The growth in nuclear medicine for both personalized healthcare and to support drug discovery efforts is creating unprecedented demand for radiopharmaceuticals, bioactive molecules labeled with a radionuclide. Given the highly specialized and costly infrastructure required to produce radiopharmaceuticals (e.g., cyclotrons, hot-cells, automated synthesis modules, specialized analytical equipment), radiopharmaceutical production capabilities are not easily expandable on a short timeframe to meet this rapid growth. As such, new approaches for how radiopharmaceutical syntheses are developed and optimized are urgently needed to meet growing routine clinical production demands on radiochemistry facilities while also continuing innovation of new radiopharmaceuticals. High-throughput experimentation (HTE) holds enormous potential in this regard, and this chapter summarizes the current state-of-the-art of HTE as it pertains to radiochemistry, including both sequential and parallel methods for high-throughput radiolabeling (using vials, multi-well plates, flow chemistry, and droplet-based methods) and analysis (including UPLC, multi-lane radio-TLC, and solid-phase extraction (SPE) approaches). Comparison of the various high-throughput approaches is considered, along with key pros and cons for the different methods, as well as thoughts on how to standardize data acquisition and future outlooks.