CN112299489B - 一种超小氧化铁纳米颗粒及其制备方法及应用 - Google Patents
一种超小氧化铁纳米颗粒及其制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种超小氧化铁纳米颗粒,所述超小磁性氧化铁纳米颗粒为由内部自旋有序的铁磁核及表面自旋无序的顺磁壳层组成的MxFe3‑xO4@MxNyFe3‑x‑yO4核‑壳结构且组分可调。本发明还提供了上述超小氧化铁纳米颗粒的制备方法,将两种金属前驱体、表面活性剂按照比例溶于有机溶剂中形成均匀的反应体系,在惰性气体氛围内加热到200‑280℃后,冷却降温,离心洗涤分散于四氢呋喃溶液中,之后加入金属盐溶液,惰性气体氛围内加热到50‑70℃后,离心洗涤即可。本发明属于磁性氧化铁技术领域,本发明提供的超小氧化铁纳米颗粒可同时调控铁磁内核以及顺磁表面的组分,可实现弛豫率的协同增强,可更好的应用于磁共振成像领域。
Description
技术领域
本发明属于磁性氧化铁技术领域,具体是指一种超小氧化铁纳米颗粒及其制备方法及应用。
背景技术
近年来,超小磁性氧化铁纳米颗粒由于其优异的造影性能,良好的生物安全性,有望取代现有临床钆基造影剂成为新一代磁共振T1造影剂。为了制备高度单分散,造影性能优异的磁性氧化铁纳米颗粒,韩国首尔大学Taeghwan Hyeon课题组发表的J.Am.Chem.Soc.2011,133,12624,中国发明专利(CN103153348B);中国科学院化学所高明远课题组发表的Nanotechnology.2011,22,245604;Li,Z.Adv.Funct.Mater.2012,22,2387;Adv.Heathcare.Mater.2013,2,958.等文件都公开报道了制备尺寸形貌均匀的超小氧化铁、铁氧体纳米颗粒。
虽然通过以上方法制备的超小氧化铁纳米颗粒尺寸形貌均一,可以作为磁共振成像T1造影剂,但是这些超小氧化铁纳米颗粒作为磁共振成像T1造影剂依然存在着成像灵敏度不足的问题。为提高超小氧化铁纳米颗粒的T1造影性能,有报道将含钆的物质掺杂到超小氧化铁内部(ACS Nano.2013,7,3287)从而诱导内部产生自旋倾斜效应,提高其T1造影性能,但由于钆从纳米颗粒中的泄露容易造成患者肾源***纤维化甚至肾衰竭,并在体内长期滞留在中枢神经***,对人体构成潜在风险。因此,也有人采用其他金属离子掺杂的报道,如利用Zn2+的掺杂,提高氧化铁纳米颗粒的饱和磁化强度(Angew Chem Int Ed,2009,48,1234;Chem Commun,2008,19,2224),进而提高提高其造影性能,如其中15nm的Zn0.4Fe2.6O4纳米颗粒在4.5T下的r2值高达860mM-1s-1,是Fe3O4纳米颗粒的2.5倍。最近,厦门大学高锦豪课题组通过Mn2+掺杂增加可提高氧化铁纳米颗粒T1弛豫率,报道了不同形貌,不同大小纳米颗粒作为磁共振T1造影剂(J Mater Chem B,2018,6,401,Nanoscale,2014,6,10404)。锰铁氧体立方块的r1值在0.5T下为57.8mM-1s-1,是相同尺寸的氧化铁纳米颗粒3.5倍,以上研究表明均匀掺杂金属离子的方法能够提高超小氧化铁纳米颗粒的T1造影性能。
