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Method for identifying ultra-high-temperature sterilized milk and reconstituted milk based on lipid group

A technology of ultra-high temperature sterilization and reconstituted milk, which is applied in the field of food inspection, can solve the problems of loss of nutritional value, complicated processing, and long time consumption, and achieve the effect of high accuracy, simple processing method and strong feasibility

Active Publication Date: 2019-05-28
INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The temperature used in the processing of UHT milk is 138-145°C, 2-5s, while the processing of milk powder needs to undergo UHT instantaneous sterilization and spray drying, so its nutritional value is greatly lost
The current methods for detecting reconstituted milk mainly focus on certain specific targets, such as furosine, lactulose, and heat-denatured proteins. These methods are not only complicated in pretreatment, time-consuming, but also prone to false positives

Method used

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  • Method for identifying ultra-high-temperature sterilized milk and reconstituted milk based on lipid group
  • Method for identifying ultra-high-temperature sterilized milk and reconstituted milk based on lipid group
  • Method for identifying ultra-high-temperature sterilized milk and reconstituted milk based on lipid group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1, the pretreatment of sample

[0042]10 brands of ultra-high temperature sterilized milk and 10 brands of whole milk powder were purchased from major supermarkets in Beijing. Take 0.2 mL of milk samples in glass centrifuge tubes, add 1 mL of water, vortex for 5 min; add 3 mL of CHCl 3 : MeOH (2:1, V / V), vortex for 10min; centrifuge at 2000rpm for 15min; take the lower layer solution and blow with nitrogen; 2 Cl 2 : MeOH (2:1, V / V) reconstitution, take 1mL in the injection vial, as a lipid sample for the next step of detection;

[0043] Each sample was taken in parallel 5 times.

Embodiment 2

[0044] The integral area analysis of each characterization factor in two kinds of milks of embodiment 2:

[0045] 1) Detection by high-resolution mass spectrometry:

[0046] The high-resolution mass spectrometer model used in the experiment is UPLC-Q-Exactive orbitrap massspectrometer (Thermo, CA), the chromatographic column model used in positive and negative ion modes is XSelect CSH C18column, and the temperature of the column oven is 45°C.

[0047] After the sample is subjected to lipid extraction pretreatment, the lipid sample is subjected to chromatographic separation-high-resolution mass spectrometry analysis, and the mass spectrometry includes MS and MS / MS; the mobile phase A and mobile phase B used in the positive and negative ion modes are respectively containing 10mM ammonium acetate Acetonitrile:water (6:4 volume ratio), isopropanol:acetonitrile (9:1 volume ratio) containing 10mM ammonium acetate, the elution gradient is as follows:

[0048] step

total...

Embodiment 3

[0064] Use high-resolution mass spectrometry to detect lipid samples of unknown milk samples, extract the characterization factors that distinguish the two milks in the two modes under the positive and negative ion modes, and integrate the peak areas of the lipids in Tables 1 and 2 respectively, and the integral values Use the model established in Example 2 for discrimination. Specifically according to Figure 5 and Figure 6 , falling in the black dot area on the left is UHT milk, and falling in the gray dot area on the right is reconstituted milk.

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Abstract

The invention provides a method for identifying ultra-high-temperature sterilized milk and reconstituted milk based on a lipid group, which comprises the following steps:1) performing lipid extractionpretreatment on an ultra-high-temperature sterilized milk sample and a reconstituted milk sample to obtain a lipid sample; 2) performing chromatographic separation-mass spectrometry scanning on the lipid sample of the ultra-high-temperature sterilized milk and the reconstituted milk by adopting a high-resolution mass spectrometry technology; 3) extracting and filtering peaks of lipid samples of two types of milk, carrying out qualitative analysis on each lipid component, and carrying out integral processing on each lipid component; 4) carrying out orthogonal partial least square variance discrimination analysis on an integral result, and determining a characterization factor capable of completely classifying the two types of milk; 5) establishing an orthogonal partial least square variance discrimination model by using the screened characterization factor. According to the method, the high-resolution mass spectrometer is adopted for measurement, the pretreatment method is simple and easy to operate, the types and the contents of substances in the two types of milk can be comprehensively analyzed, the on-line automatic detection of the sample is achieved, and the detection efficiency of the sample is greatly improved.

Description

technical field [0001] The invention belongs to the field of food inspection, and in particular relates to a detection and discrimination method for dairy products. Background technique [0002] Milk has a unique taste and rich nutritional value, and is widely loved by consumers. With the improvement of consumption level, the demand for milk continues to increase, resulting in insufficient supply of raw milk. In order to reduce costs, many companies use milk powder to blend reconstituted milk in the production process without labeling, which greatly reduces the nutrition of milk. value, seriously infringing on the legitimate rights and interests of consumers. The common commercially available liquid milk mainly includes ultra-high temperature sterilized milk and pasteurized milk, and the phenomenon of mixing milk powder into ultra-high temperature sterilized milk is particularly prominent. The temperature used in the processing of UHT milk is 138-145°C for 2-5s, while the ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86G01N30/88
Inventor 陈刚崔婧朱丹苏美丞谭冬飞贾曼
Owner INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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