Simultaneous polarographic analysis of pyrazine and its methyl derivatives by iterative target transformation factor analysis

The polarographic waves of pyrazine and its methyl derivatives are seriously overlapping, so they cannot be determined individually by polarographic methods without a prior separation. In this paper, a chemometric approach, iterative target transformation factor analysis (ITTFA), is developed and applied to the determination of mixtures of pyrazines at trace level (2.0–9.0 × 10⁻⁶moll⁻¹) by using differential pulse polarography (DPP) and a static mercury drop electrode (SMDE). Different from the general ITTFA method, only one-dimensional measurement data of n − 1 standards and an unknown were used in this work. It produced acceptable results with average recoveries in the 96–108% range and relative standard errors in the 3.4–9.5% range.     

Simultaneous mixture analysis by using non-linear spectrophotometric data and linear iterative target transformation factor analysis

Non-linear absorption spectral data obtained from ternary mixtures of analytes are analyzed by using a linear model, iterative target transformation factor analysis (ITTFA). The use of transformed original variables is used to correct non-linearities in the original data. Absorbance below a certain limit (k) is described as linear and above this limit as non-linear. The extension of the regressor variables is the squared absorbances above the linear range. The variation of the prediction error as a function of the number of the factors and the k-values were considered and the minimum prediction error was evaluated for reaching to optimum. Except the natural non-negativity constraint the correlation constraint also is used on concentration vector in each iteration of ITTFA algorithm. The reliability of the method is evaluated using model data for ternary mixtures by spectral overlapping and different degrees of non-linearity. Simultaneous spectrophotometric determination of Eu³⁺, UO₂²⁺ and Th⁴⁺ with arsenazo III as chromogenic reagent is used as experimental model systems with non-linearity behavior of Eu³⁺and UO₂²⁺ components. The application to both synthetic and real data sets with different degrees of non-linearity demonstrate the ability of the proposed methodology to obtain better results than original data and ITTFA. The relative standard errors of prediction for proposed method in comparison with using the PLS calibration on original and extended data are nearly smaller.     

迭代目标转换因子分析光度法同时测定钇和其它稀土合量

以三氯偶氮胂为显色剂，根据钇(Y^3 )与其它稀土组分的显色络合物吸收光谱差别较大的特点，提出应用迭代目标转换因子分析光度法同时测定钇和其它烯土合量的计算光度分析法，通过对不同组成的人工模拟样品和龙南稀土氧化物标准样中的钇和其它稀土合量的测定，取得了满意的结果。     

Comparison of Multicomponent Determination of Iprodione,Procymidone and Chlorothalonil by Partial Least Squares Modelling Using Spectrophotometric and High-Performance Liquid Chromatography Data

Abstract

A Partial Least Squares (PLS) calibration method was applied to the simultaneous determination of iprodione, procymidone and chlorothalonil in mixtures, by uv-vis absorption spectrophotometry and by high performance liquid chromatography (HPLC). Signals and first-derivative (¹D) signals were used to optimize the calibration matrices by the PLS-1 method. Quantitative results are presented for synthetic mixtures and for extracts from soil and groundwater samples. Significant improvements were achieved by using the PLS-1 method built with first-derivative chromatograms, in the determination of iprodione, procymidone and chlorothalonil in environmental samples.     

Hypepontine,a new quaternary alkaloid with antimicrobial properties

Abstract

New isoquinoline alkaloid hypepontine (1) together with a five known compounds, were identified in Hypecoum ponticum Velen, the partial synonym of Hypecoum procumbens L. The structure of the new substance was elucidated based on spectroscopic evidence. The tertiary and quaternary alkaloid mixtures as well as the isolated alkaloids were evaluated for their antibacterial and antifungal activity. The result revealed that the crude alkaloid mixture containing quaternary isoquinoline alkaloids showed potent antifungal and antibacterial activity.     

