CN104945424B - 一种稀土配位聚合物纳米粒子制备方法及其应用 - Google Patents
一种稀土配位聚合物纳米粒子制备方法及其应用 Download PDFInfo
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Abstract
一种稀土配位聚合物纳米粒子制备方法及其应用,将硝酸铕和间苯二甲酸分别溶于纯水和乙醇中,所述硝酸铕溶液和间苯二甲酸溶液的浓度均为40 mM,本发明的制备方法操作简单、环境要求低,作为Hg2+的荧光探针,具有简单高效、反应时间短、灵敏度高和选择性好的优点,同时,由于制备的稀土配合物聚合物纳米粒子的分散性好、尺寸均一和荧光强度高,所以在化学传感、药物运输和细胞成像等领域提供了一种新材料,从而有助于拓展稀土配位聚合物在生物分析领域的应用。
Description
技术领域
本发明涉及一种纳米粒子制备方法,尤其涉及一种稀土配位聚合物纳米粒子制备方法及其应用。
背景技术
汞是一种高毒性的物质,它容易在生物体内积累。二价汞离子(Hg2+)是最稳定的无机汞之一,它对人体的健康有着严重的影响,能严重损伤人体的脑、神经系统、肾功能和内分泌系统。目前,汞污染作为全球性问题已经引起了人们广泛的关注。据估计,全球每年大约有 3000 吨的汞通过人类活动释放到大气层中,汞是不可降解的,它在环境中不能被分解,只能被稀释或被转化,因此,发展快速、简便和灵敏的Hg2+检测方法一直是化学和材料科
学研究领域的一个重要方向。
稀土配位聚合物是一类由稀土离子和有机配体通过自组装形成的新型有机-无机杂化材料,兼具有无机和有机基团的性质和功能。荧光稀土配位聚合物的出现不仅极大地丰富了稀土荧光探针的种类,而且因其具有大的 Stokes 位移(>150 nm)、窄的发射峰(半缝宽<10 nm)以及能有效消除背景荧光干扰的长荧光寿命( ms 级)等优点使其在化学传感、药物运输以及细胞成像等方面显示出了诱人的应用前景。尽管如此,稀土配位聚合物的重金属离子荧光检测应用还需进一步的发展。虽然已有少量的稀土配位聚合物被报道合成并作为荧光探针检测 Hg2+,但是仍存在着一些不足。例如,陈扬等人报道合成的荧光稀土配位聚合物纳米粒子的制备需要第二客体分子的参与(ACS Nano 2012, 6, 10505-10511),孙亚光等人合成的荧光稀土配位聚合物的尺寸较大,形貌也不均一,且重复性较差(中国专利公开号CN 102079752 A)。因此,发展新型的稀土配位聚合物纳米粒子,并用于Hg2+的荧光检测就显得尤为重要。在本发明中,我们首次利用水热法合成了以间苯二间甲酸为桥连配体和铕离子为金属中心的稀土配位聚合物纳米粒子。与已报道的油浴方法相比(Chemistry-A European Journal 2013, 19, 6546-6550),本方法不仅能得到产量高、尺寸均一的纳米粒子,而且还具有操作过程更简单和更绿色的优势。并且,基于荧光内滤效应原理,首次利用稀土配位聚合物纳米粒子为荧光探针检测了水溶液、尿液和血清中Hg2+的含量。
发明内容
本发明的目的在于提供一种稀土配位聚合物纳米粒子制备方法及其应用,其与已报道的苯二甲酸/铕配位聚合物纳米粒子的合成方法不同,本发明是利用水热法直接合成,得到纳米粒子产量更高和操作过程更简单,并且,基于荧光内滤效应原理,利用该稀土配位聚合物纳米粒子为荧光探针检测了水溶液、尿液和血清中Hg2+的含量。
本发明是通过以下步骤来实现的:
1、将硝酸铕和间苯二甲酸分别溶于纯水和乙醇中,所述硝酸铕溶液和间苯二甲酸溶液的浓度均为40 mM;
2、将咪唑二羧酸溶于纯水后,边超声边加入氢氧化钠溶液,直到咪唑-二羧酸完全溶解后,用盐酸将溶液的pH调为中性备用,所述咪唑二羧酸溶液的浓度为10 mM;
3、向含有8mL 的N, N’-二甲基甲酰胺的烧杯中,依次加入2 mL的硝酸铕溶液和2mL的间苯二甲酸溶液,在室温下搅拌反应30 分钟后,将该溶液转移到反应釜中,在170℃温度下反应8小时;
4、上一步骤反应结束后,离心收集溶液中的白色产物—即稀土配位聚合物纳米粒子,用乙醇进行充分洗涤后,所得沉淀重悬于乙醇备用;
5、向含有1 μL稀土配位聚合物纳米粒子的Tris-HCl缓冲液中加入400 μL的咪唑-4,5-二羧酸溶液,所述Tris-HCl缓冲液的浓度为25 mM、pH=7,之后在室温下反应5分钟后,加入不同浓度的汞离子,其浓度范围为0-1mM,所述Tris-HCl缓冲液补充至反应总体积为100 μL,在室温下继续反应5 分钟后,测定反应液的荧光强度。
所述间苯二甲酸为咪唑-4,5-二羧酸。