为了进一步提高超小氧化铁纳米颗粒的T1造影性能,本发明提供一种在超小氧化铁纳米颗粒均匀掺杂的基础上,调控超小氧化铁纳米颗粒的顺磁表面组分,进一步提高超小氧化铁纳米颗粒成像弛豫率,实现超小氧化铁纳米颗粒中核壳的组分协同增强效果的方法,并将其更好的应用于磁共振成像领域。本发明提供的可调控铁磁内核及顺磁表面组分的超小氧化铁纳米颗粒,调控铁磁内核的组分可调节超小氧化铁纳米颗粒的饱和磁化强度(Ms),从而调控弛豫率外球模型的贡献;调控顺磁表面的组分可调节超小氧化铁纳米颗粒与水分子的交换速率,从而调控弛豫率内球模型的贡献。这种同时调节内外球模型贡献的策略可以实现弛豫率的协同增强。
发明内容
为了解决上述难题,本发明提供了一种在超小氧化铁纳米颗粒均匀掺杂的基础上,调控超小氧化铁纳米颗粒的顺磁表面组分,来进一步提高超小氧化铁纳米颗粒成像弛豫率的方法,并将其应用于磁共振成像。
为了实现上述功能,本发明采取的技术方案如下:一种超小氧化铁纳米颗粒,所述超小磁性氧化铁纳米颗粒为由内部自旋有序的铁磁内核及表面自旋无序的顺磁壳层组成的MxFe3-xO4@MxNyFe3-x-yO4核-壳结构且铁磁内核及顺磁壳层的组分可调,所述M为Fe、Co、Ni、Mn、Cu、Zn、Mg、Ca中的一种,x值为0-1.5,所述N为稀土金属、第四周期过渡金属和后过渡金属中的一种,y值为0-0.5。
进一步地,所述超小磁性氧化铁纳米颗粒粒径为2-6nm。
为了实现上述目的,本发明还提供了超小氧化铁纳米颗粒的制备方法,包括以下步骤:
S1、在50ml三口烧瓶中加入铁的前驱体、另一种金属M前驱体、表面活性剂和有机溶剂,升温至200-280℃,保温0-1h,将所得产物采用离心-分散的方式进行3-5次清洗,收集产物分散于正己烷中。
S2、取一定量S1中所得产物,一定量的金属N盐溶液,加入一定体积的四氢呋喃溶液中,通入氩气,50-70℃保持10-60min。
S3、将S2中产物离心洗涤,保存。
进一步地,S1中所述铁的前驱体包括含铁有机配合物和含铁的碳酸盐,S1中所述另一种金属M前驱体包括金属有机配合物和金属碳酸盐;
其中,所述含铁有机配合物包括:芥酸铁、乙酰丙酮铁Fe(acac)3、油酸铁Fe(OA)3、羰基合铁Fe(CO)5、亚硝基羟基苯胺合铁FeCup3;所述铁的碳酸盐为FeCO3;
其中,所述另一种金属M前驱体包括:乙酰丙酮铁Fe(acac)3、油酸铁Fe(OA)3、五羰基合铁Fe(CO)5、亚硝基羟基苯胺合铁FeCup3、Co2(CO)8、Co(acac)2、Ni(OOCCH3)2、Ni(acac)2、油酸稀土配合物、乙酰丙酮稀土配合物;所述金属碳酸盐包括碳酸锌、碳酸亚铁、碳酸锰、碳酸钴、碳酸镍、碳酸镁和碳酸铜。
进一步地,S1中所述表面活性剂包括碳链长度介于6-25之间的有机酸、碳链长度介于6-25之间的有机胺和碳链长度介于6-25之间的有机醇,S1中所述有机溶剂包括十八烯、苄醚、十六碳烯、辛醚和三辛胺。
进一步地,S2中所述金属盐溶液包括氯化锰、氯化钆、氯化铜、氯化镍、氯化钴、氯化镁、硝酸钆和硝酸镁的金属盐溶液。
本发明提供了通过上述方法合成的超小氧化铁纳米颗粒的应用,可以应用于磁共振成像、细胞长期跟踪以及磁纳米颗粒成像领域。
与现有技术相比,本发明还提供了核壳结构的超小氧化铁纳米颗粒制备方法,首先通过热分解法实现金属离子在超小磁性氧化铁铁磁内核的掺杂,然后通过温和的阳离子交换反应实现超小磁性氧化铁顺磁表面组分的调控;本发明提供的可同时调控铁磁内核以及顺磁表面的组分的超小氧化铁纳米颗粒,可实现弛豫率的协同增强,因而能够更好的应用于磁共振成像领域。
附图说明
图1为本发明实施例1的超小磁性氧化铁纳米颗粒透射电镜(TEM)图;
