CN107356579B - 一种用纳米银催化共振散射光谱测定nh4+的方法 - Google Patents
一种用纳米银催化共振散射光谱测定nh4+的方法 Download PDFInfo
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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- G—PHYSICS
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
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- G01N21/64—Fluorescence; Phosphorescence
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Abstract
本发明公开了一种用纳米银催化共振散射光谱测定NH4 +的方法，其特征是，包括如下步骤：（1）制备已知浓度的NH4 +标准溶液体系；2、制备不含NH4 +的空白对照溶液体系；（3）计算ΔI=I‑I0；（4）以ΔI对NH4 +的浓度做工作曲线；（5）制备被测样品溶液，测定其共振散射峰强度值为I样品，计算ΔI样品=I样品‑I0；（6）依据步骤（4）的工作曲线，计算出样品溶液NH4 +的含量。这种方法采用配体调控纳米酶催化活性，方法简便、快速、灵敏度高。
Description
技术领域
本发明涉及分析化学领域，具体是一种用纳米银催化共振散射光谱测定NH4 +的方法。
背景技术
纳米酶是一种人工酶，又称纳米模拟酶，最早由Scrimin和Pasquato 提出，被用于描述具有显著核糖核酸酶活性的金簇。由于纳米研究领域的飞速发展以及纳米材料独特的物理化学性质，纳米酶的影响已经在无数领域普及开来，包括：生物传感、免疫分析、癌症诊断和治疗、神经保护、干细胞生长和污染物清除等。CeO2中存在三价和四价铈两种混合价态以及氧空缺，因而在各种应用中体现出极好的催化性能，鉴于纳米铈可以消除超氧化物自由基，研究其模拟超氧化物氧化酶的性质则十分合理，研究发现，具有氧空缺的纳米铈可以保护正常细胞免受辐射损伤但却对肿瘤细胞起不到任何作用，该“保护力”源自纳米铈具备消除自由基的能力，后续大量研究证实，纳米铈具有多种酶（超氧化物氧化酶、过氧化氢酶和氧化酶）的性质，其优越的消除自由基性质被广泛用于体内和体外生物学应用中。由于合成方法简便及功能化手段的发展，柠檬酸钠法制备的金纳米颗粒在各种应用中被广泛研究，曾经有报道考察纳米金的催化活性。但是，当Rossi和他的同事发现裸金可以凭借溶解氧氧化葡萄糖时，学术界还是十分震惊的，这个反应与葡萄糖氧化酶(GOX)催化类似，暗示金纳米颗粒可以作为GOX模拟物，该课题组也报道了相关的机理研究。基于得到的实验结果，他们提出Eley Rideal机理解释催化现象：葡萄糖首先吸附到金纳米颗粒的表面上；然后氧气靠近金属表面并与附着的葡萄糖反应产成葡萄糖酸和双氧水。金纳米酶的催化反应也遵从 Michaelis Menten动力学，但是天然酶的活性比纳米酶高55倍。纳米金颗粒不仅仅具有氧化物模拟酶性质，而且也可以显示过氧化物模拟酶性质。有文献报道合成了铁蛋白包裹的铂纳米颗粒并测试了材料消除活性氧的能力，在体外条件下，所制备的材料显示了较好的超氧化物歧化模拟酶活性并且具有长期的稳定性，利用铁蛋白介导的过程，材料进入细胞并在外部诱导应力的作用下增加细胞活力。以纳米颗粒的质量为标准且不考虑聚丙烯酸(PAA)对Pt纳米颗粒活性的影响，实验结果表明，Pt纳米颗粒的超氧化物歧化模拟酶活性要低于CeO2纳米颗粒，但是文章并没有对该实验现象从理论的角度做出解释。