Preparation method and product of mulberry silk capable of fluorescing under irradiation of near-infrared light

A near-infrared light, mulberry silk technology, applied in chemical instruments and methods, luminescent materials, molding or processing of animal feed, etc., can solve imaging, detection application difficulties, low fluorescence specificity, weak excitation light penetration, etc. problems, to achieve the effect of a wide range of applications, high biosafety, and stable properties

Active Publication Date: 2019-10-25
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] In order to overcome the defects of low fluorescence specificity, weak excitation light penetration, and difficult imaging and detection applications in the existing technology for preparing fluorescent silk, the present invention provides a preparation method for preparing mulberry silk that is excited by near-infrared light and fluoresces. This method can not only improve fluorescent silk fibers with high fluorescence intensity, strong penetrating power and good biocompatibility, but also is suitable for mass production and has no pollution to the environment

Method used

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  • Preparation method and product of mulberry silk capable of fluorescing under irradiation of near-infrared light
  • Preparation method and product of mulberry silk capable of fluorescing under irradiation of near-infrared light

Examples

Experimental program
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Embodiment 1

[0041] (1) Prepare green fluorescent core-shell structure upconversion nanoparticles (β-NaYF4:Yb,Er@β-NaYF4) by hydrothermal method, with a diameter of about 50nm, and graft the surface with polyacrylic acid (PAA) after modification Legumin, as a raw material for food addition, is synthesized as follows:

[0042] The core-shell upconversion nanoparticles (β-NaYF 4 :Yb,Er@β-NaYF 4 ), which were dispersed in n-hexane solution. The surface of nanoparticles was grafted with polyacrylic acid (PAA) by ligand exchange method. 1 mL of upconversion nanoparticles solution was blended with 5 mL of dimethylformamide (DMF), and then 4 mL of n-hexane was added and stirred for 3 hours. Add 5-10 mL of isopropanol to precipitate and wash with DMF several times. Resuspend the precipitate in PAA / DMF solution with a PAA concentration of 10mg / mL (5-10mL), stir overnight and wash by centrifugation. Take 10mg of PAA-modified nanoparticles and disperse them in 1mL of aqueous solution, add 1mg of ...

Embodiment 2

[0049] (1) Upconversion nanoparticles (NaYF 4 : 1% Er, 1% Tm), with a diameter of about 60nm, the surface is modified with polyacrylic acid and grafted with concanavalin as a raw material for food addition. The synthesis method is as follows:

[0050] Red fluorescent upconversion nanoparticles (NaYF 4 : 1% Er, 1% Tm), which was dispersed in n-hexane solution. The surface of nanoparticles was grafted with polyacrylic acid (PAA) by ligand exchange method. 1 mL of upconverting nanoparticles solution was mixed with 5 mL of dimethylformamide (DMF), and then 4 mL of n-hexane was added and stirred for 3 hours. Add 5-10 mL of isopropanol to precipitate and wash with DMF several times. Resuspend the precipitate in PAA / DMF solution with a PAA concentration of 10mg / mL (5-10mL), stir overnight and wash by centrifugation. Take 10mg of PAA-modified nanoparticles and disperse them in 1mL of aqueous solution, add 1mg of EDC and NHS respectively, stir and react for 3-6h, then 30uL of concan...

Embodiment 3

[0056] (1) Prepare green fluorescent core-shell structure upconversion nanoparticles (NaGdF4:Yb / Er@NaGdF4:Yb / Nd) by hydrothermal method, with a diameter of about 50nm, and graft concanavalin after surface polyacrylic acid modification , as a raw material for adding food;

[0057] (2) disperse the up-conversion nanoparticles synthesized in step (1) with water, and prepare a dispersion solution whose concentration is 5g / L;

[0058] (3) Pick mature mulberry leaves, soak them in the nanoparticle solution in step (2), soak them for 5 minutes, remove them, and let them dry naturally.

[0059] (4) On the third day of the 5th instar silkworm, feed the silkworm the treated mulberry leaves in step (3) until it spins silk and cocoons.

[0060] (5) After the silkworm spins and cocoons, silkworm cocoons are taken for silk reeling to obtain green fluorescent mulberry silk excited by near-infrared light, and the fluorescence intensity is higher.

[0061] The mulberry silk prepared in embod...

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Abstract

The invention discloses a preparation method of mulberry silk capable of fluorescing under irradiation of near-infrared light, including the steps of (1), preparing upconversion nanoparticles, performing surface modification with concanavalin to obtain modified upconversion nanoparticles; (2), uniformly dispersing the upconversion nanoparticles in water to prepare aqueous solution of upconversionnanoparticles; (3), picking mature mulberry leaves, soaking the mulberry leaves in the aqueous solution of upconversion nanoparticles, draining water and then drying in air naturally; (4), feeding silkworms the processed mulberry leaves until the silkworms spin and make cocoons when the silkworms grow to the designed stage; (5), collecting silk so as to obtain the mulberry silk capable of fluorescing under irradiation of near-infrared light. According to the preparation method, the upconversion nanoparticles applied to preparation is capable of fluorescing under irradiation of near-infrared light having higher penetrating power, and accordingly has better application in imaging of deep tissue. Besides, the upconversion nanoparticles have much stable property, higher bio-security, higher signal to noise ratio and wider application range.

Description

technical field [0001] The invention belongs to the field of silk fiber production and processing, and in particular relates to a method for preparing mulberry silk that fluoresces under near-infrared light. Background technique [0002] Silk cellulose has the reputation of "fiber queen". It has excellent mechanical properties, and the formed fabric is smooth, bright in color, and has good air permeability and heat insulation. Therefore, silk fiber has played an important role in the course of my country's economic development. However, with the rapid development of man-made fiber industrial synthesis technology, the traditional sericulture textile industry is facing severe challenges. In recent years, research on the modification of natural silk has received more and more attention. Researchers have introduced or modified functional macromolecules into silk fibers by different means to improve the performance of silk fibers and enhance their application value. At present,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A01K67/04A23K50/90A23K20/105A23K20/147C09K11/02C09K11/85
CPCA01K67/04A23K50/90A23K20/105A23K20/147C09K11/025C09K11/7773A23K10/30A23K20/22A23K40/00B82Y5/00B82Y30/00C09K11/02B82Y99/00C09K11/7766
Inventor 杨明英王捷陈玉银张颖
Owner ZHEJIANG UNIV
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