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Method for detecting content of 3-monochloropropanol-1, 2-diol ester in edible oil

A technology of propylene glycol ester and propylene glycol palmitate diester is applied in the field of detecting the content of 3-chloro-1,2-propylene glycol ester in edible oil, and can solve the problems of polluting a gas chromatography-mass spectrometer, complicated processing steps, affecting analysis efficiency and the like, Achieve the effect of avoiding instrument maintenance, low instrument contamination, and avoiding cross-contamination

Active Publication Date: 2014-12-24
INST OF AGRO FOOD SCI & TECH CHINESE ACADEMY OF AGRI SCI
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  • Abstract
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Problems solved by technology

[0003] 3-Chloro-1,2-propylene glycol ester (3-MCPD ester) is the esterification product of 3-chloropropanol and fatty acid. It is another potential hazard factor introduced in the oil refining process. In 1983, Spain first refined aniline with hydrochloric acid. 3-MCPD ester was detected in rapeseed oil, but it has not been taken seriously for more than 20 years
(For the evaluation of the above acid and base catalyzed indirect methods, see the discussion of Zhang Rui et al. in "Research Progress in the Determination of 3-Chloro-1,2-Propanediol Esters in Edible Oils", which was published in "Journal of China Cereals and Oils" in December 2012 Volume 27, No. 12, 122-127), the current international acid-catalyzed transesterification pretreatment steps are very cumbersome, and the transesterification time is as long as 16 hours, which seriously affects the analysis efficiency
[0012] Therefore, it is necessary to provide a method that overcomes the problems of low analytical efficiency, low sensitivity, and contamination of the gas spectrometer in the prior art, and on the basis of ensuring the authenticity of the method.

Method used

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  • Method for detecting content of 3-monochloropropanol-1, 2-diol ester in edible oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] 1. Sample pretreatment

[0061] Weigh 0.100g of homogenized peanut oil into a centrifuge tube with a cover, heat slightly at 40°C to dissolve the fat completely, add 1mL THF solution of the sample, and add 80μL d 5 -3-Chloro-1,2-propanediol palmitic acid diester internal standard solution (4.675 μg / mL, calculated as free state), vortexed to mix.

[0062] 2. Acid catalyzed transesterification, salting out, extraction

[0063] Add 0.5mL of 0.1% sulfuric acid-methanol solution to the centrifuge tube, screw it tightly, and then place it at 40°C for 2 hours of constant temperature reaction. After the reaction is completed, add saturated sodium bicarbonate solution to neutralize and vortex, so that the pH after neutralization is 6.7. Add 2 mL of 20% (v / v) sodium sulfate aqueous solution to the centrifuge tube, and extract with 2 mL of n-heptane solution, discard the organic phase containing fatty acid methyl ester in the upper layer, and obtain the aqueous phase containing 3...

Embodiment 2

[0089] 1. Sample pretreatment

[0090] Weigh 0.150 g of homogenized perilla oil into a centrifuge tube with a cover, and heat slightly at 45°C to dissolve the fat completely. Add 1 mL of tetrahydrofuran solution to the sample, and add 80 μL d 5 -3-Chloro-1,2-propanediol palmitic acid diester internal standard solution (4.675 μg / mL, calculated as free state), vortexed to mix.

[0091] 2. Acid catalyzed transesterification, salting out, extraction

[0092] Add 0.5mL of 0.1 (v / v) sulfuric acid-methanol solution to the centrifuge tube, screw it tightly, and place it at 45°C for 1 hour of constant temperature reaction. After the reaction is over, add saturated sodium bicarbonate solution to neutralize and vortex, so that the pH after neutralization is 7.6. Add 2 mL of 20% (v / v) sodium sulfate aqueous solution to the centrifuge tube, and extract with 2 mL of n-heptane solution, discard the organic phase containing fatty acid methyl ester in the upper layer, and obtain the aqueous...

Embodiment 3

[0098] 1. Sample pretreatment

[0099] Weigh 0.200g of homogenized corn oil into a centrifuge tube with a cover, and heat slightly at 50°C to completely dissolve the fat. Add 1 mL of tetrahydrofuran solution to the sample, and add 80 μL d 5-3-Chloro-1,2-propanediol palmitic acid diester internal standard solution (4.675 μg / mL, calculated as free state), vortexed to mix.

[0100] 2. Acid catalyzed transesterification, salting out, extraction

[0101] Add 0.5 mL of 0.1 (v / v) sulfuric acid-methanol solution to the centrifuge tube, screw it tightly, and place it at 55°C for 30 min at a constant temperature for reaction. After the reaction is over, add saturated sodium bicarbonate solution to neutralize and vortex, so that the pH after neutralization is 8.0. Add 2 mL of 20% (v / v) sodium sulfate aqueous solution to the centrifuge tube, and extract with 2 mL of n-heptane solution, discard the organic phase containing fatty acid methyl ester in the upper layer, and obtain the aqueo...

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Abstract

The invention relates to a method for detecting content of 3-monochloropropanol-1, 2-diol (3-MCPD) ester in edible oil. The method comprises the following steps: preprocessing a sample, carrying out acid-catalytic ester exchange, salting out, extracting, purifying, carrying out derivatization and detecting. According to the method, the internal labeling of stable isotopes is adopted, and the acid-catalytic ester exchanging is combined with the derivatization of heptafluorobutyrylimidazole to indirectly quantitatively analyze 3-MCPD ester by utilizing a single four-level lever GC-MS, so that the preprocessing time is shortened, the analysis efficiency is improved, the consumption amount of an organic solvent is greatly reduced, the environmental pollution is avoided, meanwhile, the analysis cost is also reduced, after the derivatization of heptafluorobutyrylimidazole, the information of a sample mass spectrum fragment is rich, and a gas chromatograph-mass spectrometer is hardly polluted.

Description

technical field [0001] The invention relates to a food detection method, in particular to a method for detecting the content of 3-chloro-1,2-propanediol ester in edible oil. Background technique [0002] 3-chloro-1,2-propanediol (3-monochloropropanol-1,2-diol, 3-MCPD) widely exists in the form of fatty acid ester (hereinafter referred to as 3-MCPD ester) in fried, baked and other foods, and It mainly comes from the refined edible oil added during processing. [0003] 3-Chloro-1,2-propylene glycol ester (3-MCPD ester) is the esterification product of 3-chloropropanol and fatty acid. It is another potential hazard factor introduced in the oil refining process. In 1983, Spain first refined aniline with hydrochloric acid. 3-MCPD ester was detected in rapeseed oil, but it has not been paid attention to for more than 20 years. With the development of science and technology and the high emphasis on food safety, 3-MCPD ester has attracted more and more attention from scientists an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 王强石爱民焦博刘红芝胡晖刘丽
Owner INST OF AGRO FOOD SCI & TECH CHINESE ACADEMY OF AGRI SCI
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