亚临界水耦合冷冻干燥法制备芹菜素纳米分散体  

Preparation of apigenin nanoparticles by combining subcritical water technology with freeze-drying processing

作　　者：田济阳 邹源佐 蒲源 王丹[1,2] TIAN Jiyang;ZOU Yuanzuo;PU Yuan;WANG Dan(State Key Laboratory of Organic-Inorganic Composites,Beijing University of Chemical Technology,Beijing 100029,China;Research Center of the Ministry of Education for High Gravity Engineering and Technology,Beijing University of Chemical Technology,Beijing 100029,China)

机构地区：[1]北京化工大学有机无机复合材料国家重点实验室,北京100029 [2]北京化工大学教育部超重力工程研究中心,北京100029

出　　处：《化工学报》2020年第6期2768-2779,共12页CIESC Journal

基　　金：国家自然科学基金项目(21808009)。

摘　　要：在溶剂(亚临界水)-反溶剂(去离子水)体系下,利用溶剂反溶剂沉淀耦合冷冻干燥法,对芹菜素原料药进行了纳米化及改性,制备出了超细芹菜素颗粒及其水相分散体。系统地探究了反溶剂温度、亚临界水温度、反应压力、表面活性剂种类与浓度对造粒过程产生的影响,并通过扫描电子显微镜(SEM)、红外吸收光谱(FTIR)、X射线衍射(XRD)、质谱分析(MS)等手段对原料药和产物进行了对比分析。结果表明,当反溶剂温度为0℃,亚临界水温度为160℃、反应压力为5 MPa、表面活性剂γ-环糊精的质量分数为5%时,可得到粒径在20~30 nm范围内,分布均匀,稳定程度较高且具有较低结晶度的纳米颗粒。本文报道的芹菜素纳米颗粒制备方法,全程无有机溶剂参与,易于生物医用推广,为基于芹菜素的口服药物设计与开发提供了参考。Under the system of solvent(subcritical water)-antisolvent(deionized water),based on the combination of subcritical water technology and freeze-drying processing,we prepared apigenin nanoparticles by nanocrystallization and modification.The study comprehensively explores the influencing factors,including the temperature of desolvation,the temperature of subcritical water,the pressure of reaction system,and surfactant concentration in the process of the granulation.The study compares raw materials and products through scanning electronic microscopy(SEM),Fourier transform infrared spectrophotometry(FTIR),X-ray diffraction(XRD)and mass spectrometry(MS).The results show that when the antisolvent temperature is 0℃,the subcritical water temperature is 160℃,the reaction pressure is 5 MPa,and the surfactantγ-cyclodextrin mass fraction is 5%,the particle size can be obtained at range 20—30 nm,the nanoparticles are evenly distributed,with high stability and low crystallinity.The preparation method of apigenin nanoparticles reported in this article,without the participation of organic solvents in the whole process, is easy for biomedical promotion, and provides a reference for the designand development of oral drugs based on apigenin.

关 键 词：芹菜素 亚临界水 反溶剂 造粒 绿色制备 纳米颗粒 

分 类 号：TQ460.62[化学工程—制药化工]