Voltametric and Flow Injection Determination of Oxytetracycline Residues in Food Samples Using Carbon Fiber Microelectrodes

A voltammetric method for the determination of the antibiotic oxytetracycline (OTC) in food samples is reported. Carbon fiber microelectrodes (CFMEs), which allow voltammetric measurements to be performed in a small volume (1 mL) of the analyte extract from the samples, are employed. Repeatable electroanalytical responses were obtained with no need of applying cleaning treatments to the CFME. Under the optimized square‐wave conditions, a linear calibration plot for OTC was obtained in the 1.0×10^?6–1.0×10^?4 mol L^?1 range, with a detection limit of 2.9×10^?7 mol L^?1 (150 ng mL^?1) OTC. The determination of OTC by a flow‐injection method with amperometric detection using a homemade flow cell specially designed to work with CFMEs, was also evaluated using pure acetonitrile as the carrier. The SW voltammetric method was applied to the determination of OTC in spiked milk and eggs samples, at 100 ng mL^?1 and 200 ng g^?1 levels, respectively. The procedure involved the extraction of the analyte in ethyl acetate, evaporation of the solvent and reconstitution of the residue in acetonitrile ?5.0×10^?4 mol L^?1 tetrabutylammonium perchlorate medium. Recoveries of 96±8 and 91±8% were obtained for milk and eggs, respectively, by applying the standard additions method.     

Status and dreams of photonics polymer for IT

We have proposed a low-loss, high-bandwidth and large-core graded-index plastic optical fiber (GI POF) in data-corn, area. The GI POF enables us to eliminate the “modal noise” problem which is observed in medium-core silica fibers. Therefore, stable high-speed data transmission can be realized by the GI POF rather than medium-core silica fibers. Furthermore, advent of perfluorinated (PF) polymer based GI POF network can support higher transmission than silica fibers network because of the small material dispersion of PF polymer compared with silica. In addition, we proposed a “highly scattering optical transmission (HSOT) polymer” and applied it to a light guide plate of a liquid crystal display backlight. The HSOT polymer backlight that was designed using the HSOT designing simulator demonstrated twice the brightness of the conventional taransparent backlight with sufficient color uniformity. Furthermore, we proposed the two types of zero-birefringence polymers synthesized by the random copolymerization method and the anisotropic molecule dopant method. Both of the polymers exhibited no orientational birefringence for any orientation of polymer chains.     

Divergent effects of static disorder and hole doping in geometrically frustrated β-CaCr2O4

The gallium substituted and calcium deficient variants of geometrically frustrated β-CaCr₂O₄, β-CaCr_2-2xGa_2xO₄ (0.02≤x≤0.25) and β-Ca_1−yCr₂O₄ (0.075≤y≤0.15), have been investigated by X-ray powder diffraction, magnetization and specific heat measurements. This allows for a direct comparison of the effects, in a geometrically frustrated magnet, of the static disorder that arises from non-magnetic substitution and the dynamic disorder that arises from hole doping. In both cases, disturbing the Cr³⁺ lattice results in a reduction in the degree of magnetic frustration. On substitution of Ga, which introduces disorder without creating holes, a gradual release of spins from ordered antiferromagnetic states is observed. In contrast, in the calcium-deficient compounds the introduction of holes induces static ferrimagnetic ordering and much stronger perturbations of the β-CaCr₂O₄ host.     

Pesticides in water and the performance of the liquid-phase microextraction based techniques. A review

The control of pesticides in surface, drinking and groundwater is nowadays a real necessity. In the European Community, their concentration must comply with the established parametric and environmental quality standards (EQSs). Regarding the new legislation, this article updates the information concerning the monitoring of pesticides and the technical specifications for their measurement in water samples where ultra-sensitive analytical methods are required. For some compounds, like pesticides, there is still a need to improve the performance of the existing methods. High sensitive techniques like gas chromatography tandem mass spectrometry (GC–MS/MS) and liquid chromatography coupled with mass spectrometry (LC–MS) have been developed. However, for most of the substances present at trace and ultra-trace levels the extraction and preconcentration steps are so far essential for their detection. Advances at a micro scale have been made and different types of microextractions are being developed. Liquid-phase microextraction (LPME) is an example. The study of this technique has increased in the last years and some innovations have been recently reported for pesticides water analysis. This article reviews the new developed LPME-based techniques and compares its performance with the analytical specifications established for pesticides water monitoring. The results show that LPME-based techniques can be a promising tool to improve the nowadays performance of methods used in pesticides water control.     

