Comparative Study of the Ratio Spectra Derivative Spectrophotometry,Derivative Spectrophotometry and Vierordt's Method Appued to the Analysis of Lisinopril and Hydrochlorothiazide in Tablets

Abstract

Three new spectrophotometric methods are described for the determination of lisinopril and hydrochlorothiazide in their binary mixturer: First derivative spectrophotometry ratio spectra derivative and Vierordt's method. The procedures do not require any prior separation. In the derivative spectrophotometry, the dA/dλ values in the first derivative spectra of the mixture were measured at 269.6 nm for lisinopril and at 279.8 nm for hydrochlorothiazide. The calibration graphs were linear in the range 25.56–129.50 μg.ml^?1 for lisinopril and 10.60–139.80 μg.ml^?1 for hydrochlorothiazide. In ratio spectra derivative spectrophotometry, the calibration graphs for 15.68–129.50 μg.ml^?1 lisinopril and for 5.98–139.80 μg.ml^?1 hydrochlorothiazide were obtained by measuring the signals at 253.7 nm and 243.6 nm for lisinopril and at 280.1 nm and 270.8 nm for hydrochlorothiazide. In Vierordt's method, A¹ ₁ (1 %, 1 cm) values of lisinopril and hydrochlorothiazide were determined at 259.8 nm and 272.7 nm in the zero-order spectra. The quantity of both compounds were calculated by using the A¹ ₁ (1 %, 1cm) values. The methods were successfully applied to a pharmaceutical formulation for determination of both active compounds.     

UV-Spectroscopic Determination of Mixtures of Tetramethrin and Piperonyl Butoxide in Pharmaceutical Formulations

Abstract

A simple rapid and accurate UV-spectroscopic method have been developed for determination of tetramethrin in presence of piperonyl butoxide, which are present in Licid^R, a newly introduced pharmaceutical drug in Egypt used as antilice, and antiscopis. The method is applicable in the concentration range of 1–12 μg.ml^?1 and 1–50 μg.ml^?1 for tetramethrin and piperonylbutoxide respectively. Average recoveries for tetramethrin and piperonyl butoxide in Licid^R spray and Licid^R lotion are 98.14 ± 0.3 – 103.88 ± 1.88 (Tetra), 103.78 ± 1.23 (piperonyl) and 100.62 ± 0.89 – 100.94 ± 1.10 (Tetra), 102.38 ± 1.02 (piperonyl) for the spray and lotion, respectively.     

Spectrophotometric Determination of Trace Amounts of Cobalt and Copper with 3- (2′-Thiazolylazo)- 2,6- Diaminopyridine

Abstract

Sensitive methods for the determination of trace amounts of cobalt and copper by complexation with 3-(2′-Thiazolylazo)-2,6- diaminopyridine (2,6-TADAP) are described. Copper forms a 1:2 violet complex with the reagent having a molar absorptivity of 1.00 × 10⁴ L mol^?1cm^?1, Baer's law is obeyed over the range 0 ?50.84 μg in the total volume of 10ml. Cobalt also forms a 1:1 green complex with a molar absorptivity of 1.07 × 10⁴L mol^?1cm^?1 and obeying Beer's law over the range 0 –23.57 μg in the total volume of 10 ml. The procedure is simple and rapid without any tedious extraction steps for copper and without oxidation of cobalt (II) to cobalt (III).     

Flow Injection Analysis of Pharmaceutical Compounds. VI. Determination of Some Central Nervous System Acting Drugs by UV-Spectrophotometric Detection

Abstract

The Present work describes a direct flow injection analysis (FIA) of five commonly used central nervous system (CNS) acting drugs namely amitriptyline hydrochloride, carbamazepine, clomipramine hydrochloride, fluphenazine hydrochloride and imipramine hydrochloride. The characteristics of the system and the conditions of the speatrophotometric determination are evaluated. The proposed technique can be applied for pharmaceutical quality control of the pure material and pharmaceutical dosage forms containing the drug. Amount ranging from 16 to 80 μg. ml^?1 of amitriptyline hydrochloride.

