CN108941601A - 一种金纳米粒子及其制备方法 - Google Patents
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Abstract
本发明公开了一种金纳米粒子及其制备方法，用于快速检测湖水、自来水、矿泉水、人体血样或尿样中钾离子。该技术方法基于团聚机理，利用有机化合物配体上的氨基能够形成强的氢键作用或通过有机化合物配体上的苯环形成强的π‑π堆积作用，从而引起金纳米粒子团聚，使得溶液颜色发生变化，引起金纳米粒子表面等离子共振吸收峰的峰位以及吸收强度发生变化，直接利用肉眼和紫外可见分光光度进行判定，即可快速地检测样品中是否含有K+离子，实现对样品中K+离子的快速检测。该技术方案具有操作简单、成本低、灵敏度高，适用范围广等优点。
Description
技术领域
本发明属于纳米材料领域，具体涉及一种金纳米粒子及其制备方法。
背景技术
钾离子是由钾原子失去最外层的一个电子得到的正1价离子，书写为K+。钾离子原子核外达到稳定结构为8个电子。钾离子是细胞内液的主要阳离子，体内98％的钾存在于细胞内。正常情况下，日常饮食中的钾含量足以满足机体的需要，不会出现缺钾。钾由肠道吸收后，约有30％由肾脏排泄，肾脏对钾的排泄没有限制，即使机体处于缺钾状态，肾脏仍继续排钾。钾离子对人体健康有益，但人体内的钾离子浓度不正常时会导致一系列的疾病如：高血压、中风、肾脏等。心肌和神经肌肉都需要有相对恒定的钾离子浓度来维持正常的应激性。血清钾过高时，对心肌有抑制作用，可使心跳在舒张期停止，血清钾过低能使心肌兴奋，可使心跳在收缩期停止。血钾对神经肌肉的作用与心肌相反。
人体内钾离子浓度过高或过低都会引起严重后果。人体内钾离子异常分为高血钾和低血钾。(一)当血清钾大于5.5/L为高血钾，主要是由一下两个方面引起的，(1)钾排出减少，如肾功能衰竭少尿期，长期口服安体舒通、氨苯喋啶等利尿剂，肾小管排钾功能缺陷，肾上腺皮质机能减退，尿毒症；(2)细胞内钾外移，如挤压伤、溶血等。(二)当血清钾小于3.5mmol/L为低血钾症，原因在于(1)钾丢失过多，如严重腹泻、呕吐、肾上腺皮质功能亢进、钡盐中毒，应用排钾利尿剂；(2)钾分布异常，如低钾性周期麻痹在发作时血清钾下降，可低至2.5mmol/L，但在发作间歇期血清钾可正常。
因此，敏感的K+选择性传感器对于生理水平测量钾离子是非常重要的，同时也可用于诊断或检测复杂体系中钾离子的含量。目前钾离子检测技术或方法主要有原子吸收光谱法，光纤传感器，荧光光谱法，电化学传感技术等。上述技术方法的优点是灵敏度高，速度快，操作简单；弱点是所需仪器设备笨重、昂贵，一般不适合现场检测等。为此，人们发展了新的检测方法，如比色检测。比色检测往往是基于金属离子纳米颗粒团聚或抗团聚机理导致颜色变化，从而实现对目标物的检测。在比色检测中，使用最多金纳米粒子，其优点是操作简单，灵敏性高，能够满足现场检测。金纳米粒子比色检测常用于检测有机小分子如瘦肉精、吡蚜酮、三苯胺等(Jiang等人，Plos One,2017,12,e0177131)，也可以用于检测蛋白质(马等Rsc Adv.,2016,6,106608-106614)、DNA(M.K.Lam等人Langmuir, 2016,32,1585-1590)等生物大分子，检测重金属离子等(Y.M.Leng等人Appl.Phys a-Mater., 2017,123(9),607)。S.Y.Lin等人使用含巯基的15-冠-5衍生物修饰金纳米颗粒，并成功地实现了对K+的检测(Anal.Chem.,2005,77,4821-4828)。这种含巯基的15-冠-5衍生物修饰剂合成过程复杂且价格昂贵，成本较高，难以推广应用。宋等人通过使用含荧光基团和苯胺-18-crown-6芳纶醚基团的半花菁染料(a fluorophore and phenylaza-[18]crown-6 lariat ether，简写为ACLE)修饰金纳米颗粒，实现了对K+的高效检测。这种修饰剂结构复杂，操作繁琐，价格贵(Chem.Commun.,2017,53,5602-5605)。
