Study on Chemiluminescence Reactions of L ucigenin and Reductants by Flow Injection Analysis

The chemiluminescence reactions between lucigenin and reductants such as Mo(LII),V( II), U(III), W(III), Cr(II), Ti(III) and Fe( II), which were produced on-line by passing Mo(VI),V(V),U(VI), W(VI), Cr(VI,III),Ti(IV) and Fe(III) through a micro Jones column, are studied in detail. Results show that the reactions can be used directly for the determination of these substances. The mechanism of the reactions is also investigated.

Flow Injection Analysis of Histidine with Enhanced Electrogenerated Chemiluminescence of Luminol

A simple and sensitive flow injection method is presented for the determination of histidine based on its enhancement of electrogenerated chemiluminescence (ECL) of luminol. After optimization of the experimental parameters, the working range for histidine was in 1.0 x 10-6 to 1.0 x 10 -3 mol/L with a detection limit (S/N = 3) of 0.56 mmol/L. The relative standard deviation was 1.6% for 11 measurements of 5 x 10 5 mol/L histidine solution. The proposed method has been successfully applied to the determination of histidine in real pharmaceutical preparation.

Flow injection chemiluminescence determination of meloxicam using potassium permanganate and formaldehyde system

A simple, rapid and sensitive flow injection chemiluminescence （FI-CL） method has been developed for the determination of meloxicam. The method is based on the CL-emitting reaction between meloxicam and potassium permanganate in a hydrochloric acid medium, enhanced by formaldehyde （HCHO）. Under optimum conditions, calibration curve over the range of 1.0-20.0μg/mL was obtained. The proposed method was successfully applied to the determination of meloxicam in capsules with no evi- dence of interference from common excipients. The detection limit of this method was 25.6 ng/mL. The relative standard deviation was 2.1% for 10.0 μg/mL meloxicam. The sample throughput was found to be 120 samples/h.

SELECTIVE SULFUR DIOXIDE DETERMINATION BY GAS DIFFUSION FLOW INJECTION ANALYSIS WITH CHEMILUMINESCENT DETECTION

Sulfur dioxide has been found to decrease the chemiluminescence of luminol-iodine system.A new determination method for sulfur dioxide in atmosphere is developed by applying this reaction to a flow injection gas diffusion separation system.This permits the determination of sulfur dioxide selectively and rapidly.

Chemiluminescence Determination of Molybdenum by on-Line Reduction with a Flow Injection System

The chemiluminescence (CL) reaction between lucigenin (Lu) and molybdenum (III) produced by a Jones reductor was investigated using a flow injection system. On the basis of this, a novel method for the determination of trace amount of molybdenum has been established. The emission intensity was linear with molybdenum concentration in the range of 0.1-1000 ng/mL; the detection limit was 0.02 ng/mL molybdenum; the relative standard deviation was less than 2% for the determination of 0.1 ng/mL molybdenum (n=11). The method has been applied successfully to the analysis of trace molybdenum in water and steel samples.

Study on Quenching Effect of Holmium (Ⅲ) Ion in Chemiluminescence System of Luminol H_2O_2-Cr(Ⅲ) by Flow Injection Technique

A new chemiluminescence (CL) analytical method for determination of rare earth Ho(Ⅲ) ion is reported. It is based on the quenching effect of Ho(Ⅲ) ion on CL intensity of Luminol H 2O 2 Cr(Ⅲ) system. The detection limit is 3×10 -8 mol/L, the linear range is from 1×10 -7 to 1×10 -4 mol/L; the relative standard deviation is less than 3% (for 2×10 -7 mol/L Ho, n=11). The method was applied to determination of Ho(Ⅲ) in pure samples with satisfactory results.

Determination of ribavirin by flow injection chemiluminescence

Objective： To establish a rapid and precise continuous flow-injection chemiluminescence （CL） method to determine ribavirin. Methods： The ribavirin could restrain strongly CL reaction of luminol in sodium hydroxide （NaOH） solution with potassium chlorate （KClO3）. The different experimental parameters affecting the CL intensity were studied carefully. Results： Under optimum conditions （The concentrations of luminol, KClO3, and NaOH were at 0.1 mmol/L, 0.5μmol/L, and 0.2 mol/L, respectively）, the linear range of the working curves was 0.01-7.00μg/ml with a detection limit of 0.004μg/ml. Conclusion： The method is simple, rapid and sensitive, and successfully applied to the determination of ribavirin in pharmaceutical preparations and biological fluids.

