A flow injection chemiluminescence system for the determination of isoniazid

A chemiluminescence (CL) flow system is described for the determination of isoniazid based on its enhancement on the chemiluminescence (CL) emission produced upon mixing a hexacyanoferrate(III) solution with an alkaline luminol solution. The system responds linearly to isoniazid concentration in the range 0–1 mg/L with a detection limit (3σ) of 0.03 μg/L, relative standard deviation (RSD) of 1.2% for 0.1 mg/L isoniazid (n = 11). The system has been successfully applied to the determination of isoniazid in pharmaceutical preparations.     

采用甲基丙烯酸丁酯整体微柱芯片系统测定血样中痕量异烟肼

将合成的甲基丙烯酸丁酯(BMA)整体柱与微流控芯片技术结合,在PMMA芯片上以K3Fe(CN)6-NaOH-异烟肼化学发光体系为样品对象,在优化混合发光试剂比例和流速以及选择适合的洗脱液基础之上,实现了BMA整体微柱对异烟肼样品的富集作用,平均富集倍数和回收率分别达到16.8和84.2%,由此建立了流动注射化学发光(FIA-CL)芯片系统测定血液中痕量异烟肼的浓度的方法,可有效地实现异烟肼血药浓度分析的片上预处理和快速测定,检出限低于0.2 mg/L。     

流动注射后化学发光法测定异烟肼

本文发现了异烟肼在铁氰化钾-钙黄绿素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异烟肼的流动注射化学发光分析法。方法的检出限为6×10-8g/mL, 相对标准偏差为1.8% (2.0×10-6 g/mL 异烟肼,n=11）,线性范围为2.0×10-7~1.0×10-5 g/mL。此法已用于异烟肼片剂中异烟肼含量的测定,结果与药典方法测定值一致。     

鲁米诺-铁氰化钾流动注射化学发光法测定头孢拉定

在碱性介质中,铁氰化钾氧化鲁米诺产生化学发光,头孢拉定对该体系有显著的增强作用。基于此并结合流动注射技术建立了测定头孢拉定含量的化学发光新方法。该法线性范围为0.16~160 mg/L,检出限为0.028 mg/L;对80 mg/L的头孢拉定进行平行测定11次,其相对标准偏差为0.99%。用本法对胶囊中头孢拉定进行测定,并初步探讨了该化学发光的反应机理。     

高效液相色谱—化学发光法研究异烟肼和利福平

基于异烟肼和利福平在碱性介质中能与K3Fe(CN)6反应产生强的化学发光，因 此设计了一个经高效液相色谱（HPLC）分离柱后同时检测一线抗结构病药物异烟肼 、利福平的化学发光检测器。研究并优化了流动相、流速以及化学发光检测的条件 。该方法测定异烟肼、利福平的线性范围分别为0.05～6.0mg/L，0.08～20.0mg/L ，其检出限：异烟肼为2×10^-2mg/L，利福平为4×10^-2mg/L，测定的相对标准偏 差分别为1.9，2.9。该方法已成功地用于同时测定复方利福平片中利福平和异烟肼 的含量。     

Gold Nanoparticles‐enhanced Chemiluminescence Determination of Fenfluramine

A simple and sensitive chemiluminescence method was developed for the determination of fenfluramine. The chemiluminescence signal arising from the reaction between alkaline luminol and N‐bromosuccinimide was found to be greatly enhanced by fenfluramine in the presence of gold nanoparticles. But fenfluramine alone slightly inhibited the CL signal of N‐bromosuccinimide‐luminol in the absence of gold nanoparticles. The experimental parameters that affected the chemiluminescence signal were thoroughly investigated. Under the optimum experimental conditions, the enhanced chemiluminescence intensity was proportional to the concentration of fenfluramine in the range of 0.005‐1.0 mg/L. The detection limit was 0.9 μg/L fenfluramine with a relative standard deviation of 2.5% for 0.1 mg/L fenfluramine solution (n = 11). The method was applied to the determination of fenfluramine in some weight‐reducing tonics and in spiked human urine. A possible CL reaction mechanism was proposed.     

