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Objective: Several heavy metals have been reported to be associated with metabolic syndrome(MetS) in general population, while effects of multiple metals exposure on MetS in residents living in heavy metal polluted regions have not been investigated. We aimed to assess the association of 23 metal levels and MetS among population living in China’s heavy metal polluted regions. Methods: From August 2016 to July 2017, a total of 2109 eligible participants were consecutively enrolled in our study in Hunan province, China. The levels of plasma and urine metals were measured by inductively coupled plasma mass spectrometer (ICP-MS). MetS was defined by the criteria of the International Diabetes Federation. Multivariable regression models were applied to analysis the potential relationship. Results: In the overall population, crude model showed positive relationship of plasma titanium (Ti) with MetS and negative association of urine vanadium, iron, and selenium with MetS. After adjusted for potential confounders, only plasma Ti was positive associated with MetS (adjusted OR for Q4 versus Q1: 1.46; 95% CI: 1.06–1.99), and this positive correlation was explained by abdominal obesity (OR = 1.84, 95% CI: 1.41–2.39) and high triglycerides (OR = 2.23, 95% CI: 1.68–2.96). Further linear regression analysis revealed significant association of plasma Ti levels with waist circumference (β = 0.0056, 95% CI: 0.0004–0.0109, P = 0.036) and triglycerides (β = 0.0012, 95% CI: 0.0006–0.0019, P