Â Objectives: Two simple, sensitive and economic spectrophotometric methods are developed for the determination of desvenlafaxine in pure and itspharmaceutical formulations.Methods: The developed methods are based upon the reaction of oxidative coupling of desvenlafaxine with 3-methyl-2-benzthiazolinonehydrazone(MBTH) (Method A) and 2, 2' bipyridyl (Method B) in the presence of ferric chloride. The colored complex produced was measured at 663 nm,522 nm for method A and B respectively against the reagent blank. The optimum experimental parameters for the color productions areselected.Results: Beer's law is valid within a concentration range of 20-100 Î¼g/ml and 5-25 Î¼g/ml and for method A, B respectively. The percentage recoverieswere found in the range of 99.47Â±0.1789 for method A and 100.08Â±0.144 for method B. The limit of detection and limit of quantification were foundto be 0.825 Î¼g/ml and 2.5 Î¼g/ml respectively for method A and 0.1061 Î¼g/ml and 0.321 Î¼g/ml for method B respectively.Conclusion: The developed methods are applied for the determination of desvenlafaxine in bulk and its pharmaceutical formulations without anyinterference from excipients.Keywords: Spectrophotometric, Desvenlafaxine, Oxidative coupling, 3-methyl-2-benzthiazolinone hydrazone, 2, 2- bipyridyl, FeCl3

Chandan Rs

Gurupadayya Bm

Sreeja U

Objectives: Two simple, sensitive and economic spectrophotometric methods are developed for the determination of desvenlafaxine in pure and its pharmaceutical formulations. Methods: The developed methods are based upon the reaction of oxidative coupling of desvenlafaxine with 3-methyl-2-benzthiazolinonehydrazone (MBTH) (Method A) and 2, 2 ’ bipyridyl (Method B) in the presence of ferric chloride. The colored complex produced was measured at 663 nm, 522 nm for method A and B respectively against the reagent blank. The optimum experimental parameters for the color productions are selected. Results: Beer’s law is valid within a concentration range of 20-100 μg/ml and 5-25 μg/ml and for method A, B respectively. The percentage recoveries were found in the range of 99.47±0.1789 for method A and 100.08±0.144 for method B. The limit of detection and limit of quantification were found to be 0.825 μg/ml and 2.5 μg/ml respectively for method A and 0.1061 μg/ml and 0.321 μg/ml for method B respectively

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NOVEL SPECTROPHOTOMETRIC METHODS FOR THE QUANTIFICATION OF DESVENLAFAXINE IN PURE AND PHARMACEUTICAL DOSAGE FORM

