Luminescent LaF 3 -Ce 3+ /Tb 3+ nanocrystals have been successfully prepared via a simple wet chemical technique. For the next bioapplication, these nanoparticles dispersed in cyclohexane have also been functionalized with poly(Stco-MAA), based on a designed oil-in-water microemulsion system. These polymer-coated nanospheres are water-soluble and bioconjugable. Unlike semiconductor quantum dots, the as-prepared lanthanum fluoride nanocrystals possess nonsize-dependent emissions and completely stable photocycles. With functionalized LaF 3 nanospheres as fluorescence probes, a fluorescence method was developed for the rapid quantitative analysis of DNA, due to the quenching effect of fluorescence by the DNA. Under optimum conditions, the fluorescence intensity was proportional to the concentration of the introduced DNA over the range 2.5-35 mg/mL for calf thymus DNA (ctDNA) and 2.5-30 mg/mL for fish sperm DNA (fsDNA), respectively.