The impact of improved spectroscopic techniques on structural elucidation is shown by examples from recent work on CNS active tiglianes from Pycnocoma cornuta Muell. The limited quantities of substance now needed for structural analysis can usually be obtained by routine high performance chromatography, but this methodology is less suited for large scale preparations. It may then be worthwhile also to consider earlier materials and methods. Particularly liquid-liquid partitioning in old or new versions (CCC) may have advantages with respect to selectivity and mildness. In special cases activated carbon adsorbents may offer the benefits of selectivity and tolerance to high sample loads.