Stability-Indicating Method for the Determination of Meloxicam and Tetracaine Hydrochloride in the Presence of their Degradation Products

Abstract

Sensitive, spectrophotometric and densitometric methdos are described for the determination of meloxicam I and tetracaine hydrochloride II in the presence of their degradation products.

Meloxicam was determined in the presence of its degradation products (5-methyl-2-aminothiazole) III and benzothiazine carboxylic acid IV by two methods. These methods are the first derivative Spectrophotometry at 338 nm and TLC densitometric method at 365nm. The methods were applicable over the concentration range of 5–20μg.m^?1 and 2–10μg with mean accuracies of 99.66±0.91% and 99.99±0.70% respectively.     

SPECTROPHOTOMETRIC DETERMINATION OF ZINC IN PHARMACEUTICAL SAMPLES USING DI-2-PYRIDYL KETONE SALICYLOYLHYDRAZONE

ABSTRACT

A highly sensitive procedure for spectrophotometric determination of zinc has been developed. At pH 4.5, in 50% (V/V) ethanol-water medium and in the presence of di-2-pyridyl ketone salicyloylhydrazone (DPKSH), zinc forms a yellow complex which has maximum absorption at 376 nm The molar absorptivity is 4.82×10⁴ L mol^?1 cm^?1. The detection limit of this method is 62.1 nM for Zn(II).

The method has been applied to the spectrophotometric determination of zinc in pharmaceutical formulations and the results comply with those obtained by AAS. The proposed method is simple, rapid and accurate.     

Spectrophotometric Studies of the Reaction of Zinc(II) with Some Azo‐Triazol Compounds and Its Application to the Spectrophotometric Determination of Microamounts of Zinc(II)

Abstract

A new, simple, and sensitive quantitative spectrophotometric method for the rapid determination of zinc(II) using six azo compounds based on 3‐amino‐1,2,4‐triazole, namely {3‐(2,4‐dihydroxy‐1‐phenylazo)‐1,2,4‐triazole) (I), 3‐(2‐hydroxy‐5‐methyl‐1‐phenylazo)‐1,2,4‐triazole) (II), 3‐(2‐hydroxy‐5‐acetyl‐1‐phenylazo)‐1,2,4‐triazole) (III), 3‐(2‐hydroxy‐5‐ethylcarboxylate‐1‐phenylazo)‐1,2,4‐triazole) (IV), 3‐(2‐hydroxy‐5‐formyl‐1‐phenylazo)‐1,2,4‐triazole) (V), and 3‐(2‐hydroxy‐5‐bromo‐1‐phenylazo)‐1,2,4‐triazole) (VI), has been developed for use in aqueous media containing 40% (v/v) methanol. Linear calibration graphs are obtained up to 2.6, 5.9, 5.2, 5.2, 8.2 and 9.0 µg mL^?1 using ligands I, II, III, IV, V, and VI, respectively. Absorption maxima, molar absorptivities, and Sandell's sensitivities of 1:2 (M:L) complexes were found to be 490, 530, 505, 520, 550, and 510 nm, 4.86×10⁴, 2.10×10⁴, 1.26×10⁴, 0.10×10⁴, 0.19×10⁴, and 0.29×10⁴ L mol^?1 cm^?1, and 0.0014, 0.0031, 0.0052, 0.0662, 0.0348, and 0.0225 µg cm^?1 for ligands I, II, III, IV, V, and VI, respectively. Using the masking agents, the color reactions are free from interference by more than 30 ions investigated. The method has been applied to the spectrophotometric determination of trace amounts of zinc in pharmaceutical formulations and human hair samples. A study of some zinc solid complexes showed that chelation takes place through one nitrogen atom of the azo group and proton displacement from the hydroxyl group.     

Effect of In3+ ions on the electrochemical performance of the positive electrolyte for vanadium redox flow batteries

Influence of In³⁺ ions on electrochemical performance of positive electrolyte for vanadium redox flow battery was investigated in this paper. The electrochemical activity and kinetics of V(IV)/V(V) redox couple can be enhanced by the addition of In³⁺ ions, and the optimal concentration of In³⁺ ions was found at 10 mM. At this condition, the oxidation peak current with 10 mM In³⁺ ions is 46.6 mA at a scan rate of 20 mV s^?1, larger than that of pristine electrolyte (41.8 mA), and the standard rate constant is 6.53?×?10^?5 cm s^?1, 42 % larger than that of the pristine electrolyte (4.58?×?10^?5 cm s^?1). The cell using electrolyte with 10 mM In³⁺ ions was assembled, and the charge–discharge performance was evaluated, and the average energy efficiency increases by 1.9 % compared with the pristine cell. The improved electrochemical performance may be ascribed to that In³⁺ ions change the hydration state of vanadium ions in electrolyte and promote charge transfer process.     

