流动注射化学发光分析法的应用
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摘要
流动注射-化学发光分析方法是分析化学研究中被广泛使用的高效的测试手段，它具有灵敏度高、响应快、操作简便和动态分析范围宽等优点。在本论文中，我们利用流动注射-化学发光分析方法的优势，建立了一些更有效的分析方法来检测一些化学和生物物质，并利用具有独特性能的纳米粒子来提高所建立的分析方法的灵敏度。此外，我们还探讨了在待测物测定过程中的反应机理。主要研究内容包括：
（1）高灵敏的流动注射化学发光法检测血液中的血红蛋白
在这一章中，我们建立了一个高灵敏的流动注射化学发光分析体系用于定量检测血红蛋白。该方法是基于血红蛋白和碲化镉量子点能增强过氧化氢-亚铁氰化钾-荧光素发光体系的信号来检测血红蛋白的含量。
（2）利用流动注射化学发光法检测杀虫剂中的氨基硫脲成分
在这一章中，我们成功的建立了一个简单快速的流动注射化学发光分析体系用于检测杀虫剂中的氨基硫脲成分。主要机理是氨基硫脲成分可以抑制在酸性介质中高锰酸钾-亚硫酸钠反应所产生的化学发光信号。
（3）利用高锰酸钾-鲁米诺-碲化镉纳米粒子化学发光体系检测药品中的生物素
由于生物素和亲和素间具有高的亲和力，因此表面修饰有亲和素的聚苯乙烯微球可以吸附生物素。利用生物素能增强高锰酸钾-鲁米诺-碲化镉纳米粒子体系的化学发光信号的特性，建立了对生物素定量分析的新方法。
（4）利用高锰酸钾-鲁米诺-流动注射-化学发光体系检测葡萄糖
我们利用葡萄糖可以增强高锰酸钾-鲁米诺碱性体系中的化学发光信号的这一特性，建立了对葡萄糖检测的分析方法。在优化条件下，化学发光信号和葡萄糖浓度具有良好的线性关系，本方法对葡萄糖的检测范围是2.3×10-87.2×10-5M，检出限(3σ)是1.2×10-9M，11次测量的相对标准偏差为2.12％。
The chemiluminescence analysis in combination with flow-injection techniqueappears as a potent versatile tool for analytical chemistry. This versatility is due to itsmultiple advantages such as sensitivity, rapidity, simplicity and the wideness of itdynamic analytical range. In this study, these benefits are put to good use to developmore efficient methods for different chemical or biological compounds determination.The main content includes:
(1) Sensitive flow‐injection chemiluminescence determination of hemoglobin in the human blood.
In this work, a sensitive and simple flow-injection chemiluminescence methodwas developed for quantitative analysis of hemoglobin. The method is based onthe ability of hemoglobin to enhance the chemiluminescent signal generated byH2O2-K4Fe(CN)6-fluorescein alkaline system enhanced by CdTe quantum dots.Under the optimized conditions, hemoglobin has be detected in concentrationrange of7.35×10-9-2.5×10-6mol.L-1with a detection limit (3σ) of1.8×10-9mol.L-1,and the relative standard deviation（for5×10-7mol.L-1hemoglobin） of2.06%(n=11). The present chemiluminescence method has been successfully appliedfor the determination of hemoglobin in three kinds of blood samples taken frominfant, adult man, adult woman and two reference samples. Compared withprevious reports, the chemiluminescence method described in this work is simpleand rapid with high sensitivity.
(2) Flow‐injection chemiluminescence determination of thiosemicarbazyl compounds in the insecticides
In this work a simple and rapid flow-injection chemiluminescence method isreported for the thiosemicarbazyl compounds determination in the insecticides. It was found that the thiosemicarbazyl compounds have the behavior to inhibit theCL signal generated by KMnO4-Na2SO3system in the acidic medium. Thelinearly correlation between the generated CL and the concentration logarithmwas detected in the range of7.3×10-9-5.4×10-7M for thiosemicarbazide，and6.8×10-9-3.6×10-7M for the thiosemicarbazone; with the relative standarddeviations (for12measurements) of2.3%and2.6%respectively. The limits ofdetection (3б) are2.2×10-10M and1.8×10-10M respectively. The influences ofdifferent physic-chemical parameters have been studied. The sample throughput is100samples/h. The proposed method has been used to determine thethiosemicarbazide in the synthetic samples with satisfactory result. To prove thepractice use of the method, it was applied to determine the thiosemicarbazide andthiosemicarbazone concentrations in the insecticides.
