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Method and device of ultrafast detection of antibiotic substances by combined voltage driven solid phase microextraction-raman spectroscopy

A voltage-driven, detection method technology, applied in the field of analytical chemistry, can solve the problems that affect the efficiency and results of the detection results, the inability to detect antibiotics, and the inability to enrich a large amount of analytes, so as to achieve stable and reliable Raman signals and save samples Pretreatment process, the effect of low density

Active Publication Date: 2019-01-08
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The current active substrate (extraction probe) is mostly a metal wire with a certain thickness of coating on the surface. Most of the coating on the active substrate is coated on the outer surface of the metal wire by soaking or polymerizing. The probe contains impurities, impurity, and uneven distribution, which leads to the inability to enrich a large amount of analytes, which affects the efficiency and results of the detection results. In addition, due to the variety of organic substances in the water body, the existing solid-phase microextraction and surface-enhanced Raman spectroscopy technology It can realize the analysis and detection of environmental organic pollutants, but cannot carry out special detection of antibiotic substances
Furthermore, the existing direct solid-phase microextraction combined with surface-enhanced Raman spectroscopy utilizes free diffusion to enrich the analyte. The free diffusion enrichment method often takes several hours and is time-consuming, which is not conducive to on-site in-situ extraction. Monitoring and Testing

Method used

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  • Method and device of ultrafast detection of antibiotic substances by combined voltage driven solid phase microextraction-raman spectroscopy
  • Method and device of ultrafast detection of antibiotic substances by combined voltage driven solid phase microextraction-raman spectroscopy
  • Method and device of ultrafast detection of antibiotic substances by combined voltage driven solid phase microextraction-raman spectroscopy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Preparation of porous silver wire wrapped with gold nanoparticles:

[0057] a. Preparation of porous silver wire: select a silver wire with a diameter of 0.4 mm and cut it into a uniform length of 1.5 cm, ultrasonically clean it with acetone and ethanol for 5 min, and then use ultrapure water for 10 min to cycle 3 times, and clean the silver wire The wire is used as the working electrode, the saturated calomel electrode is used as the reference electrode, and the platinum electrode is used as the counter electrode to form a three-electrode system, placed in a 0.1mol / L hydrochloric acid solution prepared by ultrapure water and concentrated hydrochloric acid, using cyclic voltammetry scanning mode, the voltage range -0.2V---0.2V, sweep speed 25mV / s, cycle 15 times, clean the prepared porous silver wire with ultra-pure water for 5 minutes, and then use it for later use.

[0058] b. Preparation of gold nanoparticle-wrapped porous silver wire: prepare 0.1mol / L KNO with ultra...

Embodiment 2

[0061] A voltage-driven solid-phase microextraction-Raman spectroscopy method for ultra-fast detection of antibiotic substances, the steps are as follows:

[0062] 1) A gold nanoparticle-wrapped porous silver wire is used as the working electrode, a saturated calomel electrode is used as the reference electrode, and a platinum electrode is used as the counter electrode to form an electrode system. The electrode system is placed in the water sample to be tested, and -0.1V is applied to the electrode Voltage, under the drive of voltage, the antibiotic substances in the water sample are quickly enriched to the working electrode for 40s, realizing in situ solid phase microextraction;

[0063] 3) Take out the extraction wire of the working electrode after enrichment and use a 785nm portable Raman spectrometer for detection, the laser intensity is 300mW, and the integration time is 1s to obtain a Raman spectrum.

experiment example 1

[0065] respectively to simulate 10 -5 mol / L malachite green MG water sample and 10 -5 The mol / L nitrofurazone NH water sample is the test solution, which is adjusted by hydrochloric acid solution and sodium hydroxide solution for 10 -5 mol / L malachite green MG water sample and 10 -5 The pH value of mol / L nitrofurazone NH water sample, utilizes the method for embodiment 2 to detect, and the influence of water sample pH value environment on detection sees Figure 11 , Figure 12 shown, from Figure 11 It can be seen that the 10 -5 mol / L malachite green solution had the strongest detection signal at pH 4.5, from Figure 12 It can be seen that the 10 -5 The detection signal of mol / L nitrofurazone NH water sample was the strongest when the pH value was 5.0.

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Abstract

The invention relates to a method of ultrafast detection of antibiotic substances by combined voltage driven solid phase microextraction-raman spectroscopy. The method comprises the following steps: taking a nano golden particle wrapped porous silver wire as a working electrode, a saturated calomel electrode as a reference electrode and a platinum electrode as a counter electrode to form an electrode system, putting the electrode system in a water sample to be detected, applying -0.05 to -0.2V voltage to the electrodes, quickly enriching the antibiotic substances in the water sample onto the working electrode due to voltage driving to achieve in-situ solid phase microextraction, and performing exciting irradiation on the surface of the working electrode through a raman spectrometer for raman spectroscopy. The method increases a diffusion rate of the substances to be detected in the water sample; the nano golden particle wrapped porous silver wire is specific to the antibiotic substances, so that the antibiotic substances are enriched onto the working electrode directionally selectively; the enrichment detection speed is greatly increased; and actual applications in quick field detection and water sample pollutant surveillance are achieved.

Description

technical field [0001] The invention relates to a method and device for ultra-fast detection of antibiotic substances by voltage-driven solid-phase microextraction-Raman spectroscopy, and belongs to the technical field of analytical chemistry. Background technique [0002] With the improvement of the health level and the continuous clinical application of new drugs, people are more and more dependent on antibiotics. Regardless of the type or quantity of antibiotics, they are increasing year by year. In actual use, antibiotics in humans or animals Only part of it can be metabolized, and 10-90% of antibiotics cannot be metabolized, but are excreted in the form of parent structure through urine or feces. Therefore, the extensive use of antibiotics inevitably leads to their entry into the environment through multiple routes. More and more studies have found that antibiotics in the environment have certain toxicity to environmental organisms, and antibiotics in the environment h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65G01N1/34
CPCG01N1/34G01N21/658
Inventor 占金华关琪张晓丽
Owner SHANDONG UNIV
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