发明内容
本发明要解决的技术是针对上述存在的技术现状，制备一种稳定性能好，颗粒均匀、廉价的金纳米粒子传感器，该传感器可用于湖水、自来水、矿泉水、血样、尿样以及其他复杂体系中K+的现场快速检测。
本发明解决上述技术问题所采取的技术方案为：
一种金纳米粒子的制备方法，采用4'-氨基-二苯并-18-冠醚-6和柠檬酸钠作为修饰剂、稳定剂和还原剂将三价的金还原成零价的金并制成金纳米粒子(图1)；将所制备的金纳米粒子加到含不同浓度钾离子的溶液中，溶液颜色从红色变成灰色或灰黑色。4'-氨基-二苯并 -18-冠醚-6作为配体稳定剂、修饰剂与金纳米粒子作用时，通过其氨基形成强的氢键作用或通过其苯环形成强的π-π堆积作用，从而引起金纳米粒子团聚，使得溶液颜色发生变化，实现对溶液中钾离子的裸眼快速定性检测；通过金纳米粒子的团聚引起金纳米粒子表面等离子共振吸收峰的峰位以及强度发生变化，实现对溶液中钾离子的定量检测。
4'-氨基-二苯并-18-冠醚-6配体的结构如下式所示：
本发明提供的一种金纳米粒子的制备方法，具体包括如下步骤：
在圆底烧瓶中加入一定浓度的氯金酸水溶液，搅拌加热至沸腾，快速加入4'-氨基-二苯并-18-冠醚-6乙醇溶液和柠檬酸钠的水溶液，反应8-15分钟，溶液颜色由浅黄色变为红色，静置冷却至室温，制得金纳米粒子(图1)，放入0～4℃的冰箱中保存备用。
上述方案中，所述的氯金酸水溶液的浓度为0.3～1.5mM，所述金纳米粒子水溶液的pH 范围在2.5～6.5之间，所述的4'-氨基-二苯并-18-冠醚-6乙醇溶液的浓度为0.5mM，所述的柠檬酸钠水溶液的浓度为0.8mM。
将所制备的金纳米粒子与含有不同浓度K+离子的标准溶液反应，根据不同的颜色变化制成标准卡片，包括空白实验结果的卡片，用于不同环境下待检测样品的现场检测。将所制备的金纳米粒子与待检测样品反应，通过紫外吸收光谱测试金纳米粒子表面等离子共振吸收峰的峰位以及强度发生变化，实现对样品中钾离子的定量检测(图2)。裸眼检测限为40μM，紫外光谱检测限为30μM。
所述待检测样品可以是湖水、自来水、矿泉水，也可以经过处理后获得的样品，如血液样品、尿液样品以及食品与蔬菜样品等。
综上所述，本发明提供了一种金纳米粒子及其制备方法，以及用所制备的金纳米粒子检测K+技术，该技术方法基于团聚机理，利用有机化合物配体上的氨基能够形成强的氢键作用或通过有机化合物配体上的苯环形成强的π-π堆积作用，从而引起金纳米粒子团聚，使得溶液颜色发生变化，引起金纳米粒子表面等离子共振吸收峰的峰位以及吸收强度发生变化，因此，直接利用肉眼和紫外可见分光光度进行判定，即可快速地检测样品中是否含有K+离子，实现对样品中K+离子的快速检测。
优选的，所述参加反应的物质为分析纯。
与现有技术相比，本发明的优点在于：本发明提一种金纳米粒子及其制备方法与离子检测的应用技术，该技术方法操作简单方便、原料廉价易得、成本低、检测快速、灵敏度高、选择性强并且可实施现场裸眼比色检测，适用于湖水、自来水、矿泉水、血样、尿样以及其他复杂体系中K+的快速检测，具有广泛的潜在应用价值。
附图说明
图1金纳米粒子的TEM图，粒子直径范围6-20nm。
图2不同组分条件下的粒子表面等离子共振紫外吸收光谱，ABC代表4'-氨基-二苯并 -18-冠醚-6配体，AuNPs金纳米粒子。
具体实施方式
下面通过具体实施例进一步描述本发明，但不限制本发明的内容。
实施例1
在圆底烧瓶中加入50mL 0.3mM浓度的氯金酸水溶液，搅拌加热至沸腾，快速加入10mL 0.5mM的4'-氨基-二苯并-18-冠醚-6乙醇溶液和10mL 0.8mM柠檬酸钠的水溶液，反应混合物溶液的pH值用HCl调控为6.5，反应15分钟后，溶液颜色由浅黄色变为红色，静置冷却至室温，制得金纳米粒子。将制得的金纳米粒子TEM测试(图1)。4‐氨基苯并‐18‐冠‐6作为配体、稳定剂和修饰剂，其结构简单，价格相对低廉。
实施例2
