Tunisian Ons Jabeur became the first major casualty on the opening day of the French Open on Sunday when the in-form sixth seed crashed out with a 3-6, 7-6 (4), 7-5 loss to Poland's Magda Linette.
Later, 10th-seeded Spaniard Garbine Muguruza went down 2-6, 6-3, 6-4 to Estonia's Kaiai Kanepi.
Jabeur, seen as one of the big threats to World No. 1 Iga Swiatek at the claycourt Grand Slam, came to Paris at a career-high ranking and with a tour-leading 17 wins on the surface.
With her win in Madrid and runner-up finishes in Rome and Charleston, it seemed like Jabeur would have an easy outing against Linette when she made a strong start on Court Philippe Chatrier under overcast skies.
The 27-year-old suffered an early break of serve before breezing through the opening set in 37 minutes before Linette, who was ranked 56th before the start of the second major of the year, raised her game.
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Linette, 30, had only defeated Jabeur in the first of their four meetings back in 2013 but she staged an inspired fightback in the second set, saving four breakpoints to level the match in the tiebreak.
As drops of rain fell on the main showcourt, Jabeur's level also dipped and her unforced errors climbed and she made her frustration evident by kicking balls away after losing points.
Linette, who lost to Jabeur in the third round last year, went up 4-2 in the third set but saw her advantage slip away when Jabeur broke her serve back to stay alive.
But the Pole sealed the match when the Tunisian wasted a 40-0 lead in the 12th game and found the net on match point to be broken for the second time in the set.
"I had so many tough matches with Ons and last year here I lost to her in the third round so I knew how difficult it's going to be," Linette said on court.
"She was playing so well all this time. I knew I have to be focused and play every single point and try to make her uncomfortable. I am happy that I just managed to fight for every single point."
Linette will next play Martina Trevisan of Italy or Briton Harriet Dart.
Muguruza's freefall continues
Former champion Muguruza suffered a second consecutive first-round exit at the French Open, biting the red dirt in a 2-6, 6-3, 6-4 loss to Kanepi.
Muguruza, who lifted the Suzanne Lenglen Cup in 2016 and reached the semi-finals at Roland Garros two years later, was in cruise control in a one-sided first set before Kanepi ground her way back into the match.
The decider was close but the 36-year-old Kanepi, who has reached the last eight in all the Grand Slam tournaments, took her chances and prevailed when Muguruza made an unforced error.
Muguruza finished last year on a high, winning the WTA finals, but the world number has had a dreadful 2022, managing consecutive wins only once.
The 28-year-old Spaniard was at a loss to explain her decline.
"It is very hard, in the end. You have nothing guaranteed. The fact that you finished the year, the previous year well doesn't guarantee that you're going to start the year playing at the same level," Muguruza told a news conference.
"You've got to work and you've got to fight for it. We all know that every year is different and so far just working through it.
"It's been a tough season though. I mean, I've had matches so much in control, but then I don't manage to close and it gets complicated and then a match is a match and at the end there's only a winner. But I feel that I'm training hard, I'm putting the work.
Muguruza is, however, confident she can turn things around.
"I'm playing tournaments, trying to switch those moments, try to get more confident," she said.
"So we're going to keep doing it. I mean at some point I'm a hundred percent sure that I'm going to go out there and get those wins that have been slipping away from me."
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