Solid-Phase Extraction Using Polymer-Based Cartridge Modified with 2-(2-benzothiazolylazo)-3-hydroxyphenol for Preconcentration of Uranium(VI) Ions from Water and Real Samples

ABSTRACT

A highly sensitive, selective, and rapid method for the determination of ng mL^?1 level of U(VI) based on the rapid reaction of U(VI) with 2-(2-benzothiazolylazo)-3-hydroxyphenol (BTAHP) and the solid-phase extraction of the colored complex with a reversed-phase polymer-based C18 cartridge was developed. The BTAHP reacted with U(VI) to form a violet complex of molar ratio 2:1 [BTAHP to U(VI)] in the presence of 4.0 M of phosphoric acid solution and Triton X-114 medium. This complex was enriched by the solid-phase extraction with a polymer-based C18 cartridge. The enrichment factor of 200 was achieved. The molar absorptivity of the complex is 2.73 × 10⁶ L mol^?1 cm^?1 at 639 nm in the measured solution. The system obeys Beer's law in the range of 2.0–125 ng mL^?1, whereas the optimum concentration range obtained from Ringbom plot was 8.0–115 ng mL^?1. The relative standard deviation for 10-replicates sample of 100 ng mL^?1 level is 1.05%. The detection and quantification limits are 0.6 and 1.98 ng mL^?1 in the original sample. This method was applied to the determination of uranium(VI) in sea, tap, and waste waters, ore standard reference material, soil and sediment samples with good results comparing to the graphite furnace atomic absorption spectroscopy (GFAAS) method.     

Flow Injection Kinetic Spectrophotometric Determination of Cerium Based on the Decolorization Reaction Between Arsenazo III and Cerium (IV)

ABSTRACT

Trace amounts of cerium were analyzed by flow injection kinetic spectrophotometry, based on the decolorization reaction between arsenazo III and Ce(IV) in sulfuric acid medium at room temperature. The absorbance difference (ΔA) of decolorization was linear with the concentration of Ce(IV). The flow injection technique was used to precisely control the timing. Under the optimum conditions, the determination of Ce(IV) in the range 0.0–8.0 µg mL^?1 with a correlation coefficient (r) of 0.9982, the regression equation was ΔA = 0.0014 + 0.0406c (µg mL^?1). The detection limit (3σ) of 0.2 µg mL^?1 was achieved at a sampling frequency of 60 h^?1. The proposed method was applied to the analyses of Ce in soil successfully.     

Determination of Selenium (IV) in Natural Waters by HG‐AAS Using an Integrated Reaction Chamber Gas–Liquid Separator

Abstract

A simple online sequential insertion manifold coupled to a hydride generation atomic absorption spectrometer (HG‐AAS) has been developed for selective inorganic Se(IV) determination. The online method is based on the sequential insertion of sample and reagents in the integrated reaction chamber gas–liquid separator (RC‐GLS), which operates initially as reaction chamber for various sample volumes (up to 20 mL) and subsequently as gas–liquid separator with limited dead volume. The generated hydride from a large sample volume is trapped in the RC‐GLS for a short time and then it is flashed in the atomic absorption cell. The HCl and the NaBH₄ concentration was optimized for selective inorganic Se(IV) determination. For 8‐mL and 16‐mL sample consumption, the sampling frequency is 40 h^?1 and 24 h^?1, while the detection limit is 0.04 µg L^?1 and 0.03 µg L^?1, respectively. The precision (relative standard deviation) for 2.0 µg L^?1 Se(IV) (n=10) is 2.6% and 2.8% for 8 mL and 16 mL sample volumes, respectively. The accuracy of the proposed method was evaluated by analyzing the certified reference material, NIST CRM 1643d, and also by analyzing spiked natural water.     

