Organic media enhanced spectrofluorimetric determination of L-ascorbic acid

A novel spectrofluorimetric method for the determination of L-ascorbic acid is proposed. It is based on the inhibition of L-ascorbic acid on the formation of 2,3-diaminophenazine, which is an oxidation product ofo-phenylenediamine catalyzed by laccase. The fluorescence (at λ_cx/λ_cm=464 nm /530 nnm) was enhanced strongly in the presence of organic media. The mechanism ofo-phenylenediamine oxidation reaction catalyzed by laccase in the presence of L-ascorbic acid is discussed. L-ascorbic acid is determined in the ethanol, 1,4-dioxane and acetone over the linear range of 4.0×10⁻⁷≈1.2×10⁻⁴ mol/L, 4.0×10⁻⁷≈8.0×10⁻⁵ mol/L and 4.0×10⁻⁷≈1.0×10⁻⁴ mol/L with a detection limit of 1.20×10⁻⁵ mol/L, 1.19×10⁻⁵ mol/L and 1.24×10⁻⁸ mol/L, respectively. The method has been successfully applied to the simple and rapid determination of L-ascorbic acid in pharmaceuticals and milk powder. Supported by National Natural Science Foundation of China and the Special Funds of State Education Committe for Doctorate Research Huang Zuyun: born in Aug. 1963. Ph.D     

光谱法研究6-糠氨基嘌呤与牛血清白蛋白的相互作用

利用荧光光谱法、紫外光谱法、荧光寿命和圆二色光谱法等方法研究了6-糠氨基嘌呤(KT)与牛血清白蛋白(BSA)之间相互作用机理.结果表明,KT可以显著猝灭BSA的内源荧光,其猝灭机制为静态猝灭,猝灭常数Ksv在288 K和303 K时分别为1.45×104和1.42×104L/mol,Stern-Volmer曲线是两段相交于cKT=8.0×10-5mol/L的回归曲线,说明KT与BSA之间存在两类结合位点.数据处理及热力学参数计算表明:低浓度KT-BSA(cKT8.0×10-5mol/L)的结合主要是疏水作用,结合位点数约为1;较高浓度KT(cKT8.0×10-5mol/L)主要以氢键、范德华力与BSA结合,结合位点数为3.7.紫外光谱和圆二色光谱实验结果表明,KT的存在使BSA二级结构发生了改变.     

基于纳米金/氮掺杂石墨烯的电化学适配体传感器检测汞离子的研究

以离子液体修饰碳糊电极(CILE)为工作电极,利用直接滴涂法将氮掺杂石墨烯(NG)固定于CILE表面后,利用恒电位法将纳米金(AuNPs)沉积在电极表面,再通过自组装法将适配体(aptamer)固定在AuNPs/NG/CILE表面制得一种新型电化学适配体传感器(aptamer/AuNPs/NG/CILE)。利用示差脉冲伏安法(DPV)对修饰电极进行表征,建立了汞离子(Hg~(2+))的电化学适配体检测方法,线性范围为1.0×10~(-9)～3.0×10~(-7)mol/L,检测限为3.33×10~(-10)mol/L。     

HPLC determination of ascorbic acid using luminol-Cu (II) chemiluminescence-application to the analysis of Juice beverage

The chemiluminescence (CL) of luminol-Cu (II) was applied to HPLC determination of ascorbic acid, which was separated by a C₁₈ reverse-phase column with a mobile phase of 0.25 mol/L HAc. The eluted ascorbic acid was mixed with 0.3 mmol/L luminol and 0.05 mol/L CuSO₄. The light emission from the reaction of Cu(II) oxidized ascorbic acid and luminol was detected by a modified luminometer. The detection limit was 3.6×10⁻⁶ mol/L for ascorbic acid at aS/N ratio of 3, and the linear calibration range was 2×10⁻⁴–2×10⁻³ mol/L. The relative standard deviation for 5 replicate injections of 1×10⁻³ mol/L ascorbic acid was calculated as 4.3%. The method was successfully applied to determination of ascorbic acid in juice beverage. Foundation item: National Natural Science Foundation of China (29605001) Biography: Wu Feng-wu(1963-), male, research direction: analytical chemistry.     

