CN109406507B - 一种采用稳定化金纳米粒子检测海水中银离子的方法 - Google Patents
一种采用稳定化金纳米粒子检测海水中银离子的方法 Download PDFInfo
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Abstract
本发明公开了一种基于氧化石墨烯‑超支化聚合物稳定化金纳米粒子（AuNPs）对海水中银离子（Ag+）的比色检测方法。该比色探针的制备是通过氧化石墨烯‑超支化聚合物还原并稳定AuNPs。在检测过程中利用AuNPs的表面等离子体共振性质，当Ag+存在时，体系出现颜色由红变黄、紫外吸收光谱发生蓝移的双重响应。该比色探针对海水中Ag+的检测范围为0‑0.132 mM，最低检测浓度为0.44µM。本发明的比色探针具有制备简单、稳定性好等优点，能够实现成分复杂、盐度较高的海水体系中Ag+的高灵敏、高选择性快速检测，具有广阔的应用前景。
Description
技术领域
本发明涉及海水中重金属离子检测领域，具体涉及一种稳定化AuNPs的制备方法和海水中Ag+的比色检测方法。
背景技术
近年来，随着工业经济的发展，工业废水和生活污水的排放使得海水中重金属离子污染日趋严重，对我国的海洋事业的发展造成了巨大的影响。其中银离子（Ag+）虽然具有较高的导电导热性、延展性和光敏性，广泛应用于摄影、影像、电器、医药等领域。但是Ag+对海洋生态系统和食物链都具有极大的破环性，能通过食物链最终富集于人体，并可与各种代谢物的胺类、咪唑类、羧基等功能基团结合，严重影响、损害人类的健康，例如：皮肤病，肝肾变性和人体呼吸系统疾病等。因此，急需发展能够快速准确检测海水中Ag+的方法，及时有效监测与防控Ag+对海水的污染。
目前传统的Ag+检测方法主要包括原子吸收光谱法、电感耦合等离子体质谱法、原子荧光光谱法、原子发射光谱法等。然而，这些检测方法都需要大型精贵仪器，操作繁琐费时，分析成本较高，不能用于现场实时快速检测，以上不足在一定程度上限制了这些方法的应用。相比于上述仪器检测方法，基于金纳米粒子（AuNPs）的比色检测方法由于具有操作简单、成本低、方便携带、可现场实时检测等优点而在Ag+的检测应用中受到了重要关注。但其应用多局限于饮用水、自来水、河水、湖水等成分简单、盐度不高的水体系中，而在盐度较高、成分较复杂的海水体系中却难以应用。这是因为AuNPs粒径较小，表面能较高，本身聚集倾向较大，在海水高盐、高离子强度下更易聚集，甚至会沉淀析出，从而干扰检测或无法应用。因此提高AuNPs的稳定性，使其能够应用于海水体系中Ag+的检测便具有重要意义。
本发明为了提高海水体系中AuNPs的稳定性，选用氧化石墨烯-超支化聚合物来还原并稳定AuNPs，其中氧化石墨烯较大的比表面积、较多的官能团以及超支化聚合物的类球型结构可增加粒子之间的空间位阻，避免其发生聚集，从而提高AuNPs的稳定性。同时，超支化聚合物既可以作为稳定剂又可以用作还原剂，避免了传感器复杂的制备过程和后期纯化过程。同时，在后期的检测应用中，Ag+的加入使得AuNPs表面等离子体共振发生变化，最终引起体系颜色和紫外吸收峰的变化，信号响应明显，检测过程简单。因此，基于氧化石墨烯-超支化聚合物稳定化AuNPs实现对成分复杂、盐度较高的海水体系中Ag+的检测具有重要意义。
发明内容
本发明内容的目的是提供一种原位还原制备并稳定AuNPs的方法，解决AuNPs在成分复杂、盐度较高的海水体系中稳定性差，易聚集的难题。本发明的另一目的是提供一种能够快速、高效检测海水中Ag+的比色检测方法，解决现有基于AuNPs比色检测方法灵敏度低、选择性差等问题。
解决上述技术问题，本发明采用的技术方案是：
1. 比色探针的合成
a. 氧化石墨烯-超支化聚合物的制备