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Vol 8, Issue 2, 2015 ISSN - 0974-2441NOVEL SPECTROPHOTOMETRIC METHODS FOR THE QUANTIFICATION OF DESVENLAFAXINE IN PURE AND PHARMACEUTICAL DOSAGE FORMSREEJA U, GURUPADAYYA BM*, CHANDAN RSDepartment of Pharmaceutical Analysis, JSS College of Pharmacy, JSS University, Mysore - 570 015, Karnataka, India. Email: bmgurupadayya@jssuni.edu.inReceived: 14 January 2014, Revised and Accepted: 03 February 2015ABSTRACTObjectives: Two simple, sensitive and economic spectrophotometric methods are developed for the determination of desvenlafaxine in pure and its pharmaceutical formulations.Methods: The developed methods are based upon the reaction of oxidative coupling of desvenlafaxine with 3-methyl-2-benzthiazolinonehydrazone (MBTH) (Method A) and 2, 2’ bipyridyl (Method B) in the presence of ferric chloride. The colored complex produced was measured at 663 nm, 522 nm for method A and B respectively against the reagent blank. The optimum experimental parameters for the color productions are selected.Results: Beer’s law is valid within a concentration range of 20-100 μg/ml and 5-25 μg/ml and for method A, B respectively. The percentage recoveries were found in the range of 99.47±0.1789 for method A and 100.08±0.144 for method B. The limit of detection and limit of quantification were found to be 0.825 μg/ml and 2.5 μg/ml respectively for method A and 0.1061 μg/ml and 0.321 μg/ml for method B respectively.Conclusion: The developed methods are applied for the determination of desvenlafaxine in bulk and its pharmaceutical formulations without any interference from excipients.Keywords: Spectrophotometric, Desvenlafaxine, Oxidative coupling, 3-methyl-2-benzthiazolinone hydrazone, 2, 2- bipyridyl, FeCl3.INTRODUCTIONDesvenlafaxine is chemically, 4-[2-(dimethylamino)-1-(1-hydroxycyclohexyl) ethyl] phenol succinate hydrate (Fig. 1). It is an antidepressant of the serotonin-nor epinephrine reuptake inhibitor class. Desvenlafaxine is a synthetic form of the isolated major active metabolite of venlafaxine and is grouped as a serotonin nor epinephrine reuptake inhibitor [1]. Literature survey reveals some methods for quantitative analysis of desvenlafaxine. The methods adapted to the analysis of desvenlafaxine include high-performance liquid chromatography (LC) [2-5], spectrophotometric [6-12], LC-ultraviolet (UV) and LC-mass spectrometry [13]. The present study describes simple, rapid, accurate and reproducible methods for the estimation of desvenlafaxine in tablet formulation.2, 2 bi-pyridyl and 3-methyl-2-benzthiazolinonehydrazone (MBTH) have been used as derivatizing reagent for the spectrophotometric determination of many pharmaceutical amines [14,15]. However, the reaction of MBTH reagent and 2, 2 bi-pyridyl with desvenlafaxine has not been investigated so far. The present study describes the evaluation of 2, 2-bipyridyl and MBTH as derivatizing reagents in the development of simple and fast spectrophotometric method for the determination of desvenlafaxine in its pharmaceutical dosage forms.METHODSEquipmentA shimadzu UV-visible spectrophotometer model 1800 with 1 cm matched quartz cell was used for the absorbance measurements. The systonics electronic balance was used for weighing the samples.Reagents and solutionsAll employed chemicals were of analytical grade and distilled water was used throughout the experiment. Desvenlafaxine pure sample was obtained as a gift sample from R L FINE Chemicals, Bengaluru, India.MBTH 0.5% (w/v)0.5 g of MBTH reagent was accurately weighed transferred into a 100 ml calibrated volumetric flask, dissolved in distilled water, and made up the volume to the mark to obtain a solution of 0.5% (w/v).2, 2’bi-pyridyl 0.2% (W/V)200 mg of 2,2’ bi pyridyl reagent was accurately weighed transferred into 100 ml calibrated volumetric flask, dissolved in distilled water, made up the volume to the mark to obtain 0.2% (w/v).Ferric chloride (1%)It was prepared by dissolving 1 g of ferric chloride in 100 ml of distilled water.Standard solutionsDesvenlafaxine stock solution (1000 μg/ml) was prepared by dissolving 100 mg of drug in 100 ml of methanol. Working solutions of the drug were prepared by dilution of the stock solution. The marketed tablets form of desvenlafaxine used in the determination was with a labeled strength of 50 mg.Research ArticleFig. 