Validated Stability-Indicating Method for Alendronate Sodium Employing Zwitterionic Hydrophilic Interaction Chromatography Coupled with Charged Aerosol Detection

Alendronate sodium is widely used in the treatment of osteoporosis and Paget’s disease. The HPLC method development for alendronate sodium, in particular, is challenging owing to the absence of chromophoric group and its high polarity. In the present study, a short and simple isocratic method was developed involving hydrophilic interaction liquid chromatography, coupled with a charged aerosol detector. The developed method was validated according to the ICH Q2(R1) guideline and was successfully applied for the analysis of a marketed formulation containing the drug.

     

General strategy for a short and efficient synthesis of 3-hydroxy-4-methylprolines (HMP)

The non-proteinogenic amino acid 3-hydroxy-4-methylproline (HMP) is an active constituent of some potent antimicrobials including echinocandins, nostopeptins, pneumocandins, sporiofungin and mulundocandins. A synthesis has been achieved in 10 steps with 29% overall yield; the Evans’ aldol reaction using Crimmins’ modified method was pivotal to the success of the strategy.     

Fatty acid binding site of mitochondrial uncoupling protein UCP2 as probed by EPR spectroscopy of spin-labeled fatty acids

Electron paramagnetic resonance (EPR) spectroscopy of spin-labeled fatty acids was used to investigate their interaction withEscherichia coli-expressed human mitochondrial uncoupling protein UCP2 refolded from inclusion bodies in nonaethylene glycol monododecyl ether (C₁₂E₉) micelles. 5-DOXYL-stearic acid and 4-PROXYL-palmitic acid bound to UCP2 exhibited additional clearly separated h_+1I, h_?1I “immobile” peaks in the low- and high-field region, respectively, separated by 42 and 44 Gauss, and extensively reduced h_+1M, h_?1M “mobile” peaks, separated by about 30 G, whereas with 7-DOXYL-stearic acid the I and M peaks were smoothed together into one wide peak. Competition of 4-PROXYL-palmitic acid with added palmitic acid, arachidonic acid, and all-cis-8,11,14-eicosatrienoic acid and of 7-DOXYL-stearic acid with arachidonic acid was indicated by the disappearance of the h_+1I, h_?1I “immobile” peaks, whereas redistribution in micelles without protein was indicated by the rising of the h_+1M, h_?1M “mobile” peaks. In conclusion, a competition of palmitic, arachidonic, and eicosatrienoic acid within a putative fatty acid binding site was observed for mitochondrial uncoupling protein UCP2. This finding together with the observation of EPR spectra of highly immobilized probes exclusively in the presence of the recombinant UCP2 suggest the existence of a fatty acid binding site on UCP2 which is a prerequisite of the fatty acid cycling mechanism as previously postulated for UCP1.     

EPR and optical absorption studies on VO ions in KZnClSO4·3H2O single crystals—an observation of superhyperfine structure

EPR spectra of VO²⁺ ions doped in KZnClSO₄·3H₂O single crystals have been studied at different temperatures. The EPR spectrum shows a well-resolved hyperfine and superhyperfine structure patterns. The angular variation of EPR spectra reveals the presence of more than three magnetic complexes, which correspond to distinct sites of VO²⁺ ion. From the angular variation EPR data, the spin-Hamiltonian parameters are evaluated and discussed. The optical absorption spectrum studied at room temperature shows bands corresponding to C_4v symmetry. From the EPR and optical data, the molecular-orbital bonding coefficient ε² and β² are evaluated and discussed. The observed five-line superhyperfine structure has been attributed to four protons (with I=1/2) from the surrounding water molecules of one of the vanadyl sites.     

