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Nuclear magnetic resonance spectroscopy method for identifying ultrahigh-temperature sterilized milk and reconstituted milk

A technology of nuclear magnetic resonance spectroscopy and ultra-high temperature sterilization, which is applied in the fields of nuclear magnetic resonance analysis, material analysis through resonance, and measuring devices, which can solve the problems of loss of nutritional value, complicated processing, and long time consumption, and achieve high accuracy , Improve the detection efficiency, the effect of strong feasibility

Active Publication Date: 2019-02-22
INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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  • 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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  • Nuclear magnetic resonance spectroscopy method for identifying ultrahigh-temperature sterilized milk and reconstituted milk
  • Nuclear magnetic resonance spectroscopy method for identifying ultrahigh-temperature sterilized milk and reconstituted milk
  • Nuclear magnetic resonance spectroscopy method for identifying ultrahigh-temperature sterilized milk and reconstituted milk

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1, the pretreatment of sample

[0033] 10 brands of UHT milk and 10 brands of whole milk powder (milk powder) were purchased from major supermarkets in Beijing.

[0034] The preparation method of the reconstituted milk is as follows: according to the protein content of 3.0g per 100mL of milk, the milk powder is added to the ultrapure water, and then the temperature is kept in a water bath to 40°C, and the reconstituted milk is homogenized by hand to obtain a milk sample of the reconstituted milk.

[0035] Take 2 mL each of the above ultra-high temperature sterilized milk and reconstituted milk, and centrifuge at 8000 rpm for 30 min; separate the lower layer solution, take 1 mL, add 2 mL of acetonitrile, and vortex for 5 min; then centrifuge at 10000 rpm for 10 min, separate the upper layer solution, and take 2 mL for nitrogen blowing . With 1mL containing 3mmol / L TSP D 2 O was redissolved, and 600 μL was taken in an NMR tube for the next step of detection. ...

Embodiment 2

[0036] The integral area analysis of each characterization factor in two kinds of milks of embodiment 2:

[0037] Get a pair of milk sample prepared in embodiment 1, utilize nuclear magnetic resonance technology to detect:

[0038] The model of nuclear magnetic resonance instrument used in the experiment is Bruker Advance Ⅲ 400MHz, and the detection temperature is 298K. 1H NMR nuclear magnetic resonance technology was used to detect and analyze the samples, and the detection parameters were set as follows:

[0039] Number of data points, 64K; spectral width, 8223.7Hz; relaxation time, 2s; number of scans, 8; acquisition time, 4s. For the spectra obtained, see Figure 4 and Figure 5 .

[0040] II. The relative integral of the peak area of ​​each characteristic factor in different types of milk:

[0041] Phase adjustment and baseline correction of the spectra were performed using the NMR spectrum analysis software Topspin version 2.1. Using 3mM TSP as the internal standar...

Embodiment 3

[0054] Utilize nuclear magnetic resonance spectrometer to detect unknown milk sample, detection parameter is the same as embodiment 2.

[0055] The peak areas at δ=4.30, 4.56, 2.41, 1.93, and 4.59ppm were integrated relative to each other, and the integral value was judged by this model. If the relative integral value of the peak area of ​​the unknown milk sample falls within the numerical range of the reconstituted milk, the unknown milk sample is determined to be reconstituted milk; if the relative integral value of the area falls outside the numerical range of the reconstituted milk, The unknown milk sample is determined to be UHT milk.

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Abstract

The invention provides a nuclear magnetic resonance spectroscopy method for identifying ultrahigh-temperature sterilized milk and reconstituted milk. The nuclear magnetic resonance spectroscopy methodcomprises the steps: 1) respectively detecting milk samples of the reconstituted milk and the ultrahigh-temperature sterilized milk prepared from whole milk powder by using a nuclear magnetic resonance spectroscopy, and integrating peak area at each chemical shift position; 2) analyzing a principal component of a relative integral result, establishing a partial least square variance analysis model, and determining a characterization factor capable of completely classifying the two milks; and 3) establishing a partial least square variance discriminant analysis model for identifying the ultrahigh-temperature sterilized milk and the reconstituted milk based on the determined characterization factor. By using the method provided by the invention, a nuclear magnetic resonance spectrometer isadopted for measurement, a pretreatment method is simple and easy to operate, the kinds and contents of substances in the two milks can be comprehensively analyzed, the online automatic detection forthe samples is realized, and the sample detection efficiency is greatly increased. An identifying model established by using the nuclear magnetic resonance spectroscopy method is strong in feasibilityand high in accuracy and provides a convenient and practical technical support for the identification of truth of milk products in the future.

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] Liquid milk is deeply loved by consumers because of its unique taste and rich nutritional value. With the improvement of consumption level, the demand for liquid milk continues to increase, resulting in insufficient supply of cow milk and goat milk as raw materials. In order to reduce costs, many companies use milk powder to blend reconstituted milk in the production process without labeling, which is extremely Dadi has reduced the nutritional value of body milk and seriously violated 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 u...

Claims

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Application Information

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IPC IPC(8): G01N24/08
CPCG01N24/08G01N24/082
Inventor 陈刚崔婧朱丹苏美丞谭冬飞
Owner INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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