Electrogeneration of ferrate (Ⅵ) in low concentration NaOH solution for flow-injection-chemiluminescence detection

The possibility of direct analytical applications of ferrate（Ⅵ） solution,which was freshly electrogenerated in low-concentration NaOH electrolyte,was studied by a flow-injection-chemiluminescence（FI-CL） system.It was found that some inorganic ions, organic molecule and biomolecule could enhance the chemiluminescence emission caused by ferrate（Ⅵ）-luminol reaction.V（Ⅴ）, Ca（Ⅱ）,Mg（Ⅱ）,phloroglucinol,and bovine hemoglobin（Hb） chosen as samples were successfully detected by this developed method.The analytical characteristics of the system for the analytes determination including linear ranges,correlation coefficients, limits of detection combined with FI analysis were studied.

Flow Injection Determination of Tramadol Based on Its Sensitizing Effect on the Chemiluminescent Reaction of Permanganate-Sulfite

In this paper, a novel chemiluminescence (CL) method for the determination of tramadol has been developed by combining the flow injection technique and its sensitizing effect on the weak CL reaction between sulfite and acidic KMnO4. A mechanism for the CL reaction has been proposed on the basis of fluorescent and CL spectra. Under the optimized conditions, the proposed method allows the measurement of tramadol hydrochloride over the range of 0.04 - 4 ?g/mLwith a correlation coefficient of 0.9995 (n = 8) and a detection limit of 0.01 ?g/mL (3σ), and the relative standard deviation for 2.0 ?g/mL tramadol (n = 11) is 2.1%. The utility of this method was demonstrated by determining tramadol hydrochloride in tablets and injections.

Determination of Lanthanu m in Lu minol- H_2 O_2- Cr( Ⅲ) Syste m by Flow Injection Chemilu minescence

A novel method of flow injection chemiluminescence (CL) analysis for the determination of rare earth La(Ⅲ) ion is prensented. It is based on the quenching effect of La(Ⅲ) ion in the CL system of Luminol H 2O 2 Cr(Ⅲ). The CL emission intensity is linear with La(Ⅲ) concentration in the range 1×10 -7 ～1×10 -4 mol/L; the detection limit is 4×10 -8 mol/L, the relative standard deviation is less than 3% (for 2×10 -7 mol/L La, n =11).

Flow Injection Chemiluminescence Method for Nalbuphine Hydrochloride in Pharmaceutical Formulations Using Tris(2,2′-bipyridyl)ruthenium(II)Chloride-diperiodatocuprate(III)Reaction

A sensitive and selective method employing chemiluminescence(CL)coupled with flow injection(FI)is reported for nalbuphine hydrochloride(NAL)assay in pharmaceutical formulations.The enhancement effect of NAL on the CL reaction between tris(2,2′-bipyridyl)ruthenium(II)chloride-diperiodatocuprate(III){Ru[(bpy)_(3)]^(2+)-Cu(III)complex}in acidic medium is used as analytical measurement.The optimal conditions of the CL reaction were sulfuric acid 1.0×10^(−3) mol/L,Ru[(bpy)s]2+7.5×10^(−5) mol/L,Cu(III)/Ag(III)complexes 4.0×10^(−4)/5.0×10^(−4) mol/L,sample loop volume of 120µL and flow rate of 2.5 mL/min.The sensitivities of the method in terms of detection(S/N=3)and quantification(S/N=10)limits are 5×10^(−4) and 0.001 ppm(1 ppm=1 mg/L),respectively.The linear response of the instrument in the form of CL intensity with respect to NAL concentration is over the range 0.001-15.0 ppm(R^(2)=0.9999)with relative standard deviation from 0.8%to 3.2%and injection throughput of 120 injection/h.The applications of the method include the quantitative analysis of NAL in pharmaceutical injection samples.Variations and the average results of the proposed method are not significantly different from the results of a reported method by applying F-and paired student t-test.The most likely CL reaction mechanism is written in accordance with spectrophotometric and CL studies.

Chemiluminescent Determination of Cyromazine in Milk Samples Using Copper（III） Chelate-Triton X-100 by Flow Injection Analysis

Cyromazine（CYR） was determined in milk samples using copper（HI） chelate-Triton X-100 chemiluminescence（CL） system associated with flow-injection（FI） in KOH medium. The relative CL intensity for CYR concentration was linear over the range of 5×10^-4-10μg/mL（R2=0.9990, n=11） with injection rate of 160 h-1 and the relative standard deviation（RSD, n=4） of 1.2%-2.6%. The limit of detection（LOD） for signal-to-noise ratio of 3 was 1.5×10^4μg/mL. The influences of key chemical and physical parameters, some major fresh water ions at their maximum admissible concentrations and a number of pesticides were examined as potential interferences. The concentrations of CYR in spiked milk samples were successfully determined by the proposed method and the results were in good agreement with that of the previously reported HPLC method, having recovery range of （92% a=4%）-（106% a：2%）. The possible CL reaction mechanism for copper（m） chelate-Triton X-100-CYR was also briefly discussed.

