银(Ⅲ)配合物-鲁米诺体系流动注射法测定醋酸泼尼松北大核心CSCD

在碱性环境下,银（Ⅲ）配合物可与鲁米诺产生化学发光,醋酸泼尼松对该发光体系具有显著的增敏作用,据此提出了流动注射银（Ⅲ）配合物-鲁米诺化学发光体系测定醋酸泼尼松含量的方法。优化的试验条件如下：1鲁米诺溶液中氢氧化钠的浓度为0.6mol·L-1;2鲁米诺溶液的浓度为8.0×10-7 mol·L-1;3银（Ⅲ）配合物溶液中氢氧化钠的浓度为1.7mol·L-1;4银（Ⅲ）配合物溶液的浓度为5.0×10-5 mol·L-1。醋酸泼尼松的线性范围为6.0×10-8~8.0×10-5 mol·L-1,方法的检出限（3s/k）为2.9×10-9 mol·L-1。对1.0×10-6 mol·L-1醋酸泼尼松标准溶液连续测定11次,测定值的相对标准偏差为2.9%。加标回收率在100%~105%之间。     

银(Ⅲ)配合物-鲁米诺体系流动注射法测定醋酸泼尼松

在碱性环境下,银(Ⅲ)配合物可与鲁米诺产生化学发光,醋酸泼尼松对该发光体系具有显著的增敏作用,据此提出了流动注射银(Ⅲ)配合物-鲁米诺化学发光体系测定醋酸泼尼松含量的方法。优化的试验条件如下:1鲁米诺溶液中氢氧化钠的浓度为0.6mol·L-1;2鲁米诺溶液的浓度为8.0×10-7 mol·L-1;3银(Ⅲ)配合物溶液中氢氧化钠的浓度为1.7mol·L-1;4银(Ⅲ)配合物溶液的浓度为5.0×10-5 mol·L-1。醋酸泼尼松的线性范围为6.0×10-8~8.0×10-5 mol·L-1,方法的检出限(3s/k)为2.9×10-9 mol·L-1。对1.0×10-6 mol·L-1醋酸泼尼松标准溶液连续测定11次,测定值的相对标准偏差为2.9%。加标回收率在100%~105%之间。     

双酚A的流动注射化学发光法测定

基于双酚A对鲁米诺 铁氰化钾化学发光反应体系的化学发光的抑制作用,建立了一种测定环境雌激素双酚A的流动注射化学发光分析新方法。双酚A的浓度在8.0×10-7～1.0×10-5mol/L范围内与ΔI成良好的线性关系,检出限为3.05×10-7mol/L,已用于聚碳酸酯塑料水溶出液中双酚A的测定。     

鲁米诺-过硫酸钠-卡托普利化学发光体系的研究

基于卡托普利对过硫酸钠鲁米诺化学发光体系的强烈抑制作用,建立起一种直接测定卡托普利的流动注射化学发光新方法。该方法灵敏、简单、快速。线性范围为5.0×10-5～1.0×10-3g·L-1,检出限为1.7×10-5g·L-1,相对标准偏差为3.2%。利用该方法对卡托普利片剂含量的测定,结果满意。     

用偶合反应流动注射化学发光法测定矿样和水样中的痕量铊

将Tl(Ⅲ)置换Co(Ⅱ)-EDTA配合物中的Co(Ⅱ)与Co(Ⅱ)-鲁米诺-H2O2化学发光体系相偶合,建立了流动注射化学发光测定铊的新方法。本方法测定铊的线性范围为3.0×10-6~1.0×10-2mg/mL,检出限为1.0×10-6mg/mL。对1.0×10-4mg/mL的Tl(Ⅲ)标准溶液连续11次测定的相对标准偏差为2.0%。方法可用于矿样和水样中铊的测定。     

铁氰化钾-鲁米诺体系后化学发光行为的研究-流动注射后化学发光法测定可待因

发现了可待因在铁氰化钾鲁米诺化学发光反应体系中的后化学发光反应。优化了反应条件,建立了一种利用后化学发光反应测定可待因的流动注射化学发光新方法。方法的检出限为3×10-8g mL,相对标准偏差为1.9%(1.0×10-6g mL可待因,n=11),线性范围为8.0×10-8～1.0×10-5g mL。此法已用于可待因片剂中可待因的测定,结果与药典方法测定值一致。     

