A Fluorimetric Method for the Determination of Atmospheric Sulphur Dioxide With 2′, 7′—Dichlorofluorescein∗

Abstract

A rapid, simple and sensitive fluorimetric method has been developed for the determination of atmospheric sulphur dioxide with dichlorofluorescein as fluorogenic reagent (λ_ex = 505 nm, λ_em = 520 nm) at pH 4.0–6.0. A linear calibration curve was obtained in the range 0.01–0.40 μg SO₂/25 ml. The detection limit is 0.01 μg SO₂/25 ml. Nitrogen dioxide does not interfere with the method. The method was successfully applied to the determination of atmospheric sulphur dioxide.

     

Spectrophotometric determination of clozapine in pharmaceuticals

New Spectrophotometric methods for the assay of clozapine (CZP) in pure and dosage forms are described. Method A is based on the oxidative coupling reaction of CZP with 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) in the presence of ceric ammonium sulphate to form a coloured species (_max 570 nm). Method B is also based on the oxidative coupling reaction of CZP withP-,N,N-dimethylpheny-lenediamine dihydrochloride (DMPD) in the presence of sodium hypochlorite to form a coloured species (_max 690 nm). Method C is based on the formation of coloured charge-transfer complex between CZP and chloranilic acid (_max 540 nm). Regression analysis of Beer-Lambert plots showed good correlation in the concentration ranges 2–25, 10–120 and 15–300 g/ml for methods A, B and C, respectively. The validity of the proposed methods was tested by analysing pharmaceutical dosage forms containing CZP and the relative standard deviation values were within 1.0%.     

Assay of cisapride in pharmaceutical formulations by visible spectrophotometry

Three spectrophotometric methods (A-C) for the assay of cisapride (CPD) in pure and dosage forms are described. Method A is based on the oxidative coupling reaction of CPD with 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) in the presence of ferric chloride to form a coloured species (_max; 565 nm.) Method B is based on the oxidation of CPD with Fe (III) and subsequent chelation of Fe(II) to form a coloured complex with 1,10-phenanthroline (_max: 520 nm). Method C is based on the formation of a coloured charge-transfer complex between CPD and chloranilic acid (_max; 555 nm). Regression analysis of Beer-Lambert plots showed good correlation in the concentration ranges 2.0–32.0, 0.4–6.4 and 25.0–450.0 g/ml for methods A,B and C, respectively. The validity of the proposed methods was tested by analysing pharmaceutical dosage forms containing CPD and the relative standard deviations were within 1.0%     

Extraction-Spectrophotometric Determination of Arsenic in Environmental Samples with Iodide and Amidines

Abstract

A simple and rapid method for the spectrophotometric determination of traces of total arsenic present in industrial waste waters is described. It is based on the reaction of As(III) with I^? in 5 –6 M HCl, and extraction of the iodo-arsenite complex formed into chloroform with amidines. The molar absorptivity of AsI₄ ^? with 11 different amidines is in the range (3.9 –7.9) × 10³ lmol^?1 cm^?1 at λ_max = 380 –395 nm; the simplest compound, N,N′-diphenylbenzamidine (DPBA) has been chosen for further studies. The limit of detection with DPBA is 0.1 μg As/ml. The method is highly selective with almost no interference from all anions and cations tested.     

A Fluorimetric Method for the Determination of Cyanide with Fluorescein and Iodine∗

Abstract

A rapid, simple and sensitive fluorimetric method has been developed for the determination of cyanide with fluorescein as fluorogenic reagent (λ_ex = 494 nm, λ_em = 514 nm) at pH 6.0–7.0. A linear calibration curve was obtained in the range 0.004–2.0 μg CN^?/25 ml. The detection limit is 0.004 μg CN^-/25 ml. The method was successfully applied to the determination of cyanide in waste water.

     

Extract-Photometric Determination of Vanadium with Isophthaldihydroxamic Acid

Abstract

The spectrophotometric study of violet complex isophthaldihydroxamic acid-vanadium extracted into solution of trioctylmethylammonium chloride in ethylacetate was made (λ_max = 380 nm, ? = 7500 l.mol^?1.cm^?1; λ_max = 510 nm, ? = 5510 l.mol^?1 .cm^?1; stoichiometries, 1:1 and 1:2, V:reagent). A new method for the extract-spectrophotometric determination of V(V) in the range 14–80 μg of vanadium is proposed.     

