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Method for detecting content of free and combined 3-chlorine-1, 2-propylene glycol in grease

A technology of propylene glycol and 3-mcpd-d5, which is applied in the direction of measuring devices, material separation, instruments, etc.

Inactive Publication Date: 2014-07-09
SHANGHAI RONGS HEALTH IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the methods for detecting the content of different forms of 3-MCPD in oils and fats have not been reported in the literature at present.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Detection method for free and bound 3-MCPD content in oils and fats:

[0022] Measure 10 mL of first-grade soybean oil (accurately weighed to be 9.12 g) in a 50 mL screw-cap glass test tube, add 25 mL of acetonitrile, vortex, mix well for 1-3 min, and then let stand for stratification for about 1 hour. Pipette the upper acetonitrile phase into a 25mL graduated cylinder, read the volume of the acetonitrile phase and record it accurately, then transfer the acetonitrile phase in the graduated cylinder into a 100mL round bottom flask, and wash the graduated cylinder with an appropriate amount of acetonitrile (about 3mL). Put it into a 100 mL round-bottomed flask, and at 55 °C under vacuum conditions, rotary evaporate the solvent to dry out the solvent and refrigerate at 4 °C for later use.

[0023] (1) Further processing of free 3-MCPD assay:

[0024] The above residue was dissolved in 2.5 mL of tetrahydrofuran (THF), and 1 mL of the tetrahydrofuran solution was pipetted, ...

Embodiment 2

[0038] Detection method for free and bound 3-MCPD content in oils and fats:

[0039] Measure 10 mL of edible blending oil (accurately weighed as 9.02 g) into a 50 mL screw-cap glass test tube, add 25 mL of acetonitrile, vortex, mix thoroughly for 1-3 minutes, and then let stand for stratification for about 1 hour, use a disposable pipette Transfer the upper acetonitrile phase into a 25mL graduated cylinder, read the volume of the acetonitrile phase and record it accurately, then transfer the acetonitrile phase in the graduated cylinder into a 100mL round bottom flask, and wash the graduated cylinder with an appropriate amount of acetonitrile (about 3mL), and the acetonitrile used for cleaning is incorporated into In a 100 mL round-bottomed flask, at 55 °C, under vacuum conditions, rotary evaporate the solvent to dryness and refrigerate at 4 °C for later use.

[0040] (1) Further processing of free 3-MCPD assay:

[0041] The above residue was dissolved in 2.5 mL of tetrahydrof...

Embodiment 3

[0055] Detection method for free and bound 3-MCPD content in oils and fats:

[0056] Measure 10 mL of corn germ oil (accurately weighed to be 9.13 g) into a 50 mL screw-cap glass test tube, add 25 mL of acetonitrile, vortex, mix thoroughly for 1-3 minutes, and then let stand for 1 hour, and then use a disposable pipette. Transfer the upper acetonitrile phase into a 25mL graduated cylinder, read the volume of the acetonitrile phase and record it accurately, then transfer the acetonitrile phase in the graduated cylinder into a 100mL round bottom flask, and wash the graduated cylinder with an appropriate amount of acetonitrile (about 3mL), and the acetonitrile used for cleaning is incorporated into In a 100 mL round-bottomed flask, at 55 °C, under vacuum conditions, rotary evaporate the solvent to dryness and refrigerate at 4 °C for later use.

[0057] (1) Further processing of free 3-MCPD assay:

[0058] The above residue was dissolved in 2.5 mL of tetrahydrofuran (THF), and 1 ...

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Abstract

The invention discloses a method for detecting content of free and combined 3-chlorine-1, 2-propylene glycol in grease, comprising the following steps: enriching polar components in grease, wherein the enriched polar components are divided into three groups to be treated, the first group is added with internal standard substance 3-MCPD-d5, the second group is added with the internal standard substance 3-MCPD-d5 after being subjected to acid catalysis alcoholysis, and the third group is subjected to acid catalysis alcoholysis after being treated by a sold-phase extraction column and is added with the internal standard substance 3-MCPD-d5; carrying out phenylboronic acid derivatization treatment on the three groups of mixtures after treatment so as to respectively obtain a derivative product; respectively carrying out GC-MS detection on the obtained derivation product; calculating the content of free and combined 3-MCPD in the grease. According to the invention, the contents of the 3-MCPD in the grease in different existence forms can be respectively detected so as to obtain the content data of free 3-MCPD, 3-MCPD monoester and 3-MCPD diester.

Description

technical field [0001] The invention relates to a method for detecting hazard factors in oil and fat samples, in particular to a method for detecting the content of free and bound 3-MCPD in oil and fat. Background technique [0002] A large number of toxicological studies have shown that 3-chloro-1,2-propanediol (ie free 3-MCPD) has the effect of reducing sperm count, reducing sperm motility, and disturbing the balance of sex hormones in the body and reducing the reproductive capacity of male animals. Carcinogenic, potentially carcinogenic and toxic to the kidneys, liver and reproduction, can cause renal tubular hyperplasia and liver damage, is genotoxic in vitro (El Ramy, R., Ould Elhkim, M., Lezmi, S., Poul, J.M., Evaluation of the genotoxic potential of 3-monochloropropane-1, 2-diol (3-MCPD) and its metabolites, glycidol and beta-chlorolactic acid, using the single cell gel / comet assay. Food Chem Toxicol. 2007, 45 , 41-48; Cho, W.S., Han, B.S., Lee, H., Kim, C., Nam, K.T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 金青哲周红茹纪聪利曾君瑞王兴国刘睿杰邹孝强
Owner SHANGHAI RONGS HEALTH IND CO LTD
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