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Method for determining plasticizer through ultrahigh pressure assisted liquid-liquid micro extraction

An ultra-high pressure, auxiliary liquid technology, used in measuring devices, instruments, scientific instruments, etc., can solve the problems of a large number of solvents, environmental pollution, complex pretreatment methods of plasticizers, etc., to meet the requirements of monitoring, good repeatability, and measurement speed. quick effect

Inactive Publication Date: 2015-05-20
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] From the differences in the above documents, it can be seen that the whole society attaches great importance to the research and monitoring of plasticizers, especially for the research and monitoring of phthalic plasticizers, which has a great impact on improving food safety to a certain extent. However, the pretreatment methods for various plasticizers are relatively complicated, and most pretreatment processes require a large amount of solvents, which will cause certain pollution to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A method for ultra-high pressure assisted liquid-liquid extraction to enrich plasticizers, which is obtained through the following steps:

[0025] After the sewage discharged from a factory was filtered through filter paper, 25 mL of filtrate was accurately pipetted and placed in a double-layer composite bag, 8.0 g of potassium sulfate and 1.5 mL of n-hexane were added, and the double-layer composite bag was heat-sealed and placed in an ultra-high pressure treatment chamber. Ultrahigh pressure treatment under 650 MPa pressure for 3 minutes. After the treatment, the n-hexane phase was taken out, and the n-hexane phase was analyzed by gas chromatography-mass spectrometry, and the internal standard standard curve method was used for quantitative determination. The content of dibutyl phthalate (DBP) in the sewage was determined to be 19.23 μg / L.

[0026] Compared with the traditional method: take the same sewage sample and filter it through filter paper, accurately pipett...

Embodiment 2

[0028] A method for enriching plasticizers by ultra-high pressure assisted liquid-liquid microextraction, which is obtained through the following steps:

[0029]Take 15g of soil in the suburbs, add 500mL of distilled water, filter after fully stirring, accurately pipette 25mL of filtrate samples and place them in a double-layer composite bag, add 10.0g of anhydrous sodium sulfate and 2.5 mL of dichloromethane, heat the double-layer composite bag After sealing, place it in an ultra-high pressure treatment chamber for 5 minutes under a pressure of 450 MPa. After the treatment, the dichloromethane phase was taken out, and the dichloromethane phase was analyzed by gas chromatography-mass spectrometry, and the internal standard standard curve method was used for quantitative determination. The content of tributyl citrate (TBC) in the soil was determined to be 5.61 μg / Kg.

[0030] Compared with the traditional method: take 15g of the same soil sample, add 500mL of distilled water,...

Embodiment 3

[0032] A method for enriching plasticizers by ultra-high pressure assisted liquid-liquid microextraction, which is obtained through the following steps:

[0033] Take commercially available liquid milk products, after demulsification by a high-speed centrifuge, accurately pipette 25mL supernatant into a double-layer compound bag, add 8.0g of potassium sulfate and 3.5 mL of methyl tert-butyl ether, and place the double-layer compound bag After being heat-sealed, it was placed in an ultra-high pressure treatment chamber for 5 minutes at a pressure of 750 MPa. After the treatment, the methyl tert-butyl ether phase was taken out, the methyl tert-butyl ether phase was analyzed by gas chromatography-mass spectrometry, and the internal standard standard curve method was used for quantitative determination. After determination, the diphthalic acid in the milk product The content of (2-ethyl)hexyl ester (DEHP) was 3.69 μg / L.

[0034] Compared with the traditional method: take the same...

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Abstract

The invention relates to a method for determining a plasticizer through ultrahigh pressure assisted liquid-liquid micro extraction. The method comprises the following steps: dispersing a sample to be detected with distilled water, carrying out solid-liquid separation to remove solid substances, adding 5.0-25g of inorganic salt into 25-50ml of filtrate and putting into a double-layer composite bag; or directly obtaining 25-50ml of the sample to be detected, or filtrate of the sample to be detected or liquid supernatant obtained after centrifugation of the sample to be detected, adding 5.0-25g of inorganic salt and putting into the double-layer composite bag; and adding 0.5-5.0mL of organic solvent, then sealing the double-layer composite bag, placing the double-layer composite bag into an ultra high pressure treatment cavity for ultra high pressure treatment for 1-10min under the pressure of 200-900 MPa, taking out an organic phase after treatment, and quantitatively detecting the content of the plasticizer by use of a gas chromatography-mass spectrometer. The method is carried out at normal temperature, the measurement speed is high, no side reaction is caused, the method is environment-friendly, the repeatability is good and the monitoring requirement for the trace plasticizer can be met.

Description

technical field [0001] The invention belongs to the technical field of plasticizer determination, and in particular relates to a method for enriching and separating trace plasticizers contained in a sample by means of ultra-high pressure auxiliary liquid-liquid micro-extraction technology and quantitatively measuring them. Background technique [0002] There are many kinds of plasticizers. According to incomplete statistics, there are more than 100 specific types of plasticizers. According to the commonly used chemical structures, they can be classified into: 1) phthalates; 2) aliphatic Dibasic acid esters; 3) Phosphate esters; 4) Benzoic acid esters; 5) Citric acid esters; 6) Polymeric plasticizers; 7) Cyclohexane diacid esters; Plasticizer; 9) Alkyl sulfonate, etc. In recent years, phthalates among phthalates have frequently appeared in food. [0003] Phthalate ester plasticizers are the most commonly used plasticizers, but because of their nephrotoxicity, reproductive t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/08
Inventor 张峻松张秀芝李瑞丽苗晨琳李强侯鹏娟李皓
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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