Titrimetric and Spectrophotometric Determination of Some Phenothiazine Psychotropics in Pure Form and in Pharmaceutical Formulations with Metavanadate

 Two simple, fast, accurate and precise methods for the determination of six phenothiazines and a number of their pharmaceutical formulations are described. The titrimetric method involves the oxidation of the drugs by metavanadate in sulphuric acid medium and titration of vanadium(IV) formed, with cerium(IV) using ferroin indicator and acetone as catalyst. In spectrophotometry, vanadium(IV) formed was reacted with ferriin and the resulting ferroin measured at 510 nm. Phenothiazines in the ranges 5–100 mg and 2.5–25.0 μg mL⁻¹ can be determined by titrimetry and spectrophotometry, respectively, with detection limits of 0.96–2.05 mg and 0.0359–0.0565 μg mL⁻¹, respectively. Both methods were applied successfully to the determination of the studied drugs in pharmaceutical preparations. The reliability of the assays was established by parallel determination by the official methods of British Pharmacopoeia and the results being statistically evaluated. Received September 26, 2000. Revision March 25, 2001.     

Second-Derivative Spectrophotometric Determination of Some Benzenoid Drugs

Abstract

A rapid second-derivative spectrophotometric assay procedure has been described for the determination of some benzenoid drugs in pharmaceutical dosage forms. Spectral interference from formulation excipients in simple uv spectrophotometric methods has been eliminated by the application of the proposed method. The different assay parameters, linearity and precision of the method have been assessed. The assay results obtained for eight batches of the pharmaceutical formulations of these drugs are in accord with the declared amounts. The high specificity, ease and simplicity offered by second-derivative spectrophotometry permit unit dose assay of these formulations.     

Difference spectrophotometric determination of some pharmaceutically important thioxanthene derivatives in dosage forms

A Spectrophotometric method is described for the rapid determination of four thioxanthene derivatives, namely chlorprothixene, thiothixene, flupenthixol hydrochloride and clopenthixol hydrochloride. The method is based on measuring the first derivative spectrum (D ₁) of the oxidized drug relative to a solution of the underivatized drug. At the wavelength of maximum difference in first derivative (range 285–315 nm), only the oxidation products have an appreciable difference in first derivative and the oxidizing agent has no absorbance. The oxidation products (assumed to be the thioxanthone sulphoxides) are formed rapidly at room temperature by the addition of peroxyacetic acid, prepared by the slow reaction of hydrogen peroxide and glacial acetic acid. The first derivative of the absorbance is proportional to the concentration of the drugs in solution over the ranges 2–14 g ml^–1 for chloroprothixene, 2–20 g ml^–1 for clopenthixol hydrochloride, 2–24 g ml^–1 for thiothixene and 4–40 g ml^–1 for flupenthixol hydrochloride. The method is specific for the intact drug and can be adopted in the presence of oxidative and photochemical decomposition products and tablet excipients. The recoveries ranged from 99.7 ± 1.3 to 100.2 ± 1.5%. The validity of the method was tested by analysing synthetic samples of thioxanthenes and some dosage forms containing the drugs; the results were in accordance with those given by the official methods.     

Spectrophotometric Determination of Chlorpromazine and Levomepromazine Hydrochlorides In Injectables and Drops By Reaction With Ferric Ion

Abstract

The principal aim of this research was the standardization of a spectrophotometric method using the reaction with ferric ion for quantitative determination of these substances in pharmaceutical preparations. By reaction with ferric ion chlorpromazine gave a pink compound with maximum absorption at 525 nm. the violet product obtained by the reaction with ferric ion and levomepromazine had a maximum at 565 nm. Beer's law was obeyed in a wide range of concentrations for both compounds. the method was applied to simulated and commercially available samples. the efficiency of the method was confirmed by recovery tests.     

Extraction-spectrophotometric determination of some antihistaminic agents with fast green FCF

A rapid, simple, precise, accurate and highly sensitive method for the determination of some antihistaminic agents such as dimethindene maleate (DMM), embramine hydrochloride (EMH), isothipendyl hydrochloride (IPH), mebhydrolin napadisylate (MHn), methdilazine hydrochloride (MDH), promethazine hydrochloride (PMH), trimeprazine tartrate (TMT) and triprolidine hydrochloride (TPH) in bulk samples and pharmaceutical preparations is proposed. The method is based on the formation of a chloroform-soluble ion-association complex between the antihistaminic agent and Fast Green FCF at pH 5.0 with an absorption maximum at 620 nm. The composition of antihistaminic agent and Fast Green FCF in each ion-association complex is studied. The relative standard deviation of the proposed method is less than 1.3%, the percent recovery is 99.4–100.2% and the results are not significantly different from the standard methods at the 95% confidence level.     

