反相流动注射胶束增敏化学发光分析法测定硝苯地平

基于胶束介质中硝苯地平对碱性鲁米诺-过氧化氢化学发光体系的增敏作用,结合反相流动注射技术,建立了流动注射化学发光分析法测定硝苯地平的新方法.硝苯地平浓度在3.5×10-10～4.0×10-8 g·mL-1范围内时,化学发光强度与硝苯地平的浓度呈良好的线性关系,其相对标准偏差为1.4%(n=11,c=3.5×10-9 g...     

Detection of Oxidase Generated Hydrogenperoxide by a Solid State Peroxyoxalate Chemiluminescence Detector

Abstract

The compatability of a solid state peroxyoxalate chemiluminescence detector for hydrogen peroxide with an immobilized oxidase reactor is investigated. As a model system glucose oxidase immobilized by electrostatic forces on an ion-exchanger or chemically bonded to glass beads were chosen. The former support is less suitable for immobilization of oxydases due to strong retention of hydrogenperoxide on the ion exchanger.

The relatively little flow dependence of these systems renders them suitable for low-cost manual sample injection monitors as well as in a flow injection analyses (FIA) mode with low-cost pumping systems. The system was operated with 80% acetonitrile water solutions. A detection limit of 8 × 10^?7M of glucose was achieved in directly injected samples.

Enzymes more sensitive to organic solvents can be operated with pure water and adjustment for optimal chemiluminescence condition is achieved with a make-up flow prior to detection. A detection limit of 5 × 10^?8M glucose is achieved under these conditions. The feasability of this approach to other oxidase based monitors and to detection in liquid chromatography is discussed.     

Subnanogram determination of aniracetam in pharmaceutical preparations and biofluids by flow injection analysis with chemiluminescence detection based on its enhancement of the myoglobin-luminol reaction

A novel flow injection chemiluminescence method with a myoglobin-luminol system is described for determining aniracetam. Myoglobin-bound aniracetam produced a complex that catalyzed the chemiluminescence reaction between luminol and myoglobin, leading to fast chemiluminescence. The chemiluminescence intensity in the presence of aniracetam was remarkably enhanced compared with that in the absence of aniracetam. Under the optimum reaction conditions the chemiluminescence increment produced was proportional to the concentration of aniracetam in the range of 0.1-1000.0 ng/mL (R2 = 0.9992), with a detection limit of 0.03 ng/mL (3delta). At a flow rate of 2.0 mL/min, the whole process, including sampling and washing, could be completed in 0.5 min, offering a sampling efficiency of 120/h; the RSD was less than 3.0% (n = 5). The method was satisfactory for determination of aniracetam in pharmaceutical preparations and human urine and serum samples. A possible mechanism of the reaction is also discussed.     

Development of solid-phase chemiluminescence immunoassays for digoxin comparing flow injection and sequential injection techniques.

The development of a competitive solid-phase immunoassay for digoxin making use of the acridinium chemiluminescence system is described. Two different instrumental approaches are compared. One is based on a continuous flow system using a peristaltic flow injection analysis pump; the other uses a new sequential injection technique. In both systems a flow cell, consisting of transparent PTFE tubing packed with immobilized antibodies, acts as an immunoreactor. The entire assay, including both the immunoreaction and the chemiluminescence reaction, takes place in this immunoreactor cell. Compared with the flow injection technique, the sequential injection mode showed higher precision, ranging from 2.16 to 5.5% RSD depending on concentration. The total assay time, including regeneration, is less than 8 min with the sequential injection technique. The detection limit for both techniques is in the low femtomole range.     