Ni(Ⅳ)-鲁米诺化学发光体系测定磺胺噻唑

在碱性介质中,磺胺噻唑对Ni(IV)配合物-鲁米诺化学发光新体系有显著增敏作用,且化学发光强度在一定范围内与磺胺噻唑浓度呈线性关系。由此建立Ni(IV)流动注射化学发光体系测定磺胺噻唑方法。在优化的条件下,方法检出限(3σ)为5×10-11mol·L-1,在1.0×10-10~1.0×10-9mol·L-1和4.0×10-9~4.0×10-8mol·L-1范围内成良好线性关系。取5.0×10-9mol·L-1磺胺噻唑进行11次平行测定,相对标准偏差(RSD)为2.57%。该方法简便、准确,用于磺胺噻唑针剂中磺胺噻唑的测定,结果满意。     

鲁米诺-过硫酸钠体系后化学发光法测定银

邻菲罗啉存在下,银对鲁米诺-Na2S2O8体系的后化学发光具有增敏作用,建立了流动注射后化学发光测定银的新方法.在优化实验条件下,该法测定银的线性范围为1.0×10-9～4.0×10-7 mol/L,线性相关系数为0.9987(n =7),检出限为3.53×10-10mol/L(n=11),对1.0×10-7 mol/...     

流动注射阻抑化学发光法测定己烯雌酚

基于在碱性介质中,己烯雌酚对N-溴代丁二酰亚胺-鲁米诺化学发光体系的阻抑作用,建立了测定己烯雌酚的流动注射化学发光分析新方法,探讨并优化了流动注射化学发光的分析条件。该方法测定己烯雌酚的线性范围为1.5×10-8~2.6×10-7g/mL,检出限为5.0×10-9g/mL,对1.0×10-7g/mL的己烯雌酚标准溶液进行11次测定,相对标准偏差为2.6%。并应用于饲料、己烯雌酚片剂中的己烯雌酚的测定。     

偶合反应流动注射化学发光测定锆的研究

基于Ｚｒ置换Ｃｏ－ＮＴＡ配合物中的Ｃｏ（Ⅱ）和Ｃｏ（Ⅱ）催化过氧化氢氧化鲁米诺产生化学发光的反应，建立了偶合反应流动注射化学发光测定锆的新方法。方法的线性范围为１×１０＾－１０－１×１０＾－７ｇ．ｍｌ＾－１，检出限为３×１０＾－１１ｇ．ｍｌ＾－１，方法用于地矿术中锆的测定，结果满意。     

Determination of Baicalin by High Performance Liquid Chromatography Coupling with Flow Injection Chemiluminescence Detection

A new method for the determination of baicalin in Scutellariae Radix extract and its preparations by high performance liquid chromatography (HPLC) coupling with flow injection chemiluminescence detection (FIA‐CL) has been developed. The method was based on the chemiluminescence reaction of potassium permanganate with baicalin in nitric acid medium; the CL intensity can be enhanced by formaldehyde. In this study, the conditions of chemiluminescence and chromatography were examined, and the schematic diagram of the HPLC‐FIA‐CL analyzer was optimized. The analytes were separated on Hypersil RP‐C18 columns (100 × 4.6 mm, I.D., 5 μm) by equality elution with 47:53 (v/v) methanol‐0.3% phosphoric acid as a mobile phase at a flow rate of 0.8 mL·min^?1 and a column temperature of 40 °C. Under the optimum condition, the CL intensity was proportional to the concentration of baicalin over the range of 4.10 × 10^?7 ? 6.15 × 10^?5mol·L^?1. The limit of detection (S/N = 3) was 2.79 × 10^?7mol·L^?1 with the relative standard deviation 2.5% (Cs = 6.15 × 10^?6 mol·L^?1, n = 5). The method has been applied to the determination of baicalin in Scutellariae Radix extract and its preparations, and satisfactory results were obtained.     

Peroxyoxalate Chemiluminescence Based on Fluorescent Conjugated Polymer for the Determination of Triton X-100

A novel peroxyoxalate chemiluminescence system has been designed for the determination of Triton X‐100 (TX‐100), in which a hydrophobic fluorescent conjugated polymer, poly[2,5‐bisnonyloxy‐1,4‐phenylene‐ethynylene‐9,10‐anthrylene] (PPEA) was employed as a fluorophor. A strong enhanced intensity of chemiluminescence (CL) was observed in the presence of TX‐100, due to the improved emission efficiency of PPEA in the presence of TX‐100. Under optimum conditions, the detection range of Triton X‐100 is between 1.0×10^?7 and 1.0× 10^?4 mol·L^?1, with a detection limit at 6.0×10^?8 mol·L^?1. The relative standard deviation is 2.4% (n=6) for 1.0×10^?6 mol·L^?1 Triton X‐100. This method provides satisfying results in the detection of TX‐100 in nature water and biological samples with high sensitivity and wide linear range.     

