The continuous evolution of analytical chemistry requires the harmonization of efficient sample preparation with high-resolution separation technologies. This contribution focuses on the strategic integration of Anton Paar microwave digestion systems with chromatographic and electrophoretic techniques—namely HPLC, UHPLC, TLC, HPTLC, GC, GC×GC, LC×LC, and Capillary Electrophoresis (CE). The objective is to demonstrate how advanced sample digestion workflows can significantly improve accuracy, reproducibility, and throughput across research, quality control, and industrial applications. Microwave-assisted digestion ensures complete and rapid sample mineralization, even for complex matrices in environmental, clinical, and materials analysis. The controlled energy transfer and real-time temperature and pressure monitoring provided by Anton Paar systems optimize sample homogeneity while minimizing matrix interferences. When coupled with chromatographic platforms such as HPLC or GC, these digestion technologies reduce background noise and matrix effects, leading to improved quantification limits and enhanced peak resolution. Furthermore, the integration with multidimensional separation techniques such as GC×GC and LC×LC enables the detailed characterization of trace-level compounds and complex mixtures. In parallel, coupling with FFF and CE expands analytical capabilities to macromolecules, nanoparticles, and biomolecular assemblies. These synergies establish a fully traceable analytical workflow, compliant with current regulatory standards and aligned with the principles of green analytical chemistry by reducing reagent consumption and waste. This presentation will provide a comprehensive overview of these combined methodologies, highlighting real case studies in pharmaceutical development, food safety, environmental monitoring, and advanced materials. Emphasis will be placed on performance metrics, workflow optimization, and cross-platform compatibility, illustrating how Anton Paar’s microwave digestion solutions empower modern laboratories to achieve reproducible, high-throughput, and regulation-ready results.