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Tsiklomitsin molecular engram integral column preparation method

A molecular imprinting and monolithic column technology, applied in the field of bioengineering, can solve the problems of high false positive and long time consumption, and achieve the effect of fast mass transfer rate, low back pressure and good molecular recognition performance.

Inactive Publication Date: 2008-08-20
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to solve the problem that most conventional detection methods of tetracycline antibiotic residues cannot accurately detect trace antibiotic residues from complex samples, which directly leads to high false positives in rapid detection methods such as ELISA and high false positives in chromatographic methods such as HPLC and GC. For the problem of time-consuming (over 3 days), a preparation method for tetracycline molecularly imprinted polymer monolithic column is provided. This method has simple steps, can avoid cumbersome grinding process, and can obtain imprinted polymer with good molecular recognition performance, which can be directly used as a new liquid phase Chromatographic packing can be used for off-line or on-line solid phase extraction pretreatment, so as to achieve the purpose of removing impurities in complex samples and selectively enriching trace tetracycline antibiotic residues

Method used

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  • Tsiklomitsin molecular engram integral column preparation method
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  • Tsiklomitsin molecular engram integral column preparation method

Examples

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example 1

[0027] First, 0.1 mmol of template molecule tetracycline TC was dissolved in 20 mmol of methanol by ultrasonic, and 0.8 mmol of porogen (cyclohexanol 1.10 g) functional monomer MAA was added to interact for 6 h to form a complex, and then 4 mmol of cross-linking agent EDMA was added. (TC:MAA:EDMA=1:8:40), initiator AIBN 20mg, the solution was ultrasonically degassed for 5-10min, passed nitrogen for deoxygenation for 20min, then the mixture was injected into a 10cm stainless steel column, thermally induced at 60°C Water bath reaction for 12h. The prepared molecularly imprinted monolithic column was connected to a high-pressure infusion pump and washed with methanol and acetonitrile / acetic acid (94:6, v / v) solution to remove porogen and template molecules to obtain polymer 1 (MIP1).

example 2

[0029] A porogen (1.10 g of dodecanol) was added, and others were the same as in Example 1 to obtain MIP2.

example 3

[0031] The porogen (0.20 g of cyclohexanol and 0.90 g of dodecanol) was added, and others were the same as in Example 1 to obtain MIP3.

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Abstract

The invention provides a preparing method of Tetracycline molecular imprinting column. The invention includes the following steps: dissolving template molecular Tetracycline (TC) with ultrasound in methanol, adding functional monomer and pore-forming agent (cyclohexanol and lauryl alcohol), oscillating for 6 hours, adding crosslinking agent (ethylene glycol dimethacrylate) and initiator (azobisisobutyronitrile), after ultrasonic degassing, adding nitrogen for 20 minutes, deoxidizing, pouring the solution into 10cm stainless column with bottom sealed, sealing the top end, putting the column into 60 DEG C water for water bath, after 12 hours, obtaining the molecular imprinting column by heat initiation reaction. Connecting the column to the high-pressure pump for washing away the pore-forming agent and template molecular, in the end the molecular imprinting column with good separation effect is obtained. Compared with traditional bulk polymerization method, the invention has the characteristics of simple preparation for avoiding process of lapping, good molecular recognition ability and so on. The molecular imprinting column provided by the invention is used as a liquid chromatogram filling, and can realize separation, enrichment and purification of Tetracycline antibiotics.

Description

【Technical field】: [0001] The invention belongs to the technical field of bioengineering, and relates to the preparation of a molecularly imprinted monolithic column, in particular to the preparation of a molecularly imprinted monolithic column with specific recognition of tetracycline antibiotics. 【Background technique】: [0002] Tetracyclines (TCs) are a class of broad-spectrum antibiotics produced by Streptomyces. As feed additives, they are used in animal husbandry to prevent, control and treat diseases such as animal and plant diseases and insect pests. The drug residues in the source food pose a potential hazard to human health. Many countries routinely monitor TCs residues. my country stipulates that the maximum residue limit of tetracycline antibiotics in animal-derived food is 0.1 mg / kg. [0003] At present, the detection methods of tetracycline antibiotic residues in agricultural products mainly include: ① Microbial method: the detection has poor specificity, low ...

Claims

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Application Information

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IPC IPC(8): G01N30/56
Inventor 陈朗星孙祥丽何锡文李文友张玉奎
Owner NANKAI UNIV
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