流动注射化学发光法测定利福喷丁

基于碱性介质中利福喷丁能增敏鲁米诺-铁氰化钾体系的化学发光这一现象,结合流动注射分析技术,建立了流动注射化学发光法测定利福喷丁的新方法。在最佳实验条件下,利福喷丁检测浓度的线性范围为0.008~0.88 mg/L,检出限(3σ)为1.2×10-3mg/L。对6.0×10-2mg/L的利福喷丁进行平行测定,其相对标准偏差(RSD,n=11)为1.9%。该方法已用于测定胶囊和血浆中利福喷丁的含量,结果满意。     

流动注射化学发光法测定头孢噻肟钠

基于在碱性介质中头孢噻肟钠对鲁米诺-K3Fe(CN)6化学发光体系的增强作用,建立了流动注射化学发光测定头孢噻肟钠的新方法.头孢噻肟钠的质量浓度与化学发光强度的变化在2.4～30 mg/L和60～300 mg/L范围内呈良好的线性关系,检出限为0.63 mg/L,对浓度为30 mg/L的头孢噻肟钠进行9次平行测定,相对标准偏差(RSD)为1.0%.该法简便、快速、可靠,将其用于头孢噻肟钠针剂的测定,结果令人满意.     

Determination of Cr(III) in urine, blood serum and hair using flow injection chemiluminescence analysis

A flow injection (FI) chemiluminescence method for the determination of Cr(III) in blood serum, urine and hair samples is reported. It is based on the chromium-catalyzed light emission from the luminol oxidation by hydrogen peroxide. The apparatus consists of an FI system with a flow cell formed by a coiled transparent tube suitable for chemiluminescence detection. The specificity of the method is achieved in presence of EDTA. The detection limit under optimum conditions is 0.01 μg L^–1 of Cr(III). Precision and accuracy were evaluated by determining Cr(III) concentrations in urine standards from the National Institute of Standard and Technology (NIST).     

流动注射-鲁米诺-高碘酸钾-过氧化氢体系的化学发光行为及其应用

详细研究了流动注射－鲁米诺－高碘酸钾－过氧化氢体系化学发光行为，给出了反应的最佳条件。拟定了一种化学发光测定过氧化氢的新方法。方法的检测限为３．０Ｘ１０－８ｍｏｌ／ＬＨ２Ｏ２；线性范围为２．０×１０－７～６．０×１０－４ｍｏｌ／Ｌ。评价了该体系的应用前景。     

Flow injection with inhibited chemiluminescence method for the determination of dopamine hydrochloride.

A simple rapid and accurate flow injection inhibitory chemiluminescence method has been developed for the determination of dopamine hydrochloride based on its inhibition of the chemiluminescence from the luminol-potassium hexacyanoferrate(III) system. The linear range of determination is 4.0 x 10(-9) - 4.0 x 10(-7) g ml(-1) for dopamine hydrochloride and the detection limit is 1.14 x 10(-9) g ml(-1). The method has been applied to determine the content of dopamine in pharmaceutical preparation with satisfactory results.     

高锰酸钾-甲醛化学发光体系测定甲氧氯普胺

基于在甲醛的作用下,高锰酸钾对甲氧氯普胺的氧化作用而产生化学发光的现象,建立了一种新的用流动注射-化学发光法测定甲氧氯普胺含量的方法.该方法测定甲氧氯普胺的线性范围为0.2~100 mg/L,检出限为0.1 mg/L.对于8 mg/L的甲氧氯普胺标准溶液连续11次测定的相对偏差为1.2%.该方法可用于对制药废水、片剂和针剂中甲氧氯普胺含量的测定.     

Chemiluminescence assay for uric acid in human serum and urine using flow-injection with immobilized reagents technology

A novel chemiluminescence (CL) flow sensor for the determination of uric acid in human urine and serum has been developed by using controlled-reagent-release technology. The reagents involved in the chemiluminescence (CL) reaction, luminol and periodate, are immobilized on anion-exchange resin packed in a column. After injection of water, chemiluminescence generated by released luminol and periodate in alkaline media is inhibited in presence of uric acid. By measuring the decreased chemiluminescence (CL) intensity the uric acid is sensed. The decreased response is linear in the 5.0-500.0 ng mL(-1) range, with a detection limit of 1.8 ng mL(-1). The flow sensor showed remarkable operational stability and could be easily reused for over 80 h with sampling frequency of 100 h(-1). The proposed sensor was applied to the determination of uric acid in human urine and serum, and monitoring metabolic uric acid in human urine with RSD less than 3.0%.     

