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Sample pretreatment method for detection of free and bonded 3-chlorine-1,2-propylene glycol in grease

A propylene glycol and free-type technology, which is applied in measuring devices, material separation, instruments, etc., can solve the problems of large solvent consumption, high price of solid-phase extraction columns, and unsatisfactory results.

Active Publication Date: 2014-02-12
SHANGHAI RONGS HEALTH IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of the silica gel column chromatography method is that the whole pretreatment period is long, the amount of solvent consumed is large (some even greater than 500mL), and the packing effect of the column directly affects the effect of sample pretreatment. Reproducibility suffers greatly
The disadvantage of the solid-phase extraction column extraction method is that the price of the solid-phase extraction column is relatively high, which increases the cost of sample pretreatment. It is easy to be polluted, which increases the operation requirements of the whole pretreatment process, and a little carelessness in the operation process will lead to unsatisfactory results of sample pretreatment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Sample pretreatment method for the detection of free and bound 3-chloro-1,2-propanediol in oils:

[0028] Measure 15mL of oil (13.68g by accurate weighing) into a 50mL screw-cap glass test tube, add 25mL of acetonitrile, vortex, mix well for 1-3min → let the layers stand for about 1 hour, and use a disposable straw to remove the upper layer Transfer the 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 pour the acetonitrile for cleaning into a 100mL round bottom flask In a bottom flask, at 55°C, under vacuum conditions, rotary evaporate to dry the solvent, dissolve the residue with 2.5mL tetrahydrofuran (THF), transfer it into a 5mL screw cap sample bottle, seal it with a parafilm, and refrigerate at 4°C for later use....

Embodiment 2

[0034] Another sample pretreatment method for the detection of free and bound 3-chloro-1,2-propanediol in oils:

[0035] Measure 5mL of oil (accurately weigh its mass to 4.56g) into a 50mL screw cap glass test tube, add 25mL of acetonitrile, vortex, mix well for 1-3min, centrifuge at 10000 rpm for 5 minutes, 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-bottomed flask, and wash the graduated cylinder with an appropriate amount of acetonitrile (about 3mL), and pour the acetonitrile used for cleaning into In a 100mL round-bottomed flask, at 55°C, under vacuum conditions, rotary evaporate to dry the solvent, dissolve the residue with 2.5mL tetrahydrofuran (THF), transfer it into a 5mL screw cap sample bottle, seal it with a parafilm, and refrigerate at 4°C for later use.

[0036] (1) ...

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PUM

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Abstract

The invention discloses a sample pretreatment method for detection of free and bonded 3-chlorine-1,2-propylene glycol in grease. The method comprises the steps of weighing proper amount of grease, adding a polar solvent at certain volume, taking out a solvent phase after the solution is layered, rotatably evaporating the solvent under a vacuum condition, dissolving the residue with tetrahydrofuran, and respectively conducting the following operations: (1) further processing of detection of free 3-chlorine-1,2-propylene glycol, and (2) further processing of detection of bonded 3-chlorine-1,2-propylene glycol. According to the invention, a sample for detecting the free and bonded 3-chlorine-1,2-propylene glycol in the grease can be pre-treated by using the simple method.

Description

technical field [0001] The invention relates to a pretreatment method for oil samples, in particular to a sample pretreatment method for the detection of free and combined 3-chloro-1,2-propanediol (3-MCPD) in oil. Background technique [0002] 3-Chloro-1,2-propanediol ester (3-MCPDE) is a by-product formed during thermal processing of fats and fat-containing foods, and exists in fats in the form of 3-MCPD. Since 3-chloro-1,2-propanol ester can be hydrolyzed to form free 3-MCPD under certain conditions, which shows its toxicity, researchers believe that it is a potential food safety hazard factor. The formation mechanism and influencing factors of 3-MCPDE in oils are current research hotspots at home and abroad. In order to ascertain these problems, it is necessary to have convenient and feasible sample pretreatment methods as support. [0003] Among the methods reported in the literature for the detection of free and bound 3-MCPD in oils and fats, they can be roughly divide...

Claims

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Application Information

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