High-brightness near-infrared fluorescent composite microsphere and preparation method thereof
A composite microsphere and near-infrared technology, applied in the field of fluorescent labeling, can solve the problems of low structural stability, poor uniformity of microspheres, weak fluorescence intensity, etc., and achieve the effects of improving labeling efficiency, less background interference, and low detection limit
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Embodiment 1
[0046] A kind of preferred concrete preparation process of embodiment 1 fluorescent composite microsphere of the present invention
[0047] The synthetic process of indocyanine green dye Cypate used below is as references: Ye, Y.; Bloch, S.; Kao, J.; Achilefu, S., Multivalent Carbocyanine Molecular Probes: Synthesis and Applications.Bioconjugate Chemistry 2005,16 ), 51-61. The steps are recorded in, and its UV and fluorescence properties are as follows Figure 4 shown;
[0048] Synthesis of dye silica precursor: weigh 4mg (0.0064mmol) of Cypate dye and dissolve it in 1mL DMF, add 2.5mg (0.013mmol) of EDC·HCl and 1.5mg (0.013mmol) of NHS, and react in the dark for 3 to 6 hours , and then add 1.8 μL or 0.0064 mmol of APTES to continue the reaction for 12 hours to obtain the dye silica precursor solution Cypate-APTES;
[0049] Synthesis of dye silica microspheres: Take 50mL absolute ethanol, add 4mL5 ammonia water and 1mL water, stir for 30min, add 250μL of the above-mentioned ...
Embodiment 2
[0055] Embodiment 2 changes the feeding amount of ammonia water to control microsphere size
[0056]Set up 4 comparison groups, each group in the synthesis step of dye silica microspheres, set different ammonia water feeding amount, the added ammonia water (25%~28%wt.) dosage is respectively 2mL (concentration 0.5M), 3mL (0.7M) and 4mL (0.9M), the rest of the operations were obtained under the same conditions as in Example 1 to obtain different sizes of dye silica microspheres Cypate@SiO 2 powder;
[0057] Such as Figure 8 Shown is the size control diagram of the dye silica microspheres obtained under different ammonia feeding conditions.
Embodiment 3
[0058] Embodiment 3 changes the synthesis time to achieve the adjustable emission of quantum dots
[0059] Set up 5 comparison groups, each group is in the synthesis step of CdTe / CdS quantum dots, the specific operation is as follows: Weigh 90mg of NaBH 4 (about 2mmol) dissolved in 2mL of distilled water, quickly degassed under nitrogen for 0.5h, the whole process was carried out under ice bath, quickly added 127mg (1mmol) of tellurium powder, continued to react for 0.5h, sealed the ep tube and placed it in 4 ℃ refrigerator, the solution slowly turns into a transparent purple solution, which is NaHTe solution. Take 366.6mg (2mmol) CdCl 2 Dissolve in 100mL of distilled water, add 314μL (3.6mmol) of 3-mercaptopropionic acid, add 2M NaOH solution dropwise, adjust the pH to alkaline, then quickly add the prepared anaerobic NaHTe into the above solution, stir well . Finally, transfer 10mL of the mixed precursor solution to a stainless steel autoclave lined with polytetrafluoroet...
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