Preparation method of amphipathic hydroxyethyl starch-grafted polylactic acid nano-micelle
A technology of hydroxyethyl starch and nano micelles is applied in the fields of chemistry and medicine, and achieves the effects of good biocompatibility, uniform distribution, and simple and easy synthesis method.
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Embodiment 1
[0041] At room temperature, dissolve 3g of hydroxyethyl starch (130 / 0.4) in 30ml of DMSO until it becomes clear and transparent, and add a hydroxyl protecting agent (32.28g of hexamethyldisilazane or 1.09g of trimethylchlorosilane) under nitrogen protection. React at 60° C. for 24 hours to form a reaction liquid. The above reaction solution was added to methanol for precipitation, washed, and dried in a vacuum oven. The hydroxyethyl starch with partially protected hydroxyl groups was obtained as a white solid.
[0042] Under the protection of nitrogen, the hydroxyethyl starch powder whose hydroxyl groups are partially protected is dissolved in 20ml of toluene, and after it is completely dissolved at 80°C, a total content of 5% of the catalyst stannous octoate and lactide is added to make the hydroxyethyl starch unit sugar ring The molar ratio to lactide was kept at 1:4, stirred at 110° C. for 24 hours, and dried by rotary evaporation to obtain a crude product.
[0043] The c...
Embodiment 2
[0047] Based on the conditions of Example 1, the molar ratio of hydroxyethyl starch unit sugar rings to lactide was changed to 1:7. The proton NMR spectrum of the product is shown in image 3 The spectrum in C. According to the data calculation of spectrogram C, the average degree of polymerization of grafted polylactic acid in the HES-g-PLA copolymer is 7.6 (abbreviated as HES-g-PLA 7.6 ). The transmission electron micrographs of the nanomicelles prepared by this copolymer are shown in Figure 4 B, the particle size is 97nm.
Embodiment 3
[0049] Based on the conditions of Example 1, the molar ratio of hydroxyethyl starch unit sugar ring to lactide was changed to 1:15. The proton NMR spectrum of the product is shown in image 3 The spectrum in D. According to the data calculation of spectrogram D, the average degree of polymerization of grafted polylactic acid in the HES-g-PLA copolymer is 23.9 (abbreviated as HES-g-PLA 23.9 ). The transmission electron micrographs of the nanomicelles prepared by this copolymer are shown in Figure 4 B, the particle size is 65nm.
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