流动注射化学发光法测定尿酸

在碱性条件下,铁氰化钾氧化鲁米诺,产生化学发光,尿酸对该体系的化学发光有显著的增强作用（亚铁氰化钾存在时）。基于此,建立了一种直接测定尿酸的流动注射化学发光分析法。方法的线性范围为２．０×１０－８～５．０×１０－６　ｇ／ｍＬ;检测限（３σ）为６．７×１０－９　ｇ／ｍＬ;相对标准偏差为１．１％（尿酸１．０×１０－７　ｇ／ｍＬ,ｎ＝１１）。用于血清及尿样中尿酸的分析,结果令人满意。     

A chemiluminescence flow injection system for nitrite ion determination

A chemiluminescence system is described for the determination of nitrite ion based on new designs for an ozone generator, liquid-gas separator and chemiluminescence reaction cell. The method is based on the gas-phase chemiluminescence reaction between ozone and nitric oxide, which is generated from the reduction of nitrite with iodide in sulfuric acid solution. The efficiency of the system was evaluated by investigation of the analytical performance characteristics of the system for nitrite determination in batch and flow injection procedures. Under optimal conditions, the chemiluminescence response of the system was linear against the nitrite concentration over the range 1 to 1 × 10⁴ ng ml^?1 in the batch procedure and 10 to 5 × 10³ ng ml^?1 in the flow injection procedure, with detection limits of 1 and 10 ng ml^?1, respectively. The method is highly selective and allows for the determination of nitrite in the presence of high concentrations of several cationic, anionic and nitrogen containing species. It has been successfully applied to the analysis of nitrite in natural water and soil extracts.     

Noncompetitive enzyme immunoassay for α-fetroprotein using flow injection chemiluminescence

A novel, direct noncompetitive flow injection enzyme immunoassay for α-fetoprotein (AFP) was developed by enhanced chemiluminescence detection. The method was based on off-line incubation of AFP and horseradish peroxidase (HRP)-labeled anti-AFP, and then trapping of the unbound enzyme conjugate by an immunoaffinity column filled with AFP-modified Sepharose. The immunocomplex formed in incubation passed through the column and then was directly detected by a postcolumn chemiluminescence technique. The optimal conditions for the immunoassay procedure and chemiluminescence detection were established. At a 1:10 dilution of enzyme conjugate solution, the linear range for chemiluminescence detection of AFP was from 2.0 to 75 ng/mL with a correlation coefficient of 0.993 and a coefficient of variation of 2.67% at 30 ng/mL. The detection limit was 0.5 ng/mL. This method was flexible, sensitive, and rapid. The immunoaffinity column of 200 μL could be repeatedly used 100 times without a single decrease. The whole assay time including the preincubation step was only 30 min for one sample.     

流动注射化学发光法测定安痛定注射液中的氨基比林

在甲醛存在下,高锰酸钾与氨基比林能够发生化学发光反应,产生很强的化学发光,由此建立一种测定氨基比林的流动注射化学发光分析法。方法的检出限为３．０×１０－８ｇ／ｍＬ,相对标准偏差为１．３％（４．０×１０－５ｇ／ｍＬ氨基比林,ｎ＝１１）,线性范围为１．０×１０－７～８．０×１０－５ｇ／ｍＬ氨基比林。该法已用于安痛定注射液中氨基比林含量的测定。     

A simple and rapid flow injection chemiluminescence determination of cysteine with Ru(phen)3(2+)-Ce(IV) system

A new chemiluminescence system was developed for the determination of cysteine by flow injection system. This method is based on the reaction of L-cysteine with Ru(phen)3(2+) and Ce(IV) to produce chemiluminescence. The calibration curve was linear over the range 8.0x10(-7) to 4.0x10(-5) and 4.0x10(-5) to 1.0x10(-3) M with a detection limit of 7.0x10(-7) M (S/N=3). The relative standard deviation of 4.0x10(-6) M cysteine was found 3.5% (n=10). The influence of potential interfering substances was studied. The proposed method was successfully applied for the flow injection determination of cysteine in the real samples with minimum sampling rate of 90 sample/h.     

