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Development of LC Method for the Simultaneous Determination of Antidepressant Drug Combination Melitracen Hydrochloride and Flupentixol Dihydrochloride in their Combined Dosage Form  [PDF]
Usmangani K. Chhalotiya,Kashyap K. Bhatt,Dimal A. Shah,Gautam R. Chauhan,Sunil L. Baldania
Chromatography Research International , 2011, DOI: 10.4061/2011/632820
Abstract: A simple, specific and stability-indicating reversed-phase high-performance liquid chromatographic method was developed for the simultaneous determination of melitracen hydrochloride and flupentixol dihydrochloride in tablet dosage form. A Brownlee C-18, 5?μm column having 2 5 0 × 4 . 6 ?mm i.d. in isocratic mode, with mobile phase containing 0.025?M potassium dihydrogen phosphate: methanol (10?:?90, v/v; pH 7.3) was used. The flow rate was 1.0?mL/min, and effluents were monitored at 230?nm. The retention times of melitracen hydrochloride and flupentixol dihydrochloride were 7.75?min and 5.50?min, respectively. The linearity for melitracen hydrochloride and flupentixol dihydrochloride were in the range of 0.5–60?μg/mL. The recoveries obtained for melitracen hydrochloride and flupenthixol dihydrochloride was 99.81–100.77% and 99.42–100.12%, respectively. Both the drugs were subjected to acid and alkali hydrolysis, chemical oxidation, and dry heat degradation and photodegradation. The proposed method was validated and successfully applied to the estimation of melitracen hydrochloride and flupentixol dihydrochloride in combined tablet dosage form. 1. Introduction Melitracen hydrochloride (MEL) is a white to off white powder and amorphous in nature. Chemically, it is 3-(10, 10-dimethyl anthracen-9-ylidene)-N, N-dimethylpropan-1-amine) [1, 2] (Figure 1(a)). It is a Tricyclic Antidepressant and work by inhibiting uptake of the neurotransmitters norepinephrine and serotonin by neurons. Flupentixol dihydrochloride (FLU) is white or almost white powder. Chemically, it is (Z)-4-[3-[2-(Trifluoromethyl)-9H thioxanthen-9-ylidene] propyl]-1-piperazin ethanol dihydrochloride [3] (Figure 1(b)). It is very soluble in water, soluble in alcohol and practically insoluble in methylene chloride [4]. Flupentixol acts by blocking the dopamine (a neurotransmitter) receptors in brain cells. Excess amount of dopamine receptors normally act to modify behavior and overstimulation resulting in psychotic illness. Flupentixol blocks these receptors to control psychotic illness. Thus it is neuroleptic with anxiolytic and antidepressant properties. The combination of FLU and MEL is indicated in the treatment of trigeminal neuralgia [5]. Figure 1: (a) Chemical structure of melitracen hydrochloride. (b) Chemical structure of flupentixol dihydrochloride. Literature survey revealed that melitracen hydrochloride can be estimated by spectrophotometry [6, 7] and by liquid chromatographic methods [8–11] individually or in combination with other drugs, and flupentixol dihydrochloride can be
Ahmed A. Elbary,Afaf A. Ramadan,Ihab R. Bendas,Dalia Abd Elaty Mostafa
International Research Journal of Pharmacy , 2011,
Abstract: The aim of the present study was to develop rapid disintegrating tablets of Flupentixol dihydrochloride, a slightly bitter antipsychatric drug. An attempt has been made to prepare bitterless rapid disintegrating tablet using Eudragit E100 as a taste masking agent. The tablet was prepared with three superdisintegrants e.g. sodium starch glycolate, crosscarmellose sodium and crospovidone , each one was added in three different concentration 2%, 3% and 4% ; mass extrusion was the technique used for the preparation of these tablets. The blend was examined for angle of repose, bulk density, tapped density, compressibility index and Hausner’s ratio. The compressed tablets were evaluated for hardness, drug content, friability, disintegration time in-vitro and in-vivo, wetting time and dissolution rate. The contents of the prepared tablets were characterized by X-ray diffraction and Fourier transform infrared spectroscopy (FTIR). Different nine formulas showed in-vitro disintegration times ranges from 11.8 sec to 61 sec , but it was 150 sec for F1 ( formula without any superdisintegrant). These results were nearly correlated with in vivo disintegration times for the ten formulas. In vitro dissolution studies showed the release in the following descending order of superdisintegrants: Crospovidone > Croscarmellose sodium > Sodium Starch Glycolate. Maximum in vitro dissolution rate was found to be with formulation F10 which contains crospovidone (4%). Thus, F10 was considered the best among the other formulations. The stability study was conducted as the International Conference on Harmonization (ICH) guidelines and the formulations subjected again for changes in hardness, friability, drug content, wetting time and disintegration time. Crospovidone at a concentration of 4% w/w is suitable for preparing rapid disintegrating tablet of Flupentixol dihydrocloride.