1: Chemical structure of desvenlafaxineAsian J Pharm Clin Res, Vol 8, Issue 2, 2015, 267-270 Sreeja et al. 268Analytical method developmentMethod AStandard solutions of desvenlafaxine in methanol, having final concentrations in the range of 20-100 μg/ml were transferred into a series of 10 ml volumetric flasks. To each 2 ml of MBTH, 2 ml of ferric chloride was added, and the volume was made up to mark with distilled water and allowed to stand for 20 minutes. The absorbance of each solution was measured at 663 nm against the reagent blank. The colored species was stable for 2 hrs and the amount of drug in the sample was computed from its calibration curve represented in Fig. 2. Overlain spectrum was represented in Fig. 3.Method BIn method B, different aliquots of stock reference solution (1000 μg/ml) from 5 to 25 μg/ml were transferred into a series of 10 ml standard flasks. To each flask 0.5 ml of ferric chloride and 1.5 ml of 2,2’ bi-pyridyl were added and kept in a water bath (60±1°C) for 15 minutes, then immediately cooled to room temperature (25±1°C) using a cold water. The absorbance of each solution was measured at 522 nm against the reagent blank. The amount of drug in the sample was computed from its calibration curve represented in Fig. 4 and overlain spectrum was represented in Fig. 5.QuantificationThe limits of the Beer’s law, the molar absorptivity and the Sandell’s sensitivity values were evaluated and are given in Table 1. Regression analyses of the Beer’s law plots at their respective λmax values revealed a good correlation. Graphs of absorbance versus concentration showed zero intercepts and are described by the regression equation, y=bx+c (where y is the absorbance of a 1 cm layer, b is the slope, c is the intercept and x is the concentration of the drug in μg/ml) obtained by the least-squares method. The results are summarized in Table 1.Procedure for analysis tabletsTwenty tablets were weighed accurately and ground into a fine powder. An amount of powder equivalent to 10 mg of desvenlafaxine was weighed and transferred in to a 100 ml volumetric flask, 50 ml of the distilled water was added and sonicated for 15 min, then the volume was made up to the mark with the same solvent, mixed well and filtered using a Whatman filter paper No. 41. The assay of the tablets was carried out according to the general procedure.Fig. 3: Overlay linearity spectra of desvenlafaxine (method A)Fig. 4: Calibration curve of desvenlafaxine (method B)Fig. 5: Overlay linearity spectra of desvenlafaxine (method B)Fig. 2: Calibration curve of desvenlafaxine (method A)Table 1: Optical characteristics and validation data of desvenlafaxineParameters Method A Method Bλmax 663 nm 522 nmLinearity (µg/ml) 20-100 5-25Regression coefficient 0.967 0.9745Wave length 663 nm 522 nmLOD (µg/ml) 0.825 0.1061LOQ (µg/ml) 2.5 0.321Molar absorptivity (L/mol/cm) 1.0535×103 5.1095×103Sandell’ sensitivity (mg cm−2 per absorbance unit)0.1470 A.U 0.02840 A.ULOD: Limit of detection, LOQ: Limit of quantificationAsian J Pharm Clin Res, Vol 8, Issue 2, 2015, 267-270 Sreeja et al. 269RESULT AND DISCUSSIONAnalytical method validationRecovery studies were performed by adding a known amount of standard drug (80%, 100% and 120%) to pre-analyzed sample and contents were reanalyzed by proposed method. The other validation parameter like precision (interday, intraday) were also studied (ICH Q2B). The results of validation studies for estimation of desvenlafaxine are presented in Tables 2-4.The method developed for spectrophotometric determination of desvenlafaxine in tablet formulation was found to be simple and convenient for the routine analysis. Beer-lambert’s law was obeyed in the concentration range of 20-100 μg/ml for method A and 5-25 μg/ml proves methods are sensitive. Coefficient of variation was found to be 0.967 for method A and 0.974 for method B. The percentage recoveries were found in the range of 99.47±0.1789 for method A and 100.08±0.144 for method B. The method was found to be precise with % relative standard deviation ± (0.203%) for the interday precision and ± (0.203%) for intraday for method A and ± (0.210%) for interday precision and ± (0.156%) for intraday precision. The limit of detection and limit of quantification were found to be 0.825 μg/ml and 2.5 μg/ml respectively for method A and 0.1061 μg/ml and 0.321 μg/ml for Method B respectively.CONCLUSIONThe reagents utilized in the proposed methods are cheap, readily available, and the procedures do not involve any critical reaction conditions or tedious sample preparation. Moreover, the methods are free from interference by common additives and excipients. The wide applicability of the new procedures for routine quality control was well established by the assay of des venlafaxine in pure form and in pharmaceutical preparations.ACKNOWLEDGMENTSThe authors express their sincere thanks to R L FINE Chemicals, Bengaluru, India for supplying the gift samples of