Computer-assisted optimization and validation of LC analysis of trimetazidine dihydrochloride and its impurities

Trimetazidine dihydrochloride is an anti-anginal drug, which possesses protective properties against ischemia inducing heart damage. In this paper, a new procedure for liquid chromatographic analysis was successfully developed, optimized, and applied in assessment of trimetazidine dihydrochloride content and its impurities, Y-145, Y-235, and Y-234 at most 1.0%, 0.2%, and 0.2%, respectively, in commercially available pharmaceutical preparation containing 35 mg of trimetazidine dihydrochloride. The retention behavior of trimetazidine dihydrochloride and its impurities is investigated by using several stationary and mobile phases to settle a simple, sensitive, and precise RP-HPLC method. The separation conditions are optimized by DryLab 2000 Plus Chromatography Optimization Software version 3.5.00. Separations are performed on PurospherSTAR RP18 endcapped (150 x 4.6 mm, 5 microm particle size) column at 20 degrees C with UV detection at 210 nm. The mobile phase composition is acetonitrile-aqueous phase (10 mmol/L disodium hydrogenphosphate and 2 mmol/L sodium dihydrogen phosphate, pH 7.6) (30:70 v/v). Afterwards, the method is validated; the important statistical parameters for selectivity/specificity, linearity, precision, limit of detection, and quantitation are defined. The recovery value of the trimetazidine dihydrochloride is 98.06%, and the content of impurities is 0.23% for Y-145, less than 0.02% for Y-235, and less than 0.01% for Y-234. In addition, this method is used for analyzing trimetazidine dihydrochloride and its impurities in pharmaceuticals and bulk drug.     

A note on the article “Fuzzy alpha-sets and alpha-continuous maps”

In this note we show that some results which appeared in the article by M.K. Singal and N. Rajvanshi [Fuzzy Sets and Systems 48 (1992) 383–390] are incorrect.     

Applying Multivariate Methods in the Estimation of Bioactivity Properties of Acetamide Derivatives

JPC – Journal of Planar Chromatography – Modern TLC - It has been established that the selected acetamide derivatives fulfill Veber’s and Pardridge’s rule of good...     

Copper Oxide – Graphite Composite Electrodes: Application to Nitrite Sensing

A simple method for the modification of carbon powder with copper oxides is presented. Carbon powder is impregnated with copper(II) nitrate by stirring carbon powder in copper(II) nitrate solution for 1 hour and subsequently thermally treated at 823 K. The modified carbon powder was characterized using electrochemical and spectroscopic techniques. The existence of both copper(I) and copper(II) oxides have been established. The copper oxide modified carbon powder was used for preparation of composite electrodes, and the electrochemical and electrocatalytic behavior of the resulting composite electrodes was studied. The copper oxide modified carbon powder – epoxy composite electrodes showed a high electrocatalytic activity for the nitrite detection in aqueous media, with the detection limit comparable or lower than detection limits obtained with other electrochemical sensors.     

UPLC Method for Determination of Moxonidine and Its Degradation Products in Active Pharmaceutical Ingredient and Pharmaceutical Dosage Form

A simple, rapid, isocratic, stability-indicating reverse phase ultra-performance liquid chromatographic (RP-UPLC) method was developed and validated for the routine analysis of moxonidine in the presence of its degradation products in active pharmaceutical ingredient and pharmaceutical dosage forms. Forced degradation studies were performed according to the guidance of International Conference for Harmonization and were used to evaluate moxonidine intrinsic stability. The drug was subjected to acid, neutral and base hydrolysis as well as to oxidative, thermal and photolytic decomposition in both solution and solid state. The drug appeared to be unstable towards acid and base hydrolysis. To achieve desirable conditions for UPLC analysis, the method development was done with the assistance of experimental design and multivariate optimization methodology by means of Derringer’s desirability function. Stress samples were analyzed according to the experimental plan for fractional factorial screening design and Box-Behnken optimization design. The chromatographic separation was achieved on a C₁₈ Hypersil Gold aq. column (100 mm × 2.1 mm, 1.9 μm) with the mobile phase consisting of methanol–ammonium acetate buffer (10 mM, pH 3.43) mixture (0.9:99.1, v/v) pumped at a flow rate of 870 μL min^?1 and detection wavelength of 255 nm. The UPLC–MS and UPLC–MS/MS analyses were further used to characterize the found degradation products. The validation of the proposed method was also performed considering selectivity, linearity, accuracy, precision, limit of detection and limit of quantification, and the results indicated that the method fulfilled all required criteria. The method was successfully applied to the analysis of commercial tablets.     