Spectrophotometric Determination of Some Phenolic Antibiotics in Dosage Forms

 A simple and sensitive spectrophotometric method is described for the determination of some phenolic antibiotics namely: cefadroxil, amoxicillin and vancomycin. The method is based on the measurement of the orange yellow species produced when the drugs are coupled with diazotized benzocaine in triethylamine medium. The method is applicable over the range of 0.8–12 μg/ml for cefadroxil, 2–16 μg/ml for amoxicillin and 2–18 μg/ml for vancomycin. The formed compounds absorb at 455 nm for both cefadroxil and amoxicillin and at 442 nm for vancomycin. The proposed method has detection limits of 0.018 μg for cefadroxil, 0.0034 μg for amoxicillin and 0.0156 μg for vancomycin. The stoichiometric ratio for the studied compounds was found to be 1:1 and a proposal of the reaction pathway was made. The proposed method was applied for the analysis of the cited drugs in their pharmaceutical preparations. The results are in good agreement with those obtained by the official methods. Received February 7, 2000. Revision June 14, 2000.     

Determination of Some Phenothiazine Drugs Based on Colour Reaction with Potassium Periodate

ABSTRACT

A simple, rapid and sensitive method for the determination of six phenothiazine drugs, either in pure form or in pharmaceutical formulations, is described. The method is based on the formation of stable phenothiazine free radical by the use of potassium periodate as the chromogenic reagent in sulphuric acid medium. The reaction is suggested to proceed via oxidation of the phenothiazine nucleus into a semiquinonoid radical. The wavelengths of maximum absorption range from 500 to 525nm. Molar absorptivities range from     

Spectrophotometric Determination of Trace Amounts of Ascorbic Acid

Abstract

Colourless silver-gelatin complex is quantitatively reduced by ascorbic acid to yellow silver sol in water within the pH range 7.5–10.0 at room temperature. The determination of 1–10μg/ml of ascorbic acid is possible at 415 nm in the presence of glycine, alanine, fructose, sucrose, citric, tartaric, oxalic, malic, succinic acids and also in the presence of various reducing agents. The molar absorptivity of ascorbic acid at the δ_max is found to be 21500 lit mol^?1 cm^?1 and the Sandell sensitivity of the sol is 8.18x10^?3 μg ascorbic acid cm^?2 for 0.001 absorbance. The relative standard deviation is ±0.22% and the confidence limit (20 determinations, 95%) being 8.806±0.0093%.     

Determination of 1,4-benzodiazepines in drug dosage forms by difference spectrophotometry

A spectrophotometric method has been developed for the determination of seven 1,4-benzodiazepines, namely: chlordiazepoxide, diazepam, nitrazepam, oxazepam, lorazepam, temazepam and cinolazepam. The method involves reduction of the target compounds using Zn/HCl and measuring the difference in the absorbance before and after reduction. The quantities of zinc and acid required for efficient reduction were carefully studied. 1–20 g ml^–1 of the compounds could be determined with < 1% error. The method was applied successfully to the determination of these compounds in pharmaceutical dosage forms. The results were sufficiently accurate and precise and comparable to those from the official methods.     

Fluorimetric Determination of Certain Phenothiazine Derivatives Using Eosin

Abstract

Eosin reacts with phenothiazine derivatives in dichloroethane to give intense fluorescent compounds having their excitation maximum at 318 nm and emission maxima at 450, 460 and 465 nm for prochlorperazine dimaleate, thiethylperazine dihydrochloride and trifluoperazine dihydrochloride, respectively. Under the optimum conditions, samples of 1-10 μg ml^?1 could be determined rapidly with coefficient of variation less than 1.8 %. This fluorescence reaction was also applied successfully to the determination of phenothiazine drugs in some pharmaceutical preparations.     

Spectrophotometric method for assay of penicillins

Ninhydrin in 0.2M citrate buffer (pH 5) containing SnCl₂ is proposed as a new reagent for Spectrophotometric determination of penicillins and analysis of their pharmaceutical formulations. The method is based on acid hydrolysis of penicillins with 5M HCl and subsequent treatment with ninhydrin. The resulting violet colour exhibits maximum absorption at 570 nm.     

Colorimetric Determination of Some N-Substituted Phenothiazine Derivatives Using 2-Iodoxybenzoate

Abstract

A new, sensitive colorimetric method has been described for the quantitative determination of six N-substituted phenothiazines. the method depends on the formation of stable phenothiazine free radical by the use of 2-iodoxybenzoate as chromogenic reagent. the drug in 50% sulphuric acid is treated with reagent (5×10^?4 M). the produced red or purple color possesses characteristic absorption maximum for each of the drugs tested. Beer's law is obeyed over the concentration range 2-30 μg.ml^?1 with apparent molar absorptivities ranging from 9.4-12.4×10^?3 for the studied phenothiazine derivatives. the average % recovery is 99.5±0.96 - 101.6±1.01. the method was applied successfully to the microdetermination of promazine. HCl, chlorpromazine, HCl, promethazine. HCl, perphenazine, levomepromazine HCl and mesoridazine besylate either in pure form or incorporated in their representative pharmaceutical preparations. the stoichiometry of the reaction was assumed and a reaction mechanism was suggested. the precision of the assay was comparable with the official ones.     

