CN114674908B

CN114674908B - Preparation method of electrochemical sensor for tigecycline detection

Info

Publication number: CN114674908B
Application number: CN202111410499.XA
Authority: CN
Inventors: 方建; 蒋成; 赵继华
Original assignee: Lanzhou University
Current assignee: Lanzhou University
Priority date: 2021-11-25
Filing date: 2021-11-25
Publication date: 2023-03-31
Anticipated expiration: 2041-11-25
Also published as: CN114674908A

Abstract

The invention discloses a preparation method of an electrochemical sensor for tigecycline detection, which comprises the following steps: s01, preprocessing GF; s02, preparing CeY-C submicron spheres; s03, ceYO _x Preparing; s04, ceYO _x The preparation of GF, in the S01, the pretreatment operation of GF comprises the following specific operations: s001, cutting the commercially available GF; s002, alternately washing GF by using ultrapure water and ethanol, removing GF surface residues, and vacuum-drying GF at 60 ℃ overnight; in S003, S002, the volume ratio of sulfuric acid: water =1:1, activating GF with the activation time of 1 h, wherein the specific operation steps comprise: s0001, 6 mL of a cerium nitrate solution (0.1 mol/L), 3 mL of an yttrium nitrate solution (0.2 mol/L), and 6 mL of a urea solution (0.5 mol/L) were added to 20 mL of a glucose solution (0.5 mol/L) by a peristaltic pump, and the mixture was stirred while being peristaltic. The preparation method of the electrochemical sensor for detecting tigecycline overcomes the defects of high cost, complex operation and long time consumption of the traditional detection method.

Description

Preparation method of electrochemical sensor for tigecycline detection

Technical Field

The invention belongs to the technical field of electrochemical sensors, and particularly relates to a preparation method of an electrochemical sensor for detecting tigecycline.

Background

Tigecycline (TGC) is a novel broad-spectrum active antibiotic for intravenous injection, is also active against methicillin-resistant staphylococcus aureus, and is the first drug of glycyltetracyclines. TGC has been officially approved by the FDA in the united states for the treatment of complex adult abdominal infections and complex skin and soft tissue infections, including complex appendicitis, burn infections, intra-abdominal abscesses, deep soft tissue infections, and ulcer infections.

At present, the TGC detection method mainly comprises ultraviolet spectrometry, fluorescence spectrometry, liquid chromatography-tandem mass spectrometry (LC-MS/MS), matrix assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS), reverse liquid chromatography (RP-LC), double-gradient high-performance liquid chromatography (DGLC), immunoassay and the like. The existing TGC detection method has high cost, complex operation and long time consumption, and the electrochemical method has simple operation and low cost, but the prior art does not disclose a case for detecting TGC by the electrochemical method.

Disclosure of Invention

The invention aims to provide a preparation method of an electrochemical sensor for tigecycline detection, so as to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of an electrochemical sensor for tigecycline detection comprises the following steps:

s01, preprocessing GF;

s02, preparing CeY-C submicron spheres;

S03，CeYO _x preparing;

S04，CeYO _x preparation of/GF.

Preferably, in S01, the preprocessing of GF specifically includes:

s001, cutting the commercially available GF;

s002, alternately washing GF by using ultrapure water and ethanol, and removing GF surface residues;

in S003, S002, the volume ratio of sulfuric acid: water =1:1 activates GF.

Preferably, in S02, the specific operation steps include:

s0001, respectively adding 6 mL of cerium nitrate solution (0.1 mol/L), 3 mL of yttrium nitrate solution (0.2 mol/L) and 6 mL of urea solution (0.5 mol/L) into 20 mL of glucose solution (0.5 mol/L) through a peristaltic pump, and stirring while peristaltic motion is performed;

after the mixed solution in S0002 and S0001 is stirred, the mixed solution is transferred into a 50 mL Teflon autoclave and heated to 160 ℃ at the speed of 5 ℃/min;

s0003, S0002, the temperature after reaction was cooled to room temperature and the samples were collected by centrifugation and washed several times with ultrapure water and ethanol.