十六烷基三甲基溴化铵(CTAB)保护的 10nm Pt纳米立方体也被报道具有过氧化物模拟酶活性，催化反应为Eley Rideal机理。在双氧水存在与否的条件下，材料均可以氧化底物OPD和TMB，证实了其氧化物模拟酶和过氧化物模拟酶的性质，利用材料的模拟酶性质，通过免疫测试实现了小鼠白细胞介素2定量分析，随后，他们又发现 Au@Pt 纳米棒同样具有抗坏血酸氧化酶的活性，这可用于检测葡萄糖时消除抗坏血酸的干扰。
配体（ligand，也称为配基）是可与中心原子（金属或类金属）产生键结的原子、分子和离子，一般而言，配体在参与键结时至少会提供一个电子，配体扮演路易斯碱的角色，但在少数情况中配体接受电子，充当路易斯酸。以4-巯基苯甲酸为调控分子,对照巯基己醇,基于配体交换法对纳米金表面的寡核苷酸自组装进行调控,并用凝胶电泳进行表征的方法已有研究；铜离子是调控制备金纳米粒子的有效试剂，随着Cu2+增加浓度从0mmol/L到0.2mmol/L，金纳米颗粒的形状从棒变为立方体，浓度再增至1.6mmol/L，其形状变为十面体，该方法提出了一种基于选择性延迟平面生长速率的机制；另外，基于Hg2+配体调控赖氨酸修饰的纳米金的聚集,建立了线性范围在5nmol/L至100 nmol/L之间,检测限为3.6nmol/L简单的黄曲霉毒素可视化检测的方法，该方法可应用于大米等食品样品中黄曲霉素的定量检测。
铵盐是一类常用的无机化肥，在农作物中经常使用，过量的使用铵肥，对环境水质造成一定的污染，目前测定铵根的方法有滴定法、分光光度法、离子色谱法、荧光法等。滴定法是基于甲醛与铵根反应生成六亚甲基四胺和氢离子，再用NaOH滴定，同时要做氢离子的滴定以扣除氢离子消耗的NaOH，方法较为繁琐，对微量的铵根无法进行测定；离子色谱法，具有重现性好、准确度高等优点，但耗时、易受其他共存离子的干扰；荧光分析法具有操作简便、灵敏、快速的特点，但干扰因素多，分析过程较长；色谱法高校，但分离效果不稳定等。
共振散射光谱法（Resonance Scattering，简称RS）具有仪器简单、灵敏度高、所需样品量少、分析速度快等优点，受到人们青睐，被用于核酸检测、蛋白质分析、免疫分析及细胞器结构功能检测技术等。有关RS测定阴离子也有一些报道，基于当有NO2 -存在时，NO2 -与过量的I-反应生成I3 -，I3 -与AO形成缔合微粒，NO2 -浓度与共振散射光强度成正比，据此可建立NO2 -的共振散射光谱分析法，检测限为0.068 mg/L；基于抗坏血酸将Cu(Ⅱ)还原为Cu(Ⅰ)，Cu(Ⅰ)进一步与SCN-形成CuSCN沉淀，建立了测定SCN-的共振光散射新方法，检出限为0.167mg/L。根据维生素B1与氯酚红结合生成的缔合物使共振散射显著增强并产生新的共振散射光谱，最大共振散射峰位于339nm处，维生素B1的质量浓度在0.03-0.42mg/L内与其对应的共振散射增强值呈线性关系，检出限为0.0042mg/L。目前尚未见采用四苯硼钠配体调控纳米酶催化的共振散射光谱方法测定铵根离子的报道。
发明内容
本发明的目的是针对测定NH4 +现有技术的不足，而提供一种用纳米银催化共振散射光谱测定NH4 +的方法。这种方法采用配体反应调控纳米酶催化活性，方法简便、快速、灵敏度高。
实现本发明目的的技术方案是：
一种用纳米银催化共振散射光谱测定NH4 +的方法，包括如下步骤：