达旦黄与牛血清白蛋白作用的光谱特性

以达旦黄为探针,应用荧光及紫外光谱法研究达旦黄(TY)与牛血清白蛋白(BSA)分子间的结合反应,测定了不同温度下的结合常数和结合位点数.实验表明:TY对BSA内源荧光的猝灭机理为静态猝灭,作用力类型为疏水作用.根据Frster能量转移理论,求得不同温度(16 ,30 ,40 ℃)下的能量转移效率E分别为0.419 6,0.401 9,0.386 5,作用距离r分别为3.05,3.04,3.10 nm.BSA存在猝灭TY的荧光,以此为基础建立了测定BSA的方法,线性范围:3×10-7～2×10-5 mol/L,检出限:9.07×10-7 mol/L,相对标准偏差:RSD=1.7%.     

Spectrofluorimetric method for the determination of triamcinolone acetonide

0　IntroductionTriamcinoloneAcetonide,9 fluoro 11β,2 1 dihydroxy 16α,17[(1 methylethylidene)bis (oxy) ] pregn 1,4 diene 3,2 0 dione,Mris 4 34.4 8(abr.TA ) .Itbelongstoaclassofadrenalcortexhormonedrug ,whosefunctionsareaffectionofsugarmetabolism ,anti inflammationandresistancehypersusceptibilityetc.TAcanbesuitabletorheumatoidarthritisanddermatosissuchashypersusceptibilityandneuropathicdermatitis .ThefunctionsofTAisstrongerandlongerthantriamcinolone[1 ,2 ] .ThecommonmethodsofdetectingTAm…     

Chemiluminescence determination of thiourea using tris (1,10-phenanthroline)-ruthenium (II) KMnO4 system

The light emission produced by thiourea in oxidation process by permanganate in acidic solution in the presence of Ru(phen) ₂ ^{3 +} is used to determine 1.0×10⁻⁵ −1.0×10⁻⁵ mol/L thiourea. The limit of detection is 9.8×10⁻⁹ mol/L and the relative standard deviation is 1.1% for a 1.0×10⁻⁵ mol/L thiourea solution (n=10). The method was applied satisfactorily to the determination of thiourea. Foundation item, Support by Ministry of Education, Wuhan University and Alumni Association of it Biography: Wu Feng-wu(1963-), Male, Ph. D, research direction: analytical chemistry.     

Simultaneous Fluorescence Detection of Mercury(Ⅱ) and Silver Ions Based on Rhodamine B Isothiocyanate and 5-Carboxyfluorescein-ss DNA Modified Probe

A new fluorescence sensor is developed for simultaneous detection of Hg~(2+) and Ag~+. During the detection process,Hg~(2+) forms complexes with the fluorescent dye rhodamine B isothiocyanate(RBITC) modified onto the surface of gold nanoparticles(Au NPs),resulting in RBITC's displacement from the surface of Au NPs and the recovery of fluorescence. Meanwhile,Ag~+ forms “C-Ag~+-C” complex with C-rich 5-carboxyfluorescein(FAM)-ss DNA modified onto the surface of Au NPs,which keeps the fluorescent dye FAM close to the Au NPs and results in quench of fluorescence. The experimental results show a wide linear range and a good sensitivity. The limit of detection is 1.06 nmol/L for Ag~+ and 0.48 nmol/L for Hg~(2+). This detection method is not only easy to operate but also efficient.     

