Vanillin (4-hydroxy-3-methoxybenzaldehyde) is one of the most widely used food spices. Aimed at bio-vanillin green production, the natural materials were directly catalytically oxidized efficiently in one pot under low O2 pressure (0.035 MPa) in the presence of a non-noble metal oxidation combined catalyst (NiCo2O4/SiO2 nanoparticles), which showed remarkable advantages of a short synthetic route and less industrial waste. The catalytic system showed good universality to many natural substrates with nearly 100% conversion and 86.3% bio-vanillin yield. More importantly, carbon isotope ratio investigations were employed to verify the origin of the organic matter. One hundred percent 14C content of the obtained vanillin was detected, which indicated that it was an efficient method to distinguish the vanillin from biomass or fossil materials. Furthermore, the 13C isotope examination showed effective distinguishing ability for the vanillin from a particular biomass source. The C isotope detection provides an effective method for commercial vanillin identification.
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