将氧化石墨烯和超支化聚合物混合于N，N-二甲基甲酰胺中，然后一定温度下搅拌反应24 h；反应结束后，将混合物进行过滤，乙醇多次洗涤，将产物进行真空干燥24 h，得到产品氧化石墨烯-超支化聚合物。
b. 氧化石墨烯-超支化聚合物稳定化AuNPs的制备
将氯金酸（AuCl3·HCl·4H2O）水溶液加热煮沸，然后加入氧化石墨烯-超支化聚合物水溶液，反应20 min，直至混合溶液变为红色，降温冷却，得到氧化石墨烯-超支化聚合物稳定化AuNPs。
2. 比色探针的应用
将Ag+的海水溶液和抗坏血酸的海水溶液置于氧化石墨烯-超支化聚合物稳定化AuNPs溶液中，体系由原来的红色变为黄色。
氧化石墨烯-超支化聚合物稳定化AuNPs对海水中Ag+的最低检测浓度为0.44 µM。
传感器对Na+, Cd2+, Pb2+, Ba2+, Sr2+,Cs2+, Mg2+, Zn2+, Mn2+, Cu2+, Hg2+等金属离子的比色检测均无明显的变化。
本发明所述超支化聚合物为超支化聚乙烯亚胺、超支化聚酰胺-胺、超支化聚硫醚多胺的任意一种或任意两种及两种以上的混合物。
与现有技术相比，本发明的有益效果：
本发明克服了现有技术的不足，以氧化石墨烯-超支化聚合物稳定化AuNPs作为比色探针，利用其颜色变化和表面等离子体共振性质，建立了一种快速检测Ag+的比色方法。
该发明中，选用含胺类超支化聚合物对氯金酸进行还原，其一，利用超支化聚合物的还原性实现原位制备AuNPs，可显著提高AuNPs的稳定性；其二，可以协同发挥氧化石墨烯和超支化聚合物本身各自的优点，满足面对成分复杂、盐度较高的海水体系中基于AuNPs检测Ag+的苛刻条件要求。
本发明中，比色探针具有很高的灵敏度，响应时间快速，而且其对海水中Ag+的最低检测浓度低至0.44 µM，具有很高的实用性。
本发明中的比色探针对海水中Ag+的检测具有较好的选择性，抗干扰性强，应用广泛。
附图说明
图1为海水中不同浓度Ag+存在时比色体系的紫外-可见吸收光谱和其线性关系拟合图。
图2为海水中不同金属离子存在时比色体系的紫外-可见吸收光谱。
具体实施方式
本发明所要解决的技术问题是提供一种简单、高稳定比色传探针的制备方法和快速检测Ag+的应用新技术，下面结合实施例对本发明做进一步的描述：
实施例1：氧化石墨烯-超支化聚合物的制备
以氧化石墨烯和超支化聚合物为原料来制备氧化石墨烯-超支化聚合物复合材料。将氧化石墨烯和超支化聚合物以2:1的质量比混合于20 mL N，N-二甲基甲酰胺中，搅拌回流反应24 h；然后，将混合物进行过滤，并用乙醇进行多次洗涤；将产物置于40 °C的条件下真空干燥24 h，得到氧化石墨烯-超支化聚合物复合材料。
实施例2：氧化石墨烯-超支化聚合物稳定化AuNPs的制备
取20 mL 0.15 mM氯金酸（AuCl3·HCl·4H2O）水溶液加热煮沸，加入0.4 mL 0.25-2.45 mg/mL氧化石墨烯-超支化聚合物水溶液，混合溶液反应20 min，直至溶液变为红色；最后，将混合液冷却静置，得到氧化石墨烯-超支化聚合物稳定化AuNPs。
实施例3：比色检测方法的构建和检测灵敏度的考察
在本发明中，以氧化石墨烯-超支化聚合物稳定化AuNPs作为检测探针，检测海水体系中Ag+的存在。检测过程中，当存在Ag+时，由肉眼可以观察到检测体系会由原来的浅红色变为黄色，紫外吸收光谱的特征吸收峰会发生蓝移，从而实现对海水中Ag+的比色检测。取0-2.0 mL 3.94×10-4 M的Ag+海水溶液和0.5 mL 100 mg/mL抗坏血酸的海水溶液于0.10-1.50 mL 0.15 mM氧化石墨烯-超支化聚合物稳定化AuNPs溶液中，并使检测体系最终定容为4.5 mL，通过记录颜色和紫外吸收光谱变化来考察比色探针对Ag+的检测灵敏度（图1）。由图1可知，氧化石墨烯-超支化聚合物稳定化AuNPs的特征吸收峰强度随Ag+浓度变化而线性增加，并伴随蓝移。这是因为Ag+浓度的升高，引起了氧化石墨烯-超支化聚合物稳定化AuNPs表面等离子体共振性质的变化，最终由单分散状态逐渐发生聚集，并团聚在一起，引起体系颜色变化与紫外特征吸收峰的位移。最后得知氧化石墨烯-超支化聚合物稳定化AuNPs对海水中Ag+的最低检测浓度为0.44 µM。
