CN110907405A - 一种基于四羧基镍酞菁测定痕量过氧化氢的方法 - Google Patents

一种基于四羧基镍酞菁测定痕量过氧化氢的方法 Download PDF

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CN110907405A
CN110907405A CN201911175379.9A CN201911175379A CN110907405A CN 110907405 A CN110907405 A CN 110907405A CN 201911175379 A CN201911175379 A CN 201911175379A CN 110907405 A CN110907405 A CN 110907405A
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hydrogen peroxide
solution
scattering intensity
mol
resonance scattering
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唐宁莉
王文平
梁文汇
慕欣悦
付慧云
方业毅
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Guilin University of Technology
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Guilin University of Technology
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N21/49—Scattering, i.e. diffuse reflection within a body or fluid
    • G01N21/51—Scattering, i.e. diffuse reflection within a body or fluid inside a container, e.g. in an ampoule
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

本发明公开了一种基于四羧基镍酞菁测定痕量过氧化氢的方法。于7支比色管中，分别加入HAc‑NaAc缓冲液、NiC4Pc溶液和 OPD溶液，再依次加入0.0、0.0017、0.0025、0.005、0.01、0.02、0.04mL 1.97×10‑5mol/L H2O2溶液，于25℃水浴中反应15min后，再在每支管中加入纳米金溶液，4分钟后用二次蒸馏水稀释至5mL，于荧光光度计上以λex=λem的方式扫描散射光谱。在700nm波长处分别测定加有H2O2溶液的散射强度I700nm和不加H2O2的试剂空白的散射强度I0，计算散射强度差值ΔI700nm=I700nm‑I0。本发明测定方法选择性好、灵敏度高。

Description

一种基于四羧基镍酞菁测定痕量过氧化氢的方法
技术领域
本发明涉及痕量过氧化氢的测定方法，特别是基于四羧基镍酞菁测定过氧化氢的共振散射光谱法。
背景技术
过氧化氢是一种常见的消毒剂和漂白剂，常被用于食品、制药、临床医学、有机合成和环境分析等行业。但同时过氧化氢也具有一定危害性，长期接触引起呼吸及皮肤疾病、加快人体的衰老和诱发基因突变等。因此，建立过氧化氢简便、快速和经济的监测方法十分重要。常用于检测过氧化氢的方法包括：滴定分析法、分光光度法、液相色谱法、电化学法、荧光光度法、共振散射光谱法等。共振散射光谱法具有操作简单、灵敏度高、检出限低等优点，而将共振散射光谱技术与酶催化反应相结合可进一步提高检测的灵敏度。四羧基镍酞菁(NiC4Pc)具有过氧化氢模拟酶的性质，它可在弱酸性溶液中催化过氧化氢氧化邻苯二胺(OPD)，生成中间产物2,3-二氨基-5,10-二氢吩嗪和最终产物2,3-二氨基吩嗪，2种产物均可诱导纳米金发生聚集，导致反应体系的共振散射信号增强，根据反应前后体系共振散射强度的变化可建立定量测定过氧化氢的方法，目前此方法尚未见报道。
发明内容
本发明的目的是提供一种基于四羧基镍酞菁测定痕量过氧化氢的共振散射光谱法。
具体步骤为：
于7支5mL比色管中，分别加入0.06～0.10mL pH＝5.4的醋酸-醋酸钠(HAc-NaAc)缓冲液，0.01～0.08mL浓度为1.0×10-6mol/L的四羧基镍酞菁(NiC4Pc)溶液，0.04～0.08mL浓度为0.01mol/L的邻苯二胺(OPD)溶液，然后依次加入0.0、0.0017、0.0025、0.005、0.01、0.02、0.04mL浓度为1.97×10-5mol/L的过氧化氢溶液，摇匀，于25℃水浴中反应15分钟后，再在每支比色管中加入0.3～0.7mL浓度为58.0μg/mL的纳米金(AuNPs)溶液，摇匀，放置3～5分钟后，用二次蒸馏水稀释至刻度，用1cm石英比色皿于荧光光度计上以λex＝λem的方式扫描共振散射光谱。在700nm波长处分别测定加有过氧化氢溶液的共振散射强度I700nm和不加过氧化氢的试剂空白溶液的共振散射强度I0，计算共振散射强度的差值ΔI700nm＝I700nm-I0，其共振散射强度的差值ΔI700nm与过氧化氢浓度c在6.90×10-9～1.576×10-7mol/L范围内成线性关系，线性回归方程为ΔI＝1.530×109c+1.727，相关系数0.9995，检出限2.16×10-9mol/L；另取池塘水、新鲜雨水和河水过滤，取0.2mL滤液同法测定共振散射强度值，计算出池塘水、新鲜雨水和河水中过氧化氢的含量。
本发明测定方法选择性好、灵敏度高。
附图说明
图1为本发明实施例空白与78.8×10-9mol/L过氧化氢的共振散射光谱图；
图中标记：a：空白；b：pH5.4 HAc-NaAc缓冲液-0.01mol/L OPD-1.0×10-6mol/LNiC4Pc-78.8×10-9mol/L H2O2-AuNPs。
具体实施方式
实施例：
于7支5mL比色管中，分别加入0.09mL pH＝5.4HAc-NaAc缓冲溶液、0.04mL浓度为1.0×10-6mol/L的NiC4Pc溶液和0.06mL浓度为0.01mol/L的OPD溶液，然后依次加入0.0、0.0017、0.0025、0.005、0.01、0.02、0.04mL浓度为1.97×10-5mol/L的过氧化氢溶液，摇匀，于25℃水浴中反应15分钟后，再在每支比色管中加入0.5mL浓度为58.0μg/mL的纳米金溶液，用二次蒸馏水稀释至刻度，摇匀，放置4分钟后，用1cm石英比色皿于荧光光度计上以λex＝λem的方式扫描共振散射光谱。在700nm波长处分别测定加有过氧化氢溶液的共振散射强度I700nm和不加过氧化氢的试剂空白溶液的共振散射强度I0，计算共振散射强度的差值ΔI700nm＝I700nm-I0，其共振散射强度的差值ΔI700nm与过氧化氢浓度c在6.90×10-9～1.576×10-7mol/L范围内成线性关系，线性回归方程为ΔI＝1.530×109c+1.727，相关系数0.9995，检出限2.16×10-9mol/L；另取池塘水、新鲜雨水和河水过滤，取0.2mL滤液同法测定共振散射强度值，代入上述回归方程中，计算出池塘水、新鲜雨水和河水中过氧化氢的含量。同时做了加标回收实验，结果见表1。
表1水样分析结果(n＝5)
样品 测定值(10<sup>-7</sup>mol/L) 回收率(％) RSD(％)
池塘水 13.89 95.85 2.72
雨水 7.156 94.82 1.45
河水 3.156 95.41 1.56
。

