In summary, a novel sample preparation method is demonstrated for routine users to improve sensitivity and reduce deuterated solvents, which together brings down the running cost of NMR and applicable in a conventional set-up. This sample preparation methodology has the potential to improve the study of a small quantity of natural product and a small quantity of samples in a synthesis lab using 5 mm o.d. regular NMR tube. Similar triple layers for other deuterated solvents and proton NMR spectroscopy is on progress.