图2为本发明实施例1的超小磁性氧化铁纳米颗粒金属元素分布图;
图3为本发明实施例1和实施例3的超小磁性氧化铁纳米颗粒T1弛豫率图;
图4为本发明实施例1和实施例3的超小磁性氧化铁纳米颗粒弛豫速率r1结果柱状图。
具体实施方式
下面结合具体实施对本发明的技术方案进行进一步详细地说明,本发明所述的技术特征没有进行详细描述的部分均为采用的现有技术。
结合以下实施例,对本发明做进一步详细说明。
实施例1
超小氧化铁纳米颗粒(Zn0.4Fe2.6O4@Zn0.4Mn0.2Fe2.4O4)的制备
(1)称量2.14g芥酸铁,0.09g碳酸锌,3.22g油醇,加入10mL苄醚中,置于50ml三口烧瓶内,270℃保温30min,至溶液呈澄清透亮黑褐色,反应结束;
(2)降温至50℃以下,采用氯仿分散-离心的方式对产物进行三次清洗,最终产物分散于10mL正己烷中;
(3)取1ml(2)中所得产物,5mg MnCl2,加入5ml THF,在氩气保护下升温至50℃,保温30min;
(4)采用氯仿分散-离心的方式对产物进行三次清洗,最终产物分散于10mL正己烷中。
对所制备的超小氧化铁纳米颗粒(Zn0.4Fe2.6O4@Zn0.4Mn0.2Fe2.4O4)进行一系列表征,具体是将所制备的超小氧化铁纳米颗粒分散在正己烷中,取2μL分散有纳米颗粒的正己烷溶液滴在镀有碳膜的Cu网上,自然干燥后做表征。图1为透射电镜图,从图1中可以看出,超小氧化铁纳米颗粒大小形貌均一,具有单分散性,尺寸在3.8nm左右;图2为金属元素分布图,从图2中可以看出超小氧化铁纳米颗粒含有Mn、Fe和Zn元素。
实施例2
超小氧化铁纳米颗粒(Zn0.9Fe2.1O4@Zn0.9Gd0.2Fe1.9O4)的制备
(1)称量2.14g芥酸铁,0.3g碳酸锌,3.22g油醇,加入10mL苄醚中,置于50ml三口烧瓶内,270℃保温30min,至溶液呈澄清透亮黑褐色,反应结束;
(2)降温至50℃以下,采用氯仿分散-离心的方式对产物进行三次清洗,最终产物分散于10mL正己烷中;
(3)取1ml(2)中所得产物,8mg Gd(NO)3,加入5ml THF,在氩气保护下升温至60℃,保温30min;
(4)采用氯仿分散-离心的方式对产物进行三次清洗,最终产物分散于10mL正己烷中。
实施例3
超小氧化铁纳米颗粒(MnFe2O4@MnCu0.1Fe1.9O4)的制备
(1)称量1.07g芥酸铁,1.1g油酸锰,3.22g油醇,加入10mL苄醚中,置于50ml三口烧瓶内,250℃保温30min,至溶液呈澄清透亮黑褐色,反应结束;
(2)降温至50℃以下,采用氯仿分散-离心的方式对产物进行三次清洗,最终产物分散于10mL正己烷中;
(3)取1ml(2)中所得产物,5mg CuCl2,加入5ml THF,在氩气保护下升温至50℃,保温30min;
(4)采用氯仿分散-离心的方式对产物进行三次清洗,最终产物分散于10mL正己烷中。
实施例4
将实施例1制备的调控铁磁内核及顺磁表面组分的超小氧化铁纳米颗粒(Zn0.4Fe2.6O4@Zn0.4Mn0.2Fe2.4O4)和常规超小氧化铁纳米颗粒(γ-Fe2O3)分散在水中,使其Fe浓度分别为0.0625、0.125、0.25、0.5和1mM。分别取10mL颗粒溶液,使用3T磁共振成像仪(Siemens,Germany)进行扫描。MRI扫描参数为:TR=4000ms,TE=19ms。得到样品磁共振扫描图像后,计算出不同浓度梯度样品的弛豫时间T1值如图3所示,进而求出弛豫速率r1如图4所示。