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Detection method of plasticizer phthalate based on surface enhanced raman spectroscopy

A phthalate ester and surface-enhanced Raman technology, which is applied in Raman scattering, measurement devices, and material analysis through optical means, can solve the difficulties in realizing low-concentration rapid detection and making high-activity Raman substrates , complex and large instruments, etc., to achieve the effect of short detection time, high reproducibility, and simple enrichment method

Inactive Publication Date: 2019-01-04
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for the detection of plasticizer phthalates based on surface-enhanced Raman spectroscopy, and realize the detection of phthalates with the double enrichment strategy of host-guest identification and coffee ring effect and distinction, a simple and convenient production of active Raman substrates is proposed, which solves the difficulties in the production of highly active Raman substrates, the long preparation period in the conventional methods for detecting phthalates, the high cost and complicated Large-scale instruments, it is difficult to achieve low-concentration rapid detection and other existing detection problems

Method used

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  • Detection method of plasticizer phthalate based on surface enhanced raman spectroscopy
  • Detection method of plasticizer phthalate based on surface enhanced raman spectroscopy
  • Detection method of plasticizer phthalate based on surface enhanced raman spectroscopy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Step 1: Preparation of Raman-enhanced active material Au@Ag@β-CD nanosol

[0041] Add 0.4g β-CD into 40mL deionized water, heat it under magnetic stirring to dissolve it, when the temperature rises to 100°C, add 0.4mL HAuCl to the above solution 4 (10 mM) in water. After 2min, add 0.2mL NaOH (1.0M), react for 20min, the color of the solution turns pink, and obtain Au nano sol; then add 0.1mL AgNO to the sol 3 (10mM), reacted for 30min, the color of the sol turned reddish yellow, and the final product was obtained.

[0042] Step 2: Preparation of Raman-enhanced substrate by depositing self-assembled Au@Ag@β-CD nanoparticles using the coffee ring effect

[0043] Soak the silicon wafer in 50% piranha solution for 4 hours, take it out, rinse it with distilled water, dry it with a hair dryer, and then put it in a slide box for use. Take 5 μL of different types 1ⅹ10 -5 Put the standard samples of M phthalates (DMP, DEP, DPRP, DPP, DHP, DNP) into a 1ml centrifuge tube, add ...

Embodiment 2

[0047] Step 1: Preparation of Raman-enhanced active material Au@Ag@β-CD nanosol

[0048] Add 0.4g β-CD into 40mL deionized water, heat it under magnetic stirring to dissolve it, when the temperature rises to 100°C, add 0.4mL HAuCl to the above solution 4 (10 mM) in water. After 2min, add 0.2mL NaOH (1.0M), react for 20min, the color of the solution turns pink, and obtain Au nano sol; then add 0.4mL AgNO to the sol 3 (10mM), reacted for 30min, the color of the sol turned reddish yellow, and the final product was obtained.

[0049] Step 2: Preparation of Raman-enhanced substrate by depositing self-assembled Au@Ag@β-CD nanoparticles using the coffee ring effect

[0050] Soak the slides in 80% piranha solution for 4 hours, take them out, rinse them with distilled water, dry them with a hair dryer, and put them in slide boxes for later use. Take 5 μL of the same species with different concentrations (1ⅹ10 -5 M, 1ⅹ10 -6 M,1ⅹ10 -7 M,1ⅹ10 -8 M,1ⅹ10 -9 M,1ⅹ10 -10 M), take stand...

Embodiment 3

[0054] Step 1: Preparation of Raman-enhanced active material Au@Ag@β-CD nanosol

[0055] Add 0.4g β-CD into 40mL deionized water, heat it under magnetic stirring to dissolve it, when the temperature rises to 100°C, add 0.4mL HAuCl to the above solution 4 (10 mM) in water. After 2min, add 0.2mL NaOH (1.0M), react for 20min, the color of the solution turns pink, and obtain Au nano sol; then add 0.1mL AgNO to the sol 3 (10mM), reacted for 30min, the color of the sol turned reddish yellow, and the final product was obtained.

[0056] Step 2: Preparation of Raman-enhanced substrate by depositing self-assembled Au@Ag@β-CD nanoparticles using the coffee ring effect

[0057] Soak the silicon wafer in 100% piranha solution for 4 hours, take it out, rinse it with distilled water, dry it with a hair dryer, and then put it in a slide box for use. Take 5 μL rhodamine 6G (1ⅹ10 -5 M, 1ⅹ10 -6 M,1ⅹ10 -7 M,1ⅹ10 -8 M,1ⅹ10 -9 M,1ⅹ10 -10 M, 1ⅹ10 -11 M,1ⅹ10 -12 M) Put the standard sample ...

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Abstract

The invention discloses a detection method of a plasticizer phthalate based on the surface enhanced raman spectroscopy. According to the method, an Au@Ag@beta-CD material is used and mixed with to-be-detected substances, the mixture is dripped on a silicon wafer or a glass slide to form coffee-ring deposits, and a substrate with a good surface-enhanced raman effect is obtained. The coffee-ring effect can gather and concentrate the to-be-detected substances, the surface of the Au@Ag@beta-CD material is modified by cyclodextrin with a cavity structure, the to-be-detected substance can be adsorbed, the large number of to-be-detected substances can be gathered on the surface of the Au@Ag@beta-CD material, the secondary enrichment effect is generated, and the enrichment not only improves the concentration of the to-be-detected substances on the surface of the material, but also effectively distinguishes the to-be-detected substances from other substances in a solution. After enrichment, a strong raman signal is generated under the substrate, and phthalate can be qualitatively analyzed. The invention provides a method which can simply and rapidly detect phthalate (PAEs) and has low cost,high sensitivity and stable result, and the method can successfully achieve the rapid detection of PAEs in life.

Description

technical field [0001] The invention belongs to the technical field of environmental analysis and detection, and in particular relates to a method for detecting plasticizer phthalate by combining coffee ring effect and Raman spectrum technology. Background technique [0002] Surface-enhanced Raman spectroscopy (SERS) has attracted increasing attention in various fields due to its advantages such as high signal-to-noise ratio, molecular specificity, no photobleaching, and the use of single-wavelength excitation. These features make SERS one of the techniques for noninvasive, online and in vivo analysis of biological and chemical substances. However, the application of surface-enhanced Raman spectroscopy in the determination of trace analytes requires complex and expensive techniques to prepare substrates with high SERS activity and has low sensitivity to trace substances in complex matrices due to the interference of a large number of background signal molecules. and selecti...

Claims

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Application Information

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IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 施国跃张京飞张宇杨苗张闽朱安伟
Owner EAST CHINA NORMAL UNIV
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