Stability-Indicating HPTLC Method for Analysis of Moclobemide, and Use of the Method to Study Degradation Kinetics

A sensitive, selective, precise, and stability-indicating HPTLC method for analysis of moclobemide in the bulk drug and in formulations has been established and validated. Aluminium TLC plates precoated with silica gel 60 F₂₅₄ were used with benzene–methanol–40% ammonia 7:3:0.1 (v/v) as mobile phase. Densitometric analysis was performed in absorbance mode at 238 nm. Compact bands were obtained for moclobemide (R _F 0.67 ± 0.02; n = 6). The drug was subjected to acidic and alkaline hydrolysis, oxidation, dry heat treatment, and photodegradation. The drug undergoes degradation under acidic, basic, and oxidising conditions. The degradation products were well resolved from the pure drug with significantly different R _F values, so the method can be regarded as stability-indicating. Response to moclobemide was a linear function of amount in the range 50–600 ng per band, with a correlation coefficient, r ², of 0.9967 ± 0.51. LOD and LOQ, determined experimentally, were 10 and 30 ng per band, respectively. Statistical analysis proves the method is repeatable and specific for analysis of moclobemide. The method was used to investigate the kinetics of alkaline degradation. The Arrhenius plot was constructed and the activation energy calculated.     

Development and validation of a visible absorption densitometry method for quantitation of conessine in Holarrhena antidysenterica (Kurchi)

A selective, precise, and accurate high-performance thin-layer chromatographic (HPTLC) method has been proposed for the analysis of conessine in Holarrhena antidysenterica. The method involves visible densitometric evaluation of conessine resolving it by HPTLC on aluminium-based silica gel plates. For visible densitometric evaluation, peak areas were recorded at 520 nm after the resolved bands were derivatized with Dragendorff's reagent and then sprayed with a 10% solution of aqueous sodium nitrite which resulted in reddish brown color. The correlation between the concentration and area was found to be linear within the range of 10 to 60 ng/spot. The method was validated for precision (interday and intraday), repeatability, and accuracy. Mean recovery for conessine was 98.34-100.25%. The method was applied for the quantitation of conessine in Kurchi. The proposed HPTLC method was found to be precise, specific, sensitive, and accurate and can be used for routine analysis of Kurchi.     

Simultaneous estimation of acetylsalicylic acid and clopidogrel bisulfate in pure powder and tablet formulations by high-performance column liquid chromatography and high-performance thin-layer chromatography

This paper describes validated high-performance column liquid chromatographic (HPLC) and high-performance thin-layer chromatographic (HPTLC) methods for simultaneous estimation of acetylsalicylic acid (ASA) and clopidogrel bisulfate (CLP) in pure powder and formulations. The HPLC separation was achieved on a Nucleosil C8 column (150 mm length x 4.6 mm id, 5 microm particle size) using acetonitrile-phosphate buffer, pH 3.0 (55 + 45, v/v) mobile phase at a flow rate of 1.0 mL/min at ambient temperature. The HPTLC separation was achieved on an aluminum-backed layer of silica gel 60F254 using ethyl acetate-methanol-toluene-glacial acetic acid (5.0 + 1.0 + 4.0 + 0.1, v/v/v/v) mobile phase. Quantitation was achieved with UV detection at 235 nm over the concentration range 4-24 microg/mL for both drugs, with mean recoveries of 99.98 +/- 0.28 and 100.16 +/- 0.66% for ASA and CLP, respectively, using the HPLC method. Quantitation was achieved with UV detection at 235 nm over the concentration range of 400-1400 ng/spot for both drugs, with mean recoveries of 99.93 +/- 0.55 and 100.21 +/- 0.83% for ASA and CLP, respectively, using the HPTLC method. These methods are simple, precise, and sensitive, and they are applicable for the simultaneous determination of ASA and CLP in pure powder and formulations.     

A threshold for charge transfer in aromatic interactions? A quantitative study of pi-stacking interactions

[structure: see text] Attractive interactions between substituted arenes in the parallel displaced configuration have been quantitatively studied using triptycene-derived molecular conformational reporters. Charge-transfer bands are observed for models where the interactions are between strong donor and acceptors. Substituent effects on the strength of the aromatic interaction follow opposite trends for strongly electron-deficient arenes and mildly perturbed arenes. The free energy of interactions for models with strong electron donors and acceptors does not follow a linear correlation in the Hammett plot. Electrostatic models alone do not account for the nonlinearity of the free energy-substituents plot.     

Tracking individual fish from a moving platform using a split-beam transducer

Tracking of individual fish targets using a split-beam echosounder is a common method for investigating fish behavior. When mounted on a floating platform like a ship or a buoy, the transducer movement often complicates the process. This paper presents a framework for tracking single targets from such a platform. A filter based on the correlated fish movements between pings is developed to estimate the platform movement, and an extended Kalman filter is used to combine the split-beam measurements and the platform-position estimates. Different methods for gating and data association are implemented and tested with respect to data-association errors, using manually tracked data from a free-floating buoy as a reference. The data association was improved by utilizing the estimated velocity for each track to predict the location of the next observation. The data association was more robust when estimates of platform tilt/roll were used. Other techniques to estimate position and velocity, like linear regression and smoothing splines, were implemented and tested on a simulated data set. The platform-state estimation improved the estimates for methods like the Kalman filter and a smoothing spline with cross validation, but not for robust methods like linear regression and smoothing spline with a fixed degree of smoothing.     

Observation of the hc(1P1) state of charmonium

The h(c)((1)P(1)) state of charmonium has been observed in the reaction psi(2S) --> pi(0)h(c) --> (gammagamma)(gammaeta(c)) using 3.08 x10(6) psi(2S) decays recorded in the CLEO detector. Data have been analyzed both for the inclusive reaction, where the decay products of the eta(c) are not identified, and for exclusive reactions, in which eta(c) decays are reconstructed in seven hadronic decay channels. We find M(h(c)) = 3524.4 +/- 0.6 +/- 0.4 MeV which corresponds to a hyperfine splitting DeltaM(hf)(1P) triple-bond pi(0)h(c)) x B(h(c) --> gammaeta(c)) = (4.0 +/- 0.8 +/- 0.7) x 10(-4).     

Thermodynamics and kinetics of complexation of iron(III) ion by picolinic and dipicolinic acids

The complexation reactions of iron(III) with 2-pyridine carboxylic acia (picolinic acid) and 2,6-pyridine dicarboxylic acid (dipicolinic acid) in aqueous solutions have been studied by spectrophotometric and stopped flow techniques. Equilibrium constants were determined for the 1 : 1 complexes at temperatures between 25 and 80°C. The values obtained are: Picolinic Acid (HL): Fe³⁺+ H₂L⁺? FeHL³⁺+H+(K₁ = 2.8,ΔH = 2 kcal mole^?1 at 25°C, μ = 2.67 M) Dipicolinic Acid (H₂D): Fe³⁺+H₂D? FeD⁺+2H⁺(K₁K_1A= 227 M, ΔH = 3.4 kcal mole^?1 at 25°C,μ = 1.0 M). The rate constants for the formation of these complexes are also given. The results are used to evaluate the effects of these two acids upon the rate of dissolution of iron(III) from its oxides.