Determination of the degree of degradation of specific impurity B contained in the substance of the drug «Lomustine» by high-resolution HPLC–MS/MS method

2021 ◽  
pp. 56-65
Author(s):  
Irina Olegovna Reshetnikova ◽  
Sergey Vasilievich Metlitskikh ◽  
Nadezhda Dmitrievna Stekleneva ◽  
Aleksandr Nikolaevich Volov
Keyword(s):  
High Resolution ◽  
Degradation Product ◽  
European Pharmacopoeia ◽  
Specific Impurity ◽  
Degree Of Degradation

A high-resolution HPLC–MS/MS method was proposed for the study of solutions of standards of specific impurity B contained in the substance of the drug «Lomustine», which is included in the List of Vital Medicines. A characteristic degradation product of specific impurity B, the content and quantity of which is not regulated by the European Pharmacopoeia, has been found.

scholarly journals Development of Validated and Stability-Indicating LC-DAD and LC-MS/MS Methods for Determination of Avanafil in Pharmaceutical Preparations and Identification of a Novel Degradation Product by LCMS-IT-TOF

Molecules ◽  
2018 ◽  
Vol 23 (7) ◽  
pp. 1771 ◽  
Author(s):  
Nafiz CAN
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Resolution ◽  
Quantitative Determination ◽  
Degradation Product ◽  
Degradation Products ◽  
Pde5 Inhibitor ◽  
Forced Degradation ◽  
Qualitative Determination

Avanafil (AVA), one of the most effective drugs prescribed for erectile dysfunction, is a pyrimidine-derivative PDE5 inhibitor. In the current work, new LC methods were developed and validated for quantitative determination of avanafil and qualitative determination of its degradation products. The quantitative determination of avanafil was carried out using liquid chromatography with photodiode array detection (LC-DAD) and liquid chromatography-tandem mass spectrometry LC-MS/MS methods, and fully validated according to the ICH Q2 (R1) guideline, while qualitative determination was performed using a liquid chromatography mass spectrometry-ion trap-time of flight (LCMS-IT-TOF) instrument. The separation of avanafil and its degradation products was carried out using the same reversed-phase chromatographic conditions, in which a second-generation C18-bonded monolithic silica column (Chromolith® High Resolution RP-18e, 100 × 4.6 mm, Merck KGaA) was used as stationary phase. Briefly, the methods enable quantitation of avanafil with high accuracy (recovery > 95%) and precision (RSD% < 2.0), within the ranges of 0.5–20 μg/mL for LC-DAD and 150–6000 ng/mL for LC-MS/MS. In the forced degradation studies, over and above currently existing data, a new oxidation-based degradation product, whose predicted m/z is 367.1168, was identified and its structure was confirmed by high-resolution mass spectrometric analysis. As the main advantage, either an LC-DAD or LC-MS/MS instrument can be chosen for interference-free quantitation of AVA, according to the facilities in quality-control laboratories.

High-resolution microscopy of twin boundaries in gold

1987 ◽  
Vol 45 ◽  
pp. 260-261
Author(s):  
William Krakow ◽  
David A. Smith
Keyword(s):  
High Resolution ◽  
Specimen Preparation ◽  
Gold Films ◽  
Boundary Area ◽  
Transmission Electron ◽  
Recent Developments ◽  
Tilt Boundaries ◽  
High Resolution Microscopy ◽  
Twist Boundaries

Recent developments in specimen preparation, imaging and image analysis together permit the experimental determination of the atomic structure of certain, simple grain boundaries in metals such as gold. Single crystal, ∼125Å thick, (110) oriented gold films are vapor deposited onto ∼3000Å of epitaxial silver on (110) oriented cut and polished rock salt substrates. Bicrystal gold films are then made by first removing the silver coated substrate and placing in contact two suitably misoriented pieces of the gold film on a gold grid. Controlled heating in a hot stage first produces twist boundaries which then migrate, so reducing the grain boundary area, to give mixed boundaries and finally tilt boundaries perpendicular to the foil. These specimens are well suited to investigation by high resolution transmission electron microscopy.

High-Resolution Image Simulation of a Tilted Crystal

1990 ◽  
Vol 48 (1) ◽  
pp. 68-69
Author(s):  
C. J. D. Hetherington
Keyword(s):  
High Resolution ◽  
Crystal Thickness ◽  
Thin Specimen ◽  
Atomic Structures ◽  
Kikuchi Lines ◽  
High Resolution Images ◽  
Final Estimate ◽  
Simulated Images ◽  
Habit Planes

Most high resolution images are not directly interpretable but must be compared with simulations based on model atomic structures and appropriate imaging conditions. Typically, the only parameters that are adjusted, in addition to the structure models, are crystal thickness and microscope defocus. Small tilts of the crystal away from the exact zone axis have only rarely been considered. It is shown here that, in the analysis of an image of a silicon twin intersection, the crystal tilt could be accurately estimated and satisfactorily included in the simulations.The micrograph shown in figure 1 was taken as part of an HREM study of indentation-induced hexagonal silicon. In this instance, the intersection of two twins on different habit planes has driven the silicon into hexagonal stacking. However, in order to confirm this observation, and in order to investigate other defects in the region, it has been necessary to simulate the image taking into account the very apparent crystal tilt. The inability to orientate the specimen at the exact [110] zone was influenced by i) the buckling of the specimen caused by strains at twin intersections, ii) the absence of Kikuchi lines or a clearly visible Laue circle in the diffraction pattern of the thin specimen and iii) the avoidance of radiation damage (which had marked effects on images taken a few minutes later following attempts to realign the crystal.) The direction of the crystal tilt was estimated by observing which of the {111} planes remained close to edge-on to the beam and hence strongly imaged. Further refinement of the direction and magnitude of the tilt was done by comparing simulated images to experimental images in a through-focal series. The presence of three different orientations of the silicon lattice aided the unambiguous determination of the tilt. The final estimate of a 0.8° tilt in the 200Å thick specimen gives atomic columns a projected width of about 3Å.

Determination of the Activity of Pulmonary Tuberculosis: the Utility of High-Resolution Computed Tomography

2000 ◽  
Vol 42 (5) ◽  
pp. 757
Author(s):  
Myung Hee Chung ◽  
Hae Giu Lee ◽  
Won Jong Yu ◽  
Hong Jun Chung ◽  
Bo Sung Yang ◽  
...  
Keyword(s):  
Computed Tomography ◽  
High Resolution ◽  
Pulmonary Tuberculosis ◽  
High Resolution Computed Tomography
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