A Novel Pyrene Fluorescent Sensor Based on the π–π Interaction Between Pyrene and Graphene of Graphene–Cadmium Telluride Quantum Dot Nanocomposites

In this article, water-soluble graphene–cadmium telluride quantum dot nanocomposites were fabricated through the synthesis of cadmium telluride quantum dots in the presence of graphene aqueous dispersion. It was found that pyrene could remarkably quench fluorescence of graphene–cadmium telluride quantum dot nanocomposites. On this basis, a novel method for the determination of pyrene was developed. Factors affecting the pyrene detection were investigated, and the optimum conditions were determined. Under the optimum conditions, a linear relationship could be established between the quenching of fluorescence intensity of graphene–cadmium telluride quantum dot nanocomposites and the pyrene concentration in the range of 6.00 × 10^?8–2.00 × 10^?6 mol L^?1 with a correlation coefficient of 0.9959. The detection limit was 4.02 × 10^?8 mol L^?1. Furthermore, the nanocomposites were applied to practical determination of pyrene in different water samples with satisfactory results.     

Preconcentration and Separation of Gold(III) from Ore Samples by Solid-Phase Extraction Prior to Its Catalytic Fluorescent Determination

ABSTRACT

A new catalytic kinetic fluorescent quenching method for the determination of trace gold(III) was investigated. The method was based on the catalytic effect of gold on oxidation of 3-(3′-methylphenyl)-5- (2′-arsenoxylphenylazo) rhodanine by hydrogen peroxide in potassium hydrogen phthalate–hydrochloric acid (pH = 3.4). Under the optimum conditions, the great decrease of fluorescence intensity has a linear relationship against the concentration of gold in the range of 0 to 12.0 µg·L^?1 with a detection limit of 6.0 × 10^?10g·L^?1. The coexistent metal ions can be separated, and gold can be enriched by TBP resin of solid-phase extraction, which greatly improves the selectivity and sensitivity of the system. The method can be used to determine trace amounts of gold in ore samples successfully with satisfactory results.     

Synthesis of 2-Mercaptonicotinic Acid-Capped CdSe Quantum Dots and its Application to Spectrofluorometric Determination of Cr(VI) in Water Samples

The CdSe quantum dots (QDs) capped with 2-mercaptonicotinic acid (H₂MN) were prepared through a controllable process at 80 °C. The prepared QDs were characterized by XRD, TEM, IR, UV–Vis and fluorescence (FL) techniques. It was found that the QDs were nearly mono-disperse with the diameters in the range of 8–10 nm. These QDs are capable to exhibit strong FL even in concentrated acidic media. They exhibit an enhanced fluorescence in the presence of Cr(VI), which was used for the determination of Cr(VI) in water samples. The linear range was found to be 1?×?10^?7–6.0?×?10^?6 M with the RSD and DL of 0.92 % and 5?×?10^?8 M, respectively. Except that Ca²⁺ and Fe³⁺ which can be eliminated through a simple precipitation process, the other co-existent ions present in natural water were not interfered. The recoveries obtained for the added amounts of Cr(VI) were in the range of 96.9–103.2 %, which denote on application of the method, satisfactorily.     

Comparative Study on Three Different Systems of Chemiluminescence Flow‐Injection Determination of Leucogen

Abstract

The effects of three systems on the chemiluminescence (CL) intensity have been studied in this paper, such as leucogen–potassium permanganate–rhodamine B, leucogen–cerium (IV)–rhodamine B, and leucogen–luminol–hydrogen peroxide (called system 1, system 2, and system 3, respectively). The mechanism of these reactions is also discussed. Surfactant (CTMAB) has a remarkably sensitive effect on these systems mentioned above. Therefore, three new flow injection chemiluminescence methods for the determination of leucogen have been established. For system 1, the linear range is 8.0×10^?8 to 4.0×10^?5 g mL^?1, with limits of detection 2×10^?8 g mL^?1; the relative standard deviation is 2.5% (n=11, Cs=4.0×10^?6 g mL^?1). For system 2, the linear range is 1.0×10^?8 to 5.0×10^?6 g mL^?1, with limits of detection 3×10^?9 g mL^?1; the relative standard deviation is 5.1% (n=11, Cs=1.0×10^?6 g mL^?1). For system 3, the linear range is 4.0×10^?8 to 2.0×10^?6 g mL^?1, with limits of detection 1×10^?8 g mL^?1; the relative standard deviation is 1.3% (n=11, Cs=1.0×10^?7 g mL^?1). Compared with the three methods above, system 3 is confirmed as the best method. This method has been applied to the determination of leucogen with satisfactory results.     