Claims (1)

1.一种测定痕量过氧化氢的方法，其特征在于具体步骤为：
于7支5mL比色管中，分别加入0.06～0.10mL pH=5.4的醋酸-醋酸钠缓冲液，0.01～0.08mL浓度为 1.0×10-6 mol/L的四羧基镍酞菁溶液，0.04～0.08mL 浓度为0.01mol/L的邻苯二胺溶液，然后依次加入0.0、0.0017、0.0025、0.005、0.01、0.02、0.04mL 浓度为1.97×10-5mol/L的过氧化氢溶液，摇匀，于25℃水浴中反应15分钟后，再在每支比色管中加入0.3～0.7mL L浓度为58.0μg/mL的纳米金溶液，摇匀，放置3～5分钟后，用二次蒸馏水稀释至刻度，用1cm石英比色皿于荧光光度计上以λex=λem的方式扫描共振散射光谱；在700nm波长处分别测定加有过氧化氢溶液的共振散射强度I700nm和不加过氧化氢的试剂空白溶液的共振散射强度I0，计算共振散射强度的差值ΔI700nm =I700nm-I0，其共振散射强度的差值ΔI700nm与过氧化氢浓度c在6.90×10-9～1.576×10-7 mol/L范围内成线性关系，线性回归方程为ΔI=1.530×109c+1.727，相关系数0.9995，检出限2.16×10-9 mol/L；另取池塘水、新鲜雨水和河水过滤，取0.2 mL滤液同法测定共振散射强度值，计算出池塘水、新鲜雨水和河水中过氧化氢的含量。
CN201911175379.9A 2019-11-26 2019-11-26 一种基于四羧基镍酞菁测定痕量过氧化氢的方法 Pending CN110907405A (zh)

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CN1207173A (zh) * 1995-10-30 1999-02-03 株式会社京都第一科学 物质的测定方法及试片
GB9914983D0 (en) * 1999-06-28 1999-08-25 Procter & Gamble Detergent compositions
CN1546457A (zh) * 2003-12-18 2004-11-17 北京工业大学 仿生催化氧气氧化邻硝基甲苯制备邻硝基苯甲醛的方法
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Application publication date: 20200324