Flow Injection Chemiluminescence Determination of Isoniazid Using On-Line Electrogenerated Manganese(III) as Oxidant

A novel flow injection chemiluminescence (CL) system for the determination of isoniazid has been proposed. It is based on the direct CL reaction of isoniazid and Mn(III) in sulfuric acid medium. The unstable Mn(III) was on-line electrogenerated by constant current electrolysis. The CL emission intensity was linear with isoniazid concentration in the range 0.1–10 μg/mL; the detection limit was 3.2 × 10⁻² μg/mL. The whole process could be completed in 1 min with a relative standard deviation of less than 5%. The proposed method is suitable for automatic and continuous analysis and has been applied successfully to the analysis of isoniazid in pharmaceutical preparation.     

Reversed Flow Injection Chemiluminescence Determination of Pyridoxine Hydrochloride Based on the Cerium(IV)-Sodium Sulfite System

A rapid chemiluminescence (CL) reaction was observed when Ce(IV) was injected into the mixed solution of pyridoxine hydrochloride and sodium sulfite. A new flow-injection CL method for the determination of pyridoxine hydrochloride was established. The detection limit (3σ) was 0.5 mg/L pyridoxine hydrochloride and the relative standard deviation (RSD) was 3.3% (n = 11, γ = 5 mg/L). The CL intensity responded linearly to the concentration of pyridoxine hydrochloride in the ranges 1.0–10.0 mg/L and 10.0–100.0 mg/L with linear correlation coefficients of 0.9994 and 0.9991, respectively. The method had been applied to the determination of pyridoxine hydrochloride in tablets and injections successfully.     

Simultaneous determination of rifampicin and isoniazid by continuous-flow chemiluminescence with artificial neural network calibration

In this paper a continuous-flow chemiluminescence (CL) system with artificial neural network calibration is proposed for simultaneous determination of rifampicin and isoniazid. This method is based on the different kinetic spectra of the analytes in their CL reaction with alkaline N-bromosuccinimide as oxidant. The CL intensity was measured and recorded every second from 1 to 300 s. The data obtained were processed chemometrically by use of an artificial neural network. The experimental calibration set was 20 sample solutions. The relative standard errors of prediction for both analytes were approximately 5%. The proposed method was successfully applied to the simultaneous determination of rifampicin and isoniazid in a combined pharmaceutical formulation.     

流动注射化学发光抑制法测定阿魏酸钠

提出了Fe2+-H2O2-亚甲基蓝化学发光新体系并用于阿魏酸钠的测定。实验发现,在酸性介质中,Fe2+-H2O2体系可与亚甲基蓝反应产生极强的化学发光,阿魏酸钠对此化学发光具有显著的抑制作用。据此,结合流动注射技术,建立了阿魏酸钠化学发光分析新方法。研究了影响化学发光强度的因素,化学发光信号的降低值(ΔI)与阿魏酸钠浓度在4.5×10-6～4.5×10-5mol/L范围内呈良好的线性关系,方法的检出限为7.0×10-7mol/L。对4.8×10-6mol/L的阿魏酸钠进行了11次平行测定,其RSD=0.8%,该法已用于片剂中阿魏酸钠含量的测定。     

流动注射-化学发光法测定头孢氨苄

头孢氨苄在H2SO4溶液中降解后,其产物可在酸性条件下与Ce（Ⅳ）产生化学发光反应,罗丹明6G对该反应有较强的增敏作用。据此建立了流动注射－化学发光法测定头孢氨苄的新方法。该方法的线性范围为0.10－10.0mg/L检出限为0.06mg/L,相对标准偏差(n=11,c=1.00mg/L）为0.85。方法用于药物中头孢氨苄含量的测定,其结果与标准方法一致,回收率为96％－106％。     

Flow-injection chemiluminescence sensor for determination of isoniazid in urine sample based on molecularly imprinted polymer