Characterization of Anabaena cylindrica Solution System Using Synchronous-Scan Fluorescence Spectroscopy

The characterization of the algaeAnabaena cylindrica solution with Fe (III) was investigated using fluorescence emission and synchronous-scan spectroscopy. The ranges of concentrations of algae and Fe (III) in aqueous solutions were 5.0×10⁸ 2.5×10⁸ cell/L and 1060 μmol/L. respectively. The effective characterization method used was synchronous-scan fluorescence spectroscopy (SFS). The wavelength difference (Δλ) of 90 nm, was maintained between excitation wavelength (λen) and emission wavelength (λen). The peak was observed at about (λex) (λem) 326 nm for synchronous scan fluorescence spectroscopy. The fluorescence quenching in system of algae Fe(III)-HA was studied using synchronous-scan spectroscopy for the first time, Fe(III) was clearly the effective quencher. The relationship betweenI I (quenching efficiency) andc (concentration of Fe (III) added) was, a linear correlation for the algae solution with Fe(III). Also, Aldrich humie acid (HA) was found to be an effective quencher. Foundation item: Supported by the National Natural Science Foundation of China (20177017) and the Scientific Research Foundation of Wuhan Environmental Protection Bureau Biography: LIU Xian li(1965), male. Ph.D. Associate professor, research direction: environmental chemistry.     

Synthesis and optical properties of nanosized CdS prepared in a quaternary CTAB/ nhexanol/n-heptane/water reverse micelle

Quaternary water-in-oil reverse micelles consisting of cetyltrimethylammonium bromide (CTAB), nhexanol, n-heptane and water were prepared and characterized. The optimized reaction conditions were determined, and monodispersed droplets of the reverse micelles were used as microreactors to synthesize CdS nanoparticles. By using transmission electron microscopy (TEM), UV-Vis spectroscopy and fluorescence spectroscopy, the influences of the reverse micelle components on the size, size distribution, morphology, stability and optical properties of CdS nanoparticles were investigated. CdS nanoparticles with narrow size distribution were obtained and the size range is 6–8 nm whenW=24 (W=[water]/[CTAB]), P=5.27 (P=[n-hexanol]/ [CTAB]), [CTAB]=0.2 mol/L, [Cd²⁺] and [S^2-] are 8.45×10⁻⁴ mol/L.     

Electrochemical Behavior and Determination of Trifluoperazine at Decanethiol Self-Assembled Monolayer Modified Gold Electrodes

0　IntroductionTrifluoperazine is a derivative of phenothiazine. It hasneuroleptic and antidepressive actions, hence has beenwidely used in the treatment of psychotic patients[1]. As it hassuch function and application, trifluoperazine’s characteristicsand detection methods were studied by means of spectropho tometry[2], capillary zone electrophoresis[3], titrimetry[4],fluorometry[5], high performance liquid chromatographyetc[6]. Because of the electroactivity of trifluoperaz…     

Preparation and application of electrochemical barbital sensor based on molecularly imprinting technique

A molecularly imprinted electrochemical sensor was prepared based on poly folic acid(PFA) for rapid detection of barbital(BAR). The PFA membrane was obtained via directly electropolymerization technique on the surface of chemically modified Au electrode(Au/CME) by means of cyclic voltammetry(CV) in the potential range between-0.4 and 1.0 V in phosphate buffer solution(PBS) pH 7.04. The molecularly imprinted polymers(MIP) membrane was synthesized with BAR as template molecules and folic acid(FA) as the functional monomer. The performance and surface feature of the proposed imprinted sensor were investigated using CV, differential pulse voltammetry(DPV), electrochemical impedance spectroscopy(EIS) and scanning electron microscope(SEM). Under the optimized conditions, the peak current decrease(ΔI_p) was proportional to the BAR concentration in the range of 1.00×10~(–7)-1.00×10~(–4) mol/L(R~2=0.998 2) with a detection limit(S/N=3) of 4.65×10~(–8) mol/L. The results indicated that the imprinted sensor exhibited an excellent selectivity for BAR and it was successfully used to determine BAR in real samples with recoveries of 94.7%-106.2% by using the standard addition method.     

