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Method for enriching endocrine interfering substances by using silica self-assembled microcapsule

A technology of endocrine disruptors and silicon dioxide, which is applied in the direction of measuring devices, material separation, and analysis of materials, can solve the problems of long processing period, complex matrix interference, low concentration, etc., and achieve the goal of short time and good enrichment index Effect

Active Publication Date: 2018-08-17
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the pollution of environmental endocrine disruptors is becoming more and more serious, in general, its concentration in the environment is still relatively low (ppt-ppb level), and there is interference from complex matrix. The pretreatment is trace environmental endocrine disruptors An indispensable and important link in the analysis, it needs to be enriched to meet the needs of high sensitivity and high efficiency detection of trace endocrine disruptors
Traditional sample pretreatment methods, such as Soxhlet extraction, liquid-liquid extraction, etc., mostly have the disadvantages of complicated operation, high work intensity, long processing cycle, large loss of organic solvent, and low extraction efficiency.

Method used

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  • Method for enriching endocrine interfering substances by using silica self-assembled microcapsule
  • Method for enriching endocrine interfering substances by using silica self-assembled microcapsule
  • Method for enriching endocrine interfering substances by using silica self-assembled microcapsule

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment 1 (product preparation):

[0049] A kind of silicon dioxide self-assembled microcapsule, its preparation steps are as follows:

[0050] (1) Preparation of amphiphilic silica particles:

[0051]Dissolve 0.60g CTAB and 0.20g polyoxyethylene lauryl ether Brij56 in 100ml of well-stirred buffer solution (0.16g of sodium hydroxide and 0.68g of sodium dihydrogen phosphate), heat up to 80°C, and when the solution is uniform, put 2.00mL of TEOS was added dropwise into the above surfactant solution, and stirred by magnetic force for 20h. After the reaction was completed, it was centrifuged, washed 5 times with ethanol, and vacuum-dried at 60° C. for 48 hours to obtain 80 mg of amphiphilic silica particles.

[0052] (2) Preparation of silica self-assembled microcapsules:

[0053] Take 5 mg of the amphiphilic silica particles obtained in step (1) and place them in eight test tubes respectively, add 2 ml of 10 mg / L BPA solution as the water phase, and fully ultrasonica...

Embodiment 2

[0058] Embodiment 2 (microcapsule morphology observation):

[0059] A self-assembled microcapsule of amphiphilic silicon dioxide, the preparation steps of which are as follows:

[0060] (1) Preparation of amphiphilic silica particles:

[0061] The preparation method is the same as step (1) of Example 1.

[0062] (2) Preparation of silica self-assembled microcapsules:

[0063] Take 5 mg of amphiphilic silica particles obtained in step (1) and place them in a test tube, add 2 ml of calcein solution with a concentration of 5 mmol / L, and fully ultrasonically disperse; then add 100 μl of dodecane to the test tube to prepare a concentration of 10 mmol / L of Nile red dye, placed in a tumbler and tumbled for 2 hours at a speed of 80rad / min.

[0064] Observing the microcapsule morphology formed in step (2) under a fluorescence microscope, obtained Figure 5 (a), found to be in the size range of 100 μm to 500 μm, by water-soluble calcein Figure 5 (b) and oil-soluble Nile Red Fig...

Embodiment 3

[0065] Embodiment 3 (simulation application experiment): the application experiment of low-concentration BPA enrichment simulation sewage in the microcapsule of silicon dioxide self-assembly

[0066] Take respectively 5 mg of the amphiphilic silica particles prepared by step (1) of Example 1 and place them in eight test tubes, add 2 ml of bisphenol A (BPA) solution with a concentration of 10 mg / L, and fully ultrasonically disperse them; then Add 100 μl of cyclohexane, n-hexane, n-heptane, dodecane, n-hexanol, n-octanol, oleic acid and olive oil to each of the eight test tubes, place them in a tumbler at a speed of 80 rad / min for 24 hours, sufficient enrichment to reach equilibrium.

[0067] The concentration of BPA in the organic phase and the residual water phase was detected by high performance liquid chromatography, and the enrichment effect was evaluated.

[0068] Image 6 It is a comparison chart of the enrichment effect of low-concentration BPA in simulated sewage by s...

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Abstract

The invention belongs to the technical field of enrichment of low-concentration endocrine interfering substances, and specifically discloses a method for enriching endocrine interfering substances byusing an amphiphilic silica self-assembled microcapsule. The method comprises: modifying with surfactants such as cetyltrimethylammonium bromide and polyoxyethylene lauryl ether by using tetraethoxysilane as a precursor to obtain amphiphilic silica particles, dispersing the amphiphilic silica particles as a film material in sewage containing endocrine interfering substances, adding a small amountof an alcohol or alkane or oleic acid or olive oil as an oil phase, and self-assembling to form the microcapsule having the oil-in-water structure. According to the present invention, with the microcapsule extraction method, the low-concentration endocrine interfering substances (such as phenols or titanates and the like) in the sewage can be enriched in the microcapsule so as to achieve the highconcentration, such that the subsequent treatment is convenient; an compared to the traditional liquid-liquid micro-extraction and the solid-liquid micro-extraction, the method of the present invention has the following advantages that the operation is simple, the enrichment effect is good, the film material can be repeatedly recovered and utilized, and the subsequent analysis and the non-toxic treatment can be conveniently performed.

Description

technical field [0001] The invention relates to the technical field of enrichment of low-concentration endocrine disruptors, in particular to a method for enriching endocrine disruptors by silica self-assembled microcapsules. Background technique [0002] Environmental endocrine disruptors are generally discharged by humans. Natural and synthetic endocrine disruptors mainly enter the sewage system, and are discharged into surface water and sediments after being treated by sewage treatment plants. Fish and wild animals are thus polluted, and human beings drink them. water and higher food chains. Although the pollution of environmental endocrine disruptors is becoming more and more serious, in general, its concentration in the environment is still relatively low (ppt-ppb level), and there is interference from complex matrix. The pretreatment is trace environmental endocrine disruptors An indispensable and important link in the analysis, it needs to be enriched to meet the nee...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/40G01N30/02
CPCG01N1/4055G01N30/02
Inventor 孙杰范顶进尹杉杉喻玲玲
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES