柠檬酸修饰的超顺磁性氧化铁纳米粒的制备及表征

doi:10.3969/j.issn.1671-167X.2018.02.023

北京大学学报(医学版) ›› 2018, Vol. 50 ›› Issue (2): 340-346. doi: 10.3969/j.issn.1671-167X.2018.02.023

柠檬酸修饰的超顺磁性氧化铁纳米粒的制备及表征

王欢1，覃小雅1，李子圆1，郑卓肇2，范田园1△

（1. 北京大学药学院天然及仿生药物国家重点实验室，北京大学药学院分子药剂学与新释药系统北京市重点实验室，北京100191； 2. 北京清华长庚医院核医学科，北京100044）

出版日期:2018-04-18 发布日期:2018-04-18
通讯作者: 范田园 E-mail:tianyuan_fan@bjmu.edu.cn
基金资助:
国家自然科学基金（81571779）资助

Preparation and characterization of citric acid-modified superparamagnetic iron oxide nanoparticles

WANG Huan1, QIN Xiao-ya1, LI Zi-yuan1, ZHENG Zhuo-zhao2, FAN Tian-yuan1△

(1. The State Key Laboratory of Natural and Biomimetic Drugs, Beijing Key Laboratory of Molecular Pharmaceutics and New Drug Delivery Systems, Peking University School of Pharmaceutical Sciences, Beijing 100191， China; 2. Department of Nuclear Medicine, Beijing Tsinghua Changgung Hospital, Beijing 100044, China)

Online:2018-04-18 Published:2018-04-18
Contact: FAN Tian-yuan E-mail:tianyuan_fan@bjmu.edu.cn
Supported by:
Supported by the National Natural Science Foundation of China (81571779)

摘要/Abstract

摘要： 目的：制备并表征柠檬酸（citric acid，CA）修饰的超顺磁性氧化铁纳米粒（superparamagnetic iron oxide nanoparticles，SPIONs）用于磁靶向、热疗和磁共振成像（magnetic resonance imaging，MRI）。方法：应用共沉淀法制备柠檬酸修饰的SPIONs（CA-SPIONs），并通过磁铁、透射电子显微镜、激光粒度测定仪、傅里叶转换红外（Fourier transform infrared，FT-IR）光谱仪、热重差热同步分析仪、振动样品磁强计、X射线衍射仪分别对CA-SPIONs的磁响应性、形态、粒径、红外特征、柠檬酸的质量分数、磁学性质、X射线衍射图谱等进行表征；采用高频感应加热机对CA-SPIONs的发热性能进行考察；通过3.0 T的MRI扫描仪对CA-SPIONs的横向弛豫效能（r2）进行评价。结果：制备的CA-SPIONs在水中分散性良好，呈深黑色，具有良好的磁响应性，其形态圆整、大小均一，平均粒径在12 nm左右，水力学平均粒径为（72.35±4.47） nm，多分散系数为0.231±0.029。红外光谱结果证明CASPIONs表面成功修饰上了CA，修饰的CA所占的重量百分比为9.0%。CA-SPIONs具有良好的超顺磁性，其饱和磁化强度为63.58 emu/g；CA-SPIONs为反尖晶石型结构，经Debye-Scherrer半宽公式可计算出晶粒大小为12.4 nm；在9 A和45~50 kHz的交变电磁场下，CA-SPIONs呈现出良好的发热性能，比吸收率（specific absorption rate，SAR）值为26 W/g；在3.0 T的MRI扫描仪下，测得CA-SPIONs的r2为338 (mmol/L)-1·s-1，表明CA-SPIONs具有良好的MRI负性对比增强作用。结论： CA-SPIONs有希望用于磁靶向、热疗和MRI诊断。

关键词: 柠檬酸, 超顺磁性氧化铁, 纳米粒, 磁共振成像, 磁靶向

Abstract: Objective： To prepare and characterize citric acid (CA)-modified super paramagnetic iron oxide nanoparticles (SPIONs) for magnetic targeting, hyperthermia and magnetic resonance imaging (MRI). Methods: CA-modified SPIONs (CA-SPIONs) were prepared by co-precipitation method and then the magnetic responsiveness, morphology, particle size, infrared feature, weight percentage of CA, magnetic property and X-ray diffraction pattern of CA-SPIONs were respectively characterized by magnet, transmission electron microscope, laser particle size analyzer, Fourier transform infrared (FT-IR) spectroscopy, thermogravimetry-differential thermal analyzer, vibrating sample magnetometer and X-ray diffractometer (XRD). The heating efficiency of the CA-SPIONs was investigated by a high frequency induction heater. The transverse relaxivity (r2) of the CA-SPIONs was evaluated by a 3.0 T MRI scanner. Results: The CA-SPIONs prepared were dispersed well in water with a dark black color and had good magnetic responsiveness. The CA-SPIONs were spherical in shape and uniform in size with an average size around 12 nm. The hydrodynamic average size of the CA-SPIONs was (72.35±4.47) nm with a polydispersity index of 0.231 ± 0.029. The result of infrared spectrum indicated that CA was successfully modified to the surface of SPIONs. The result of thermogravimetric analysis showed that the weight percentage of CA modified on the CA-SPIONs was 9.0%. The result of magnetic property evaluation demonstrated that the CA-SPIONs exhibited excellent superparamagetism with a saturation magnetism of 63.58 emu/g. The XRD result indicated that the CA-SPIONs were in inverse spinel structure. The crystallite size of the CA-SPIONs was calculated to be 12.4 nm by Debye-Scherrer equation. Under the high frequency alternating electromagnetic field with electric current of 9 A and frequency ranging from 45 to 50 kHz, the CA-SPIONs exhibited excellent heating efficiency and the specific absorption rate (SAR) value was calculated to be 26 W/g. The r2 of the CA-SPIONs was assessed to be 338 (mmol/L)-1·s-1 by a 3.0 T MRI scanner, which suggested the excellent negative contrast enhancement effect of the CA-SPIONs. Conclusion: The CA-SPIONs are expected to be used as a promising agent for magnetic targeting, hyperthermia and MRI detection.

Key words: Citric acid, Superparamagnetic iron oxide, Nanoparticles, Magnetic resonance imaging, Magnetic targeting

中图分类号:

R943

王欢，覃小雅，李子圆，郑卓肇，范田园. 柠檬酸修饰的超顺磁性氧化铁纳米粒的制备及表征[J]. 北京大学学报(医学版), 2018, 50(2): 340-346.

WANG Huan, QIN Xiao-ya, LI Zi-yuan, ZHENG Zhuo-zhao, FAN Tian-yuan. Preparation and characterization of citric acid-modified superparamagnetic iron oxide nanoparticles[J]. Journal of Peking University(Health Sciences), 2018, 50(2): 340-346.

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柠檬酸修饰的超顺磁性氧化铁纳米粒的制备及表征

Preparation and characterization of citric acid-modified superparamagnetic iron oxide nanoparticles

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