流动注射化学发光法测定DL-酪氨酸

在甲醛存在下 ,高锰酸钾与DL 酪氨酸能够发生化学发光反应 ,产生很强的化学发光。据此采用流动注射技术 ,建立了一种测定DL 酪氨酸的化学发光分析法。方法的检出限为 2 .9× 1 0 - 8g/mL ,相对标准偏差为 1 .5 % ( 1 .0× 1 0 - 6g/mLDL 酪氨酸 ,n =1 1 ) ,线性范围为 1 .0× 1 0 - 7g/mL～ 5 .0× 1 0 - 6g/mL。     

流动注射化学发光法测定甲硝唑

在碱性条件下 ,铁氰化钾氧化鲁米诺产生化学发光 ,甲硝唑对该体系有显著的增强作用 (亚铁氰化钾存在时 )。基于此 ,建立了流动注射化学发光测定痕量甲硝唑的新方法。甲硝唑浓度在 2 .0× 1 0 -6～ 4 .0× 1 0 -4 mol L范围内与发光强度呈良好的线性关系 ;检出限 (3σ)为 1 .5× 1 0 -7mol L。相对标准偏差 (c =1 .0× 1 0 -5mol L ,n=1 1 )为 3.6 %。方法已用于制剂中甲硝唑含量测定     

流动注射化学发光法测定褪黑素

在强碱性介质中,铁氰化钾可直接氧化褪黑素产生化学发光。基于此,建立了一种测定褪黑素的流动注射化学发光分析方法。线性范围为1.9×10-6~2.3×10-4g/mL,检出限为5×10-7g/mL,该法已用于药物中褪黑素的测定。     

Determination of iodide by detection of iodine using gas-diffusion flow injection and chemiluminescence

This work describes development of a flow injection (FI) system for determination of iodide, based on the chemiluminescence (CL) reaction between iodine and luminol. Iodide in the sample zone is oxidized to iodine. Employment of a gas-diffusion (GD) unit allows for selective detection of the generated CL (425 nm). Preliminary results showed for concentrations of less than 2 mg L⁻¹, that signals were irreproducible and that the calibration was not linear.In order to solve these problems, a method of ‘membrane conditioning’ was investigated, in which iodide stream was continuously merged with oxidant to generate I₂ that conditioned the GD membrane and tubing. This minimized surface interaction between the active surface and the I₂ generated from the samples, thus improving both precision and sensitivity. By employing membrane conditioning, it has been possible to reliably detect concentrations down to 0.1 mg L⁻¹.At the optimized condition, an excellent linear calibration (r² = 0.999) was obtained from 0.1 to 1.0 mg L⁻¹. The method was successfully applied to determine iodide in some pharmaceutical products such as potassium iodide tablets and a liquid patent medicine. However, for vitamin tablets, ascorbic acid was found to interfere seriously by causing a negative signal.     

Potassium permanganate-glyoxal chemiluminescence system for flow injection analysis of cephalosporin antibiotics: cefalexin, cefadroxil, and cefazolin sodium in pharmaceutical preparations

A sensitive flow injection chemiluminescence (FL-CL) method for the determination of cephalosporin antibiotics, was developed. The method was based on that cephalosporin antibiotics could enhance the CL reaction of glyoxal and KMnO₄ in sulfuric acid. Method development included the optimization of reagent concentrations and flow-rate. Under the optimized conditions, three cephalosporin antibiotics: cefalexin, cefadroxil, and cefazolin sodium, were determined. The detection limits of the method are 10 ng ml⁻¹ cefalexin, 2 ng ml⁻¹ cefadroxil, and 2 ng ml⁻¹ cefazolin sodium. The method was successfully applied to the determination of three cephalosporin antibiotics in pharmaceutical preparations.     

流动注射-化学发光法测定富马酸依美斯汀

在酸性条件下,KMnO4与甲醛能够产生微弱的化学发光,而富马酸依美斯汀的存在能够大大增强该化学发光强度;结合流动注射技术,建立了测定富马酸依美斯汀的流动注射-化学发光新方法。该方法的线性范围分别为3.0×10-8～2.0×10-7g/mL,2.0×10-7～1.0×10-6g/mL和1.0×10-6～8.0×10-6g/mL。检出限为1.0×10-8g/mL,对2.0×10-6g/mL富马酸依美斯汀滴眼液平行测定11次,其相对标准偏差为1.3%。该方法已成功应用于滴眼液中富马酸依美斯汀的含量测定。     

流动注射化学发光法测定甲氧氯普胺

在酸性条件下，甲醛对高锰酸钾氧化甲氧氯普胺的化学发光反应有很强的增敏作用，据此，建立了流动注射化学发光法测定甲氧氯普胺纳新方法。方法的线性范围为0．4-100μg/mL，检出限为0．2μg/mL，对10μg/mL的甲氧氯普胺标准溶液连续11次测定的相对标准偏差为1．8％。方法已用于药物中甲氧氯普胺含量的测定。     

