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Method for quickly detecting azlocillin sodium in milk by surface enhanced Raman spectroscopy

A surface-enhanced Raman and azlocillin sodium technology, which is applied in the detection field of penicillin antibiotics, can solve the problems of cumbersome processing, complicated operation, and high cost, and achieve the effects of simple pretreatment, high sensitivity, and small sample volume

Pending Publication Date: 2021-01-05
武夷学院
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the methods for detecting the residues of penicillin antibiotics in milk mainly include high performance liquid chromatography, gas chromatography, microbial detection, immunoassay and other methods. These detection methods have high accuracy and good sensitivity, but the operation is relatively complicated. Sample pretreatment is cumbersome, time-consuming and costly

Method used

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  • Method for quickly detecting azlocillin sodium in milk by surface enhanced Raman spectroscopy
  • Method for quickly detecting azlocillin sodium in milk by surface enhanced Raman spectroscopy
  • Method for quickly detecting azlocillin sodium in milk by surface enhanced Raman spectroscopy

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Effect test

Embodiment 1

[0038] This embodiment shows the preparation and concentration method of nano-gold sol,

[0039] First remove 1 mL of 1% HAuCl 4 Put the solution in a 250mL round bottom flask, add 99mL of purified water to get 0.01% HAuCl 4 solution. Place the round bottom flask in an electric heating mantle for heating, wait until the moment of boiling, quickly remove the condenser tube, add 1mL of 1% Na 3 C 6 h 5 o 7 Then continue to heat it. After 25 minutes, stop heating. Cool to room temperature, put in a brown glass bottle, and place in the refrigerator to refrigerate.

[0040] Take 1.5 mL of the above self-made gold colloid solution in a 1.5 mL centrifuge tube, centrifuge for 10 min in a small centrifuge, remove the supernatant to obtain 20 μL of concentrated gold colloid.

[0041] It should be noted that the nano-gold sol used in the present invention can also be prepared by other methods, or can be directly purchased commercially.

Embodiment 2

[0043] The present embodiment demonstrates the method for detecting unknown milk samples, comprising the following steps:

[0044] (1) Sample pretreatment: Use a pipette gun to pipette 40mL of Jindian milk into a 50mL centrifuge tube, place it in a centrifuge at 3000r / min, and centrifuge at 20°C for 10min, then pipette the fat floating on the upper layer The gun sucks away slowly, being careful not to waste the milk. Take another 25mL of fat-free Jindian milk, heat it to 40°C, add 1mL of acetic acid (1:9), and stir. Centrifuge again at 3000r / min, 20°C for 10min. Take 2 mL of the supernatant to pass through a solid-phase microextraction column (Envi-carb), add 1 mL of pure water to elute, and take 200 μL of the eluate for detection.

[0045] (2) Standard solution preparation: Accurately weigh 2 mg of azlocillin sodium standard powder, add 2 mL of pure water, mix well to obtain a 1 mg / mL (1000 mg / L) azlocillin sodium standard solution, take 1 mL of 1000 mg / L Azlocillin sodium...

Embodiment 3

[0048] The present embodiment adopts the detection method in embodiment 2, detects and analyzes the azlocillin sodium standard solution of different concentrations, and the results are shown in figure 1 ,From figure 1 It can be seen that at 1150, 1383, 1530cm -1 Sharp and obvious characteristic peaks appear nearby, and as the concentration of azlocillin sodium standard increases, the SERS signal gradually increases, so 1150, 1383, 1530cm -1 Nearby peaks can be used as characteristic peaks for qualitative identification of azlocillin sodium.

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Abstract

The invention relates to a method for quickly detecting azlocillin sodium in milk by surface enhanced Raman spectroscopy, which comprises the following steps of pretreating a sample to obtain an eluent, thereby obtaining a pretreated milk sample, preparing standard solutions, namely weighing azlocillin sodium standard substances, adding water, uniformly mixing to obtain azlocillin sodium standardsolutions, and respectively preparing azlocillin sodium standard solutions with different concentrations for later use, raman detection: respectively adding the pretreated milk sample and azlocillin sodium standard solutions with different concentrations in the previous step into nanogold sol, uniformly mixing, adding an aqueous solution of sodium chloride, uniformly mixing, and carrying out Ramanspectrum detection, and finally, conducting linear fitting. The method disclosed by the invention has the advantages of high sensitivity, short time, strong specificity, no damage, small required sample amount, simple pretreatment and the like, is suitable for detecting azlocillin sodium in milk, and has a relatively good application prospect.

Description

technical field [0001] The invention relates to a method for detecting penicillin antibiotics, in particular to a method for rapidly detecting azlocillin sodium in milk by surface-enhanced Raman spectroscopy. Background technique [0002] Penicillin antibiotics are the most common in the current application, it can effectively prevent and treat animal diseases, most enterprises because antibiotics can play a significant role in the prevention of animal diseases. For example, azlocillin sodium (Azlocillin Sodium) is a third-generation broad-spectrum semi-synthetic penicillin, which has a strong preventive and therapeutic effect on infections caused by Gram-positive bacteria, Gram-negative bacteria and anaerobic bacteria. Due to improper handling and management problems, there may be residues of azlocillin sodium in milk after cows have been treated with azlocillin sodium. [0003] At present, the methods for detecting the residues of penicillin antibiotics in milk mainly inc...

Claims

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Application Information

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IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 马春华郭志勇
Owner 武夷学院
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