In this paper, molecularly imprinted polymer (MIP) of isoniazid is synthesized through thermal radical copolymerization of metharylic acid (MAA) and ethylene glycol dimethacrylate (EGDMA) in the presence of isoniazid template molecules. A novel flow injection chemiluminescence sensor for isoniazid determination is developed by packing the isoniazid-MIP into the flow cell as recognition elements. Isoniazid could be selectively adsorbed by the MIPs and the adsorbed isoniazid was sensed by its great enhancing effect on the weak CL reaction between luminol and periodate which were mixed in the flow cell. The enhanced CL intensity is linear in the range 2x10(-9) to 2x10(-7) g/mL and the detection limit is 7x10(-10) g/mL (3sigma) isoniazid with a relative standard deviation 2.8% (n=9) for 8x10(-8) g/mL. The sensor is reversible and reusable. It has a great improvement in sensitivity and selectivity for CL analysis. As a result, the sensor has been successfully applied to determination of isoniazid in human urine. At the same time, the binding characteristic of the polymer to isoniazid was evaluated by batch method and the dynamic method, respectively.     

Chemiluminescence sensor for isoniazid with controlled-reagent-release technology

A novel chemiluminescence (CL) sensor for isoniazid combined with flow-injection technology is presented in this paper. The analytical reagents, luminol and ferricyanide, were both immobilized on an anion-exchange column. The CL signal produced by the reaction between luminol and ferricyanide, which were eluted from the column through sodium phosphate injection, was decreased in the presence of isoniazid. The decreased CL intensity was linear with isoniazid concentration in the range 0.001–1.0 μg·ml⁻¹; and the detection limit was 0.35 ng·ml⁻¹ (3s). The whole process, including sampling and washing, could be completed in 2 min with a relative standard deviation of less than 4.1%. The sensor could be reused more than 400 times and has been applied for the determination of isoniazid in pharmaceutical preparations.     

在线电生强氧化剂钴(Ⅲ)化学发光法测定地塞米松磷酸钠

本文基于Co3+在硫酸介质中能氧化地塞米松磷酸钠产生化学发光这一特性,建立了一种流动注射化学发光测定地塞米松磷酸钠的新方法。其中不稳定的强氧化剂Co3+是通过在硫酸介质中恒电流电解CoSO4在线产生的,从而消除了由于试剂不稳定性带来的一些不利因素。该方法测定地塞米松磷酸钠的线性范围为1～20 mg/L,检出限为3.2×10－7g/mL(DL=3S/r),相对标准偏差小于5%。该方法已成功地用于地塞米松磷酸钠注射液中地塞米松磷酸钠的测定。     

Chemiluminescence Flow Injection Analysis of Menadione Sodium Bisulfite Based on Luminol Reaction

ABSTRACT

A chemiluminescence(CL) flow system is described for the determination of menadione sodium bisulfite based on its repression on the chemiluminescence(CL) emission produced upon mixing a hexacyanoferrate(III) solution with an alkaline luminol solution in the absence of co-oxidizer. The system responds linearly to menadione sodium bisulfite concentration in the range 0-1 μg/mL with a detection limit (3σ) of 0.01 μg/mL. Relative standard deviation (RSD) of 0.16% for 0.4 μg/mL menadione sodium bisulfite (n=11). The system has been successfully applied to the determination of menadione sodium bisulfite in tablets and injections.     

Flow Injection Chemiluminescence Determination of Puerarin in Pharmaceutical Preparations Using Eosin Y‐Fenton System

A novel chemiluminescence (CL) system was established for the determination of puerarin in pharmaceutical preparations. It was shown that a strong CL signal was observed when Eosin Y reacted with the hydroxyl radicals which were generated from Fenton reagent in acidic medium. The CL intensity was decreased significantly when puerarin was added to the reaction system and partially scavenged the hydroxyl radicals in the solution. The extent of decrease in the CL intensity had a good stoichiometrical relationship with puerarin concentration. Based on this, a new method for the determination of puerarin using a flow injection chemiluminescence technique was developed. The experimental parameters that affected the CL intensity were optimized. Under the optimal conditions, the linear range for puerarin concentration was 8.0×10^?8?2.0×10^?6 mol/L (R=0.9982) with a detection limit of 7.5×10^?9 mol/L (S/N=3) and the relative standard deviation was 1.7% for 4.0×10^?7 mol/L puerarin (n=11). The proposed method was applied to the determination of puerarin in a puerarin injection with satisfactory results.     