Effects of Precursors and Plasma Parameters on Fullerene Synthesis in RF Thermal Plasma Reactor

Synthesis of fullerenes from graphite powders of different grade was studied in a radiofrequency (RF) plasma reactor. Dependence of fullerene yield on the properties and feed rate of precursors and on the helium content of plasma gas was studied in details. The fullerene yield was influenced by the mean size and the thermal conductivity of graphite particles on the one hand, and the helium content of the gas phase on the other. Soot containing fullerene mixture of 5.9% was produced in best conditions found in this work. The main component of the fullerene mixture was C₆₀. In addition, it contained about 30% of C₇₀ (corresponding to a C₆₀/C₇₀ mass ratio of 2.64). Higher fullerenes such as C₈₄ were also detected by mass spectroscopy (MS) and high performance liquid chromatography (HPLC).     

Effect of Vitamin B Complex Treatment on Macrophages to Schwann Cells Association during Neuroinflammation after Peripheral Nerve Injury

Peripheral nerve injury (PNI) triggers a complex multi-cellular response involving the injured neurons, Schwann cells (SCs), and immune cells, often resulting in poor functional recovery. The aim of this study was to investigate the effects of the treatment with vitamin B (B1, B2, B3, B5, B6, and B12) complex on the interaction between macrophages and SCs during the recovery period after PNI. Transection of the motor branch of the femoral nerve followed by reconstruction by termino-terminal anastomosis was used as an experimental model. Isolated nerves from the sham (S), operated (O), and operated groups treated with the B vitamins (OT group) were used for immunofluorescence analysis. The obtained data indicated that PNI modulates interactions between macrophages and SCs in a time-dependent manner. The treatment with B vitamins complex promoted the M1-to M2-macrophage polarization and accelerated the transition from the non-myelin to myelin-forming SCs, an indicative of SCs maturation. The effect of B vitamins complex on both cell types was accompanied with an increase in macrophage/SC interactions, all of which correlated with the regeneration of the injured nerve. Clearly, the capacity of B vitamins to modulate macrophages-SCs interaction may be promising for the treatment of PNI.     

Characterization of pottery from Republic of Macedonia. III. A study of comparative mineralogical detection efficiency using micro‐Raman mapping and X‐ray diffraction

Point‐to‐point micro‐Raman and X‐ray diffraction (XRD) techniques were employed for characterization of minerals present in the pottery body of 27 glazed Byzantine and Ottoman pottery shreds, excavated at two different archaeological sites in the Republic of Macedonia: in Skopje (Skopsko Kale) and in Prilep (Markovi Kuli and Sv. Atanas Church). The Raman spectra of 18 Byzantine samples (dating from 12th−14th century) and nine Ottoman samples (dating from 17th−19th century) revealed 26 different minerals. XRD measurements were further performed on the same powder samples to validate the mineralogical assessment obtained by point‐to‐point micro‐Raman spectroscopy. Although only 13 different mineral phases were obtained by the XRD, the results obtained from the Raman and XRD spectra for the most abundant minerals in the investigated pottery bodies match quite well. However, the identification of the less abundant minerals in the clay matrixes from the XRD data was very difficult, if at all possible. The results emphasize the specifics of the applied techniques and their limits. Additionally, wavelength dispersive X‐ray fluorescence spectroscopy was used for the elemental analysis. Copyright © 2011 John Wiley & Sons, Ltd.     

Kinetic study of the reaction Ca+ + N2O from 188 to 1207 K

Ion-molecule reactions involving metallic species play a central role in the chemistry of planetary ionospheres and in many combustion processes. The kinetics of the Ca(+) + N(2)O --> CaO(+) + N(2) reaction was studied by the pulsed multiphoton dissociation at 193 nm of organo-calcium vapor in the presence of N(2)O, followed by time-resolved laser-induced fluorescence spectroscopy of Ca(+) at 393.37 nm (4(2)P(3/2) <-- 4(2)S(1/2)). This yielded k(188-1207 K) = 5.45 x 10(-11) (T/300 K)(0.53) exp(282 K/T) cm(3) molecule(-1) s(-1), with an estimated accuracy of +/-13% (188-600 K) and +/-27% (600-1207 K). The temperature dependence of this barrierless reaction, with a minimum in the rate coefficient between 400 and 600 K, appears to be explained by the role of N(2)O vibrational excitation. This is examined using a classical trajectory treatment on a potential energy surface calculated at the B3LYP/6-311+g(2d,p) level of theory.