Ru(phen)32+-SDBS-KMnO4化学发光体系检测还原型谷胱甘肽的研究

当硫酸介质中有阴离子表面活性剂十二烷基苯磺酸钠(SDBS)存在时,还原型谷胱甘肽(G-SH)可以增强三(1,10-菲咯啉)钌(Ⅱ)[Ru(phen)32+]-KMnO4化学发光体系的发光强度.基于此,建立了一种化学发光直接检测G-SH的新方法.在优化的实验条件下,该方法的线性范围和检出限分别为5.0×10-2～2.0μg·mL-1和3.5×10-2μg·mL,对1.0μg·mL-1的G-SH溶液平行测定11次的相对标准偏差(RSD)为5.8%.将其用于合成样品中G-SH含量的测定,结果满意.并提出了可能的化学发光机理.     

Ru（phen）32＋-Ce（Ⅳ）化学发光体系检测吲哚乙酸的研究

基于吲哚乙酸(IAA)对三(1, 10-菲咯啉)钌(Ⅱ)[Ru(phen)2+3]-Ce(Ⅳ)化学发光体系的发光增强作用,建立了一种化学发光直接检测IAA的新方法.在优化的实验条件下,该方法的线性范围为5.0×10-3 ～2.0 μg·mL-1,检出限为2×10-3μg·mL-1 ;对含0.50 μg·mL-1IAA的溶液平行测定11次的相对标准偏差(RSD)为5.5%.方法用于合成样品中IAA含量的测定,结果满意.本文还对可能的化学发光机理进行了探讨.     

Pr3+或La3+与克拉红霉素对大肠杆菌的协同作用

用LKB-2277生物活性检测系统采用停流法于37℃测定了克拉红霉素及克拉红霉素分别与Pr(NO3)3和La(NO3)3混合后,对大肠杆菌生长抑制作用的热效应变化.根据热动力学模型进行了定量解析,得到了各体系的克拉红霉素浓度c与大肠杆菌生长速率常数k之间关系式及其半抑制浓度Ic50.克拉红霉素:k=0.03106-1.273×10-3cIc50=8.81μg·mL-1(0.5～20μg·mL-1)克拉红霉素+Pr3+:k=0.02967-1.332×10-3cIc50=7.38μg·mL-1(1～15μg·mL-1)克拉红霉素+La3+:k=0.02741-1.194×10-3cIc50=6.34μg·mL-1(1～15μg·mL-1)微量热结果不仅表征了克拉红霉素的抗菌活性强于红霉素,Pr3+或La3+与克拉红霉素协同作用也使抗菌活性增强,而且反映了不同药物作用下细菌的生理、生化和代谢过程热动力学特征的变化.     

Ru(phen)_3~(2+)-Ce(Ⅳ)化学发光体系检测吲哚乙酸的研究

基于吲哚乙酸(IAA)对三(1,10-菲咯啉)钌(Ⅱ)[Ru(phen)32+]-Ce(Ⅳ)化学发光体系的发光增强作用,建立了一种化学发光直接检测IAA的新方法。在优化的实验条件下,该方法的线性范围为5.0×10-3~2.0μg.mL-1,检出限为2×10-3μg.mL-1;对含0.50μg.mL-1IAA的溶液平行测定11次的相对标准偏差(RSD)为5.5%。方法用于合成样品中IAA含量的测定,结果满意。本文还对可能的化学发光机理进行了探讨。     

色谱膜法富集气体中痕量的SO2和NO2

自行研制了一套简易装置,用微孔型色谱膜,可富集与测定气体中痕量SO2、NO2。在优化条件下,用该法测定NO2,线性范围:0～4.5×10-2μg·mL-1,检测限:8.0×10-4μg·mL-1,变异系数:0.9%;测定SO2,线性范围:0～2.0μg·mL-1,检测限:8.4×10-2μg·mL-1,变异系数:3.0%。方法可靠。1　实验部分1.1　仪器和试剂　721型分光光度计;恒温水浴锅。富集气体装置自制,其中微孔型色谱膜池(由俄罗斯圣彼得堡大学化学系提供)。亚硝酸钠标准溶液:5.0μg·mL-1;亚硫酸钠标准溶液:2.0μg·mL-1;盐酸萘乙二胺和四氯汞钾吸收液按常规方法配制。试剂均为分析…     