A Fluorescence Quenching Method for the Determination of Iodide Ion with Salicylfluorone and Hydrogen Peroxide

Abstract

A highly sensitive and selective fluorescence quenching method has been developed for rapid determination of iodide ion with salicylfluorone (SAF) as fluorogenic reagent (λ_ex = 495 nm, λ_em = 520 nm) at pH 2.5-3.0. The calibration graph is linear over the range 0.05-300 μg/25 ml. The detection limit is 0.05 μ/25 ml iodide. Other halide ions do not interfere with the determination even when present in large excess. The method is rapid and was successfully applied for the determination of iodide ion in sodium chloride, table salt and low sodium salt.     

Utility of Derivative Spectrophotometry in the Determination of Carbochromen Hydrochloride and Dipyridamole in the Presence of Their Oxidative Degradation Products

Abstract

Direct spectrophotometric methods for the determination of carbochromen hydrochloride and dipyridamole, each in the presence of its oxidative degradation products, are presented. the methods are based on the first derivative (D₁) and second derivative (D₂) spectrophotometric measurement (absolute trough, U) at 336 nm and (Peak-trough, Y) at 309–342 nm for carbochromen hydrochloride and at 240–260 nm(U) and 246–268 nm(Y) for dipyridamole. Plots of D₁ or D₂ versus concentration were linear over the concentration range of 8.00–16.00 μg/ml for carbochromen hydrochloride and 4.00–12.00 μg/ml for dipyridamole. Oxidative degradation of these drugs has been optimized with respect to hydrogen peroxide concentration. Determining the intact in coexistence with its oxidative degradation product, the proposed derivative spectrophotometric methods proved to be of high potential in correcting the systematic error appearing in the results of the A_max method due to the latter. Assaying the commercial tablets, the proposed method gave results of high accuracy and reproducibility.     

Spectrophotometric Determination of Trimethoprim in Pure Form and in Pharmaceutical Preparations using Bromothymol Blue,Bromocresol Green and Alizarin Red S

ABSTRACT

Simple, sensitive and selective methods for the determination of trimethoprim (TMP) in pure form and in pharmaceutical formulations are described. The methods are based on the reaction of TMP as a π-electron donor with bromothymol blue (BTB), bromocresol green (BCG) and alizarin red S (ARS) as electron acceptors. The coloured products are quantified spectrophotometrically at their corresponding λ_max.

Beer's law is obeyed in case of BTB in the range 2.9-23.2 μg/ml (CHCl₃), 2.9-20.0 μg/ml (CH₂Cl₂) and 5.0-29.0 μg/ml (ClC₆H₅), in the case of BCG 2.9-27.5 μg/ml (H₂O/alc.), 2.9-18.3 μg/ml (CHCl₃) and 2.9-20.3 μg/ml (CH₂Cl₂) and for ARS in the range 3.0-12.0 μg/ml in H₂O/alc medium.

The specific absorptivities, molar absorptivities, Sandell sensitivities, standard deviations and percent recoveries are evaluated. Application of the suggested methods to dosage forms is presented and compared with the pharmacopoeial method. The interference from additives and sulfa compounds, especially sulfamethoxazole, has been overcome by extraction into chloroform or methylene chloride.     

Comparison of activities of homogeneous Ti-based catalysts in the presence of methylaluminoxane (MAO) for synthesis of syndiotactic polystyrene by UV/visible spectroscopic study

