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Stability indicating RP-HPLC estimation of nebivolol hydrochloride in pharmaceutical formulations  [cached]
Shah D,Bhatt K,Mehta R,Baldania S
Indian Journal of Pharmaceutical Sciences , 2008,
Abstract: A simple, specific, accurate and stability indicating reversed phase liquid chromatographic method was developed for the determination of nebivolol hydrochloride in tablet dosage forms. A phenomenex Gemini C-18, 5 mm column having 250x4.6 mm i.d., with mobile phase containing methanol: acetonitrile: 0.02 M potassium dihydrogen phosphate (60:30:10, v/v/v; pH 4.0) was used. The retention time of nebivolol hydrochloride was 2.6 min. The linearity for nebivolol hydrochloride was in the range of 0.2-10 mg/ml. The recovery was found to be in the range of 98.68-100.86%. The detection limit and quantification limit were found to be 0.06 mg/ml and 0.2 mg/ml, respectively. Nebivolol stock solutions were subjected to acid, alkali and neutral hydrolysis, chemical oxidation and dry heat degradation. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time values. The proposed method was validated and successfully applied to the estimation of nebivolol hydrochloride in tablet formulations.
Stress Degradation Behavior of Paliperidone, an Antipsychotic Drug, and Development of Suitable Stability-Indicating RP-LC Method  [PDF]
Sanjay A. Jadhav,Shashikant B. Landge,Pramod M. Choudhari,Pavankumar V. Solanki,Saroj R. Bembalkar,Vijayavitthal T. Mathad
Chromatography Research International , 2011, DOI: 10.4061/2011/256812
Abstract: A new, simple, rapid, and stability-indicating reversed phase liquid chromatographic (RP-LC) method for the determination of both assay and related substances in paliperidone has been developed and validated. During the forced degradation at hydrolysis, oxidative, photolytic, and thermal stressed conditions, the degradation was observed in the oxidative and acid stress conditions. Five process-related impurities (Imp-A to Imp-E) in test sample of paliperidone have been detected using newly developed RP-LC method. Among the five, Imp-C and Imp-D were found to be degrdants. Good resolution between the peaks corresponding to degradation and process-related impurities from the analyte was achieved on a Hypersil BDS C18 ( 2 5 0 × 4 . 6 ?mm, 5?μm) column. The stress samples were assayed against a qualified reference standard, and the mass balance was found to be close to 99.0%. The method was validated as per ICH guideline and was found to be robust. The proposed RP-LC method was successfully applied to the analysis of commercial formulation and was found to be specific and selective. 1. Introduction Paliperidone, a major metabolite of risperidone (9-hydroxy-risperidone), has been approved by the FDA for the treatment of schizophrenia since 2006. Paliperidone is a centrally active dopamine D2 and serotinergic 5-HT 2 A antagonist. It is also active as an antagonist at α1 and α2 adrenergic receptors and H1-histaminergic receptors. Paliperidone has one chiral centre but as the pharmacological profiles of the racemate and the two enantiomers are similar with respect to in vitro binding assays, in vitro receptor occupancy studies and in vivo functional interaction studies, hence, it is marketed in its racemic mixture [1–8]. Paliperidone is chemically designated as (±)-3-[2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethyl]-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4Hpyrido[1,2-a]pyrimidin-4-one (Figure 1). It corresponds to the molecular formula, C23H27FN4O3, and its relative molecular mass is 426.49. The development of an accurate and efficient analytical method to determine the quality of the product is a critical activity during the process development of the product in generic companies as process is either improved continuously with the use of new reagents, intermediates, and so forth, or route of synthesis itself changes some time. During the study of synthetic process in our laboratory, we discovered five process-related impurities, namely, Imp-A, Imp-B, Imp-C, Imp-D, and Imp-E among them two impurities (Imp C and Imp D) were found to be
Development and Validation of a Stability-Indicating RP-HPLC Method for the Simultaneous Estimation of Guaifenesin and Dextromethorphan Impurities in Pharmaceutical Formulations  [PDF]
Thummala V. Raghava Raju,Noru Anil Kumar,Seshadri Raja Kumar,Annarapu Malleswara Reddy,Nittala Someswara Rao,Ivaturi Mrutyunjaya Rao
Chromatography Research International , 2013, DOI: 10.1155/2013/315145