（1）制备已知浓度的NH4 +标准溶液体系：于刻度试管中，依次加入25μL-500μL 10μmol/L的NH4 +标准溶液、10μL-50μL 0.1mmol/L纳米银、450μL-550μL 10µmol/L的四苯硼钠溶液、30μL-100μL 0.3 mol/L的葡萄糖、100μL-200μL 1 mmol/L AgNO3和10μL-50μL 0.5mol/L NaOH溶液，于60℃水浴反应6分钟，摇匀，然后冰水冷却至室温，加入80μL-150μL1mol/L NaCl，用二次蒸馏水定容至2.0 mL；
（2）制备空白对照溶液体系：用步骤（1）的方法不加NH4 +标准溶液制备空白对照溶液体系；
（3）分别取按步骤（1）、(2）制备的NH4 +标准溶液体系及空白对照溶液体系倾入石英比色皿中，在荧光光谱仪上，设定仪器参数，扫描获得体系的共振散射光谱，测定420nm处的共振散射峰强度值为I，同时测定空白对照溶液体系的共振散射峰强度值为I0，计算ΔI =I - I0；
（4）以ΔI对NH4 +的浓度关系做工作曲线；
（5）依照步骤（1）的方法制备样品溶液，其中加入的NH4 +标准溶液替换为样品溶液，并按步骤（3）的方法测定样品溶液的共振散射峰强度值为I样品，计算ΔI样品= I样品- I0；
（6）依据步骤（4）的工作曲线，计算出样品溶液NH4 +的含量。
步骤（1）中所述纳米银的制备方法是：在一个50m L三角烧瓶中加入44mL二次蒸馏水，按顺序加入2mL 10mmol/L AgNO3，3mL 60mmol/L柠檬酸三钠溶液，600µL 30% H2O2，600µL 0.1mol/L NaBH4溶液，混匀，用玻璃棒搅拌至溶液颜色变蓝，静置，制得蓝色纳米银胶，立即将其转入微波炉中，用800W功率微波90s，得到红色棒状纳米银胶，用二次蒸馏水定容至50mL，其浓度以Ag计为0.4mmol/L，用前用二次蒸馏水稀释至0.1mmol/L，该棒状纳米银的制备方法为现有技术。
在本技术方案条件下，纳米银对葡萄糖-AgNO3生成银纳米粒子这一反应具有较强的催化作用，当四苯硼钠包裹在纳米银纳米酶表面时，抑制了葡萄糖-AgNO3生成银纳米粒子这一反应，当体系加入NH4 +时，NH4 +与四苯硼钠反应生成(C6H5)4BNH4并从纳米银纳米酶表面脱离，纳米银催化活性恢复，体系中随着NH4 +浓度的增大，纳米银催化活性增强，生成的银纳米粒子增多，NH4 +浓度与体系共振散射峰增强值呈一定的线性关系，据此建立测定NH4 +的四苯硼钠调控纳米银活性共振散射光谱方法。
这种方法的优点是：与现有的方法相比，本测定方法采用配体调控纳米酶催化活性，方法简便、快速、灵敏度高。
附图说明
图1为实施例中的共振散射光谱图。
图中，a.0.75µmol/L Ag+2.5µmol/L (C6H5)4BNa+7.5mmol/L葡萄糖+75µmol/LAgNO3+6.25mmol/L NaOH +50 mmol/L NaCl b. a+125nmol/L NH4 + c. a+750nmol/L NH4 +d.a+ 1500nmol/L NH4 + e.a+ 2000 nmol/L NH4 + f.a+ 2500nmol/L NH4 +。
具体实施方式
下面结合实施例和附图对本发明内容作进一步的阐述，但不是对本发明的限定。
实施例：
一种用纳米银催化共振散射光谱测定NH4 +的方法，包括如下步骤：
（1）制备已知浓度的NH4 +标准溶液体系：于5支刻度试管中，分别加入25μL、150μL、300μL、400μL、500μL 10μmol/L的NH4 +标准溶液，然后每支刻度试管中再依次加入15μL 0.1mmol/L纳米银、500 μL 10µmol/L的四苯硼钠溶液、50 µL 0.3 mol/L的葡萄糖、150μL 1mmol/L AgNO3和25μL 0.5 mol/L NaOH溶液，于60℃水浴反应6分钟，摇匀，然后冰水冷却至室温，加入100 µL 1mol/L NaCl，用二次蒸馏水定容至2.0 mL；