Direct Synthesis of Nitriles from Aldehydes Using Chloramine-T/KI in Aqueous Ammonia

A convenient method for direct conversion of aldehydes into nitriles has been developed using chloramine-T/KI in aqueous ammonia.

[Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications® for the following free supplemental resource: Full experimental and spectral details.]     

吩噻嗪和吩噁嗪氧化中间体的共振喇曼光谱研究

本文对吩噻嗪和吩噁嗪的单电子氧化产生的两种氧化态的亚稳态正离子进行了共振喇曼光谱研究。随着吩噻嗪的p电子逐步失去, 结构变形振动δ_(CNC)和δ_(CSC)的喇曼频移显著地增大, 环C=C伸缩振动区域的喇曼峰数目明显变多。由此推断, 随着吩噻嗪正离子氧化态的增高, 正离子转变成平面共轭结构。     

A Comparative Study on Spectrophotometric,Conductometric and Potentiometric Determination of Ascorbic Acid

Abstract

A comparison has been made on the selectivity, accuracy and precision of spectrophotometric, conductometric and potentiometric methods for the determination of ascorbic acid in water which is based on the reduction of gold(III) ion by ascorbic acid. Gold(III) ion forms a complex with gelatin in alkaline medium which on reduction with ascorbic acid produces coloured gold sol. The sol shows an absorption maximum at 540 nm with molar absorptivity of 2.3×10^?3litre mol^?1 cm^?1 and the Sandell's sensitivity of 7.6 × 10^?2 μgcm^?2. The relative standard deviation is 0.22% and the confidence limit (20 determinations, 95%) is 2.0 ± 0.009%. To examine the extent of sensitivity of the spectrophotometric method the proposed method is compared with the sensitivities of the conductometric and potentiometric methods.     

主成分分析-紫外光谱法同时测定四种维生素B

采用主成分分析法(PCA)完成对多组分样品分析的建模及解析研究,用于处理紫外光谱数据,实现了维生素B_1、B_2及B_6及烟酰胺四组分的同时测定,结果可靠,操作简便。     

Spectrophotometric Determination of Cefadroxil and Metyrosine in Dosage Forms

Abstract

A simple and sensitive spectrophotometric method is described for the determination of cefadroxil and metyrosine in pure form and in pharmaceutical formulations. The method is based on reacting these drugs with 4-aminoantipyrine (AAP) in the presence of an alkaline oxidising agent. The coloured products were measured spectrophotometrically at 500 nm and 470 nm for cefadroxil and metyrosine, respectively. Beer's law was obeyed over the concentration range 1-28 and 2-44 μg ml^-1 for cefadroxil monohydrate and metyrosine, respectively. The molar ratio in both cases was established and a proposal for the reaction pathway was suggested. The percentage recoveries obtained were in accordance with those given by the reference methods.     

Spectrophotometric assay of cephalosporins in pharmaceutical products,using chromotrope 2B and chromotrope 2R

A simple, rapid and sensitive Spectrophotometric method is proposed for the determination of cephadroxil (I), cephalexin (II) and cephradine (III). The method is based on ion-pair complex formation between these derivatives and Chromotrope 2B (C2B) or Chromotrope 2R (C2R), to give a highly coloured radical anion. The coloured products are quantified spectrophotometrically at 542 and 564 nm for C2B and C2R, respectively. The optimization of the experimental conditions is described. The method has been used for the determination of 0.4–15, 0.4–14 and 0.4–18 g/ml of drugs I, II and III, respectively. The accuracy of the method is indicated by the excellent recovery (100.0±1.7%) and the precision is supported by the low relative standard deviations 1.5%. The sensitivity of the method is discussed and the results are compared with the official method. The interference from common degradation products and excipients was also studied. The proposed method was applied successfully to the determination of the different cephalosporins in dosage forms, with good precision and accuracy. The results were compared with those given by the official B.P. 1993 method.     

Interactions of Human Serum Albumin with Phenothiazine Drugs: Insights from Fluorescence Spectroscopic Studies

This study was based on the use of fluorescence quenching and differentiation between static and dynamic quenching, as well as energy transfer for distance measurements. The interactions of human serum albumin with phenothiazine drugs, i.e. phenothiazine, chlorpromazine, perphenazine and promethazine, were studied and extrapolated important information on quenching mechanism, types of interaction force, binding‐site number and distance between Trp214 in HSA and the bound drugs. This study has great significance in methodology and understanding the protein‐drug interaction mechanism.     

Spectrophotometric Determination of Ceftazidime in Pharmaceutical Preparations Using Neocuproin as a Complexing Agent

Abstract

A simple and reproducible spectrophotometric method for the assay of ceftazidime with neocuproin-copper(II) reagent has been developed. The procedure is based on the drug in an acidic medium, subsequent formation of yellow ternary complex in citrate buffer solution (pH 4.2), and measurement at 454 nm. Beer's law is obeyed in the range 15.0–40.0 µg mL^?1 with correlation coefficient r ² = 0.9995. The procedure holds good accuracy and precision when applied to the analysis of ceftazidime in powder for injection with good recovery percent ranging from 100.17±1.0 without interference from additives.