Flow‐Injection Online Reduction Atomic Fluorescence Spectrometry Determination of Se(IV) and Se(VI) with Electrochemical Hydride Generation

Abstract

A new flow‐injection online reduction electrochemical hydride generation system for the determination of Se(IV) and Se(VI) by atomic fluorescence spectrometry (AFS) was developed. In the system, an electromagnetic induction oven was used as heating resource to reduce Se(VI) to Se(IV) and a homemade tubular electrolytic cell as hydride generator. All analytical procedures were automatically controlled by a computer. The conditions of online reduction, including temperature, HCl concentration, and reduction time, have been studied in detail. The detection limits (3σ) of Se(IV) and Se(VI) in aqueous solution were 0.26 µg L^?1 and 0.23 µg L^?1, respectively. The precision for 11 replicate measurements of 50 µg L^?1 Se(IV) and Se(VI) was 2.2% and 2.5%. This proposed method has been applied to the determination of Se(IV) and Se(VI) in springwater samples.     

Study of Specific Interaction between bis(<Emphasis Type="Italic">p</Emphasis>-phenylene)-34-crown-10-based Substituted Macrocycle and Ni<Superscript>2+</Superscript>

A novel macrocyclic host has been synthesized for the determination of Ni (II) ions in aqueous solution (H₂O-CH₃CN, v/v?=?1:1). Its molecular structure has been verified by ¹H-NMR, ¹³C NMR and mass spectrometry (ESI).This probe shows selectivity towards the presence of Ni (II) ion among various alkali, alkaline earth, and transition metal ions. The formation of a new fluorescence band at 311 nm has been detected due to possible complex formation with increasing Ni²⁺ concentration in the range of 10^?5–10^?4 M. The detection limit is calculated to be 5.22 μM. To our knowledge, it will be the first case for bis(p-phenylene)-34-crown-10 based molecules to recognize Ni²⁺ ions.     

Influence of Diffusion Parameters on the Spectral Characteristics of Raman Modes of Titanium-Diffused Lithium Niobate Planar Waveguides

ABSTRACT

A systematic investigation on the influence of the diffusion parameters (time and temperature) and initial titanium film thickness on the spectral characteristics of the LiNbO₃ Raman modes is reported. Raman spectra are measured in the range 50–1000 cm^?1 ～2 µm below the surface of the crystals. Broadening of the Raman lines and, therefore, crystal lattice disorder induced by the titanium ions are found to depend on the fabrication parameters. The disorder associated with the titanium ions near the surface of LiNbO₃ is encoded in the broadening of the A₁(TO₁) Raman line. A linear relation between the A₁(TO₁) mode broadening and the Ti concentration is presented. The diffusion theory is used to explain the experimental data. Raman spectroscopy combined with diffusion theory can be used to estimate the evolution of the titanium surface concentration.     

Optical properties of Yb3+ ions in fluorophosphate glasses for 1.0 μm solid-state infrared lasers

Yb³⁺-doped fluorophosphate glasses were prepared by melt-quenching technique and characterized their spectroscopic properties to assess the laser performance parameters. The magnitude of absorption (emission) cross-sections at 975 nm for all the studied Yb³⁺-doped glasses is found to be in the range of 0.29–1.50 × 10^?20 (0.59–1.99 × 10^?20 cm²) which is much higher than those of commercial Kigre QX/Yb: 1.06 × 10^?20 (0.5 × 10^?20 cm²) laser glass. The luminescence lifetimes of ²F_5/2 level decrease (1.15–0.45 ms) with increase in Yb₂O₃ concentration (0.1–4.0 mol%). Effect of OH^? content on luminescence properties of Yb³⁺ ions has also been investigated. The effect of radiative trapping has been discussed by using McCumber (McC) and Fuchtbauer–Ladenburge (F–L) methods. The product of experimental lifetimes and emission cross-sections for 0.1 mol% Yb₂O₃-doped glass is found to be 2.28 × 10^?20 cm² ms which indicates that the higher energy storage and extraction capability could be possible. The detailed spectroscopic results suggest that the studied glasses can be considered for high-power and ultrashort pulse laser applications.     

Vibrational Spectrometry Strategies for Quality Control of Procymidone in Pesticide Formulations

Abstract

Two vibrational spectrometry–based methodologies were developed for procymidone determination in wettable powdered pesticide formulations. The Fourier‐transform infrared (FTIR) procedure was based on the selective extraction of procymidone by chloroform and determination by peak area measurement between 1451 and 1441 cm^?1, using a baseline correction established between 1490 and 1410 cm^?1, and a precision of 0.4% and a limit of detection of 0.01% w/w procymidone for a sample mass of 25 mg were obtained. For FT‐Raman determination, the selected conditions were peak area measurement between 1005 and 995 cm^?1 Raman shift, with a baseline correction fixed between 1030 and 947 cm^?1, and a relative standard deviation of 1% and a limit of detection of 0.8% procymidone in the original sample were obtained. The sample frequency for FTIR determination was 30 hr^?1, lower than that for Raman with 40 hr^?1. FT‐Raman reduces to the minimum the reagent consumption and waste generation, also avoiding the sample handling and contact of the operator with the pesticide. It can be concluded that the proposed methods are appropriate for quality control in commercial pesticide formulations.     

