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Two-photon fluorescent bio-silk material and preparation method thereof

A two-photon fluorescence and biofilament technology, which is applied in the direction of luminescent materials, rayon manufacturing, chemical instruments and methods, etc., can solve the problems of large photodamage, achieve stable interaction, improve detection depth and sensitivity, and good mechanical properties Effect

Inactive Publication Date: 2011-05-18
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, the excitation light source of existing single-photon fluorescent silk protein materials is short-wavelength ultraviolet light, etc., and the photodamage is large.

Method used

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  • Two-photon fluorescent bio-silk material and preparation method thereof
  • Two-photon fluorescent bio-silk material and preparation method thereof
  • Two-photon fluorescent bio-silk material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Two-photon Fluorescent Molecules Containing Nitrofluorene Derivatives Synthesized

[0041]

[0042] The silk comes from Liangguang No. 2 silkworm variety. Contains soap for silk raw silk (10g·L -1 ) and sodium carbonate (5g·L -1 ) solution at 85°C for 45 minutes, then washed and degummed with distilled water, and dried naturally. Due to the strong polarity of the nitro groups at both ends of the molecule, they can form hydrogen bonds with the carbonyl groups on the protein molecular chain. At 60-110° C., 1 g of silk fiber / fabric and 0.04 g of the above-mentioned two-photon fluorescent organic molecule are sealed and stirred in 20 mL of dimethyl sulfoxide (DMSO) solution for 30-100 minutes. Take out the silk, wash it with distilled water ultrasonic wave, and dry it to obtain two-photon fluorescent silk.

[0043] By z-scan method, we got 2,7-dinitrostyryl-9,9'-dibutylfluorene and 2,7-dinitrostyryl-9,9'-dioctyl The two-photon absorption cross sections of fluorene a...

Embodiment 2

[0046] Silkworm cocoons from Liangguang No. 2 silkworm variety were used, and the cocoons were cut into pieces and treated with 0.05% (w / v) NaHCO 3 The solution was washed at 100°C for 50 minutes to remove sericin, then washed several times with deionized water, and dried naturally. Dissolve the obtained dried silk fibers in 9.3 mol / L LiBr solution at 40° C., and then precipitate LiBr in distilled water by dialysis to obtain a silk protein solution. The concentration of silk protein was determined to be ~4.0 wt.% by weighing method.

[0047] Add 0.5mL containing 0.5mg 2,7-dibromo-9,9-dibutylfluorene or 2,7-dinitrostyryl-9,9'-dioctylfluorene dimethyl to the above silk protein solution base sulfoxide (DMSO) solution, mixed evenly to obtain a yellow transparent fluorescent silk protein solution. At room temperature, two-photon fluorescent silk protein gel was obtained after 10-100 h ( Image 6 ).

[0048] Take 1mL of the above-mentioned yellow transparent two-photon fluoresce...

Embodiment 3

[0051] Under the protection of nitrogen atmosphere, 1 g of silk fiber / fabric, Rhodamine B (2.0 mmol, 958 mg) and a catalytic amount of DMAP were dissolved in dry anhydrous DMSO (25 mL), and cooled in an ice-water bath at 0 °C. A solution of DCC (2.2 mmol, 454 mg) in dichloromethane (5 mL) was added dropwise into the above solution with stirring. Gradually raise the reaction temperature to room temperature and stir the reaction for 6-10 h. The silk was taken out, washed with dichloromethane and distilled water ultrasonically, and dried to obtain single-photon fluorescent silk. The reaction formula is as follows:

[0052]

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Abstract

The invention relates to a two-photon fluorescent bio-silk material and a preparation method thereof. The material is prepared by evenly compounding a two-photon organic fluorescent substance and a bio-silk protein material, wherein the mass ratio of the two-photon organic fluorescent substance to the bio-silk protein material is (0.001-50):100; the excitation wavelength of the two-photon fluorescent bio-silk material is in near-infrared, and the fluorescence wavelength of the same is shorter than the excitation wavelength. The preparation method of the two-photon fluorescent bio-silk material comprises the following steps of: adding pretreated silk into a dimethyl sulfoxide solution containing the two-photon organic fluorescent substance at 20-110 DEG C, stirring, washing and drying to obtain the finished product; or adding a silk protein solution to the dimethyl sulfoxide solution containing the two-photon organic fluorescent substance, stirring to obtain a mixed solution, and drying, standing or spinning to obtain the finished product. The two-photon fluorescent bio-silk material has stronger two-photon absorption performance and adjustable two-photon fluorescence performance under near-infrared laser irradiation; an excitation light source has photobiologically transparent wavelength and has no damages to biological tissues; and the two-photon fluorescent bio-silk material has favorable biocompatibility, strong mechanical property, easiness of preparation and good economic benefit and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of two-photon fluorescent biological silk material and its preparation, in particular to a two-photon fluorescent biological silk material and its preparation method. Background technique [0002] Biofilament is a biological fiber formed from biodegradable polymers. There are many kinds of biological silk, and the most studied ones include spider silk and silkworm silk. Spider silk is unmatched by other synthetic fibers, its specific modulus is better than steel, and its toughness is better than Kevlar fiber. As an excellent energy-absorbing fiber, spider silk is considered to be an ideal material for parachutes and body armor, and has broad application prospects in the fields of textiles, biotechnology, medical care, fine chemicals, and military materials. People have been studying spider silk for more than a century, and the research content involves gene identification, expression, structure and performance, bion...

Claims

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Application Information

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IPC IPC(8): C08L89/00C08K5/32C08K5/03D01F4/02D01F1/10D06M13/392D06M13/08C09K11/06C08J5/18C08J9/28C08J3/075D01D5/00D06M101/12
Inventor 刘向阳徐洪耀林乃波
Owner DONGHUA UNIV
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