Subsecond FFT‐adsorptive Voltammetric Technique as a Novel Method for Subnano Level Monitoring of Piroxicam in its Tablets and Bulk Form at Au Microelectrode in Flowing Solutions

Abstract

In this work a novel method for the determination of piroxicam in flow‐injection systems has been developed. A system using fast Fourier transform continuous cyclic voltammetry (FFTCV), at a gold microelectrode in flowing solution, was used for determining piroxicam in its pharmaceutical formulations. The developed technique is very simple, precise, accurate, time saving, and economical, compared to all of the previously reported methods. The effects of various parameters on the sensitivity of the method were investigated. The best performance was obtained with a pH value of 2, scan rate value of 40 V/s, accumulation potential of (400) mV, and accumulation time of 0.4 s. The proposed method has some advantages over other reported methods, such as, no need for the removal of oxygen from the test solution, a picomolar detection limit, and finally that the method is fast enough for the determination of any such compound, in a wide variety of chromatographic methods. To obtain a sensitive determination, the integration range of currents was set for all the potential scan ranges, including oxidation and reduction of the Au surface electrode, while performing the measurements. The potential waveform, consisting of the potential steps for cleaning, accumulation, and potential ramp of analyte, was applied on an Au disk microelectrode (with a 12.5 µm in radius) in a continuous way. The method was linear over the concentration range of 1.5–364000 pg/ml (r=0.998) with a limit of detection and quantitation of 0.33 and 1.5 pg/ml, respectively. The method has the requisite accuracy, sensitivity, precision, and selectivity to assay piroxicam in tablets.     

Determination of Vitamin A in Infant Milk-Based Formulas and Pharmaceutical Formulations Using Flow Injection with Ce(IV)–Na2SO3 Chemiluminescence Detection

A rapid and simple flow injection (FI) method is reported for the determination of vitamin A (retinol) based on its strong enhancing effect on the Ce(IV)–Na₂SO₃ chemiluminescence (CL) reaction in an acidic solution. The effect of key chemical and physical parameters (i.e., reagent concentrations, flow rate, and sample volume) was optimized and potential interferences examined. Under the selected experimental conditions, a linear calibration was obtained between the CL intensity and vitamin A concentration in the range 0.1–8.0 µg mL^?1 (r ²  = 0.9986, n = 8). The limit of detection (3 s x blank) was 0.01 µg mL^?1 retinol (n = 6) and the relative standard deviation (RSD) for 0.25 µg mL^?1 retinol was 2.3% (n = 10) with a sampling rate of 180 h^?1. The method was successfully applied to infant milk-based formulas and pharmaceutical formulations and the results were not significantly different at 95% confidence interval with those obtained by using a spectrophotometric reference method. The possible CL mechanism is also discussed briefly supporting with UV-visible, fluorescence, and CL spectra.     

Determination of Diammonium Glycyrrhizinate and Its Antioxidant Activity Using a Novel Chemiluminescence System

A novel chemiluminescence (CL) system was established for the determination of diammonium glycyrrhizinate (DG) in pharmaceutical preparations and its ability of scavenging hydroxyl radical. It was shown that a strong CL signal was observed when Eosin Y mixed with Fenton reagent. The CL intensity was decreased significantly when DG was added to the reaction system and partially scavenged the hydroxyl radicals in the solution. The extent of decrease in the CL intensity had a good stoichiometrical relationship with DG concentration. Based on this, we developed a new method for the determination of DG using a flow injection chemiluminescence (FI-CL) technique. Under the optimal conditions, the linear range of DG concentration was 6.0 × 10^?8–5.0 × 10^?6 mol/L (R = 0.9982) with a detection limit of 8.0 × 10^?9 mol/L (SN = 3), and the RSD was 3.8% for 2.0 × 10^?7 mol/L DG (n = 11). This method was successfully used in the determination of DG in tablets and the evaluation of hydroxyl radical scavenging capacity of DG. The possible reaction mechanism of the CL system is discussed.     

Batch and Flow Injection Fluorimetric Determination of Fluoxetine

Abstract

A method for the fluorimetric determination of fluoxetine in continuous and discontinuous systems is reported. The method is based on the hydrolysis of fluoxetine in acid medium. The fluorescent product has a spectrum with excitation and emission maxima at 253 and 306 nm, respectively. The method was applied to the determination of fluoxetine in pharmaceutical products.     