Determination of Melatonin in Rat Pineal Gland and Drug with Flow-Injection Chemiluminescence

A flow-injection chemiluminescence （CL） method for the determination of melatonin based on the CL reaction of melatonin with hydrogen peroxide and sodium hypochlorite （NaOCl） in a basic alkaline solution was developed. The possible CL mechanism has been discussed, and a proposal for the reaction pathway was given that singlet oxygen was clarified to be produced in this reaction system and was responsible for the CL emission. Under the optimized conditions, the linear concentration range of application was 1.0×10^-7-2.5 × 10^-4 moloL-I with a de- tection limit of 5.0 ×10^-8 moloL-1 （S/N= 3）. The relative standard deviation for eight repeated measurements of 1.0×10^-6 mol·L^-1 melatonin was 2.8%. The interferences of several important biological substances, some indole compound, cations and anions were studied. No interference was found for the anions, glucose, starch, most of cations and low concentration （less than 3.0 × 10^-6 mol·L^-1） of some biological substances and indole compound. The method was applied to the determination of melatonin in rat pineal gland and drug with satisfactory results. The sample throughput was 90 injections per hour.     

A Flow Injection Chemiluminescence Method for the Determination of Protein Using Copper(II)-Alizarin Red S Complex as an Efficient Chemiluminescent Probe

A sensitive flow injection chemiluminescence (CL) method is proposed for the determination of bovine serum albumin (BSA) using Copper(II)-Alizarin Red S (ARS) complex as an efficient chemiluminescent probe. The detection is based on the binding of the copper(II)-ARS complex to proteins and the catalytic activity of copper(II)-ARS in the luminol-H₂O₂ CL system. Under the selected conditions, the CL intensity is linear with the concentration of BSA in the range of 5.0 × 10^?11 to 1.0 × 10^?9 mol · L^?1. The detection limit was 2.0 × 10^?11 mol · L^?1. The method is successfully applied to the determination of protein in urine.     

Determination of Gallic Acid by Flow Injection Analysis Based on Luminol‐AgNO3‐Ag NPs Chemiluminescence System

A novel flow injection procedure has been developed for the determination of gallic acid based on the enhancement function for luminol‐AgNO₃‐Ag NPs chemiluminescence (CL) system by gallic acid. The enhancement mechanism was proposed for the reinforcing effect of the gallic acid on the CL system. The UV‐vis absorption spectrum and CL emission spectrum were applied to confirm the mechanism. The method is simple, rapid and sensitive with a detection limit of 5×10^?10 g·mL^?1 and a linear range of 8.0×10^?10–1.0×10^?7 g·mL^?1. The relative standard deviation (RSD) is 1.3% for eleven measurements of 5×10^?8 g·mL^?1 gallic acid. The method has been successfully applied to the determination of gallic acid in Chinese proprietary medicine–Jianmin Yanhou tablets and synthesized samples.     

Label-Free Electrochemiluminescent Determination of DNA Using Luminol and Hemin Functionalized Nanoparticles

Luminol and hemin dual-functionalized silica nanoparticles were synthesized using a typical reverse water-in-oil microemulsion protocol. The obtained nanoparticles were further characterized by transmission electron microscopy, scanning electron microscopy, atomic absorption spectrometry, chemiluminescence, and electrochemiluminescence. The results indicated that the luminol and hemin dual-functionalized silica nanoparticles exhibited significantly higher chemiluminescence and electrochemiluminescence intensities than those of luminol functionalized silica nanoparticles due to the catalytic effect of hemin on the chemiluminescence and electrochemiluminescence of luminol. Furthermore, a simple and sensitive label-free electrochemiluminescence DNA biosensor was developed based on the chitosan modified luminol and hemin dual-functionalized silica nanoparticles and a single-stranded DNA probe. The chitosan modified luminol and hemin dual-functionalized silica nanoparticles were immobilized on the surface of an indium-doped tin oxide electrode and the single-stranded DNA probe was immobilized on the surface of the nanoparticles through electrostatic interactions between single-stranded DNA and chitosan, which allowed hybridization with the target DNA sequences. The hybridization events were evaluated by electrochemiluminescence, and only the complementary sequence formed double-stranded DNA with the DNA probe to give strong electrochemiluminescence signals. Finally, the electrochemiluminescence intensity was found to be linearly related to the concentration of the complementary sequence at concentrations from 1.0?×?10^?12 to 1.0?×?10^?6?mol·L^?1 with a detection limit of 5.0?×?10^?13?mol·L^?1.     

