This study reports an empirical research of metacognitive skills and self-regulated learning of prospective chemistry teachers through the implementation of metacognitive skill-based teaching materials. This research involved 73 prospective chemistry teachers from Universitas Negeri Surabaya, Indonesia, who were studying solution chemistry matter. The metacognitive skills of prospective chemistry teachers were obtained by the essay tests, in accordance with indicators of metacognitive skills and questionnaires to measure prospective chemistry teacher' self-regulated learning. The data analysis use percentage, n-gain, mean, standard deviation, and simple correlation Pearson Product Moment. The results showed that (1) the majority of prospective chemistry teachers had metacognitive skills and self-regulated learning in "high" and "very high," category of and (2) a positive and significant correlation between metacognitive skills and self-regulated learning. In summary, the implementation of metacognitive-based teaching materials improved the metacognitive skills, build self-regulated learning, and metacognitive skills have a significant correlation on self-regulated learning with positive correlation.