Method for determining 3-chloro-1,2-propanediol in seasoning

A technology of propylene glycol and condiments, which is applied in the field of analytical chemistry, can solve the problems of high consumption of toxic organic solvents, complicated and time-consuming operations, and increased detection costs, and achieve the effects of easy promotion, low detection cost and high accuracy

Inactive Publication Date: 2019-01-22
大连市食品检验所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of the existing determination methods consume a large amount of toxic organic solvents, and the operation is complicated and time-consuming
The derivatization reagent heptafluorobutyrylimidazole or silanization reagent is expensive and is particularly sensitive to water. After opening for a long time, it will react with water and deteriorate. The detection of individual samples also needs to consume a package of derivatization reagents, which will undoubtedly greatly increase the detection cost.
At the same time, fluorine-containing compounds are particularly stable and are likely to cause persistent pollution to the environment

Method used

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  • Method for determining 3-chloro-1,2-propanediol in seasoning
  • Method for determining 3-chloro-1,2-propanediol in seasoning
  • Method for determining 3-chloro-1,2-propanediol in seasoning

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Embodiment 1, optimization of experimental method

[0063] (1) Optimization of pretreatment method

[0064] ① Optimization of extraction conditions

[0065] The solvent for extracting 3-MCPD from liquid seasoning should be able to meet the following requirements: 1. easy to separate from the water phase, 2. good solubility to 3-MCPD, after distribution, 3-MCPD and its content in the organic phase The content of the target should be sufficient to meet the detection requirements after derivatization. 3. If the extraction solvent needs to be removed, the solvent used should have a lower boiling point.

[0066] The results of screening common laboratory solvents such as ethanol, methanol, ethyl acetate, isopropanol, acetonitrile, acetone, methyl ethyl ketone, n-hexane, toluene, chloroform, ether and tetrahydrofuran show that alcohol solvents such as methanol and ethanol are not easy Separated from the water phase, isopropanol has a certain extraction efficiency and is eas...

Embodiment 2

[0073] Embodiment 2, method verification experiment of the present invention

[0074] (1) Linear range and correlation coefficient

[0075] Prepare a series of standard working solutions containing 0.6 μg internal standard and 0.008, 0.016, 0.06, 0.12, 0.4, 1.2 μg of 3-MCPD respectively, and perform detection according to the determined analysis conditions, and quantify the ions of the target substance with the internal standard substance. The ratio of the peak area of ​​the ion is the ordinate (y), and the content of the target substance (x, μg) is used as the abscissa for linear regression, and the linear equation of 3-MCPD in the content range of 0.008-1.2 μg is y = 1.43 x+0.0071, the correlation coefficient (r) is 1.000, and the linear relationship is good.

[0076] (2) Recovery rate and precision

[0077] Blank soy sauce and chicken bouillon samples were used for addition and recovery experiments. The addition levels of soy sauce were 0.005, 0.02, and 0.40 mg / kg, and th...

Embodiment 3

[0082] Embodiment 3, soy sauce actual sample detection

[0083] (1) Preparation of solution

[0084] ① Saturated sodium chloride solution: Weigh sodium chloride, then add water, and use ultrasound to fully dissolve sodium chloride. The dosage ratio of sodium chloride to water is: 200g: 500mL;

[0085] (2) Preparation of standard solution

[0086] ①Preparation of standard stock solution: weigh 3-chloro-1,2-propanediol standard substance and internal standard D 5 -3-Chloro-1,2-propanediol was placed in volumetric flasks, and the volume was adjusted to the mark with ethyl acetate to obtain 1 mg / mL standard stock solutions, which were stored at -18°C in the dark;

[0087] ②Preparation of standard use solution: draw appropriate amount of 3-chloro-1,2-propanediol standard stock solution and D 5 -3-Chloro-1,2-propanediol standard stock solution in a volumetric flask, dilute to the mark with ethyl acetate respectively, and prepare a standard use solution with a concentration of 40 μg...

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Abstract

The invention belongs to the field of analytical chemistry, and provides a method for determining 3-chloro-1,2-propanediol in a seasoning. The 3-MCPD in the seasoning is extracted by butanone, and reacts with butanone to generate a cyclic compound under the catalysis of toluenesulfonic acid for determination. The method comprises the following detection steps: preparation of the solution, preparation of the standard stock solution, preparation of the sample solution, qualitative analysis by gas chromatography-mass spectrometry, and quantitative determination. The method provided by the invention can be used for detecting liquid seasonings such as soy sauce, fish sauce and protein seasoning liquid, and 3-MCPD in solid seasonings such as chicken essence and seafood powder. The use of butanone as extraction solvent and derivatization reagent eliminates the need for concentration and solvent conversion processes, avoiding expensive derivatization reagents in traditional detection methods.The method has the advantages of simple pretreatment, low organic solvent dosage, environmental protection, mild derivatization conditions, high accuracy, low detection cost, easy promotion, and the like.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and relates to a detection method, in particular to a method for measuring 3-chloro-1,2-propanediol (3-MCPD) in condiments which is environmentally friendly, low in cost and simple in operation, and is mainly used for Detection of 3-MCPD in soy sauce, protein seasoning liquid and solid seasoning. Background technique [0002] Chloropropanols are a class of internationally recognized food pollutants, among which 3-chloro-1,2-propanediol (3-MCPD) has the highest content and toxicity, and its main pollution source comes from acid hydrolyzed vegetable protein liquid. Naturally brewed soy sauce is produced from soybeans through microbial fermentation. During the fermentation process, protein is hydrolyzed to amino acids to produce umami flavors. The fermentation process takes 3 months. Under high temperature and strong acidic conditions, animal and plant proteins can be rapidly hydrolyzed into free...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/025G01N2030/062
Inventor 张敬波姜俊戴学东董广彬李鹏毛希琴单婷婷余巍张海丛长庚
Owner 大连市食品检验所
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