在圆底烧瓶中加入20mL 1.5mM浓度的氯金酸水溶液，搅拌加热至沸腾，快速加入20mL 0.5mM的4'-氨基-二苯并-18-冠醚-6乙醇溶液和20mL 0.8mM柠檬酸钠的水溶液，反应混合物溶液的pH值用HCl调控为2.5，反应8分钟后，溶液颜色由浅黄色变为红色，静置冷却至室温，制得金纳米粒子。
实施例3
在圆底烧瓶中加入30mL 1.0mM浓度的氯金酸水溶液，搅拌加热至沸腾，快速加入15mL 0.5mM的4'-氨基-二苯并-18-冠醚-6乙醇溶液和15mL 0.8mM柠檬酸钠的水溶液，反应混合物溶液的pH值用HCl调控为4，反应10分钟后，溶液颜色由浅黄色变为红色，静置冷却至室温，制得金纳米粒子。
实施例4
“自来水”中钾离子的检测
(a)量取两份等体积相同的所制备金纳米粒子溶液；配制不含钾离子(在检测极限范围内)的水溶液作为对比溶液，将对比溶液和“自来水”等体积的待检测溶液分别加入所述的两份金纳米粒子溶液中，形成第一混合液和第二混合液；
(b)反应15分钟后，对比第二混合液与第一混合液的颜色，若存在颜色变化，则待检测的“自来水”溶液中存在钾离子，若不存在颜色变化，则待检测的“自来水”溶液中不存在钾离子，或者对比第二混合液与第一混合液的紫外可见吸收强度、峰值，若其紫外可见吸收强度、峰值发生变化，则待检测的“自来水”溶液中存在钾离子，若没有发生变化，则待检测的“自来水”溶液中不存在钾离子。
实施例5
“矿泉水”中钾离子的检测
(a)量取两份等体积相同的所制备金纳米粒子溶液；配制不含钾离子(在检测极限范围内)的水溶液作为对比溶液，将对比溶液和“矿泉水”等体积的待检测溶液分别加入所述的两份金纳米粒子溶液中，形成第一混合液和第二混合液；
(b)反应15分钟后，对比第二混合液与第一混合液的颜色，若存在颜色变化，则待检测的“矿泉水”溶液中存在钾离子，若不存在颜色变化，则待检测的“矿泉水”溶液中不存在钾离子，或者对比第二混合液与第一混合液的紫外可见吸收强度、峰值，若其紫外可见吸收强度、峰值发生变化，则待检测的“矿泉水”溶液中存在钾离子，若没有发生变化，则待检测的“矿泉水”溶液中不存在钾离子。
实施例6
“湖水”中钾离子的检测
(a)取所在地湖水10mL进行过滤，除去不溶性的悬浮物后将其作为待测溶液；配制不含钾离子(在检测极限范围内)的水溶液作为对比溶液；将对比溶液和等体积的待检测溶液分别加入等体积相同的所制备金纳米粒子溶液，形成第一混合液和第二混合液；
(b)反应15分钟后，对比第二混合液与第一混合液的颜色，若存在颜色变化，则待检测溶液中存在钾离子，若不存在颜色变化，则待检测溶液中不存在钾离子，或者对比第二混合液与第一混合液的紫外可见吸收光谱，若紫外可见吸收强度、峰值发生变化，则待检测溶液中存在钾离子，若没有发生变化，则待检测溶液中不存在钾离子。
实施例7
人体血液中钾离子的检测
(1)血液样品中钾离子的提取
将血液样品进行高速离心离心30min后，取上清液作为待检测溶液；
(2)血液样品中钾离子的检测
量取两份等体积相同的所制备金纳米粒子溶液；配制不含钾离子(在检测极限范围内) 的水溶液作为对比溶液，将对比溶液和等体积的待检测溶液分别加入所述的两份金纳米粒子溶液中，形成第一混合液和第二混合液；
反应15分钟后，对比第二混合液与第一混合液的颜色，若存在颜色变化，则待检测溶液中存在钾离子，若不存在颜色变化，则待检测溶液中不存在钾离子，或者对比第二混合液与第一混合液的紫外可见吸收光谱，若紫外可见吸收强度、峰值发生变化，则待检测溶液中存在钾离子，若没有发生变化，则待检测溶液中不存在钾离子。
实施例8
人体尿液中钾离子的检测
(1)人体尿液样品中钾离子的提取
将人体尿液进行高速离心离心30min后，取上清液作为待检测溶液；
(2)人体尿液样品中钾离子的检测
量取两份等体积相同的所制备金纳米粒子溶液；配制不含钾离子(在检测极限范围内) 的水溶液作为对比溶液，将对比溶液和等体积的待检测溶液分别加入所述的两份金纳米粒子溶液中，形成第一混合液和第二混合液；