Study on Chemiluminescence Reaction between Lucigenin and Four Rare Metal Ions

The chemiluminescence (CL) reactions between lucigenin and four rare metal reductants were studied systematically using a flow injection system.The results show that the reactions can be used for determination of rare metals.The probable mechanism of the CL reactions involves the reduction of dissolved oxygen to the superoxide radical O - 2·by the reductant,followed by the O - 2·reacting with alkaline Lu to generate CL.The pathway involves a dioxetane intermediate.

Flow-injection Chemiluminescence Sensor for the Determination of Gallic Acid by Immobilizing Luminol and Periodate on Anion-exchange Resin

A novel chemiluminescence (CL) sensor for the determination of gallic acid combined with flow injection analysis was developed by electrostatically immobilizing luminol and periodate on anion-exchange resins respectively. Gallic acid was sensed by its enhancing effect on the weak CL reaction between luminol and periodate, which were eluted from the ion exchange column. The possible reaction mechanism of the CL system was suggested and discussed. The response of the sensor to gallic acid concentration was linear over the range of 8.0×10 -9-1.0×10 -6 mol/L with a detection limit of 6.5×10 -9 mol/L (3σ). The relative standard deviation (RSD) for 7 repetitive determinations of gallic acid (1.0×10 -7 mol/L) was 1.8%. The sensor could be used for over 400 times determination with a good reproducibility.

测定利福平的化学发光新体系

基于碱性介质中铜离子催化过氧化氢可氧化利福平产生化学发光这一现象，并结合流动注射分析技术建立起了一种测定利福平的新方法。该方法测定利福平的线性范围为 ４ × １０－７× １０－４ｇ／ｍｌ，方法的检出限为 ７× １０－８ｇ／ｍＬ，７次平行测定 ２ × １０－５ｇ／ｍＬ利福平的相对标准偏差为 ４．９％。成功地用于利福平眼药水中利福平含量的测定。

流动注射化学发光法测定双嘧达莫

采用流动注射技术研究了酸性条件下，双嘧达莫与高锰酸钾和过氧化氢的化学发光行为，对影响化学发光强度的诸因素进行了实验和探讨，建立了流动注射化学发光法测定双嘧达莫的新方法。方法的检出限为5．8×10-8g／mL，线性范围为2×10-7～8×10-5g／mL，对4×10-6g/mL双嘧达莫进行了11次平行测定，相对标准偏差为1．4％。方法用于药剂中双嘧达莫含量的测定，结果与药典标准法测得值一致。

流动注射化学发光法在药物分析中的应用

流动注射化学发光法作为一种有效的痕量分析技术,因其具有灵敏度高、线性范围宽、而且分析速度快、重现性好等特点,在分析化学领域得到了迅速发展.文章系统评述了2002～2004年间该法在药物方面的应用,引用文献74篇.

锰C-抗坏血酸甲醛-化学发光体系的研究

实验观察到锰 氧化抗坏血酸可以产生弱的化学发光 ,甲醛对这一化学发光反应有较强的增敏作用 ,据此建立了测定抗坏血酸的流动注射化学发光分析法。方法的检出限为 2× 1 0 -8mol/L抗坏血酸 ;线性响应范围为 6 .0× 1 0 -8～ 2 .0× 1 0 -5mol/L。对 1 .0× 1 0 -6mol/L的抗坏血酸进行 1 1次测定 ,相对标准偏差为 2 3%。该方法已成功应用于维生素C针剂和片剂中抗坏血酸含量的测定 。

用偶合反应-流动注射化学发光法测定食品和水中痕量亚硝酸根

基于在酸性介质下，ＮＯ２－与Ｉ－快速反应产生Ｉ２，和Ｉ２氧化Ｌｕｍｉｎｏｌ产生化学发光反应，建立了Ｌｕｍｉｎｏｌ－Ｉ－－ＮＯ２－偶合发光体系测定痕量 ＮＯ２－的方法。本法测定 ＮＯ２－线性范围：８．０×１０－９～１．０×１０－６ｇ／ｍＬ；检出限１．６×１０－９ｇ／ｍＬ；对１．０×１０－８ｇ／ｍＬＮＯ２连续１１次测定的相对标准偏差为１．５％。用于食品及水中亚硝酸根的测定，结果满意。

流动注射化学发光法测定扑热息痛

研究发现在碱性条件下 ,扑热息痛对鲁米诺 -铁氰化钾体系发光反应具有强烈的抑制作用 ,据此建立了流动注射化学发光测定痕量扑热息痛的新方法。扑热息痛浓度在 4 .0× 1 0 - 5～1 .0× 1 0 - 3g L范围内与发光强度呈良好的线性关系 ;检出限 ( 3σ)为 2 .4× 1 0 - 6 g L。相对标准偏差 (C =8.0× 1 0 - 4 g L ,n =1 1 )为 2 .3 %。方法用于片剂中扑热息痛含量测定 ,结果与标准方法一致。