CN109503565A - 一种镉离子检测试剂及其制备方法和应用 - Google Patents

一种镉离子检测试剂及其制备方法和应用 Download PDF

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CN109503565A
CN109503565A CN201811646412.7A CN201811646412A CN109503565A CN 109503565 A CN109503565 A CN 109503565A CN 201811646412 A CN201811646412 A CN 201811646412A CN 109503565 A CN109503565 A CN 109503565A
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detection reagent
cadmium ion
ion detection
methanol
cadmium
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CN109503565B (zh
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徐括喜
万方霞
程春
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Henan Kun And Information Technology Co Ltd
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D413/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and oxygen atoms as the only ring hetero atoms
    • C07D413/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and oxygen atoms as the only ring hetero atoms containing two hetero rings
    • C07D413/12—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and oxygen atoms as the only ring hetero atoms containing two hetero rings linked by a chain containing hetero atoms as chain links
    • G—PHYSICS
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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
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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    • C09K2211/1025—Heterocyclic compounds characterised by ligands
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    • G—PHYSICS
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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
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N2021/6432—Quenching

Abstract

本发明一种镉离子检测试剂，只需要一步高收率合成所述镉离子检测试剂，以甲醇为溶剂，把原料醛和邻氨基苯酚溶于甲醇中，然后加热回流的条件下反应12h，经过滤、甲醇洗涤2‑3次，减压除去甲醇，得到所述镉离子检测试剂。

Description

一种镉离子检测试剂及其制备方法和应用
技术领域
本发明属于金属离子检测领域，具体涉及一种镉离子检测试剂及其制备方法和应用。
背景技术
铁是生命体中必需元素之一,在生物体的生命活动中起着举足轻重的作用,涉及生物体的各项生理活动,如肌肉的收缩、DNA和RNA的合成、酶催化、神经传导、细胞内渗透压调节以及维持酸碱平衡等.细胞内铁含量的减少会导致生命体系的紊乱,而过量的铁同样对机体是有害甚至是致命的.因此,实现高选择性、高灵敏度地在活细胞中检测铁显得极其重要.现在常用的检测铁离子(III)的方法主要有原子吸收法、分光光度法、电感耦合等离子体发射光谱法、电感耦合等离子体质谱法、电化学法及荧光分析法等,这些方法各有优缺点。近几年,荧光探针法受到了极大的关注,由于该技术不仅操作简单、成本低、灵敏度高、选择性好、响应时间短等方面有突出优点.因此，对它的研究和探索，对于金属离子的定性和定量检测领域有着非常重要的意义，对开发新型铁离子(III)检测试剂也会产生很大的影响。
发明内容
本发明的目的是提供一种镉离子检测试剂及其制备方法和应用。
为实现上述目的，本发明采用的技术方案是，一种镉离子检测试剂，所述镉离子检测试剂的结构如下：
只需一步合成所述镉离子检测试剂；以甲醇为溶剂，原料醛和邻氨基苯酚在加热回流的条件下反应12h，过滤、洗涤、减压除去甲醇，得到化合物镉离子检测试剂；其结构式如下：
本发明产生的有益效果是：本发明提供的镉检测试剂具有能在水溶液中定性和定量地检出镉的性能，具有定性和定量地检出镉的应用前景，检出极限可达5.82×10-8M；并且本发明的镉离子检测试剂制备工艺简单，收率达86％以上。
具体实施方式
以下以具体实施例来说明本发明的技术方案，但本发明的保护范围不限于此。
实施例1
实施例1的镉离子检测试剂的合成路线如下：
镉离子检测试剂的具体合成过程如下：取原料醛(1.0mmol)和邻氨基苯酚(1.0mmol) 加入10mL的甲醇中，然后在氮气保护下加热回流的条件下反应12h，过滤产生的浅黄色沉淀后经甲醇(3×5mL)洗涤，经减压除去溶剂得镉离子检测试剂，收率为86％。
目标产物的表征结果如下：
1)红外光谱测定：
用溴化钾压片法在400～4000cm–1范围内用美国Nicolet magna 750傅里叶红外光谱仪测定。所得化合物的主要红外吸收峰为：3372,2924,1662,1507,1473,1255,692cm-1.
2)核磁共振氢谱测定：
用氘代二甲亚砜为溶剂，四甲基硅烷为内标，用Bruker400核磁共振波谱仪测定氢谱。所得化合物的核磁共振氢谱为：
10.08(s,1H),9.88(s,1H),8.37(s,1H),8.25(d,J＝4.0Hz,1H),7.82(d,J＝4.0Hz,1H), 7.69(s,1H),7.69–7.51(m,4H),7.35(d,J＝4.0Hz,1H),7.24–7.06(m,6H),5.28(s,2H).
3)核磁共振碳谱测定：
用氘代二甲亚砜为溶剂，四甲基硅烷为内标，用Bruker400核磁共振波谱仪测定碳谱。所得化合物的核磁共振碳谱为：159,157,155,152,151,148,138,137,135,133,132,131,129,128,128,125,122,119,117,116,115,113,111,110,73.
4)高分辨质谱测定：
高分辨质谱用美国Thermo Scientific LTQ Orbitrap XL质谱仪测定：所得化合物的质谱为：438.1446[M+H]+(理论值：438.1448)。
目标镉离子检测试剂在检测镉中的应用
将镉离子检测试剂配制成1.0×10-5mmol/L的DMSO溶液。在对分别含有(Li+,Na+,K+,Ag+,Mg2+,Ca2+,Ba2+,Pb2+,Zn2+,Co2+,Cd2+,Hg2+,Ni2+,Cu2+,Mn2+,Fe2+,Cr3+,Al3+, Fe3+和Eu3+等)的DMSO溶液为检测对象。结果表明：在入镉离子时，检测试剂的荧光猝灭，而加入其它离子时检测试剂的荧光几乎不变。实验中，取3mL镉离子检测试剂加入到比色皿中，然后加入到含不同种类和浓度的金属离子均匀混合，测定各组溶液的荧光数据。经荧光滴定和拟合计算得测定其检出极限可达5.82×10-8M。本发明的镉离子检测试剂可定性和定量地检测镉离子。

Claims (3)

1.一种镉离子检测试剂，其特征在于，所述镉离子检测试剂的结构如下：
2.如权利要求1所述镉离子检测试剂制备方法，其特征在于只需要一步高收率合成所述镉离子检测试剂。
以甲醇为溶剂，把原料醛和邻氨基苯酚溶于甲醇中，然后加热回流的条件下反应12h，经过滤、甲醇洗涤2-3次，减压除去甲醇，得到所述镉离子检测试剂。
3.如权利要求1所述镉离子检测试剂在检测镉中的应用。
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CN110317175A (zh) * 2019-06-26 2019-10-11 山西大学 一种萘衍生物及其合成方法和应用
CN112250674A (zh) * 2020-10-27 2021-01-22 山西大学 一种2，3-二氨基吩嗪衍生物及其合成方法和应用

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Publication number Priority date Publication date Assignee Title
CN110317175A (zh) * 2019-06-26 2019-10-11 山西大学 一种萘衍生物及其合成方法和应用
CN110317175B (zh) * 2019-06-26 2021-11-19 山西大学 一种萘衍生物及其合成方法和应用
CN112250674A (zh) * 2020-10-27 2021-01-22 山西大学 一种2，3-二氨基吩嗪衍生物及其合成方法和应用

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