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Continuous-flow reactor–based synthesis of carbohydrate and dihydrolipoic acid–capped quantum dots

Abstract

A detailed protocol for the large-scale synthesis of carbohydrate and dihydrolipoic acid (DHLA)-coated CdSe/ZnS and CdTe/ZnS nanoparticles using continuous flow reactors is described here. Three continuous flow microreaction systems, operating at three different temperatures, are used for the synthesis of mannose-, galactose- or DHLA-functionalized quantum dots (QDs). In the first step of synthesis, the CdSe and CdTe nanoparticles are prepared. The size and spectral properties of the CdSe core of the nanoparticles are controlled by adjustment of the residence time and the temperature. As a second step, the zinc sulfide capping under homogenous conditions is carried out at a substantially lower temperature than is required for nanoparticle growth in batch processes. Finally, the trioctylphosphine/oleic acid ligand is effectively replaced with either carbohydrate PEG-thiol moieties or DHLA at 60 °C. This new protocol allows the synthesis of biologically active fluorescent QDs in 4 d.

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Figure 1: Scheme for the synthesis of mannose-SH (5) and Gal-SH (10) derivatives.
Figure 2
Figure 3: Schematic overview of continuous flow system used for QD synthesis.
Figure 4: Image of CdSe samples under an UV lamp.
Figure 5: Fluorescence spectra of CdSe QDs prepared at different times at 160 °C.
Figure 6: Fluorescence spectra of CdSe QDs prepared at different temperatures.
Figure 7: TEM image of CdSe QDs.
Figure 8: TEM images of nanoparticles.
Figure 9: Kinetics of turbidity.

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Acknowledgements

Generous funding from the Max Planck Society is gratefully acknowledged.

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Authors

Contributions

P.L. and R.K. carried out the experiments and designed the protocol. P.H.S. designed and supervised the project. P.L., R.K. and P.H.S. wrote the manuscript.

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Correspondence to Peter H Seeberger.

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Laurino, P., Kikkeri, R. & Seeberger, P. Continuous-flow reactor–based synthesis of carbohydrate and dihydrolipoic acid–capped quantum dots. Nat Protoc 6, 1209–1220 (2011). https://doi.org/10.1038/nprot.2011.357

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