流动注射-阻尼最小二乘法用于多组分分析

研究了用流动注射分析进行阻尼最小二乘分光光度法同时测定锌、铜和钴的新方法。方法基于阻尼最小二乘法改进CPA法,将阻尼因子和非零截距引入CPA法,降低了P系数矩阵的病态程度和改善了校正模型的预报能力,使结果更加准确,已将方法成功用于锌铜钴混合体系的分析。     

An inter-company cross-validation exercise on capillary electrophoresis testing of dose uniformity of paracetamol content in formulations

Summary Successful transfer of an MECC method for the determination of paracetamol between 7 companies is shown. The method was applied to the quantitative determination of paracetamol levels in capsules. The results obtained agreed well between companies and with both HPLC data and the label claim. Acceptable method performance in terms of relative migration time precision and response factor precision was reported by each company.     

Indirect Spectrophotometric Determination of Fluoride In Water With Zirconium-Spadns By Flow Injection Analysis

Abstract

The zirconium-SPADNS method for the determination of fluoride based on the effect of fluoride ion on the color system (Zr-SPADNS), has been adapted to the continuous flow spectrophotometry. A manifold consisting of two lines was used. the decrease in the absorbance of Zr-SPADNS reagent at 590 nm is linear with fluoride concentration in the range 0.00-3.5 ppm. the method has a detection limit of 0.02 ppm fluoride. At a sampling rate of 50 determinations per hour, the precision was about 1% relative standard deviation. the method is applied to the determination of fluoride in natural water samples. the good agreement between the results obtained by this method and those obtained by a potentiometric method using a fluoride ion-selective electrode, show that the new method is potentially suitable for routine analysis. the effects of reaction conditions, flow parameters, and interferences on the FIA-spectrophotometric signals are reported. amount of interfering ion is present in quantity great enough to produce an error of 0.1 ppm or more, the sample must be distilled¹⁷     

Determination of Coumarin in Vanilla Flavorings by Quantitative High Performance Thin Layer Chromatography

Abstract

High performance silica gel TLC was used to qualitatively and quantitatively determine coumarin in real and artificial vanilla flavorings. Coumarin was detected as a fluorescent or colored zone and quantified by scanning with a densitometer. Recoveries and reproducibility values are reported for fortified samples. The method was applied to a qualitative survey of domestic vanilla samples and quantification of coumarin in an adulterated foreign sample. The result of this determination was verified by standard addition analysis. The method was also applied to the determination of coumarin in a spiked wine sample.     

还原剂与鲁米诺化学发光反应的研究(Ⅱ)——钒(Ⅱ)-鲁米诺化学发光反应

Fe(Ⅱ)和Ti(Ⅲ)与鲁米诺的化学发光反应已有报道,我们发现,Cr(Ⅱ)、Mo(Ⅲ)、W(Ⅲ)、U(Ⅲ)、CN^-、SO₃^2-、抗坏血酸等一大类还原剂均可与鲁米诺溶液作用产生化学发光,本文利用Jones还原柱产生V(Ⅱ),首次研究了V(Ⅱ)与鲁米诺的化学发光反应,在此基础上建立了钒的流动注射化学发光分析法,方法的检出限是8×10^-11g/mL钒,线性范围是4×10^-10～1×10^-5g/mL钒。测定的相对标准偏差小于2％,考察了20余种常见离子对测定的干扰情况,方法已用于水样中痕量钒的测定,初步探讨了发光反应的机理。     

Liquid chromatographic determination of trimethylamine in water

A method for the selective determination of trimethylamine (TMA) in aqueous matrices by liquid chromatography is reported. The proposed procedure is based on the derivatization of the analyte with 9-fluorenylmethyl chloroformate (FMOC) in a precolumn (Hypersil C18, 30 microm, 20 mm x 2.1 mm i.d.) connected on-line to the analytical column (LiChrosphere 100 RP18, 5 microm, 125 mm x 4 mm i.d.). Gradient elution was performed with a mixture of acetonitrile-water-0.05 M borate buffer (pH 9.0). The method has been applied to the direct determination of TMA in water within the 0.25-10.0 microg/ml concentration interval, and can also be adapted to the determination of TMA over the range 0.05-1.0 microg/ml by incorporating a preconcentration stage with C18 solid-phase extraction (SPE) cartridges. Good linearity, reproducibility and accuracy was achieved within the tested concentration intervals. The limits of detection at 262 nm were 50 and 5 ng/ml for the direct method and for the method involving preconcentration, respectively. The proposed conditions allowed the selective determination of TMA in the presence of other primary and secondary short-chain aliphatic amines. The utility of the described procedure has been tested by determining TMA in different water samples.     

