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Method for preparing estrogen substitution template molecular imprinting solid phase micro extraction head

A technology that replaces templates and molecular imprinting, applied in the field of analysis and detection, can solve the problems of leakage, difficult elution, affecting the measurement accuracy, etc., and achieve the effect of avoiding leakage interference, large adsorption capacity, and good identification performance.

Inactive Publication Date: 2013-01-23
NANJING MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0006] In order to overcome the above problems, the present invention provides a method for preparing an estrogen-substituting template molecularly imprinted solid-phase microextraction head. The prepared extraction head solves the problem that the above-mentioned template molecules are not easy to elute and completely cause leakage, which affects the measurement accuracy.

Method used

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  • Method for preparing estrogen substitution template molecular imprinting solid phase micro extraction head
  • Method for preparing estrogen substitution template molecular imprinting solid phase micro extraction head
  • Method for preparing estrogen substitution template molecular imprinting solid phase micro extraction head

Examples

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Embodiment 1

[0038] Quartz fiber (200 μm in diameter, 3 cm in length, Nanjing Feidis Fiber Mechatronic Engineering Manufacturing Center) was first soaked in acetone for 1 h to remove the protective layer, then soaked in 1 mol / L sodium hydroxide for 1 h, 0.1 mol / L hydrochloric acid Soak in water for 1 hour, wash with deionized water to remove residual acid on the surface until neutral, vacuum dry and activate at 70°C for 2 hours, and place it in γ-methacryloxypropyltrimethoxysilane with a concentration of 10% by mass after drying Silanize in acetone solution for 1.5 h, wash the remaining reaction solution on the surface with methanol, and blow dry with nitrogen gas for later use.

[0039] Mix 0.5mmol 17-ethylestradiol and 156mg trifluoromethacrylic acid in 40mL toluene, pre-polymerize for 6h, then add 119μL 4-vinylpyridine (the amount of trifluoromethacrylic acid and 4-vinylpyridine in moles ratio of 1:1), and pre-polymerize again after mixing for 6 hours, add 398.6 μL ethylene glycol dimet...

Embodiment 2

[0041] Quartz fibers (100 μm in diameter and 4 cm in length) were first soaked in acetone for 1 hour, then in 1 mol / L sodium hydroxide for 1 hour, in 0.1 mol / L hydrochloric acid for 1 hour, and washed with deionized water to remove residual acid on the surface. Activation by vacuum drying at 70°C for 2 hours, after drying, put it in 20% γ-methacryloxypropyltrimethoxysilane acetone solution for silanization for 2 hours, and wash the remaining reaction solution on the surface with methanol Afterwards, blow dry with nitrogen gas for later use.

[0042] Mix 0.5mmol 17-ethylestradiol and 156mg trifluoromethacrylic acid in 40mL methanol, prepolymerize for 6h, then add 119μL 4-vinylpyridine, mix well, prepolymerize again for 6h, add 398.6μL ethylene glycol Dimethacrylate and 30mg azobisisobutyronitrile (making the mol ratio of the replacement template molecule, functional monomer and crosslinking agent be 1:4:4, the molar weight of the initiator is 15% of the replacement template mol...

Embodiment 3

[0044] Quartz fibers (200 μm in diameter and 4 cm in length) were first soaked in acetone for 1 hour, then in 1 mol / L sodium hydroxide for 1 hour, in 0.1 mol / L hydrochloric acid for 1 hour, and washed with deionized water to remove residual acid on the surface. Reaction, vacuum drying and activation at 70°C for 2 hours, after drying, put it in a solution of γ-methacryloxypropyltrimethoxysilane acetone with a mass percent concentration of 30% for silanization for 1.5 hours, and wash the residual reaction on the surface with methanol After liquid, blow dry with nitrogen gas for later use.

[0045] Mix 0.5mmol 17-ethylestradiol and 312mg trifluoromethacrylic acid in 40mL toluene, pre-polymerize for 6h, then add 238μL 4-vinylpyridine, mix for another 6h, add 1.6mL ethylene glycol Dimethacrylate and 30mg azobisisobutyronitrile (the molar ratio of the substitute template molecule, functional monomer and crosslinking agent is 1:8:8, and the molar amount of the initiator is 15% of the...

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Abstract

The invention provides a method for preparing an estrogen substitution template molecular imprinting solid phase micro extraction head. The method comprises the following steps of: a, treating and silanizing the surface of a quartz fiber; b, prepolymerizing a template molecule and a functional monomer in a perforating agent, adding a cross-linking agent and an initiator, placing into the silanized quartz fiber, ultrasonically removing oxygen, and polymerizing under the condition of nitrogen at the temperature of 55 to 60 DEG C for 6 to 12 hours; and c, aging the quartz fiber for at least one hour and diluting the template molecule by using methanol or acetic acid solution. The solid phase micro extraction head prepared by the method has special identification capability to estrogen internal secretion chaff interferent, so the problem that the template is leaked can be solved; and when the solid phase micro extraction head is applied to testing an actual sample, the accuracy of the method can be improved. After reuse, a coating layer is free from breakage and falling. The substitution template molecular imprinting solid phase micro extraction head is linked with a color spectrum soas to be used for separating and gathering estrogen internal secretion chaff interferent in complicated base materials such as environmental samples, food, biological samples and the like.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to a method for preparing an estrogen-substituting template molecularly imprinted solid-phase microextraction head. The prepared extraction head has the characteristics of high exclusive selectivity and good practicability. Background technique [0002] After the destruction of the ozone layer and global warming, environmental estrogen (EEs) pollution has become the third major environmental problem for human beings, and has been hailed as a time bomb that threatens the survival of human beings. EEs are a class of compounds with estrogen-like effects, which are widely distributed and diverse, and with the process of industrialization, the pollution of EEs has a tendency to further expand, which not only becomes a potential threat to human health, but also threatens the biological race. Survival. Since the 1990s, the influence of environmental estrogen on ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/08C03C25/00C08F226/06C08F220/04C08J9/28
Inventor 周学敏吴晓丽李芸王舒文婷婷王若禹李飞张军
Owner NANJING MEDICAL UNIV
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