Rapid and Accurate Determination of Acetaminophen and Phenprobamate in Binary Mixtures by Derivative-Differential UV Spectrophotometry and Ratio-Spectra Derivative Spectrophotometry

ABSTRACT

Derivative-Differential UV spectrophotometry and ratio-spectra first derivative spectrophotometry are presented for the simultaneous determination of analgesic and myorelaxan mixtures, namely acetaminophen (A)- phenprobamate (P). Derivative-Differential UV spectrophotometry is based on pH changes. The other method depends on the application ratio-spectra first derivative spectrophotometry to resolve the interference due to spectral overlapping.

The proposed methods were applied to the determination of this compound in synthetic mixtures and in pharmaceutical preparations. The proposed methods, which give thoroughly comparable data, are simple and rapid, and allow one to obtain precise and accurate results.     

Studies of Hydrous Zirconium Oxide. I. Thin-Layer Chromatography of Some Metal Ions on Hydrous Zirconium Oxide: Quantitative Separation of Bi(III) from Several other Metal Ions

Abstract

The analytical potentiality of hydrous zirconium oxide as an ionexchanger has been investigated by thin-layer chromatographic (TLC technique. Binder-free thin-layers of hydrous zirconium oxide are useful for 25 ternary and 12 quaternary separations. Quantitative separation of Bi (III) from some ternary and quaternary mixtures of metal ions has been achieved.     

Kinetic-Turbidimetric Determination of Stachyose Based on Its Inhibitory Action on Sucrose Crystallization.

Abstract

The effects of 9 saccharides on the crystallization of sucrose have been comparatively studied with analytical purposes. A sensitive (detection limit 0.1 μg mL^?1) and simple kinetic turbidimetric procedure is used for determination of stachyose, based on its inhibitory action on the crystallization of sucrose. The supersaturated solutions of sucrose were prepared by addition of acetone to stable water sucrose solutions. The induction period of the crystallization process was turbidimetrically measured. Controlled constant stirring and temperature are convenient in order to obtain reproducible results. The method was applied to the determination of stachyose in synthetic mixtures.     

Simultaneous First-Derivative Spectrophotometric Determination of Nickel and Manganese Complexes with 2-(2-Pyridylmethyleneamino)phenol

Abstract

A method is proposed for the simultaneous determination of nickel and manganese by first-derivative spectrophotometry based on their reactions with 2-(2-pyridylmethyleneamino)phenol (PMAP) Schiff base. The method allows the determination of Ni and Mn in the concentration range 0.3–3.0 μg ml^?1 in mixtures with their ten-fold concentration ratio. The method has been applied for Ni and Mn determination in bronzes. To optimize the experimental conditions for spectrophotometric determination of Mn with PMAP stability constants at different pH values have been determined. A critical evaluation of the proposed method was performed by statistical analysis of the experimental data.     

Resolution of Ternary and Quaternary Mixtures of Drugs in Pharmaceutical Preparations by Use of Spectrophotometric Data in Conjunction with PLS-1 and PLS-2 Data Processing Methods

Abstract

Two variants of partial least-squares methodology (PLS-1 and PLS-2) have been used for the analysis of ternary and quaternary mixtures of acetaminophen-acetylsalicylic acid-codeine and caffeine, respectively. This methodology permits the simultaneous quantification of the aforementioned drugs even with closely overlapping spectral bands without any separation step. The concentration ranges are 4.0–12.0, 0.2–1.0 and 4.0–12.0 μg·ml^?1 for acetaminophen-acetylsalicylic acid-codeine and 10.0–20.0, 6.0–16.0, 1.0–5.0 and 0.2–1.0 μg·ml^?1 for acetaminophen-acetylsalicylic acid-caffeine and codeine, respectively. A systematic study of the experimental data by applying an exhaustive statistical analysis to demostrate the validity of the proposed methods is presented. The results of the determination of these drugs in pharmaceutical preparations are also presented. The analytical results were quite good in all cases.     

