A kind of anti-inflammatory type rapid hemostasis medical glue material and preparation method thereof
A fast, carboxymethyl chitosan technology, applied in the direction of pharmaceutical formulation, application, medical science, etc., can solve the problem of poor hemostatic performance, achieve the effect of improving hemostatic performance, good antibacterial performance, and hemostatic performance
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preparation example 1
[0023] Preparation Example 1 Preparation of n-butyl cyanoacrylate
[0024] This preparation example is used to prepare the required n-butyl cyanoacrylate, and specifically includes the following steps:
[0025] (1) butyl ester transesterification reaction
[0026] CNCH 2 COOC 2 H 5 +C 4 H 9 OH—C 2 H 5 ONa→CNCH 2 COOC 4 H 9 +C 2 H 5 OH
[0027] In a 5L three-neck beaker equipped with a stirrer and a thermometer, put in 1400ml of ethyl cyanoacetate and 1200ml of n-butanol, turn on stirring, condense water, heat up to 40 degrees and above and add 25g of sodium ethoxide; At -82°C, ethanol began to distill. When the internal temperature reached 110°C and the top temperature reached 98-100°C, the heating was stopped and about 680ml of ethanol was collected;
[0028] Cool down to about 50°C inside temperature, turn on heating, change the bottle with vacuum pump to receive n-butanol, the vacuum degree is -0.1MPa, when the inner temperature rises to about 95°C and the top...
preparation example 2
[0038] Preparation Example 2 Preparation of n-octyl cyanoacrylate
[0039] This preparation example is used to prepare the required n-octyl cyanoacrylate, which specifically includes the following steps:
[0040] (1) with step (1) in Preparation Example 1;
[0041] (2) with step (2) in Preparation Example 1;
[0042] (3) Synthesis of n-octyl α-cyanoacrylate
[0043]
[0044]Add 380ml of methanol-formaldehyde solution and 0.95ml of piperidine to a 5L three-necked flask equipped with a stirrer, dropping funnel, condenser and water separator. When the temperature in the flask reaches 40°C and above, start to add cyanoacetic acid dropwise. 750ml of octyl ester, after the dropwise addition, collect methanol until the internal temperature is 120℃; then add 300ml of petroleum ether dropwise, start dehydration, speed up stirring, when the ether water layer in the reflux separator is clarified, the actual water is about 16ml, and the After the water is finished, about 300ml of pe...
Embodiment 1
[0049] The preparation method of the medical glue material for rapid hemostasis described in this embodiment includes the following steps:
[0050] (1) get the above-mentioned n-butyl cyanoacrylate and n-octyl cyanoacrylate according to the mass ratio of 55wt%: 45wt% and fully mix to obtain a medical glue base, for subsequent use;
[0051] (2) take carboxymethyl chitosan and place it with 1-methylimidazolium trifluoroacetate ionic liquid (accounting for 8wt% of the quality of the carboxymethyl chitosan) and corrugated pine juice (with corrugated pine directly Squeeze to obtain juice, accounting for 5wt% of the carboxymethyl chitosan mass) in a closed container, remove air and fill the container with CO 2 , control the temperature in the airtight container to 80°C and the pressure to 8MPa, so that the charged CO 2 The gas is in a supercritical state, and under the condition that the carboxymethyl chitosan is not in contact with the ionic liquid and the anti-inflammatory active...
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