Determination of Puerarin in Pharmaceutical Injection by Flow Injection Analysis with Acidic Potassium Permanganate–Glyoxal Chemiluminescence Detection

Abstract

A simple flow injection chemiluminescence method with synergistic enhancement has been investigated for the rapid and sensitive determination of puerarin. The method is based on the enhancing effect of puerarin on the chemiluminescence emission generated by the oxidation of glyoxal with potassium permanganate in a sulfuric acid medium. The optimization of chemical variables influencing the chemiluminescence response of the method has been carried out by applying experimental design, using the proposed flow?injection manifold. Under the optimal conditions, the enhanced chemiluminescence intensity was linear with the concentration of puerarin over the range from 10.0 ng · ml^?1 to 7.0 µg · ml^?1 (R²=0.9972) with a detection limit (3σ) of 3.0 ng · ml^?1. At a flow rate of 3.0 ml · min^?1, a complete analytical process could be performed within 0.5 min, including sampling and washing, with a relative standard deviation of less than 3.0%. The proposed method was applied successfully in the assay of puerarin in pharmaceutical injection and human urine. The mechanism of chemiluminescence reaction was discussed briefly.     

Determination of Cr(III) in urine, blood serum and hair using flow injection chemiluminescence analysis

A flow injection (FI) chemiluminescence method for the determination of Cr(III) in blood serum, urine and hair samples is reported. It is based on the chromium-catalyzed light emission from the luminol oxidation by hydrogen peroxide. The apparatus consists of an FI system with a flow cell formed by a coiled transparent tube suitable for chemiluminescence detection. The specificity of the method is achieved in presence of EDTA. The detection limit under optimum conditions is 0.01 μg L^–1 of Cr(III). Precision and accuracy were evaluated by determining Cr(III) concentrations in urine standards from the National Institute of Standard and Technology (NIST). Received: 30 June 1997 / Revised: 16 January 1998 / Accepted: 23 January 1998     

流动注射化学发光检测法的进展

评述近年来流动注射化学发光检测法及生物发光检测法的最新进展。内容涉及各类化学发光反应、生物发光和电致化学发光反应同流主射体系的耦合方式，仪器设计，多种无机、有机、生物大分子、生物活性的药物的分析方法及其在环境、生物医学客生命科学、化学及药物化学中的应用和发展方向。     

The effects of solvent preoxidation on inhibited chemiluminescence of pyrogallol oxidation in flow injection analysis and liquid chromatography

A new extension of chemiluminescence technique using pre-oxidation of a carrier solvent before the conventional inhibited chemiluminescence detection is presented in this study. The method is based on the modification of the oxidation chemistry of pyrogallol upon contact with a flow stream consisting of an organic solvent in mixture with an aqueous solution of a soft oxidant. The final response was found to depend on the kind of solvent and the oxidant/pre-oxidant mixture employed for the oxidation of pyrogallol and the solvent, respectively. By selecting the appropriate combination two detection modalities with increased sensitivity can be achieved. The first is based on the enhancement of the analytes signal through intensification of their scavenging effect on pyrogallol oxidation and the second on the enhancement of signal above the emission induced during the pyrogallol oxidation. Various combinations of organic solvents, oxidizing and pre-oxidizing mixtures were examined for their response in inhibited chemiluminescence measurements yielding very interesting results. The analytical utility of this new technique to the improvement of previous analytical methods as well as to the development of new procedures employing flow injection analysis is demonstrated. Furthermore, the application of the proposed method in combination with liquid chromatographic analysis is also presented.