Simultaneous Determination of Acetaminophen with Orphenadrine Citrate,Ibuprofen or Chlorzoxazone in Combined Dosage Forms by Zero-Crossing Derivative Spectrophotometry

Abstract

A derivative spectrophotmetric procedure for the simultaneous determination of acetaminophen-orphenadrine citrate, acetaminophen-ibuprofen and acetaminophen-chlorzoxazone, binary mixtures is described. The procedure minimises the mutual interference between these drugs in mixtures and allows the determination of these compounds without a previous extraction step. The precision of the method, expressed as the relative standard deviation, is better than 4%. The method has been successfully applied to laboratory mixtures and commercial tablets containing these drugs.     

Spectrophotometric Simultaneous Determination of Amaranth,Ponceau 4R,Allura Red and Red 2G by Partial Least Squares and Principal Component Regression Multivariate Calibration

ABSTRACT

The multivariate calibration methods, partial least square regression type 1 (PLS 1) and principal component regression (PCR), were proposed for the simultaneous spectrophotometry determination of Amaranth (E-123), Ponceau 4R (E-124), Allura red (E-129) and Red 2G (E-128) in their mixtures. The parameters of the chemometric procedures were optimized and the proposed method was validated with synthetic samples and applied to analyze these dyes in spiked samples of beverages with satisfactory results.     

Ion-Exchange Separtion and Determination of Mn,Co, Zn and Ni with Xylenol Orange as Post-Column Reagent

ABSTRACT

A method for the simultaneous determination of Mn, Co, Zn and Ni which combines Ion-chromatography and a post column reaction with xylenol orange is described. Using 0.07 M oxalic acid (pH adjusted to 5.5 with lithium hydroxide) as eluent, Mn, Co, Zn and Ni were first separated on a 4x250mm IonpacCS-5 column having both sulphonic acid and Alkyl quaternary ammonia functional groups and then transferred to a post-column reaction coil, where the elements react with xylenol orange. The coloured complexes formed were spectrophotometrically measured at 570 nm. The procedure has been successfully applied for the determination of Co, Zn and Ni in Al-bronze.     

Spectrofluorimetric determination of some water-soluble vitamins

Two simple and sensitive spectrofluorimetric methods were developed for determination of three water-soluble vitamins (B1, B2, and B6) in mixtures in the presence of cyanocobalamin. The first one was for thiamine determination, which depends on the oxidation of thiamine HCl to thiochrome by iodine in an alkaline medium. The method was applied accurately to determine thiamine in binary, ternary, and quaternary mixtures with pyridoxine HCl, riboflavin, and cyanocobalamin without interference. In the second method, riboflavin and pyridoxine HCl were determined fluorimetrically in acetate buffer, pH 6. The three water-soluble vitamins (B1, B2, and B6) were determined spectrofluorimetrically in binary, ternary, and quaternary mixtures in the presence of cyanocobalamin. All variables were studied in order to optimize the reaction conditions. Linear relationship was obeyed for all studied vitamins by the proposed methods at their corresponding lambda(exc) or lambda(em). The linear calibration curves were obtained from 10 to 500 ng/mL; the correlation ranged from 0.9991 to 0.9999. The suggested procedures were applied to the analysis of the investigated vitamins in their laboratory-prepared mixtures and pharmaceutical dosage forms from different manufacturers. The RSD range was 0.46-1.02%, which indicates good precision. No interference was observed from common pharmaceutical additives. Good recoveries (97.6 +/- 0.7-101.2 +/- 0.8%) were obtained. Statistical comparison of the results with reported methods shows excellent agreement and indicates no significant difference in accuracy and precision.     