Magnetic properties of lanthanum orthoferrite fine powders prepared by different chemical routes

Fine powders of lanthanum iron oxide, LaFeO₃, have been prepared by solid state reaction as well as sol-gel synthesis and nebulized spray pyrolysis. Structures, morphologies and magnetic susceptibility measurements of these powders have been examined. The powders prepared by all the three low-temperature routes contain nearly spherical particles with an average diameter of 40 nm. These samples show a lower Neel temperature than the powder prepared by solid state reaction besides showing much lower magnetic susceptibility at low temperatures. Dedicated to Professor C N R Rao on his 70th birthday     

Tevatron: Recent results and prospects at the upgrade

In this article, we review some of the recent results from CDF and DØ experiments at the Tevatron and their prospects at the upgrade. Among the topics discussed are top quark physics, electroweak physics, qcd physics and new physics beyond standard model.     

Study of fiber optic sugar sensor

Over the last two decades, the fiber optic technology has passed through many analytical stages. Some commercially available fiber optic sensors, though in a small way, are being used for automation in mechanical and industrial environments. They are also used for instrumentation and controls. In the present work, an intensity-modulated intrinsic fiber optic sugar sensor is presented. This type of sensor, with slight modification, can be used for on-line determination of the concentration of sugar content in sugarcane juice in sugar industry. In the present set-up, a plastic fiber made of polymethylmethacrylate is used. A portion of the cladding (1 cm, 2 cm, 3 cm) at the mid-point along the length of the fiber is removed. This portion is immersed in sugar solution of known concentration and refractive index. At one end of the fiber an 850 nm source is used and at the other end a power meter is connected. By varying the concentration of sugar solution, the output power is noted. These studies are made due to the change in refractive index of the fluid. The device was found to be very sensitive which is free from EMI and shock hazards, stable and repeatable and they can be remotely interfaced with a computer to give on-line measurements and thus become useful for application in sugar industries.     

Valence band and chemical interactions of Zn/CdSnAs2 interfaces

X-ray photoelectron spectroscopy (XPS) together with argon ion sputtering was used to investigate the interface of the Zn/CdSnAs₂ system at various temperatures. The formation of an intermediate compound between Zn and As is proposed. The surface enrichment of Cd and Sn at 200 and 400°C is explained in terms of bond breaking and lattice strain theories.NCL Communication No. 4352     

Use of a chiral surfactant for enantioselective reduction of a ketone

The influence of a chiral surfactant and a polymer-supported chiral additive on reduction of ketones using sodium borohydride will be described. Initial preparations involved methylation of (S)-leucinol to give (2S)-N , N-dimethyl-2-amino-4-methyl-1-pentanol (1) (67%). The chiral surfactant (2) was synthesized by reacting (1) with bromohexadecane (71%). The functionalized styrene for the polymer-supported chiral additive (5) was synthesized by reacting (1) with 4-vinylbenzyl chloride. Polymerization was carried out with 10% of the functionalized monomer (4), 5% cross-linking agent divinylbenzene, and 85% styrene with AIBN as the initiator. The activity of the chiral surfactant and polymeric additive were examined by using them as additives in a standard reduction of 2-pentanone with sodium borohydride to yield (R)- and (S)-2-pentanol (3) (20%). The resulting alcohol was analyzed by polarimetry (ee 9.5%) and also esterified with (2S)-methylbutyric acid prior to characterization by NMR. 13C NMR indicated an enantiomeric excess of 5.2% when the chiral surfactant was used, and 7% when the polymeric additive was used.     

Fermion masses

In this paper, we show that 2m _e m /(m _e ² +m ² = (g _V/g _A) _e ² . From this expression, the Weinberg mixing parameter is shown to be 0·2254 or 0·2746. Assuming that the electron and muon neutrino masses are degenerate, we find thatm _v = (g _V/g _A) _e ² . (m _e m )/M _WL, where M_WL is the mass of the standard W^± boson. The neutrino mass turns out to be 6·5 eV. The -neutrino mass is found to be about 81 MeV. The masses of c, t, s and b quarks are found to be respectively 1·7 GeV, 21·2 GeV, 0·57 GeV and 2·18 GeV by assumingm _d=m _u= 0·3 GeV. All these masses agree with other estimates except the b quark which has about half of its expected value.