Study on the Cofluorescence Effect of Europium (III)–Yttrium (III)–Balofloxacin–Sodium Dodecyl Sulfate System and Its Analytical Application

A new fluorescence enhancement phenomenon in the europium(III)–balofloxacin–sodium dodecyl sulfate system was observed when yttrium(III) was added. Based on this, a sensitive cofluorescence assay for the estimation of balofloxacin was established. Under the optimized conditions, the enhanced fluorescence signal was linear over the concentration of balofloxacin ranging from 3.0 × 10^?9 to 7.0 × 10^?6 mol L^?1 with a correlation coefficient of 0.9993. The detection limit (3 σ) was determined as 8.3 × 10^?10 mol L^?1. The presented method was successfully applied to determination of balofloxacin in pharmaceutical preparations, human serum, and urine. The possible fluorescence enhancement mechanism was also discussed.     

Spectroscopic Study on the Interaction of Pyronine Y with Nucleic Acids and Its Analytical Application

ABSTRACT

The interaction of pyronine Y (PY) with nucleic acids was studied by resonance Rayleigh scattering (RRS) for nucleic acid detection. The enhanced RRS intensity of nucleic acids reacted with PY was proportional to the concentration of nucleic acids in the ranges of 27.0–625 ng ml^?1 for fish sperm DNA, 39.0–500 ng ml^?1 for calf thymus DNA, and 59.0–375 ng ml^?1 for yeast RNA. The limits of determination were 0.2 ng ml^?1 for fish sperm DNA, 0.6 ng ml^?1 for calf thymus DNA, and 0.7 ng ml^?1 for yeast RNA. The method had been successfully applied to the quick determination of nucleic acids in synthetic and natural samples.     

Hydrodynamic Sequential Injection Spectrophotometric System for Determination of Manganese in Soil

ABSTRACT

A novel hydrodynamic sequential injection (HSI) spectrophotometric system for determination of manganese was developed. It is based on the complexation of Mn(II) with formaldoxime in basic solution (pH ≥ 10) to produce product that could be monitored spectrophotometrically at 450 nm. Based on the HSI concept, both sample and reagents were aspirated through solenoid valves to fill a defined volumes conduit between 3-way connectors connected in series, forming stacked zones of solutions similar to those in normal SI. The concept was successfully demonstrated for manganese determination. A linear calibration graph over a range of 0.5 to 30 mg L^?1 Mn(II) with a detection limit of 0.2 mg L^?1 was obtained. Relative standard deviations for 11 replicated injections of 5 and 20 mg Mn L^?1 were 5.6% and 2.4%, respectively. A sample throughput of 45 h^?1 was achieved. The results from investigation of exchangeable manganese in soil samples by the developed method were found to be in good agreement with the results obtained by a batch spectrophotometric method, despite the proposed system employed simpler and more cost-effective devices/instruments, had higher degrees of automation with full microcontroller control of the operation, and consumed smaller amounts of chemicals (250 µL each of hydroxylamine, sample, and formaldoxime solutions and 2.5 mL of buffer carrier solution per operation cycle).     

Dispersive liquid–liquid microextraction based on solidification of floating organic drop for separation and preconcentration of malachite green before its determination by flow injection spectrophotometry

ABSTRACT

A simple and fast dispersive liquid–liquid microextraction based on solidification of floating organic drop has been developed for the separation and preconcentration of malachite green in water samples prior to its determination by flow injection spectrophotometry. Sodium lauryl sulfate, an anionic surfactant, was used for the ion-pair formation with malachite green. The factors affecting the ion-pair formation and extraction were optimized. Under the optimized conditions (volume of 1-undecanol as the extraction solvent, 40 μL; the volume of ethanol as the disperser solvent, 100 μL; sodium lauryl sulfate concentration, 7.5 × 10^?7 mol L^?1, and the pH of the sample, ～3.0), the calibration graph was linear over the range of 0.8–25 µg L^?1 with the detection limit of 0.3 µg L^?1 and the preconcentration factor of 750. The relative standard deviation at 7 µg L^?1 (n = 6) was found to be 2.1%. The developed method was successfully applied to the determination of malachite green in river water and fish farming water samples.