Stability indicating HPLC method for the simultaneous determination of moxifloxacin and prednisolone in pharmaceutical formulations

BACKGROUND: A simple, specific, and fast stability indicating reverse phase liquid chromatographic method was established for instantaneous determination of moxifloxacin and prednisolone in bulk drugs and pharmaceutical formulations. RESULTS: Optimum chromatographic separations among the moxifloxacin, prednisolone and stress-induced degradation products were achieved within 10 minutes by use of BDS Hypersil C8 column (250 X 4.6 mm, 5 μm) as stationary phase with mobile phase consisted of a mixture of phosphate buffer (18 mM) containing 0.1% (v/v) triethylamine, at pH 2.8 (adjusted with dilute phosphoric acid) and methanol (38:62 v/v) at a flow rate of 1.5 mL min(-1). Detection was performed at 254 nm using diode array detector. The method was validated in accordance with ICH guidelines. Response was a linear function of concentrations over the range of 20–80 μg mL(-1) for moxifloxacin (r2 ≥ 0.998) and 40–160 μg mL(-1) for prednisolone (r2 ≥ 0.998). The method was resulted in good separation of both the analytes and degradation products with acceptable tailing and resolution. The peak purity index for both the analytes after all types of stress conditions was ≥ 0.9999 indicated a complete separation of both the analyte peaks from degradation products. The method can therefore, be regarded as stabilityindicating. CONCLUSIONS: The developed method can be applied successfully for simultaneous determination of moxifloxacin and prednisolone in pharmaceutical formulations and their stability studies

N-(4-Meth­oxy­phen­yl)-4-methyl­benzene­sulfonamide

In the title compound, C14H15NO3S, the dihedral angle between the aromatic rings is 59.39 (14)° and the C—S—N—C torsion angle is −71.4 (2)°. In the crystal, a supra­molecular chain running along the b axis with a C(4) graph set is formed via N—H⋯O hydrogen bonds

2-(4-Methyl­benzene­sulfonamido)-2-phenyl­acetic acid

In the title compound, C15H15NO4S, the dihedral angle between the phenyl and benzene rings is 46.0 (3)° and a weak intra­molecular N—H⋯O inter­action is present. The crystal structure is stabilized by inter­molecular O—H⋯O, N—H⋯O and C—H⋯O hydrogen bonds

2,5-Dichloro-N-(4-meth­oxy­phen­yl)benzensulfonamide

In the title compound, C13H11Cl2NO3S, the dihedral angle between the benzene rings is 74.37 (3)°. In the crystal, inter­molecular N—H⋯O hydrogen bonds link the mol­ecules into chains along the b axis

Hexaaqua­chromium(III) pyridine-2,4,6-tricarboxyl­ate dihydrate

The chromium(III) atom in the title salt, [Cr(H2O)6](C8H2NO6)·2H2O, has an octa­hedral coordination geometry. In the crystal, the cation, anion and uncoordinated water mol­ecules, both of which are disordered over two positions in a 1:1 ratio, are linked by O—H⋯O hydrogen bonds

[KDy(Hptc)3(H3ptc)]n·2n(Hbipy)·5n(H2O), a layered coordination polymer containing DyO6N3 tri-capped trigonal prisms (H3ptc = Pyridine 2,4,6-Tricarboxylic Acid, C8H5NO6; Bipy = 2,2'-Bipyridine, C10H8N2)

Peer reviewedPublisher PD

Simultaneous RP-HPLC determination of sparfloxacin and dexamethasone in pharmaceutical formulations