Abstract: A sensitive, stability-indicating gradient RP-HPLC method has been developed for the simultaneous estimation of impurities of Guaifenesin and Dextromethorphan in pharmaceutical formulations. Efficient chromatographic separation was achieved on a Sunfire C18, 250?×?4.6?mm, 5?μm column with mobile phase containing a gradient mixture of solvents A and B. The flow rate of the mobile phase was 0.8?mL min?1 with column temperature of 50°C and detection wavelength at 224?nm. Regression analysis showed an r value (correlation coefficient) greater than 0.999 for Guaifenesin, Dextromethorphan, and their impurities. Guaifenesin and Dextromethorphan formulation sample was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, and photolytic degradation. Guaifenesin was found stable and Dextromethorphan was found to degrade significantly in peroxide stress condition. The degradation products were well resolved from Guaifenesin, Dextromethorphan, and their impurities. The peak purity test results confirmed that the Guaifenesin and Dextromethorphan peak was homogenous and pure in all stress samples and the mass balance was found to be more than 98%, thus proving the stability-indicating power of the method. The developed method was validated according to ICH guidelines with respect to specificity, linearity, limits of detection and quantification, accuracy, precision, and robustness. 1. Introduction Guaifenesin (GN), (+)-3-(2-methoxyphenoxy)-propane-1,2-diol, is a widely used expectorant, useful for the symptomatic relief of respiratory conditions. Its empirical formula is C10H14O4, which corresponds to a molecular weight of 198.21. It is a white or slightly gray crystalline substance with a slightly bitter aromatic taste. Its solid oral dosage form is available as extended release tablets for oral administration [1]. Dextromethorphan (DN) [2–4] is the dextrorotatory enantiomer of the methyl ether of??levorphanol and stereoisomer of levomethorphan. DN is an antitussive (cough suppressant) drug and used for pain relief and psychological applications [5–7]. Its empirical formula is C8H25NO, which corresponds to a molecular weight of 271.4. It is a white powder. The combination of GN and DN is used to treat cough and chest congestion caused by the common cold, infections, or allergies. The chemical structures of GN and DN are shown in Table 1. Table 1: Structures of Guaifenesin and Dextromethorphan. Impurity profiling of active pharmaceutical ingredients (API) in both bulk material and finalized formulations is one of the most challenging tasks
Stability-Indicating RP-HPLC Method for the Simultaneous Estimation of Efavirenz, Tenofovir and Emtricitabine in Pharmaceutical Formulations  [PDF]
PSRCHNP Varma D, A Lakshmana Rao
Indian Journal of Pharmacy and Pharmacology , 2014,
Abstract: A simple, precise and rapid HPLC method has been developed for the simultaneous determination of Efavirenz, Tenofovir and Emtricitabine in pharmaceutical dosage form. The method was carried out using Zorbax C8 column (150 mm x 4.6 mm, 5 μm) and mobile phase comprised of mixture of dilute orthophosphoric acid solution pH 2.4±0.02 as buffer and acetonitrile in the ratio of 70:30 v/v and degassed under ultrasonication. The flow rate was 1.0 mL/min and the effluent was monitored at 252 nm. The retention times of Efavirenz, Tenofovir and Emtricitabine were 1.81 min, 2.80 min and 7.30 min respectively. The method was validated in terms of linearity, precision, accuracy, specificity, limit of detection, limit of quantitation and by performing recovery study. Linearity was in the range of 600.13 to 1800.39 μg/mL for Efavirenz, 300.54 to 900.44 μg/mL for Tenofovir and 200.46 to 601.38 μg/mL for Emtricitabine respectively. The percentage recoveries of all the three drugs were ranging from 98.2 to 101.9 for Efavirenz, 99.7 to 101.9 for Tenofovir and 98.7 to 101.6 for Emtricitabine respectively from the tablet formulation. The proposed method is suitable for the routine quality control analysis of simultaneous determination of Efavirenz, Tenofovir and Emtricitabine in bulk and pharmaceutical dosage form.
Development and Validation of Stability Indicating Rapid RP-LC Method for Determination of Process and Degradation Related Impurities of Apremilast, an Anti-Inflammatory Drug  [PDF]
Shashikant B. Landge, Sunil B. Dahale, Sanjay A. Jadhav, Pavankumar V. Solanki, Saroj R. Bembalkar, Vijayavitthal T. Mathad
American Journal of Analytical Chemistry (AJAC) , 2017, DOI: 10.4236/ajac.2017.86029
Abstract: A new, specific, rapid and stability indicating reversed phase liquid chro-matographic (RP-LC) method for the determination of process related and degradation related impurities of Apremilast has been developed and validated. The degradation study performed in acid, base, oxidative, photolytic, and thermal stressed conditions. Eight process related impurities (Imp-1 to Imp-8) in test sample of Apremilast have been detected by developed RP-LC method. The good chromatographic resolution between the peaks of process related impurities, degradation impurities and Apremilast has been achieved on a Synergi Max-RP 80 A (150 × 4.6 mm ID), 4 μ column. The process and degradation related impurities were characterized by mass spectrometry, 1H NMR and FT-IR spectral data. The method was validated as per ICH guideline and found to be specific, rapid, and stability indicating. The proposed RP-PLC method was successfully applied to the analysis of drug substance samples of Apremilast.
