Isolation and characterization of process-related impurities and degradation products in larotaxel

2011 ◽  
Vol 55 (5) ◽  
pp. 1190-1196 ◽  
Author(s):  
Xin Che ◽  
Li Shen ◽  
Hui Xu ◽  
Ke Liu
Keyword(s):  
Degradation Products ◽  
Related Impurities ◽  
Isolation And Characterization

Identification, Characterization, and Quantification of Impurities of Safinamide Mesilate: Process-Related Impurities and Degradation Products

2017 ◽  
Vol 100 (4) ◽  
pp. 1029-1037 ◽  
Author(s):  
Liang Zou ◽  
Lili Sun ◽  
Hui Zhang ◽  
Wenkai Hui ◽  
Qiaogen Zou ◽  
...  
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Formation Mechanisms ◽  
Stability Indicating ◽  
Related Impurities ◽  
Related Substances ◽  
Water Ph ◽  
Bulk Drug ◽  
First Time

Abstract The characterization of process-related impurities and degradation products of safinamide mesilate (SAFM) in bulk drug and a stability-indicating HPLC method for the separation and quantification of all the impurities were investigated. Four process-related impurities (Imp-B, Imp-C, Imp-D, and Imp-E) were found in the SAFM bulk drug. Five degradation products (Imp-A, Imp-C, Imp-D, Imp-E, and Imp-F) were observed in SAFM under oxidative conditions. Imp-C, Imp-D, and Imp-E were also degradation products and process-related impurities. Remarkably, one new compound, identified as (S)-2-[4-(3-fluoro-benzyloxy) benzamido] propanamide (i.e., Imp-D), is being reported here as an impurity for the first time. Furthermore, the structures of the aforementioned impurities were characterized and confirmed via IR, NMR, and MS techniques, and the most probable formation mechanisms of all impurities proposed according to the synthesis route. Optimum separation was achieved on an Inertsil ODS-3 column (250 × 4.6 mm, 5 μm), using 0.1% formic acid in water (pH adjusted to 5.0) and acetonitrile as the mobile phase in gradient mode. The proposed method was found to be stability-indicating, precise, linear, accurate, sensitive, and robust for the quantitation of SAFM and its process-related substances, including its degradation products.

scholarly journals Synthesis, Isolation and Characterization of Process-Related Impurities in Oseltamivir Phosphate

2012 ◽  
Vol 9 (1) ◽  
pp. 113-120 ◽  
Author(s):  
Yogesh Kumar Sharma ◽  
Dau Dayal Agarwal ◽  
Sudesh Bhure ◽  
Sanjay Singh Rathore ◽  
Chakravir Rawat ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Mass Number ◽  
Reverse Phase ◽  
Related Impurities ◽  
Isolation And Characterization ◽  
Bulk Drug ◽  
Oseltamivir Phosphate

Three known impurities in oseltamivir phosphate bulk drug at level 0.1% (ranging from 0.05-0.1%) were detected by gradient reverse phase high performance liquid chromatography. These impurities were preliminarily identified by the mass number of the impurities. Different experiments were conducted and finally the known impurities were synthesized and characterized.

IMPURITY PROFILING IMPURITY PROFILING OF THIAMINE HYDROCHLORIDE INJECTION BY RP-HPLC AND CHARACTERIZATION OF DEGRADATION PRODUCT BY LC-MS/MS/QTOF

2020 ◽  
pp. 151-161
Author(s):  
SRINIVASU KONDRA ◽  
BAPUJI A. T. ◽  
D. GOWRI SANKAR ◽  
POTTURI MURALI KRISHNAM RAJU
Keyword(s):  
Degradation Product ◽  
Degradation Products ◽  
Hplc Method ◽  
Thiamine Hydrochloride ◽  
Injectable Formulation ◽  
Hyphenated Technique ◽  
Isolation And Characterization ◽  
Impurity Profiling ◽  
Rp Hplc