Flow-injection system for automated dissolution testing of isoniazid tablets with chemiluminescence detection

A simple and sensitive flow-injection chemiluminescence (CL) system for automated dissolution testing is described and evaluated for monitoring of dissolution profiles of isoniazid tablets. The undissolved suspended particles in the dissolved solution were eliminated via on-line filter. The novel CL system of KIO(4)-isoniazid was also investigated. The sampling frequency of the system was 120 h(-1). The dissolution profiles of isoniazid fast-release tablets from three sources were determined, which demonstrates the stability, great sensitivity, large dynamic measuring range and robustness of the system.     

Flow Injection Chemiluminescence Determination of Prednisone Acetate by Oxidation with N-Bromosuccinimide

A simple flow injection chemiluminescence (CL) method for the determination of prednisone acetate was developed. This method is based on the fact that the strong CL of N-bromosuccinimide (NBS) and calcein can be inhibited by prednisone acetate. The CL intensity correlated linearly with the concentration of prednisone acetate over the ranges of 0.02–0.4 mg/L and 0.4–10 mg/L. The CL mechanism was also proposed. The detection limit (3σ) of prednisone acetate was 13 ng/mL and the relative standard deviation was 1.3% at 0.1 mg/L prednisone acetate (n = 11 measurements). This method was applied to the determination of prednisone acetate in the tablets with good results.     

Determination of Diammonium Glycyrrhizinate and Its Antioxidant Activity Using a Novel Chemiluminescence System

A novel chemiluminescence (CL) system was established for the determination of diammonium glycyrrhizinate (DG) in pharmaceutical preparations and its ability of scavenging hydroxyl radical. It was shown that a strong CL signal was observed when Eosin Y mixed with Fenton reagent. The CL intensity was decreased significantly when DG was added to the reaction system and partially scavenged the hydroxyl radicals in the solution. The extent of decrease in the CL intensity had a good stoichiometrical relationship with DG concentration. Based on this, we developed a new method for the determination of DG using a flow injection chemiluminescence (FI-CL) technique. Under the optimal conditions, the linear range of DG concentration was 6.0 × 10^?8–5.0 × 10^?6 mol/L (R = 0.9982) with a detection limit of 8.0 × 10^?9 mol/L (SN = 3), and the RSD was 3.8% for 2.0 × 10^?7 mol/L DG (n = 11). This method was successfully used in the determination of DG in tablets and the evaluation of hydroxyl radical scavenging capacity of DG. The possible reaction mechanism of the CL system is discussed.     

ClO3--SO32--Rh6G-SDBS体系的化学发光及其用于亚硫酸根测定

Based on the micelle synergism mechanism, a chemiluminescence （CL） flow system for the determination of sulfite was described. The CL signal generated from the reaction of chlorate with sulfite in acidic solution was very weak, while the interfusion of sodium dodecylbenzenesulfonate （SDBS） resulted in a highly chemiluminescent intensity. The major goal of this work was to investigate and develop the SDBS rnicelle synergetic CL system. The mechanism was proposed and proved by spectrometry. The results indicated that the unique structure of SDBS micelles prorooted the aggregation of rhodamine 6G （Rh6G） and a much easier energy transfer, leading to a marked shift to red in the CL emission. This CL system was developed for the determination of sulfite and the concentration of sulfite was proportional to the CL intensity in the range of 5.0× 10^-8--1.0× 10^-5 mol/L with the detection limit of 1.7×10^-8 mol/L （S/N=3）. The relative standard deviation was 3.3% for 1.0×10^ 6 mol/L sulfite solution with eleven repeated measurements. This method was successfully applied to the determination of sulfite in powder sugar.