反相高效液相色谱-增敏化学发光同时测定VB1和VC

本文基于维生素B1(VB1)、维生素C(VC)对鲁米诺(Luminol)和铁氰化钾(K3[Fe(CN)6])化学发光反应的增敏作用原理,建立了反相高效液相色谱(RP-HPLC)分离、柱后化学发光检测VB1与VC的新方法。当在鲁米诺中加入KBr时可以大大增敏该反应。本法已成功运用于蜂蜜和复合维生素片中VB1与VC的测定。     

化学发光分析法测定动物蛋白粉等样品中的锰

基于Mn(Ⅱ) 邻菲罗啉对鲁米诺 KIO4化学发光体系的催化作用建立了测定Mn(Ⅱ)的分析方法。Mn(Ⅱ)质量浓度在2.0×10-6～5.0×10-5mg/mL范围与发光强度呈线性响应,回归方程为ICL=0.6+1.39×106ρ(mg/mL),检出限为2.0×10-6mg/mL。Cr3+、Fe2+、Co2+、Au3+等离子有干扰,使用EDTA、F-、8 羟基喹啉等为掩蔽剂可消除或降低干扰。将该法应用于生物化工产品丙酸钙、动物蛋白粉等中痕量锰的测定,加标回收率98%～102%,10次测定RSD为4 6%。将测定的结果与原子吸收法比较,相对偏差≤±3%。     

Selective flow-injection determination of methanol in the presence of ethanol based on a multi-enzyme system with chemiluminescence detection

A highly selective flow-injection system was developed for the determination of methanol. The system consisted of three immobilized enzymes with luminol chemiluminescence detection. First, methanol was oxidized in the presence of alcohol oxidase to yield formaldehyde and hydrogen peroxide. The hydrogen peroxide produced was then destroyed by catalase. The formaldehyde formed in the first stage was further oxidized by NAD⁺-formaldehyde dehydrogenase. The NADH formed was oxidized by 1-methoxy-5-methylphenazinium methylsulphate (1-MPMS), and finally the reduced 1-MPMS was spontaneously oxidized and hydrogen peroxide was produced. The concentration of the hydrogen peroxide produced, which was proportional to the initial concentration of methanol, was determined by luminol chemiluminescence. The determination range was from 0.1 to 100 mg l⁻¹ and the response time was less than 2 min per sample with a relative standard deviation of less than 3%. The system showed good selectivity for methanol; the response was ca. 50 times higher than for ethanol.     

Characterization of chemiluminescence from singlet oxygen under laminar flow conditions in a micro-channel and its quenching with beverages

Singlet oxygen was generated by reaction of sodium hypochlorite and hydrogen peroxide in a micro-channel. The two reagent solutions were delivered into the micro-channel by a syringe pump, providing a laminar flow liquid-liquid interface. The chemiluminescence from the singlet oxygen was emitted in the collapse of the interface due to molecular diffusion under laminar flow conditions. The chemiluminescence intensity was observed continuously and stably for each combination of reagents fed into the micro-channel; while, in the normal batch-type reactor the chemiluminescence peaks from singlet oxygen were observed within ca. 5 s. The features of the chemiluminescence emitted under laminar flow conditions were examined by changing the concentrations of sodium hypochlorite and hydrogen peroxide; the concentrations of 2.5 mM sodium hypochlorite and 7.5 mM hydrogen peroxide provided highest chemiluminescence intensities without bubble formation. Also, the effects of beverages, such as green tea, coffee, white wine, red wine, and sake (rice wine), on the chemiluminescence intensity as well as the concentrations of sodium hypochlorite and hydrogen peroxide were examined. The chemiluminescence intensities observed with addition of the beverages to the reagents decreased in the following orders; green tea > coffee > red wine > rice wine > white wine (being added to sodium hypochlorite); coffee > white wine > green tea > red wine > rice wine (being added to hydrogen peroxide). It was found that coffee decreased the chemiluminescence intensity (ca. 33% chemiluminescence decrease) without altering the concentrations of sodium hypochlorite or hydrogen peroxide. The cause of the decrease in chemiluminescence with coffee is discussed.     

