CN116333743B - 一种制备磁共振/荧光双模成像材料的方法 - Google Patents
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Abstract
本发明涉及定量分析和医学检测领域，具体公开了一种同时具备磁共振和荧光性能的谷胱甘肽‑四氧化三锰‑CdTe量子点复合材料的制备方法。所述方法包括如下步骤：将高锰酸钾滴加到谷胱甘肽和氯化镉溶液后加入碲氢化钠，回流加热后，加入丙酮，沉淀离心分离，真空干燥，得红色粉末。本发明制得的谷胱甘肽‑四氧化三锰‑CdTe量子点复合物为片状结构，同时具有荧光和磁共振性能。
Description
技术领域
本发明涉及定量分析和医学检测领域，涉及一种同时具备磁共振和荧光性能的谷胱甘肽-四氧化三锰-CdTe量子点的复合材料的制备方法。
背景技术
自1973年磁共振成像(MRI)成为了现代医学诊断中无可代替的一种检测技术，它可在体内直接监测疾病的起因、发生、发展及一系列的病理生理变化，更可实现肿瘤的早期诊断，但是存在成像的速度慢、不能进行动态成像、像是体内具有金属物体的患者是不适合进行磁共振检查等缺点。在复杂疾病的诊断上，单一的检测手段已经到达了瓶颈阶段了，而使用不同的检测模态可以相互验证补足检测信息，于是就形成了双模或者多模态的成像检测技术。其中荧光成像具有较高的敏感性，现在的仪器已经能检测出极少量的光子，并将一定区域荧光光子数量的检测结果用图像反映在计算机中，从而得到一种可视化的荧光显示模式，尤其是近红外的荧光具有较高的组织穿透能力。因此将磁共振成像和荧光成像结合起来的双模成像探针具有高灵敏度和空间分辨率的双重优点，可以增强对肿瘤的识别和诊断能力。但是现有的合成技术多是分别合成两种材料，再复合在一起，具有反应时间长、材料不稳定等问题。
发明内容
为了改进材料合成方法，本发明提供了一种以谷胱甘肽、高锰酸钾、氯化镉、碲粉和硼氢化钠为原料制备磁共振荧光双模成像材料的方法，用于解决现有技术中操作过程复杂、反应时间长等问题。
为了实现上述目的及其他相关目的，本发明首先提供了谷胱甘肽四氧化三锰CdTe量子点复合材料的制备方法，具体包括如下步骤：(1)容积为10毫升的圆底烧瓶中加入2毫升双蒸水，依次加入碲粉和硼氢化钠，磁力搅拌1h左右，直到溶液呈白色，得到碲氢化钠溶液，待用。(2)容积为250毫升的圆底烧瓶中加入100毫升双蒸水，通氮气20分钟除去氧气，依次加入谷胱甘肽和氯化镉，搅拌至溶解，调节pH，滴加高锰酸钾，搅拌，得到棕黄色溶液，加入碲氢化钠溶液。回流加热后，加入丙酮，沉淀离心分离，真空干燥，得红色粉末。
进一步，所述(2)中谷胱甘肽和氯化镉的质量比为1.2:1、1:1和1:1.2，优选为1:1.2，实验中谷胱甘肽为0.05克，氯化镉为0.06克。
进一步，所述(2)中磁力搅拌下，滴加高锰酸钾以使高锰酸钾与谷胱甘肽充分反应。
进一步，所述(2)中高锰酸钾浓度为30毫摩尔每升，所采用的量为1～10毫升，优选为5.2毫升。
进一步，所述(2)中搅拌时间为10分钟～1小时，优选搅拌时间为30分钟。
进一步，所述(2)中加热温度为80、100和120摄氏度，优选温度为100摄氏度。
进一步，所述(2)中加热时间为15～2小时，优选为1小时。
进一步，所述(2)中真空干燥优选温度为40摄氏度，烘干时间20分钟。
进一步，所述复合材料为片状结构。
