Australian firebrand Kyrgios went down 7-6 (7/2), 6-7 (4/7), 7-6 (7/3) to Frenchman Giovanni Mpetshi Perricard in almost two and a half hours as serve dominated.
The 2022 Wimbledon finalist Kyrgios, 29, is making his comeback following wrist reconstruction and other injuries over the past couple of years.
Ahead of the Australian Open starting on January 12, big-serving Mpetshi Perricard said Kyrgios had shown enough to suggest that his comeback would be a success.
Kyrgios played and won in the doubles with Novak Djokovic on Monday.
“Playing Nick here wasn’t a good match-up for me,” the 21-year-old Mpetshi Perricard said, asked about playing Kyrgios in front of his home crowd.
“He did some good things — he played with confidence. I’m sure he’s going to be back in the next few months.”
The Frenchman, who has risen from 205 in the world at the start of 2024 to his current ranking of 31, fired down 36 aces.
Sabalenka kickstarted her bid to win the Australian Open for a third consecutive time with a straight-sets win.
The Belarusian appeared bothered by the high humidity on Pat Rafter Arena in Brisbane, particularly during an error-strewn first set.
But after breaking Mexico’s Renata Zarazua at 5-4, the 26-year-old surged through the second set to wrap up the match 6-4, 6-0 in 65 minutes.