Benzene derivatives are seriously harmful to environment and human health, and sensitively detecting these compounds is of great significance but is a challenge. Hence, we designed and synthesized two luminescent lanthanide-organic frameworks, [{Ln(SIP)(H2O)4}]n, [Ln = Tb (1), Eu (2)], with high solvent and pH stability, which can be used as luminescent probes to detect toluene and benzaldehyde among various reagents, and the detection limit can reach up to 10-7 mol L-1 for toluene, and 10-6 mol L-1 for benzaldehyde. Regenerated experimental results indicate that both 1 and 2 can be used for at least five cycles with high precision. To the best of our knowledge, this is the first example of the two-dimensional regenerable luminescent sensor for toluene and benzaldehyde through luminescent quenching.