A kind of pH-responsive vitamin E drug-loaded material and its preparation method and application
A vitamin and responsive technology, applied in pharmaceutical formulations, medical preparations with non-active ingredients, and medical preparations containing active ingredients, etc., can solve the problem of no patent application, etc. The effect of simple processing and preparation methods
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Embodiment 1
[0035] The synthesis of embodiment 1 polymer
[0036] Step (1) terminal allyl polyoxyethylene-co-polycaprolactone polymer (APEG n -PCL m ) preparation
[0037] Allyl polyether (APEG 2.37g, 1.19mmol) was placed in a 100mL round-bottomed flask, and vacuum-dried in a drying oven at 80°C for 4 hours, and then ε-caprolactone (ε-PCL, 7.0g, 61.4 mmol) into the round-bottomed flask, then placed in the oil bath of a magnetic heating stirrer, the system was heated to 100°C, sealed and filled with nitrogen to remove oxygen for 30min, dripped with 44mg of stannous octoate, and heated to 120°C , sealed and reacted for 12 hours, the reaction was completed, cooled to room temperature, dissolved with 6mL of dichloromethane, the reaction system was precipitated twice with 100mL of ice anhydrous ether, filtered with suction, and dried in vacuum at 25°C to obtain allyl-terminated polyoxyethylene-co- -Polycaprolactone polymer (APEG n -PCL m , 8.9g),
[0038] Determination by NMR 1 H NMR sp...
Embodiment 2
[0044] The molecular weight of embodiment 2 polymer
[0045] The PL-GPC 220 gel chromatograph (GPC) of Agilent Company was used, and the test conditions were as follows: THF was used as the mobile phase, the flow rate of the mobile phase was 1.0 mL / min, polystyrene was used as the calibration standard, and the column temperature was 40°C. Get polymer 6mg and be mixed with the solution of 2mg / mL with THF, the molecular weight Mn of raw material and product and distribution PD thereof have been characterized by GPC, from figure 2 It can be clearly seen that the molecular weight of APEG increases significantly, indicating that the ring-opening polymerization is successful and the corresponding product is obtained.
Embodiment 3
[0046] Embodiment 3 dialysis method prepares polymer micelle solution
[0047] 100mg polymer Me 2 N-PEGn-PCLm was dissolved in 6mL tetrahydrofuran, and magnetically stirred at room temperature for 5h. Then, 12 mL of distilled water was slowly dropped into the solution system with a constant pressure dropping funnel, and the dropping speed was controlled to be 20 seconds / drop. After the dropping was completed, the solution was left open and stirred at room temperature for 5 hours. Transfer the mixed solution to a dialysis bag (molecular weight cut-off: Mw 2000Da), change the water every four hours, and dialyze for 24 hours (remove the solvent THF). The liquid in the dialysis bag was collected, and the large particle aggregate was filtered with a 0.45 μm aqueous phase filter membrane to obtain a polymer micelle solution.
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