A Compound Specific Stable Isotope (CSSI) sediment tracing approach is evaluated for the first time in an agricultural catchment setting against established geochemical fingerprinting techniques. The work demonstrates that novel CSSI techniques have the potential to provide important support for soil resource management policies and inform sediment risk assessment for the protection of aquatic habitats and water resources. Analysis of soil material from a range of crop covers in a mixed land-use agricultural catchment shows that the carbon CSSI signatures of particle-reactive fatty acids label surface agricultural soil with distinct crop-specific signatures, thus permitting sediment eroded from each land-cover to be tracked downstream. High resolution sediment sampling during a storm event and analysis for CSSI and conventional geochemical fingerprints elucidated temporal patterns of sediment mobilisation under different crop regimes and the specific contribution that each crop type makes to downstream sediment load. Pasture sources (65% of the catchment area) dominated the sediment load but areal yield (0.13 +/- 0.02 t ha(-1)) was considerably less than that for winter wheat (0.44 +/- 0.15 t ha(-1)). While temporal patterns in crop response matched runoff and erosion response predictions based on plot-scale rainfall simulation experiments, comparison of biomarker and geochemical fingerprinting data indicated that the latter overestimated cultivated land inputs to catchment sediment yield due to inability to discriminate temporary pasture (in rotation) from cultivated land. This discrepancy, however, presents an opportunity since combination of the two datasets revealed the extremely localised nature of erosion from permanent pasture fields in this system (estimated at up to 0.5 t ha(-1)). The novel use of CSSI and geochemical tracers in tandem provided unique insights into sediment source dynamics that could not have been derived from each method alone. Research into CSSI signature development (plant and soil processes) and the influence of cultivation regimes are required to support future development of this new tool. (C) 2011 Elsevier B.V. All rights reserved.