Water-soluble β-cyclodextrin (β-CD)-modified carbon nanocrystals (CNCs) have been synthesized by the reaction of CNCs with mono(6-diethylenetriamino-6-deoxy)-β-CD (DETA-β-CD) and comprehensively characterized by 1 H NMR, FT-IR, transmission electron microscopy (TEM) and UV-Vis. DETA-β-CD-modified CNCs (DETA-β-CD-CNCs) are luminescent, and the quantum yield is 8.41%. The photoinduced electron transfer (PET) process between DETA-β-CD-CNCs and (ferrocenylmethyl) trimethylammonium iodide (Fc + ) was investigated by means of fluorescence spectroscopy. carbon nanocrystals, β-cyclodextrin, supramolecular chemistry, fluorescence Citation: Jiang Q, Zhang H Y, Liu Y. Synthesis of β-cyclodextrin-modified carbon nanocrystals and their fluorescent behavior. Fluorescent carbon nanocrystals (CNCs) [1-14] are quantum-sized carbon analogues used as biomarkers, bioimaging and bioprobes. CNCs are carbon-based nanomaterials, comparable to fullerenes, carbon nanotubes, graphite and nanodiamonds, which possess fluorescent properties. They are monodispersed in aqueous solution with a scale of 2-10 nm and have high photostability fluorescence. Compared with such semiconductor nanocrystals as CdSe [15], CdTe [16], and CdSe/ZnSe [17], CNCs have lower toxicity to human health or to the environment. As a result, CNCs may be suitable for various applications in chemistry and biology.Cyclodextrins (CDs) are a class of cyclic oligosaccharides with generally 6-8 D-glucose units linked by α-1,4-glucose bonds. They have the ability to selectively bind various inorganic or organic guests, which leads to widespread applications of CDs not only in pharmaceutical chemistry, food technology, analytical chemistry, chemical synthesis, and catalysis [18][19][20][21][22][23][24][25], but also for constructing molecular devices and machines [26][27][28][29][30][31]. Therefore, the combination of CNCs with CDs might yield valuable future applications. Here, we *Corresponding author (email: yuliu@nankai.edu.cn) prepared mono(6-diethylenetriamino-6-deoxy)-β-cyclodextrin (DETA-β-CD) modified CNCs (DETA-β-CD-CNCs), which have been characterized by 1 H NMR, FT-IR, transmission electron microscopy (TEM) and UV-Vis, and investigated the photoinduced electron transfer (PET) process between DETA-β-CD-CNCs and (ferrocenylmethyl) trimethylammonium iodide (Fc + ) by means of fluorescence. Importantly, 1-adamantanecarboxylic acid sodium salt (Ad -) could modulate the PET process between CNCs with Fc + .