Electrocatalytic oxidation of H<Subscript>2</Subscript>O<Subscript>2</Subscript> at a carbon paste electrode modified with a nickel (II)-5, 11, 17, 23-tetra-tert-butyl-25, 27-bis(Diethylcarbamoylmethoxy) calix[4] arene complex and its application

Electrochemical behavior of a carbon paste electrode (CPE) modified with nickel(II)-5, 11, 17, 23-tetra-tert-butyl-25, 27-bis(diethylcarbamoylmethoxy) calix[4]arene (Ni (II)-L) complex and its electrocatalytic activity towards the oxidation of hydrogen peroxide were investigated by cyclic voltammetric technique in a 5.0×10⁻² mol/L NaClO₄+1.0×10⁻³ mol/L NaOH solution. It was found that Ni(II)-L acts as an effective catalyst for the oxidation of hydrogen peroxide. The modified electrode exhibited a linear response over a hydrogen peroxide concentrations in the range of 2.0×10⁻⁵−1.0×10⁻⁴ mol/L with a detection limit as low as 1.0×10⁻⁶ mol/L. The relative standard deviation was 3.5% for 5 successive determinations of H₂O₂ at 1.0×10⁻⁵ mol/L. The modified electrode was used successfully in rainwater analysis. Foundation item: Supported by the Natural Science Foundation of Hubei Province (98J040). Biography: Li Chun ya(1972-), Ph. D. candidate, research direction: electroanalysis and electrosynthesis.     

Fluorescence Determination of Artemisinin Using Hemoglobin as Catalyst and Pyronine B as Substrate

0 IntroductionMaalnadria siusb atr ompajicosr .he aAltrthe pmrisoibnlienmi (n qtihneghtraoopsiucs,QHS,Fig.1) is a sesquiterpene endoperoxide isola-ted fromArtemisia annuaL., an ancient Chineseherbal medicine usedfor treatment of fever and ma-laria.Studies of the structure and activity relation-ship have shownthat endoperoxide groupis essentialfor anti malarial activity of QHS and absence of thismoiety lead to completely loss in activity of thedrug. Many techniques have been developed to de…     

Study on state of terbium ion in liposome by one-order derivative fluorescence quenching method

The state of Tb³⁺ is investigated in liposome. When the concentration of PC is below CMC (critical micell concentration), most of Tb³⁺ is associated with PC, the binding constant is about 3.35×10³ L/mol. When the concentration of PC is beyond CMC, most of Tb³⁺ is dimerized, the dimerization constant is about 3.92×10⁴L/mol. In PC−CH−H₂O system, the binding constant of Tb³⁺−CH complex 2.93×10⁴L/mol is obtained. Biography:Mu Xiao-jing (1974-), female, MS.     

Study of the voltammetric behavior of heme and its direct analysis application

The electroanalytical method of ferriheme was studied by linear sweep voltammetry in medium of 0.05 mol/L Tris+0.05 mol/L NH₃−NH₄Cl buffer at hang mercury drop electrodes (HMDE). Heme exhibits two pair reversible redox peaks and one irreversible peak. The cathodic peak potentials are−;0.236 V, −0.422 V and −1.408 V respectively. The first and the third peaks can be used for directly quantitative determination of heme concentrations. The peak currents are good linear relationship with heme concentration in ranges of 3×10⁻⁶–6×10⁻⁵ mol/L and 3×10⁻⁷–1.5×10⁻⁵ mol/L respectively. Supported by the National Natural Science Foundation of China Lju Huihong: born in 1965, Lecturer. Visiting scholar from Xiangyang Teacher’s College, Hubei, 441053     

抗生素亚胺培南探针分子设计及传感性能研究

抗生素亚胺培南（imipenem,IPM）用药治疗败血症患者感染需要快速做出反应,目前的血药监测方法严重延迟药物注射。设计金属元素掺杂型石墨烯量子点（graphene quantum dots,GQDs）,可实现荧光法快速测定IPM和开辟荧光法检测抗生素的新途径。采用水热法制备了铁掺杂GQDs （Fe-GQDs）,用于快速探测IPM。采用透射电子显微镜（transmission electron microscopy,TEM）、X射线光电子能谱（X-ray photoelectron spectroscopy,XPS）以及荧光光谱等方法,探讨不同铁源起始剂对GQDs荧光性能及传感性能的影响,并分析了乙酸铁为铁源制备的Fe-GQDs的微观结构及荧光性能。结果表明：以乙酸铁为起始剂制备的Fe-GQDs荧光性能最佳,且对IPM具有显著的荧光淬灭效应。所制备的Fe-GQDs荧光淬灭强度（F/F₀）与IPM浓度（concentration,C）呈线性关系,线性方程为${F/}{{F}}_{\text{0}}\text{= 0.983}-\text{4.23×}{\text{10}}^{-3}\text{}$C,线性相关系数（R²）为 0.997,线性范围为0.007～0.073 g/L。Fe-GQDs探针分子对血浆中常见有机分子和金属离子具有良好的抗干扰性,检测IPM误差为1.6%～4.6%。     

