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Detection method for 3-MCPD ester in oil product

A product and oil testing technology, which is applied in the field of 3-chloropropanol ester detection, can solve the problems of further improvement of sensitivity, specificity and precision, decreased sperm activity, and weakened reproductive capacity of male animals.

Active Publication Date: 2017-01-18
COFCO GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

3-MCPD esters have attracted widespread attention mainly because 3-MCPD esters will be hydrolyzed by fatty acid enzymes into free 3-MCPD after being ingested by the human body. Free 3-MCPD has potential carcinogenicity and can inhibit male The secretion of hormones will reduce the number of sperm, reduce the activity of sperm, and weaken the reproductive ability of male animals, even infertility
[0006] At present, in the method of indirect determination, the sensitivity, specificity and precision still need to be further improved

Method used

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  • Detection method for 3-MCPD ester in oil product
  • Detection method for 3-MCPD ester in oil product
  • Detection method for 3-MCPD ester in oil product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] This embodiment is used to illustrate the method for detecting 3-chloropropanol esters in oil products provided by the present invention

[0072] (1) Alkaline hydrolysis

[0073] Take 100 mg of soybean oil samples that do not contain 3-MCPD ester, and add 3-MCPD ester to prepare standard samples with concentrations of 50 μg / kg, 150 μg / kg, 300 μg / kg, 1500 μg / kg, and 12000 μg / kg, respectively. 6 repetitions, then add 0.0397mL deuterated isotope internal standard d 5 - 3-MCPD ester standard solution (126 μg / mL) and 100 μL of tBME, vortex to fully dissolve and mix. 200 μL of 25 g / L NaOH methanol solution (25 g NaOH dissolved in 1 L of methanol) was added thereto, vortexed for 1 min for hydrolysis, and a hydrolyzate was obtained.

[0074] (2) Acid neutralization

[0075] Add 600 µL of NaBr-H to the hydrolyzate from step (1) 2 SO 4 Mixed solution (3.5mL 25% H 2 SO 4 Dissolve in 100mL of 600g / L NaBr solution), vortex and mix well to carry out the neutralization reaction...

Embodiment 2

[0093] This embodiment is used to illustrate the method for detecting 3-chloropropanol esters in oil products provided by the present invention

[0094] (1) Alkaline hydrolysis

[0095] Take 100 mg of olive oil samples that do not contain 3-MCPD esters, and add 3-MCPD esters to prepare standard samples with concentrations of 50 μg / kg, 150 μg / kg, 300 μg / kg, 1500 μg / kg, and 12000 μg / kg, each sample 6 repetitions, then add 0.0397mL deuterated isotope internal standard d 5 - 3-MCPD ester standard solution (126 μg / mL) and 80 μL of tBME, vortex to fully dissolve and mix. 180 μL of 28 g / L NaOH methanol solution (28 g NaOH dissolved in 1 L of methanol) was added thereto, vortexed for 1.5 min for hydrolysis, and a hydrolyzed product was obtained.

[0096] (2) Acid neutralization

[0097] Add 650 μL of NaBr-H to the hydrolyzate from step (1) 2 SO 4 Mixed solution (3.5mL 25% H 2 SO 4 Dissolve in 100mL of 600g / L NaBr solution), vortex and mix well to carry out the neutralization re...

Embodiment 3

[0105] This embodiment is used to illustrate the method for detecting 3-chloropropanol esters in oil products provided by the present invention

[0106] (1) Alkaline hydrolysis

[0107] Take 100 mg of sesame oil samples that do not contain 3-MCPD esters, and add 3-MCPD esters to prepare standard samples with concentrations of 50 μg / kg, 150 μg / kg, 300 μg / kg, 1500 μg / kg, and 12000 μg / kg, respectively, each sample 6 Repeat, then add 0.0397mL deuterated isotope internal standard d 5 - 3-MCPD ester standard solution (126 μg / mL) and 120 μL of tBME, vortex to fully dissolve and mix. 220 μL of 23 g / L NaOH methanol solution (23 g NaOH dissolved in 1 L of methanol) was added thereto, vortexed for 2.5 min for hydrolysis, and a hydrolyzed product was obtained.

[0108] (2) Acid neutralization

[0109] Add 550 µL of NaBr-H to the hydrolyzate from step (1) 2 SO 4 Mixed solution (3.5mL 25% H 2 SO 4 Dissolve in 100mL of 600g / L NaBr solution), vortex and mix well to carry out the neutra...

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Abstract

Relating to the detection field of 3-MCPD ester, the invention discloses a detection method for 3-MCPD ester in an oil product. The method includes: (1) contacting a to-be-detected oil product with a methanol solution of sodium hydroxide to perform hydrolysis so as to obtain a hydrolysis product; (2) contacting the hydrolysis product with a mixed solution containing sulfuric acid and sodium halide to perform neutralization so as to obtain a neutralization product, wherein the sodium halide is sodium bromide and / or sodium iodide; (3) using an organic solvent to extract the neutralization product, and subjecting the obtained extracted solution and phenylboronic acid to contact reaction; and (4) conducting gas chromatography-mass spectrometry on the reaction product obtained by reaction in step (3). According to the technical scheme, the methanol solution of sodium hydroxide is employed to conduct alkaline hydrolysis on the to-be-detected sample, the mixed solution of sodium bromide and sulfuric acid is employed to conduct neutralization treatment on the alkaline hydrolysis product, thus effectively improving the sensitivity, specificity and precision of subsequent detection.

Description

technical field [0001] The invention relates to the detection field of 3-chloropropanol ester (3-MCPD ester), in particular to a method for detecting 3-chloropropanol ester in oil products. Background technique [0002] 3-MCPD ester is a monochlorine substitute formed by replacing the hydroxyl group at the 1st or 3rd position in glycerin with a chlorine atom. It is colorless and has a pleasant fragrance. Soluble in ethanol, water, acetone, etc. In 1980, Davidek et al. first discovered 3-chloropropanol (3-MCPD) esters in acid hydrolyzed vegetable protein (HVP). Since then, researchers have found different levels of 3-MCPD esters in various heat-processed foods. 3-MCPD esters are mainly formed during food processing, especially thermal processing, such as oil refining, hydrogenation, deodorization, etc. 3-MCPD esters have attracted widespread attention mainly because 3-MCPD esters are hydrolyzed by fatty acid enzymes into free 3-MCPD after being ingested by the human body. F...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 苗雨田杨悠悠王浩刘佟杨永坛
Owner COFCO GROUP
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