鲁米诺-过氧化氢化学发光体系测定利福平

基于鲁米诺在碱性条件下可以被H2O2氧化产生化学发光,利福平对此化学发光具有增敏作用这一现象,结合流动注射技术建立了一种直接测定利福平的流动注射化学发光新方法.该方法的线性范围在1.0×10-6～2.0×10-8g·mL-1,检出限为3.0×10-9g·mL-1,对5.0×10-7g·mL-1的利福平连续进行11次平行测定,其相对标准偏差为3.0%.该法已成功测定了利福平胶囊及眼药水中利福平的含量.     

基于I--N-氯代丁二酰亚胺-鲁米诺反应体系流动注射化学发光法测定白藜芦醇

基于在碱性介质中,白藜芦醇对I-增强N-氯代丁二酰亚胺-鲁米诺化学发光体系的阻抑作用,建立了测定白藜芦醇的流动注射化学发光分析新方法.优化了流动注射化学发光的分析条件和探讨了反应的可能机理.测定白藜芦醇的线性响应质量浓度范围为2.5×10-9～8.0×10-8g·mL-1,检出限为6.3×10-10g·mL-1,用5.0×10-8g·mL-1的白藜芦醇标准溶液进行11次测定,相对标准偏差(RSD)为2.2%.应用本法测定了虎杖、葡萄酒、葡萄皮样品中的白藜芦醇含量,结果满意.     

蘑菇组织催化氧化-流动注射荧光法测定去甲肾上腺素和左旋多巴

研究发现富含多酚氧化酶的蘑菇组织可催化溶解氧氧化去甲肾上腺素和左旋多巴在碱性条件下生成具有强荧光的三羟基和二羟基吲哚类物质 ,建立了以蘑菇组织柱为酶反应器的去甲肾上腺素和左旋多巴的流通式荧光分析法 .该法对去甲肾上腺素和左旋多巴响应的线性范围分别为 6× 10 -8～ 1× 10 -5g·mL-1和 3× 10 -8～ 1× 10 -5g·mL-1,检测限分别为 2×10 -8g·mL-1和 1× 10 -8g·mL-1( 3S/k) .该组织反应器可连续使用 14d ,对 1× 10 -7g·mL-1去甲肾上腺素和 1× 10 -7g·mL-1左旋多巴测定的相对标准偏差 (R .S .D .)均小于 3 % (n =11) .详细研究了常见离子和抗氧化剂对本体系的干扰情况 .将该体系用于药物制剂中去甲肾上腺素和左旋多巴含量的测定 ,结果与药典标准方法测得值一致 .实验结果证明了方法的可行性和可靠性     

单扫描极谱法测定罐装水果中微量锡

建立了一种简易、快速检测罐装水果中锡的单扫描极谱法.在 0. 05mol·L-1H2C2O4和 0. 003 %次甲基绿体系中,Sn(Ⅳ)在汞电极上于-0. 52V(vs.SCE)处有一灵敏的极谱波.该极谱波的波高与Sn(Ⅳ )的浓度在3. 0×10-8 ~ 5. 0×10-6 g·mL-1范围内呈线性关系,检测下限为 8. 2×10-9 g·mL-1,应用该法测定了罐装水果中的微量锡,并同光度法所获结果进行了对照,结果基本一致.     

甲基睾酮-KMnO_4-Ru(bipy)_3~(2+)-Ce(Ⅳ)化学发光检测甲基睾酮的研究

在KMnO4存在下甲基睾酮可增强三(2,2′-联吡啶)钌(Ⅱ)[Ru(bipy)32+]-Ce(Ⅳ)化学发光体系的发光强度,基于此建立了一种化学发光检测甲基睾酮的新方法。在优化的实验条件下,该方法的线性范围和检出限分别为1.0×10-7~4.0×10-6mol.L-1和5.0×10-8mol.L-1。该法用于药片中甲基睾酮含量的测定,结果满意。文中还提出了可能的化学发光机理。     