The catalytic activities in syndiospecific polymerization of styrene in hydrocarbon using homogeneous Ti-based catalysts in the presence of methylaluminoxane (MAO) were investigated through UV/visible spectroscopic analysis. A strong UV absorption band of CpTiCl₃, itself, incipiently appeared at λ_max = 400 nm in toluene, followed by a bathochromic shift with its remarkable decrease by the addition of MAO. The absorption band intensity at λ_max = 400 nm arising from delocalization of π-electrons on the cyclopentadienyl ring decreased by methylation in the presence of MAO with regard to the mechanism for production of an active center (“cation-like”), for example, the change of the ionic nature. The intensity decrease at λ_max = 400 nm was suppressed over 2000 of the [Al]/[Ti] ratio. In the case of Ti(OC₄H₉)₄ having a σ-ligand, new and broad UV absorption bands were developed at λ_max = 340 nm and 410 nm in the presence of MAO in contrast with the CpTiCl₃/MAO system. Comparison between the relative absorption intensities at λ_max = 340 nm and 410 nm led to the determination of a maximum catalytic activity of Ti(OC₄H₉)₄ in the presence of MAO related to the polymerization yield. The maximum polymerization yield was observed with regard to the relative maximum value of the absorption intensity at λ_max = 410 nm with the [Al]/[Ti] ratio (500). From observation for polymorphism of the final products via differential scanning calorimetric analysis (DSC), the thermally unstable β-form seemed to be produced by the CpTiCl₃/MAO system independent of the MAO concentration, the Ti(OC₄H₉)₄/MAO system produced a thermally stable α-form in the low MAO concentration (up to 100 of the [Al]/[Ti] ratio), and a mixture of α- and/or β-forms over 200 of the [Al]/[Ti] ratio under our experimental conditions. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1733–1741, 1998     

Spectrophotometric determination of mebeverine hydrochloride

Three simple, sensitive and reproducible visible spectrophotometric methods (A-C) for the determination of mebeverine hydrochloride (MVH) in bulk samples and pharmaceutical formulations are described. Methods A and B are based on the formation of ion-association complexes between the drug and fast green FCF (FGFCF, _max 625 nm) or bromothymol blue (BTB, _max 405 nm). Method C is based on the formation of a molecular complex between the drug and cobalt thiocyanate (CTC, _max 625 nm). Regression analysis of Beer's plots showed good correlation in the concentration ranges 2–40, 2–25 and 100–600 g/ml for methods A, B and C respectively. No interference was observed from the usually existing additives in pharmaceutical formulations and the applicability of the methods was examined by analysing tablets containing MVH. Standard deviations were typically 0.75 mg per dose (RSD: 0.25–0.5%). Recoveries were 99.0–100.2%.     

Spectrophotometric estimation of microgram amounts of sodium N-chloro-p-toluenesulfonamide (chloramine-T) and sodium N-chlorobenzenesulfonamide (chloramine-B)

A novel ultraviolet spectrophotometric method for the assay of microgram amounts (1–80 μg/ml) of CAT and CAB in aqueous solution has been developed. The method is highly sensitive, simple, and rapid within the limits of the experimental conditions described. The present method is also applicable for the determination of these two compounds present in a mixture since they have identical λ_max and nearly the same ξ_mmax. The ultraviolet spectra of the compounds have been presented and the values of λ_max and ξ_ax are reported.     

Spectrophotometric Determination of Certain Local Anaesthetics in Pharmaceutical Preparations

Abstract

A direct colorimetric method was described for the rapid, sensitive and accurate determination of dibucaine, lidocaine, bupivacaine, procaine and tetracaine in pharmaceutical preparations. The method involves the use of haematoxylin reagent in the presence of boric acid to give a reddish-violet chromogen (λ_max = 555 nm). Beer's law was obeyed in the range from 2–60 μg/ml. No interference was observed from the commonly present additives or agents in pharmaceutical formulations.     

The Stabilization of Small Concentrations of Formaldehyde in A queous Solutions

Abstract

Based on the Hantzsch-reaction, a stabilization (fixation) of small concentrations of formaldehyde in aqueous solutions (<0.4μg CH₂0/ml) can be performed, allowing a storage of these solutions for 1 week at room temperature, in darkness. Using the fluorescent nature of 3,5-diacetyl-1,4-dihydrolutidine (λ_ex = 410 nm, λ_em = 510 nm), formed as a result of the Hantzsch-reaction, CH₂0-concentrations down to 0.02 μ/ml can be determined fluorimetrically up to 7 days after preparation (sampling).     

Spectrophotometric Method of Determination for Cycloserine Using Chlornil

Abstract

Cycloserine has been determined by a spectrophotometric method based on n → charge-transfer complex formation with chloranil. The method involves addition of cycloserine solution to chloranil reagent in borate buffer of pH 9; and heating at 65°C for 45 min. The complex formed exhibits absorption maximum of 348 nm; and A_max is linearly related to concentration over the range 2–8 μg/ml. The mean percentage found for the authentic sample is 100.32 ± 0.70. When applied to commercial capsules claimed to contain 250 mg each, the mean percentage found is 102.45 ± 1.05. These results have shown good agreement when compared with those obtained by the pharmacopoeial (B.P.) methods.     

