World number five and the tournament's top seed, Aryna Sabalenka, was upset by American Amanda Anisimova 3-6 6-4 6-3 in the third round at the Charleston Open.
Sabalenka's serve was the key to her early success, connecting on 73 per cent of her first serves, and winning 15 of the 19 points in that situation (79 per cent).
When Sabalenka's first serve percentage fell to 48 in the second set, Anisimova found her footing, breaking twice in the frame, before pouncing on the Belarusian's lacklustre second serve in the deciding set, winning seven of nine opportunities to earn the break and the win.
Sixth seed Jessica Pegula was also bounced in surprising fashion, losing 6-4 3-6 6-4 to unseeded compatriot Coco Vandeweghe.
In a razor-close contest, it came down to who took their chances, as Vandeweghe saved seven of the 10 break points she faced, while Pegula could only save one of five.
World number 10 Ons Jabeur had no problem navigating the challenge of Emma Navarro, winning 6-3 6-2 as she broke her opponent's serve on six occasions.
Canadian seventh seed Leylah Hernandez also fell victim to an unseeded upset, going down 3-6 6-3 6-4 against Poland's Magda Linette.
In a meeting between two top-10 seeds, Belinda Bencic got the better of Madison Keys to edge it 6-4 6-4.
Second seed Paula Badosa had to come from a set down to eventually get the better of Claire Liu 3-6 7-6 (10-8) 6-1.
In the late session, French 12th seed Alize Cornet went down in a close tussle against Ukraine's Anhelina Kalinina 7-6 (7-5) 7-5, while Jabeur won her second match of the day, beating Irina Begu 6-3 6-2.
Meanwhile, in Bogota at the Copa Colsanitas, top seed Camila Osorio dispatched Turkish opponent Ipek Oz 6-3 7-6 (7-4) to move on to the quarter-final where she will meet Elina Avanesyan.
Alcaraz begins Madrid Open campaign with emphatic win
Carlos Alcaraz continued his fine record at the Madrid Open with an emphatic 6-2 6-1 victory over Alexander Shevchenko on Friday.
The two-time defending champion made it 12 straight wins at his home tournament to ensure he will face Brazilian Thiago Seyboth Wild in the last 32.
Alcaraz was playing his first match on the ATP Tour since March 28 after being unable to compete in the Monte-Carlo Masters and Barcelona Open due to an arm injury.
But he was still able to make a fine start to his clay-court season, breaking serve in the first game and racing to victory in only one hour and eight minutes.
Data Debrief
Sometimes the scoreline can be harsh on a beaten player, but on this occasion Alcaraz was clearly dominant, breaking the Kazakh seven times in the match and forcing 11 break-point opportunities while conceding only three for his opponent.
That allowed the Spaniard to claim a dominant victory despite being broken once in each set. He will now turn his attention to a clash with Seyboth Wild, who battled past Lorenzo Musetti with a 6-4 6-4 win.
Reigning champion Sabalenka pushed by Linette at Madrid Open
Aryna Sabalenka got her Madrid Open campaign started with a 6-4 3-6 6-3 win over Magda Linette on Friday.
Sabalenka could not quite hit her peak form against Linette, but the world number two nevertheless got the job done after going the distance.
The Belarusian is hunting a record-equalling third title in Madrid, where she is the reigning champion, though she has not won back-to-back matches at a tournament since winning the Australian Open.
"It's not about being confident," Sabalenka said. "It's about how much you're ready to do to get it. It's about the hard work and to be ready, be ready for the big fights. I feel like confidence is not going to help you in those big matches. It's about staying there and fighting for it."
Data Debrief
Sabalenka (70 per cent, 56-24) is now one of five active players since 2020 to hold a winning percentage of 70 per cent or higher at WTA-1000 events.
Iga Swiatek, Simona Halep, Elena Rybakina and Jessica Pegula are the other players to feature on that list.
Rybakina continues clay winning streak with victory over Bronzetti
In-form Elena Rybakina has moved into the last 32 of the Madrid Open after a straight sets victory over Italian Lucia Bronzetti.
Number four seed Rybakina triumphed 6-4 6-3 on Friday and will next face either Marta Kostyuk or Mayar Sherif.
Rybakina was broken early in each set but ultimately had few problems getting over the line, converting four of her five break points to continue an impressive run of results after winning the Stuttgart Open last week.
She has now won five consecutive WTA matches and has 13 straight wins on clay courts to her name in a superb streak that started one year ago.
Data Debrief: Rybakina in elite company
Since the start of 2020, only two other players have claimed as many 13 consecutive WTA wins on clay, and they are Iga Swiatek and Simona Halep, so Rybakina is in elite company.
Rybakina's last defeat on this surface came in the 2023 edition of the Madrid Open, when she fell to Anna Kalinskaya in her first match, so this win represented a better start to her campaign in the Spanish capital.
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