阻抑动力学荧光法测定头孢曲松钠

在弱酸性介质中,头孢曲松钠能够阻抑过硫酸钾氧化荧光桃红的荧光淬灭反应,从而建立了阻抑动力学荧光法测定头孢曲松钠含量的新方法．头孢曲松钠的质量浓度与荧光强度的变化在1．0×10^-6～1．3×10^-5g·mL^-1范围内呈良好线性关系,R=0．9980,对浓度为1．0×10^-5g·mL^-1的头孢曲松钠进行11次平行测定,相对标准偏差为1．29％,检出限为3．8×10^-8g·mL^-1．该法简便、快速,结果可靠,可应用于药物制剂中头孢曲松钠含量的测定,结果令人满意．     

Determination of Rifampicin by Peroxomonosulfate‐Cobalt(II) Chemiluminescence System

Rifampicin can enhance the chemiluminescence (CL) of peroxomonosulfate‐cobalt(II) system, and the CL intensity is strongly dependent on the rifampicin concentrations. Based on this phenomenon, a rapid and sensitive flow injection CL method was developed for the determination of rifampicin. The relative CL intensity was linear with the rifampicin concentration over the range of 5×10^?8 to 1×10^?6 g·mL^?1 (r=0.9991), the detection limit was 7×10^?9 g·mL^?1 (S/N=3), and the relative standard deviation was 2.7% for 6×10^?7 g·mL^?1 rifampicin (n=11). Furthermore, this method was successfully applied to the determination of rifampicin in real eye drop and capsules sample.     

Molecular Imprinting-Chemiluminescence Sensor for the Determination of Amoxicillin

The amoxicillin-imprinted polymer was synthesized with methacrylic acid (MAA) as a functional monomer and ethylene glycol dimethacrylate (EGDMA) as a cross-linker. The binding characteristic of the imprinted polymer to amoxicillin was evaluated by equilibrium binding experiments. Using the imprinted polymer as recognition material, 3-(3′-nitrophenyl)-5(2′-sulfonylphenylazo)-rhodanine (4NRASP) was synthesized by the authors and was used as chemiluminescence (CL) reagent. A novel chemiluminescence (CL) sensor for the determination of amoxicillin was developed based on the CL reaction of amoxicillin with potassium permanganate in an acidic medium. The sensor displayed excellent selectivity and high sensitivity. The linear response range of the sensor was from 5.0 × 10^?9 to 1.0 × 10^?6 g · mL^?1 (r = 0.9985) and the detection limit was 1.3 × 10^?9 g · mL^?1. The relative standard deviation for the determination of 1.0 × 10^?7 g · mL^?1 amoxicillin solution was 1.7% (n = 11). The sensor was applied to the determination of amoxicillin in urine samples with satisfactory results.     

Flow Injection Chemiluminescence Sensor with Novel Rhodanine Ramification for Determination of Fenfluramine Based on Molecularly Imprinted Polymer

Abstract

Flow injection chemiluminescence (FI-CL) with molecularly imprinted polymer (MIP) was applied to determine fenfluramine. The fenfluramine-imprinted polymer was prepared with acrylamide (AM) as functional monomer and ethylene glycol dimethacrylate (EGDMA) as cross-linker. Methyl and sulfonic group were introduced to rhodanine matrix, and a novel rhodanine ramification 3MORASP was synthesized by the author, and it was used as chemiluminescence reagent. 3-(3′-Methoxyphenyl)-5(2′-sulfonylphenylazo)-rhodanine (3MORASP), first synthesized by the authors, was used as chemiluminescence (CL) reagent. The novel flow path of FI-CL was designed, which made three merged streams of reactants injected into MIP column move through different pathways simultaneously. Fenfluramine was detected based on the reaction of fenfluramine, 3MORASP, and potassium permanganate in an acidic medium. The CL intensity was correlated linearly with the concentration of fenfluramine over the range of 1.0 × 10^?7 to 5.0 × 10^?6 g · mL^?1, and the detection limit was 9.48 × 10^?9 g · mL^?1. The relative standard deviation (RSD) was 2.4% for determination of 1.0 × 10^?6 g · mL^?1 fenfluramine (n = 11). This method was successfully applied to the determination of fenfluramine in weight-reducing tonic.     