Stability-Indicating Gradient RP-LC Method for the Determination of Process and Degradation Impurities in Bosentan Monohydrate: An Endothelin Receptor Antagonist
Sanjay A. Jadhav,Shashikant B. Landge,Sonali L. Jadhav,Navanath C. Niphade,Saroj R. Bembalkar,Vijayavitthal T. Mathad
Chromatography Research International , 2011, DOI: 10.4061/2011/929876
Abstract: Described is a simple, rapid, selective, and stability-indicating RP-LC method for the determination of process and degradation-related impurities of bosentan monohydrate. Chromatographic separation was achieved on Zorbax SB-Phenyl column thermostated at 35°C under gradient elution by a binary mixture of solvent A (60% phosphate buffer, pH 2.5, and 40% methanol) and solvent B (acetonitrile) at a flow rate of 1.0 mL/min. Forced degradation was carried out under acidic, alkaline, oxidative, photolytic, and thermal conditions. Significant degradation is observed in acid and alkali stress conditions. Process- and degradation-related impurities were characterized by mass spectrometry, 1H NMR, and FT-IR spectral data. Validation of the developed method was carried out as per ICH requirements. Regression analysis shows an “” value (correlation coefficient) of greater than 0.999 for bosentan and five potential impurities. This method was capable to detect the five impurities at 0.01% of the test concentration of 1.0 mg mL−1.
Lanka A.Rama Prasad,J.V.L.N.S.Rao,Pamidi.Srinivasu,Jagadabi.Vara Prasad
International Research Journal of Pharmacy , 2012,
Abstract: The objective of the current study was to develop and validate precise, specific and stability-indicating reverse phase LC method for the simultaneous quantitative determination of Lamivudine, Tenofovir disoproxil fumarate and Nevirapine and their related impurities. The determination was done for extended release tablets dosage form where Tenofovir and Lamivudine are formulated into immediate release and Nevirapine into extended relase. The pharmaceutical formulation along with individual active ingredients was subjected to stress conditions of hydrolysis (acid and base), oxidation and thermal degradation as per International Conference on Harmonization (ICH) prescribed stress conditions to show the stability-indicating power of the method. It was found Tenofovir disoproxil fumarate is very sensitive to various stress conditions and readily degrades into Monoester impurity. The chromatographic conditions were optimized using an impurity-spiked solution and the samples generated from forced degradation studies. Regression analysis shows an r value (correlation coefficient) of greater than 0.997 for individual active drug substances and their all the related impurities. The chromatographic separation was achieved on a core shell technology C18 stationary phase. The method employed a linear gradient elution and the detection wavlength was set at 260 nm. The mobile phases consists of buffer and acetonitrile delivered at a flow rate of 0.8 mL min–1. The stress samples were assayed against a qualified reference standard and the mass balance was found to be close to 98.5%. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness.
Stability-Indicating RP-TLC/Densitometry Determination of Raloxifene Hydrochloride in Bulk Material and in Tablets  [PDF]
A. A. Shirkhedkar,J. K. Rajput,D. K. Rajput,S. J. Surana
Chromatography Research International , 2012, DOI: 10.1155/2012/356216
Abstract: A stability-indicating RP-TLC/Densitometry method for analysis of Raloxifene hydrochloride both in bulk material and in tablets was developed and validated. Densitometric analysis of Raloxifene hydrochloride was carried out at 311?nm on TLC aluminium plates precoated with silica gel 60RP-18 S as the stationary phase and methanol?:?water?:?ammonia (95?:?05?:?0.1 ) as mobile phase. Raloxifene hydrochloride was well resolved at 0.55 ± 0.02. The linear regression analysis data for the calibration plots showed good linear relationship with with respect to peak area in the concentration range 100–600?ng per band. The mean value ± SD of slope and intercept was found to be and with respect to peak area. The limits of detection and quantification were 9.27?ng and 27.10?ng, respectively. Raloxifene hydrochloride was subjected to acid and alkali hydrolysis, oxidation, dry heat, and photodegradation. The drug underwent degradation under basic and oxidation conditions. This indicates that the drug is susceptible to alkali hydrolysis and oxidation. The proposed developed RP-TLC/Densitometry method can be applied for identification and quantitative determination of Raloxifene hydrochloride in bulk material and tablets. 