The Present work describes a direct flow injection analysis (FIA) of five commonly used central nervous system (CNS) acting drugs namely amitriptyline hydrochloride, carbamazepine, clomipramine hydrochloride, fluphenazine hydrochloride and imipramine hydrochlorode. The characteristics of the system and the conditions of the spectrophotometric determination are evaluated. The proposed technique can be applied for pharmaceutical quality control of the pure material and pharmaceutical dosage forms containing the drug. Amount ranging from 16 to 80 μ.ml^?1 of amitriptyline hydrochloride, carbamazepine and fluphenazine hydrochloride and from 32 to 160 μ. ml^?1 of clomipramine hydrochloride and imipramine hydrochloride dissolved and/or extracted in ethanol could be accurately analyzed. Standard addition (0.5 to 3 times of the claimed amounts) of authentic samples to powdered tablets gave good mean percent recoveries with low standard deviations. Samples can be introduced at rates of about 180 per hour or even more. The results obtained by applying the proposed FIA method are statistically analyzed and compared with those obtained from applying pharmacopoeial procedures.     

Spectrophotometric and Fluorimetric Methods for the Determination of Methoxamine Hc1 in Bulk Drugs and in Ampoules

Abstract

Three simple and sensitive methods for the determination of methoxamine HCl in bulk drugs and in ampoules were proposed. The methods are based on the oxidation of methoxamine HCl by sodium periodate, potassium permanganate and cerium(IV)sulphate. The first two reactions are followed spectrophotometrically by measuring the absorbance at 352 &; 608 nm for the periodate and permanganate methods, respectively. The third method is based on measuring the relative fluorescence intensity of Ce(III)arising from Ce(IV) at 348 nm with excitation wavelength at 257 nm. The different experimental parameters were carefully studied. Under the described conditions the proposed methods were applicable over the concentration ranges 10.0 - 40.0, 2.0-10.0 and 0.05-0.30 μg ml^?1 for the three methods, respectively.     

RAYLEIGH LIGHT SCATTERING ENHANCING REACTION OF DIBROMOCHLOROARSENAZO AND PROTEINS SYSTEM AND ITS ANALYTICAL APPLICATION

Based on the enhancement effects of Rayleigh light scattering (RLS) on Arsenazo-DBC, a novel quantitative method for the determination of proteins in aqueous solutions has been proposed. The reaction of Dibromochloroarsenazo (Arsenazo-DBC) and five proteins (BSA, HSA, egg albumin, human γ-IgG, Lysozyme) has been studied. Under optimal conditions the dynamic ranges for proteins were 2.5–60.0 μg·ml^?1, and the detection limits for HSA and BSA were at 98.50 ng·ml^?1 and 88.10 ng·ml^?1, respectively. Comparing with other methods, the method is simple, practical and relatively free from interference from coexisting substances. The method was employed for the determination of total protein in human serum with satisfactory results.     

New fluorimetric reagents, sodium pyrophosphate, sodium trimetaphosphate, and sodium tetrametaphosphate, for the determination of cerium(III)

Three sensitive and selective new alternatives for fluorometric determination of cerium(III) are described in this study. Ce(III) is highly fluorescent in sodium pyrophosphate, sodium trimetaphosphate, and sodium tetrametaphosphate solutions. For these reagents, the maximum excitation/emission wavelengths are 300/350, 297/340, and 299/352 nm, respectively. Maximum fluorescence intensities are obtained by irradiating Ce(III) dissolved in 0.033 g L⁻¹ sodium pyrophosphate, 41.4 g L⁻¹ sodium trimetaphosphate, and 0.96 g L⁻¹ sodium tetrametaphosphate at room temperature. The fluorescence intensities are linear over the range 0.001–30, 0.001–75, and 0.001–70 μg ml⁻¹. The detection limits are calculated as 9.5 × 10⁻³, 1.1/10⁻³, and 3.8 × 10^-3 μg ml⁻¹ Ce(III), respectively. The relative standard deviations for 15/0.05 Μg ml⁻¹ Ce(III) are 1.1/1.2, 1/1.1, and 1.2/1.3%, respectively. Quenching effects of other lanthanides and some inorganic anions were investigated. The methods have been applied to rare earth mixtures with a good accuracy.     

