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Preparation method and application of micro-needle-shaped solid-phase surface-enhanced Raman substrate

A solid-phase surface and Raman substrate technology, applied in the field of analytical chemistry, can solve the problems of low sensitivity, poor qualitative analysis ability, poor stability, etc., and achieve the effects of high sensitivity, small target damage and small sample volume.

Active Publication Date: 2020-05-12
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

TLC is a classic separation and analysis method that has many advantages, but the detection method when it is used for qualitative identification is somewhat primitive, and has low sensitivity, poor stability, and poor qualitative analysis ability.

Method used

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  • Preparation method and application of micro-needle-shaped solid-phase surface-enhanced Raman substrate
  • Preparation method and application of micro-needle-shaped solid-phase surface-enhanced Raman substrate
  • Preparation method and application of micro-needle-shaped solid-phase surface-enhanced Raman substrate

Examples

Experimental program
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Effect test

Embodiment 1

[0040]A preparation method of a microneedle-shaped solid-phase surface-enhanced Raman substrate, comprising the following steps (see figure 1 ):

[0041] (1) Preparation of carbon fibers with pore structure and functional group modification

[0042] Select 10 carbon fibers with a length of 2 cm and a diameter of 5 μm, first ultrasonically clean them in 8M potassium hydroxide (KOH) solution for 4 hours, then ultrasonically clean them with 8M hydrochloric acid and water until neutral; Potassium oxide and water were ultrasonically cleaned to neutrality to obtain activated carbon fibers with a pore structure and functional group modification.

[0043] (2) Preparation of bonded body

[0044] Select a carbon fiber obtained in step (1) with a pore structure and functional group modification, and bond it to a silver wire with conductive glue, so that one end is a silver wire and the other end is a carbon fiber to obtain a bonded body.

[0045] (3) Preparation of conjugates

[0046...

Embodiment 2

[0058] A method for preparing a microneedle-shaped solid-phase surface-enhanced Raman substrate, comprising the following steps:

[0059] (1) Preparation of carbon fibers with pore structure and functional group modification

[0060] Select 10 carbon fibers with a length of 3 cm and a diameter of 10 μm, first ultrasonically clean them in 10M potassium hydroxide (KOH) solution for 6 hours, then ultrasonically clean them with 6M hydrochloric acid and water until neutral; Potassium oxide and water were ultrasonically cleaned to neutrality to obtain activated carbon fibers with a pore structure and functional group modification.

[0061] (2) Preparation of bonded body (same as Example 1).

[0062] (3) Preparation of conjugates

[0063] Then insert the bonded body obtained in step (2) into a glass tube with a length of 15 cm and an inner diameter of 1 mm, expose the silver wire end by 5 cm, and the carbon fiber end by 1 cm; The interface was sealed with paraffin paste in a 90°C ...

Embodiment 3

[0075] A method for preparing a microneedle-shaped solid-phase surface-enhanced Raman substrate, comprising the following steps:

[0076] (1) Preparation of carbon fibers with pore structure and functional group modification

[0077] Select 10 carbon fibers with a length of 3 cm and a diameter of 7 μm, and first ultrasonically clean them in 9M potassium hydroxide (KOH) solution for 5 hours, then ultrasonically clean them with 7M hydrochloric acid and water until neutral; Potassium oxide and water were ultrasonically cleaned to neutrality to obtain activated carbon fibers with a pore structure and functional group modification.

[0078] (2) Preparation of bonded body (same as Example 1).

[0079] (3) Preparation of conjugates

[0080] Then insert the bonded body obtained in step (2) into a glass tube with a length of 12cm and an inner diameter of 0.8mm, expose the silver wire end by 4cm, and the carbon fiber end by 8mm; The interface of the glass tube was sealed with paraffi...

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Abstract

The invention discloses a preparation method of a micro pinpoint-shaped solid-phase surface enhanced Raman substrate. The preparation method comprises the following steps of (1) preparing carbon fiberprovided with a hole structure and modified by a functional group, (2) preparing a bonding body, (3) preparing a combining body, (4) preparing an electrode and (5) preparing the micro pinpoint-shapedsolid-phase surface enhanced Raman substrate, wherein a to-be-detected object such as pesticide residues in food can be rapidly separated and analyzed when the micro pinpoint-shaped solid-phase surface enhanced Raman substrate and a thin-layer chromatography are combined in use. The preparation method is simple in preparation process and easy to implement; the prepared micro pinpoint-shaped solid-phase surface enhanced Raman substrate is of a pinpoint-shaped macrostructure and has an excellent Raman enhancement property, with a Raman scattering enhancement factor reaching 107; since the sizeis small, sampling is convenient and sampling modes are flexible, the damage to a target object is small, the usage amount of samples is low, and the sensitivity is high; the micro pinpoint-shaped solid-phase surface enhanced Raman substrate is easily placed in other equipment and coupled with other technologies like the thin-layer chromatography, and is used for is used for the target object in acomplex system.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a preparation method and application of a micro-needle-shaped solid-phase surface-enhanced Raman substrate; the application focuses on combining the micro-needle-shaped solid-phase surface-enhanced Raman substrate with thin-layer chromatography (TLC) for the separation and analysis of analytes in mixed systems. Background technique [0002] Surface enhanced Raman (Surface enhancement Raman scattering, referred to as SERS) is a new type of high-sensitivity spectroscopy technology derived on the basis of Raman spectroscopy. Plasmon resonance amplifies the Raman spectral signal. Among them, the surface-enhanced Raman substrate is the core of amplifying Raman spectral signals. Therefore, the preparation of surface-enhanced Raman substrates with high sensitivity, controllable morphology, convenient sampling, and recyclability has always been a hot spot in th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D3/48C25D5/54C25D7/06G01N21/65C25F1/04
CPCC25D3/48C25D5/54C25D7/0607C25F1/04G01N21/658
Inventor 康燕吴婷杜一平韩孝朕
Owner EAST CHINA UNIV OF SCI & TECH
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