desvenlafaxine. Authors also extend their thanks to the Principal, JSS College of Pharmacy, Mysore for providing the facilities to carry out the present work.REFERENCES1. Liebowitz MR, Yeung PP, Entsuah R. A randomized, double-blind, placebo-controlled trial of desvenlafaxine succinate in adult outpatients with major depressive disorder. J Clin Psychiatry 2007;68(11):1663-72.2. Rohith T, Ananda S. Quantification of potential impurities by a stability indicating HPLC method in desvenlafaxine succinate monohydrate active pharmaceutical ingredient. Int J Res Pharm Chem 2012;2(4):947-56.3. Pingle RK, Salunkhe K. Chaudhari S. RP-HPLC method development and validation of desvenlafaxine succinate monohydrate in tablet dosage form. World J Pharm Res 2014;3(6):657-74.4. Mallikarjuna R, Kishore AN, Kumar BP, Sukhen S. Method development Table 2: Recovery studies of desvenlafaxine for method AS.No Amount of drug taken (µg/ml)Amount of drug addedTotal amount of drug (µg/ml)Total amount of drug found% Recovery % RSD1. 40 20 60 59.5 99.1 0.27959.75 99.5859.5 99.1Mean±SD 99.26±0.2772. 40 40 80 79.5 99.37 0.17992679.5 99.3779.75 99.68Mean±SD 99.47±0.17893. 40 60 100 99.5 99.5 0.14494199.5 99.599.75 99.75Mean±SD 99.58±0.1443RSD: Relative standard deviationTable 3: Recovery studies of desvenlafaxine for method BS.No Amount of drug taken (µg/ml)Amount of drug added (µg/ml)Total amount of drug (µg/ml)Total amount of drug found% Recovery % RSD1. 10 5 15 15 100.00 0.328915.05 100.3315.10 100.66Mean±SD 100.33±0.332. 10 10 20 20 100.00 0.144220.05 100.2520 100.00Mean±SD 100.08±0.1443. 10 15 25 24.57 98.28 0.140824.63 98.5224.57 98.28Mean±SD 98.36±0.1385RSD: Relative standard deviationTable 4: Method precision data of desvenlafaxine for method A and BConcentration (µg/ml) Parameters Intraday InterdayMethod A40 SD 0.000548 0.000548% RSD 0.203237 0.203237Method B40 SD 0.000408 0.000548% RSD 0.156918 0.210258RSD: Relative standard deviationAsian J Pharm Clin Res, Vol 8, Issue 2, 2015, 267-270 Sreeja et al. 270and validation for the simultaneous estimation of desvenlafaxine and clonazepam in bulk & tablet formulation by RP-HPLC method. Indian J Res Pharm Biotech 2013;1(4):525-32.5. Moussa BA, El-Bagary RI, Al-Eryani YA. Development and validation of a stability-indicating HPLC method for the analysis of desvenlafaxine succinate in the presence of its acidic induced degradation product in bulk and pharmaceutical preparation. J Chem Pharm Res 2011;3(5):425-37.6. Ankit S, Ujiwal S, Ashim kumar S, Dhanya BS, Seth AK. Development and validation of UV spectrophotometric method for estimation of desvenlafaxine succinate ER-tablets form. Asian J Pharm Health Sci 2011;1(3):137-41.7. Abirami G, Logesh R, Vetrichelvan T. Spectrophotometric method for estimation of desvenlafaxine succinate in tablet dosage form. Res J Pharm Bio Chem Sci 2011;2(2):721-9.8. Anand A, Dubey SK. New sensitive and validated spectrofluorimetric method for the estimation of desvenlafaxine succinate in bulk and in pharmaceutical formulations. World J Pharm Sci 2014;2(2):196-202.9. Mansing GP, Kumar BS, Bonde CG, Gurmeet SC. UV spectrophotometric method development for the determination of desvenlafaxine succinate in tablet formulation. Bull Pharm Res 2011;1(1):40-3.10. Dole MN, Amit SM, Sangeeta C, Sanjay DS. Development and validation of analytical methods for estimation of desvenlafaxine succinate in bulk and solid dosage forms by UV spectroscopy. Pharm Chem 2013;5(5):270-3.11. Keval LC, Rujuta DP, Dilip GM. Absorption correction spectrophotometric method for simultaneous estimation of desvenlafaxine and clonazepam in their combined dosage form. Der Pharm Lettre 2014;6(2):61-8.12. Krupa MP, Jayant BD. Development and validation of UV spectrophotometric method for simultaneous estimation of desvenlafaxine and clonazepam in tablet dosage form. Int J Pharm Res Bio-Sci 2014;3(3):87-96.13. Shubhangi MP, Laxman DK, Sathish YG, Sunil RD. LC-UV and LC-MS evaluation of stress degradation behavior of desvenlafaxine. J Pharm Anal 2012;2(4):264-71.14. Sowjanya K, Thejaswini JC, Gurupadayya BM, Indupriya M. Spectrophotometric determination of pregabalin using Gibb’s and MBTH reagent in pharmaceutical dosage form. Der Pharm Chem 2011;3(1):112-22.15. Nagaraju P, Pasumarthy, Gopal NV, Srinivas VD, Padma SV. Spectrophotometric methods for the determination of atorvastatin calcium in pure and it’s pharmaceutical dosage forms. Asian J Res Chem 2008;1(2):64-6.

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NOVEL SPECTROPHOTOMETRIC METHODS FOR THE QUANTIFICATION OF DESVENLAFAXINE IN PURE AND PHARMACEUTICAL DOSAGE FORM

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