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A method for detecting the content of 3-chloro-1,2-propanediol ester in edible oil

A technology of propylene glycol ester and edible oil, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of polluting the gas spectrometer, affecting the analysis efficiency, and cumbersome processing steps, so as to avoid instrument maintenance, avoid cross-contamination, and instrument low pollution effect

Active Publication Date: 2016-01-20
INST OF AGRO FOOD SCI & TECH CHINESE ACADEMY OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A method for detecting the content of 3-chloro-1,2-propanediol 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 in a centrifuge tube with a lid, heat slightly at 40°C to dissolve all the fat, add 1mL tetrahydrofuran solution of the sample, and add 80μLd 5 -3-Chloro-1,2-propanediol palmitic acid diester internal standard solution (4.675μg / mL, in free form), vortex and mix well.

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

[0063] Add 0.5 mL of 0.1% sulfuric acid-methanol solution to the centrifuge tube, screw it tightly and place it at 40°C for constant temperature reaction for 2 hours. After the reaction is over, add saturated sodium bicarbonate solution to neutralize and vortex to make the pH 6.7 after neutralization . 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 upper organic phase containing fatty acid methyl esters to obtain an aqueous phase containing 3-MCPD.

[0064] 3. Purification

[0065] ...

Embodiment 2

[0089] 1. Sample pretreatment

[0090] Weigh 0.150g of homogenized perilla oil in a centrifuge tube with a lid, and heat it slightly at 45°C to dissolve all the fat. Add sample 1mL tetrahydrofuran solution, and add 80μLd 5 -3-Chloro-1,2-propanediol palmitic acid diester internal standard solution (4.675μg / mL, in free form), vortex and mix well.

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

[0092] Add 0.5 mL of 0.1 (v / v) sulfuric acid-methanol solution to the centrifuge tube, screw it tightly and place it at 45°C for constant temperature reaction for 1 hour. After the reaction is over, add saturated sodium bicarbonate solution to neutralize and vortex to make the pH 7.6 after neutralization. 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 upper organic phase containing fatty acid methyl esters to obtain an aqueous phase containing 3-MCPD.

[0093] 3. Purification

[0...

Embodiment 3

[0098] 1. Sample pretreatment

[0099] Weigh 0.200g of homogenized corn oil in a centrifuge tube with a lid, and heat slightly at 50°C to dissolve all the fat. Add sample 1mL tetrahydrofuran solution, and add 80μLd 5 -3-Chloro-1,2-propanediol palmitic acid diester internal standard solution (4.675μg / mL, in free form), vortex and mix well.

[0100] 2. Acid-catalyzed transesterification, salting out, and 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 constant temperature reaction for 30 minutes. After the reaction is over, add saturated sodium bicarbonate solution to neutralize and vortex to make the pH 8.0 after neutralization. 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 upper organic phase containing fatty acid methyl esters to obtain an aqueous phase containing 3-MCPD.

[0102] 3. Purification

[010...

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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-monochloropropanol-1,2-diol (3-monochloropropanol-1,2-diol, 3-MCPD) in the form of fatty acid ester (hereinafter referred to as 3-MCPD ester) is widely present in foods such as frying and baking, and It is mainly derived from refined edible oil added during processing. [0003] 3-Chloro-1,2-propanediol ester (3-MCPD ester) is an ester compound of 3-chloropropanol and fatty acid. It is another potential hazard factor introduced in the process of oil refining. In 1983, Spain was the first to contaminate aniline in hydrochloric acid refining 3-MCPD ester was detected in rapeseed oil, but it has not received attention for more than 20 years. With the development of science and technology and the great importance of food safety, 3-MCPD ester has attracted more and more attention fro...

Claims

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Application Information

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Patent Type & Authority Patents(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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