经计算调控铁磁内核及顺磁表面组分的超小氧化铁纳米颗粒(Zn0.4Fe2.6O4@Zn0.4Mn0.2Fe2.4O4)和常规超小氧化铁纳米颗粒(γ-Fe2O3)的r1分别为20.22mM-1s-1和3.92mM-1s-1,Zn0.4Fe2.6O4@Zn0.4Mn0.2Fe2.4O4的r1是γ-Fe2O3的5倍以上,说明Zn0.4Fe2.6O4@Zn0.4Mn0.2Fe2.4O4 MRI的T1造影性能远远高于γ-Fe2O3。
以上对本发明及其实施方式进行了描述,这种描述没有限制性,附图中所示的也只是本发明的实施方式之一,并不局限于此。总而言之如果本领域的普通技术人员受其启示,在不脱离本发明创造宗旨的情况下,不经创造性的设计出与该技术方案相似的结构方式及实施例,均应属于本发明的保护范围。
Claims (6)
1.一种超小氧化铁纳米颗粒,其特征在于,所述超小氧化铁纳米颗粒为由内部自旋有序的铁磁内核及表面自旋无序的顺磁壳层组成的MxFe3-xO4@MxNyFe3-x-yO4核-壳结构且铁磁内核及顺磁壳层的组分可调,所述M为Fe、Co、Ni、Mn、Cu、Zn、Mg、Ca中的一种,x值为0-1.5,所述N为稀土金属、第四周期过渡金属和后过渡金属中的一种,y值为0-0.5,所述超小氧化铁纳米颗粒粒径为2-6 nm。
2.一种根据权利要求1所述的超小氧化铁纳米颗粒的制备方法,其特征在于,包括以下步骤:
S1、在50 ml三口烧瓶中加入铁的前驱体、另一种金属M前驱体、表面活性剂和有机溶剂,升温至200-280℃,保温0-1h,将所得产物采用离心-分散的方式进行3-5次清洗,收集产物分散于正己烷中;
S2、取一定量S1中所得产物,一定量的金属N盐溶液,加入一定体积的四氢呋喃溶液中,通入氩气,50-70℃保持10-60 min;
S3、将S2中产物离心,保存。
3.根据权利要求2所述的一种超小氧化铁纳米颗粒的制备方法,其特征在于,S1中所述铁的前驱体包括含铁有机配合物和含铁的碳酸盐,S1中所述另一种金属M前驱体包括金属有机配合物和金属碳酸盐;
所述含铁有机配合物包括:芥酸铁、乙酰丙酮铁Fe(acac)3、油酸铁Fe(OA)3、羰基合铁Fe(CO)5、亚硝基羟基苯胺合铁FeCup3;所述铁的碳酸盐为FeCO3;
所述另一种金属M前驱体包括:乙酰丙酮铁Fe(acac)3、油酸铁Fe(OA)3、五羰基合铁Fe(CO)5、亚硝基羟基苯胺合铁FeCup3、Co2(CO)8、Co(acac)2、Ni(OOCCH3)2、Ni(acac)2、油酸稀土配合物、乙酰丙酮稀土配合物;所述金属碳酸盐包括碳酸锌、碳酸亚铁、碳酸锰、碳酸钴、碳酸镍、碳酸镁和碳酸铜。
4.根据权利要求2所述的一种超小氧化铁纳米颗粒的制备方法,其特征在于,S1中所述表面活性剂包括碳链长度介于6-25之间的有机酸、碳链长度介于6-25之间的有机胺和碳链长度介于6-25之间的有机醇,S1中所述有机溶剂包括十八烯、苄醚、十六碳烯、辛醚和三辛胺。
5.根据权利要求2所述的一种超小氧化铁纳米颗粒的制备方法,其特征在于,S2中所述金属N盐溶液包括氯化锰、氯化钆、氯化铜、氯化镍、氯化钴、氯化镁、硝酸钆和硝酸镁的金属盐溶液。
6.一种根据权利要求1所述的超小氧化铁纳米颗粒的应用,其特征在于,将权利要求1所述的超小氧化铁纳米颗粒应用于磁共振成像、细胞长期跟踪以及磁纳米颗粒成像领域。
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