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A method for detecting benzoic acid in milk based on surface-enhanced Raman spectroscopy

A technology of surface-enhanced Raman and spectroscopy, which is applied in Raman scattering, measurement devices, and material analysis by optical means, to achieve the effects of enhancing Raman signals, improving detection capabilities, and enhancing grasping.

Active Publication Date: 2022-08-02
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the field of benzoic acid detection, some scholars proposed to use SERS technology to detect benzoic acid in aqueous solution (beverage). There are few detection reports, and the sensitivity and detection limit need to be further optimized and improved

Method used

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  • A method for detecting benzoic acid in milk based on surface-enhanced Raman spectroscopy
  • A method for detecting benzoic acid in milk based on surface-enhanced Raman spectroscopy
  • A method for detecting benzoic acid in milk based on surface-enhanced Raman spectroscopy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1A

[0050] Example 1 Preparation of Ag-COF substrate

[0051] The preparation method of Ag-COF substrate comprises the following steps:

[0052] 1,3,5-tris(4-aminophenyl)benzene (TPB, 0.04mmol) and 2,5-divinylterephthalaldehyde (DVA, 0.06mmol) were added to a 10mL test tube, followed by 5mL of acetonitrile, Ultrasonic for 1 min to completely dissolve the solid; after that, add 12 mol / L 0.7 mL of acetic acid to the test tube; then shake for 10 s, let stand at room temperature for 72 h, and centrifuge to collect the yellow precipitate, which is then washed three times with tetrahydrofuran (THF) and ethanol, respectively. ; Finally, it was dried under vacuum at 60 °C for 24 h to obtain COF material.

[0053] Mix 50 mL of silver nitrate solution with a concentration of 100 mg / L and 2.5 mg of COF material evenly, and incubate at 100 °C for 30 min; then add 0.25 mL of 1% sodium citrate aqueous solution, and conduct reduction reaction at 100 °C for 40 min. An Ag-COF substrate (solution...

Embodiment 2

[0054] Example 2 Construction of standard curve

[0055] (1) Prepare the sample solution:

[0056] Take the benzoic acid solution of 1000mg / L as the mother solution, and take the solutions of the mother solution diluted to 40, 80, 120, 160, 200, 400, 800mg / L as the standard solution;

[0057] Using the Ag-COF substrate of Example 1, whole milk, and the standard solution according to the volume ratio of 10:1:1, vortexed for 2 minutes to obtain concentrations of 2, 4, 6, 8, 10, 20, 40, and 60, respectively. , 80, 100, 150, 200 mg / L sample solution;

[0058] (2) Carry out Raman detection:

[0059] According to the volume ratio of acetonitrile and the sample solution 1:1, the centrifugation pretreatment was carried out (centrifugation speed was 8000rpm, and the centrifugation time was 10min). Raman detection was carried out under the condition of 50% laser power, and Raman spectrum was obtained;

[0060] (3) Construct the standard curve:

[0061] A standard curve was construc...

Embodiment 3

[0065] The influence of embodiment 3 reaction time on the detection of benzoic acid

[0066] Adjust the time of vortex oscillation in the step (1) of Example 2 to be 1-10min to obtain a 100 mg / L sample solution of benzoic acid concentration; carry out Raman detection according to the step (2) of Example 2, and the detection results are as follows:

[0067] image 3 Be the Raman characteristic peak of benzoic acid in embodiment 3 (1003cm -1 ) intensity versus reaction time line graph, starting from image 3 It can be seen that after the reaction time of 2 minutes, the Raman intensity changes gradually, and the fluorescence intensity is basically unchanged within 2-10 minutes of the reaction time, so the reaction time is selected to be 2 minutes for measurement.

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Abstract

The invention discloses a method for detecting benzoic acid in milk based on surface-enhanced Raman spectroscopy technology, and belongs to the field of analysis and detection. The method of the present invention comprises the following steps: (1) mixing and heating the silver nitrate solution and the COF material for incubation, and adding sodium citrate solution for reduction after the incubation to obtain an Ag-COF substrate; (2) mixing the milk to be tested Mix evenly with the Ag-COF substrate to obtain the sample solution to be tested; (3) mix the sample solution to be tested and acetonitrile evenly, and centrifuge to obtain the pretreated sample solution to be tested; (4) mix the pretreated sample solution to be tested The sample solution is subjected to Raman detection to obtain a Raman spectrum; the characteristic peak in the Raman spectrum is 1003 cm ‑1 ±5cm ‑1 The peak intensity at is brought into the standard curve model to obtain the concentration of benzoic acid in the milk to be tested. The Ag-COF substrate in the present invention can be used as a Raman enhanced substrate to detect benzoic acid in milk, the detection time is within 5 minutes, and the detection limit is as low as 0.1 mg / L.

Description

technical field [0001] The invention relates to a method for detecting benzoic acid in milk based on surface-enhanced Raman spectroscopy technology, and belongs to the field of analysis and detection. Background technique [0002] Benzoic acid is widely used in the sterilization and preservation of food and beverages. Although benzoic acid can be added to food at a much higher concentration than other additives, the abuse of benzoic acid can still cause symptoms such as asthma and stomach, and even reduce the normal metabolism of the human body. Countries such as China, New Zealand and the United States have promulgated standards for the addition of benzoic acid in food. Therefore, a sensitive and reliable benzoic acid detection method is needed in the food industry. [0003] At present, the main methods for the detection of benzoic acid in milk are: chromatography, high performance liquid chromatography, and enzyme-linked immunosorbent assay. These methods have high prec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 陈国庆杨子晨吴亚敏马超群李磊朱纯辜姣高辉
Owner JIANGNAN UNIV
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