流动注射-化学发光法测定决明子蒽醌类化合物

基于在碱性条件下,蒽醌对ClO- Luminol化学发光体系的显著抑制作用,结合反向流动注射技术,提出了蒽醌的流动注射 化学发光分析新方法。蒽醌的质量浓度在0.5～100μg mL范围内与化学发光的抑制强度呈良好的线性关系。检出限为0.05μg mL,RSD=1.6%,采样频率为150次 h,回收率为105%～107.5%。     

流动注射化学发光法测定青霉素G钾

在甲醛的存在下,酸性KMnO4与青霉素G钾能够产生很强的化学发光,从而建立了KMnO4-甲醛-青霉素G钾化学发光体系来测定青霉素G钾.青霉素G钾的测定线性范围为2.0×10-7～1.0×10-5 g/mL,方法的检出限为1.4×10-7 g/mL,对4.0×10-7 g/mL的青霉素G钾进行11次平行测定,相对标准偏差为1.0%,用此法测定青霉素G钾取得了较好的结果.     

流动注射化学发光法测定丹皮酚

丹皮酚有解热、消炎、止痛、镇静等功效[1]。目前测定丹皮酚的方法有高效液相色谱法[2,3]、薄层色谱法[4]、毛细管气相色谱法[5]、毛细管电泳法[6,7]、紫外分光光度法[8]。流动注射是一种高度重现的进样技术[9],它同化学发光法联用,具有快速、灵敏和仪器简单等优点。用化学发光     

Determination of nicotinamide by stopped-flow injection method in pharmaceutical formulations

A simple stopped-flow injection system with spectrophotometric detection was proposed for the determination of nicotinamide (NAM) in pharmaceutical formulations. In this system cyanogen chloride formed from the combination of an acidic KSCN with the NaClO streams reacts with injected NAM to form glutaconic aldehyde. Then the product of these three components was coupled with another buffered (pH 3.5) stream of barbituric acid and directed towards the detector. A 45 s after sample injection the pump was stopped for 130 s. During this time the reactants in the flow cell were provided with the required temperature (40 °C) by placing the cell in a home made cell jacket to increase the yield of the polymethine dye product. Eventually, the absorbance of the formed pink color dye was monitored spectrophotometrically at 560 nm and NAM in the concentration range of 1.0–25.0 μg/mL (R = 0.9974 and D.L = 0.5 μg/mL) was determined. The results obtained by this method were compared statistically and agree with those obtained by the method described in the British Pharmacopoeia.     

铁氰化钾-钙黄绿素体系流动注射化学发光法测定孔雀石绿

基于在碱性条件下,孔雀石绿可以增强铁氰化钾-钙黄绿素的化学发光,且其浓度在一定范围内与化学发光强度呈线性关系,结合流动注射技术,建立了化学发光法测定孔雀石绿的新方法。在优化的实验条件下,方法的线性范围为3.0×10-8～1.0×10-6 g/mL,检出限为2.5×10-9 g/mL,对浓度为1.0×10-7g/mL的孔雀石绿溶液进行11次平行测定,相对标准偏差为2.3%。方法可应用于环境水样的测定。     

Sensitive Determination of Nanogram Levels of Diacerein in a Pharmaceutical Formulation by Flow Injection Chemiluminescence Analysis

A simple, sensitive and inexpensive flow injection chemiluminescence (FI‐CL) method for the determination of diacerein was proposed. It was based on the greatly enhancive effect of diacerein on the CL reaction between luminol and hydrogen peroxide in alkaline medium. The enhanced CL intensity was linear with the concentration of diacerein over the range 1.0–500 ng/mL with a detection limit (3σ) of 0.2 ng/mL. The relative standard deviation was 1.1% (n = 8, 20 ng/mL diacerein) and the sample throughput was about 120 samples h^?1. This simple method has been successfully applied for the determination of diacerein in a pharmaceutical formulation without interference from its potential impurities. The degradation of diacerein was also investigated briefly.     

流动注射化学发光法测定痕量NO_2~-的研究与应用

Based on the principle of the reaction of NO2-with I-and formation of I2 in HCl solution,and the chemiluminescence(CL) reaction between luminol and I2 in an alkaline medium.A fairly sensitive,simple and rapid flow-injection analysis-chemiluminescence method for the determina-tion of trace nitrite with the luminal-I——NO2-coupling luminescence system has been developed.Experiment conditions of flow-injection analysis are optimized.When satisfying the condition that Luminol as 4.0×10-4 mol/L,0.7 % KI,0.04 mol/...     