Spectrophotometric Determination of Cobalt with Di-2-Pyridyl Ketone Benzoylhydrazone

Abstract

A method for the spectrophotometric determination of cobalt (II) by complexation with di-2-pyridyl ketone benzoylhydrazone (DPKBH) in 50% (v/v) ethanolic solution is described. Cobalt (II) forms a 1:2 complex with DPKBH. The complex has maximum absorbance at 370 nm. Beer's law is obeyed over the range 0.1 – 2.8 μg.ml^?1. The effect of pH, effect of excess reagent, stability of the complex and the tolerance limit of many metal ions have been reported. The method is applied to the determination of cobalt in different alloys containing other metals ions.     

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.     

Spectrophotometric Determination of Lead with 2-(5-Bromo-2-pyridylazo)-5-diethylaminophenol and Cetyltrimethylammonium Bromide

Abstract

A new spectrophotometric method was employed for the determination of lead (II) based on the ternary complex formation with 2-(5-Bromo-2-Pyridylazo)-5-diethylaminophenol(5-BrPADAP) and cetyltri-methyl-ammonium bromide (CTAB). At pH 7.00 a violet ternary complex, whose molar absorptivity is 5.1×10⁴ 1.mole^?1 cm^?1 at 575 nm, is formed. Beer's law range (0.5 ? 4.9 μg ml^?1 of lead), the apparent stability constant (log β=9.90) and δG° were evaluated. A large number of ions do not interfer at pH 7.00 because they form complexes with 5-Br-PADAP at higher pH's (< 9.40) or at lower pH's (> 4.86). The method offers the advantages of simplicity and requires no extraction.     

Determination of Trace Bismuth by a Solid Substrate Room Temperature Phosphorescence Quenching Method Based on Anionic Polymeric Acryclic Acid Lead Particles Containing Luminescent Eosine Molecules

Abstract

Luminescent particles of Anionic Polymeric Acryclic Acid Lead (Pb(PAA)₂) which containing eosine(HFInBr₄), Eosine nanomicroball of anionic polypropylene acid lead contained luminophores (short for E.N.PAA.L.C.L), were synthesized by a sol‐gel method, using anionic polymeric acryclic acid sodium (PAANa) as the precursor and Pb²⁺ as the precipitant. NH₄Ac‐HAc can react with the Pb²⁺ in E.N.PAA.L.C.L, causing it to decompose into aqueous soluble components. E.N.PAA.L.C.L‐ NH₄Ac‐HAc can emit strong and stable solid substrate room temperature phosphorescence (SS‐RTP) on filter paper, and bismuth, mercury or iodine can cause a decrease in phosphorescence intensity. Based on the facts above, a new method for the determination of trace bismuth by an SS‐RTP quenching method was established. The linear range of this method was 0.01–0.20(pg spot^?1) (4.0×10^?12 g ml^?1) of Bi³⁺, with a detection limit (LD) of 0.0016 pg spot^?1, and the regression equation of the working curve was ΔIp=61.01+237.8 m_Bi3+ (pg spot^?1), r=0.9992. This method was applied to the determination of trace bismuth in human hair and well water samples with satisfactory results. The mechanism of SS‐RTP emission was also discussed.     

A setup for synchrotron‐radiation‐induced total reflection X‐ray fluorescence and X‐ray absorption near‐edge structure recently commissioned at BESSY II BAMline

An automatic sample changer chamber for total reflection X‐ray fluorescence (TXRF) and X‐ray absorption near‐edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF‐XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml^?1 to µg ml^?1). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NIST water 1640. Low limits of detection of less than 100 fg absolute (10 pg ml^?1) for Ni were found. TXRF‐XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state.     

Radiochelatometric Determination of Lead

This paper deals with radiochelatometric determination of lead. 10^?3M EDTA solution,, Dowex 50 W-X2 cation exchanger and Zn⁶⁵ radionuclide were used as the titrant, for the separation of components, and as the non-isotopic indicator, respectively. The method, the procedure, and the results obtained are described. In this way 0·33–1·40 μg-equ. of lead was determined in model solutions. The method cal also be used to determine submicrogram amounts of lead.     