A Fluorescence Synergistic Method for the Determination of Stilboestrol

Abstract

A simple, highly sensitive and selective fluorescence synergistic method has been developed for rapid determination of stilboestrol with Triton × — 100 (λ_ex = 318nm, λ_em = 415nm) at pH 8.80 ～ 10.20. The calibration graph is linear over the range of 0.0 ～ 30.0μg/10ml. The detection limit is 0.03μg/ml stilboestrol. The method has been successfully applied for the determination of stilboestrol in tabellae stilboestrol and injectio stilboestrol with satisfactory results. It can also be applied for the determination of stilboestrol in body fluid of special patients.     

New water-soluble hydrogen donors for the enzymatic spectrophotometric determination of hydrogen peroxide

Eight N -alkyl-N-V-sulphopropylaniline derivatives have been synthesized and assessed as water-soluble hydrogen donors for the spectrophotometric determination of hydrogen peroxide in the presence of peroxidase. The sodium salts of N-ethyl-N-sulphopropylaniline (ALPS), N-ethyl-N-sulphopropyl-m-toluidine (TOPS) and N -ethyl-N-sulphopropyl-m-anisidine (ADPS) are recommended. They have excellent water solubilities, and the optimum pH range for oxidative condensation with 4-aminoantipyrine in the presence of hydrogen peroxide and peroxidase is 5.5–9.5. The absorbances of the resulting chromogens are 2–3 times higher than that achieved with phenol. The molar absorptivities of the chromogens with 4-aminoantipyrine are 41300 (ALPS, λ_max 561 nm), 37400 (TOPS, λ_max 550 nm) and 27900 (ADPS, λ_max 540 nm). Calibration graphs for the determination of hydrogen peroxide in the presence of a control serum are linear for 7–40 × 10^-6 mol H₂O₂ l^-1.     

Pulse radiolysis studies of styrene

We have applied the pulse radiolysis technique of studying short-lived, radiation-produced intermediates to a study of pure, dry liquid styrene. We have observed at least three distinct species. The most rapidly decaying species (τ1/2 = 4 μsec., λ_max ≈ 370 mμ) exhibits an apparent first-order decay which is slowed down in the presence of dry oxygen, occurs too rapidly to be measured in the presence of water, and has a temperature coefficient of approximately 1 kcal./mole between 25 and 45°C. We have tentatively identified the species as the styryl anion with a G value for formation of approximately 0.15. A second species (τ1/2 = 220 μsec. λ_max ≈ 320–330 mμ) exhibits a first-order decay which appears to be independent of oxygen and water. From its spectrum, we have tentatively identified it as the styryl radical. The third species (λ_max ≈ 310 and 320 mμ) is relatively stable in the dark, but is radily photolyzed by the analyzing light of the usual experimental set-up for pulse radiolysis studies. The formation of this species appears to be independent of the water and oxygen content of the styrene.     

Four spectrophotometric methods for determination of nitrofurazone in pharmaceutical formulations

Four simple and sensitive visible spectrophotometric methods (A-D) for the determination of nitrofurazone in bulk samples and pharmaceutical formulations are described. They are based on the formation of colored species by treating either its reduction product with 3-methylbenzothiazolin-2-one hydrazone in the presence of ferric chloride (method A: _max 600 nm) or its hydrolysis product with thiobarbituric acid (method B: _max 520 nm, 440 nm) or barbituric acid (method C: _max 400 nm) or by oxidizing it with excess N-bromosuccinimide and determining the consumed NBS using metol-isonicotinic acid hydrazide (method D: _max 620 nm).     

Time-resolved emission studies of poly(n-v1nyl carbazole) using pulsed laser excitation

Time-resolved fluorescence spectroscope of poly(N-vinyl carbazole) in tetrahydrofuran solution has revealed the presence of three emitting species, namely a normal excimer emitting at λ_max = 420 nm, a higher-energy excimer site at λ_max = 370 nm which interconverts with the “normal” site, and a third species which emits at 370 nm but not at 420 nm. and which does not convert to the normal excimer. The identity of this species, and the kinetics of fluorescence of the polymer, are discussed.