1-(2-Hydroxyethyl)-4-{3-[(E)-2-(trifluoromethyl)-9H-thioxanthen-9-ylidene]propyl}piperazine-1,4-diium bis(3-carboxyprop-2-enoate)
M. S. Siddegowda,Ray J. Butcher,Mehmet Akkurt,H. S. Yathirajan
Acta Crystallographica Section E , 2011, DOI: 10.1107/s160053681102722x
Abstract: In the title salt, C23H27F3N2OS+·2C4H3O4 , a non-merohedral twin [ratio of the twin components = 0.402 (1):0.598 (1)], the –CF3 group is disordered over two sets of sites with occupancy factors in the ratio 0.873 (2):0.127 (2). The dihedral angle between the two outer aromatic rings of the 9H-thioxanthene unit, whose thiopyran ring has a screw-boat conformation, is 33.01 (9)°. The diprotonated piperazine ring adopts a chair conformation. In the crystal, intermolecular O—H...O, N—H...O and C—H...O hydrogen bonds between neighboring molecules form zigzag chains along the a axis and contribute to the stabilization of the packing.
Opipramol dihydrochloride
Richard Betz,Thomas Gerber,Eric Hosten,Budanoor P. Siddaraju
Acta Crystallographica Section E , 2011, DOI: 10.1107/s1600536811042280
Abstract: The title compound (systematic name: 4-{3-[2-azatricyclo[,8]pentadeca-1(15),3,5,7,11,13-hexaen-2-yl]propyl}-1-(2-hydroxyethyl)piperazine-1,4-diium dichloride), C23H31N3O+·2Cl , is the dihydrochloride of a piperazine derivative bearing a bulky 3-(5H-dibenz[b,f]azepin-5-yl)propyl substituent. Protonation took place on both N atoms of the piperazine unit. The diazacyclohexane ring adopts a chair conformation. N—H...Cl, O—H...Cl and C—H...Cl hydrogen bonding as well as C—H...O contacts connect the components into a three-dimensional network in the crystal. Two C—H...π contacts are also observed.
Fluphenazine dihydrochloride dimethanol solvate  [cached]
Joanna Petrus,Rafał Petrus,Bogusława Czarnik-Matusewicz
Acta Crystallographica Section E , 2012, DOI: 10.1107/s1600536812008707
Abstract: In the title compound {systematic name: 1-(2-hydroxyethyl)-4-[3-(2-trifluoromethyl-10H-phenothiazin-10-yl)propyl]piperazine-1,4-diium dichloride dimethanol disolvate}, C22H28F3N3OS2+·2Cl ·2CH3OH, the dihedral angle between the planes of the two outer benzene rings of the tricyclic phenothiazine system is 46.91 (13)°. The piperazine ring adopts a chair conformation. The crystal structure is stabilized by O—H...Cl, N—H...Cl, C—H...O, C—H...Cl and C—H...F hydrogen bonds and contacts.
Piperazine-1,4-diium diacetate
Shao-Gang Hou
Acta Crystallographica Section E , 2011, DOI: 10.1107/s1600536811047441
Abstract: In the title salt, C4H12N22+·2C2H3O2 , the piperazine-1,4-diium cation has 2/m symmetry with the NH2 unit located on a mirror plane and the acetate anion has m symmetry with all non-H atoms and one H atom located on a mirror plane. The piperazine ring adopts a chair conformation. In the crystal, the cations are linked with the anions via N—H...O hydrogen bonding into chains parallel to the c axis.