小示波图及其应用

提出了小示波图的概念, 建立了基于小示波图的示波计时电位法. 在以汞电极为工作电极的示波计时电位法中, 采用端点去极剂切割经典示波计时电位图后形成的小示波计时电位图(简称为小示波图). 根据切割经典示波图所用的端点试剂不同, 将小示波图分为三种类型. 推导了小示波图的理论公式, 提出了小示波图的调节方法, 并将其用于几种物质的定量测定. 研究表明, 利用小示波图不仅能使在经典示波图端点附近不易准确测定的物质得以测定, 还可以在宽广的电位窗口内灵活、稳定、灵敏、高选择性地进行示波测定. 因此, 小示波图示波测定法是对经典示波测定法的一个重要的补充和发展.     

Direct elemental analysis of cancer cell lines by total reflection X-ray fluorescence

The elemental content of Cu, Fe and Zn in two human adenocarcinoma cell lines was investigated by total reflection X-ray fluorescence (TXRF) spectrometry. Cancer cells were sedimented directly to the quartz plates using a modified cytospin slide holder setup. Special glass stands and caps were also constructed to hold the quartz plates with the cells during the vapour-phase microwave assisted digestion. The method was validated by analysis of certified reference materials. The signal-to-noise ratio was optimized by washing the cells with different solutions. The technique was applied to the determination of Cu, Fe and Zn content of HT-29 and HCA-7 colorectal adenocarcinoma cell lines. Dry mass of the centrifuged cells were determined and the elemental analysis data reported for the two cell lines were referred either to cell numbers, to the total protein content or to the dry mass.     

Simultaneous Voltammetric Determination of Three Herbicides in Food and Water Samples with the Aid of Chemometrics

Differential pulse stripping voltammetry method(DPSV) was applied to the determination of three herbicides,ametryn,cyanatryn,and dimethametryn.It was found that their voltammograms overlapped strongly,and it is difficult to determine these compounds individually from their mixtures.With the aid of chemometrics,classical least squares(CLS),principal component regression(PCR) and partial least squares(PLS),voltammogram resolution and quantitative analysis of the synthetic mixtures of the three compounds were successfully performed.The proposed method was also applied to the analysis of some real samples with satisfactory results.     

流动注射分析光泽精-H2O2-Pb(Ⅱ)化学发光体系测定痕量铅的研究

检测铅离子常用的方法有AAS法和双硫腙比色法,前者直接测定工业废水中的铅,灵敏度不高;后者操作步骤繁琐,须使用剧毒试剂氰化钾,污染环境,用流动注射化学发光法测定铅,仪器简单、操作简便、试样消耗量少、精密度高、分析快速准确、自动化程度高。     

Determination of Silicate By Nonsuppressed Ion Chromatography

Abstract

In previous papers the authors reported that nonsuppressed ion chromatography using potassium hydroxide solution as an eluent was a very sensitive and effective method for the analysis of anions and that this method could be applied to the determination of anions in environmental water samples.

In this paper, this method was applied to the determination of silicate without the interference of fluoride ion when using 0.5mM potassium hydroxide solution, Moreover, this method was compared with silicomolybdate methods and good agreement was obtained between these two methods.

The percent standard deviation was 5.5% when determining lppm of silicate and the calibration curve was linear at concentrations less than 2.5ppm. The detection limit was less than 50ppb.     