Computational study on structures,thermochemical properties,and bond energies of disulfide oxygen (S–S–O)‐bridged CH3SSOH and CH3SS(=O)H and radicals

Cleavage of disulfide bonds is a common method used in linking peptides to proteins in biochemical reactions. The structures, internal rotor potentials, bond energies, and thermochemical properties (Δ_fH°, S°, and Cp(T)) of the S–S bridge molecules CH₃SSOH and CH₃SS(=O)H and the radicals CH₃SS?=O and C?H₂SSOH that correspond to H‐atom loss are determined by computational chemistry. Structure and thermochemical parameters (S° and Cp(T)) are determined using density functional Becke, three‐parameter, Lee–Yang–Parr (B3LYP)/6‐31++G (d, p), B3LYP/6‐311++G (3df, 2p). The enthalpies of formation for stable species are calculated using the total energies at B3LYP/6‐31++G (d, p), B3LYP/6‐311++G (3df, 2p), and the higher level composite CBS–QB3 levels with work reactions that are close to isodesmic in most cases. The enthalpies of formation for CH₃SSOH, CH₃SS(=O)H are ?38.3 and ?16.6 kcal mol^?1, respectively, where the difference is in enthalpy RSO–H versus RS(=O)–H bonding. The C–H bond energy of CH₃SSOH is 99.2 kcal mol^?1, and the O–H bond energy is weaker at 76.9 kcal mol^?1. Cleavage of the weak O–H bond in CH₃SSOH results in an electron rearrangement upon loss of the CH₃SSO–H hydrogen atom; the radical rearranges to form the more stable CH₃SS· = O radical structure. Cleavage of the C–H bond in CH₃SS(=O)H results in an unstable [CH₂SS(=O)H]* intermediate, which decomposes exothermically to lower energy CH₂ = S + HSO. The CH₃SS(=O)–H bond energy is quite weak at 54.8 kcal mol^?1 with the H–C bond estimated at between 91 and 98 kcal mol^?1. Disulfide bond energies for CH₃S–SOH and CH3S–S(=O)H are low: 67.1 and 39.2 kcal mol^?1. Copyright © 2011 John Wiley & Sons, Ltd.     

Break-Through Investigation on Uranium Isotope Separation in the System Uranyl Ion Solution Ti(III)-Cationic Resin

A break-through experiment on separation of uranium isotopes was carried out by use of a cation-exchange resin in Ti(III) form. By analyzing the experimental results the apparent equilibrium constants of the order K = 1·00021–1·00034 were determined.

The maximum value on the experimental curies of the isotopic ratio versus effluent volume was interpreted by considering two antagonistic isotope effects: one relatively large given by an exchange reaction between U(IV) in resin and U(VI) in solution and another smaller given by the reduction reaction of U(VI) with Ti(III). The difference of the equilibrium constants of the these two isotope effects as a function of temperature was used for the determination of the apparent thermodynamic values of the resultant process, determined experimentally: ΔH⁰ = 0.8542 cal mol^?1 and ΔS⁰ = 3.33×10^?3cal°K^?1.     

Electronic and Resonance Raman Spectra of the μ-tris(Bipyrazine)ruthenium(II)-Hexaquis{ruthenium(II)EDTA} Supramolecular Complex

Abstract

Resonance Raman and electronic spectra of the μ-tris(bipyrazine)ruthenium(II)-hexaquis{ruthenium(II)EDTA} supramolecular complex are reported in this paper. Excitation in the 457–676 nm range leads to the selective enhancement of the Ru-bipyrazine vibrational peaks according to distinct patterns, supporting the assignment of the absorption bands at 670 and 490 nm as charge-transfer (MLCT) transitions from the [Ru^IIEDTA] d_π orbitals to the π₁? and π₂? LUMO levels of the bipyrazine ligand. A vibronic coupling mechanism involving the two excited states is suggested for the excitation at 490 nm. The occurrence of MLCT transitions in the [Ru(bpz)₃]²⁺ central unity, around 440 nm, is supported by the Raman and fluorescence excitation profiles.     