(3) Determination of biotin in pharmaceutical formulations by potassiumpermanganate-luminol-CdTe nanoparticles chemiluminescence system
In this work, a sensitive flow–injection chemiluminescence method has beendeveloped for the determination of biotin in the pharmaceutical formulations. Theaffinity between avidin and biotin was used to adsorb biotin on the surface ofpolystyrene, with subsequent quantification of biotin based on its ability toenhance the chemiluminescence (CL) signal generated by the redox reaction ofpotassium permanganate-luminol-CdTe nanoparticles chemiluminescence system.The investigations prove that apart from3-aminophthalate, the CdTe quantum dots(QDs) play both of catalytic and emitter roles Under optimum conditions, thelinear range for the determination of biotin was1×10-2ng/mL to25ng/mL with adetection limit of7.3×10-3ng/mL (S/N=3). The relative standard deviation of5ng/L biotin was2.06%(n=7). The proposed method was successfully used todetermine the biotin concentration in the pharmaceutical formulations and therecovery was between96.4and104%. The proposed method is simple, convenient,rapid and sensitive.
(4) Flow-injection chemiluminescence determination of glucose using potassiumpermanganate-luminol system
In this work, a new flow-injection chemiluminescence method was developed for thedetermination of glucose in physiologic liquids, which is based on the enhancementeffect of glucose on the chemiluminescence signal generated by KMnO4-luminolsystem in alkaline medium. Under optimized conditions, a linear correlation wasestablished between the chemiluminescence intensity and the glucose concentration inthe range of2.3×10-8to7.2×10-5M with a detection limit (3σ) of1.2×10-9M. Therelative standard deviation for11measurements is2.12%. The method was applied todetermine the glucose concentration in the human serum samples and the results areconsistent with those obtained by the standard spectrometric method.
（1）高灵敏的流动注射化学发光法检测血液中的血红蛋白
在这一章中，我们建立了一个高灵敏的流动注射化学发光分析体系用于定量检测血红蛋白。该方法是基于血红蛋白和碲化镉量子点能增强过氧化氢-亚铁氰化钾-荧光素发光体系的信号来检测血红蛋白的含量。
（2）利用流动注射化学发光法检测杀虫剂中的氨基硫脲成分
在这一章中，我们成功的建立了一个简单快速的流动注射化学发光分析体系用于检测杀虫剂中的氨基硫脲成分。主要机理是氨基硫脲成分可以抑制在酸性介质中高锰酸钾-亚硫酸钠反应所产生的化学发光信号。
（3）利用高锰酸钾-鲁米诺-碲化镉纳米粒子化学发光体系检测药品中的生物素
由于生物素和亲和素间具有高的亲和力，因此表面修饰有亲和素的聚苯乙烯微球可以吸附生物素。利用生物素能增强高锰酸钾-鲁米诺-碲化镉纳米粒子体系的化学发光信号的特性，建立了对生物素定量分析的新方法。
（4）利用高锰酸钾-鲁米诺-流动注射-化学发光体系检测葡萄糖
我们利用葡萄糖可以增强高锰酸钾-鲁米诺碱性体系中的化学发光信号的这一特性，建立了对葡萄糖检测的分析方法。在优化条件下，化学发光信号和葡萄糖浓度具有良好的线性关系，本方法对葡萄糖的检测范围是2.3×10-87.2×10-5M，检出限(3σ)是1.2×10-9M，11次测量的相对标准偏差为2.12％。
The chemiluminescence analysis in combination with flow-injection techniqueappears as a potent versatile tool for analytical chemistry. This versatility is due to itsmultiple advantages such as sensitivity, rapidity, simplicity and the wideness of itdynamic analytical range. In this study, these benefits are put to good use to developmore efficient methods for different chemical or biological compounds determination.The main content includes:
(1) Sensitive flow‐injection chemiluminescence determination of hemoglobin in the human blood.
