Linear Scan Stripping Voltammetry at Glassy-Carbon Based Thin Mercury Film Electrodes for Determination of Trace Aluminium in Dialysis Fluids.

Abstract

Linear scan cathodic stripping voltammetry at glassy-carbon based thin mercury film electrodes is a simple and inexpensive alternative for determining trace Al(III) in dialysis fluids.

The efficiency of a variety of ligands (SVRS, Cupferron and Blue Black Eriochrome R) was evaluated comparing their voltamperometric response by application of a linear scan mode, after preconcentration into the mercury film electrode as Al(III) complexes.

The best results were obtained when Cupferron was used as ligand, since its stripping current compares favourably in terms of sensitivity and resolution. The sharply defined cathodic peak at -1.3 V, corresponding to the reduction of the interfacial accumulated complex, could be used for quantitation. The response is linear up to 50 μg/l; correlation coefficient, 0.995. The relative standard deviation (at 20 μg/l level) is 3.5%, a detection limit of 0.5μg/l was estimated from the signal to noise characteristics of the response for 5 μg/l, which compares favourably among the reported electroanalytical methods for aluminium.

We calibrated the method under conditions of use estimating the trace aluminium exposure in patients undergoing dialytic treatment.     

The Analysis of Sulphonamide Drug Residues in Pork Muscle using Automated Dialysis

ABSTRACT

The aim of this study was to assess the suitability of automated dialysis, using a commercial system, for the analysis of sulphonamides in porcine tissue. The system involves automated dialysis, followed by trace enrichment of the dialysate prior to HPLC determination. The procedure was applied to the analysis of nine sulphonamide drug residues using reversed phase HPLC as the method of determination. Muscle samples were blended in saline, centrifuged and the supernatant was filtered before dialysis for an optimised time of 11 min. The resulting dialysate was concentrated on a reversed phase trace enrichment cartridge prior to HPLC analysis with UV detection at 280 nm. The developed method was evaluated by carrying out intra- and inter-assays on fortified porcine muscle. Mean recoveries, evaluated from the inter-assay study, were 80% or higher for the nine sulphonamides studied and the limit of determination for the method was 40 ng g^?1.     

尿素诱导牛血红蛋白变性的微量热和平衡渗析研究

应用恒温微量热技术和平衡渗析技术,对尿素与牛血红蛋白在30℃水溶液中的结合作用及造成牛血红蛋白变性的过程进行了研究,得到了尿素在牛血红蛋白上的平均结合数、二者之间的结合焓及每摩尔尿素与牛血红蛋白结合的焓效应,并根据简单结合模型,计算了它们之间的结合常数、结合自由能.对实验结果的热力学分析表明,尿素是通过直接和间接的两种作用造成牛血红蛋白变性的,它们之间的相互作用分为三个阶段:尿素浓度达到4molL-1之前为第一阶段,主要产生的是尿素与牛血红蛋白的直接结合作用,在弱酸性条件下这种作用较强;尿素浓度为4molL-1到6molL-1之间为第二阶段,主要通过尿素与溶剂水的作用造成牛血红蛋白周围水结构的变化,在尿素浓度达到6molL-1时两种作用的叠加造成牛血红蛋白结构的破坏,暴露出原来处于结构内部的基团;尿素浓度超过6molL-1之后为第三阶段,尿素分子继续与暴露出来的基团进行结合.牛血红蛋白次级结构的维系具有协作性,其结构的破坏不是渐进的,而是一次性全部打开,结构破坏产生的热效应并不太大.     

Charge‐mosaic membrane prepared from microspheres

A new type of charge‐mosaic membrane was prepared from poly(4‐vinyl pyridine) microspheres 250–350 nm in diameter as an anion‐exchange element and from linear poly(sodium styrene sulfonic acid) as a cation‐exchange element. The mosaic structure on the surface of the membrane and the continuous connection of the microspheres in the membrane were confirmed by scanning electron microscopy observations and the electrical conductivity of the membrane. The microspheres were continuously connected from one side to the other side of the membrane surface when the weight fraction of the microspheres increased more than 20–25 wt % in the membrane. The flux of KCl, the permeability coefficient of KCl, the volume flux, and the selectivity dialysis separation of the electrolyte (KCl) and nonelectrolyte (glucose and saccharose) of the membrane indicated that it had the characteristic properties of a charge‐mosaic membrane. Ion‐exchange membranes composed of each raw material of the charge‐mosaic membrane did not show these properties. © 2003 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 41: 1251–1261, 2003     

在线透析-流动注射光度法测定奶及奶制品中尿素含量

建立了在线透析-流动注射光度法测定奶及奶制品中尿素的方法.加人三氯乙酸使样品中蛋白质沉淀,离心过滤去除沉淀的蛋白质,在线透析去除剩余的脂肪及大分子,避免干扰光度分析.在Fe3+存在时,尿素与二乙酰一肟在酸性溶液中水解生成的二乙酰反应生成红色化合物,在534 nm处测量吸光度,加入硫代氨基脲提高显色强度.实验对试剂的浓度...     

