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A method for identifying adulteration of waste oil in refined vegetable oil

A technology for refining vegetable oil and waste oil, which is applied in the direction of analysis using electron paramagnetic resonance, can solve the problem of low sensitivity, and achieves the effect of simple technology, easy operation and high sensitivity

Active Publication Date: 2018-04-06
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has the disadvantage of low sensitivity. Therefore, a new method with high efficiency and high sensitivity is needed to replace the traditional low-field NMR method.

Method used

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  • A method for identifying adulteration of waste oil in refined vegetable oil
  • A method for identifying adulteration of waste oil in refined vegetable oil
  • A method for identifying adulteration of waste oil in refined vegetable oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Ditch oil decolorization: Ditch oil is collected from old frying oil in fast food restaurants, added with 5% activated clay, heated to 100°C, rotated slowly under vacuum for 30 minutes, and then centrifuged at 5000r / min for 10 minutes, and the supernatant is taken.

[0030] Configure PBN solution: Weigh a certain amount of PBN sample and dissolve it in toluene deoxygenated by nitrogen to make the concentration 150mM.

[0031] ESR detection: Put 100 μL of decolorized refined vegetable oil and 20 μL of 150 mM PBN solution in a nuclear magnetic tube by vortexing and dissolving, and then perform ESR detection. ESR detection adopts Bruker EMXplus-10 / 12, and the temperature of the detector is controlled to 140℃ through temperature control software. The ESR detection conditions are: center field strength: 3360G; sweep width: 100G; resolution: 1024 points; microwave power: 20mW; modulation Amplitude: 1.0G; modulation power: 100kHz; time constant: 20.48ms.

[0032] Spectrum analysis: ...

Embodiment 2

[0034] Waste oil after decolorization 1 (Chinese fast food restaurant-fried dough sticks) The same refined bulk soybean oil as adulterated ratios of 1%, 2%, 5%, 8%, 10%, 20%, 50% and 80% for sample preparation, accurately measure 100μL to be ready The test sample and 20 μL of 150 mM PBN toluene solution were placed in a 4mm NMR tube and vortexed, and ESR was detected at 140°C. Then, the adulteration of waste oil was qualitatively analyzed by spectrum analysis. The detection conditions and spectrum analysis method were the same as in Example 1. The result is image 3 As shown, adulterated soybean oil with an adulteration ratio of 1 to 80% can measure the adulteration ratio of waste oil.

Embodiment 3

[0036] Waste oil after decolorization 1 (Chinese fast food restaurant-fried dough sticks) The same as refined bulk soybean oil according to the adulteration ratio of 1%, 2%, 5%, 8%, 10%, 20% for sample preparation, the adulteration ratio of 1%, 2%, 5 %, 8%, 10%, 20% of the samples were measured and analyzed, and a standard curve was drawn between the intensity of the free radical peak and the adulteration ratio. The results showed ( Figure 4 ), the standard curve has good linearity, R 2 = 0.9657. Then measure all the samples obtained. The specific steps are: accurately measure 100μL of the sample to be tested and 20μL of 150mM PBN toluene solution, place them in a 4mm NMR tube, vortex, and perform free radical detection at 140°C according to ESR instrument conditions, and then The adulteration of waste oil was quantified by spectral analysis, and the detection conditions and spectral analysis method were the same as in Example 1. Among them, the samples with adulteration ratio...

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Abstract

The invention discloses a method for identifying adulterating gutter in refined vegetable oil and belongs to the technical field of food detection. The method includes: using fried used oil and refined mass vegetable oil, using PBN (polybutylene naphthalate) as a spinning trap, detecting changes in free radical strength before and after refined vegetable oil is adulterated by using Bruker electron spin resonance (ESR) spectrometer, and quantitating the ratio of adulterating gutter in the vegetable oil by using spectrum fitting method; the method is high in sensitivity and easy to perform and enables the adulterated vegetable oil with less than 20% of adulterating ratio to be accurately identified and the adulterating ratio to be precisely quantitated.

Description

Technical field [0001] The invention aims to identify adulterated refined vegetable oils in waste oil, and specifically adopts an ESR spin capture method, which belongs to the field of food engineering. Background technique [0002] Used and severely oxidized oil is called waste oil. Refined vegetable oil undergoes frying or cooking. Under high temperature and long time heating, the unsaturated fatty acids in the oil are prone to oxidation, and oxidation, polymerization and hydrolysis reactions will occur. These reactions will generate a series of substances with greater polarity than triglycerides, such as extremely Polymeric lipids, triglyceride oxides, oxyglycerides, fatty acids, etc. These substances have oxygen-containing groups such as carboxyl groups, aldehyde groups, and hydroxyl groups, which cause the quality of grease to decrease, such as increased viscosity, darker color, and transmission Heat drop, etc., will cause harm to human health after eating. [0003] The repr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N24/10
CPCG01N24/10
Inventor 刘元法陈洪建李进伟曹培让
Owner JIANGNAN UNIV