反应15分钟后，对比第二混合液与第一混合液的颜色，若存在颜色变化，则待检测溶液中存在钾离子，若不存在颜色变化，则待检测溶液中不存在钾离子，或者对比第二混合液与第一混合液的紫外可见吸收光谱，若紫外可见吸收强度、峰值发生变化，则待检测溶液中存在钾离子，若没有发生变化，则待检测溶液中不存在钾离子。
以上所述的实施例对本发明的技术方案进行了详细说明，应理解的是以上所述仅为本发明的具体实施例，并不用于限制本发明，凡在本发明的原则范围内所做的任何修改和改进等，均应包含在本发明的保护范围之内。
Claims (3)
1.一种金纳米粒子的制备方法，其特征在于，所述制备方法包括以下步骤：
在圆底烧瓶中加入一定浓度的氯金酸水溶液，搅拌加热至沸腾，快速加入4'-氨基-二苯并-18-冠醚-6乙醇溶液和柠檬酸钠的水溶液，反应8-15分钟，溶液颜色由浅黄色变为红色，静置冷却至室温，制得金纳米粒子；
所述氯金酸水溶液的浓度为0.3～1.5mM；
所述的4'-氨基-二苯并-18-冠醚-6乙醇溶液的浓度为0.5mM；
所述的柠檬酸钠水溶液的浓度为0.8mM；
所述金纳米粒子水溶液的pH范围在2.5～6.5之间。
2.一种金纳米粒子，其特征在于，其根据权利要求1所述的制备方法制备。
3.一种如权利要求2所述的金纳米粒子的用途，其特征在于，所述金纳米粒子可用于湖水、自来水、矿泉水、人体血样或尿样中钾离子的快速检测，裸眼检测限为40μM，紫外光谱检测限为30μM。
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Effective date of registration: 20221223 Address after: No. 777, Zhongguan West Road, Zhuangshi Street, Ningbo City, Zhejiang Province 315000 Patentee after: Ningbo University Science Park Development Co.,Ltd. Address before: 315211, Fenghua Road, Jiangbei District, Zhejiang, Ningbo 818 Patentee before: Ningbo University |
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Application publication date: 20181207 Assignee: Ningbo Yongdian Technology Co.,Ltd. Assignor: Ningbo University Science Park Development Co.,Ltd. Contract record no.: X2023980033949 Denomination of invention: A kind of gold nanoparticles and its preparation method Granted publication date: 20211214 License type: Exclusive License Record date: 20230325 |
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Denomination of invention: A Kind of Gold Nanoparticle and Its Preparation Method Effective date of registration: 20231111 Granted publication date: 20211214 Pledgee: Ningbo Zhenhai Rural Commercial Bank Co.,Ltd. Zhuangshi Sub branch Pledgor: Ningbo University Science Park Development Co.,Ltd. Registration number: Y2023330002640 |