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Minoxidil molecularly imprinted polymer, preparation method of minoxidil molecularly imprinted polymer, minoxidil solid-phase extraction column and method for separating and purifying minoxidil

A technology of molecular imprinting and polymers, which is applied in separation methods, solid adsorbent liquid separation, and other chemical processes, can solve the problems of sample interference and complex operation of processing methods, and achieve the effects of reducing interference, improving purity, and facilitating implementation

Inactive Publication Date: 2017-05-10
新疆维吾尔自治区分析测试研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention provides a minoxidil molecularly imprinted polymer and a preparation method thereof. The minoxidil molecularly imprinted polymer obtained according to the method of the present invention has a relatively high affinity for minoxidil. The present invention also provides A minoxidil solid-phase extraction column and a method for extracting, separating and purifying minoxidil using the minoxidil solid-phase extraction column are disclosed, and the minoxidil solid-phase extraction column is used to extract, separate and purify rice The method of Nordil effectively solves the problems of complex operation and large sample interference in the determination of minoxidil in the hair growth products containing minoxidil currently available on the market

Method used

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  • Minoxidil molecularly imprinted polymer, preparation method of minoxidil molecularly imprinted polymer, minoxidil solid-phase extraction column and method for separating and purifying minoxidil

Examples

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Effect test

Embodiment 1

[0033] Example 1, the minoxidil molecularly imprinted polymer is obtained according to the following preparation method:

[0034] The first step is to reflux clean the spherical silica gel with inorganic acid for 18 hours to 24 hours to obtain activated silica gel, then wash the activated silica gel with water until it is neutral, and then dry it to constant weight. Among them, the inorganic acid and spherical silica gel The mass ratio is 5:1 to 10:1, and the spherical silica gel is 300 mesh to 400 mesh spherical silica gel;

[0035] The second step is to disperse 1 part of activated silica gel in 10 to 25 parts of organic reagent I in parts by weight to obtain a silica gel dispersion solution, and then add 3-aminopropyltriethoxysilane to spherical silica gel Carry out silanization, the reaction condition of silanization is 110°C to 150°C under nitrogen atmosphere for 18 hours to 24 hours, the mass ratio of spherical silica gel to 3-aminopropyltriethoxysilane is 1:1 to 1:1.5, ...

Embodiment 2

[0041] Example 2, the minoxidil molecularly imprinted polymer is obtained according to the following preparation method: first, the spherical silica gel is first reflux cleaned with inorganic acid for 18 hours or 24 hours to obtain the activated silica gel, and then the activated silica gel is purified with water. The silica gel is washed to neutral and then dried to constant weight, wherein the mass ratio of inorganic acid to spherical silica gel is 5:1 or 10:1, and the spherical silica gel is 300 mesh or 400 mesh spherical silica gel;

[0042] The second step is to disperse 1 part of activated silica gel in 10 parts or 25 parts of organic reagent I in parts by weight to obtain a silica gel dispersion solution, and then add 3-aminopropyltriethoxysilane to spherical silica gel For silanization, the reaction conditions for silanization are 110°C or 150°C under nitrogen atmosphere for 18 hours or 24 hours, the mass ratio of spherical silica gel to 3-aminopropyltriethoxysilane is ...

Embodiment 3

[0048] Example 3, as an optimization of the above examples, the polymerization in the fifth step adopts thermal initiation polymerization, the temperature of thermal initiation polymerization is 60°C to 90°C, and the polymerization reaction time is 6 hours to 48 hours; or, in the fifth step The polymerization adopts photoinitiated polymerization, and the conditions of photoinitiated polymerization are: the power of the high-pressure mercury lamp is 125W or 150W, and the polymerization time is 0.5 hours to 48 hours.

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Abstract

The invention relates to the technical field of minoxidil detection and discloses a minoxidil molecularly imprinted polymer, a preparation method of the minoxidil molecularly imprinted polymer, a minoxidil solid-phase extraction column and a method for separating and purifying minoxidil by using the minoxidil solid-phase extraction column. The minoxidil molecularly imprinted polymer obtained by the method disclosed by the invention has relatively high affinity on minoxidil. The method for extracting, separating and purifying minoxidil is performed by using the minoxidil solid-phase extraction column prepared by the minoxidil molecularly imprinted polymer disclosed by the invention, so that the pretreatment means of measuring minoxidil in commercially available minoxidil-containing hair growth products is simple and convenient to implement. Moreover, to-be-detected samples are separated and purified by adopting the minoxidil molecularly imprinted polymer with relatively high affinity on minoxidil, the purity of the to-be-detected samples is effectively improved, and the interference on the samples in the process of measuring the to-be-detected samples by high performance liquid chromatography is effectively reduced.

Description

technical field [0001] The invention relates to the technical field of minoxidil detection, and relates to a minoxidil molecularly imprinted polymer and a preparation method thereof, a minoxidil solid-phase extraction column and the use of the minoxidil solid-phase extraction to separate and purify minoxidil Er's method. Background technique [0002] Minoxidil is a potassium channel opener developed in the 1970s and is mainly used for the treatment of resistant hypertension. Minoxidil is a type II 5a reductase inhibitor. Because minoxidil was found to have the effect of making hair longer and thicker in the treatment of high blood pressure, it is currently being developed and applied as a topical drug for the treatment of male baldness. So far, the mechanism by which minoxidil induces hair growth has not been fully explained and is thought to involve multiple pathways. In 1988, the U.S. FDA approved minoxidil for the treatment of male androgenetic alopecia. With the impr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/56C08F220/58C08F226/06C08F220/06C08F220/24C08F220/14C08F220/28C08F220/34C08F222/14C08F222/38C08F212/36C08J9/26B01D15/22B01J20/26B01J20/30C07D239/50
CPCB01D15/22B01J20/268C07D239/50C08F212/36C08F220/06C08F220/14C08F220/24C08F220/28C08F220/281C08F220/34C08F220/56C08F220/58C08F220/585C08F222/1006C08F222/103C08F222/385C08F226/06C08J9/26C08J2201/0424
Inventor 韩飞王苗苗宋良辉李慕春
Owner 新疆维吾尔自治区分析测试研究院