Preferably, a proper amount of CeY-C submicron powder is placed in a porcelain boat and kept for 6 hours at 550 ℃ under air atmosphere.

Preferably, 1.6 mL of CeYO is measured in S04 _x An aqueous solution (0.6 mg/mL) was placed in a test tube, the activated GF was immersed and sonicated for 15 min, and the GF was removed and washed with ultrapure water.

The invention has the technical effects and advantages that: according to the preparation method of the electrochemical sensor for detecting tigecycline, the nano material with uniform appearance can be prepared by the method; the method is used for efficiently and rapidly detecting TGC by an electrochemical method for the first time, and overcomes the defects of high cost, complex operation and long time consumption of the conventional detection method;

CeYO prepared by the invention _x the/GF composite electrode not only can exert the respective advantages of the three components, but also enhances the conductivity, stability and electrochemical response of the composite material due to the synergistic effect of the components;

the composite electrode can detect the TGC under a neutral medium, and has the advantages of good detection sensitivity, circulation stability, anti-interference performance, high sample recovery rate and the like.

Drawings

FIG. 1 shows CeY-C submicrospheres and CeYO _x Morphology;

FIG. 2 is CeYO _x Potential optimization and quantification curves of the/GF electrode pair TGC detection;

FIG. 3 is CeYO _x Testing the anti-interference capability and the circulation stability of the TGC detection by the GF electrode;

FIG. 4 is CeYO _x Determination of TGC recovery in actual samples by/GF electrode.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.

Example 1

1. Pretreatment of commercially available GF

And S01, GF is cut, preferably GF produced by Gansu Hesho carbon fiber Co, and the thickness of the GF is 3 mm.

S02, washing the cut GF with ultrapure water to remove surface scum, and alternately washing the GF with ultrapure water and ethanol until no scum exists.

S03, putting cleaned GF into a reactor with the volume ratio of 200 mL to sulfuric acid: water =1:1 for 1 h and then washed with ultrapure water.

Preparation of CeY-C submicrospheres

Respectively adding 6 mL of cerium nitrate solution (0.1 mol/L), 3 mL of yttrium nitrate solution (0.2 mol/L) and 6 mL of urea solution (0.5 mol/L) into 20 mL of glucose solution (0.5 mol/L) through a peristaltic pump, and stirring while peristaltic motion is performed;

after stirring for 15 min, it was transferred to a 50 mL Teflon autoclave and heated to 160 ℃ at a rate of 5 ℃/min;

cooling to room temperature, centrifuging to collect a sample, washing with ultrapure water and ethanol for several times, and vacuum drying to obtain black CeY-C submicron sphere powder;

it is noted that the preferred manufacturer of the cerium nitrate solution is the chemical company of Synechococcus, the preferred manufacturer of the yttrium nitrate solution is the scientific company of Shanghai Aladdin, the preferred manufacturer of the urea solution is the science and technology development company of Tianjin, and the preferred manufacturer of the glucose solution is the chemical reagent factory of Synechococcus.

3.CeYO _x Preparation of

Placing proper amount of CeY-C submicron powder in a porcelain boat, keeping at 550 ℃ for 6h in air atmosphere, and cooling to obtain CeYO _x White powder.

4. CeYO _x Preparation of/GF

1.6 mL of CeYO was measured _x The activated GF was immersed in an aqueous solution (0.6 mg/mL) in a test tube, followed by ultrasonic treatment, and the GF was taken out and washed with ultrapure water.

Example 2

Preparation of GF electrodes

The commercially available GF is subjected to cutting, cleaning and activating treatment to obtain the GF electrode.

2.CeO ₂ Preparation of/GF electrodes

Compared with S02 of example 1, except that 3 mL of 0.2 mol/L Y (NO) was not used ₃ The procedure of example 1 was followed except for the solution.

3.Y ₂ O ₃ Preparation of/GF electrodes

Compared with S02 of example 1, except that 3 mL of 0.2 mol/L Ce (NO) was not used ₃ The procedure is as in example 1 except for the solution.

