The champions were sluggish throughout at Estadio Jose Zorrilla and Fausto Rossi's early goal ensured the initiative at the top is now with Atletico Madrid, who visit Celta Vigo later on Saturday, and Real Madrid, who host Levante on Sunday.
Gerardo Martino's men had very little to shout about in the first half, as Valladolid goalkeeper Diego Marino kept them at bay with several important stops, with Rossi firing the relegation-threatened home side into a 17th-minute lead.
Lionel Messi saw numerous chances saved by Marino, while Neymar spurned a huge opportunity from close-range to level matters in the second half.
Barca piled on the pressure in the latter stages, but their inability to salvage a draw leaves Real Madrid a point clear at the top ahead of their clash with Levante, while Atletico will go second if they win in Vigo.
Valladolid, meanwhile, move out of the relegation zone, overtaking Almeria on goal difference.
The build-up to the game was dominated by the news that Barca captain Carles Puyol will end his 19-year association with the club at the end of the season, and he was left out in favour of the returning Gerard Pique.
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