（2）制备空白对照溶液体系：用步骤（1）的方法不加NH4 +标准溶液制备空白对照溶液体系；
（3）分别取按步骤（1）、(2）制备的NH4 +标准溶液体系及空白对照溶液体系倾入石英比色皿中，在F-7000型荧光光谱仪上，设定仪器参数检测器电压为350V, 狭缝为2 nm，同步扫描激发波长和发射波长，获得体系的共振散射光谱如图1，测定420nm处的共振散射峰强度值为I，同时测定空白对照溶液体系的共振散射峰强度值为I0，计算ΔI = I - I0；
（4）以ΔI对NH4 +的浓度关系做工作曲线，获得线性回归方程为ΔI = 0.928C-0.54，其中NH4 +浓度C的单位为nmol/L，测定线性范围为125-2500nmol/L，检出限为41.2nmol/L；
（5）样品测定：取某氨水厂附近排放的废水，用滤纸过滤，量取适量滤液，依照步骤（1）的方法制备被测样品，其中加入的NH4 +标准溶液替换为被测样品，按步骤（2）-（4）操作，算出被测样品的ΔI 样品= I 样品- I 0；
（6）依据步骤（4）的工作曲线，计算出被测样品NH4 +的含量为152.3 nmol/L。
本例步骤（1）中所述纳米银的制备方法是：在一个50m L三角烧瓶中加入44mL二次蒸馏水，按顺序加入2mL 10mmol/L AgNO3，3mL 60mmol/L柠檬酸三钠溶液，600µL 30% H2O2，600µL 0.1mol/L NaBH4溶液，混匀，用玻璃棒搅拌至溶液颜色变蓝，静置，制得蓝色纳米银胶，立即将其转入微波炉中，用800W功率微波90s，得到红色棒状纳米银胶，用二次蒸馏水定容至50mL，其浓度以Ag计为0.4mmol/L，用前用二次蒸馏水稀释至0.1mmol/L。
本技术方案检测方法的验证：
取上述实施例步骤（5）中的废水样三份，加入浓度为100 nmol/L的NH4 +标准溶液，进行加标回收实验，求得回收率分别为97.4%、98.6%、99.1%，相对标准偏差为3.7%。
说明该技术方案方法准确可靠。
Claims (1)
1.一种用纳米银催化共振散射光谱测定NH4 +的方法，其特征是，包括如下步骤：
（1）制备已知浓度的NH4 +标准溶液体系：于刻度试管中，依次加入25μL-500μL 10μmol/L的NH4 +标准溶液、10μL-50μL 0.1mmol/L纳米银、450μL-550μL 10µmol/L的四苯硼钠溶液、30μL-100μL 0.3 mol/L的葡萄糖、100μL-200μL 1 mmol/L AgNO3和10μL-50μL 0.5 mol/LNaOH溶液，于60℃水浴反应6分钟，摇匀，然后冰水冷却至室温，加入80μL-150μL 1mol/LNaCl，用二次蒸馏水定容至2.0 mL；
（2）制备空白对照溶液体系：用步骤（1）的方法不加NH4 +标准溶液制备空白对照溶液体系；
（3）分别取按步骤（1）、(2）制备的NH4 +标准溶液体系及空白对照溶液体系倾入石英比色皿中，在荧光光谱仪上，设定仪器参数，扫描获得体系的共振散射光谱，测定420nm处的共振散射峰强度值为I，同时测定空白对照溶液体系的共振散射峰强度值为I0，计算ΔI = I -I0；
（4）以ΔI对NH4 +的浓度关系做工作曲线；
（5）依照步骤（1）的方法制备样品溶液，其中加入的NH4 +标准溶液替换为样品溶液，并按步骤（3）的方法测定样品溶液的共振散射峰强度值为I样品，计算ΔI样品 = I样品 - I0；
（6）依据步骤（4）的工作曲线，计算出样品溶液NH4 +的含量。
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