实施例4：检测选择性的考察
在氧化石墨烯-超支化聚合物稳定化AuNPs作为比色探针检测Ag+的实验中，同时选用多种金属离子（Na+, Cd2+, Pb2+, Ba2+, Sr2+, Mg2+, Zn2+, Mn2+,Cs2+, Cu2+, Hg2+）作为干扰离子来考察比色传感器的检测选择性。分别取0.5 mL 3.94×10-4 M金属离子溶液和0.5 mL 100 mg/mL抗坏血酸溶液于0.5 mL 0.15 mM氧化石墨烯-超支化聚合物稳定化AuNPs溶液中，检测体系最终定容4.5 mL，通过记录颜色和紫外吸收光谱变化来考察比色探针对Ag+检测的选择性。由图2可知，加入相同浓度的其他金属离子，氧化石墨烯-超支化聚合物稳定化AuNPs特征吸收变化较小，表明AuNPs仍保持着单分散状态。加入Ag+之后，氧化石墨烯-超支化聚合物稳定化AuNPs在430 nm处有特征吸收峰出现，并伴随明显的位移，这是由于AuNPs与Ag+结合形成Au-Ag合金。实验结果表明，氧化石墨烯-超支化聚合物稳定化AuNPs对海水中Ag+的检测具有非常高的选择性。
AuNPs浓度、氧化石墨烯-超支化聚合物用量、水质体系的改变等因素都能影响本发明的实现，在此不再一一列举实施例。
Claims (5)
1.一种采用氧化石墨烯-超支化聚合物稳定化金纳米粒子对海水中银离子(Ag+)进行检测的方法，其特征在于包括以下步骤：向氧化石墨烯-超支化聚合物稳定化金纳米粒子溶液中依次加入抗坏血酸的海水溶液和被检测的Ag+的海水溶液，静置，观察纳米粒子溶液颜色和紫外吸收光谱的特征吸收峰的变化；其中所采用的氧化石墨烯-超支化聚合物稳定化金纳米粒子由以下方法制备：将氧化石墨烯和超支化聚合物混合于N，N-二甲基甲酰胺中，一定温度下搅拌反应24 h，反应结束后，将混合物进行过滤，乙醇多次洗涤，将产物真空干燥24 h，得到氧化石墨烯-超支化聚合物，其中氧化石墨烯和超支化聚合物的质量比为1:1-3:1；将氯金酸水溶液加热煮沸，然后加入氧化石墨烯-超支化聚合物水溶液，反应15-30 min，直至混合溶液变为红色，降温冷却，得到氧化石墨烯-超支化聚合物稳定化金纳米粒子；所述的超支化聚合物为超支化聚乙烯亚胺、超支化聚酰胺-胺、超支化聚硫醚多胺的任意一种或任意两种及两种以上的混合物。
2.根据权利要求1所述的采用氧化石墨烯-超支化聚合物稳定化金纳米粒子对海水中银离子(Ag+)进行检测的方法，其特征在于：氧化石墨烯-超支化聚合物稳定化金纳米粒子作为比色探针，其使用浓度范围为1.0×10-3-5.0×10-2 M。
3.根据权利要求1所述的采用氧化石墨烯-超支化聚合物稳定化金纳米粒子对海水中银离子(Ag+)进行检测的方法，其特征在于：Ag+作为目标物，其检测浓度范围为0-0.132 mM。
4.根据权利要求1所述的采用氧化石墨烯-超支化聚合物稳定化金纳米粒子对海水中银离子(Ag+)进行检测的方法，其特征在于：抗坏血酸溶液的浓度范围为0.1-15.0 mg/mL。
5.根据权利要求1所述的采用氧化石墨烯-超支化聚合物稳定化金纳米粒子对海水中银离子(Ag+)进行检测的方法，其特征在于：氧化石墨烯-超支化聚合物稳定化金纳米粒子还可用于纯净水、自来水、湖水、河水及土壤体系中Ag+的检测。
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