Chemiluminescence determination of tetracycline and oxytetracycline in pharmaceutical preparations using Ru (bipy)3 2+-cerium (IV) system

A new chemiluminescence (CL) method for the determination of tetracycline and oxytetracycline is developed, based on the CL reaction of tetracycline and oxytetracycline with Ru (bipy)₃ ²⁺ and Ce (IV). In sulfuric acid medium, the CL emission is generated upon continuous oxidtion of Ru(bipy)₃ ²⁺ by cerium (IV). The emission intensity is greatly enhanced when tetracycline and oxytetracycline are introduced into the reaction system after acid degradation. Under the optimum conditions, the calibration curves are linear over the range of 8.0×10⁻⁸∼4.0×10⁻⁶ mol/L for tetracycline and of 2.0×10⁻⁷∼4.0×10⁻⁵ mol/L for oxytetracycline, with the detection limits are 4.2×10⁻⁸ mol/L for tetracycline and 1.5×10⁻⁷ mol/L for oxytetracycline, respectively. The proposed method was used for the determination of tetracycline and oxytetracycline in pharmaceutical formulations with good results. Foundation item: Supported by the National Natural Science Foundation of China and the Natural Science Foundation of Hubei Province. Biography: HAH He-you (1962), male, Associate profeddor, Ph.D graduate candidate. Present address, Department of Chemistry, Huainan Teacher's College, Huainan.     

铂微粒修饰固体石蜡碳糊电极对过氧化氢的电催化特征及分析应用

研究铂微粒修饰的固体石蜡碳糊电极(Pt-SCPE)对H2O2的电催化行为。在pH值4.6的柠檬酸盐-0.03 mol/L硝酸钾溶液中,用该电极H2O2在+0.18V(vs．SCE)可产生灵敏的还原电流,线性范围为1.0×10-1 mol/L～3.0×10-7 mol/L,检出限为7.5×10-8 mol/L。Pt-SCPE与液体石蜡碳糊电极比较,在峰电位、线性响应范围、检出限方面有更好的结果。用该电极测定样品中的过氧化氢,获得满意结果。     

Nanostructured multilayer thin films of multiwalled carbon nanotubes/gold nanoparticles/glutathione for the electrochemical detection of dopamine

In the present study, multiwalled carbon nanotubes (MWCNTs), gold nanoparticles (AuNPs), and glutathione (GSH) were used to fabricate multilayer nanoscale thin films. The composite thin films were fabricated by layer-by-layer technique as the films were constructed by the alternate deposition of cationic and anionic polyelectrolytes. The MWCNTs were modified via a noncovalent surface modification method using poly(diallydimethylammonium chloride) to form a cationic polyelectrolyte. An anionic polyelectrolyte was prepared by the chemical reduction of HAuCl4 using sodium citrate as both the stabilizing and reducing agent to form anionic AuNPs. GSH was used as an electrocatalyst toward the electro-oxidation of dopamine. The constructed composite electrode exhibits excellent electrocatalytic activity toward dopamine with a short response time and a wide linear range from 1 to 100 μmol/L. The limits of detection and quantitation of dopamine are (0.316±0.081) μmol/L and (1.054±0.081) μmol/L, respectively. The method is satisfactorily applied for the determination of dopamine in plasma and urine samples to obtain the recovery in the range from 97.90% to 105.00%.