因子分析在速差动力学分析中的应用──肾上腺素和去甲基肾上腺素的同时测定

将一种改进的目标因子分析法(MTFA)用于复杂反应的速差动力学分析体系,采用此法处理实验数据时,引入了一个非零截距因子,采用模拟纯谱运算。可使方法的准确度大大提高。据此建立了一种停流技术进样、速差动力学分析同时测定、因子分析处理实验数据的新方法;对于10^-6mol·L^-1级的肾上腺素-去甲基肾上腺素混合物,比例范围在1:5～5:1之间,测定相对误差小于±10%,用于合成样品中肾上腺素和去甲基肾上腺素的同时测定,获得了满意结果。     

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.     

光化学反应在流动注射分析中的应用研究 Ⅳ.亚甲基蓝光化学反应体系测定抗坏血酸

基于抗坏血酸光化学还原亚甲基蓝光化学反应,建立了流动注射光化学反应测定抗坏血酸的新方法。方法线性范围为0.12～5.60μg/ml,进样频率为55～60次/h。应用于医用维生素C片剂中抗坏血酸的测定,结果满意。     

化学计量学在锕系元素分析中的应用

锕系元素的化学性质相似,各元素的分离和分析都很困难,用传统的数据解析手段,难以实现各元素的同时、快速分析。化学计量学是一种高效、功能强大的数据解析方法,对于样品复杂,基体干扰严重以及多组分样品的分析具有独特优势。将化学计量学应用于锕系元素的分析中,利用数学分离代替化学分离,可直接对样品进行测定。化学计量学方法也可用来指导试样的科学采集,进行实验设计、仪器分析操作条件选择等。从吸收光谱、ICP–AES及放射性测量3个方面综述了化学计量学在锕系元素分析中的应用,阐明了化学计量学在锕系元素分析中的应用难点及发展前景。     

Voltammetric Ultra Trace Determination of Tellurium

Abstract

A simple and convenient method is described for the determination of low concentration tellurium based on differential pulse polarographic reduction of Te(IV) in alkaline medium. Linearity of the calibration curve was achieved up to 25.5 ppm with a limit of determination of 0.02 µg/mL. The possible interference of coexisting metal ions was examined and ruled out. The method has been successfully applied for the analysis of tellurium in industrial waste samples.     

Spectrofluorometric determination of fluvoxamine in dosage forms, spiked plasma, and real human plasma by derivatization with fluorescamine

A sensitive, simple, and selective spectrofluorometric method was developed for the determination of fluvoxamine (FXM) in pharmaceutical formulations and biological fluids. The method is based upon the reaction between the drug and fluorescamine in borate buffer of pH 8.0 to yield a highly fluorescent derivative that is measured at 481 nm after excitation at 383 nm. The different experimental parameters affecting the development and stability of the reaction product were carefully studied and optimized. The method was applied for the determination of the drug over the concentration range of 0.1-1.1 microg/mL with a detection limit of 0.01 microg/mL (2 x 10(-8) M). The proposed method was successfully applied to the analysis of commercial tablets. The results obtained were in good agreement with those obtained using a reported spectrophotometric method. The method was applied for the determination of FXM in spiked human plasma with recovery (n=4) of 97.32 +/- 1.23%, while that in real human plasma (n=3) was 90.79 +/- 2.73%. A proposal for the reaction pathway is presented.     

Phase Solubility Analysis of Some Organophosphate Pesticides

Abstract

Phase solubility analysis (PSA) was applied to the determination of azinphos-ethyl and - methyl standards. The presence of 0.5% purity was detected by the method. A linear cumulative effect was obtained when known amounts of two impurities were added to standards of both organophosphate materials which were then analyzed by the phase solubility method.     

Different approaches to proximate analysis by thermogravimetry analysis

The experimental optimization by the simplex method of the proximate analysis of coal and biomass by thermogravimetry analysis (TGA) is reported. Heating rate, final temperature, holding time, Ar flow rate and sample size were the control variables. The response function used was chosen to minimize the difference in percentage of volatile matter with the ASTM characterization. The relative accuracy of the method was demonstrated by determination of the volatile matter contents of a number of coals in parallel with the ASTM certified method. The method is successfully used with biomass samples.