快速化学发光联用流动注射技术测定西咪替丁

在NaOH-NaHCO3介质中,铁氰化钾氧化西咪替丁产生快速化学发光反应,0.5 s后发光达到最大,2 s后迅速衰减至零。本文结合流动注射技术,建立了一种化学发光测定西咪替丁的新方法。针对这一快速发光反应,设计了与之相应的管路系统和最短的反应管道来捕捉最大化学发光信号,发光强度与西咪替丁质量浓度在5×10-7~1×10-4g/mL范围内呈线性关系,检出限为1.1×10-7g/mL。对5×10-6g/mL西咪替丁进行11次平行测定,相对标准偏差为1.8%。本法已用于西咪替丁片剂的测定。     

Sensitive determination of captopril by flow injection analysis with chemiluminescence detection based on the enhancement of the luminol reaction

This work reports a novel flow injection (FI) method for the determination of captopril, 1-[(2S)-3-mercapto-2-methylpropionyl]-l-proline (CPL), based on the enhancement CPL affords on the chemiluminescence (CL) reaction between luminol and hydrogen peroxide. For this purpose alkaline luminol and hydrogen peroxide solutions were mixed online, the sample containing CPL was injected into an aqueous carrier stream, mixed with the luminol-hydrogen peroxide stream and pumped into a glass flow cell positioned in front of a photomultiplier tube (PMT). The increase in the CL intensity was recorded in the form of FI peaks, the height of which was related to the CPL mass concentration in the sample. Different chemical and instrumental parameters affecting the CL response were investigated. Under the selected conditions, the log-log calibration curve was linear in the range 5-5000 μg l⁻¹ of CPL, the limit of detection was 2 μg l⁻¹ (at the 3σ level), the R.S.D., s_r was 3.1% at the 100 μg l⁻¹ level (n=8) and the sampling rate was 180 injections h⁻¹. The method was applied to the determination of CPL in pharmaceutical formulations with recoveries in the range 100±3%.     

Sensitive determination of phenothiazines in pharmaceutical preparation and biological fluid by flow injection chemiluminescence method using luminol-KMnO4 system

A flow injection chemiluminescence method was described for the determination of four phenothiazine drugs, namely, chlorpromazine hydrochloride, perphenazine hydrochloride, fluphenazine hydrochloride and thioridazine hydrochloride. Strong Chemiluminescence (CL) signal was produced when above-mentioned drug was injected into the mixed stream of luminol with KMnO₄. The linear ranges of the method were 0.0020-1.0 μg/mL chlorpromazine hydrochloride, 0.0040-3.0 μg/mL perphenazine hydrochloride, 0.0020-5.0 μg/mL fluphenazine hydrochloride and 0.0050-1.0 μg/mL thioridazine hydrochloride. The detection limits were 0.4 ng/mL chlorpromazine hydrochloride, 0.7 ng/mL perphenazine hydrochloride, 2 ng/mL fluphenazine hydrochloride and 0.7 ng/mL thioridazine hydrochloride. The proposed method was applied to the determination of chlorpromazine hydrochloride in injections and in mental patient's urine samples and the satisfactory results were achieved. The possible CL reaction mechanism was also discussed briefly.     

流动注射化学发光法测定茶饮料中的茶多酚

在碱性条件下,茶多酚对鲁米诺-KMnO4化学发光体系具有较强的抑制作用,据此建立了茶多酚的流动注射化学发光测定法。该法的化学发光抑制值ΔICL与茶多酚质量浓度在2.0×10-6~5.0×10-4mg/mL范围内,呈现出良好的线性关系,检出限为1.2×10-7mg/mL,对1.0×10-5mg/mL茶多酚测定的相对标准偏差为2.9%(n=11)。用于茶饮料中茶多酚的测定。     

Selective determination of amino acids using flow injection analysis coupled with chemiluminescence detection

The determination of the amino acids proline, histidine, tyrosine, arginine, phenylalanine and tryptophan using flow injection analysis (FIA) with chemiluminescence detection is described. Proline was the only amino acid to exhibit chemiluminescence with the tris(2,2-bipyridyl)ruthenium(III) reaction at pH 10. While, histidine was found to selectively enhance the reaction of luminol with Mn(II) salts in a basic medium. Acidic potassium permanganate chemiluminescence was able to selectively determine tyrosine at pH 6.75. Low pressure separations using a C18 guard column allowed the simultaneous determination of tyrosine and tryptophan or phenylalanine and tryptophan with acidic potassium permanganate and copper(II)-amino acid-hydrogen peroxide chemiluminescence, respectively. Precision for each method was less than 3.9% (R.S.D.) for five replicates of a standard (1×10⁻⁵ M) and the detection limits ranged between 4×10⁻⁹ and 7×10⁻⁶ M. Preliminary investigations revealed that the methodology developed was able to selectively determine the individual amino acids in an equimolar mixture of the 20 naturally occurring amino acids.     

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。