本发明合成了一种兼具磁共振和荧光成像性能的谷胱甘肽-四氧化三锰-CdTe量子点复合材料，其荧光强度为1600，磁共振成像性能中弛豫率为81.66M-1s-1。通过透射电镜可见所合成材料为200nm左右的片状结构，高分辨透射电镜可见晶格间距为0.28埃和0.33埃分别对应四氧化三锰和CdTe量子点的晶格特征。XRD分析可见四氧化三锰特征峰。XPS证明复合材料中包含Cd、Te、N、O、S、Mn等元素，通过高分辨XPS分析证明该复合材料为CdTe量子点和四氧化三锰复合材料。荧光光谱图和磁共振成像表明所合成复合材料具有磁共振荧光双模成像性能。
附图说明
图1为所合成材料的透射电镜图。
图2为所合成材料的XRD图。
图3为所合成材料的XPS图。
图4为所合成材料的荧光光谱和荧光衰减曲线图。
图5为所合成材料的弛豫率R1(1/T1)图。
具体实施方式
以下通过特定的具体实例说明本发明的实施方式，本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用，本说明书中的各项细节也可以基于不同观点与应用，在没有背离本发明的精神下进行各种修饰或改变。具体实施过程如下：
实施例一：1、制备谷胱甘肽-四氧化三锰-CdTe量子点复合材料，具体方法为：容积为10毫升的圆底烧瓶中加入2毫升双蒸水，依次加入碲粉和硼氢化钠，磁力搅拌1h左右，直到溶液呈白色，为A溶液，待用。2)容积为250毫升的圆底烧瓶中加入100毫升双蒸水，通氮气20分钟除去氧气，依次加入0.05克谷胱甘肽和0.06克氯化镉，搅拌至溶解，滴加30毫摩尔每升的高锰酸钾5.2毫升，搅拌30分钟，得到棕黄色溶液，加入碲氢化钠溶液，继续搅拌20分钟。所得溶液100摄氏度下，回流加热1小时，加入丙酮，沉淀离心分离，40摄氏度下真空干燥20分钟，得红色粉末。2、采用TEM、XRD和XPS对上述合成复合材料进行表征，TEM如图1所示，XRD如图2所示，XPS如图3所示。
实施例二：谷胱甘肽-四氧化三锰-CdTe量子点复合材料的荧光成像性能和磁共振性能评价荧光性能分析：如图4(a)所示所合成材料荧光强度为1600nm，激发波长380nm，狭缝宽度为5，5nm。如图4(b)所示所合成材料的荧光寿命为27.63ns。磁共振性能分析：如图5所示，所合成材料的r值为81.66M-1·S-1。
Claims (5)
1.一种同时具备磁共振和荧光成像性能的复合材料的制备方法，其特征在于，包括如下步骤：
(1)容积为10毫升的圆底烧瓶中加入2毫升双蒸水，依次加入碲粉和硼氢化钠，磁力搅拌1h，直到溶液呈白色，得到碲氢化钠溶液，待用；
(2)容积为250毫升的圆底烧瓶中加入100毫升双蒸水，通氮气20分钟除去氧气，依次加入谷胱甘肽和氯化镉，搅拌至溶解，调节pH，滴加高锰酸钾，搅拌，得到棕黄色溶液，加入(1)得到的溶液，搅拌20分钟，所得溶液回流加热后，加入丙酮，沉淀离心分离，真空干燥，得红色粉末。
2.根据权利要求1所述的制备方法，其特征在于：谷胱甘肽和氯化镉的质量比1:1.2，实验中谷胱甘肽为0.05克，氯化镉为0.06克。
3.根据权利要求1所述的制备方法，其特征在于：高锰酸钾浓度为30毫摩尔每升，加入的体积为5.2毫升。
4.根据权利要求1所述的制备方法，其特征在于：加入高锰酸钾的搅拌时间为30分钟，回流加热温度为100摄氏度，加热时间为1小时。
5.根据权利要求1所述的制备方法，其特征在于：所述复合材料为片状结构。
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