Spectrofluorimetric determination of certain biologically active phenothiazines in commercial dosage forms and human plasmaby Abdel-Maaboud I. Mohamed, Osama H. Abdelmageed, Hesham Salem, Dalia M. Nagy, Mahmoud A. Omar



Chemistry (miscellaneous) / Biophysics


Fluorimetric Determination of Certain Phenothiazine Derivatives Using Eosin

N. A. Zakhari, M. Rizk, M. I. Walash, F. Ibrahim

Biological and immunological characterization of inhibin forms in human plasma.

D Robertson, H G Burger, J Sullivan, N Cahir, N Groome, E Poncelet, P Franchimont, T Woodruff, J P Mather


Spectrofluorimetric determination of certain othiazines in ms and human plasma

H b,d c a m dr alo rovide a deep yellow to brown colour with green florescence. d a ucc ed dit in res s, L alo these drugs requires the development of simple, rapid, accuhydrochloride and promethazine hydrochloride were supplied by Misr

Research article

Accepted: 30 April 2012 Published online in Wiley Online Libraryrate, sensitive, applicable and less expensive methods for their determination in pure and dosage forms. As a result, this study describes a simple and very sensitive spectrofluorimetric method for the determination of these drugs based on the presence of a tertiary amine moiety. The use of a mixed anhydride system [malonic acid/acetic anhydride (MAA)] in the present work made the proposed method highly specific to the analysis of tertiary amine bases as well as amine salts without interference of primary, secondary or quaternary amines.


Co. for Pharmaceutical Industries, Alexandria, Egypt; trifluperazine hydrochloride supplied by El-Kahira Co., Cairo, Egypt; thioridazine hydrochloride supplied by Novartis Pharma S.A.E., Cairo, Egypt; perazine maleate supplied * Correspondence to: Mahmoud A. Omar, Analytical Chemistry Department, faculty of Pharmacy, Minia University, Minia, Egypt. E-mail: momar1971g@yahoo.com a Pharmaceutical Analytical Chemistry Department, faculty of Pharmacy,

Assiut University, Assiut, Egypt b Pharmaceutical Chemistry Department, Faculty of Pharmacy, King Abdulaziz

University, Jeddah, Kingdom of Saudi Arabia cIntroduction

Phenothiazines such as chlorpromazine hydrochloride, promethazine hydrochloride, trifluperazine hydrochloride, thioridazine hydrochloride, perazine maleate and oxomemazine are commercially available psychoactive drugs extensively used in Egypt in a variety of pharmaceutical formulations as tablets or ampoules (1). Several methods have been published for the determination of these drugs in bulk or in different pharmaceutical formulations as well as in biological fluids. These methods include volumetric methods (2–4), spectroscopy (5–13), electrochemical methods (14–16), flow injection spectrophotometry (17,18), flow injection spectrofluorimetry (19–21), chromatography (22–28), capillary electrophoresis (29) and immunoassay (30). The wide use of

WINLAB™ software with slide width of 10 nm. A spectronic GENESYS™ 2PC Ultraviolet visible spectrophotometer (Milton Roy Co, Westhaven,

USA) withmatched 1-cm quartz cell connected to an IBM computer loaded with WinSpec™ application software was used for all measurements. Other instruments used included a Jenway 5056 ultraviolet–visible spectrophotometer (Bibby Scientific Limited, Staffordshire, U.K.); anMLW type thermostatically controlled water bath (LabexchangeW, Burladingen, Germany); an

AG 29 digital analytical balance ( Meltter Toledo, Glattbrugg, Swizerland); a

Milwaukee SM 101 pHmeter (Milowaukee, Szeged, Hungary) and a 4000c/s laboratory centrifuge (Germany).


Pharmaceutical compounds used in this study included chlorpromazinebiologically active phen commercial dosage for

Abdel-Maaboud I. Mohameda, Osama

Dalia M. Nagyd and Mahmoud A. Om

ABSTRACT: A validated simple and sensitive spectrofluorimetric hydrochloride, promethazine hydrochloride, trifluperazine hy oxomemazine. The method was based on condensation of m the tertiary amine moiety of the studied phenothiazines to p

Relative fluorescence intensity of the products was measure the reaction were studied and optimized. The method was s in commercial dosage forms. The lower detection limits allow compounds in plasma as an example of a biological fluid. In ad of tertiary amines in the presence of primary and secondary am the cited drugs in the presence of their degradation products sulphoxides or sulphones. Copyright © 2012 John Wiley & Son

Keywords: spectrofluorimetric determination; phenothiazines; mReceived: 27 November 2011, Revised: 28 April 2012, (wileyonlinelibrary.com) DOI 10.1002/bio.2388Apparatus

A PerkinElmerW LS 45 luminescence spectrometer (PerkinElmerW, Waltham,

MA, USA) was used connected to an IBM PC computer loaded with FL

Luminescence 2012 Copyright © 2012 Johnt lexc 398 nm and lem 432 nm. Different variables affecting essfully applied for the determination of the studied drugs the application of this method for the determination of the ion, the method was considered specific for the determination es; as a result, it was deemed suitable for the determination of ulting from N-dealkylation or oxidation of the corresponding td. nic acid; acetic anhydride; dosage forms; plasma. Abdelmageed , Hesham Salem , rd* ethodwas developed for the determination of chlorpromazine ochloride, thioridazine hydrochloride, perazine maleate and nic acid/acetic anhydride (MAA) under the catalytic effect ofPharmaceutical Analytical Chemistry Department, faculty of Pharmacy,

MSA University, Cairo, Egypt d Analytical Chemistry Department, faculty of Pharmacy, Minia University,

Minia, Egypt

Wiley & Sons, Ltd. concentration of 500–6000ng/mL. Next, the general procedure was followed as described for calibration under general procedure using the prepared sample solution instead of the standard working solutions.

A volume of promethazine HCl or oxomemazine equivalent to 5mgwas transferred to a 100-mL separating funnel contained~20mL distilled water and the aqueous layer was rendered alkaline by addition of 33% w/v aqueous ammonia solution and the liberated phenothiazine base was extracted with three volumes of 15mL of chloroform. The chloroformic extract was filtrated through anhydrous Na2SO4 supported on filter paper. The obtained filtrate was evaporated to dryness using a rotary evaporator. The residue was dissolved in ~ 15mL methanol and the resultant solution was transferred into a 50-mL volumetric flask and completed to volume with the same solvent. The final solution was diluted to obtain working standard solutions in the general concentration range of 500–6000 ng/mL. Next, the general procedure was followed as described for calibration under general procedure using the prepared sample solution instead of the standard working solutions.