Simultaneous UV spectrophotometric estimation of ambroxol hydrochloride and levocetirizine dihydrochloride  [cached]
Prabu S,Shirwaikar A,Shirwaikar Annie,Kumar C
Indian Journal of Pharmaceutical Sciences , 2008,
Abstract: A novel, simple, sensitive and rapid spectrophotometric method has been developed for simultaneous estimation of ambroxol hydrochloride and levocetirizine dihydrochloride. The method involved solving simultaneous equations based on measurement of absorbance at two wavelengths 242 nm and 231 nm, the g max of ambroxol hydrochloride and levocetirizine dihydrochloride, respectively. Beer′s law was obeyed in the concentration range 10-50 μg/ml and 8-24 μg/ml for ambroxol hydrochloride and levocetirizine dihydrochloride respectively. Results of the method were validated statistically and by recovery studies.
A.K. Doshi*, B.N. Patel and C.N. Patel
International Journal of Pharmaceutical Sciences and Research , 2012,
Abstract: A simple, accurate and precise spectrophotometric method has been developed for simultaneous estimation of Propranolol hydrochloride and Flunarizine dihydrochloride in combined dosage form. Simultaneous equation method is employed for simultaneous determination of Propranolol hydrochloride and Flunarizine dihydrochloride from combined dosage forms. In this method, the absorbance was measured at 289 nm for Propranolol hydrochloride and 253 nm for Flunarizine dihydrochloride. Linearity was observed in range of 24-64 μg/ml and 6-16 μg/ml for Propranolol hydrochloride and Flunarizine dihydrochloride respectively. Recovery studies confirmed the accuracy of proposed method and results were validated as per ICH guidelines. The method can be used for routine quality control of pharmaceutical formulation containing Propranolol hydrochloride and Flunarizine dihydrochloride.
Measurement of antioxidant activity with trifluoperazine dihydrochloride radical cation
Asghar, M.N.;Khan, I.U.;
Brazilian Journal of Medical and Biological Research , 2008, DOI: 10.1590/S0100-879X2008000600003
Abstract: a novel, rapid and cost-effective trifluoperazine dihydrochloride (tfph) decolorization assay is described for the screening of antioxidant activity. a chromogenic reaction between tfph and potassium persulfate at low ph produces an orange-red radical cation with maximum absorption at 502 nm in its first-order derivative spectrum. tfph was dissolved in distilled water to give a 100 mm solution. the tfph radical cation solution was made by reacting 0.5 ml of the solution with k2s2o8 (final concentration: 0.1 mm) and diluting to 100 ml with 4 m h2so4 solution. a linear inhibition of color production was observed with linearly increasing amounts of antioxidants, with correlation coefficients (r2) ranging from 0.999 to 0.983. the antioxidant capacity of standard solutions of an antioxidant was evaluated by comparing with the inhibition curve using trolox as the standard. comparison of antioxidant capacity determined with this newly developed tfph assay and with the well-known 2,2'-azinobis-[3-ethylbenzthiazoline-6-sulfonic acid] (abts)-persulfate decolorization assay indicated the efficacy and sensitivity of the procedure. the proposed assay is less expensive (costs about us$4 per 100 assays) and requires only 20 min for preparation of radical cation solution in comparison with abts assay, in which almost 12-16 h are required for preparation of a stable abts radical cation solution. the present assay has the advantage over abts assay that it can be used to measure the antioxidant activity of the samples, which are naturally found at a ph as low as 1, because the radical cation itself has been stabilized at low ph.
Raja Sundararajan et al
International Journal of Pharmaceutical Sciences and Research , 2012,
Abstract: A rapid reverse phase high performance liquid chromatographic method was developed for the estimation of Manidipine dihydrochloride in its pure form as well as in tablet dosage forms. Chromatography was carried out on an phenomenex C18 column (250 4.6mm, 5 μm), using a mixture of acetonitrile and water (80: 20 v/v) with pH adjusted to 3.5 with ortho phosphoric acid (0.1 % v/v) as the mobile phase at a flow rate of 1.3 mL/min The detection wavelength is 230 nm. The retention time of the drug was 3.54 min. The method produced linear responses within concentration range of 25 to 125 μg/mL of Manidipine dihydrochloride. The method was found to be reproducible for analysis of the drug in tablet dosage forms.
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