硫酸铈-亚硫酸钠流动注射化学发光法测定多贝斯

基于多贝斯对硫酸铈-亚硫酸钠化学发光体系的抑制作用,建立了流动注射-化学发光测定多贝斯的新方法,并且研究了各种实验条件的影响。在酸性介质中,发光强度的降低(ΔICL)与多贝斯浓度在4.0×10-6~6.0×10-5mol/L范围内呈良好线性关系,回归相关系数为0.9976,方法的检出限为2.0×10-6mol/L,相对标准偏差为1.2%(n=6)。     

A New Chemiluminescence Amplification Reaction for the Determination of HRP and Labelled HRP

A new chemiluminescence amplification reaction has been developed, which is on the coupling of the oxidation of Eosin by hydrogen peroxide under the catalysis of HRP at pH 3. 5 to the chemiluminescent reaction of luminol and hydrogen peroxide catalyzed by HRP at pH 10 to measure the activity of HRP and labelled-HRP. The detection limit of HRP is 10-10 g/mL. The lowest dilution ratio of HBsAb-HRP is 1 : 1. 8×102 and 1 : 106 for the direct method and coupled method respectively.     

用微芯片化学反应器实现酶催化化学发光测定葡萄糖的研究

葡萄糖是临床化学诊断以及食品分析中重要的检测项目 ,最常用的测定方法是采用葡萄糖氧化酶(GOD)催化葡萄糖与氧分子间反应 ,生成葡萄糖酸和过氧化氢 [1] ,而对过氧化氢的检测则可采用过氧化酶 (POD)催化鲁米诺的化学发光反应进行 [2 ] .FIA对整个过程的实现是十分有效的方式 ,但由于多采用固定化酶反应器 [3～ 5] 使其在制备及分析上较复杂且费用高 .由 Manz等[6] 提出的微型全分析系统(μ- TAS)在针对不同体系的微量分析及在线监测上均具有突出的优越性 .本文使用的含微混合器的微芯片化学反应器采用μ- TAS设计思想 ,建立了化学发…     

In Vitro Determination of Dobesilate in Medicine and Human Urine with Chemiluminescence Detection

A unique flow injection chemiluminescence (CL) method for the determination of calcium dobesilate in pharmaceutical preparations and human urine is presented in this paper. The analytical reagents involved in the CL reaction, luminol and ferricyanide, were both immobilized on an anion-exchange column in an FI system. The CL signal produced by the reaction of luminol with ferricyanide (the reagents had been eluted from the column through sodium phosphate injection) decreased in the presence of dobesilate. The decreased CL intensity was linear to the dobesilate concentration in the range 0.2100.0ngmL^–1. At a flow rate of 2.0mLmin^–1, one analytical cycle can be completed in 1.5min, including sampling and washing, resulting in a throughput of 40 cycles per hour. The proposed method was applied successfully to the determination of dobesilate in pharmaceutical preparations and human urine without any pre-treatment. It was found that, after oral administration, the dobesilate concentration reached its maximum after three hours, and the dobesilate metabolism ratio in 24 hours was 57.1% in the bodies of volunteers.Received September 14, 2002; accepted March 11, 2003 Published online July 16, 2003     

偶合反应化学发光法测定痕量银的研究——K4Fe（CN）6—Luminol体系

将Ａｇ（Ｉ）催化Ｋ４Ｆｅ（ＣＮ）６的水合反应与Ｌｕｍｉｎｏｌ同Ｃｕ（ＣＮ）＾２－４的化学发光反应相偶合，建立起一种新的灵敏测定痕量银的化学发光分析法，在所研究的优化条件下，该法测定银的选择性较好，检测限达到４．０×１０＾－１３ｇ／ｍＬＡｇ线性浓度范围为１．０×１０＾－１２～１．０×１０＾－６ｇ／ｍＬＡｇ对４×１０＾－１１ｇ／ｍＬＡｇ（Ｉ）溶液连续１１次测定的ＲＳＤ≤３．５％，用于环境水和岩矿中银的     

偶合反应化学发光法测定痕量银的研究

本将Ａｇ（Ⅰ）催化Ｓ２Ｏ＾２－８氧化Ｍｎ（Ⅱ）生成ＭｎＯ＾－４的催化反应与ＬｕｍｉｎｏｌＭｎＯ＾－４－ＯＨ＾－的化学发光反应相偶合，建立起一种新的灵敏测定痕量银的化学发光分析法，在所研究的优化条件下，该法测定银的选择性较好，检测限达到３．２×１０＾－１２ｇ／ｍＬＡｇ线性浓度范围为１．０×１０＾－１１－１．０×１０＾－５ｇ／ｍＬＡｇ，用于水样分析，结果较为满意。