1. Introduction Raloxifene hydrochloride (RLX), [6-Hydroxy-2-(4-hydroxy-phenyl) benzo [b] thien-3-yl] [4-[2-(1-piperidinyl)-ethoxy] phenyl]-methanone-, hydrochloride (Figure 1) is a selective estrogen receptor modulator (SERM) used in the treatment of osteoporosis in postmenopausal women [1]. Clinically, it is effective in the treatment of breast cancer [2, 3]. Figure 1: Chemical structure of Raloxifene hydrochloride (RLX). Literature survey revealed that RLX was analyzed by HPLC [4–9], Stability-indicating UPLC [10], and several UV-spectrophotometric [11–14] in pharmaceutical formulations. Few methods such as LC-MS-MS [15] and HPLC [16] have been reported for estimation of RLX in biological samples. Although the RP-HPLC and UPLC procedures are accurate and effective means of assaying RLX, they are time and solvent consuming, and therefore, disadvantageous for serial estimation for a large number of samples [17]. However, the prominent application of HPTLC is that many samples can be run simultaneously using a small quantity of mobile phase unlike HPLC, thus reducing the analysis time and cost per analysis. In-reverse phase chromatography, polar mobile phase is used and the stationary phase is nonpolar. It is increasingly being experienced that different components of formulation which could not be resolved using normal-phase TLC could easily be
Development and Validation of a Stability Indicating RP-UPLC Method for Analysis of Imipramine Hydrochloride in Pharmaceuticals  [PDF]
H. N. Deepakumari,K. B. Vinay,H. D. Revanasiddappa
ISRN Analytical Chemistry , 2013, DOI: 10.1155/2013/913765
Abstract: The objective of the current study was the development of a simple, rapid, and accurate isocratic reverse-phase ultra-performance liquid chromatographic (RP-UPLC) method for the routine control analysis of imipramine hydrochloride (IMH) in bulk drug and in pharmaceutical formulations. This work was carried out in order to reduce analysis time and maintaining good efficiency which in turn is focused on high-speed chromatographic separations. The method was developed using Waters Acquity BEH C18 column (100?mm × 2.1?mm, 1.7?μm) with mobile phase consisting of a mixture of acetonitrile and ammonium acetate buffer of pH-5 (80?:?20, v/v/v). UV detection was performed at 220?nm for eluted compound. An excellent linearity was observed in the concentration range 0.2–3?μg/mL IMH with a regression coefficient ( ) value of 0.9999. The method developed was validated and forced degradation was performed as per ICH guidelines. The limit of detection ( ) was 0.2532?ng/mL and the limit of quantitation ( ) was found to be 0.7672?ng/mL. The drug IMH was subjected to hydrolytic, acidic, basic, thermal, photolytic, and oxidative stress conditions according to ICH regulations. IMH was found to be stable in basic, thermal, and photolytic conditions and degrades in acidic, hydrolytic, and oxidative stress conditions. 1. Introduction Imipramine hydrochloride (IMH) is a tricyclic antidepressant. It is a dibenzazepine derivative and chemically IMH is 3-(10,11-Dihydro-5H-dibenz[b,f]azepin-5-yl) propyldimethylamine hydrochloride (Figure 1). IMH is commonly used to treat the depressive disorders owing to their efficiency in elevating the mood of patients by interfering to the reuptake of norepinephrine or serotonin [1]. The drug is official in European Pharmacopoeia [2]. Figure 1: Structure of imipramine hydrochloride. The literature on the methods for the determination of IMH is vast. Several analytical methods have been reported for the determination of IMH in biological fluids and/or pharmaceutical formulations. These include chromatographic techniques like HPLC [3–9], TLC [10], GC [11–14], LC with direct injection and electrochemical detection [15], adsorptive stripping voltammetry [16], chemometric methods [17], flow-injection extraction spectrophotometry [18], derivative spectrophotometry [19, 20], and visible spectrophotometry [20–24]. Many of the reported methods for the determination of imipramine suffer from one or the other disadvantages like time consuming and require expensive experimental setup [11–14], and chemometric methods are less sensitive [17]. Besides, the
V.Kalyana Chakravarthy
International Journal of Pharmaceutical Research and Development , 2011,
Abstract: An isocratic reverse phase liquid chromatography (RP-LC) method has been developed and subsequently validated for the determination of Entecavir in pharmaceutical formulation. Separation was achieved with a Develosil ODS MG-5 (250 mmx4.6 mm I.D; particle size 5 μm) and Trifluoroacetic acid Buffer (0.5 ml in 2000ml of water v/v): Acetonitrile (93:7) as eluent at flow rate 1.0 mL/min. UV detection was performed at 254nm. The method is simple, rapid, and selective. The described method of Entecavir is linear over a range of 4.8 μg/mL to 71.93 μg/mL. The method precision for the determination of assay was below 2.0%RSD. The percentage recoveries of active pharmaceutical ingredient (API) from dosage forms ranged from 99.5 to 100.2. The method is useful in the quality control of pharmaceutical formulations.
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