化工学报 ›› 2020, Vol. 71 ›› Issue (6): 2768-2779.DOI: 10.11949/0438-1157.20200049
收稿日期:
2020-01-14
修回日期:
2020-03-26
出版日期:
2020-06-05
发布日期:
2020-06-05
通讯作者:
王丹
作者简介:
田济阳(1993—),男,硕士研究生,基金资助:
Jiyang TIAN1,2(),Yuanzuo ZOU1,2,Yuan PU2,Dan WANG1,2()
Received:
2020-01-14
Revised:
2020-03-26
Online:
2020-06-05
Published:
2020-06-05
Contact:
Dan WANG
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。
中图分类号:
田济阳, 邹源佐, 蒲源, 王丹. 亚临界水耦合冷冻干燥法制备芹菜素纳米分散体[J]. 化工学报, 2020, 71(6): 2768-2779.
Jiyang TIAN, Yuanzuo ZOU, Yuan PU, Dan WANG. Preparation of apigenin nanoparticles by combining subcritical water technology with freeze-drying processing[J]. CIESC Journal, 2020, 71(6): 2768-2779.
图2 亚临界水法制备芹菜素纳米颗粒实验装置1—加热套;2—高温高压反应釜;3—搅拌桨;4—过滤器;5—热电偶;6—样品收集装置;7—取样控制阀门;8—反应温度、搅拌转速、反应压力控制及检测系统;9—泄压阀门;10—压力表;11—搅拌电机;12—高精度高压泵出气控制阀门;13—高压高精度柱塞泵;14—高精度高压泵进气控制阀门;15—氮气气瓶
Fig.2 Schematic diagram of apigenin nanoparticles preparation by using SBCW method
图12 芹菜素原料药与制备的纳米颗粒红外分析对比图
Fig.12 FTIR spectra of the raw materials and apigenin nanoparticlesa—raw; b—apigenin nanoparticles; c—apigenin nanoparticles with γ-cyclooctapentylose
图13 芹菜素原料药与制备的纳米颗粒XRD谱图
Fig.13 XRD patterns of raw materials and apigenin nanoparticlesa—raw; b—apigenin nanoparticles; c—apigenin nanoparticles with γ-cyclooctapentylose
图14 芹菜素原料药与制备的纳米颗粒紫外可见吸收光谱对比图
Fig.14 UV-Vis spectra of raw materials and apigenin nanoparticlesa—raw; b—apigenin nanoparticles; c—apigenin nanoparticles with γ-cyclooctapentylose
图15 芹菜素原料药与制备的纳米颗粒质谱对比图
Fig.15 Mass spectra of raw and apigenin nanoparticlesa—raw; b—apigenin nanoparticles; c—apigenin nanoparticles with γ-cyclooctapentylose
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