Example 3

Compared with S02 of example 1, except that Y (NO) ₃ The quantitative concentration of the substance of the solution becomes 0The procedure is as in example 1 except 01 mol/L.

Example 4

Compared with S02 of example 1, except that Ce (NO) ₃ The procedure of example 1 was repeated except that the quantitative concentration of the substance in the solution was changed to 0.01 mol/L.

Example 5

Compared with S04 of example 1, except that CeYO _x The procedure of example 1 was repeated except that the mass concentration of the aqueous solution was changed to 0.3 mg/mL.

Example 6

Compared with S04 of example 1, except that CeYO _x The procedure of example 1 was repeated except that the mass concentration of the aqueous solution was changed to 0.9 mg/mL.

Example 7

Compared with S04 of example 1, except that CeYO _x The procedure of example 1 was repeated except that the mass concentration of the aqueous solution was changed to 1.2 mg/mL.

The above embodiments of the present invention are verification of the effects of a preparation method of an electrochemical sensor for tigecycline detection, and can be referred to the following descriptions:

using Cyclic Voltammetry (CV) for GF and CeO ₂ /GF、Y ₂ O ₃ /GF、CeYO _x The electrochemical performance test of the/GF shows that the CeYO _x the/GF electrode has stronger current response signal, better electrochemical reversibility and cycling stability.

In order to optimize the preparation conditions of the composite electrode, an electrochemical performance test is carried out by using Cyclic Voltammetry (CV), and the result shows that: when taking 6 mL, 0.1 mol/L Ce (NO) ₃ Solution and 3 mL, 0.2 mol/L Y (NO) ₃ Solution, ceYO _x When the concentration of the aqueous solution is 0.6 mg/mL, the prepared electrode has better electrochemical performance.

Study of CeYO Using Cyclic Voltammetry (CV) _x The linear range, sensitivity and minimum detection limit of the/GF composite electrode for detecting TGC, wherein the optimized results are that the linear range is 0.16 mu M-10 mu M and 10 mu M-1000 mu M, the sensitivity is 2.81 mu A/mu M and 0.50 mu A/mu M, and the minimum detection limit is 0.022 mu M.

In summary, the invention is a preparation method of an electrochemical sensor for tigecycline detection, which has linear response ranges of 0.16 μ M to 10 μ M and 10 μ M to 1000 μ M to TGC, sensitivities of 2.81 μ A/μ M and 0.50 μ A/μ M, and a minimum detection limit of 0.022 μ M (S/N = 3).

The invention provides a preparation method of an electrochemical sensor for detecting tigecycline, which can realize high-efficiency detection of TGC and provides a feasible thought for TGC detection.

Claims

1. A preparation method of an electrochemical sensor for tigecycline detection is characterized by comprising the following steps:

s01, preprocessing GF;

s02, preparing CeY-C sub-microspheres;

s03, preparing CeYOx;

s04, preparing CeYOx/GF;

in S01, the specific operation of GF preprocessing includes:

s001, cutting the commercially available GF;

s002, washing GF alternately by using ultrapure water and ethanol, and removing residues on the surface of GF;

s003, using a volume ratio of sulfuric acid: water =1:1 activates the washed GF;

in S02, the specific operation steps comprise:

s0001, adding 6 mL of 0.1 mol/L cerium nitrate solution, 3 mL of 0.2 mol/L yttrium nitrate solution and 6 mL of 0.5 mol/L urea solution into 20 mL of 0.5 mol/L glucose solution through a peristaltic pump respectively, and stirring while peristaltic motion is performed;

s0003, cooling to room temperature, centrifuging to collect a sample, washing with ultrapure water and ethanol for several times, and then vacuum drying to obtain CeY-C submicron sphere black powder;

in S03, placing a proper amount of CeY-C submicron powder into a porcelain boat, keeping the porcelain boat at 550 ℃ for 6 hours in an air atmosphere, and cooling to obtain CeYOx white powder;

in S04, 1.6 mL of 0.6 mg/mL CeYOx aqueous solution was measured in a test tube, the activated GF was immersed in the solution and subjected to ultrasonic treatment, and the GF was taken out and washed with ultrapure water.