Laser Raman spectroscopy method for quickly analyzing content of melamine in milk powder

A technology of laser Raman spectroscopy and melamine, which is applied in the field of detection, can solve the problems of low recovery rate of melamine, cumbersome pretreatment steps, failure to meet the detection requirements, etc., achieve accurate and rapid qualitative and quantitative analysis, reduce detection interference, and simple steps Effect

Inactive Publication Date: 2011-06-08
河北省食品质量监督检验研究院
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  • Application Information

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Problems solved by technology

Among them, the Chinese patent with the application number 200810225085.8 "Raman spectroscopy and kit for on-site rapid detection of melamine in liquid milk" uses Raman spectroscopy to detect melamine, which is easy to operate, sensitive and accurate, and has good reproducibility. but only for liquid milk
For mil...

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  • Laser Raman spectroscopy method for quickly analyzing content of melamine in milk powder
  • Laser Raman spectroscopy method for quickly analyzing content of melamine in milk powder

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Experimental program
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Effect test

Embodiment 1

[0020] ① Accurately weigh 1.00g of a certain brand of milk powder, add 3.00mL of acetonitrile to shake and extract for 5min, and ultrasonically extract for 5min; Mix well; centrifuge at 8000r / min for 1min; accurately measure 0.50mL of supernatant, add 0.50mL of n-hexane, shake vigorously for 1min, and the lower layer of supernatant is the solution to be tested; carry out blank test and sample spike test at the same time, the sample The added standard amount is 2mg / kg.

[0021] ② Add 0.50mL gold nano-sol, 0.050mL solution to be tested and 0.10mL sodium chloride solution with a mass concentration of 1% in sequence in the detection cell, shake well, put the detection cell in the detection chamber of the laser Raman spectrometer, and ~1700cm -1 Scan the Raman spectrum within the range to obtain the Raman spectrum; set the instrument parameters as follows:

[0022] a) Laser power: 200mW

[0023] b) Integration time: 20sec

[0024] c) Average times: 3

[0025] d) Smoothing para...

Embodiment 2

[0041] ① Accurately weigh 2.00g of another milk powder of a certain brand, add 5.00mL of acetonitrile to shake and extract for 5min, and ultrasonically extract for 5min; after standing for 1min, accurately measure 2mL of the supernatant, and add 2% acetic acid to the supernatant Mix zinc 0.10mL; centrifuge at 8000r / min for 1min; accurately measure 1.00mL of supernatant, add 1.00mL of n-hexane, shake vigorously for 1min, and the lower layer is the solution to be tested; carry out blank test and standard addition test at the same time , the amount added to the sample is 2mg / kg;

[0042] ②Add 0.50mL of silver nano-sol, 0.050mL of the solution to be tested and 0.10mL of potassium chloride solution with a mass concentration of 1% in sequence in the detection cell, shake well, and place the detection cell in the detection chamber of the laser Raman spectrometer. ~1700cm -1 Raman spectrum scanning is carried out within the range to obtain a Raman spectrogram, and the instrument para...

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Abstract

The invention discloses a laser Raman spectroscopy method for quickly analyzing the content of melamine in milk powder, which is carried out according to the following steps of: (1) weighing 1.0 to 2.0g of milk powder, adding 3 to 5ml of acetonitrile, oscillating, ultrasonically processing and standing, then accurately weighing supernatant, adding a protein precipitation agent to the supernatant, evenly mixing and centrifuging the mixture, accurately weighing the supernatant once more, adding n-hexane, oscillating the mixture, and obtaining subnatant which is used as the solution to be detected; (2) successively adding a surface strengthening reagent, the solution to be detected and an inorganic salt flocculant to a detection pond, evenly shaking the mixture, putting the detection pond in a laser Raman spectrograph detection room, and carrying out Raman spectrum scan in 400 to 1700 cm<-1> range to obtain a Raman spectrogram; (3) carrying out qualitative judgment; and (4) carrying out quantitative calculation. The pretreatment procedure of the measurement method of the invention is simple and quick, the recovery rate of the melamine is high, the technical problem that the treatment method of the milk powder in the prior art is not suitable for Raman spectroscopy detection is overcome, and the method is the important supplement of the traditional detection technology.

Description

technical field [0001] The invention relates to a detection method, in particular to a laser Raman spectrum detection method for quickly analyzing the content of melamine in milk powder. Background technique [0002] The melamine milk powder incident in 2008 once again sounded the alarm on food safety. Mixing melamine in raw milk can increase the nitrogen content of raw milk. In the determination of the protein content of dairy products in my country, the Kjeldahl method is still used to determine the protein content through the nitrogen content in dairy products. This gives criminals an opportunity to increase the nitrogen content of raw milk by adding nitrogen-containing cheap industrial raw materials, so that the test results show the illusion of falsely high protein content. Long-term intake of melamine can cause reproductive and urinary system damage, leading to bladder and kidney stones. [0003] Although the state approved the release of the national standard of "Ra...

Claims

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Application Information

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IPC IPC(8): G01N21/65
Inventor 李挥张敬轩张岩张会军李强李国俊刘春伟
Owner 河北省食品质量监督检验研究院
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