An ultrasensitive method for detecting protein by synchronous fluorescence scan technique with a novel composite nanoclusters has been developed. The novel composite nanoclusters has been prepared by an in situ polymerization method and applied as a protein synchronous fluorescence probe. The surface of the composite nanoclusters was covered with functional groups (−COOH, −CONH−, −OH). These groups may have “synergistic effect” and play a major role in the ultrasensitive method. The nanoclusters are water-soluble, stable and biocompatible. The synchronous fluorescence intensity of the composite nanoclusters is significantly increased in the presence of trace protein at pH 1.09. Based on this, a new synchronous fluorescence scan (SFS) analysis was developed for the determination of proteins including BSA, HSA and human γ-IgG. The liner range is 0.03–2.0μgml−1 for HSA, 0.02–2.2μgml−1 for BSA and 0.02–1.5μgml−1 for human γ-IgG, respectively. Besides high sensitivity, the method is characterized by good reproducibility, excellent accuracy and few interfering substances.
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