PEGylation of CNTs-MNP result in novel nanocomposites with good water dispersibility. PEG-CNTs-MNP evaluated as DSPE adsorbent for extraction of Z-ligustilide. PEG-CNTs-MNP shows good selectivity in extracting Z-ligustilide from herbal extracts. Quick DSPE method for isolating Z-ligustilide from herbal extracts established.