Simultaneous determination of some food additives in soft drinks and other liquid foods by flow injection on-line dialysis coupled to high performance liquid chromatography

Flow injection on-line dialysis was developed for sample pretreatment prior to the simultaneous determination of some food additives by high performance liquid chromatography (FID-HPLC). A liquid sample or mixed standard solution (900 μL) was injected into a donor stream (5%, w/v, sucrose) of FID system and was pushed further through a dialysis cell, while an acceptor solution (0.025 mol L⁻¹ phosphate buffer, pH 3.75) was held in the opposite side of the dialysis membrane. The dialysate was then flowed to an injection loop of the HPLC valve, where it was further injected into the HPLC system and analyzed under isocratic reverse-phase HPLC conditions and UV detection (230 nm). The order of elution of five food additives was acesulfame-K, saccharin, caffeine, benzoic acid and sorbic acid, respectively, with the analysis time of 14 min. On-line dialysis and HPLC analysis could be performed in parallel, providing sample throughput of 4.3 h⁻¹. Dialysis efficiencies of five food additives were in ranges of 5-11%. Linear calibration graphs were in ranges of 10-100 mg L⁻¹ for acesulfame-K and saccharin, 10-250 mg L⁻¹ for benzoic acid and 10-500 mg L⁻¹ for caffeine and sorbic acid. Good precisions (RSD < 5%) for all the additives were obtained. The proposed system was applied to soft drink and other liquid food samples. Acceptable percentage recoveries could be obtained by appropriate dilution of the sample before injecting into the system. The developed system has advantages of high degrees of automation for sample pretreatment, i.e., on-line sample separation and dilution and low consumption of chemicals and materials.     

Comparative Study of The Yield and Physicochemical Properties of Collagen from Sea Cucumber (Holothuria scabra), Obtained through Dialysis and the Ultrafiltration Membrane

Collagen was extracted from the body wall of sea cucumber (Holothuria scabra) using the pepsin-solubilized collagen method followed by isolation using dialysis and the ultrafiltration membrane. The yield and physicochemical properties of the collagen obtained from both isolation methods, denoted as D-PSC and UF-PSC, were compared. The ultrafiltration method affords a higher yield of collagen (11.39%) than that of the dialysis (5.15%). The isolated collagens have almost the same amino acid composition, while their functional groups, referred to as amide A, B, I, II, and III bands, were in accordance with commercial collagen, as verified by Fourier Transform Infrared (FT-IR) spectroscopy. The UV-Vis absorption peaks at 240 nm and 220 nm, respectively, indicated that the collagens produced are type-I collagen. The D-PSC showed interconnecting sheet-like fibrils, while the UF-PSC exhibited a flaky structure with flat-sheets arranged very close to each other. The higher yield and comparable physicochemical properties of the collagen obtained by ultrafiltration as compared with dialysis indicate that the membrane process has high potential to be used in large-scale collagen production for food and pharmaceutical applications.     

Separation of copper and bichromate ions by complex methods

Separation of Cu²⁺ and Cr₂O₇ ^2– has been studied by electrodialysis combined with preliminary adsorption on bentonite. The influence of concentration, pH, and electric current on the degree of desalination has been studied. The optimum conditions for almost complete separation of the ions studied have been found. Real galvanic sewage has been examined by this method.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 7, pp. 1191–1193, July, 1994.     

Er -Li ion exchange in lithium niobate crystals: an EXAFS study

Lithium niobate crystals doped with erbium by the ion exchange process were studied by means of extended X-ray absorption fine structure spectroscopy and secondary ion mass spectrometry. The study of the local atomic order allowed the determination of the erbium environment in the crystal matrix and the investigation on the role of preparation conditions. Received 21 November 2002 Published online 1st April 2003 RID="a" ID="a"e-mail: sada@padova.infm.it     

Determination of chromium(VI) in dialysis fluids by alternating current and differential pulse voltammetry

Alternating current (ACV) and differential pulse voltammetry (DPV) are employed for the determination of Cr(VI) in dialysis fluids, using 0.1 mol/1 dibasic ammonium citrate as supporting electrolyte (pH 5.9). A three-electrode cell was used: The working electrode was a long-lasting sessile-drop mercury electrode (LLSDME) with a drop time of 240 to 300 s. Precision, expressed as relative standard deviation (s _r%), and accuracy, expressed as relative recovery (R%) are also reported.