Dopamine and Glucose Sensors Based on Glassy Carbon Electrodes Modified with Melanic Polymers

This work deals with the study of polymers electrogenerated from different catechols at glassy carbon electrodes and the analytical applications of the resulting modified electrodes for dopamine quantification and glucose biosensing. The electropolymerization was performed from a 3.0×10^?3 M catechol solution (catechol, dopamine, norepinephrine, epinephrine or L ‐dopa in a 0.050 M phosphate buffer pH 7.40) by applying 1.00 V for 60 min. The properties of the polymers are very dependent on the nature of the catechol, L ‐dopa being the best. Glassy carbon electrodes modified with melanic polymers electrogenerated from L ‐dopa and norepinephrine were found to be suitable for dopamine determinations in flow systems, although the behavior was highly dependent on the nature of the monomer. Detection limits of 5.0 nM dopamine and interferences of 9.0 and 2.6% for 5.0×10^?4 M ascorbic acid and 5.0×10^?5 M dopac, respectively, were obtained at the glassy carbon electrode modified with a melanin‐type polymer generated from L ‐dopa (using 1.0×10^?3 M AA in the measurement solution). The advantages of using a melanin‐type polymer generated from dopamine to improve the selectivity of glucose biosensors based on carbon paste electrodes containing Pt and glucose oxidase (GOx) are also discussed. The resulting bioelectrodes combines the high sensitivity of metallized electrodes with the selectivity given by the polymeric layer. They exhibit excellent performance for glucose with a rapid response (around 10 seconds per sample), a wide linear range (up to 2.5×10^?2 M glucose), low detection limits (143 μM) and a highly reproducible response (R.S.D of 4.9%). The bioelectrodes are highly stable and almost free from the interference of large excess of easily oxidizable compounds found in biological fluids, such as ascorbic acid (AA), uric acid (UA) and acetaminophen.     

Crystal, molecular and electronic structure of N,N'-diphenyl-N,N'-bis(2,4-dimethylphenyl)-(1,1'-biphenyl)-4,4'-diamine and the corresponding radical cation

Oxidation of N,N'-diphenyl-N,N'-bis(3-methylphenyl)-(1,1'-biphenyl)-4,4'-diamine (TPD, 1 a) and N,N'-diphenyl-N,N'-bis(2,4-dimethylphenyl)-(1,1'-biphenyl)-4,4'-diamine (1 b) with SbCl(5) affords the corresponding radical cations quantitatively. The crystal and molecular structure of 1 b and [1 b]SbCl(6), the first tetraphenyl benzidene derivatives to be characterised crystallographically in both the neutral and radical cation states, reveal molecular parameters in agreement with the predictions made on the basis of DFT studies. Analysis of the NIR transition in the radical cations [1](+) (.) allows an estimate of the electronic coupling parameter V (1 a(+) (.) 3200 cm(-1); 1 b(+) (.) 3300 cm(-1)), the reorganisation energy lambda(1 a(+) (.) 7500 cm(-1); 1 b(+) (.) 7800 cm(-1)), and the linear coupling constant l (1 a(+) (.) 3100 cm(-1); 1 b(+) (.) 2700 cm(-1)) of the symmetric mode.     

停流流动注射在线沉淀-原子吸收法测定盐酸苯海拉明

本文建立了一种简单快速的检测药剂中盐酸苯海拉明含量的停流流动注射在线沉淀 间接原子吸收法。该方法是基于盐酸苯海拉明与BiI-4在线定量连续生成离子对缔合物沉淀(摩尔比为1∶1),经停流过滤稀释后,以AAS法测定滤液中铋的含量来间接测定盐酸苯海拉明的量。本法的相对平均偏差小于3.5%,线性范围为2.5～40μg·mL-1,采样频率60h-1,回收率为98%～103%。     

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     

顺序注射催化动力学光度法测定织物和室内空气中痕量甲醛

在磷酸介质中 ,甲醛可以催化溴酸钾氧化　花青的反应使其退色 ,据此建立了顺序注射催化动力学光度法测定织物和室内空气中痕量甲醛的新方法。方法的线性范围 0 .5～ 7.0 μg mL ,检出限 0 .1 μg mL。用于树脂整理特殊织物和室内空气中痕量甲醛的测定 ,回收率在 97.0 %～ 1 0 5 .0 %之间。     

微波溶样流动注射分光光度法在线测定金矿石中的金

采用微波溶样 流动注射在线泡塑富集分离 分光光度联用技术建立了在线快速测定金矿石中金的方法。比较了微波溶样法与传统电热板溶样法,二者结果基本一致。前者溶样时间近似为后者的1 9。确定了两条工作曲线:校正曲线范围为0 1～1.0μg mL,检出限2.2×10-2μg mL;校正曲线范围为1.0～9 0μg mL,检出限1.6×10-1μg mL。FI SP系统分散系数为3.78。对管理样GBW(E) 070014平行11次测定,其RSD为1.3%,对所得结果进行t检验,置信度95%时,无系统误差存在。