Automated Sequential‐injection Chemiluminescence Determination of Glucosamine Sulphate via Luminol‐Hydrogen Peroxide System

A highly sensitive automated sequential‐injection chemiluminescence (SIA‐CL) method for determination of glucosamine sulphate (GLS) was developed. The goal of the present work is the evaluation of the enhancement effect of the investigated drug glucosamine sulphate on the chemiluminescence reaction between luminol and H₂O₂ in alkaline medium of 1.0 × 10^?2 mol L^?1 sodium hydroxide at pH 11. The experimental conditions affecting the CL reaction such as the sequence of the reagents, concentrations, flow rate and aspirated volumes of reactants were systematically investigated and optimized. Under optimum conditions 50 μL of 1.0 × 10^?3 mol L^?1 luminol, 30 μL of a GLS test solution and 50 μL of 1.0 × 10^?2 mol L^?1 H₂O₂ were used and the luminescing zone was pushed into the detector at a flow rate 100 μL s^?1. The proposed method recorded high sensitivity, accuracy and simplicity that could be clarified as linear concentration range 1.0‐2000 ng mL^?1 with rectilinear part (r = 0.9992, n = 9) and limit of detection 0.3 ng mL^?1, along with relative standard deviation 1.3%. It was found that the developed method can be used directly to determine the investigated drug GLS in its pharmaceutical dosage forms and in spiked serum and urine by diluting the samples for a 1000 fold. The obtained results were statistically analyzed and compared with those obtained by the reported method.     

A Multicommuted Flow‐based System for Hydrogen Peroxide Determination by Chemiluminescence Detection Using a Photodiode

Abstract

A simple, rapid, and automated assay for hydrogen peroxide in pharmaceutical samples was developed by combining the multicommutation system with a chemiluminescence (CL) detector. The detection was performed using a spiral flow‐cell reactor made from polyethylene tubing that was positioned in front of a photodiode. It allows the rapid mixing of CL reagent and analyte and simultaneous detection of the emitted light. The chemiluminescence was based on the reaction of luminol with hydrogen peroxide catalyzed by hexacyanoferrate(III).

The feasibility of the flow system was ascertained by analyzing a set of pharmaceutical samples. A linear response within the range of 2.2–210 µmol l^?1 H₂O₂ with a LD of 1.8 µmol l^?1 H₂O₂ and coefficient of variations smaller than 0.8% for 1.0×10^?5 mol l^?1 and 6.8×10^?5 mol l^?1 hydrogen peroxide solutions (n=10) were obtained. Reagents consumption of 90 µg of luminol and 0.7 mg of hexacyanoferrate(III) per determination and sampling rate of 200 samples per hour were also achieved.     

Simultaneous Detection of Dopamine and Uric Acid under Coexistence of Ascorbic Acid with DNA/Pt Nanocluster Modified Electrode

A novel biosensor by electrochemically codeposited Pt nanoclusters and DNA film was constructed and applied to detection of dopamine (DA) and uric acid (UA) in the presence of high concentration ascorbic acid (AA). Scanning electron microscopy and X‐ray photoelectron spectroscopy were used for characterization. This electrode was successfully used to resolve the overlapping voltammetric response of DA, UA and AA into three well‐defined peaks with a large anodic peak difference (ΔE_pa) of about 184 mV for DA and 324 mV for UA. The catalytic peak current obtained from differential pulse voltammetry was linearly dependent on the DA concentration from 1.1× 10^?7 to 3.8×10^?5 mol·L^?1 with a detection limit of 3.6×10^?8 mol·L^?1 (S/N=3) and on the UA concentration from 3.0×10^?7 to 5.7×10^?5 mol·L^?1 with a detection limit of 1.0×10^?7 mol·L^?1 with coexistence of 1.0×10^?3 mol·L^?1 AA. The modified electrode shows good sensitivity and selectivity.     

Simultaneous Determination of Epinephrine, Noradrenaline and Dopamine in Human Serum Samples by High Performance Liquid Chromatography with Chemiluminescence Detection

A simple, rapid and accurate high performance liquid chromatographic （HPLC） technique coupled with chemiluminescence （CL） detection was developed for the simultaneous determination of epinephrine （E）, noradrenaline （NA） and dopamine （DA）. It was based on the analyte enhancement effect on the CL reaction between luminol and potassium ferricyanide. The effects of various parameters, such as potassium ferricyanide concentration, luminol concentration, pH value and component of the mobile phase on chromatographic behaviors of the analytes （E, NA and DA） were investigated. The separation was carded out on C18 column using the mobile phase of 0.01 mol/L potassium hydrogen phthalate solution and methanol （92 ： 8, V/V）. Under the optimum condi- tions, E, NA and DA showed good linear relationships in the range of 1 × 10^-8 -5 × 10^-6, 5.0× 10^-9 -1.0× 10^-6 and 5.0×10^-9-1.0× 10^-6 g]mL respectively. The detection limits for E, NA and DA were 4.0×10^-9, 1.0× 10^-9 and 8.0 × 10^-10 g/mL. The proposed method has been applied successfully to the analysis of E, NA and DA in human serum samples.