Objective: To propose a comprehensive, simple, and affordable RP-HPLC method for impurity profiling and characterization of unknown degradation products of thiamine hydrochloride injectable formulation. Methods: The chromatographic separation employs gradient mode using the octadecyl silane column using a mobile phase consisting of phosphate buffer with ion pair reagent, acetonitrile, and methanol delivered flow rate at 1.2 ml/min. The detection was carried out at 248 nm using empower software. LC-MS/MS/QTOF hyphenated technique was used for isolation and characterization of unknown degradation impurity. The performance of the method was systematically validated as per ICH Q2 (R1) guidelines. Results: Degradation product observed in accelerated stability was characterized by LC-MS/MS/QTOF hyphenated technique and found m/z value 351.1604 and postulated as an oxidative degradation product of thiamine due to excipient interaction. The validated method was sensitive, selective, and specific data proves the method is precise and accurate from LOQ to 150% level and results are within 95-108% and less than 4.5% RSD. The developed method is linear from 0.03-58.83 µg/ml with a correlation coefficient of more than 0.990 and LOD and LOQ value ranged from 0.03 to1.51 μg/ml. Conclusion: An efficient RP-HPLC method for impurity profiling of thiamine injectable formulation was successfully developed and unknown degradation product observed instability condition samples characterized by LC-MS/MS/QTOF technique. The validated method can be successfully employed for the impurity profiling of thiamine injectable in the quality control department.

Isolation and characterization of related impurities in andrographolide sodium bisulphite injection

RSC Advances ◽  
2016 ◽  
Vol 6 (34) ◽  
pp. 28830-28837 ◽  
Author(s):  
Ji-Qin Hou ◽  
Bao-Lin Wang ◽  
Xiao-Jun Huang ◽  
Xiao-Qi Zhang ◽  
Guo-Qiang Li ◽  
...  
Keyword(s):  
Infectious Diseases ◽  
Sodium Bisulphite ◽  
Related Impurities ◽  
Isolation And Characterization

Andrographolide sodium bisulphite (ASB) injection was widely used in China for the treatment of infectious diseases.

scholarly journals Isolation and characterization of glial filaments from human brain.

1978 ◽  
Vol 78 (2) ◽  
pp. 426-440 ◽  
Author(s):  
J E Goldman ◽  
H H Schaumburg ◽  
W T Norton
Keyword(s):  
White Matter ◽  
Gel Electrophoresis ◽  
Degradation Products ◽  
Neurofilament Proteins ◽  
Human Central Nervous System ◽  
Neurofilament Protein ◽  
Isolation And Characterization ◽  
Single Protein ◽  
Filament Protein

Intermediate (8--9 nm) filaments of human central nervous system astrocytes were isolated from the gliosed white matter of cases of adrenoleukodystrophy (ALD). This hereditary lipidosis is characterized pathologically by demyelination, loss of axons, and replacement of the white matter of the caudal cerebrum by a glial scar. Glial filaments were composed largely of a single protein component with a mol wt of about 49,000 daltons. Smaller components (44,000--39,000 daltons) were detected in some samples, and appear to represent degradation products of the filament protein. Human neurofilaments were isolated from the normal frontal white matter of ALD cases by the standard myelin-free axon technique. Isolated glial and neurofilament proteins comigrated during acrylamide gel electrophoresis in SDS. Polypeptides resulting from cyanogen bromide cleavage of the two filament proteins were the same. Both proteins reacted with rabbit antisera raised against isolated bovine neurofilament protein and human glial fibrillary acidic protein.

scholarly journals Novel heparin degradation products. Isolation and characterization of novel disaccharides and oligosaccharides produced from heparin by bacterial degradation

1968 ◽  
Vol 108 (4) ◽  
pp. 647-654 ◽  
Author(s):  
Carl P. Dietrich
Keyword(s):  
Paper Chromatography ◽  
Uronic Acid ◽  
Degradation Products ◽  
Gel Filtration ◽  
Present Knowledge ◽  
Bacterial Degradation ◽  
Isolation And Characterization ◽  
Flavobacterium Heparinum

1. Heparin was degraded by enzymes of adapted Flavobacterium heparinum. Several degradation products were separated by combined Sephadex-gel filtration and paper chromatography, and chemically analysed. 2. These products were identified as glucosamine 2,6-disulphate, saturated disaccharides constituted of uronic acid and glucosamine and containing two and three sulphate residues, and tetra- and hexa-saccharides with the same basic disaccharide units. 3. The implications of these findings with respect to the present knowledge of heparin structure and its enzymic degradation are discussed.

Identification, isolation and characterization of process related impurities in ezetimibe

2014 ◽  
Vol 88 ◽  
pp. 385-390 ◽  
Author(s):  
Srikanth Guntupalli ◽  
Uttam Kumar Ray ◽  
N. Murali ◽  
P. Badrinadh Gupta ◽  
Vundavilli Jagadeesh Kumar ◽  
...  
Keyword(s):  
Related Impurities ◽  
Isolation And Characterization
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