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Rapid detection method of 3-MCPD and 3-MCPDE in edible vegetable oil

A technology of edible vegetable oil and detection method, which is applied in the field of rapid detection of 3-MCPD and 3-MCPDE in edible vegetable oil, can solve problems such as unfavorable guidance, long detection time, etc., and achieves the improvement of efficiency, dissolution effect and detection efficiency. Effect

Pending Publication Date: 2021-01-22
青岛天祥食品集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Edible vegetable oil crude oil can be refined to remove harmful substances through decolorization, degumming, dewaxing, and deodorization, but the harmful factors 3-1, 2-chloropropanediol ester (3-MCPDE) and 3-1 , the formation of 2-chloropropanediol (3-MCPD), the national standard GB 5009.191-2016 "National food safety standard for the determination of chloropropanol and fatty acid ester content in food" and the industry standard " Rapid Determination of 3-Chloropropanol Fatty Acid Esters in Grain and Oil Inspection Vegetable Oils and Oils, the traditional sample detection takes more than 17 hours from processing to machine detection results, and the detection time is too long, which is not conducive to providing edible vegetable oil refining production process. guide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of rapid detection method of 3-MCPD in edible vegetable oil, comprises the following steps:

[0022] S1. Weigh 100±5mg edible vegetable oil sample A to be tested and put it into a centrifuge tube, add 5ng of d 5 -3-chloro-1,2-propanediol palm diester, then add the toluene that adds 70uL, then add the methyl-tert-butyl ether of 100uL;

[0023] S2. Repeatedly oscillate clockwise and counterclockwise for 13-18s;

[0024] S3. Add 25 mL of n-hexane, centrifuge and discard the supernatant, add 25 mL of n-hexane again, centrifuge and discard the supernatant;

[0025] S4. Add 100uL of diethyl ether+ethyl acetate to the lower aqueous phase, and vortex for 6s;

[0026] S5. Take the supernatant and add it to a sample bottle containing a trace amount of 1+1 sodium sulfate-sodium bicarbonate, add 10 uL of phenylboronic acid to carry out the derivatization reaction for 30 seconds, add ethyl acetate to terminate the reaction, and prepare the sample to be tested;

[0027] S6....

Embodiment 2

[0034] A kind of rapid detection method of 3-MCPDE in edible vegetable oil, comprises the following steps:

[0035] S1. Weigh 100±5mg edible vegetable oil sample B to be tested and put it into a centrifuge tube, add 5ng of d5-3-chloro-1,2-propanediol palmitic ester, then add 70uL of toluene, then add 100uL of methyl- Tert-butyl ether, finally add NaOH-methanol solution;

[0036] S2. Oscillate clockwise and counterclockwise for 13-18s at a temperature of 40°C;

[0037] S3. Add 600uL concentrated sulfuric acid acidified NaBr at 40-50°C and react for 3-5min;

[0038] S4. Add 25 mL of n-hexane, centrifuge and discard the supernatant, add 25 mL of n-hexane again, centrifuge and discard the supernatant;

[0039] S5. Add 100 uL of diethyl ether+ethyl acetate to the lower aqueous phase, and vortex for 6 seconds;

[0040] S6. Take the supernatant and add it to a sample bottle containing a trace amount of 1+1 sodium sulfate-sodium bicarbonate, add 10 uL of phenylboronic acid to perfo...

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Abstract

The invention discloses a rapid detection method of 3-MCPD and 3-MCPDE in edible vegetable oil. The method comprises the following steps of: dissolving a grease sample, breaking ester bonds, performing purifying, drying and dehydrating, carrying out derivative reaction, conducting detecting and analyzing by a GC-MS gas chromatograph-mass spectrometer, and finally calculating the concentrations of3-MCPD and 3-MCPDE in a vegetable oil sample. According to the detection method, the time from sample treatment to on-machine detection is about 45min, compared with other detection methods at the present stage, the efficiency is greatly improved, the detection method is more precise, and the detection method is more beneficial for edible vegetable oil enterprises to guide production.

Description

technical field [0001] The invention relates to the field of vegetable oil detection methods, in particular to a rapid detection method for 3-MCPD and 3-MCPDE in edible vegetable oil. Background technique [0002] Edible vegetable oil crude oil can be refined to remove harmful substances through decolorization, degumming, dewaxing, and deodorization, but the harmful factors 3-1, 2-chloropropanediol ester (3-MCPDE) and 3-1 , the formation of 2-chloropropanediol (3-MCPD), the national standard GB 5009.191-2016 "National food safety standard for the determination of chloropropanol and fatty acid ester content in food" and the industry standard " Rapid Determination of 3-Chloropropanol Fatty Acid Esters in Grain and Oil Inspection Vegetable Oils and Oils, the traditional sample detection takes more than 17 hours from processing to machine detection results, and the detection time is too long, which is not conducive to providing edible vegetable oil refining production process. ...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 于小华于强刘红芝宋福荣王青孔德程杨增龙邢福国胡晖焦博
Owner 青岛天祥食品集团有限公司
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