Preparation method of surface-enhanced Raman scattering probe

A surface-enhanced Raman and probe technology, which is applied in the field of preparation of aggregated silver nanoprobes, can solve problems such as precipitation and unstable clusters, and achieve the effects of environmental friendliness, good repeatability, and low toxicity

Inactive Publication Date: 2010-04-14
SOUTHEAST UNIV
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  • Application Information

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Problems solved by technology

Aggregating metal nanoparticles can provide more "hot spots" to significantly increase the SERS intensity, however, exc

Method used

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  • Preparation method of surface-enhanced Raman scattering probe
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  • Preparation method of surface-enhanced Raman scattering probe

Examples

Experimental program
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Example Embodiment

[0017] Example 1 Probe preparation (taking rhodamine 6G probe as an example)

[0018] The first experiment uses the method reported by Lee and Meisel to prepare silver gel solution. 1.0×10 -2 The M silver nitrate solution was added to deionized water at a volume ratio of 1:10 to the silver glue solution, stirred and heated to boiling. Add 1% sodium citrate solution to the boiling silver nitrate solution in a volume ratio of 1:50 to the silver glue solution, continue to stir and heat to boil for 40 minutes to obtain the silver glue solution. The prepared silver glue solution is protected from light and sealed for future use.

[0019] In the second step, a 1mM rhodamine 6G aqueous solution was prepared, and the rhodamine 6G solution was added to the silver glue solution at a volume ratio of 1:1000-1:100 under magnetic stirring, and reacted for 5 minutes. Add 0.5M sodium chloride solution to the mixed solution of rhodamine 6G and silver glue solution according to the volume ratio of...

Example Embodiment

[0020] Example 2 Detection of chemical stability of probes (taking rhodamine 6G probe as an example)

[0021] The first step is to do a set of comparative experiments on the stability of the absorption spectrum. The first group is to prepare a 1mM rhodamine 6G aqueous solution. Take the rhodamine 6G solution under magnetic stirring and add it to the silver glue solution in a volume ratio of 1:500. React for 5 minutes. Then add 0.5M sodium chloride solution according to the volume ratio of 1:750 to the silver glue solution; in the second group, add 1% PVP aqueous solution with a molecular weight of 50,000 according to the volume ratio of 1:150 to the silver glue solution on the basis of the first group. Record the absorption spectra of the solutions of the first group and the second group over time. From the change in the intensity of the absorption spectrum, it can be known that if there is no PVP protection, such as Figure 3-1 After adding sodium chloride, the intensity of the...

Example Embodiment

[0023] Example 3 The SERS activity of the probe in living cells and the biocompatibility of the probe (SERS activity in living cells is taken as an example of 4-mercaptobenzoic acid probe, and the cell survival rate is taken as an example of rhodamine 6G probe) Put cervical cancer cells (Hela) in culture medium for in vitro culture (37℃, 5% CO 2 ). After 24 hours, add 4-mercaptobenzoic acid SERS probe solution (the preparation method is the same as that of rhodamine 6G probe solution) by volume ratio (3:1) into the cell culture medium, shake gently, and re-place it in the incubator Inside. The SERS probe enters the interior of the cell by being engulfed by the cell. After 1.5 hours, the medium was aspirated, and the cells were washed 3 times with phosphate buffered saline (PBS) to remove the SERS probe remaining in the medium that was not phagocytosed by the cells, and set aside.

[0024] In the second step, the cells washed with the buffer are placed on the stage of the confoc...

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Abstract

The invention provides a preparation method of a surface-enhanced Raman scattering probe, relating to a preparation method of a silver nano aggregation probe which has high surface-enhanced Raman scattering activity and is coated by polyvinylpyrrolidone, as well as applications thereof in regulation of aggregation degree of silver nano particles and SERS detection in cells. The method selects silver colloid solution as a raw material, selects sodium chloride as an aggregation agent, and coats the polyvinylpyrrolidone on the surface of silver aggregates; and specifically comprises the following steps: evenly mixing Raman markers and the silver colloid solution according to volume ratio of 1: 1000 to 1:100 under the stirring condition, then adding sodium chloride solution to aggregate the silver colloid solution mixed with the Raman markers into aggregates with two to five particles, finally adding the polyvinylpyrrolidone solution, continuously stirring for 5 to 15 minutes, filtering the obtained solution with a filter with the aperture specification of 100 to 220nm and then obtaining the surface-enhanced Raman scattering probe. The probe is water-soluble colloid solution.

Description

technical field [0001] The present invention relates to a preparation method of polyvinylpyrrolidone (Polyvinylpyrrolidone, PVP)-wrapped aggregated silver nanoprobe with high surface-enhanced Raman scattering (Surface enhanced Raman Scattering, SERS) activity, and its application to regulating the aggregation of silver nanoparticles Extent and detection of SERS in cells. More generally related to metallic nanomaterials, polymeric materials. Background technique [0002] In recent years, the detection of biological samples by designing optical probes with certain functions has been a research hotspot. Fluorescent probes are traditional optical probes. After a long period of development, fluorescent probes have been widely used. However, fluorescent probes have disadvantages such as narrow excitation spectrum, easy photobleaching of samples, and toxicity to biological samples when the concentration of fluorescent dye is too high. Compared with traditional fluorescence spect...

Claims

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Application Information

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IPC IPC(8): G01N21/65
Inventor 崔一平杨晶王著元谈学斌宋春元张若虎
Owner SOUTHEAST UNIV
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