O presente estudo descreve o desenvolvimento e a subsequente validação de indicador de estabilidade simples e acurada por RP-HPLC para a determinação de esparfloxacino e dexametasona em formulações farmacêuticas na presença de produtos de degradação induzidos por estresse. Tanto os fármacos quanto os produtos de degradação induzidos pelo estresse foram separados em 10 minutos, utilizando coluna C8 e mistura de methanol e tampão fosfato 0,02 M, pH 3,0 (60:40 v/v, respectivamente) como fase móvel e detector de arranjo de diodo a 270 nm, A análise de regressão mostrou linearidade na faixa de 15-105 µg/mL para esparfloxacino e 5-35 µg/mL para a dexametsona. Todos os analitos foram resolvidos adequadamente com tailing aceitável. O pico de pureza dos dois foi maior que 0.9999, não mostrando picos de co-eluição. O método desenvolvido foi aplicado para a determinação simultânea de esparfloxacino e dexametasona em formulações farmacêuticas e para estudos de estabilidade.The present study describes the development and subsequent validation of simple and accurate stability indicating RP-HPLC method for the determination of sparfloxacin and dexamethasone in pharmaceutical formulations in the presence of their stress-induced degradation products. Both the drugs and their stress-induced degradation products were separated within 10 minutes using C8 column and mixture of methanol and 0.02 M phosphate buffer pH 3.0 (60:40 v/v, respectively) as mobile phase at 270 nm using diode array detector. Regression analysis showed linearity in the range of 15-105 µg/mL for sparfloxacin and 5-35 µg/mL for dexamethasone. All the analytes were adequately resolved with acceptable tailing. Peak purity of the two drugs was also greater than 0.9999, showing no co-elution peaks. The developed method was applied for simultaneous determination of sparfloxacin and dexamethasone in pharmaceutical formulations for stability studies

Stability indicating RP-HPLC method for simultaneous determination of gatifloxacin and dexamethasone in binary combination

In this study, conditions were optimized for development of a simple RP-HPLC method for simultaneous analysis of gatifloxacin and dexamethasone in different matrices like pharmaceuticals, human serum and urine. Good separation of gatifloxacin and dexamethasone from the induced degradation products was accomplished using C8 as stationary phase; 0.02 M phosphate buffer (pH 3.0) and methanol (42:58 v/v) as mobile phase. The concentration was measured with DAD at 270 nm. Linearity was observed in the range of 0.000040-0.000280 mol/L for gatifloxacin (r2≥0.999) and 0.000013-0.000091 mol/L for dexamethasone (r2≥0.999). Both the analyte peaks were completely separated from the peaks of induced degradation products as indicated by the peak purity index (≥0.9999 for both analytes). The optimized method is recommended to be used for concurrent analysis of gatifloxacin and dexamethasone in different matrices

N-(4-Hydroxy­phen­yl)benzene­sulfon­amide

The title compound, C12H11NO3S, synthesized by the reaction of benzene sulfonyl chloride with para-amino­phenol, is of inter­est as a precursor to biologically active sulfur-containing heterocyclic compounds. The structure is stabilized by N—H⋯O and O—H⋯O hydrogen bonds

Identification of Novel Dihydrofolate Reductase Inhibitor as Potential Antimalarial Drug: In silico Studies

Abstract.-Advancement in computational biology leads to improve the efficacy for new compounds to cure the diseases. Malaria is the most virulent diseases and causing millions of deaths annually, especially in developing and under-developed countries. Plasmodium falciparum dihydrofolate reductase (PfDHFR) is one of the most important drug target for different antifolates. Pyrimethamine with sulphadoxine complex is the most recommended and efficient antifolate prescribed against PfDHFR. But malarial parasites have developed resistance against this drug due to the point mutations in PfDHFR. This study focus to design a novel antimalarial drug (analog) against mutated PfDHFR by considering the in silico approaches. The new antimalarial drugs were designed by the addition/substitution of different functional groups and molecules in parent compound of pyrimethamine. The docking studies of newly designed compound and pyrimethamine with mutated receptor protein of PfDHFR were performed by using different docking servers. Various in silico therapeutic calculations for novel antimalarial compound and pyrimethamine were executed using computational approaches. The basic of ligand properties, docking results, energy calculations and drug score favor indicated that the new antimalarial drug compound have potential to show better efficacy than pyrimethamine. This designed analog could be used for preclinical test and have the potential to eradicate P. falciparum