所述间苯二甲酸与铕离子的摩尔比为1:1。
所述汞离子检测时的反应液的总体积为100 μL。
本发明的技术效果是:本发明的制备方法操作简单、环境要求低,作为Hg2+的荧光探针,具有简单高效、反应时间短、灵敏度高和选择性好的优点,同时,由于制备的稀土配合物聚合物纳米粒子的分散性好、尺寸均一和荧光强度高,所以在化学传感、药物运输和细胞成像等领域提供了一种新材料,从而有助于拓展稀土配位聚合物在生物分析领域的应用。
附图说明
图1为本发明的扫描电镜图。
图2为本发明在检测时,在不同浓度汞离子的荧光光谱图。
图3为本发明在检测时,对Hg2+荧光响应的柱形图。
具体实施方式
下面将结合附图实施例详细说明本发明所具有的有益效果,旨在帮助阅读者更好地理解本发明的实质,但不能对本发明的实施和保护范围构成任何限定。
首先,在水热条件下制备稀土配位聚合物纳米粒子,其具体步骤如下:向含有8mL的N, N’-二甲基甲酰胺的烧杯中,依次加入2 mL的硝酸铕水溶液和2 mL的间苯二甲酸乙醇溶液,在室温下搅拌反应30 分钟后,将该溶液转移到反应釜中,在170℃温度下反应8小时,反应结束后,离心收集白色产物—即稀土配位聚合物纳米粒子,在用乙醇进行充分洗涤后,所得沉淀重悬于乙醇备用,图1显示了稀土配位聚合物纳米粒子的形貌为平均粒径为300nm的球形粒子,并具有优秀的单分散性,然后,向含有1 μL稀土配位聚合物纳米粒子的Tris-HCl缓冲液中加入400 μL的咪唑-4,5-二羧酸溶液,所述Tris-HCl缓冲液的浓度为25mM、pH=7,之后在室温下反应5分钟后,加入不同浓度的汞离子—其浓度范围为0-1mM,用Tris-HCl缓冲液补充至反应总体积为100 μL,在室温下继续反应5 分钟后,测定反应液的荧光强度,图2显示出该稀土配位聚合物纳米粒子在247 nm波长的激发下能发射出Eu3+的特征性光谱,咪唑-4,5-二羧酸的加入能显著淬灭稀土配位聚合物纳米粒子的荧光,相反,随着Hg2+的加入,稀土配位聚合物纳米粒子被淬灭的荧光能够得到恢复,且恢复的程度随着Hg2+浓度增加而增大。
为了测试其他金属离子是否也和Hg2+一样可以恢复该稀土配位聚合物纳米粒子被淬灭的荧光,我们测定了Zn2+、Cu2+、Ce3+、Fe3+、Co2+、Mn2+、Ni2+、Pb2+、Ag+、 Mg2+与该稀土配位聚合物纳米粒子和咪唑-4,5-二羧酸混合物的荧光,结果见图3,结果显示出,只有Hg2+的加入能显著地恢复稀土配位聚合物纳米粒子的荧光,这说明稀土配位聚合物纳米粒子作为Hg2+荧光探针具有优秀的选择性。
此外,在相同的实验条件下,对尿液和血清中的Hg2+进行了测定,结果发现,稀土配位聚合物纳米粒子作为Hg2+荧光探针具有良好的回收率(均>95 %),这说明稀土配位聚合物纳米粒子作为Hg2+荧光探针可以用于尿液和血清中的Hg2+的测定。
以上所述的实施例仅仅是对本发明的优选实施方式进行描述,并非对本发明的范围进行限定,在不脱离本发明设计精神的前提下,本领域普通技术人员对本发明的技术方案作出的各种变形和改进,均应落入本发明权利要求书确定的保护范围内。
Claims (3)
1.一种稀土配位聚合物纳米粒子的制备方法,步骤如下:
(1)将硝酸铕和间苯二甲酸分别溶于纯水和乙醇中,所述硝酸铕溶液和间苯二甲酸溶液的浓度均为40mM;
(2)向含有8mL的N,N’-二甲基甲酰胺的烧杯中,依次加入2mL的硝酸铕溶液和2mL的间苯二甲酸溶液,在室温下搅拌反应30分钟后,将该溶液转移到反应釜中,在170℃温度下反应8小时;
(3)上一步骤反应结束后,离心收集溶液中的白色产物——即稀土配位聚合物纳米粒子,用乙醇进行充分洗涤后,所得沉淀重悬于乙醇备用。
2.根据权利要求1所述的稀土配位聚合物纳米粒子制备方法,其特征在于:所述间苯二甲酸与铕离子的摩尔比为1:1。
3.一种根据权利要求1所述的方法制备的稀土配位聚合物纳米粒子的应用,其特征在于:将咪唑-4,5-二羧酸溶于纯水后,边超声边加入氢氧化钠溶液,直到咪唑-4,5-二羧酸完全溶解后,用盐酸将溶液的pH调为中性备用,所述咪唑-4,5-二羧酸溶液的浓度为10mM;向含有1μL稀土配位聚合物纳米粒子的Tris-HCl缓冲液中加入400μL的咪唑-4,5-二羧酸溶液,所述Tris-HCl缓冲液的浓度为25mM、pH=7;之后在室温下反应5分钟后,加入不同浓度的汞离子,其浓度范围为0-1mM;用所述Tris-HCl缓冲液补充至反应总体积为100μL,在室温下继续反应5分钟后,测定反应液的荧光强度。
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