Amperometric Immunosensor for the Detection of 2,4-Dichlorophenoxyacetic Acid (2,4-D) in Water

ABSTRACT

An amperometric immunosensor for the determination of the herbicide 2,4-dichlorophenoxyacetic acid (2,4-D) in water has been developed using sequential injection analysis techniques. The system is based on a rapid competitive enzyme immunoassay employing an alkaline phosphatase-labeled monoclonal antibody directed against the herbicide and an immunoreactor with 2,4-D immobilized via bovine serum albumin either to Eupergit in a column or directly to the surface of a glass capillary. The detection limit of the immunosensor at 0.1 μg 2,4-D/l without enrichment of the analyte makes automatic measurements of 2,4-D in drinking and ground water feasible.     

Stepwise Injection Spectrophotometric Determination of Flavonoids in Medicinal Plants

A simple, rapid, and automated method for the spectrophotometric determination of flavonoids in medicinal plants was developed using a stepwise injection manifold. The determination was based on formation of colored complexes of flavonoids with Al(III) in micellar media. Analytical characteristics of the determination were significantly improved when cetylpyridinium chloride was used as a micellar catalyst. It was found that the rate of colored complex formation of rutin with Al(III) increased (k = (1.8 ± 0.1) · 10⁴ min^?1mol^?2 L²) in the presence of cetylpyridinium chloride. Under the optimum conditions, a linear response was found from 0.004 to 0.2% (volume of weight %). The detection limit (3s) was determined as 0.001% rutin versus the weight of the sample. The developed method was used for the analysis of different medicinal plants for flavonoids.     

用深部处理剂JY-8提高注聚区残余聚合物的利用率

针对目前各油田聚合物驱转为水驱后,一般出现含水上升快,产油量大幅度下降的情况,以及油层内残余的大量聚合物未得到利用,而目前开发的残余聚合物再利用技术存在一些缺点,未得到推广应用,研制出新型复合处理剂JY-8。新型复合处理剂JY-8可与聚合物形成强度较高的凝胶体,将地层内残余聚合物有效地固定和絮凝,是很好的固定剂和絮凝剂,实现了“二剂合一”,达到对地层进行深部调剖、驱油的目的;同时,通过调整复合处理剂JY-8的加量等可调节成胶时间和凝胶强度。室内评价和现场应用表明,与以前的技术相比,复合处理剂JY-8可使油层内的残余聚合物利用率从原来的8％提高到15.65％,使聚合物驱后续水驱的采收率增加值从原来的10.33％提高到18.1％,在油井上起到了很好的增油、控水效果。     

A Numerical Investigation on the Laminar Boundary Flow Layer with Transpiration Cooling

Heat transfer characteristics in the laminar boundary layer with transpiration cooling function are numerically analyzed by an integral method. The effects of coolant injection ratio, and the Re and Pr numbers of the exterior hot flow on the temperature at porous plate surface are discussed. The numerical results and discussions indicate that the surface temperature falls with an increase of coolant injection ratio, the temperature distribution on the surface is not uniform, and the effects of the Re number under lower Pr number condition are distinctly different to that under the higher Pr number condition.     

循环电场下钙钛矿铁电薄膜的极化疲劳机制

将循环电场引起电荷注入并产生局部相分解的理论引入到氧空位模型中,建立了一个解析形式的钙钛矿结构铁电薄膜极化疲劳模型.结合该模型讨论了铁电薄膜与金属电极间的低介电常数界面层对疲劳特性的影响,认为界面层对疲劳的产生起关键作用.运用该模型分析了不同松弛时间、电压、温度下的疲劳特性,并与已报道的实验结果进行了对比,模型计算结果与实验数据具有很好的一致性.     

CO2 Injection into Saline Carbonate Aquifer Formations II: Comparison of Numerical Simulations to Experiments

Sequestration of carbon dioxide in geological formations is an alternative way of managing extra carbon. Although there are a number of mathematical modeling studies related to this subject, experimental studies are limited and most studies focus on injection into sandstone reservoirs as opposed to carbonate ones. This study describes a fully coupled geochemical compositional equation-of-state compositional simulator (STARS) for the simulation of CO₂ storage in saline aquifers. STARS models physical phenomena including (1) thermodynamics of sub- and supercritical CO₂, and PVT properties of mixtures of CO₂ with other fluids, including (saline) water; (2) fluid mechanics of single and multiphase flow when CO₂ is injected into aquifers; (3) coupled hydrochemical effects due to interactions between CO₂, reservoir fluids, and primary mineral assemblages; and (4) coupled hydromechanical effects, such as porosity and permeability change due to the aforementioned blocking of pores by carbonate particles and increased fluid pressures from CO₂ injection. Matching computerized tomography monitored laboratory experiments showed the uses of the simulation model. In the simulations dissolution and deposition of calcite as well as adsorption of CO₂ that showed the migration of CO₂ and the dissociation of CO₂ into HCO₃ and its subsequent conversion into carbonate minerals were considered. It was observed that solubility and hydrodynamic storage of CO₂ is larger compared to mineral trapping.