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Preparation method of triclosan carbon nano-tube molecule imprinted polymer and determination method of content of triclosan applied to daily chemical products

A technique of imprinting polymers and molecular imprinting, applied in chemical instruments and methods, material separation, analysis of materials, etc., can solve problems affecting accuracy, difficulty in enriching trace samples, and complicated processing

Inactive Publication Date: 2013-08-21
NAT INST OF METROLOGY CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the problems of complex sample pretreatment and difficulty in the enrichment of trace samples, the recovery rate of sample testing is not high, which affects the accuracy of the determination

Method used

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  • Preparation method of triclosan carbon nano-tube molecule imprinted polymer and determination method of content of triclosan applied to daily chemical products
  • Preparation method of triclosan carbon nano-tube molecule imprinted polymer and determination method of content of triclosan applied to daily chemical products
  • Preparation method of triclosan carbon nano-tube molecule imprinted polymer and determination method of content of triclosan applied to daily chemical products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] 1) Silicon-coated carbon nanotubes (CNTSiO 2 ) preparation

[0072] Put 250 mg of purified CNT, 0.5 mL of APTES, 100 mg of CTAB, and 48 mL of deionized water into a 100 mL Erlenmeyer flask, sonicate at 40°C for 20 min, then stir at the maximum speed of a magnetic stirrer for 3 h to obtain a mixture A. Put 5mLTEOS, 3mL deionized water, and 50mL ethanol in a 100mL Erlenmeyer flask, sonicate at 40°C for 20min, and then stir for 3h at the maximum speed of a magnetic stirrer to obtain a mixture B. After the mixture A and B were mixed again, they were sonicated at 40°C for 1 h, then stirred at the maximum speed of a magnetic stirrer for 10 min, and finally, the pH value of the mixture was adjusted to 9.5 with ammonia water. After centrifuging the resulting mixed solution, wash it repeatedly with deionized water and ethanol several times until the supernatant after centrifugation is neutral, and obtain silicon-coated carbon nanotubes CNTSiO 2 . The resulting CNTSiO 2 Vacuu...

Embodiment 2

[0097] Triclosan recovery test in river water using triclosan carbon nanotubes. Add 100 mg of triclosan carbon nanotubes to 100 mL of spiked (0.1, 0.3, 0.5 ug / L) river water for extraction. The mixture was shaken on a shaker for 30 min, centrifuged at 4000 r / min for 5 min, and the supernatant was discarded. Add 40mL methanol / acetic acid (9:1, v:v) to the above centrifuge tube, shake and elute for 12h, centrifuge at 4000r / min for 5min, collect the supernatant, pass through a 0.22μm filter membrane and transfer to another centrifuge tube middle. Blow the eluent to near dryness with nitrogen at room temperature, add 1.0 mL of methanol to dissolve, sample 60 μL, and inject it into high-performance liquid chromatography for determination.

[0098] The measurement results are shown in Table 1.

Embodiment 3

[0100] Triclosan recovery rate test in lake water using triclosan carbon nanotubes. Add 100mg triclosan carbon nanotubes to 100mL lake water spiked with standard (0.1, 0.3, 0.5ug / L) for extraction. The mixture was shaken on a shaker for 30 min, centrifuged at 4000 r / min for 5 min, and the supernatant was discarded. Add 40mL methanol / acetic acid (9:1, v:v) to the above centrifuge tube, shake and elute for 12h, centrifuge at 4000r / min for 5min, collect the supernatant, pass through a 0.22μm filter membrane and transfer to another centrifuge tube middle. Blow the eluent to near dryness with nitrogen at room temperature, add 1.0 mL of methanol to dissolve, sample 60 μL, and inject it into high-performance liquid chromatography for determination.

[0101] The measurement results are shown in Table 2.

[0102] Table 1

[0103]

[0104] (RSD is relative standard deviation)

[0105] Table 2

[0106]

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Abstract

The invention relates to a preparation method of a triclosan carbon nano-tube molecule imprinted polymer and a determination method of the content of triclosan applied to daily chemical products. The preparation method comprises the following steps of: firstly, synthesizing a template-functional monomer complex by taking triclosan (2,4,4'-trichloro-2'-hydroxydiphenyl ether) as a template molecule and 3-aminopropyl triethoxysilane as a functional monomer; and synthesizing a triclosan-imprinted carbon nano-tube polymer by using the complex and a silicon-coated carbon nano-tube through a gel-sol method. The triclosan-imprinted carbon nano-tube polymer has selective adsorption capability for triclosan molecules and is capable of directly and selectively extracting triclosan from a practical sample, and the content of triclosan in the practical sample is quantitatively analyzed by using a high performance liquid chromatography through an extracting solution obtained by eluting.

Description

technical field [0001] The invention relates to a preparation method of triclosan carbon nanotube molecularly imprinted polymer and a method for measuring triclosan content in daily chemical products. Background technique [0002] Triclosan (2,4,4'-trichloro-2-hydroxydiphenyl ether, triclosan) is an internationally popular broad-spectrum and highly effective antibacterial agent, widely used in various daily chemical products, pharmaceutical preparations, food additives and other products middle. In the past 30 years, triclosan has been widely added to various personal care products as an antiseptic and antibacterial agent, such as shampoo, soap, toothpaste, etc., as well as daily necessities and footwear. However, triclosan can cause biological poisoning in water or produce polychlorinated dioxins after photocatalytic degradation, which has caused great harm to people's health. The pollution of triclosan has aroused widespread concern, so it is very important to effectivel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/42C08G77/26C08J9/26B01J20/26B01J20/30G01N30/02
Inventor 苏福海王卫华卢春阳马联弟邵明武
Owner NAT INST OF METROLOGY CHINA
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