Determination of Lercanidipine Hydrochloride and Its Impurities in Tablets

The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for determination of lercanidipine hydrochloride and its synthetic impurities, degradation and oxidative products in Carmen^® tablets. The best separation was performed on Zorbax SB C18 column, 250 x 4.6 mm, particle size 5 m. Acetonitrile-water-triethylamine 55:44.8:0.2 (v/v/v) was used as a mobile phase with flow rate 1 mL min^–1. pH was adjusted to 3.0 with orthophosphoric acid. UV detection was performed at 240 nm. Duration of chromatographic run was about 12 min for six examined compounds. The chromatographic conditions for the determination of lercanidipine hydrochloride and its related substances were the same, but the concentration of lercanidipine hydrochloride was 0.03 mg mL^–1 for assay and 0.3 mg mL^–1 for related substances. The validation of the method performance characteristics (figures of merits, quality of parameters) was established to be adequate for the intended use. The evaluation of number of parameters, such as selectivity, linearity, accuracy, specificity, precision (repetability and reproducibility), sensitivity and detection and determination limits is entailed.Acknowledgements This work was supported by the Institute of Pharmacy of Serbia, Belgrade and by the Ministry for Science, Technology and Development of Serbia, Contact: 1458     

硅中浅杂质的激光感应光电导谱

首次采用光子能量小于硅中浅受主杂质电离能的可调谐远红外激光器作为激发源,获得了硅中浅受主杂质的光电导谱.可调谐半导体远红外激光器的调谐范围为380～500cm~(-1),光子流密度约10~(18)/cm~2·sec,用双光子跃迁对光电导谱进行了解释.对于Si:Al样品,光电导谱中的双峰分别相应于2P~1和2P~2中间态的双光子共振跃迁.也观察到了双光子透明的反共振现象.     

Recent radioactive ion beam program at RIKEN and related topics

Recent experimental programs at RIKEN concerning RI beams are reviewed. RIKEN has the ring cyclotron (RRC) with high intense heavy-ion beams and large acceptance fragment separator, RIPS. The complex can provide high intense RI-beams. By using the high intense RI-beams, a variety of experiments have been done. Recently, nuclear structure for unstable nuclei has been paid much attention. In special, disappearance and appearance of magic numbers are discussed experimentally and theoretically. Thus, in this review, related experiments concerning disappearance and appearance of magic numbers are described. Finally, future project in RIKEN, RI-beam factory. is introduced briefly.     

Synthesis and characterization of Rosuvastatin calcium impurity A; a HMG-CoA reductase inhibitor

During the process development for multistep synthesis of Rosuvastatin calcium several impurities were obtained along with the final Rosuvastatin calcium. Out of this; synthesis of impurity A (acetone adduct) a minor impurity of Rosuvastatin calcium (3R,5S,6E)-7-[4-(4-fluorophenyl)-2-[[(2-hydroxy-2-methylpropyl)sulfonyl(methyl)amino]-6-(1-methylethyl)-pyrimidin-5-yl]-3,5-dihydroxyheptenoicacid hemicalcium salt, is described. The synthesis of impurity A has been accomplished in 6 steps; starting from formation of β-hydroxy sulfonamide as the key intermediate and followed by using convenient routes with overall yield of 13.5%. The target compound can be used as the reference substance of impurity of the Rosuvastatin calcium.     

Ultra-high-speed liquid chromatography combined with mass spectrometry detection analytical methods for the determination of nitrosamine drug substance-related impurities

In the present study, five simple, feasible, and sensitive Ultra-high-speed liquid chromatography combined with mass spectrometry detection methods, using electrospray ionization are proposed. These methods were developed and validated for the determination of four different nitrosamine drug substance-related impurities—N-nitrosoacebutolol, N-nitrosobisoprolol, N-nitrosometoprolol, and N-nitrososotalol—in five beta blockers active pharmaceutical ingredients—acebutolol HCl, bisoprolol fumarate, metoprolol tartrate, metoprolol succinate, and sotalol HCl. The proposed methods were validated as per regulatory guidelines. Acquity HSS T3 (3.0 × 100 mm, 1.8 μm) column and formic acid 0.1% in water combined with methanol or acetonitrile were used for chromatographic separation in all methods. The limit of detection and the limit of quantification were found to be in the range of 0.02–1.2 and 2–20 parts per billion, respectively. The accuracy and precision of the five methods have been demonstrated in the working range of each one, giving values of recovery within the range of 64.1%–113.3%, and the regression coefficients (R) were found to be in the range of 0.9978–0.9999. These methods could be used for controlling nitrosamine drug substance-related impurities content for beta blockers drug substances batches manufactured at Moehs group.     

Influence of hydrostatic pressure on the diffusion of hydrogen in n-GaAs : Si

Hydrogen diffusion experiments have been performed in buried silicon doped GaAs epilayers under hydrostatic pressure. The deuterium diffusion profile in n-GaAs : Si depends on the hydrostatic pressure: a plateau followed by a steep decrease progressively appears as the pressure is increased. This has been interpreted as being due to the increasing importance of the trapping-detrapping process of H⁻ on Si⁺ donors during the hydrogen diffusion. This increase has been attributed to a deepening of the hydrogen acceptor level with respect to the bottom of the Γ conduction band of GaAs as the hydrostatic pressure increases.     

Studies on some alkali-phosphate glasses containing antimony and iron oxides

The effect of heat treatment on the Fe²⁺/Fe³⁺ ratio in some alkali phosphate glasses containing antimony and iron oxides has been investigated. Differential thermal analysis, Mossbauer spectroscopy, magnetic susceptibility and density measurements as well as the molar volume calculations were used in this study. The obtained data indicate that all glasses show approximately unchangeable stability. It is found, from the area under the Mossbauer absorption spectra that ferrous transformed gradually to ferric ions and the transformation rate constant was found to be 48 min⁻¹. The elapsed time was found to be 160 min. This transformation represents a first-order solid state reaction. The molar magnetic susceptibility measurements confirm the above results.     

水下Co-60源切伦科夫辐射的蒙卡模拟

随着核应用领域的不断拓宽,放射源丢失事故发生的概率也随之增加。机载伽马谱仪可有效搜寻地面放射源,然而对于放射源丢失于水域的情况,由于伽马射线经由水层屏蔽后可探测性降低,故利用放射源在水中产生的切伦科夫辐射对其进行搜寻显得十分重要。采用MCNP与Geant4相结合的方法,以及在Geant4程序中采用接续计算技巧,对Co-60源在水中的切伦科夫光产生以及传输进行了计算,计算表明,切伦科夫光经水中传播后,主要波段在300~600 nm,强度呈由边缘到中心渐强的特征分布,分布范围大致与放射源在水中的深度一致,在水中传输300 m后其光通量约为100 cm^-2,可利用光谱特征和强度分布特征对其进行测量。     

利用低能质子束产生高强度放射性束流

加拿大TRIUMF实验室利用¹¹C成功验证了一种产生高强度(～10⁸ions/s)放射性束流的方法. 该方法不同于普通在线同位素分离方法, 它利用了13MeV的低能强流质子束, 可以产生一系列核天体物理实验感兴趣的高强度放射性束流.