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Temperature sensitive MPC-b-NIPAM biblock star type polymer for vessel embolism material and preparation method and application

A kind of vascular embolism, di-block technology, applied in the preparation of vascular embolism materials, temperature-sensitive MPC-b-NIPAM di-block star copolymer field, can solve the problems of copolymer dehydration, severe, etc., achieve fast transformation speed, The effect of regular structure, good water retention and biocompatibility

Inactive Publication Date: 2007-10-17
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Recently, Liu et al. [3] The HEMA-b-NIPAM diblock star-shaped three-arm copolymer was prepared by ATRP technology. Although the molecular structure was controlled, the copolymer dehydrated very seriously after phase transition, and its biocompatibility needed to be further improved.

Method used

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  • Temperature sensitive MPC-b-NIPAM biblock star type polymer for vessel embolism material and preparation method and application
  • Temperature sensitive MPC-b-NIPAM biblock star type polymer for vessel embolism material and preparation method and application
  • Temperature sensitive MPC-b-NIPAM biblock star type polymer for vessel embolism material and preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The first step, the preparation of initiator three (2-bromoisobutyryloxy) ethylamine (TrisE), process is as follows:

[0031] Add 5.0 g of sodium hydroxide to 5.0 g (33.5 mmol) of triethanolamine before the reaction, and let stand for three days to remove water. Dissolve 5.0g (33.5mmol) of triethanolamine (33.5mmol) and 60ml of triethylamine after dehydration in 200ml of tetrahydrofuran in a round-bottomed flask, and simultaneously dissolve 45.98g (24.7ml, 0.20mol) of bromoisobutyryl bromide in 100ml of tetrahydrofuran, and then added to the dropping funnel, and added dropwise into the above-mentioned round-bottomed flask (0° C. ice-water bath) within 1 h under controlled addition rate, and continued to stir for 2 h. The ammonium salt was removed by filtration, the reactant was vacuum-dried at 30° C., and the dried product was washed with 0.1 mol / L sodium carbonate. It was extracted three more times with dichloromethane, then dried over magnesium sulfate. The solvent ...

Embodiment 2

[0041] The synthesis steps of the initiator TrisE and the macromolecular initiator PMPC-Br are the same as those in Example 1.

[0042] Only change the addition amount of NIPAM to be 3.2590 (28.8mmol) in the third step reaction, make P(I-(MPC 10 -b-NIPAM 160 ) 3 ) copolymer.

[0043] Proton NMR spectrum detection: Weigh 15mg P(I-(MPC 10 -b-NIPAM 160 ) 3 ) sample dissolved in deuterated water (D 2 O) in, record on NMR spectrometer Varian UNITY plus 400 1 H-NMR spectrum, as shown in Figure 1 and Figure 2.

[0044] Infrared spectrum detection: the application of Bio-Rad FTS 6000 Fourier Transform Infrared Spectrometer to determine MPC homopolymer and P(I-(MPC with a copolymerization ratio of 1:16 10 -b-NIPAM 160 ) 3 ) infrared spectrogram of the copolymer sample, as shown in Figure 3.

[0045] Rheological performance test: the instrument used is a rotational rheometer RELOGICA INSTRUMRENTS AB. For 5%P(I-(MPC 10 -b-NIPAM 160 ) 3 ) sample using Bob-Cup 25 abrasive to...

Embodiment 3

[0047] The synthesis steps of the initiator TrisE and the macromolecular initiator PMPC-Br are the same as those in Example 1.

[0048] In the third step reaction, only changing the addition of NIPAM is 1.6295g (14.4mmol) to make P(I-(MPC 10 -b-NIPAM 80 ) 3 ) copolymer.

[0049] Proton NMR spectrum detection: Weigh 15mg P(I-(MPC 10 -b-NIPAM 80 ) 3 ) sample dissolved in deuterated water (D 2 O) in, record on NMR spectrometer Varian UNITY plus 400 1 H-NMR spectrum, as shown in Figure 1 and Figure 2.

[0050] Infrared spectrum detection: the application of the instrument Bio-Rad FTS 6000 Fourier transform infrared spectrometer to measure the P(I-(MPC with a copolymerization ratio of 1:8 10 -b-NIPAM 80 ) 3 ) infrared spectrogram of the copolymer sample, as shown in Figure 3.

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Abstract

The invention discloses a thermo sensitive MPC-b-NIPAM star-type diblock copolymer for blood vessel embolic materials, preparation method and application thereof, belongs to preparation technic of blood vessel embolic materials of biomedical engineering field. The copolymer formula is showed as formula 1. The preparation process comprises synthesis of TrisE, PMPC-Br, MPC-b-NIPAM. The copolymer aqueous solution is used for blood vessel embolic materials. The invention is characterized in that regular polymer molecule structure by means of ATRP, the copolymer LCST approaches to human body temperature, and has advantages of fast response function, good water-retention property and biocompatibility and so on.

Description

technical field [0001] The invention relates to a thermosensitive MPC-b-NIPAM diblock star copolymer used for vascular embolic materials, a preparation method and application thereof, and belongs to the preparation technology of vascular embolic materials in the field of biomedical engineering. Background technique [0002] At present, the most commonly used embolic agent in the field of endovascular embolization is n-butylcyanoacrylate (NBCA). It brings great inconvenience, and many shortcomings limit its wide application. Non-adhesive liquid embolic agents have good operability and promising application prospects due to their non-adhesive tubes. Unfortunately, most non-adhesive embolic agents use dimethyl sulfoxide (DMSO) as a solvent. Recently, more and more The study found that DMSO has strong vascular toxicity, which can cause acute vasospasm, injury and necrosis, especially when the dose is too large, the injection speed is too fast and the concentration is too high. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61L31/10C08F220/56C08F230/02C08F4/06C08F2/44
Inventor 刘文广高鹏赵晓丽
Owner TIANJIN UNIV
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