrid Open campaign was ended by Marta Kostyuk on Friday, with the Ukrainian winning their second-round match in three sets.
Raducanu had momentum on her side after recovering from a set down to level, two days on from her straight-sets victory over Suzan Lamens.
But the 2021 US Open champion could not get over the line as Kostyuk recovered her composure to win 6-4 2-6 6-2.
Three breaks in the second set had got Raducanu back on level terms, but she was then immediately broken in the opening game of the decider.
Raducanu broke back to level the set at 2-2, but she was again unable to harness that momentum as Kostyuk reeled off the next four games to take the match.
Fantastic Friday
— wta (@WTA) April 25, 2025
What was your favorite match?#MMOPEN pic.twitter.com/7moY3mE5bo
Speaking after her win, Kostyuk said: "I knew Emma's a great fighter and she's achieved a lot and can play amazing tennis.
"It was going to be a battle, so I'm very happy with the win."
Kostyuk will be joined in the next round by Jessica Pegula, who cruised past Germany's Eva Lys 6-2 6-2 in just 74 minutes.
The world number three has now won 14 of her 20 matches at clay-court WTA 1000 events, with only Serena Williams (16) winning more from her first 20 matches at such events among American players since the format's introduction in 2009.
Elena Rybakina, meanwhile, beat former US Open champion Bianca Andreescu 6-3 6-2 to tee up a meeting with Elina Svitolina in the last 32.
Data debrief: Raducanu brought back to earth
Raducanu opened her Madrid Open campaign with her first outdoor clay-court victory in three years, but she was brought back to earth by an opponent who needed a medical timeout after struggling with a wrist issue in the first set.
Kostyuk is already on her deepest run in Madrid, having edged a topsy-turvy game that featured 16 breaks of serve – 11 for the Ukrainian and five for Raducanu.
Kostyuk has now beaten Raducanu twice in three head-to-head meetings, having lost the previous clash at the exact same stage of the Madrid Open in 2022.