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Preparation method of surface molecularly imprinted polymer of PN (pneumocandins)B0

A technology of surface molecular imprinting and neomocontin, which is applied in the fields of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., can solve problems such as complex extraction and purification processes, achieve simple industrial production, and improve purity and content, high selectivity effect

Inactive Publication Date: 2015-11-18
SHIHEZI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of this invention is to provide a novel PNB 0 The method of separation and purification adopts surface molecular imprinting technology to prepare PNB 0 As template molecular imprinting material, used for PNB in ​​fermentation broth 0 Separation and purification, which overcomes the PNB present in the prior art 0 Extraction and purification of complex defects, effective for PNB 0 Enrichment and purification, improve its purity and content, and make its industrial production easier to prepare PNB by surface molecular imprinting method 0 Surface molecularly imprinted polymer (MIP-PMAA / SiO 2 ) preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Example 1: PNB 0 Synthesis of Molecularly Imprinted Materials

[0012] The first step: take 300kgSiO2 2 Place in 1500kg of nitric acid aqueous solution with a concentration of 50%, boil in a reaction kettle for 2 hours, replenish evaporated nitric acid while boiling, let stand for 12 hours, wash with distilled water until neutral, filter with suction and dry in a double-cone rotary vacuum dryer 24h, you can get activated silica gel;

[0013] Step 2: Take 50kg of activated SiO 2 Place in 2000kg ethanol-water (1:1, m / m) solution, add coupling agent MPS50kg, react at 50°C for 24h; Dried in a rotary vacuum dryer for 20 hours for subsequent use;

[0014] Step 3: 30kg MPS-SiO 2 Add 1000kg of purified MAA to 200kg of water, use N 2 Exhaust the air, raise the temperature to 50°C, add 0.6kg of initiator ammonium persulfate, carry out the graft polymerization reaction at constant temperature for 8 hours, raise the temperature to 70°C and continue the graft polymerization re...

Embodiment 2

[0016] Example 2: PNB 0 Synthesis of Molecularly Imprinted Materials

[0017] The first step: take 300kgSiO2 2 Place in 2400kg of nitric acid aqueous solution with a concentration of 60%, boil in a reaction kettle for 3 hours, add evaporated nitric acid while boiling, let stand for 12 hours, wash with distilled water until neutral, filter with suction and dry in a double-cone rotary vacuum dryer 24h, you can get activated silica gel;

[0018] Step 2: Take 50kg of activated SiO 2 Place in 2500kg ethanol-water (1:1, m / m) solution, add coupling agent MPS50kg, react at 50°C for 20h; Dried in a rotary vacuum dryer for 10 hours for subsequent use;

[0019] Step 3: 30kg MPS-SiO 2 And 1000kg of purified MAA was added to 2000kg of water, with N 2 Exhaust the air, raise the temperature to 55°C, add 0.6kg of initiator ammonium persulfate, carry out the graft polymerization reaction at constant temperature for 10 hours, raise the temperature to 70°C and continue the graft polymeriza...

Embodiment 3

[0021] Example 3: PNB 0 Synthesis of Molecularly Imprinted Materials

[0022] The first step: take 300kgSiO2 2 Place in 1800kg of 30% nitric acid aqueous solution, boil in a reaction kettle for 1 hour, replenish evaporated nitric acid while boiling, let stand for 10 hours, wash with distilled water until neutral, filter with suction and dry in a double-cone rotary vacuum dryer 20h, the activated silica gel can be obtained;

[0023] Step 2: Take 50kg of activated SiO 2 Place in 2000kg ethanol-water (1:1, m / m) solution, add coupling agent MPS75kg, react at 45°C for 20h; Dried in a rotary vacuum dryer for 10 hours for subsequent use;

[0024] Step 3: 30kg MPS-SiO 2 And 100kg of purified MAA was added to 2000kg of water, with N 2 Exhaust the air, raise the temperature to 45°C, add 0.6kg of initiator ammonium persulfate, carry out the graft polymerization reaction at a constant temperature for 10 hours, raise the temperature to 65°C and continue the graft polymerization reactio...

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Abstract

The invention relates to a preparation method of a surface molecularly imprinted polymer of PN (pneumocandins)B0. The preparation method comprises the following steps: step 1, SiO2 is taken and placed in a container filled with a strong acid solution, reacts, and is left to stand, washed to neutral with distilled water and dried; step 2, gamma-trimethoxysilyl propyl methacrylate, ethanol and water are added to the substance obtained in the step 1, the mixture reacts, and a product is dried; step 3, water and methacrylic acid are added to the substance obtained in the step 2, N2 is adopted to exhaust air, the temperature is increased, an initiator ammonium persulfate is added, the mixture reacts, and a product is dried; step 4, PNB0, ethanol and ethylene glycol diglycidyl ether are added to the substance obtained in the step 3, pH is regulated, the mixture reacts, PNB0 is removed with a polar solvent, a product is dried, and the PNB0 molecularly imprinted material is prepared. The preparation method adopts a surface molecular imprinting technology and overcomes the defect of complex PNB0 extraction and purification processes in the prior art, the purity of PNB0 is improved, the content of PNB0 is increased, and industrial production of PNB0 is simpler and more convenient.

Description

technical field [0001] The invention relates to a method for preparing pneumocidine B by surface molecular imprinting method 0 (PNB 0 ) surface molecularly imprinted polymer (MIP-PMAA / SiO 2 ) preparation method. Background technique [0002] Pneumocandins (PN) is a new class of cyclic lipopeptide compounds produced by the fermentation of filamentous fungi, in which PNB 0 It is the raw material of the new antifungal compound caspofungin. PNB 0 It exists in the fermentation broth. At present, there is almost no separation process in my country, and most of the PNB is carried out through macroporous resins and chromatographic packing materials. 0 Separation and purification; Lu Liang et al. use centrifugation, solvent extraction and macroporous resin decolorization methods to separate and obtain PNB with ideal purity 0 , but the operation steps are cumbersome and the yield is not high. Researchers from Merck abroad conducted systematic research on it. Due to the by-produ...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08F220/06C08J9/26B01J20/26B01J20/28B01J20/30
Inventor 李迎春张路赵飞浪于锋庞丽娟李乐宋含刘江
Owner SHIHEZI UNIVERSITY
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