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A method for detecting edible oil oxidation products by proton nuclear magnetic resonance spectroscopy combined with gas chromatography external standard method

A technology of nuclear magnetic resonance proton spectrum and gas chromatography, which is applied in the direction of nuclear magnetic resonance analysis, measuring devices, instruments, etc., can solve problems such as interference of calculation formulas and unreliable calculation results

Active Publication Date: 2020-04-14
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, only the existing hydrogen nuclear magnetic resonance spectrum is used to detect the oxidation products of edible oil. Due to the generation of a large number of interfering substances, the calculation formula is seriously disturbed, resulting in unreliable calculation results.

Method used

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  • A method for detecting edible oil oxidation products by proton nuclear magnetic resonance spectroscopy combined with gas chromatography external standard method
  • A method for detecting edible oil oxidation products by proton nuclear magnetic resonance spectroscopy combined with gas chromatography external standard method
  • A method for detecting edible oil oxidation products by proton nuclear magnetic resonance spectroscopy combined with gas chromatography external standard method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0113] Draw the standard curve of oxidation products: prepare purified edible oil; add pure linolenic acid, linoleic acid, and oleic acid to purified edible oil, prepare standard samples with different gradients, and detect standard samples by gas chromatography and nuclear magnetic resonance methods, according to the experimental results Calculate the response signal A of the methylene group of the corrected glyceryl group H Add epoxy, alcohols and aldehydes pure products to purified edible oil, prepare different gradient standard samples, measure the response signals of epoxy, alcohols and aldehydes with NMR method, and correct the obtained ones in the previous stage After the A H Put the values ​​into the formula to obtain the corrected NMR response signals of epoxy, alcohols and aldehydes; take the corrected material NMR response signal as the vertical axis, and take the absolute concentration of epoxy, alcohols and aldehydes as the horizontal axis coordinates, draw the N...

Embodiment 2

[0119] According to the formula, the content of each oxidation product was calculated, as shown in Table 2. figure 1 for figure 1 It is a detection flowchart of the method of the present invention. figure 2 For the impact of the present invention before and after the improvement on drawing a standard curve. image 3 It is the hydrogen nuclear magnetic resonance spectrum of soybean oil and the information collection diagram corresponding to A, B, C, D, E, F, G, H, I, J, K, L, M, N, I peaks. Figure 4 It is a comparison chart of four H-NMR spectra of soybean oil after heating.

[0120] Oxidation product content in the edible oil calculated in table 2

[0121]

[0122]

[0123] Table 3 Summary of the average deviation (%) between the test results and the true value

[0124]

[0125] The present invention utilizes the composition of fatty acids detected by gas chromatography to correct the NMR signal of glyceryl methylene, and combines the standard curve drawn with p...

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Abstract

The invention discloses a method for detecting oxidation products of edible oil by combining a nuclear magnetic resonance hydrogen spectrum with a gas chromatography external standard method. The method comprises the steps of drawing a standard curve of the oxidation products: preparing purified edible oil, and calculating to obtain a corrected response signal AH of methylene of glyceryl; measuring response signals of epoxy, alcohols and aldehydes by using a nuclear magnetic resonance method so as to obtain corrected nuclear magnetic resonance response signals of the epoxy, the alcohols and the aldehydes; drawing nuclear magnetic resonance detection standard curves of the epoxy, the alcohol and the aldehyde substances; detecting a sample to be tested; determining the absolute concentrationof the oxidation products. The method uses the purified edible oil as substrate, thus eliminating matrix interference; the sample consumption is minimal, and only 100mu L of the sample is needed at most; the absolute contents of the eleven oxidation products can be simultaneously measured in one sample injection; the method is high in accuracy and rapid in the test speed, and the absolute quantification of the epoxy, the aldehydes and ketones in the edible oil is realized.

Description

technical field [0001] The invention belongs to the technical field of food detection methods, and in particular relates to a method for detecting edible oil oxidation products by proton nuclear magnetic resonance spectrum combined with gas chromatography external standard method. Background technique [0002] Fat and fat-containing food are important sources of nutrition and energy for human beings. The oxidative rancidity of fat not only causes the food to lose its original flavor, but also causes a serious loss of beneficial fatty acids and micronutrients, and the accompanying specific oxidation products may even endanger human health. . Indicators to characterize edible oil oxidation products include fatty acid composition, epoxides, alcohols, aldehydes, etc. Among them, epoxides, alcohols, and aldehydes need to be detected by gas chromatography-mass spectrometry, which consumes a large amount of organic solvents. Preprocessing is time-consuming and cumbersome. Therefo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N24/08G01N30/02
CPCG01N24/08G01N30/02
Inventor 刘睿杰李徐常明金青哲王兴国孟令璐郭伟唐天培薛晓凡张帆
Owner JIANGNAN UNIV
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