Spectrophotometric Assay of Fluphenazine HCL-Nortriptyline HCL Mixture in Tablets Using Fourier Function Method

Abstract

The Fourier function method has been applied to the independent determination of fluphenazine hydrochloride (FH) and nortriptyline hydrochloride (KH) (1:20) in both laboratory made mixtures and commercial tablets. The method is based on the absorbance measurement of FE (the minor component) in concentrated mixture solutions, which is then properly diluted prior to NH absorbance measure-     

N-Pyrrolyl Derivative Acids Chromatography

Abstract

A determination is made on the effects of the variation of pH, methanol %, contents of tetrabutylammonium salts, ionic strength and counterion nature of the mobile phase quaternary ammonium salt, on the retention of a series of analgesics formed by N-pyrrolyl derivative acids through a column constituted by 10 μ irregular particles of octadecyl silica.

The results obtained are applied to mixture separation of said acids.     

Effect of molecular structure on the phase behaviour of some liquid crystalline compounds and their mixtures VIII. Quaternary mixtures of enantiotropes

Transition temperatures of quaternary mixtures prepared from the cyano and nitro derivatives of the two series, 4-hexadecyloxyphenyl 4-substituted benzoates (Ia,b) and 4-substituted phenyl 4-hexadecyloxy benzoates (IIa,b) have been determined by DSC and the transitions identified with polarized light microscopy. The cyano and nitro derivatives, in both series, were used because their molecules are enantiotropic. The method described before for the ternary system was extended to elucidate the eutectic composition of the quaternary system from the knowledge of either the eutectic compositions of the four possible ternary mixtures or of those of the six individual binary systems. A general equation was deduced to calculate the eutectic composition of any multi-component system from values determined for their individual binary systems. T_c values of binary, ternary, or quaternary mixtures were related to the polarizability anisotropy, Deltaalpha_X, of the individual C_Ar-X bonds. The mixture law was successfully applied.     

Simultaneous Determination of Three Synthetic Glucocorticoids by Differential Pulse Stripping Voltammetry with the Aid of Chemometrics

Abstract

A novel voltammetric method for simultaneous determination of the glucocorticoid residues prednisone, prednisolone, and dexamethasone was developed. All three compounds were reduced at a mercury electrode in a Britton–Robinson buffer (pH 3.78), and well-defined voltammetric waves were observed. However, the voltammograms of these three compounds overlapped seriously and showed nonlinear character, and thus, it was difficult to analyze the compounds individually in their mixtures. In this work, two chemometrics methods, principal component regression (PCR) and partial least squares (PLS), were applied to resolve the overlapped voltammograms, and the calibration models were established for simultaneous determination of these compounds. Under the optimum experimental conditions, the limits of detection (LOD) were 5.6, 8.3, and 16.8 µg l^?1 for prednisone, prednisolone, and dexamethasone, respectively. The proposed method was also applied for the determination of these glucocorticoid residues in the rabbit plasma and human urine samples with satisfactory results.     

Spectrophotometric Analysis of Systems with Non-Additive Absorbances

Abstract

The increment method under least squares has been applied to the spectrophotometric determination of p-hydroxybenzoic acid complexed with polyvinylpyrrolidone in water. The mean percentage recovery for six prepared mixtures was found to be 99.49 + 1.25. When the A_max method has been applied, the mean percentage recovery was found to be 90.99+5.59. The theoretical bases of the method have been discussed.     

Novel Electrochemical Sensor for Sunset Yellow Based on a Platinum Wire–Coated Electrode

Abstract

In this research, the construction and general performance characteristics of a sunset yellow sensor based on sunset yellow–cetyl pyridinum (SY-CPY) ion pair as an ion exchanger were described. A coated platinum wire electrode (CPE) was prepared and compared with coated graphite (CGE) and membrane electrode (PME). The CPE exhibited a rapid and Nernstian response (?29.77 ± 0.2 mV decade^?1) to SY concentration range from 3.16 × 10^?7 to 3.16 × 10^?3 mol dm^?3 within pH 4.5–9.5. Interfering effects of some foreign substances were reported. The optimized matrix was successfully applied to the determination of SY in artificial mixtures and commercial soft drinks. The results showed good agreements with the determination made by use of high-performance liquid chromatography.