Electrical and structural studies of a LiBOB-based gel polymer electrolyte

A series of gel polymer electrolytes (GPEs) containing lithium bis(oxalato)borate (LiBOB), propylene carbonate (PC), and ethylene carbonate (EC) have been investigated. Poly(ethylene oxide) (PEO) was used as the polymer. First, a series of liquid electrolytes was prepared by varying the Li:O ratio and obtained the best composition giving the highest conductivity of 7.1?×?10^?3 S cm^?1 at room temperature. Then, the PEO-based GPEs were prepared by adding different amounts of LiBOB and PEO into a mixture of equal weights of EC and PC (40 % of each from the total weight). The gel electrolyte comprises of 12.5 % of LiBOB, 7.5 % of PEO, 40 % of EC, and 40 % of PC gave the highest ionic conductivity of 5.8?×?10^?3 S cm^?1 at room temperature. From the DC polarization measurements, ionic nature of the gel electrolyte was confirmed. Fourier transform infrared (FTIR) spectra of electrolytes showed the Li⁺ ion coordination with EC and PC molecules. These interactions were exhibited in the peaks corresponding to ring breathing of EC at 893 cm^?1 and ring bending of EC and symmetric ring deformation of PC at 712 and 716 cm^?1 respectively. The presence of free Li⁺ ions and ion aggregates is evident in the peaks due to the symmetric stretching of O–B–O at 985 cm^?1.     

CdTe quantum dots as fluorescence sensor for the determination of aminophylline in aqueous solution

A novel CdTe quantum dots (QDs) based technology platform was established in aqueous solution. It can perform accurate and simple determination of aminophylline concentration in pharmaceutical samples with satisfactory results. Under optimum conditions, the relative fluorescence intensity of CdTe quantum dots is linearly proportional aminophylline concentration from 2.00 to 80.0 μg mL^?1 with a correlation coefficient of 0.9979 for aminophylline determination and a detection limit of 0.531 μg mL^?1.     

The nature of the effect of Gd(III) on fluorescence of Ln(III) chelates in water solutions

The intensity of fluorescence of Eu(III) and Sm(III) ions sensitized by molecules of n-benzoyltrifluoroacetone and 1,10-phenanthroline introduced in a water solution in a ratio of 3: 1 is studied as a function of the ion concentration in the solution. The comparison of the fluorescence decay curves of Eu(III) and Sm(III) in D₂O and H₂O (pH≥7) solutions containing 10^?4 M of n-Cl-BTFA and 3×10^?5 M of 1,10-phen and the values of τ_fl of Sm(III) in themselves (51–90 μs) are indicative of an insignificant content of water molecules in the first coordination sphere of ions. The effect of other ions on I _fl and τ_fl of Eu(III) ions is studied under these conditions. The intensity of fluorescence of Eu(III) in solutions of 10^?4 M Cl-BTFA and 3×10^?5 H 1,10-phen is found to increase by 1–2 orders of magnitude in the presence of Y(III) and Gd(III) ions, and the magnitude of this effect is unaffected by deoxygenation of the solution. The introduction of a third ion Nd(III) in the solution is shown to attenuate the influence of Gd(III) on I _fl of Eu(III) for Nd(III) concentrations commensurable with the Eu(III) concentration in the solution. The strength of the influence of Gd(III) ions on I _fl of Eu(III) is found to depend on the method of preparation of the solution. The analysis of the results obtained testifies that inhomogeneities consisting of chelates of lanthanide ions displaced from the water structure appear in water. The presence of these inhomogeneities results in efficient energy transfer from ligands of Gd(III) chelates to Eu(III) chelates, which is the reason for the increasing I _fl of Eu(III). The possibility of using data on the enhancement of I _fl of Eu(III) in the presence of Gd(III) and on the reduction of τ_fl of Eu(III) in the presence of Nd(III) for estimating dimensions and structures of displaced systems is discussed.     

A Spectrophotometric Method for the Determination of Buclizine Hydrochloride Using the Charge-Transfer Spectrum of Buclizine-Iodine Complex

Abstract

A simple and sensitive spectrophotometric method is described for the determination of buclizine hydrochloride in bulk and tablets form. The method is based on the formation of charge-transfer complex between buclizine, as n-donor, and iodine, as Δ acceptor, which measured spectrophotometrically at 295 and 355 nm. A Job's plot indicated a 1:1 complex between the drug and iodine and Beer's law was obeyed in a concentration range of 4–30 μg ml^?1. A more detailed investigation of the complex was made with respect to its association constant and the free energy change. The method is simple and sensitive and has been applied successfully to the analysis of laboratory-made tablets without any interference from the tablet excipients. To validate the method, the results obtained were compared statistically with a newly developed uv-derivative spectrophotometric method. The charge-transfer method was favored due to its higher sensitivity, cheap coast and available equipments.