京尼平交联制备壳聚糖微球工艺优化与分析

Optimization and analysis for the preparation of genipin crosslinked chitosan microspheres

利用反相悬浮-交联法,以京尼平为交联剂,在单因素实验的基础上,通过正交实验优化了壳聚糖微球的制备工艺,确定最佳工艺条件为:乙酸浓度质量分数2%,壳聚糖乙酸液浓度30 g/L,京尼平用量30%(m_(京尼平)/m_(壳聚糖)),反应温度35℃,交联时间2 h,水相Tween-20用量20 g/L,搅拌速率600 r/min。利用扫描电镜、红外光谱、X-射线衍射仪及粒度分析仪对此条件下制得的微球进行表征,结果表明:壳聚糖与京尼平发生了化学交联,微球主要以无定形结构存在,表面光滑、圆整,粘连程度较小,粒径呈正态分布,中值径D_(50)为34.6μm。

Chitosan microspheres were fabricated with genipin as crosslinker by reverse phase suspension- crosslinking method. To optimize the preparation process, the orthogonal experiment was adopted on the basis of single factor experiments. The optimal preparation conditions were as follows： acetic acid solution concentration 2 % （wt. % ）, chitosan concentration in acetic acid solution 3 % （w/v）, the dosage of genipin 30 % （mgenipin/mchitosan ）, crosslinking temperature 35 ℃, crosslinking time 2 h, the dosage of Tween-20 （w/v）, stirring speed 600 r/min. The microspheres fabricated under the optimal preparation conditions were characterized by scanning electron microscope （SEM）, Fourier transform infrared spectrometer （FTIR） , X-ray dffractometer （XRD） , laser diffraction particle size analyzer. SEM indicated the spherical shape with smooth surface of chitosan microspheres. FITR and XRD confirmed chemical crosslinking of genipin with chitosan and the amorphous state of chitosan microspheres. The optimized microspheres with a D50 of 34.6 μm showed a normal size distribution.