Application of the HPLC-SPE-NMR technique to identify the alkaloids in an EtOH extract of the leaves of Neolitsea sericea var. aurata led to the characterization of 14 alkaloids while consuming plant material equivalent to 1.1 g. Of these, seven are N-oxides, four of which are new, namely, 9S,17S-pallidine Nalpha-oxide (6), 1S,2S-reticuline Nalpha-oxide (8), 6R,6aS-boldine Nbeta-oxide (9), and 6S,6aS-N-methyllaurotetanine Nalpha-oxide (13). Their structures were also confirmed by partial synthesis.