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.     

Post‐chemiluminescence Method of the Determination of Loperamide Hydrochloride in Human Plasma and Pharmaceutical by Using Dichlorofluorescein as Chemiluminescence Reagent

Abstract

A post‐chemiluminescence (PCL) was observed when loperamide hydrochloride solution was injected into the reaction mixture after the finish of CL reaction of alkaline N‐Chlorosuccinimide (NCS) and dichlorofluorescein. Based on this phenomenon, a simple, sensitive and fast flow injection PCL method was established for the determination of loperamide hydrochloride. The possible mechanism for the PCL reaction was discussed via the investigation of the CL kinetic characteristics, the CL spectra, the fluorescence spectra. The PCL intensity responded linearly to the concentration of loperamide hydrochloride in the range 8.0×10^?10 to 6.0×10^?7 g · ml^?1 with a linear correlation of 0.9995. The detection limit was 4×10^?10 g · ml^?1. The relative standard deviation was 2.4% for 4.0×10^?8 g · ml^?1 loperamide hydrochloride (n=11). This method has been applied to the determination of loperamide hydrochloride in human plasma and pharmaceutical samples with satisfactory results.     

Determination of riboflavin by enhancing the chemiluminescence intensity of peroxomonosulfate-cobalt(II) system

A weak chemiluminescent (CL) emission was observed in the decomposition of peroxomonosulfate (HSO5-), which would be accelerated in the presence of trace amounts of cobalt (II). The mechanism was due to the production of singlet oxygen (1O2). Interestedly, riboflavin can enhance the CL and the CL intensity was strongly dependent on riboflavin concentration. Based on this phenomenon, a flow injection analysis (FIA) CL method was established for the determination of riboflavin. Additionally, the possible CL mechanism is proposed based on the kinetic curve of the CL reaction, CL spectra, UV-vis spectra and fluorescent spectra. The CL intensity was correlated linearly with concentration of riboflavin over the range of 1.0x10(-4) to 1.0x10(-8) g mL-1; the detection limit was 9.0x10(-9) g mL-1(S/N=3); the relative standard deviation was 1.4% for 9x10(-7) g mL-1 riboflavin (n=11). Furthermore, this method was applied to the determination of riboflavin in real tablets and injections successfully.     

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.     

A Novel Enhanced Chemiluminescence System with Ag(III) Complex for the Determination of Ofloxacin and Levofloxacin in Pharmaceutical Preparation and Biological Fluid

A novel chemiluminescence (CL) method is developed for determination of ofloxacin and levofloxacin with Ag(III) complex in H₂SO₄ solution medium. The CL intensity is proportional to drug concentration in a wider range with a correlation coefficient of 0.999. The limit of detection (s/n = 3) for ofloxacin and levofloxacin was 5.3 × 10^?9 g ml^?1 and 8.3 × 10^?9 g ml^?1, respectively, and their recoveries from urine and serum samples were in the range of 90.1–112% with the RSDs of 1.0–2.8%. The proposed method was applied for analysis of real samples with satisfactory result. The possible CL mechanism was discussed.     

基于LaPO_4∶Ce,Tb-Au发光共振能量转移测定细胞色素C

以膦酰基羧酸共聚物为修饰剂,采用水热法制备了LaPO_4∶Ce,Tb发光纳米粒子,该粒子具有良好的水溶性和生物相容性。对合成的纳米粒子进行了发光光谱、X-射线衍射、透射电子显微镜和红外光谱表征。以制备的纳米粒子为能量供体,纳米金为能量受体,细胞色素C(Cyt C)为桥,构建了LaPO_4∶Ce,Tb-Au发光共振能量转移(LRET)体系,据此建立了测定Cyt C的新方法。实验结果表明,当Cyt C的浓度在0.333~21.0μg·mL~(-1)范围时,LRET体系发光猝灭程度与Cyt C浓度呈良好线性关系,检出限(S/N=3)为0.2μg·mL~(-1),相对标准偏差(RSD)为0.46%(c=10.0μg·mL~(-1),n=11)。该方法用于实际样品的测定,回收率范围为100%~101%。