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Molecular imprinting monolithic column, preparation method and application thereof

A molecular imprinting and monolithic column technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of interference with 8-OHdG separation and analysis, difficulty in qualitative and quantitative analysis, and complicated operation, and achieve high enrichment ability and selectivity. , long service life and simple preparation method

Inactive Publication Date: 2010-04-07
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The C18 extraction column is a general-purpose non-selective material. When processing urine samples, multiple extractions with double columns are required, which is time-consuming, laborious, and complicated to operate.
Using C18 / OH or mixed type extraction column, although the selectivity of the extraction is increased and the extraction operation is simplified, other related components in the urine sample will also be extracted at the same time, which seriously interferes with the separation and analysis of 8-OHdG with a very low content , it is difficult to give and quantify

Method used

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  • Molecular imprinting monolithic column, preparation method and application thereof
  • Molecular imprinting monolithic column, preparation method and application thereof
  • Molecular imprinting monolithic column, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Example 1 Preparation of Molecularly Imprinted Monolithic Column

[0018] The quartz capillary column was activated with NaOH, then rinsed with HCl and double distilled water, dried and filled with 3-(triethoxysilyl)propyl methacrylate to modify the inner wall of the tube.

[0019] 17.5mg of guanosine, 56mg of acrylamide, 56mg of 4-vinylpyridine, 63mg of N,N'-methylenebisacrylamide and 280mg of dodecanol were ultrasonically dissolved in 350mg of dimethyl sulfoxide in a water bath at 50°C. Nitrogen was blown for 10 minutes to remove the oxygen in the mixture, then 2 mg of azobisisobutyronitrile was added, and after ultrasonic mixing, the mixture was used as the molecularly imprinted prepolymer mixture. Then the molecularly imprinted prepolymer mixture was poured into a capillary column modified with 3-(triethoxysilyl)propyl methacrylate, sealed with silicone rubber, polymerized at a constant temperature of 60° C., and reacted for 18 hours. After the reaction is finished...

Embodiment 2

[0020] Example 2 Preparation of Molecularly Imprinted Monolithic Column

[0021] In the same manner as in Example 1, the inner wall of the quartz capillary was modified with 3-(triethoxysilyl)propyl methacrylate. 17.5mg of guanosine, 55mg of acrylamide, 48mg of 4-vinylpyridine, 62mg of N,N'-methylenebisacrylamide and 275mg of dodecanol were ultrasonically dissolved in 355mg of dimethyl sulfoxide in a water bath at 40°C. Nitrogen gas was blown in for 5 minutes to remove oxygen in the mixture, and then 1.9 mg of azobisisobutyronitrile was added, mixed uniformly by ultrasonic to serve as a molecularly imprinted prepolymer mixed solution. Then the molecularly imprinted prepolymer mixture was poured into a capillary column modified with 3-(triethoxysilyl)propyl methacrylate, sealed with silicone rubber, polymerized at a constant temperature of 55° C., and reacted for 22 hours. After the reaction, the mixed solution of acetonitrile (3mL), methanol and acetic acid (volume ratio of m...

Embodiment 3

[0022] Example 3 Preparation of Molecularly Imprinted Monolithic Column

[0023] In the same manner as in Example 1, the inner wall of the quartz capillary was modified with 3-(trimethoxysilyl)propyl methacrylate. 17.5mg of guanosine, 58mg of acrylamide, 56mg of 4-vinylpyridine, 64mg of N,N'-methylenebisacrylamide and 285mg of dodecanol were ultrasonically dissolved in 360mg of dimethylsulfoxide in a water bath at 50°C. Nitrogen gas was blown in for 5 minutes to remove oxygen in the mixture, and then 2.2 mg of azobisisobutyronitrile was added, mixed uniformly, and then used as a molecularly imprinted prepolymer mixed solution. The molecularly imprinted prepolymer mixture was poured into a capillary column modified with 3-(trimethoxysilyl)propyl methacrylate, sealed with silicone rubber, polymerized at a constant temperature of 60° C., and reacted for 16 hours. After the reaction, the mixed solution of acetonitrile (3mL), methanol and acetic acid (4mL, wherein the volume ratio...

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Abstract

The invention discloses a molecular imprinting monolithic column, a preparation method and application thereof. The molecular imprinting monolithic column comprises a quartz capillary tube and a molecularly imprinted polymer in the quartz capillary tube. Guanosine is used as template molecules. The method comprises the following steps: Guanosine, acrylamide, 4-vinyl pyridine, N,N'-methylene-bisacrylamide and dodecyl alcohol are dissolved in dimethyl suloxide by a water-bath method and an ultrasonic technique at the temperature of 40-50 DEG C, and deoxidized, then azodiisobutyronitrile is added into the dissolved solution to mix uniformly, wherein the mass ratio of guanosine, acrylamide, 4-vinyl pyridine, N,N'-methylene-bisacrylamide, dodecyl alcohol, dimethyl suloxide and azodiisobutyronitrile is 17.5:55-58:48-56:62-64:275-285:350-360:1.8-2.2, and at last polymerization is carried out at a constant temperature of 55-60 DEG C for 16-20 hours in the quartz capillary tube modified by 3-(triethoxylsilane) propyl metacrylic acid ester or 3-(trimethylsiyl) propyl metacrylic acid ester to prepare the finished product. The molecular imprinting monolithic column is used for extracting 8-hydroxyl desoxyguanosine and guanosine with higher beneficiation ability and selectivity.

Description

technical field [0001] The present invention relates to a molecularly imprinted monolithic column and its preparation method and application, in particular to a molecularly imprinted monolithic column using guanosine as a template molecule and its preparation method, the molecularly imprinted monolithic column is used for extraction and enrichment of 8 - Hydroxydeoxyguanosine and Guanosine. Background technique [0002] 8-Hydroxydeoxyguanosine (8-hydroxydeoxyguanosine, 8-OHdG) is an adduct produced by DNA oxidative damage, and it is also a biomarker that sensitively and effectively marks DNA oxidative damage. It refers to the oxidative adducts produced by oxidative damage to DNA caused by a large number of active oxygen free radicals produced in the body under the influence of chemical substances, ionizing radiation, smoking and air pollution. When the error is repaired, it will cause gene mutation, and if this mutation occurs in the expression sequence of the functional gr...

Claims

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Application Information

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IPC IPC(8): B01J20/285C08F220/54C08F226/06C08F220/56C08F2/44B01J20/30
Inventor 张少文吴采樱邢钧蔡凌霜
Owner WUHAN UNIV
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