In this work, a sensitive and simple flow-injection chemiluminescence methodwas developed for quantitative analysis of hemoglobin. The method is based onthe ability of hemoglobin to enhance the chemiluminescent signal generated byH2O2-K4Fe(CN)6-fluorescein alkaline system enhanced by CdTe quantum dots.Under the optimized conditions, hemoglobin has be detected in concentrationrange of7.35×10-9-2.5×10-6mol.L-1with a detection limit (3σ) of1.8×10-9mol.L-1,and the relative standard deviation（for5×10-7mol.L-1hemoglobin） of2.06%(n=11). The present chemiluminescence method has been successfully appliedfor the determination of hemoglobin in three kinds of blood samples taken frominfant, adult man, adult woman and two reference samples. Compared withprevious reports, the chemiluminescence method described in this work is simpleand rapid with high sensitivity.
(2) Flow‐injection chemiluminescence determination of thiosemicarbazyl compounds in the insecticides
In this work a simple and rapid flow-injection chemiluminescence method isreported for the thiosemicarbazyl compounds determination in the insecticides. It was found that the thiosemicarbazyl compounds have the behavior to inhibit theCL signal generated by KMnO4-Na2SO3system in the acidic medium. Thelinearly correlation between the generated CL and the concentration logarithmwas detected in the range of7.3×10-9-5.4×10-7M for thiosemicarbazide，and6.8×10-9-3.6×10-7M for the thiosemicarbazone; with the relative standarddeviations (for12measurements) of2.3%and2.6%respectively. The limits ofdetection (3б) are2.2×10-10M and1.8×10-10M respectively. The influences ofdifferent physic-chemical parameters have been studied. The sample throughput is100samples/h. The proposed method has been used to determine thethiosemicarbazide in the synthetic samples with satisfactory result. To prove thepractice use of the method, it was applied to determine the thiosemicarbazide andthiosemicarbazone concentrations in the insecticides.
(3) Determination of biotin in pharmaceutical formulations by potassiumpermanganate-luminol-CdTe nanoparticles chemiluminescence system
In this work, a sensitive flow–injection chemiluminescence method has beendeveloped for the determination of biotin in the pharmaceutical formulations. Theaffinity between avidin and biotin was used to adsorb biotin on the surface ofpolystyrene, with subsequent quantification of biotin based on its ability toenhance the chemiluminescence (CL) signal generated by the redox reaction ofpotassium permanganate-luminol-CdTe nanoparticles chemiluminescence system.The investigations prove that apart from3-aminophthalate, the CdTe quantum dots(QDs) play both of catalytic and emitter roles Under optimum conditions, thelinear range for the determination of biotin was1×10-2ng/mL to25ng/mL with adetection limit of7.3×10-3ng/mL (S/N=3). The relative standard deviation of5ng/L biotin was2.06%(n=7). The proposed method was successfully used todetermine the biotin concentration in the pharmaceutical formulations and therecovery was between96.4and104%. The proposed method is simple, convenient,rapid and sensitive.
(4) Flow-injection chemiluminescence determination of glucose using potassiumpermanganate-luminol system
In this work, a new flow-injection chemiluminescence method was developed for thedetermination of glucose in physiologic liquids, which is based on the enhancementeffect of glucose on the chemiluminescence signal generated by KMnO4-luminolsystem in alkaline medium. Under optimized conditions, a linear correlation wasestablished between the chemiluminescence intensity and the glucose concentration inthe range of2.3×10-8to7.2×10-5M with a detection limit (3σ) of1.2×10-9M. Therelative standard deviation for11measurements is2.12%. The method was applied todetermine the glucose concentration in the human serum samples and the results areconsistent with those obtained by the standard spectrometric method.
引文
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